Illuka Midwest Ltd v Wimmera Industrial Minerals Pty Ltd
[2001] APO 58
•27 July 2001
OFFICIAL NOTICE
DECISION OF A DELEGATE OF THE COMMISSIONER OF PATENTS
Application : Nos. 676682 in the name of ILUKA MIDWEST LIMITED
Title: Treatment of Titaniferous Materials
Action: Opposition under section 59 of the Patents Act that the nominated person is not entitled to a grant of a patent for the invention, and a request under section 32 of the Patents Act for a determination of the Commissioner as to the name in which the application is to proceed, by WIMMERA INDUSTRIAL MINERALS PTY LTD
Decision: Issued .
Abstract
The invention relates to a process for removing uranium and thorium from titaniferous materials such as ilmenite in which the material is heated to a temperature selected to enhance the accessibility of the parent isotopes and their radioactive decay chain progeny, and contacted with a reagent which forms a phase at the elevated temperature and disperses onto the internal grain surfaces of the titaniferous material to incorporate the parent and progeny radionuclides for subsequent removal by leaching. In practice the reagent forms a liquid phase at elevated temperature into which the radionuclides deport, and then cools to a leachable impurity bearing phase. The reagent is preferably a glass forming reagent.
In 1990 the Commonwealth Scientific and Industrial Research Organisation (CSIRO) were commissioned by the opponent on a confidential basis to undertake research aimed at reducing the level of uranium and thorium contaminants in their zirconium silicate (zircon) deposits. The CSIRO research team included a Dr Grey. The process developed used lime roasting prior to acid leaching to form a silicate glass phase which aided decomposition of the zircon lattice and selective deportation of the radionuclides to that phase.
It was subsequently proposed that CSIRO investigate silica removal from the opponent's high titanium (HiTi) concentrate allegedly on the basis of the link which had been found in the zircon work between the formation of a glass phase and radionuclide removal. In June 1992 Dr Grey was sent a scoping proposal for test work on a process (the soda roast process) for the removal of silica from HiTi. It was agreed that this work would be treated as an extension of the zircon work so as to avoid the need for separate confidentiality agreements. The soda roast process involved the addition of soda ash and roasting (heating) to form a glass phase before removal by caustic leaching. A memorandum was prepared by the opponent in July 1992 describing a process for the removal of a range of impurities, including silica and radionuclides, from HiTi and ilmenite when processed as a combined stream (the RUTILE process).
In 1990 CSIRO were engaged by the applicant to undertake a project concerning the removal of thorium and uranium radionuclides from ilmenite. The project ultimately became known as SREP (Synthetic Rutile Enhancement Process) from which the invention has evolved. By mid-July 1992 the SREP project team were continuing to investigate various heating and leaching regimes as a possible means of removing the radionuclides. The research focus shifted within a relatively short period subsequent to Dr Grey's direct involvement with the project to the formation of a glass phase under heat treatment conditions.
The opponent has asserted they are the inventor and that the applicant obtained the invention through them by means of the unauthorised use of information which the opponent had disclosed to third parties on a confidential basis. This disclosure is said to have included information and concepts derived from the opponent's zircon and RUTILE processes which had shown, firstly, that the formation of a glass phase at temperature in the lime roasting of zircon promoted the removal of radionuclides and, secondly, that an impurity bearing glass phase could also be used for removing radioactive impurities from HiTi concentrate using a soda roast process. It is specifically asserted that a serious question arises as to whether Dr Grey misused confidential information belonging to the opponent given that he was the principal source of SREP and the only CSIRO researcher who conducted work on behalf of both the applicant and the opponent.
Found:
Dr Grey knew from the zircon process that the formation of a glassy phase assisted the removal of thorium
Dr Grey was not made aware of the RUTILE process - the only information disclosed to him by the opponent was in respect of the soda roast process which did not contemplate the removal of radionuclides
The conduct of the SREP project team does not show that the line of enquiry followed by them was aided by knowledge of the opponent's confidential information. In particular, the evidence showed that Dr Grey was in all likelihood the first among the team to suggest the addition of glass forming agents so as to form a leachable phase which would take up the radionuclides. However, there was insufficient evidence to establish that this proposal had arisen other than from his experimental studies which were catalysed by the team's earlier test results, rather than from information communicated to him by the opponent in confidence.
Opposition consequently dismissed and the application to continue to proceed in the name of the applicant alone. Claim 39 coincidentally found to lack fair basis.
PATENTS ACT 1990
DECISION OF A DELEGATE OF THE COMMISSIONER OF PATENTS
Re:Patent Application No. 676682 in the name of Iluka Midwest Limited, and opposition under section 59 of the Patents Act that the nominated person is not entitled to a grant of a patent for the invention, and a request under section 32 of the Patents Act for a determination of the Commissioner as to the name in which the application is to proceed, by Wimmera Industrial Minerals Pty Ltd
BACKGROUND
Patent application 676682 in the name of Iluka Midwest Limited (formerly RGC Mineral Sands Limited, and hereafter referred to simply as Iluka) was filed on 28 July 1993 as PCT/AU93/00381 claiming priority from provisional applications PL3876 and PL6401 filed on 31 July 1992 and 16 December 1992, respectively. The patent application was advertised accepted on 20 March 1997.
Wimmera Industrial Minerals Pty Ltd (more conveniently referred to as WIM) filed a notice of opposition under section 59 of the Patents Act 1990 (the Act) on 19 June 1997 followed by a statement of grounds and particulars on 19 September 1997. Service of evidence in support was completed on 19 February 1998 after WIM had been granted a number of extensions of time without objection. Evidence in answer was due to be served by 19 May 1998 but on that date Iluka applied for an extension of time to 19 July. WIM objected to the extension sought and the matter was fixed for hearing on 24 June. Meanwhile, on 18 June, Iluka commenced proceeding NG 598 of 1998 in the Federal Court seeking (among other things) an order restraining WIM from representing to any person, including the Commissioner, that the invention or any part of it was obtained by Iluka from WIM. This is the only ground of opposition pursued by WIM in the present proceeding.
On 22 June Iluka sought a direction under regulation 5.10(1) that the service of evidence in answer be deferred to a date three months after the determination of proceeding NG 598 of 1998. The effect of the direction sought by Iluka would have been to stay the opposition proceeding pending the outcome of the Federal Court proceeding. I heard this matter concurrently with Iluka's application for an extension of time and found that although the extension sought was appropriate in all the circumstances, these did not favour deferring the service of evidence in answer until after the court proceeding had been determined (see RGC Mineral Sands Limited vWimmera Industrial Minerals Pty Ltd [1998] APO 43).
In the event, service of evidence in answer was completed on 23 October 1998, and service of evidence in reply on 26 July 1999. Nonetheless, in a further Federal Court proceeding (NG 981 of 1998), Iluka sought a review under the Administrative Decisions (Judicial Review) Act 1977 (the AD(JR) Act) of my decision to refuse to direct that the service of their evidence be deferred as requested. In RGC Mineral Sands Ltd v Wimmera Industrial Minerals Pty Ltd [1999] FCA 17 the court held that the opposition proceeding should go forward to a hearing in the usual way, and dismissed the AD(JR) Act proceeding.
At the request of WIM the Commissioner issued notices under section 210 for the production of documents to three parties on 23 December 1998 - Iluka, the Commonwealth Scientific and Industrial Research Organisation, and the Australian Nuclear Science and Technology Organisation. This was followed by a request from Iluka seeking the production of certain documents, and notices were issued to the Commonwealth Scientific Industrial Research Organisation on 29 October 1999 and to WIM on 8 November 1999. The documents produced in response to all notices are commercially sensitive and were for that reason treated as prescribed documents for the purpose of section 55 by virtue of regulation 4.3(2)(b). Access to these documents was subsequently granted by the Commissioner pursuant to section 56(1)(b) subject to undertakings of confidentiality agreed to by the parties.
On 11 November Iluka made a request under regulation 5.10(4) to serve further evidence which was granted by the delegate after hearing the matter on 7 December (see RGC Mineral Sands Ltd v Wimmera Industrial Minerals Pty Ltd [1999] APO 79). Service of this evidence was completed on 28 January 2000. The delegate also afforded WIM the opportunity to respond to the further evidence which they did on 17 and 18 February.
On 20 December 1999 WIM made a request for a determination under section 32 that the application proceed to grant in the name of WIM alone. A notice of the request was published on 20 January 2000 with the result that the time allowed by regulation 3.6(4) for a party wishing to be heard to notify the Commissioner fell after the period which had been set aside for hearing the section 59 opposition. The Commissioner accordingly proposed in a letter dated 22 December:
… that the hearing date proceed for both matters (the section 32 and 59) on the date currently set for the section 59 opposition. The section 32 matter will be determined as part of the section 59 opposition proceedings on the basis of the material served in the section 59 opposition. If a third party expresses a desire to be heard in the proceedings then a separate procedure will de [sic] developed to deal with this unlikely eventuality.
This proposal was adopted with the consent of the parties.
ABBREVIATIONS
In this decision I will use the following abbreviations:
AMDEL AMDEL Limited
ANSTO: Australian Nuclear Science and Technology Organisation
ARL Australian Radiation Laboratory
CCWA Chemistry Centre of WA
CRA CRA Limited
CSIRO: Commonwealth Scientific and Industrial Research Organisation
Lakefield Lakefield Research
SEM Scanning Electron Microscope
XRD X-ray Diffraction
THE HEARING
Attendances
Iluka were represented by Mr David Catterns QC assisted by Ms Sophie Goddard of Counsel, Mr Greg Noonan, patent attorney of Freehills Patent Attorneys, and Messrs Paul Fitzpatrick, Scott Crabb and Cameron Belyea, solicitors of Clayton Utz. WIM were represented by Dr John Emmerson QC assisted by Mr Peter Collison of Counsel, and Messrs Andrew Goatcher and Richard Hamer, solicitors of Arthur Robinson & Hedderwicks. Messrs David Smith and Keir Bristow of Corrs Chambers Westgarth, solicitors for CSIRO, and Mr Richard Aldous of Iluka, also attended.
Cross-Examination
Each party requested that the Commissioner summon a number of the other party's declarants under section 210 to appear at the hearing for cross-examination, and summonses were duly issued to:
As requested by Iluka: Michael John Hollitt
Frank Lawson
Matthew John Liddy
Ross Alexander McClelland
As requested by WIM: Halil Aral
Warren George Bruckard
Michael Paul Brungs
David Edward Freeman
Ian Edward Grey
Harold Robert Harris
Martin Richard Houchin
Kenneth John McDonald
Richard Ralph Merritt
Graham Jeffrey Sparrow
All but Messrs Bruckard, Freeman and McDonald were called on to give evidence. On 17 February 2000 WIM requested the Commissioner to summon Christina Li and Julian Land to provide oral evidence in chief which, as intimated by Mr Catterns, was likely to constitute "further evidence" (cf. paragraph 3.4.2 of Volume 3 of the Australian Patent Office Manual of Practice and Procedure) and thus the request would be subject to the Commissioner's discretionary power conferred by regulation 5.10. However, Dr Emmerson advised late in the hearing that evidence would not be taken from either witness.
Request for Directions
In a letter dated 15 February 2000 WIM advised that in view of the confidential nature of the material to be presented during the course of the hearing they intended to seek directions under regulation 5.10(1) that:
(a) the hearing be closed to the public; and
(b) the transcript of the hearing be confidential.
WIM also advised of their intention to seek directions that each witness not be permitted:
(c) in the hearing room as an observer unless that witness has completed giving his evidence;
(d) to discuss his testimony, or the testimony of any other witness, with any other witness until
both he and that witness have completed giving their evidence; or
(e) except with the consent of the other party to the proceeding, to discuss his testimony, or that of
any other witness, with any person while in the course of being cross-examined.
On 18 February Iluka confirmed their objection to the directions sought, particularly those arising under (a), (b) and (c) above, and the matter was further debated by the parties on the first day of the hearing. As described by Mr Collison, the directions essentially fell into two distinct categories: "The first is concerned with general issue of the confidentiality of the proceeding and access to the public; the second is concerned with the issue of witnesses who are yet to give evidence and what restrictions they should be under."
Regarding the first category, Mr Collison submitted that although hearings before the Commissioner are normally open to the public, it was evident from paragraph 2.12.5(a) of the Manual of Practice and Procedure that a different situation arises where, as in the present proceeding, reliance is placed on confidential material. He further submitted that the hearing transcript (see below) would inevitably contain references to such material and, as a consequence, should not be made a public document. In response Mr Catterns argued that a large proportion of the material to be discussed was not confidential. In taking this line of argument further he pointed out that none of the declarations filed in the opposition or the large mass of exhibits accompanying the evidence in support were confidential, and information belonging to the parties which is relevant to the present action is contained in a number of patent specifications already in the public domain. Mr Catterns went on to say that Iluka did not object to WIM's material remaining confidential if so-requested, but waived that right in respect of their own material which to date had been subject to the agreed confidentiality regime.
With regard to the second category, Mr Collison submitted that the usual practice is to have witnesses ordered out of court on the application of a party. To support this proposition he took me to R v Tait [1963] VR 520, a decision of the Full Court of the Supreme Court of Victoria, where at pages 522-523 it was said:
… it has become so customary in both civil and criminal trials for an order to be made ordering all witnesses out of court, that any party who applies for such an order has a right to have such an order made, at all events unless most cogent reasons are advanced why it should not be made in the particular case or why an exception should be made in favour of particular witnesses. It is true that such orders are frequently made and are nearly always made without excepting particular witnesses if such exception is objected to. In civil proceedings it is the practice, if not the rule, to except parties from the order, though even a party usually leaves the court while his own witnesses are giving evidence if he has not himself already given his evidence.
Mr Collison said that the final passage above refers to the well-known exception of a party to a proceeding in a court being entitled to remain in the courtroom, notwithstanding that he or she may be a witness, to enable them give instructions to their legal representative as to the conduct of the proceeding. He said this exception was also reflected in paragraph 3.5 of the Manual of Practice and Procedure which states:
where the witness is closely associated with the action, it is appropriate for him, on request of his counsel, to remain in the hearing room throughout the cross-examination. (my emphasis)
Mr Catterns argued that an effect of the direction proposed under (c) above is that Iluka would be deprived of technical assistance during cross-examination of WIM's witnesses, while WIM would benefit from the unrestrained presence of their counterpart technical experts during cross-examination of Iluka's witnesses. He further contended that Dr Grey should also be allowed to attend the hearing, or be granted access to the transcript, before giving evidence in view of the body of evidence put forward by WIM which clearly implicated Dr Grey in the alleged unauthorised disclosure of WIM's confidential information to Iluka.
In relation to the first point raised on behalf of Iluka, Mr Collison conceded that expert witnesses were a further exception to court orders of the type referred to in R v Tait and, after subsequent discussion, it was agreed that Professor Brungs and Dr Merritt could attend the hearing as technical advisors to Iluka before giving evidence, but not while WIM confidential information was being considered. A similar agreement was reached with respect to the transcript. However, Mr Collison resisted the presence of Dr Grey and drew attention to the risk of witnesses who have yet to testify tailoring their evidence to what has gone before.
It is well settled that in an opposition proceeding the Commissioner functions as an administrative tribunal whose role is to determine the truth of the matter before it, and in that light "is master of its own procedure, provided that the rules of natural justice are applied" (per T A Miller Ltd v The Minister for Housing and Local Government andAnother (1968) 1 WLR 992). This is entirely consistent with the general principle upheld by the Supreme Court in R v Tait that:
whether a witness should be allowed in Court, or ordered out of Court is, in the last analysis, a question in the discretion of the trial Judge and that discretion should be exercised in the way in which the Judge deems 'most conducive to the investigation of truth' … in the case before him.
Dr Grey is not a party to the present proceeding, and nor did Iluka seek permission for him to remain in the hearing room as an expert witness. However, I note that the proceeding is grounded on the assertion that Iluka obtained the invention from WIM through the unauthorised use of information which WIM disclosed in confidence to various research organisations, but which they, in breach of confidence, disclosed to Iluka. This assertion is further qualified as follows by the statement of particulars:
… employees of [CSIRO] who had access to the whole or part of the confidential information of the Opponent … including the said invention, assisted the Applicant in the making of the invention allegedly made by the Applicant being the subject of the opposed application and contributed to that invention as nominated inventors of the alleged invention …
It is plainly evident from the material before me that it is Dr Grey who is said to have used confidential information belonging to WIM in work undertaken by him for Iluka which led to the claimed invention. Thus, as put by Mr Collison, Dr Grey "is the central witness in this proceeding". Consequently, the principles of natural justice in my view weigh heavily in favour of allowing Dr Grey to hear or (what amounts practically to the same thing) to read the transcript of any allegations made against him during cross-examination regarding the unlawful transfer of WIM's confidential information to Iluka. The assistance to be potentially derived from Dr Grey's attendance throughout cross-examination in the elucidation of the truth is clearly another relevant consideration. As stated in R v Tait "The Crown desires to call evidence in rebuttal, but it seems to me to be an extraordinary situation if their … witnesses who were to give evidence in rebuttal were not allowed to be present to hear the evidence which they are being called to rebut." This, in my opinion, applies by analogy to the present circumstances.
Although they merely reflect standard hearings procedure, Iluka did not object to the directions sought under (d) and (e) above. With regard to the direction sought under (a), a number of the documents filed in the opposition proceeding have, as mentioned earlier, been treated as prescribed documents which I note from the Manual of Practice and Procedure is a situation where it is appropriate to close the hearing to the public.
On this basis I gave the following directions:
The hearing is closed to the public
The transcript of the hearing is confidential insofar as it relates to material indicated by WIM as being confidential
With the exception of Doctors Grey and Merritt, and Professor Brungs, a witness due to give evidence is not allowed to read the transcript of the hearing
With the exception of Doctors Grey and Merritt, and Professor Brungs, a witness is not allowed in the hearing room as an observer unless that witness has completed giving his evidence
A witness is not allowed:
(a)to discuss his testimony, or the testimony of any other witness, with any other witness until both he and that witness have completed giving their evidence; or
(b)except with the consent of the other party to the proceeding, to discuss his testimony, or that of any other witness, with any person while in the course of being cross-examined
Consistent with the first and second of these directions, I indicated to the parties that they would be afforded an opportunity to advise whether the reasons for my decision incorporated confidential material which, as a consequence, should be omitted from the published version (cf. Secton PtyLtd and Another v Delawood Pty Ltd and Others 21 IPR 136).
Hearing Sessions
The hearing was held in Melbourne from 21 February to 3 March 2000, and was re-convened on 8 and 9 March to complete oral examination. The hearing was again adjourned until 5-7 April to allow each party to present their closing submissions.
Transcript of Proceeding
Given the length of the hearing, and the emphasis placed on oral examination, the parties arranged for the provision of a "real time" transcription service. Hard copy transcript (TS) was also made available to the Commissioner for each day of the hearing.
MATERIAL FILED IN THE OPPOSITION
Declaratory Evidence
Aside from the extensive number of documents produced in response to the various notices which issued under section 210, statutory declarations made by the following persons were filed as evidence for the purposes of the opposition proceeding:
Evidence in Support
Michael John Hollitt together with exhibits MJH-1 to MJH-98 (1 Hollitt)
Frank Lawson together with exhibits FL-1 to FL-5 (1 Lawson)
Helen Mary Joan Rofe together with exhibit HMR-1 (Rofe)
Matthew Jon Liddy (Liddy)
Ross Alexander McClelland together with exhibit RAM-1 (McClelland)
Evidence in Answer
Ian Edward Grey together with exhibits IEG-1 to IEG-8 (1 Grey)
Halil Aral together with exhibits HA-1 to HA-5 (Aral 1)
Harold Robert ("Rob") Harris together with exhibits HRH-1 to HRH-21 (1 Harris)
Graham Jeffrey Sparrow together with exhibits GJS-1 to GJS-5 (1 Sparrow)
Martin Richard Houchin (1 Houchin)
David Edward Freeman (Freeman)
Kenneth John McDonald (McDonald)
Christopher Fleming (Fleming)
Warren John Bruckard (Bruckard)
The material contained in all exhibits accompanying the declaration of Mr Harris (except HRH-7 and HRH-20) is subject to a confidentiality regime set out in orders of the Federal Court, which regime has been incorporated in the terms upon which access to the produced documents was granted by the Commissioner under section 56(1)(b). These terms also apply to the material contained in exhibits IEG-4 to IEG-6, HA-2 to HA-4, HA-6, and GJS-2 to GJS-4.
Evidence in Reply
Michael John Hollitt together with exhibit MJH-99 (2 Hollitt)
Frank Lawson together with exhibits FL-6 to FL-16 (2 Lawson)
With the exception of FL-9, the material exhibited by these declarants is subject to the terms of access mentioned above.
Iluka Further Evidence
Graham Jeffrey Sparrow together with exhibits GS6 to GS8 (2 Sparrow)
Harold Robert Harris together with exhibits HRH22 to HRH34 (2 Harris)
Martin Richard Houchin (2 Houchin)
Halil Aral together with exhibits HA-7 to HA-10 (2 Aral)
Ian Edward Grey together with exhibits IEG 9 to IEG 17 (2 Grey)
Richard Ralph Merritt together with exhibits RM1 to RM6 (Merritt)
Michael Paul Brungs together with exhibits MB1 to MB6 (Brungs)
WIM Evidence in Response
Michael John Hollitt (3 Hollitt)
Frank Lawson (3 Lawson)
Court Book
To assist the conduct of the hearing, material which had either been filed as evidence or produced to the Commissioner was included in an indexed and paginated "court book" (CB). The first 13 volumes of the court book contain the declarations and exhibits filed during the evidentiary stages of the opposition, while additional material from the produced documents which each party anticipated would be referred to during oral examination was included in Volumes 15-27.
This court book was supplemented by Volumes 1 and 2 of Iluka's "Additional Bundle of Documents" (TB), and 4 volumes of material titled "Daily Activity Schedule".
Other Material
The original laboratory notebooks of a number of the witnesses were referred to during the course of the hearing but otherwise remained in the care of the respective legal representatives. However, full copies Dr Grey's notebooks covering the period 3 June 1991 to 18 March 1993 were made available to the parties and their nominated technical advisors by the representatives for CSIRO. Mr Smith indicated that these notebooks contained information of a confidential nature belonging to third parties as a consequence of which I directed that that information was subject to the confidentiality regime previously established in relation to the material produced to the Commissioner (see above).
Further, and as agreed between the parties, WIM filed a copy of their closing submissions on 22 March 2000 which was followed by a copy of Iluka's closing submissions on 30 March. WIM filed a copy of their submissions in reply on 7 April.
THE SPECIFICATION
The specification indicates that the invention relates to a process for facilitating the removal of impurities such as radionuclides from titaniferous materials, and in particular is concerned with the removal of uranium and thorium from weathered or "altered" ilmenite and products formed from the ilmenite.
Ilmenite (FeTiO3) and rutile (TiO2) are the major commercially-important mineral feedstocks for titanium metal and titanium dioxide production. Although ilmenite and rutile almost invariably occur together in nature as components of "mineral sands" or "heavy minerals", ilmenite is usually the most abundant. Natural weathering of ilmenite results in partial oxidation of the iron, originally present in the ferrous state, to ferric iron. To maintain electrical neutrality, some of the oxidised iron must be removed from the ilmenite lattice. This results in a more porous structure with a higher titanium (lower iron) content. Such weathered materials (eg. leucoxene) are known as "altered" ilmenites and may have TiO2 contents in excess of 60%. As weathering, or altering, of the ilmenite proceeds, impurities such as alumino-silicates (clays) are often incorporated into the porous structure as discrete, small grains that reside in the pores of the altered ilmenite. It appears that uranium and thorium can also be incorporated into the ilmenite pores during this process.
Most of the world's mined ilmenite is used for the production of titanium dioxide pigments for use in the paint and paper industries. Pigment grade TiO2 has been traditionally produced by reacting ilmenite with concentrated sulphuric acid and subsequent processing to produce a TiO2 pigment - the so-called sulphate route. However, this process is becoming increasingly undesirable on environmental grounds. The alternative process - the so-called chloride route - involves reaction with chlorine to produce volatile titanium tetrachloride and subsequent oxidation to TiO2. Unlike the sulphate route, the chloride route is capable of handling feedstocks, such as rutile, which are high in TiO2 content and low in iron and other impurities. The chloride route consequently presents fewer environmental problems and has become the preferred method for TiO2 pigment production.
The specification explains that as natural rutile supplies are insufficient to meet the world demands of the chloride route process, there is an increasing need to convert the more plentiful ilmenites and altered ilmenites to synthetic rutile (SR). A number of different processes have been developed to upgrade ilmenite to synthetic rutile, the most commonly used on a commercial scale being the Becher process. This process involves reducing the iron in ilmenite to metallic iron in a reduction kiln at high temperatures (900-1200oC) to give so-called reduced ilmenite, then oxidising the metallic iron in an aerator to produce a fine iron oxide that can be physically separated from the coarse titanium-rich grains forming a synthetic rutile which typically contains more than 90% TiO2. In a modification of the Becher process sulphur is added to the kiln to facilitate the removal of manganese and residual iron impurities by the formation of sulphides which are removed in the acid leach.
The Murso process is another known (but commercially little used) process which involves the oxidation of ilmenite at 800-1000oC followed by a reduction at 700-900oC to convert the iron to a ferrous state. The product is then leached with hydrochloric acid at atmospheric pressure. The solid leach product is washed and calcined to give synthetic rutile.
Whether ilmenite is marketed as the raw material or as synthetic rutile, producers are being increasingly required to meet more stringent guidelines for the levels of the radioactive elements uranium and thorium in their products. The Becher process does not significantly reduce uranium and thorium levels and so there exists an increasing need to develop a process for the removal of uranium and thorium from ilmenite and other titaniferous materials such as synthetic rutile.
In processes of the type disclosed in Australian patent applications 14980/92 and 14981/92, the titaniferous material is treated with acid containing soluble fluoride or with base followed by an acid treatment, respectively. However, while these processes were found to remove uranium and thorium from the titaniferous material, it has now been discovered that the radioactivity of the material is not reduced to the extent expected from the reduction in thorium and uranium content. Further investigation has shown that this is because the prior treatments are primarily removing the parent uranium and thorium isotopes, and the radionuclide daughters are not being removed to the same extent. This is apparently the opposite of what has generally been observed with leaching treatments of radioactive materials in other fields, where the radionuclide daughters are generally removed as well as or more readily than the parent.
According to the specification, it has been surprisingly found that a heating treatment may be applied to the titaniferous material effective to enhance the accessibility of the radionuclides and/or at least one of the radionuclide daughters to subsequent removal processes. Preferably, the parent isotope in the thorium decay chain (eg. 232Th), and its radionuclide daughters (eg. 228Ra and 228Th), are rendered substantially equally accessible to subsequent thorium and/or uranium removal processes.
In addition, one or more reagents are added to the heated titaniferous material which are believed to be effective in providing a medium for enhanced aggregation or concentration of the thorium and/or uranium, thereby facilitating separation of the thorium and/or uranium and/or their radionuclide daughters during subsequent leaching. These reagents also tend to lower the heating temperatures required to achieve a given degree of radionuclide removal. The reagents preferably comprise glass forming reagents such as borates, flourides, phosphates and silicates. By glass forming reagent is meant a compound which at an elevated temperature transforms to a glassy ie. non-crystalline phase, comprising a three-dimensional network of atoms, usually including oxygen.
The specification ends with fifty-two claims, of which the independent claims read as follows:
1. A process for facilitating the removal of radionuclides, such as eg uranium and thorium, and/or one or more of their radioactive daughters from titaniferous material which comprises contacting the titaniferous material with one or more reagents at an elevated temperature selected to enhance the accessibility of at least one of the radionuclide daughters in the titaniferous material, the reagant(s) being selected to form a phase at said elevated temperature which disperses onto the surfaces of the titaniferous material and incorporates the radionuclides and said one or more radionuclide daughters.
15. A process for facilitating the removal of radionuclides and/or one or more of their radionuclide daughters from titaniferous material which comprises the step of treating the titaniferous material to cause aggregation or concentration of the radionuclides and one or more of their radionuclide daughters, to an extent effective to enhance the accessibility of at least one of the radionuclide daughters to subsequent removal, wherein said treatment includes a heat treatment of said titaniferous material and contacting of the titaniferous material with one or more reagents selected to form a phase as a result of said heat treatment which disperses onto the surfaces of the titaniferous material and incorporates the radionuclides and said one or more radionuclide daughters.
32. A process for treating iron-containing titaniferous material, eg an ore such as ilmenite, by reducing iron in the titaniferous material largely to metallic iron in a reducing atmosphere in a kiln, thereby producing a so-called reduced titaniferous material, comprising feeding the titaniferous material, a reductant, and one or more reagents selected to enhance the accessibility of at least one of the radionuclide daughters in the titaniferous material, to the kiln, maintaining an elevated temperature in the kiln, the reagent(s) being selected to form a phase at said elevated temperature which disperses onto the surfaces of the titaniferous material and incorporates the radionuclides and said one or more radionuclide daughters, recovering a mixture which includes the reduced titaniferous material and said phase from the kiln at a discharge port, and treating the mixture to remove thorium and/or uranium and/or one or more of the radionuclide daughters.
39. A process for facilitating the removal of one or more impurities from titaniferous material which comprises contacting the titaniferous material with one or more reagents at an elevated temperature, the reagent(s) being selected to form a phase at said elevated temperature which disperses onto the surfaces of the titaniferous material and incorporates the impurity(s).
The glass forming reagents may be added individually or in a combination or mixture of two or more of the compounds. In addition, reagents that act as glass modifiers ie. as modifiers of the aforementioned network phase, such as alkali and alkaline earth compounds, may also be added with the glass forming reagents. The glass modifiers may be added as, for example, an oxide, carbonate, hydroxide, flouride, nitrate or sulphate compound. The glass forming reagents and glass modifiers added may be naturally occurring minerals such as borax, ulexite, colemanite or fluorite (calcium flouride), or chemically synthesised compounds.
A suitable elevated temperature effective to achieve a satisfactory or better level of radionuclide incorporation is in the range 900oC to 1200oC, optimally 1050oC to 1200oC.
The specification states that an especially preferred application of the invention may be to the production of synthetic rutile from ilmenite by an iron reduction process such as the Becher process. As mentioned, in this process, iron oxides in ilmenite are reduced largely to metallic iron in a reducing atmosphere in a kiln, at a temperature in the range of 900-1200oC, to obtain so-called reduced ilmenite. The aforementioned reagent(s) are also delivered to the kiln, and form(s) the phase which disperses onto the surfaces of the titaniferous material and incorporates the radionuclides and one or more of the radionuclide daughters. The cooled reduced ilmenite, or the synthetic rutile remaining after subsequent aqueous oxidation of the iron and separation out of the iron oxide, is subjected to an acid leach to remove the thorium. A proportion of the radionuclides may also be removed at the aqueous oxidation stage.
BACKGROUND TO THE DISPUTE
The written evidence and submissions discuss the research programs separately undertaken by Iluka and WIM which each party alleges lead to the invention. To help appreciate the issues raised in the proceeding, I will now broadly review the respective research programs as neutrally as possible based on the narrative provided by that body of written material.
WIM's Research Activities
General
After being engaged in the area of high temperature metallurgy for a number of years, in 1986 Dr Hollitt established the Advanced Mineral Chemistry Laboratories of CRA (now Rio Tinto Limited which holds all of WIM's issued share capital) and was assigned the task of designing initial test work aimed at upgrading ilmenite derived from CRA's titanium mineral deposits in the Wimmera region of Victoria.
Dr Hollitt subsequently joined WIM as Senior Metallurgist in late 1987. In 1990 he was appointed as General Manager - Process Development with WIM and in that position managed a team having direct responsibility for test work, process design, and other studies relating to zircon and titanium minerals upgrading processes. Dr Hollitt explains (1 Hollitt 2.7) that WIM did not themselves maintain experimental laboratories and so commissioned this work from outside research bodies such as CSIRO and ANSTO on a confidential basis. On this he says:
In general, WIM did not require outside researchers to propose experimental or process design. Rather WIM gave very specific directions for the experimental and analytical work it required. Nevertheless, in the case of particular individuals, I worked closely with those individuals to obtain their practical input on the implementation of WIM's research projects.
These individuals included Dr Grey of CSIRO Division of Mineral Products. Dr Hollitt continues as follows:
It is my view that the best approach to any research project involves those carrying out experiments being fully aware of the relevant background and objectives and consequently I ensured that researchers were fully briefed on those matters … This method of work required me to have a great degree of trust in the researchers and to be confident in the strict maintenance of confidentiality in what was being disclosed. Regardless of my usual expectation that team members would keep WIM's confidential test work confidential by reason of the nature of the relationship and the conditions of the engagement, where test work was particularly commercially sensitive, WIM required individual members of research teams who contributed to test work to sign additional personal confidentiality undertakings. By reason of the nature of the relationship I also expected that any potential conflict of interest would be identified to me before the commission was accepted by researchers in relation to proposed work.
According to Dr Hollitt, the many discussions he had with individual researchers confirmed his expectations that they were kept fully informed of WIM's confidential test work.
The Hybrid Process
By late 1987 or early 1988 Dr Hollitt had realised that the WIM ilmenites could not be upgraded to a synthetic rutile product by the Becher process because while the Becher process removed iron and manganese, it could not effectively remove magnesium or other impurities. These impurities could be removed by the Murso process but this was uneconomic. The aim was therefore to produce a high grade sulphate process compatible feedstock from which impurities had been removed to an acceptable level or rendered inert.
Despite the success of laboratory test work, business analyses predicted at the time that there would be little or no growth in the sulphate process segment and that all pigment feedstock market growth would be in the chlorine process segment. As a consequence, WIM embarked on a program of research directed to producing a synthetic rutile as a feedstock for the chloride pigment process.
The laboratory work for the synthetic rutile phase of the project was undertaken by CCWA under Dr Hollitt's direction. The aim of the work was to investigate the possibility of conducting a reduction run at lower temperatures (about 950oC to 1000oC) to produce a product with a lower degree of metallisation and with the main impurity elements (including iron) being concentrated in minor crystalline titanate phases that could be selectively leached in strong acids, thereby resulting in a high titania synthetic rutile product suitable for chloride-route pigment plants. This combination of lower temperature reduction and acid leaching of a titanate phase was referred to as the "hybrid" process by WIM. Subsequent kiln trial test work was completed in February 1990 and, during the following two years, work on ilmenite upgrading proceeded with CSIRO and CCWA to optimise the hybrid process.
The hybrid process was disclosed in application 74507/91 (now patent 639089) filed on 1 March 1991 and which claims an earliest priority date of 2 March 1990. The specification was published on 18 September 1991 and names Drs Hollitt and Grey as co-inventors.
The Zircon Process
Zircon (zirconium silicate) is another mineral sand and is mainly used as feedstock to the ceramics industry.
Research undertaken by CSIRO on behalf of WIM before mid 1989 had established that the zircon fraction of their deposits was badly contaminated with radioactive impurities, and various projects were accordingly conducted and sponsored by WIM with the aim of identifying simple chemical processing techniques to remove the uranium and thorium contaminants. Dr Hollitt appointed Messrs McClelland and Liddy to his team for this purpose.
WIM's initial test work failed to satisfactorily leach the radionuclides from the zircon, and indicated that the radionuclides were present in the zircon in two forms, either in the easily attacked material comprising the metamict zones (radiation damaged crystal structure) or locked in the actual zircon crystal lattice. In the latter instance the zircon acted like an inert capsule for the radionuclides which prevented their removal. By late 1990 Dr Hollitt had formed the view that a substantial proportion of the uranium and thorium and their radioactive decay chain "daughters" or "progeny" were present in the zircon lattice and that, as a consequence, the radioactivity in zircon could not be satisfactorily reduced by acid leaching. The focus in WIM's test work accordingly shifted to decomposing the zircon crystal lattice to enable the redistribution and possible removal of the parent and progeny radionuclides.
On 13 December 1990 a research project description was completed by Mr Liddy under Dr Hollitt's direction (exhibit MJH-15). This project was contracted to Lakefield in Ontario, Canada, after ANSTO and CSIRO had advised they could not work to WIM's proposed timetable. Preliminary test results received in late January 1991 were encouraging, particularly when the zircon was pre-ground to expose the radioactive progeny to a hydrochloric acid leach, but even so only a relatively low reduction in the gross radioactivity of WIM zircon samples was produced. In February 1991 the possibility of using lime roasting as a pre-treatment for reducing the radioactivity of WIM zircon was suggested to Lakefield. As explained in 1 Hollitt 4.13:
The zircon crystal lattice is made up of zirconia (ZrO2) and silica (SiO2) in the composition ZrSiO4. Lime (CaO) has a strong affinity for silica and I was aware of its use in processes for the production of zirconia (ZrO2). I therefore thought that this approach might break down the zircon crystal lattice and so expose the remaining radioactives to chemical attack. I did not, however, want to convert all the material to zirconia since, according to the information then available to me, this would require very large quantities of lime which would have to be leached from the end product at high cost. It was therefore necessary to determine what quantities of lime needed to be added in order to afford sufficient breakdown of the zircon lattice to enable leaching of most of the remaining radioactivity. At this stage I did not know for certain what effect the calcium in the lime would produce other than that the treatment should create a new phase. Although the zirconia was quite inert, it was possible that a reaction could occur at very high temperatures. I discussed these matters with Liddy, and we were in agreement. I instructed him to proceed with research work in this direction.
On 6 March 1991 WIM received the gross gamma results from lime roast samples leached with hydrochloric acid (exhibits MJH-39 and MJH-40) which revealed a high level of radioactivity removal from the zircon product. This was the first significant breakthrough in the project and demonstrated that radium in particular was being leached. A report received from ANSTO on 7 March (exhibit MJH-41) supported Dr Hollitt's view of late 1990 that techniques which attack the zircon matrix may be required prior to acid leaching to achieve higher radionuclide extraction.
Lakefield's project work further identified the fact that the calcium to silica ratio in the chemical composition of the test samples, calculated from the crystal structure provided by XRD analysis, did not correlate with that found in the feed material. According to 1 Hollitt 4.20:
All of the material present could not be accounted for by the production of crystalline silicate phases alone. After considering the phase diagrams for the CaO-SiO2-ZrO2 system, I concluded that a separate amorphous phase had formed under the conditions in which we were operating … An amorphous phase would not be detected by XRD and was the only explanation by which to account for the discrepancies in the calcium to silica ratios. I went on to conclude that the amorphous phase formed under these conditions was almost certainly a silicate glass which was formed as a free flowing liquid at roasting temperature. The formation of this liquid glassy phase appeared to be dependent upon the amount of lime added to the system. If too much lime were added, the liquid glassy phase would gradually disappear in favour of a crystalline silicate phase. From the results obtained it appeared to me that this liquid glassy phase might be important to the effectiveness of radioactivity removal using lime addition, but the optimum amount of lime addition required to achieve the benefits of radioactivity removal in subsequent leaching remained unknown.
In a memorandum dated 5 March 1991 to Messrs Liddy and McClelland, Dr Hollitt postulated the existence of a low melting point liquid phase which aided the breakdown of the zircon crystal lattice and to which the radioactive progeny might deport. A second research project description was sent to Lakefield on 18 March 1991 requesting them to investigate the matter further. The results of this work were formally reported in June and July 1991 (exhibits MJH-50 and MJH-51).
In about June 1991 Dr Hollitt decided to repatriate some of the work from Lakefield into Australia. During subsequent discussions Dr Hollitt told Dr Grey that the work was to be directed to the theoretical understanding and development of the Lakefield research results. Following those discussions, Mr Liddy wrote to Dr Grey enclosing a copy of the as yet unpublished zircon provisional patent application (exhibit MJH-47) and a copy of a confidentiality agreement to be executed by Dr Grey and others, and CSIRO. After a similar preliminary conversation, Mr Liddy sent a copy of the Zircon provisional application together with a confidentiality agreement to Dr Kaye Hart of ANSTO.
WIM contracted additional test work to Lakefield in July 1991 to examine the extent to which the calcium in the lime roast was removed in the hydrochloric acid leach as well as to confirm previous results. A report in relation to this additional work was produced on 10 December 1991 (exhibit MJH-58) from which Dr Hollitt and Mr Liddy concluded "that substantial removal of radioactivity was obtained only at temperatures at which a liquid phase was formed and that a liquid phase contributed in a major way to removal of radioactivity." (1 Hollitt 4.26)
On 13 September 1991 Mr Liddy sent a project description (exhibit MJH-61) to ANSTO which described various aspects of WIM's process for the removal of radioactive components from zircon minerals. A revised project description was sent on the same day to CSIRO with instructions to use a magnesium containing additive (dolomite) as a substitute for lime in some of the test work in an attempt to address the difficulties experienced by Lakefield with calcium retention.
The results of the test work conducted by CSIRO were produced in a report in December 1991 (MJH-63) and revealed that during the lime roast uranium strongly partitioned to a leach-resistant zirconia phase, whereas thorium partitioned mainly into a leachable Ca-Zr-silicate glass (quenched liquid). According to CSIRO, adjustment of the lime addition rate enabled uranium to be concentrated in the liquid phase and adding small amounts of TiO2 to the lime addition mixture improved the process by apparently enhancing the transfer of uranium to that phase. The report also determined that the extent to which uranium was incorporated in the zirconia phase increased with temperature. The use of dolomite was not pursued on the basis of the test results.
The report recommended further work be conducted to test additives that give a lower melting point liquid phase, and stated that "[t]he addition of the basic oxide as a silicate phase may help in reducing zirconia formation while still promoting the formation of a liquid." A roast test with silica addition was carried out and preliminary analyses confirmed that a higher proportion of uranium transferred to the liquid phase.
Dr Hollitt concluded that any beneficial effect of adding TiO2 was primarily attributable to the fact that it could increase the amount of liquid phase formed, and therefore the degree of uranium transfer. Dr Hollitt also concluded "beyond doubt" that the liquid phase was preferentially concentrating the radionuclides in it, and discussed his conclusions with Dr Grey by telephone on or about 16 January 1992. On 17 January Dr Hollitt sent extracts from the Lakefield reports to Dr Grey by facsimile which supported the view that breakdown of the zircon lattice was necessary for the removal of radionuclides.
Optimisation and characterisation work continued, although the process was still running at very high temperatures, viz. in excess of 1400oC. Based on his knowledge of the theory of high temperature glassy phases, Dr Hollitt contemplated the addition of a very small amount of an agent such as sodium borate (borax) to aid glassy phase formation, assist elemental redistribution in thermal processing and so allow lower temperature operation. Dr Hollitt suggested the use of a borax additive to Dr Grey during a phone conversation "on or about 4 March 1992" which he says was confirmed by facsimile on 5 March (exhibit MJH-66). In this facsimile transmission Dr Hollitt refers to the borax as a "fluxing agent".
The results of this work were reported in May 1992 (exhibit MJH-73) which noted that the use of borax appeared to have some undesirable effects and therefore suggested further studies with alternative additives such as spodumene (LiAlSi2O6) and sodium/barium compounds. The report also suggested experimenting with lower levels and different ratios of lime to silica. On 6 March 1992 Mr Liddy sent a project description to ANSTO for agglomeration test work on material to be used in the zircon process. The test work was extended on or about 24 March to include tourmaline as an alternative to commercial borax. However, the trial using tourmaline was not successful.
On 19 December 1991 a project description was sent by Mr McClelland to CCWA. The project description was revised in March and again in May 1992 (exhibit MJH-69) to disclose the thermal treatment of zircon at 1300oC, and the use of silica and borax in combination with the lime. The CCWA kiln trial work was conducted from 26-28 May and demonstrated that by adjustment of conditions to reduce accretions it was practical to operate the WIM zircon process in a rotary kiln.
A complete application relating to the WIM zircon process was filed on 15 April 1992 as application 16612/92 (now patent 670028) claiming a priority date of 15 April 1991 and naming Drs Grey and Hollitt, and Messrs Liddy and McClelland, as co-inventors. The application was published on 24 December 1992.
The RUTILE Process
This is a process for the upgrading of titaniferous materials, RUTILE being an acronym for "Recovery of Upgraded Titania by Impurity Liquefaction and Extraction".
Following initial success with the zircon process, in July 1991 Dr Hollitt proposed that WIM investigate silica removal from high titanium (HiTi) concentrate via leach digestion, soda roast/leach and lime roast/leach schemes. At Dr Hollitt's request Mr McClelland made a theoretical evaluation of the chemistry of a soda roast and concluded that the soda (Na2O) would preferentially react with the titania in the system rather than the silica and so form refractory titanates. However, Dr Hollitt was not thoroughly convinced that this conclusion would hold true under all circumstances, and so testing did not proceed at that time.
By early June 1992 WIM had accepted that silica would be a serious contaminant and consequently attention again returned to its removal from their high titania products. On this 1 Hollitt 5.7 states:
In mid June 1992, I therefore reconsidered the soda roast process. I realised that McClelland's calculations, which had established that the process was not viable, were theoretically correct but that they did not allow for the stabilisation effect of the silicate networks formed in the liquid glassy state which would increase the tendency of sodium oxide to react with silica. I theorized that if the process were conducted at a temperature at which a liquid glassy phase could form, then the preference for soda to react with titania might be reversed … I knew from WIM's zircon work that the formation of a liquid phase had greatly facilitated the extraction of radioactive impurities. I knew from WIM's Hybrid … work that in the presence of an alternative phase which could readily accommodate thorium, radium and uranium, a rutile phase tended not to retain thorium and radium and to only partially retain uranium. I concluded that if WIM could form a rutile phase plus a liquid glassy phase and avoid or minimise formation of other phases (which could take up and retain radioactive impurities) it was almost certain that the silica and most of the radioactive impurities could deport to the glassy phase and be removed in a subsequent leaching stage. I discussed this proposal with McClelland who agreed that investigations and test work should be carried out … I agreed with McClelland that I would commission the work with CSIRO directly.
This account is corroborated by Mr McClelland who states (McClelland 2.43) that he "specifically discussed with Hollitt the link, which had been found in the zircon work, between the formation of glassy phases and radioactive removal". Mr McClelland further states:
Before 19 June 1982 [sic: 1992], Hollitt and I discussed a number of further matters in relation to the proposed process. In particular, I discussed with him the possibility of processing combined concentrates, whereby products could be produced by a single upgrading process which addressed all of the impurities present. This was possible here because the problem of the silica and other impurities affected both the ilmenite and high titanium materials … In relation to leaching I discussed with Hollitt water leaching, and, as a potential option, caustic leaching. I discussed with Hollitt the further subsequent step of using of [sic] acid leaching to remove basic impurities. That the acid was hydrochloric acid was implicit in our discussions because at that time we were working on hydrochloric acid leaching processes …
On 23 June 1992 Dr Hollitt told Dr Grey by telephone that he would be sent a scoping proposal for test work on a process for removal of silica from titaniferous materials. It was agreed that this work would be treated as an extension of the zircon work so as to avoid the need for separate confidentiality agreements. The process to be tested (generally referred to as the "soda roast" process) was described by Dr Hollitt as including soda ash additions to titaniferous material, roasting to form a glassy phase and glassy phase removal by water leaching or, if that failed, by caustic leaching. Any remaining impurities were to be subsequently leached with hydrochloric acid. Dr Grey said that he did not believe the proposal would work because of the unavoidable formation of sodium titanates which would prevent the formation of a glassy phase. As stated by 1 Hollitt 5.8, "Grey's comments appeared to be based on the same theoretical assumptions that McClelland and I had made a year earlier …"
The first scoping proposal was in any case sent to Dr Grey on 24 June 1992 together with some high titania concentrate samples for initial test work, and a copy of the soda-silica-titania phase diagram which Dr Hollitt had marked to illustrate the tendency for silica to concentrate in liquids saturated with TiO2. According to 1 Hollitt 5.9:
Either on 23 June 1992 or in one of our conversations over the course of the following week I recall describing to Grey that I expected the process would produce a product lower in problem impurities, and particularly silica and contained radioactives. I also told him that I expected the process could also be used on a range of titaniferous materials including ilmenites.
Test results received between 24 June and 3 July 1992 (based on analyses using a caustic leach) confirmed Dr Hollitt's theoretical expectation that the formation of a liquid glassy phase would reverse the preference of sodium to react with titania. This reversal in chemistry enabled the impurities (silica, alumina and many minor impurities) to deport into the liquid glassy phase which was amenable to caustic leaching under easily achievable conditions. On or about 3 July 1992 Dr Hollitt prepared a detailed memorandum (exhibit MJH-77) describing a process for removal of silica and radioactives from HiTi and for removal of iron and other impurities from ilmenite, in which HiTi and ilmenite were processed as a combined stream. 1 Hollitt 5.12 states:
I was confident that the soda roast/leach process would condition iron and basic impurities (primarily magnesium and manganese) for removal by a subsequent acid leach. By reason of the body of information resulting from WIM's previous work in relation to radioactives removal, I was confident that the soda roast process would facilitate the removal of radioactives. The evidence that the sodium was reacting strongly with the silica suggested that, with optimization, the formation of refractory phases likely to take up impurities could be avoided. Most impurities would not be retained in the rutile phase but would deport to the liquid glassy phase or to an M2O3 phase from either of which they would be leachable. I was therefore confident that radioactives, particularly radium and thorium and to a lesser extent uranium, would be substantially removed in the subsequent acid leach if hydrochloric acid were used.
Dr Hollitt described the process set out in the memorandum and the reasoning behind each step in full to Dr Grey to obtain his critical comments. Matters which he recalls describing to Dr Grey included Na2O (and alternatively CaO) additions, glassy phase formation, cooling while controlling recrystallisation of the glass, leaching using sequential sodium silicate, caustic and hydrochloric acid leaching and radioactivity removal. After 3 July 1992 WIM continued to work with CSIRO in order to improve and optimise the process, and during this period Dr Hollitt had "day to day contact" with CSIRO staff members who were assisting Dr Grey. Dr Hollitt says that a particular issue "was to make the leach of the glass using water as the only reagent work better, as that would reduce the cost of reagents and would produce a sodium silicate byproduct, which could be utilized in the WIM mineral dressing plant". During July CSIRO were given directions on the sodium silicate leach aspect (exhibit MJH-78) and also were requested to include ZrO2 in analyses to allow WIM to determine whether there was a need to produce zircon free concentrates.
A complete application directed to the RUTILE process was filed on 12 August 1993 as PCT/AU93/00414 (now application 678375) claiming an earliest priority date of 14 August 1992. The complete application was published on 15 March 1994 and names Dr Hollitt and Mr McClelland as co-inventors.
Iluka's Research Activities
General
Mr Harris has been employed by Iluka or other affiliated companies since 1989, and is named as a co-inventor by the present application. He explains that the application is in broad terms concerned with a process known as SREP (Synthetic Rutile Enhancement Process) developed jointly with CSIRO during 1992-95 which evolved from an earlier project commissioned in 1990 to investigate the removal of thorium from ilmenite mined by Iluka at Eneabba in Western Australia. Mr Harris states that he was "closely involved in that project throughout the period October 1990 to August 1995, and witnessed at first hand the development of the SREP process".
CSIRO was engaged to undertake a project known as the "Thorium in Ilmenite Project" which commenced in October 1990. Mr Harris was the principle Iluka contact. Drs Grey, Houchin and Aral were nominated by CSIRO to work on the project. Dr Houchin was appointed project leader and remained on the project as a consultant when replaced as leader by Dr Sparrow in September 1991. The Iluka project team included a Mr Trevor Nicholson.
The Thorium in Ilmenite Project
By April 1991 this project had produced promising results with leaching processes in which ilmenite was leached first with caustic soda and then with sulphuric acid at elevated temperature. Exhibit HRH-14 explains the basis of this process as follows:
The predominant radiation source in the ilmenite from the Eneabba field is the thorium 232 chain of isotopes. The model proposed to explain the hydrometallurgical process developed by the CSIRO involves leaching thorium from the walls of the internal pore structure of the ilmenite grains that has precipitated from the ground water over geological time as a result of the mineral alteration processes. The mechanism of the hydrometallurgical process developed involves a caustic preparation step to activate the thorium and an acid step to allow dissolution of the activated thorium. These reactions take place within the pore structure of the ilmenite grains and essentially leave the ilmenite grain structure untouched.
As an additional attraction it was thought that sodium enhanced the synthetic rutile reactions, and that the leaching of ilmenite prior to synthetic rutile (Becher) processing would enhance the reaction rates in the kiln and lead to improved product quality and throughputs. In August 1991 approval was given to construct a pilot plant to test the caustic/acid leach proposal, and initial runs using ilmenite as the feed material resulted in a product having a significantly reduced thorium content. The project was renamed by Iluka as the "Attritioning Upgrade Project" (AUP) which I note is the subject of applications 14980/92 and 14981/92 referred to earlier.
During March 1992 samples of the pilot plant product were tested for radioactivity by ARL and ANSTO. The test results showed that while the process of leaching ilmenite reduced the thorium content, the radioactivity remained almost unchanged. Specifically, the tests indicated that the isotope 228Th was present in the ilmenite after leaching in a much higher proportion than expected from the observed level of thorium removal. A meeting between staff from Iluka, CSIRO and ANSTO was held on 25 March 1992 to discuss the unexpected test results (exhibit HRH-3). As a result of this meeting a model based on a mechanism known as "alpha recoil" was developed to explain why the parent thorium isotope, but not the daughters, was removed by the AUP caustic/acid leach. According to 1 Grey 4.12:
The model made use of the CSIRO's understanding of the nature of the thorium contaminants, as being located within the pores of the altered ilmenite grains, either as mineral fragments, or as adsorbed species on the pore walls. The thorium (and uranium) is not incorporated in the ilmenite lattice, as in the case of zircon and monazite, but is external to the lattice on the mineral surfaces (internal and external). When 232Th undergoes radioactive decay the recoil of the daughter product propels it into the ilmenite structure. Further radioactive decay will eventually lead to annealing and sealing of the damaged region behind the daughters so they are no longer accessible to leach solutions. It was recognised that the daughter products are incompatible with the titanate structures so that they are not incorporated into the lattice, but are physically entombed by the surrounding lattice into which they have been injected.
The proposed model was contrary to expectations since the more common result of alpha recoil was to cause the daughters of a parent isotope trapped in the lattice to be more accessible and therefore more readily leachable. Nonetheless, in an internal memorandum dated 13 April 1992 (exhibit HRH-8), Mr Harris reported that this model had been confirmed by tests undertaken by CSIRO and ANSTO. Attempts were then made to remove the daughter products by investigating a variety of leaching regimes using samples of ilmenite, reduced ilmenite (an intermediate material) and synthetic rutile (Bruckard 10). At a meeting with his CSIRO colleagues on 29 April 1992, Dr Grey suggested heating ilmenite to temperatures of 500oC, 750oC and 1000oC "to coarsen the ultrafine pore structure to possibly liberate the radioactive daughter elements onto the surface of the ilmenite." (1 Grey 4.13) This pre-heat treatment commenced in May (Freeman 5).
On 6 May 1992 Mr Harris attended a brainstorming meeting at CSIRO at which Dr Aral presented a report on the results of experiments he had carried out with the aim of forming a leachable thorium sulphide phase. A test performed on 2 March 1992 in which synthetic rutile was heated at 1100oC and then at about 1300oC in the presence of coal char and sulphur was unsuccessful. However, the heat treatment did result in a thorium-rich phase coming to the surface of the rutile grains. This phase was observed as micron-sized "specks" when the samples were examined by SEM. These specks were a surface phenomena due to enlargement of the internal pores (exhibit HRH-12). The test was repeated on 30 April 1992 without using sulphur or char and similar thorium-containing specks were formed when the synthetic rutile was heated at 1300oC for 3 hours.
A report was also presented by Dr Grey concerning the results of his electron microprobe studies on 4 and 5 May 1992 of the samples heated by Dr Aral which indicated a thorium:silicon atomic ratio of 1:1 suggesting that the phase was thorium silicate. Dr Grey's analyses also showed that the phase additionally contained phosphorous (exhibit IEG-6). According to 1 Grey 4.14, this indicated that the thorium was being fluxed by minor amounts of impurities within the pores of the ilmenite grains, which have a high mobility at 1300oC, and that this fluxing produced a phase that was relatively soluble in strong acid. Dr Aral noted, following a discussion regarding possible leaching of the thorium phase, that silicon and phosphorous were network former elements and so may form a glass phase that contains the thorium (exhibit HRH-9). 1 Aral 24 states:
We all had our own theories about whether the thorium specks were amorphous glass or crystalline mineral (thorium silicate, ThSiO4) phases and how they were formed.
However, according to 2 Sparrow 13, Iluka were not at that time concerned with whether the thorium was contained in a glass or crystalline phase. As further explained by 2 Houchin 13, the primary concern was to enhance the mobility of the thorium to the surface of the ilmenite grains and "once we had realised that physical separation processes would not work, to enhance the solubility of the thorium into an acid soluble phase (whether through heating, changed leaching conditions or some other way)."
During May 1992 Dr Aral conducted a number of experiments using additives which potentially could promote the mobilisation of thorium (1 Aral 26). In two experiments performed on 7 May he heated synthetic rutile, firstly, with montmorillanite (clay), and next with quartz, at 1400oC with the intention of mobilising the thorium onto the grain surfaces by providing more of the impurities (silicon and aluminium) seen in the experiment reported at the 6 May meeting. On
19 May Dr Aral treated ilmenite previously heated at 1300oC with sodium hydroxide and leached with water and weak hydrochloric acid. On 25 May he heated sodium silicate and potassium chloride soaked ilmenite, synthetic rutile and reduced ilmenite at 1300oC. The purpose of using the latter additive was to replace thorium and radium with a similarly sized large potassium atom in the thorium-rich phase. None of these tests were successful.
In parallel with this work, Dr Aral and Messrs Freeman and Bruckard developed a controlled experimental program for evaluating the performance of a range of heating and leaching regimes and thereby optimise the conditions under which thorium and its daughters could be removed. The program involved a series of heating and leaching experiments involving both ilmenite and synthetic rutile (2 Aral 11) the results of which were recorded in a matrix (exhibit GS7). Mr Harris explains the program in some detail in 2 Harris 19:
… Initially Aral and Freeman tried the lower end of the high temperature range (ie: 1100o, 1200o, 1300o). These were completed by the end of June. The next logical step was the 1400o experiment performed on 3 July [see below]. This experiment was not carried out for any other particular reason than to complete the matrix. Such temperature was well beyond a commercial application, but Aral had noted the relationship showing parent and daughter removal at temperatures above 1000o and we thought it important to improve our understanding and extend this matrix to higher temperatures (than 1000o).
As a consequence of Iluka's desire to incorporate radioactivity removal into their commercial operations, the experimental program also included pre-oxidation of test samples, followed by reduction (under Becher-type conditions) and then leaching. These experiments continued until late July or early August (2 Sparrow 20). At a major project meeting held on 3 June 1992, Mr McDonald reported that the optimum temperature for producing the thorium specks was 1200oC, although Dr Grey is recorded in Dr Sparrow's notes of that meeting to have stated "SEM work indicates not blobs on surfaces but thin films on oxide surface" (2 Harris 12). It was also reported (exhibit HRH-14) that "heating mobilises the daughters and they 'recombine' with 232Th". This result demonstrated the reversal of the alpha recoil effect which had prevented sufficient radioactivity removal by the AUP caustic/acid leach.
On 3 July 1992 Dr Aral conducted a heating/leaching experiment at 1400oC to confirm the test matrix trend that showed an increasing amount of thorium removal with increasing temperature. The experiment was repeated on 10 July. The results of these experiments were presented to the project team on 15 July and revealed a reduction of thorium to below anticipated marketing levels (100ppm [U+Th]) for the first time. According to 2 Sparrow 21, as the parent and daughter progeny were known to be largely in equilibrium in thorium at and beyond 1000oC, "we also knew in the meeting of 15 July that Aral had succeeded in reducing the radioactivity to or about the target level." The experiments further established that the thorium was present in a phase more leachable than those produced by heating to lower temperatures. This phase was later identified on 5 August by Dr Grey as a thorium enriched silicate glass phase.
In a project status report dated 22 July 1992 (exhibit HRH-14), Mr Harris states:
To date the research has indicated that heat is effective in re-uniting the isotopes. Using heat alone, in an oxidising atmosphere a temperature of about 1000 degrees centigrade is necessary to re-unite all the isotopes. This appears to begin at temperatures as low as 750 degrees and at a temperature of around 1200 degrees the thorium itself has coalesed [sic] to the point that it is visible under the scanning electron microscope. However as the heating temperatures increase the isotopes become increasingly refractory, ie, dissolution by chemical reagents becomes increasingly difficult. The increase in refractory nature continues to an inflexion point from where there is a trend to increased leachability as the temperature is increased further, although this is at the expense of significant titanium loss … The project is now at the point where the fundamental physical and chemical steps that produce the observed results and the steps responsible for driving the process are being determined.
One of the steps being examined involved the question of whether there were any additives or fluxing agents that could be added to the heating step that would enhance the solubility of the thorium containing phase at more suitable temperatures. The importance of fluxing agents was recognised among the project team (see eg. 1 Houchin 21 which refers to the discussion of flux additives at a meeting on 20 May) since the temperature at which the thorium was mobilised needed to be reduced to be useful in a commercial setting, preferably in conjunction with the existing Becher process. In this context Dr Houchin explains that by "flux" is meant something which will help mobilise or assist the formation of another phase at a lower temperature. The project team therefore agreed at their meeting on 15 July to recommence the search for a suitable fluxing agent (1 Sparrow 11).
For his part Dr Grey conducted a literature search to identify compounds which would extract thorium at the lower target temperature (about 1000oC: 1 Sparrow 10). The basis of this search is explained from 2 Grey 3.30 onwards as follows:
… I considered that the increased leachability of thorium after treatment at roast temperatures above 1000oC was due to it forming compounds with other impurity elements in the pores, particularly Si and P, and that the compounds were more leachable than the uncombined thorium oxide formed at 750-1050oC. After the 15 July meeting, I extended this line of reasoning to consider the possibility of forming a leachable thorium compound by using an additive that would react readily with the thorium at relatively low temperatures … My microprobe studies in early May had shown me that the thorium reacted readily with Si and P-containing impurities in the pores to form leachable compounds and this guided me in looking for compounds … I also had in mind compounds with elements such as alkalis and alkaline earths which I knew from my prior knowledge would be expected to have lower melting points than the binary compounds and would most likely be more leachable … I found … entries for sodium thorium phosphate compounds which I considered to be good candidates for further investigation.
According to 2 Houchin 16, phosphates were identified as the best additive since these form the lowest melting point phases with thorium. Dr Grey then performed a number of tests with synthetic materials. On 20 July 1992 he prepared a reactive form of hydrated thorium oxide (thoria) which simulated the finely dispersed form of thorium in ilmenite and was mixed with sodium dihydrogen phosphate, and then heated to 900oC. A sample of the hydrated thorium oxide alone was given the same heat treatment in order to provide a reference material for acid leaching tests. Excess flux was removed from the heated mixture with water to allow Dr Grey to analyse the sodium thorium phosphate crystalline compound he had formed. This compound could not be readily leached. Experiments using sodium silicate plus sodium hydroxide as a flux conducted on 22 July were also unsuccessful.
On 25 July Dr Grey turned to tests with ilmenite concentrate and decided to continue with [PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY] which proved successful in removing most of the thorium and radioactivity (exhibits GJS-4 and IEG 16). However, although successful in removing thorium and radioactivity from ilmenite samples under oxidising conditions, Iluka were concerned whether residual sodium would remain in the synthetic rutile following sodium phosphate reduction in the Becher process. Dr Grey consequently carried out a test on 30 July in which ilmenite with sodium phosphate added was heated to simulate plant reduction conditions. In further test work conducted on 5 August, it was found that sodium phosphate did not remain stable under these conditions because the phosphate was reduced to elemental phosphorous and incorporated into the metallic iron (1 Grey 4.26).
Following the failure of the sodium phosphate flux in a reducing environment, Dr Grey tried anhydrous sodium borate (borax) as an additive on 6 August. The use of borax was not a complete success due to its volatility under the heating conditions used (1 Sparrow 17).
This is not a clear-cut situation. I mean, glass or crystalline phase was not resolved, that's why - actually, it wasn't resolved until 1400 degrees Celsius experiment was done. Before that, it was all speculation and it was idea. (TS.799.14)
I was trying to mobilise thorium on to the grain surfaces by providing the same material that makes those specks. If those specks are glass, I am trying to make glass. (TS.802.23)
I was just trying to main [sic: make] those specks on the surfaces of the grains, more of those, or migrate them to the phase I added. Other than that, I have nothing else to add.
That's the best answer you can give? --- Yes. (TS.803.8)
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
For the reasons set out above I am unable to accept Dr Aral as a reliable witness so far as the issue of his "natural thought" is concerned, and I weigh the evidence he has given in this regard accordingly.
The source of the suggestion
Mr Harris states in 1 Harris 25 that he was immediately aware after the team meeting on 6 May that the temperature at which Dr Aral had observed the thorium specks (1300oC) was too high to be commercially acceptable. In 1 Harris 32 he recalls several discussions with other members of the project team about methods of lowering the temperature at which the thorium-containing phase might be observed, including by the addition of fluxing agents. According to Iluka, the evidence shows a common attempt by the project team to locate such an agent which could be used to lower the temperature at which the phase transformation observed in Dr Aral's experiments took place.
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
WIM have pointed to the fact that while both Mr Harris and Dr Houchin use the term "flux" (or variants thereof) frequently in their declarations, in the course of cross-examination both accepted that, prior to the 22 July meeting, the term was not used by the SREP project team in the context of solving the radioactivity problem (see eg. TS.649.27 and TS.996.16).
Dr Houchin's notes record that he made the following suggestion on 20 May 1992: "Additives to lower T's" (CB.020.347), and denied that this was not a serious suggestion of something to "put on the list of things to be done" (TS.982.1). On the contrary, Dr Houchin stated in evidence his suggestion referred to the use of additives to lower the temperature at which the migration of thorium to the surface of the ilmenite grains observed by Dr Aral took place, and was
probably prompted by the hypothesis that the thorium migrated to the surface of the ilmenite grains via mobilisation through a siliceous phase. (TS.980.6)
Dr Houchin had no recollection of when this conclusion was reached, but reasoned as follows:
… it seems to me not a great leap of faith to suggest that's the mechanism by which the thorium got to the surface. It is on the surface, it wasn't there before. It is there, associated with silica. The silica wasn't there before. It's formed a new thorium silicate phase. How did it get there? I think presented with that evidence, a lot of people would suggest it had been mobilised by a siliceous phase. (TS.990.14)
However, Dr Houchin indicated that there was nothing in his notes of any of the project team meetings up until late July which connected the mobilisation of thorium with a siliceous phase (TS.980.13), or which even implied that additives were trialled as a result of his suggestion on 20 May:
Would you agree with me that if a decision had been taken at the meeting of 20 May to investigate the use of additives to lower the temperature at which things happen, you would expect to see that reflected in minutes of that meeting and in agenda [sic] for future meetings? --- Probably. (TS.992.19)
Mr Harris made a similar concession (TS.645.11 and TS.661.5), and it is to be noted that the draft provisional SREP specification sent to Iluka on 13 July by Dr Sparrow, which he said contained "all the discoveries that I considered were significant at the time" (TS.923.9), omitted any reference to additives. In drawing attention to this omission I have not overlooked the suggestion that the draft specification only reflected discoveries for which Dr Sparrow had supporting data. Dr Sparrow referred to tests which had been carried out using additives (TS.924.3), but went no further than saying they had given no "useful result". I am as a consequence unable to form any concluded view as to the circumstances of these tests.
Dr Houchin was taken to Dr Grey's analyses of the samples heated by Dr Aral to 1300oC which confirmed the presence of thorium silicate (CB.005.107), and stated that (TS.1001.8)
the fact that the thorium ended up in a thorium silicate phase would imply to me that a silicious phase was involved in the transportation mechanism (my emphasis)
In my opinion, this statement lends credence to WIM's submission that the evidence given by Dr Houchin in this matter has been reconstructed with the benefit of hindsight. Dr Houchin also agreed that his note of 20 May referred only to "additives" which was not necessarily synonymous with "flux", and went so far as admitting that the use of the term "flux" in his written evidence may well be because of the "focus of this proceeding" (TS.983.8). In this regard Dr Houchin suggested that:
The word 'flux' has been raised and used very frequently because of these proceedings. Up until then, I mean, I wouldn't have particularly discriminated or worried about the use - the specific use of the word 'flux', but if someone starts talking about 'an additive' that does something' and uses the term 'flux', then you will naturally tend to use it yourself. (TS.995.14)
In view of the foregoing, I am unable to find that Dr Houchin's suggestion of additives on 20 May was a precursor to the subsequent use of fluxes by the SREP project team.
The first explicit reference to fluxes appears in Dr Sparrow's undated meeting notes (CB.019.153) which record:
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
When asked about the reference to "Kirk Othmer", Dr Sparrow explained:
There were a number of areas people decided they would go and try and find appropriate materials to look at and Kirk Othmer is a scientific encyclopedia, I think you class it as. It's got a lot of chemical processing information and that's one place where you would find some information about fluxing type agents.
……
Just for completeness, what is the JCPDS? --- The JCPDS cards are the results of x-ray diffraction patterns of a whole lot of phases that uses a reference for characterising materials and my understanding of this was that they contain conditions under which the different sorts of phases would form and they give references to the original reports of their form. So that was another place to go and find thorium compounds, which is what the Th was for, that might be useful in what we were trying to achieve. (TS.944.3)
The date to be assigned to Dr Sparrow's notes was the centre of significant dispute. He explained in evidence-in-chief that his practice was to glue a typed meeting sheet to the left-hand side of his notebook, and to record in handwriting the events of the meeting on the right-hand side. According to Dr Sparrow, his undated notes were made on 15 July because of their position in the notebook. However, Dr Sparrow conceded that he was unable to assign a date to his notes due to any recollection of the events recorded:
Do I take it that apart from your notebook, you don't specifically recall that meeting? --- On that meeting, the notes at the very bottom of the second handwritten page, I do recall an incident relating to those. (TS.920.18)
… but are you able to recall the date as well as the incident? --- I can only recall the date because it's noted in my notebook against 15/7.
That's right, so you are relying, as I understand it, wholly on what your notebook says for the purpose of assigning a date to that incident? --- Yes. (TS.921.10)
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
The motive for the suggestion
Professor Lawson states that fluxes have a very wide range of uses which he sets out in some detail in 3 Lawson 2.3. In 2 Houchin 11, Dr Houchin defines the meaning of "flux" as "something which will help mobilise or assist the formation of another phase at a lower temperature". This definition is not inconsistent with Prof Lawson's analysis but as further explained by Dr Houchin:
They are really two different things, are they not? Helping to mobilise something is not the same thing as assisting the formation of another phase at a lower temperature? --- That's correct.
So the word here you are using, on your own definition, can have two quite different meanings? --- No, I'm suggesting that a flux can fulfil two quite different functions.
WIM argue that the primary purpose suggested by Dr Grey on 22 July was to "flux the thorium in the pores" which is consistent with the first aspect of Dr Houchin's definition and hence an intention to promote the formation of a glassy phase, and that the words "also to lower temperature" demonstrate that temperature reduction was merely a secondary purpose of the proposed use of a fluxing agent on 22 July. On this basis WIM reject Iluka's submission that work undertaken by the SREP project team subsequent to the involvement of Dr Grey followed logically from Dr Aral's experiments.
I will return to this area of dispute in due course. For the present, it is sufficient to note that, on its face, Dr Grey's alleged motives for using a flux are in keeping with his own evidence (TS.750.31) that he
was aware that the thorium parent was in the micropores and I was suggesting work at getting a flux into the micropores in a liquid form to take up the thoria, but I also knew that the daughter products would also have to go into that phase and that there was a good chance that if there was a liquid phase present in the pores, then the pore coarsening that would take place would occur at a lower temperature and release those daughter products.
It will be recalled that Dr Grey's suggestion of heating test work on 29 April was also aimed at coarsening the pore structure to release the daughter products (cf. TS.751.23).
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
The use of additives in the zircon work
Dr Hollitt said in cross-examination that WIM "were looking to go to lower temperature" through the use of an additive (TS.181.30), but the first explicit suggestion of additives appears in the CSIRO progress report on the zircon work (exhibit MJH-63) where Dr Grey proposes the addition of spodumene and barium compounds to promote the formation of a liquid phase at a lower temperature. Dr Hollitt implicitly agreed that Dr Grey's additive suggestion was conventional practice in the field at the time (TS.182.1 and TS.183.9, and see also TS.208.29), and in this light further accepted that it was similar to his own idea in March 1992 of adding borax as a flux to lower the temperature at which the relevant phases were forming (TS.222.3).
There is no evidence that Dr Grey's suggestion prompted this idea as asserted in 1 Grey 3.16, but it must equally be said that the evidence does not lead to the conclusion that either proposal was specifically aimed at facilitating glassy phase formation. Although Dr Hollitt acknowledged that additives such as spodumene could form a glass "under the right conditions" (TS.182.4), Iluka have not advanced, nor is there in my view any evidentiary support for, the proposition that Dr Grey had this intention in mind (cf.TS.723.29). The test work conducted on borax addition was intended to promote the formation of the B phase (exhibits MJH-66 and MJH-73) and, while I accept WIM's submission that this interest arose in the context of a process in which a glassy phase was also formed, the fact remains that the B phase formed during the test work was crystalline (TS.221.6).
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
Dr Grey's Experimental Activities
Background
Dr Grey did not become directly involved in the SREP project work until mid-July, although he did attend most of the weekly project team meetings before then (1 Grey 4.17). On or about 2 July, Mr Harris went on leave for approximately three weeks. He gave evidence that he would not have gone on leave unless he thought
there was a solution or we were working in the right direction … (TS.642.5)
The solution to which Mr Harris refers was that arising (or which it was anticipated would arise) out of the oxidation and reduction test work which was carried out between May and mid-July 1992. Mr Harris was acutely aware of the commercial pressures on Iluka but "intended to [develop a research program] correctly after the failure of the AUP" (TS.642.13). At the time Mr Harris went on leave, no thought had been given by the SREP project team to the formation of a glassy phase to take up radioactive impurities (see eg. TS.618.5, TS.941.29 and 2 Houchin 13), nor had there been any discussion concerning the addition of glass forming reagents. Heating and leaching remained the "prime focus" of research (TS.616.8).
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
The notes of the 6 May 1992 project team meeting record a passing remark by Dr Aral that the thorium specks he observed may be a glass. Iluka have argued that Mr Nicholson may have had Dr Aral's remark in mind when recording this suggestion. However, it seems highly unlikely that in a section of his notes opposite the name "Ian Grey" Mr Nicholson could have intended to record a single observation made by Dr Aral more than two months earlier. Mr Harris said in evidence that he did not recall any mention of the term "glass" at the meeting (TS.649.6), but I consider this evidence must be read in the light of his inability to remember "a lot about the meeting itself on 22 July" because maintenance personnel working at Eneabba "actually blew up the attritioners, which is a pretty serious incident, and that pre-occupied my mind on the 22nd of the meeting" (TS.647.5).
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
WIM submit in response that as evidenced by his experimental activities, Dr Grey had relied on knowledge imparted to him by Dr Hollitt to find a solution to Iluka's radioactivity problem within a relatively short period despite several months of research activity by other members of the project team prior to his involvement.
The phosphate experiments
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
Dr Grey commenced his experiment by adding ammonia to a solution of thorium nitrate to obtain a gelatinous precipitate of hydrated thorium oxide which simulated the finely dispersed form of thorium in altered ilmenite concentrates.
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
Did the phosphate experiments follow from the earlier SREP work?
Prof Lawson was critical of the suggestion that the course of research on which Dr Grey embarked was catalysed by Dr Aral's heat treatment work. He firstly argued that Dr Grey's decision to heat to 900oC ran contrary to Iluka's matrix test results which had shown that the benefits of heat treatment for the removal of radionuclides were minimal at that temperature. I am not convinced by this argument since it overlooks the fact that the matrix test work had produced encouraging results at temperatures of around 1000oC in that increasing amounts of both parent 232Th and its progeny 228Th were removed equally (see eg. TS.624.23). In a related argument Prof Lawson pointed out that Iluka's test work which had been conducted at 100oC temperature intervals suggested that the optimal temperature for enhancing the accessibility of the daughter products lay between 1100oC and 1300oC. On this basis he contends that it would have been more logical following Dr Aral's heating experiments to optimise the temperature, and also the furnace and leaching conditions, rather than "looking for additives" (3 Lawson 5.5).
As a general proposition it seems reasonable to suppose that in any particular line of research there are often a number of alternative courses of action each of which may, after the event, be characterised as "logical". Prof Lawson's proposed course of optimisation no doubt falls within this category, but there is no evidence on which his contention that this course follows more logically from Dr Aral's test work than the direction in research pursued by Dr Grey can be sustained. Indeed, the evidence given by Prof Lawson in cross-examination on this point essentially goes no further than identifying a preferred choice from among possible options "had it have been me" (TS.333.10), which smacks a little of an attempt to discredit Dr Grey's stated reasons for searching for an additive from the perspective of hindsight. Importantly though, Prof Lawson did not suggest that Dr Grey had adopted an illogical line of enquiry.
Further, and as mentioned earlier, Dr Grey's microprobe studies in early May led him to consider that the increased leachability of thorium was due to it forming compounds with impurities in the pores, particularly silicon and phosphorous which were "known to go into the pore structure of ilmenite during its weathering". (TS.720.5) In fact it was this idea which had prompted Dr Aral's quartz and montmorillanite experiments beginning on 7 May (TS.800.10).
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
The shift in research direction
Prof Lawson has then drawn attention to what Mr Catterns coined as the "progression" of Dr Grey's experiments. He agreed in the course of cross-examination that there had been a logical progression in the development of the SREP process up to the stage where Dr Aral conducted his 1400oC experiments which, so far as he could see, owed nothing to WIM (TS.329.24).
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
Did Dr Grey intend to form a glass?
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
He (Dr Grey) responded as follows to Dr Emmerson's intense line of questioning on this point:
Did it not strike you, Dr Grey, that in doing this work for RGC in an attempt to remove radioactives from titanium containing minerals, you were getting perilously close to simply carrying out what Dr Hollitt had suggested you do on behalf of WIM? --- At that stage, at the beginning of that experiment, no. (TS.494.31)
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
In 2 Grey 3.39, Dr Grey states that his notes of 21 July 1992
record that the next step in my experiments was to weigh a portion of the crystalline NaTh2(PO4)3 and add it to hot 20% HCl to determine its acid solubility. The mixture of acid plus compound was stirred and maintained at 80-90oC. A parallel leach treatment was conducted on the 900oC heat treated thorium oxide sample.
He then explains that
after 1 hour of leaching, the leach solutions were examined and I noted that there appeared to be very little dissolution. I added 0.2g of NaF to each of the two leach solutions and continued the leach at 90oC for a further 45 min. The residues were filtered, dried at 115oC and weighed. There had been 68% leaching of the heated thorium oxide but only 13% leaching of the NaTh2(PO4)3. As seen by my notes, I was clearly surprised by this result (having expected the crystalline thorium compound to be more readily leached than the results indicated) and I checked the X-ray patterns of both samples, noting that the heated thorium oxide pattern had considerable line broadening whereas the peaks of the NaTh2(PO4)3 were very sharp.
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
In 2 Grey 3.46, Dr Grey says that he changed his research direction on 22 July
only when I found that the sodium thorium phosphate crystalline phase was not very soluble. Even then, however, my notebook records demonstrate that I was not motivated to make a glass.
It is contended by WIM that this statement is plainly contradicted by the notes of other team members present at the meeting on that day in which glass forming agents and glass formation are specifically mentioned.
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
Did Dr Grey use WIM's confidential information?
Dr Emmerson suggested that Dr Grey's phosphate test work involved
an approach whereby you could use any information which you had which was likely to solve the problem, didn't it? --- No, it used the information that I had progressively gained within the SREP project from the early heating work through to the microprobe work through to the sodium phosphate.
What information had you gained through the WIM project including zircon and including the soda roast? --- No, I agree that information would have been in my head but I tried to treat this problem on its own merits and work through logically on the information I had to tackle it on its own merits without trying to make use, certainly consciously not making use of any other information I had. (TS.514.3)
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
Are you agreeing with me that you do not put out of your mind what Dr Hollitt told you? --- I would have to agree it is impossible to clear your mind completely of information you've gained over the time of your research as a general principle, yes. (TS.497.16)
What I suggest to you is that this is not an adequate time for your memory of what Dr Hollitt had told you to have faded? --- No, the projects were carried out in parallel and it's reasonable to say that I would have information in my mind at the time on all projects. (TS.498.2)
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
What I am suggesting to you, Dr Grey, is you should have thought along the lines of: is this getting too close to WIM's work? --- Yes, I accept that. (TS.504.23)
This raises another of the more difficult factual issues in the proceeding, but after carefully examining the matter the basis for WIM's proposition regarding Dr Grey's alleged inability to maintain a Chinese wall is, in my opinion, misconceived. Dr Emmerson restated the outcome of Dr Grey's first experiment as follows:
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
When requested to identify "the idea" by Mr Catterns, Dr Emmerson replied:
The idea that I am referring to is the idea which was disclosed to [Dr Grey] by Dr Hollitt on the 23rd of June and the following days, the idea we discussed this morning. Do you understand that? --- That we used soda ash to remove silica from titanium concentrates? (TS.509.20)
This is without doubt a reference to the soda roast process first disclosed by Dr Hollitt to Dr Grey during a conversation on 23 June 1992. The process, it will be recalled, involved roasting WIM's HiTi concentrate with sodium carbonate and was aimed predominantly at silica removal. The evidence clearly established that the soda preferentially reacted with the silica to form a glassy phase that could take up the silica and other impurities such as alumina. However, the evidence was insufficient to satisfy me that Dr Hollitt had told Dr Grey of the shift in the process originally described to him to the treatment of HiTi and ilmenite as a combined stream and, more relevantly, that a glassy phase could be used in the combined stream process to remove radioactive impurities. The vice with WIM's approach therefore lies in the fact that it overstates the disclosures made by Dr Hollitt to Dr Grey. Moreover, this approach finds no evidentiary support that in conducting his phosphate experiments Dr Grey had simply resurrected knowledge derived from WIM.
In evidence, which was neither the subject of cross-examination nor direct rebuttal evidence, Dr Grey explained that the weight ratio chosen for his first experiment was typical of those used when forming crystallised compounds from liquid fluxes. Dr Grey's motives here are, my opinion, supported by the uncontested evidence of Prof Brungs who states that a researcher intending to dissolve a compound in a liquid (irrespective of whether it cools to a glass) usually requires a weight ratio between flux additive and starting compound of the order of 10:1 (Brungs 53). Prof Brungs accordingly argues that the weight ratio employed by Dr Grey for the purposes of his first experiment (1.6:1) is inconsistent with an intention to dissolve the thoria into the additive at elevated temperature, but rather indicates the intention to form a compound between thoria and phosphorous. Indeed, Dr Grey has explained that the weight ratio chosen by him corresponds with those typically utilised to crystallise compounds from liquid fluxes (2 Grey 3.35). Moreover, the logic inherent in Dr Grey's use of a phosphate given the identification of silicon and phosphorous in Dr Aral's specks is not in issue and it is in this context that Dr Grey submits that it is mere coincidence that both are glass forming agents.
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
According to 1 Grey 4.21, he
recognised from my earlier projects that the additive would need to penetrate the very fine pore structure to gain access to all the thorium as well as the daughter products released on heating. I decided to continue with sodium dihydrogen phosphate which was readily soluble and could be added as a concentrated solution.
He confirmed in cross-examination that the reason for using sodium phosphate in solution as before was to ensure that it penetrated the ultrafine pore structure of ilmenite which he knew from his reducibility in ilmenite project incorporated the impurities. Dr Emmerson put the proposition that the need to penetrate the ilmenite micropore structure did not remove the inference that Dr Grey had ultimately relied upon knowledge imparted to him by Dr Hollitt.
Let's understand this. Having the information from Dr Hollitt at hand, the additional step that you thought you had to take was work out how to get the reagent into the pores, is that correct?
--- What I had from Dr Hollitt was addition of a sodium compound followed by roasting, followed by leaching.
……
And you also had the information from Dr Hollitt you would make a liquid phase? --- Yes.
What I'm asking you is whether you say the additional step that you are going to take was to get the added compound into the micropore structure? --- No, I think that was just one of the difficulties I had to overcome in this particular problem. As I say, I treated each problem totally on its own merits and that was one of the difficulties I had to deal with in this problem, that I didn't have to deal with in other problems. I don't think it makes it unique as such, it is just it was another problem. (TS.530.1)
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
This passage confirms Dr Grey's initial focus on the formation of a crystalline compound and, equally, demonstrates the attempts made by Dr Emmerson to establish a causal relationship between the SREP test work undertaken by Dr Grey and the soda roast work disclosed to him by Dr Hollitt resulting from the conceptual similarity between those processes. As acknowledged by Dr Grey:
In the broad concept of using an additive to react, form a liquid phase and then leach it, if it is expressed as broadly as that it does sound the same, yes. (TS.535.1)
I do not view WIM's approach based as it is on the soda roast process as particularly cogent or persuasive since, as stressed by Mr Catterns, this unfairly assumes as an element of that process "something that Dr Grey has denied 30 times, namely that Dr Hollitt told him about radioactives." (TS.550.4) Moreover, there is a substantial quantity of evidence in relation to the work expended by Dr Grey in relation to SREP which has shown that he was uninfluenced by knowledge derived from WIM, and instead explored independent avenues of enquiry. Notably, Dr Grey's selection of a sodium phosphate compound was not based on its glass forming properties which is consistent with the perception I have gained from the evidence that Dr Grey was motivated to form a crystalline compound which would take up the thoria for subsequent leaching.
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
However, this latest attempt at demonstrating that Dr Grey's experiments were assisted by knowledge he had acquired from the soda roast work must fail for the same reasons as before. As I have repeatedly stated, the evidence does not show that that process was concerned with the removal of radionuclides, and Dr Grey's stated motives substantiated as they are by his contemporaneous notebook entries must be preferred to WIM's unsupported assertions which overstate the disclosures made by Dr Hollitt. There is also the matter of Dr Grey's uncontradicted evidence that he did not discuss sodium carbonate with Iluka due to his confidentiality obligations to WIM.
Summary
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
The evidence has also shown Dr Grey was aware, firstly, that the formation of a glassy phase in the lime roasting of zircon promoted the removal of radionuclides and, secondly, that a glassy phase could also be used for removing silica and other minor impurities from HiTi concentrate. The single fact that Dr Grey was, given the time frame involved, in all likelihood conscious of that information when conducting his test work for Iluka would, in the absence of the mix of other considerations which have emerged in this case, weigh heavily towards the position for which WIM contend.
However, I have already expressed my confidence in Dr Grey as a witness and he has, in my opinion, given his evidence truthfully in respect of this crucial issue. Moreover, this evidence is, as already indicated, internally consistent with Dr Grey's notebook entries and so must be weighed in favour of the unconfirmed evidence presented by WIM from which it is difficult to draw useful inferences.
[PASSAGE NOT PUBLISHED BY REASON OF CONFIDENTIALITY]
Accordingly, I find that Iluka have discharged their evidentiary onus of satisfying me that Dr Grey effectively compartmentalised WIM's confidential information in independently arriving at a solution to Iluka's radioactivity problem.
CONCLUSION
This proceeding has arisen in the circumstances of events which took place many years before the hearing and, as would be expected, there is significant dispute about much of what occurred. On its face the considerable array of evidence placed before me invites a number of inferences to be drawn in favour of WIM which is not altogether surprising given the timing of the events in question and the extent of Dr Grey's involvement with both parties. However, the unsubstantiated professions of recall on which WIM have principally relied have for the reasons discussed in this decision posed serious difficulties of proof for them as compared to the case for Iluka which is largely founded on contemporaneous records or other corroborative material. It is in this light that having weighed the evidence I am satisfied that Dr Grey did not acquire the invention from WIM or use their confidential information to Iluka's advantage.
I therefore conclude that WIM are unsuccessful in the section 59 opposition. In the result, the only determination left open to me under section 32 is that the application continue to proceed in the name of Iluka alone, and that the presently named inventors remain unchanged. There is, however, a final matter to consider. Iluka's closing submissions raise the point that because serious allegations have been made against them, CSIRO and individual scientists
the Commissioner should … consider making a positive finding that the allegations are wrong and should have not been maintained after the filing of the Applicant's evidence in answer.
Although perhaps relevant to the Federal Court proceeding, this submission fails to take account of the fact that the Commissioner only has power to determine matters in relation to the administration of the Act, and no other jurisdiction (cf. ReApplications by Dennis Brian Moriarty 26 IPR 21).
I have also found coincidentally that claim 39 "travels beyond the matter disclosed in the specification" (Olin Corporation v Super Cartridge Co Pty Ltd (1977) ALJR 525). Claim 39 therefore lacks fair basis with the result that the specification does not comply with section 40. As this deficiency can be easily overcome, I allow Iluka 30 days from the date of this decision to file appropriate amendments.
COSTS
The power of the Commissioner to award costs is discretionary, so I must take into account all relevant considerations (American National Can Co v W R Grace & Co-Conn 29 IPR 292).
Having considered all the circumstances in this case I see no reason to depart from the normal practice that costs follow the event, and therefore award costs against WIM in respect of the section 59 opposition. As the request for a determination under section 32 relies on the same material on which the opposition is based, I make no award of costs in respect of the section 32 request. I also consider an award of costs to be inappropriate in respect of the section 40 deficiency noted above since this was found on my own volition.
O L Haggar
Delegate of the Commissioner of Patents
Patent attorneys for the applicant : Freehills Patent Attorneys, Melbourne
Patent attorneys for the opponent : Arthur Robinson & Hedderwicks, Melbourne