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Archive of Reports on IG meetings
Late 1986-1988

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BCA Industrial Group/JCPDS-ICDD Powder Diffraction Course

The Powder Diffraction Course, held 4-6 November 1988 at the Science & Engineering Council's Daresbury Laboratory, Cheshire, was the first to be organised by the Industrial Group of the British Crystallographic Association. Since it was formed in 1983 the Group has arranged numerous one-day specialist workshops, mainly for small groups of industrial crystallographers who need an overview of a p articular topic, or wish to keep abreast of latest developments. These have covered a diversity of topics, such as residual stress analysis, studies of clay minerals, quantitative analysis, computer programs for PD and the analysis of double-crystal rocking curves, but never before had a three day PD course been attempted.

The Daresbury Laboratory, home of the UK dedicated synchrotron radiation source, with an active powder diffraction group, was an ideal venue. The course, which attracted 34 participants, was sponsored by JCPDS-ICDD and conducted with characteristic enthusiasm by its Principal Scientist, Ron Jenkins. The programme was based on the well tried format for such courses, used world-wide by the Joint Committee, except that particular emphasis was placed on the use of the CD-ROM versions of the PDF and the Crystal Data File which were introduced recently. In view of the success of this first venture and the obvious demand for tuition in basic powder diffraction, it is the G roup's intention to hold similar courses from time to time in the future. Details of these will be published in 'Crystallography News'.

J. Ian Langford


BCA Spring meeting - Warwick 1988
BCA Workshop on Practical X-ray Diffraction

(Co-ordinated by the Industrial Group)

This workshop took place at the BCA Spring meeting at the University of Warwick and was chaired by the organising co-ordinator Dr Jim Chisholm (Br itish Museum, Natural History). Over 100 people attended.

The first presentation was made by Eric Kelly (Electricity Council Research Centre) who was responsible for the organisation of the BCA Industrial Group round robin on computer programs for lattice parameter calculation. Some interesting conclusions arose concerning compiler options, data storage and use of appropriate extrapolation functions. Different software was compared on the same computer (at ECRC) and the same programs on dif ferent machines. The raw data circulated and all results are available in a summary report obtainable from Eric.(Link to report)

Paper two was concerned with the accuracy and precision of cubic unit cell lattice parameters and was given by Dermott Wood (BP Research Centre). The materials examined were CeO2 - used for calibration, PSD assessment, comparison of extrapolation functions and peak location methods, checking for off-axis effects - and Ag for calibration and testing of a high temperature environmental chamber. Some interesting results were shown relating to data collected with and without Soller slits, and both the high temperature facility and the PSD gave good results.

Dr Jim Chisholm (British Museum, Natural history) delivered the third paper on matching measured to calculated lines and least squares refinement on Debye-Scherrer powder photographs. The concern was that the precision quoted after refinement was at least a factor of 2 lower than in reali ty. A possible explanation was that "data massaging" occurs via the use of data that seems to fit well and the use of unrealistically low tolerances. Comments were made about large cell materials increasing the problem and that the use of weightings might be appropriate.

The fourth paper was given by Dr Stephen Tarling (Birkbeck College) on the subject of 'Dynamic Environmental/High Temperature Powder Diffraction using a Laboratory System'. A variety of examples were given concerning the us e of a high temperature attachment in conjunction with a PSD, ranging from paint pigments, zeolites, drugs, cements and corrosion products on Egyptian bolts. Some problems and their solutions were highlighted as well as ideas for future improvements that would be greatly beneficial.

The final presentation was made by Dr Mike Glazer (University of Oxford) on 'Rietveld Refinement in Practice', and began with an introduction to the technique. The process of Total Pattern Fitting was described for analysis of complete diffraction spectre, and the need for very good quality/high resolution data for 'ab initio' structure determination was emphasized. The basic refinement strategy was outlined

and the use of well defined peak shapes was recommended - either via good mathematical medals or simple (aberration-free) experimental systems. Finally, the range of R-factors in usage as a measure of the quality of the refinement were described.

Thanks are due to all contributors fo r an interesting and interactive session. Anyone requiring further information should contact the authors themselves who will be only too glad to give assistance, I am

sure.

Adrian Jones


BCA Industrial Group Symposium - Spring Meeting

Warwick University, 30 March 1988

The Industrial Group were delighted to welcome Dr. Bill Parrish, one of the founder members of the American Crystallographic Association, as its opening speaker.

He was soon extolling the virtues of X-ray diffraction which is undergoing a remarkable transformation as a result of the discovery of the high temperature superconductor. XRD is the single most powerful method used to determine the phases formed in the high temperature superconductor and is now benefiting from a wider exposure to materials scientists and solid state chemists. In the history of the powder method, Dr. Parrish felt that we were now in one of its most finest hours because of the recent advances made with the new source of radiation from the synchrotron. He described the optics, instrumentation and methods used with the synchrotron parallel beam, pointing out the opportunities in angle and energy dispersive diffraction. Glancing angle diffraction for thin film analysis was highlighted using iron oxide thin films as examples. However, with 15,000 diffractometers throughout the world he made it clear that there are not enough synchrotrons to meet th e potential demand! Some of the fundamental aspects of line profile analysis using synchrotron radiation were described in detail, a2 elimination, increased resolution and the detection of features obscured by long Lorentzian tails were covered. High peak to background ratios were possible for all diffraction patterns because of wavelength sensitivity. The fluorescence problem, for instance, could be reduced by tuning the wavelength just beyond the absorption edge. Dr. Parrish also commen ted on some of the less desirable effects associated with parallel beams from a synchrotron source, particularly the intensity variation caused by particle sizes greater than 10~m. He emphasised the need for good specimen preparation and ended by gratefully acknowledging his collaboration with Professor Hart.

The second paper by Dr. Lionel Clark from Shell Research was a good example of the success of teamwork in studying the surface structure of ZrO2 ceramics. ZrO2 is stabilised into a tetragonal phase by the addition of MgO but stress induced toughening causes a tetragonal to monoclinic transformation. Interest lies in the mechanism behind this transformation. XRD has been used successfully to assess the effect of lubricants on the weight fraction and distribution of the monoclinic phase in the surface. Cathodoluminescence and Laser Raman spectroscopy have also proved valuable in investigating the structure at grain boundaries. Lenticular grains of the nominal ly monoclinic phase within the tetragonal matrix were observed in the TEM but the electron diffraction pattern did not confirm a monoclinic phase. In conclusion Dr. Clark felt that XRD had been the most successful technique applied, commenting that sectioning of samples and beam heating (in the TEM) may have introduced other problems.

Dr. Judith Milledge completed the first session of talks by describing the way in which diffraction data from different sources could be reconciled, acknowled ging at the outset the longstanding co-operation between the Statistical Science and Crystallography departments at University College, London. Various techniques have been devised for R factor refinements but Dr. Milledge felt that it was admissible to restrict the input to certain peaks, suggesting that data should be sampled and not taken as a whole. In the iterative process of structure factor least squares convergence different strategies had to be devised. Silicate garnets were used as an exam ple of the method of selecting certain reflections and site occupation by magnesium and calcium was equated to unit cell parameters. In theory one reflection was all that was needed. Another example of the monitoring of certain reflections only was in the study of unstable crystals when there is a limited time to gather information. Dr. Milledge convinced many crystallographers that, in any data set, there was always the opportunity to be selective.

Professor Mike Hart of the University of Manchester presented the first paper of the second session entitled "Synchrotron Radiation - Does Industry Need It?", a topic dear to his heart, although, as he said, a title that he himself might not have used. It was after all rhetorical. He chose two topics to illustrate the totally new opportunities that now exist with synchrotron radiation at Daresbury, opportunities that, it was stressed, are not possible in conventional laboratory experiments. Special Laue patterns with 100 times as many spo ts as seen in laboratory experiments are available in a few seconds and can be used to study silicon and silica thin films. Because of the pulsed source of radiation in the storage ring, time dependent studies of surface strains and temperature distributions were also possible. The second illustrative aspect of diffraction using synchrotron radiation was the total freedom afforded to the experimentalist to optimise both wavelength and geometry for specific purposes. At glancing incidence, the top 50 Angstroms of a surface could be analysed for Bragg peaks in conjunction with a spectroscopic analysis of the fluorescent radiation excited in the specimen. Wavelength variability could be exploited by going close to the absorption edge for near surface structural analysis and beyond the edge to study bulk structure. X-ray energy just above the edge is used to excite photoelectrons for EXAFS studies, in which the backscattering of these electrons modifies the transmitted X-ray intensity. Fourier tr ansformation of the data to produce radial distribution functions of atomic positions has been used in many studies, the way in which water may leach radioactive materials from glass structures being just one example chosen. Professor Hart ended his talk by outlining the marketing aspects of industrial collaboration in using the facilities at Daresbury, and left the audience in no doubt about the answer to the question in the title of his talk.

The session ended with an enthusiastic present ation by Dr. Paul Barnes of Birkbeck College on the use of intense radiation sources for dynamic studies of phase transformations. Three examples were chosen. The first was a study of polytypism in silicon carbide crystals grown by G.E.C. Hirst Research Centre. No single polytype could account for all the observed Laue patterns but it was established that there were disordered regions in the centre of the crystals and more ordered structures in the outer cooler parts of the crystals. In the second application of the technique, the distribution of aluminium and silicon in ultramarine was determined. It was shown that there was a random occupation of the tetrahedral sites by aluminium and silicon in the synthetic ultramarine, unlike the ordered structure in geologically mined samples. Finally in a very interesting description of the curing of aerated concrete blocks in autoclaves, Dr Barnes entertainingly provided a video film of the industrial process. The morphology of growth was related to n eutron diffraction peaks; calcium hydroxide growth and free water loss were also determined. The final phase, tobermorite, was on display and has remarkable properties being extremely light and a very good thermal and acoustic insulator.

All five speakers provided a very varied and informative insight into the latest developments and applications in crystallography in industry. The organisers and our hosts, Warwick University are to be congratulated on a well thought out and a well executed programme.

P. A. TEMPEST.
Central Electricity Generating Board.


IDENTIFICATION AND THE JCPDS POWDER DIFFRACTION FILE

On Thursday, 19 February, the Industrial Group held its sixth Specialist Symposium on the identification of unknown substances by means of powder diffraction data. The venue was again the GEC Hirst Research Centre, Wembley. The Group shares the concern of the BCA Council about the inadequacy of crystallo graphic education and training, particularly with regard to the needs of industrial organisations. Previous symposia have attempted to remedy this situation in a small way, by inviting specialists in various fields to review techniques and recent developments.

The latest symposium, however, was a new venture for the Group: 17 crystallographers mainly from industrial laboratories, including some with little experience of powder methods, learnt about the routine use of the JCPDS Powder Diffra ction File (PDF) for identifying unknown materials.

The seminar was based on the PDF workbook, together with the NBS-data subfile and its search manual. The material was supplied to the Group by the JCPDS- International Centre for Diffraction Data. A short introduction on the use and scope of the PDF and the basic concepts of search/match procedures was followed by a 'tutorial' in which the participants tackled examples in the workbook. For this I was assisted by John Harding (BR Derby) and Steve Tarling (Birkbeck College). In the time available it was only possible to cover manual searches of the file by means of the alphabetical, Hanawalt and Fink indexes. It is intended to hold an 'advanced' session on computer search/match methods in due course and a symposium on the important topics of data collection and evaluation and on the treatment of instrumental and sample-induced errors is envisaged.

From our experience in conducting our first PDF workshop, it is clear that the Industrial Group can provide a valuable service in training diffractionists in search/match methods and it is likely that further short courses on the subject will be arranged from time to time.

J. Ian Langford.


Autumn Meeting, 6th November 1986, British Rail, Derby

The Autumn meeting of the B.C.A. Industrial Group was held on November 6, 1986 at British Rail's Training School, Derby, our hosts being British Rail Research Di vision.

The Chairman of the morning session, Brian Bellamy (A.E.R.E. Harwell), introduced Dr. Robert Sparrow who as Director of Research of the Railway Technical Centre welcomed the delegates. Dr. Sparrow then proceeded to give the first paper entitled 'The role of the Research Division'. He gave a breakdown of the way in which research at British Rail is funded and how it advances the technological base essential for future business, while at the same time helping to minimise costs and max imise the effective use of the Board's assets. He conclusively demonstrated these points by showing how research into effective ballast packing and track levelling had increased periods between maintenance and significantly reduced costs.

The second paper given by Miss Kath Swift (Rolls Royce PLC) was entitled "Residual Stress measurements in Aero Engine Material'. She described how quantification of elastic stress and plastic deformation generated during the manufacturing processes of the se high technology components, is leading to understanding of service fatigue life, and how X-Ray Diffraction can be use to monitor and control these surface stresses during production. The results presented demonstrated how successful their hardware and software modifications had been in analysing these residual stresses.

The third paper entitled 'Quantitative Analysis of Thin Layer Samples' was given by Cees Brandt (Philips I and E Division, Almelo, The Netherlands). A concise review of t he current techniques available for infinitely thick polycrystalline samples was presented, followed by a review of possible calculation models, and methods of overcoming instrumental variations and unknowns. Methods of applying these techniques to thin layer samples where thickness and density of packing were two further unknowns were described, and methods of overcoming these problems were presented.

The last paper of the morning session was presented by Dr. Pierre Graves (A.E.R.E. Harwe ll) entitled Applications of Laser Raman Microscopy, A Technique to complement X-Ray Diffraction. The Harwell Laser Raman Microprobe (LRM) was described together with an introduction into the field of Raman Spectroscopy. The usefulness of the technique in conjunction with XRD and EPMA was demonstrated using the results obtained from zirconia based ceramics, oxide layers on stainless steel and silicon based semiconductors.

The afternoon session chaired by Dr. Alun Bowen (R.A.E. Farnborough) opened with 'Aspects of the High Resolution Powder Diffractometer on the Spallation Neutron Source at the Rutherford Appleton Laboratory' presented by Dr. Bill David (Rutherford Appleton Laboratory). The potential of the HRPD with a D d/d of 5 x 10-4 was demonstrated by the structure determination of FeAsO4, and subtle symmetry changes in NiO. Additional information on strain distribution, sample homogeneity, anisotropic crystallite size, could also be obtained. Applications of the technique with respect to time resolved kinematic experiments and multiphase analysis were discussed.

In the second paper of the afternoon Dr. Jim Chisholm (British Museum - Department of Mineralogy) described how using a microcomputer he was now able to generate simulated powder photographs directly comparable with actual photographs. Intensity was indicated by the spacing of the spots making up the line. The closer the spots the more black the line. It was possible to select wavelengths, generate powder patterns of mixtures and calculate powder patterns to test different structural models. It was felt by a number of those present that this program, based as it is on a microcomputer, could be a valuable teaching aid.

The final paper of the day was given by Simon Clark (Birkbeck College) entitled 'Time resolved X-Ray and Neutron Diffraction Analysis of Hydrating Cements'. The chemical reactions in the manufacture and use of cements were brief ly outlined, followed by a description of the time-resolved studies carried out at Daresbury and the neutron source at ILL. The very promising data is still being fully analysed.

Over seventy people attended this meeting and were rewarded with well presented papers of a very high standard. The organisers also are to be complimented on an excellent meeting.

Derrick Hart
Plessey Research Caswell Ltd


SPECIALIST INTEREST WORKSH OP

COMPUTER PROGRAMS FOR POWDER DIFFRACTION PROBLEMS

A specialist interest workshop was held at Springfields Nuclear Power Development Laboratories on 9 October. Twenty-seven delegates attended. four of whom came from outside the U.K. The equipment manufacturers Siemens and Philips were also represented. This meeting was intended to enable everyone to describe their work on

"crystallographic" computer programs and to contact others with similar interests. The works hop was also designed to see whether not it is possible to sec up a directory of available programs and start round robin tests to find the best program in a particular field. however these undertakings require time and money which is not forthcoming.

The meeting timetable was informally divided into subjects, although the discussion varied over a wide range of topics within these limits, which are listed below.

LATTICE PARAMETER CALCULATION AND REFINEMENT

There seem to b e a number of such programs in use. Eric Kelly (Electricity Council) agreed to co-ordinate a round robin test to compare their results in the near future. Dr Ian Langford (Birmingham University) pointed out chat small micros do not offer sufficient numerical precision to produce reliable results.

INDEXING POWDER PATTERNS

These are running on either minicomputers or mainframes, not on micros. They have been summarised by R Shirley from the University of Surrey.

PATTERN PR EDICTION AND SIMULATION

Again programs are available from Philips and Siemens, different ones are in use at Daresbury, Springfields and Harwell. A program is also included as part of the Cambridge Crystallographic Library. No good methods are available for triclinic systems. Dissatisfaction was also expressed with the JCPDS choice of alpha alumina as an intensity standard as small changes in the atomic co-ordinates produce large variations in the calculated peak intensities. Programs are al so being used to simulate peak profiles. Gaussian methods were generally thought to be to unsatisfactory. This was discussed further when line broadening was considered.

LINE BROADENING, CRYSTALLITE SIZE AND INELASTIC STRAIN MEASUREMENTS

There is a considerable amount of activity in this area and it would make an interesting topic for a BCA workshop.

Dr Ian Langford described the programs used at Birmingham University for simulating peak profiles by Fourier an d Rietveld methods to enable the decomposition of overlapping peaks. Harwell are using both Fourier methods and the program supplied by Siemens for crystallite size measurement.. There was considerable debate about

exactly how realistic peak profile simulations are.

A different method is in use at Springfields for crystallite size and inelastic lattice strain measurements, using a program which allows the crystallite shape to be simulated by the user. Daresbury are also developing line broadening programs. Most other people appear to be using the programs supplied by Philips and Siemens.

STRESS ANALYSIS AND PEAK LOCATION

Rolls-Royce have developed their own programs and equipment for stress analysis. Harwell are also working on new methods. The Siemens stress package is being used at Springfields. Most people are using the Philips or Siemens programs for peak location. Both programs tend to miss peeks in patterns containing reflections with very different breadths. ICI at Runcorn have their own programs which can use a variety of search models.

SEARCH MATCH

The Siemens, Philips and Johnson-Vand search methods are in use. Most of the problems encountered have been ascribed to the original data quality. Programs are now emerging chat can be run on micros. A standard D/I file format would be useful so that data can be transferred between different search programs running on the same system.

Quantitation, texture and the locat ion of amorphous peaks were also discussed.

IDEAS FOR THE FUTURE

Dr L Garcia de Viedma described the Nuclear Energy Agency (NEA) database in France. This is a European organisation which tests programs for nuclear industry and then makes the programs available to anyone who is interested, It is funded by the EEC but cannot buy or sell programs. Most of its present work is concerned with nuclear safety. Although the NEA have never been involved in X-ray diffraction before, they are willing to distribute any programs which are given to them. These programs would then be described in their newsletter. Brian Bellamy agreed to raise the matter with the BCA

Committee and to co-ordinate future action. The principal problem here is that most people are not in a position to give their programs away, now that they face much tighter budget controls, nor are they able to offer software support.

FINALLY

The main achievement of the meeting was to put people in touch with others working in the same field. The testing of lattice parameter programs was agreed and hopefully some will be sent to the NEA database for distribution. At this point the BCA does not have the funds to set up a central program library, however most people felt that the first steps towards greater co-operation had been made.

Judith Shackleton


WORKSHOP ON PRACTICAL X-RAY DIFFRACTION

A workshop on practical X-r ay diffraction was held on 7th April as part of the BCA Spring Meeting at Heriot-Watt University, Edinburgh.

SAMPLE PREPARATION

Frank Chung (Sherwin-Williams Research Centre, Chicago) led the discussion on this topic, beginning with a reminder that the most expensive equipment and painstaking measurement can be set at naught by poor sample preparation, as can the time and effort spent on interpreting data. He then summarised briefly and comprehensively the ways of detecting specim en orientation effects and the ideas which have been adopted to counter them. Several participants then added variants, alternative materials and practical hints of their own. The problem posed by small samples was also covered but it may become intractable if there is also preferred orientation.

Colin Dineen (GEC Hirst Research Centre) raised the difficulty of mounting silicon wafers for X-ray topography without straining them. Participants suggested various possibilities but it seems imp ossible to eliminate all strain at the supports.

PROGRAMS FOR LATTICE PARAMETER DETERMINATION

Eric Kelly (Electricity Council Research Centre) drew attention to differences in the output cell dimensions from different computer programs, arising from differences in computer precision and in the corrections (if any) which are applied. A round robin test of cell refinement programs is in progress [if interested please contact Eric Kelly].

DISTANCE LEARNING VIDEO COURSE

Paul Barnes (Birkbeck College) gave delegates a preview of the first of five video recordings intended for teaching with accompanying workbook and tutorials. The introductory programme deals with powder diffraction and included appearances by several members of the Industrial Group extolling the practical value and versatility of the technique. The next two programmes are to deal with "finger printing" identification and with quantitative powder diffraction. Possible topics for the final two prog rammes include indexing and Rietveld refinement, phase transformations end chemical reactions, and neutron and synchrotron powder diffraction. The series looks promising: it could do a lot to spread the word about crystallography.

Around eighty people, including many from other groups of the BCA, attended the workshop, which continued the lively and friendly participation of earlier Industrial Group Workshops.

Jim Chisholm

British Mus eum (Natural History)


Autumn Meeting, 12 November 1987

The Autumn meeting of the BCA Industrial Group was held on November 12th 1987 at the Rothamatead Experimental Station, Harpenden, Harts. Over seventy delegates attended this meeting representing a wide range of industrial, research establishments and academic institutions. Seven papers were presented illustrating a wide range of applications of X-ray diffraction (and in one paper of IR spectroscop y) to industrial problems.

Interestingly four papers originated from academic institutions, two from research establishments and one directly from industry. Illustrating, perhaps, the interest in industrial research within academic institutions.

The first paper by Dr. Ian Wood, on home territory at Rothamstead, gave an interesting review of crystallography at Rothamstead starting some 50 years ago. he described collaborative work with, for example, W.T. Astbury (plant cellulose), J.D. Bernal (viruses), W.H. Bragg (mineralogy of soils and clay) and the more recent work of G. Brown (clay minerals) and W.R. Truter (structure and activity). In addition to the oral presentation Ian, with his colleagues, presented an impressive display of posters. Sadly, we were told that the future of crystallography at Rothamstead is bleak and that this research is likely to cease early in 1988.

The second paper given by Dr. D.F. Barlow, Rugby Group PLC, was entitled 'Some Applications of X-Ray Diffraction in the Cement Industry'. This paper contained a brief review of the composition of the various cements and the problems associated with application of XRD to their analysis. Dr. Barlow gave an interesting account of the application of XRD to the determination of glass content in hydrated cement containing CCBS (ground granulated blast furnace slag) which is a replacement for cement. This method has been introduced in BS6699.

Paper three entitled 'Time-Resolved Powder St udies of Cement and Ceramic Reactions with Neutron and Laboratory X-Ray Sources' was a double act Elizabeth Polak and Gerda Mamott from the Industrial Materials Group, Crystallography Department, Birkbeck College. Elizabeth Polak described neutron diffraction experiments on the structural changes in autoclaved lightweight concrete caused by temperature and pressure changes. Gerda Mamott described modifications to an X-ray diffractometer which enables her to study the structural changes which occur o n calcination of zirconium hydroxide. These young ladies deserved the appreciation they received from the floor for the delightful way in which they presented their work.

Dr. Peter Knight from the AFRC Institute of Food Research, Bristol, presented the fourth paper entitled 'Studies of Water Retention in Meat by X·Ray Diffraction'. This was a superb presentation of a somewhat unusual application of X-ray diffraction. Dr. Knight discussed the nutritional value of the water content an d then described the construction of muscle and how muscle contraction of about 5% results in 10% loss of water. Some interesting results concerning post mortem shrinkage of beef muscle with time were discussed and shown in the form of lattice spacing vs time and intensity vs time curves.

The Autumn meeting usually contains a presentation on alternative methods and this time it was the turn of Dr. Monica Mendelssohn, Department of Geological Sciences, University College London, who impresse d with paper five and gave a very lucid account of 'Applications of FTIR Spectroscopy'. This involves the use of an FTIR spectrometer with an optical microscope attachment and she described the application of the technique to the characterisation of diamonds and to a number of solid state reactions involving for example anthrone (electron microscopy grid sample) and to single crystal IR spectra e.g. anthracene, dianthracene and urea.

Paper six was presented by Professor J. Heizmann, Univers ity of Metz, and was entitled 'Pole Figure Measurement and Analysis using a Curved Position Sensitive Detector'. Professor Heizmann's obvious enthusiasm for his work showed clearly in his presentation which concerned the considerable advantage in time, accuracy and reduction in blind area problems when using the 120° C curved X-ray P.S.D. compared with the conventional Schultz method to obtain simultaneously the XRD data across the Debye Scherrer ring. The advantages were ably demonstrated with applications to copper sheet and to single crystals of aluminium.

Finally, the seventh paper was presented by Dr. Ruth Fenn, Portsmouth Polytechnic, who described some work carried out during a short sabbatical at the materials Development Division, Harwell Laboratory. Ruth's paper with the title 'Measurements of Residual Stress in Carbon Fibre Composite Materials using X-Ray Diffraction' was most eloquently presented and completely eliminated the temptation to r elax before the long journey home - a clever move by the organisers. The work described involves the insertion of metal particles (e.g. Al, Ni) between the fibres in carbon fibre composites so that high angle reflections can be used to determine strain due to thermal residual stresses in the cured carbon fibre composites. The conversion of strain to stress is then carried out by a calibration procedure. Some of the results were unexpected in that they showed the presence of shear strain in addition to the compressive principal strains, this is in conflict with theory which predicts no shear strain in a unidirectional polymer - oh dear!

Thus concluded a very useful and enjoyable meeting. Congratulations to the contributors; the organisers and to our hosts.

Mike Boles
Plymouth Polytechnic


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