Industrial Group meetings in 2002

• BCA Spring Meeting 25-28 March 2002, University of Nottingham
  There is considerable overlap with the Groups at this meeting and it important that you review the full programme. This section is devoted entirely to content for which the Industrial Group is solely responsible
  
  
  • Industrial Group Posters
  • Workshop - Introduction to Thin Films 26^th March 2002
  • Workshop - Powder Diffraction Surgery 26^{th March 2002}
  • Workshop - Introduction to Amorphous Materials 26^th March 2002
  • Industrial Group AGM 28^th March 2002
• Industrial Group Autumn Meeting 7^th November 2002 - Manchester

BCA Spring Meeting 2002.

University of Nottingham, 25-28 March 2002

Industrial Group Posters

Posters are invited for display at the Spring Meeting. As an extra incentive to your participation, in addition to the acclaim that your poster will no doubt bring, the Industrial Group are offering a magnificent prize of £50 for best poster.

Some guidelines follow for what we would prefer to see in our posters and our adjudicators will work from these.

Posters are encouraged that:

• are relevant to industry (including some background and value of the work to industry)
• have clear aims, results and conclusions
• concentrate on telling the story, rather than fine detail
• are not an advertisement for a commercial product

There will be an opportunity to give a brief oral presentation of the content of each poster.

For more information, contact:

Secretary/Treasurer

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Workshop - Introduction to T hin Films

09:00 - 10:30 26^th March 2002

The tutorial is designed to give a basic introduction to the analysis of thin films. This method is often referred to as "Glancing Incidence X-Ray Analysis (GIXA)" or reflectometry. It is used to determine the thickness, roughness, density etc of layers, which are less than (about) a micron in thickness. Typical examples are layers deposited to form electronic devices and also optical coatings on glass.

Th e tutorial will be divided into three sessions. Firstly, Professor Paul Fewster, Philips Research, will introduce some of the physics behind reflectometry. Next, the practical aspects of aligning the sample, collecting and analysing the data will be discussed by Dr Christoph Schug (IBM SSD Mainz, Germany). Finally, we will describe some practical examples.

This workshop is designed for the beginner as well as those who have some experience of the technique. There will be time to ask questions and to discus any problems which you have encountered.

The Physical Crystallography Group have a session on "Thin Film Analysis" on Wednesday morning, when you will be able to test your new skills.

For further information, please contact
Judith Shackleton
Manchester Materials Science Centre
Tel: 0161 200 3581
E-mail: [email protected]

Workshop - Powder Diffraction Surgery

11:00 - 12:30 26^th March 2002

Panel Session chaired by J.K.Cockcroft

Following on from the highly successful workshop on sample preparation organised by Steve Norval at the BCA 2000 meeting at Heriot-Watt University, the Industrial Group of the BCA plans to hold a "Powder Diffraction Surgery", for which active audience participation is sought. So bring along all your old powder diffraction problems that have been tucked away for years in drawers and fire them at experts on the panel who will try to suggest some ideas for solving them! Subjects up for discussion will include theoretical concerns versus practical realities, software issues, do thermal ellipsoids mean anything?, best quantitative practice, and many more.

Organiser - Jeremy Cockcroft

Workshop - Introduction to Amorphous Materials

16:00 - 17:30 26^th March 2002

A Tutorial session in two parts.

Part 1 - J.M. Parker, University of Sheffield.

For many purposes the diffuse X-ray scattering produced by a glassy phase is regarded as a nuisance when trying to obtain diffraction data from crystalline phases. However it does contain useful information about the structure and quantity of glassy phase present, although there are no diffraction pattern datafiles available to aid this process. In this tutorial session methods of measuring and interpreting the scattering from the glassy phase will be discussed and a number of case studies of applications of these techniques presented. Finally the application of neutron diffraction will be shown to provide additional valuable information, complementing the results obtainable using X-rays.

Part 2 - G. R. Mitchell, University of Reading.

Many materials exhibit structures containing both crystalline and non-crystalline phases. A key characteristic of such semi-crystalline materials is the degree of crystallinity. We can easily dis tinguish between the scattering from the crystalline and amorphous regions of the sample by the sharpness of the diffraction peaks. In this tutorial session, quantitative methods of evaluating the crystalline and amorphous fractions of these samples from x-ray scattering data will be introduced and a number of examples which illustrate the methodology will be followed. The relationship between the level of crystallinity or fraction of amorphous material measured using x-ray scattering techniques and other physical techniques will be discussed.

For more information please contact the session organiser:
Dave Taylor
[email protected]
Tel: 01744 893108

Industrial Group AGM

The 18^th ANNUAL GENERAL MEETING of the Industrial Group will be held at the University of Nottingham on 28^th March 2002.

Nominations are sought for one committee member to serve for three years from March 2002.

No minations, which shall be proposed by not less than two members of the Group and shall be accompanied by the written consent of the nominee, shall be sent to reach the Honorary Secretary of the Group not later than seven days before the Annual General Meeting.

Contact the Secretary/Treasurer

Autumn Meeting

Programme Download a 12kb .rtf version of this meeting programme for pr inting
Getting to the venue: Hulme Hall directions or view University map No 17 is Hulme Hall

Thursday 7th November 2002 at Hulme Hall, Oxford Place, Manchester.

Crystallography in Industry

The theme of this year's Industrial Group Autumn Meeting is Sample Preparation.

Registration Form The registration fe e is £30, which includes lunch.

Programme:

10:00 Registration & Coffee

10:30 Welcome and Introduction
Judith Shackleton, Manchester Materials Science Centre

10:40 J'aime la boueI, I love Mud, Geological Samples(Abstract)
Martin Gill, Museum of Natural History

11:05 Over here with that Torque Wrench!(Abstract)
Richard Morris, Huntsman, O ldbury

11:30 You Expect Me To Analyse That! Sample Preparation Challenges From Gas-Turbine Materials(Abstract)
Colin Small, Rolls-Royce, Derby

12:00 Size Matters!
Some Practical Examples of Industrial XRD(Abstract)
Roz Shwartz LSM

12:30 Lunch

13:30 Presentation of an Industrial Group Award to Jo Jutson

13:40 BCA Industrial Group Award Lecture:< br> From Spinel Analysis to Micro X-ray Diffraction - A Personal View of Applications and Advances in XRD Techniques"(Abstract)
Jo Jutson

14:20 Residual Stress and Texture - Sample Requirements and Preparation(Abstract)
Phil Holdway, QinetiQ

15:45 Lattice Parameters and Sample Displacement for Common and Unusual Samples(Abstract)
Mary Vickers, Dept of Materials Science, Cambridge University.

15:10 Pharmaceutical Samples Using Capillaries (Open Discussion Session)
Chris Frampton, University of Southampton

15:35 Open Session for Discussion
Need some help? Bring along your Problems for Discussion

16:00 Close & Tea

For further information please contact:
Judith Shackleton

Manchester Materials Science Centre,
Grosvenor Street,
MANCHESTER,
M1 7HS.

Tel. 44 (0) 161 200 3584
Fax. 44 (0) 161 200 3584
Email: [email protected]

Autumn Meeting Abstracts Follow

Size Matters!!
Some Practical Examples of Industrial XRD

Rosalind Shwartz

Analytical Services, London & Scandinavian Metallurgical Co. Ltd Fullerton Road, Rotherham, South Yorkshire, S60 1DL.

Starting from a summary of the 'ideal' crystallite and particle size for quantitative XRD work, practical sample preparation is discussed in the context of a laboratory carrying out work for contract analysis customers. Examples of particle size distributions are given which were obtained from real samples of mixed phase composition using commonly available particle reduction equipment (swing mill, McCrone microniser). The materials discussed include monoclinic/cubic zirconia and samples contai ning free crystalline silica.

You Expect Me To Analyse That!
Sample Preparation Challenges From Gas-Turbine Materials

Colin Small

Rolls-Royce plc, P.O.Box 31, Derby, DE24 8BJ

One of the challenges of running a diffraction laboratory in a diverse organisation like Rolls-Royce is the range and type of samples that you are presented with. Samples turn up from not just all over the company but all over t he world. They can be large engineering components, rubbish swept of floors and even dead and decaying birds. They are usually sent in by engineers who have no idea of the questions that they are asking (much less the answer) and are invariably spectacularly unsuitable for mounting on your average diffractometer.

Try putting a Trent turbine disc on a Philips X'Pert system - you end up with a very flat diffractometer!

This presents the analyst with some real sample preparation chal lenges - how do you deal with things that are the wrong shape, size, dangerous to handle or just plain odd? This presentation will show you how some of these things are tackled in Rolls-Royce. Examples of large metallic objects, ingested powders and even the odd dead bird will be discussed and our solutions outlined.

Over Here With That Torque Wrench!
A Method of Sample Preparation for Quantitative X-ray Powder Diffraction Analysis.

Ri chard Morris

Huntsman Surface Sciences, Trinity Street, Oldbury, West Midlands, B69 4XB

Principle

Quantitative X-ray Powder Diffraction Analysis depends upon reproducible preparation of standard sample windows and that the degree of operator induced preferred orientation (e.g. any differences in operator strength) and other sample window characteristics are kept constant i.e. effectively eliminated on the front sample surface.

This m ethod of preparing sample windows involves a back-loading technique that incorporates a press and window holder, a backing material (as used in tablet manufacture) and a torque wrench. It also has the benefit of giving the sample windows good mechanical strength (nothing worse than having your lovingly prepared sample fall out of the window onto your freshly pressed designer jeans - well I suppose the sample dropping into the goniometer would be worse………..).

This method is primarily used at Huntsman Surface Sciences, Oldbury for the analysis of sodium triphosphate powders which are incorporated into some of our "built" heavy duty laundry liquids - solid detergent particles suspended by a structured surfactant system.

Sodium triphosphate consists of three main crystalline phases, two anhydrous phases and a hexahydrate.

It is important that the ratios of the three phase are accurately known as this effects the rate of dissolution and hence the per formance of the product in the consumers washing machine.

As a grand finale to this presentation I shall demonstrate this technique
(I hope I don't make a mess of my trousers!).

J'aime la Boue

Martin Gill

Museum of Natural History, Cromwell Road, LONDON, SW17 5BD

First a look at how I got started on the road to a career in 'soft rock'……..

Then we delve headlong int o ways to get clays into suspension that are in association with such compounds as oil. Off into the world of sample preparation, where everyone thinks their technique is best. Also, genteel references along the way to flocculation & layer charge.

Residual Stress and Texture - Sample Requirements and Preparation

Phil Holdway

QinetiQ, Structures and Materials Centre
Cody Technology Park
Farnborough, Hants GU1 4 0LX

Sample preparation for X-ray residual stress and texture measurements are often limited to cutting/sectioning and, for texture, metallographic polishing. In many cases, for residual stress measurements, no preparation is necessary and samples are measured in the 'as-received' condition.

Of equal importance for these techniques, are certain sample requirements, which will result in good quality raw data. These requirements, such as grain size, texture, and measurement location, will be briefly discussed and illustrated with a few examples from work carried out at QinetiQ.

Lattice Parameters and Sample Displacement for Common and Unusual Samples

Mary Vickers

Department of Materials Science and Metallurgy, University of Cambridge CB2 3QZ [email protected]

Reliable peak positions, and thus d-spacings, are required to provide accurate cell parameters. Cell parameters are us eful because they can provide information such as the chemical composition, crystalline density, strain and thermal expansion coefficient. The major systematic error in this type of work is usually sample displacement: genuine physical displacement and / or sample transparency. Ways of minimising this error by sample preparation and special sample holders will be discussed as well as and mathematical correction methods. The talk will be illustrated with examples from work on polymers, steel and a hi gh temperature conductor.

Polymer samples with their low absorption coefficient can have a large transparency error. Copolymers, or side-chains, are commonly added to reduce the melting point and alter mechanical properties. They usually reduce both crystallinity and crystalline density ¹ but inhomogenity in the placement of side-chains can alter well-established structure / property relationships and provide a grade with an improved balance of properties.

Steel sample s may have a large grain size which gives poor sampling and thus less reliable relative intensities. Sample rotation and a large illuminated specimen area can improve the sampling. A new steel microstructure with high strength has been produced ². It contains fine grained bainite (ferrite). Relationships have been established between the carbon content and cell parameters of both ferrite and austenite ³. Thus the experimentally determined cell parameters provide the carbon cont ent of both phases which are key values to confirm the transformation mechanism ⁴.

For YBa₂Cu₃O(_7- ) neutron diffraction has established that the c parameter of this orthorhombic structure increases with increasing ⁵. The critical temperature, Tc, and other desirable properties increase with increasing oxygen content and thus the c parameter provides on good check on the quality of the sputtered film. We found some unexpected informatio n about the cell parameters in a YBCO film on LaAlO₃ for potential application as a microwave device ⁶.

References

1. P R Howard and B Crist, J. Polym. Sci. Phys. (1989) 27 2269 R Popli and L Mandlekern, J. Polym. Sci. Phys. (1987) 25 441

2. F G Callallero, H K D H Badheshia, K J A Mavella, D G Jones and P Brown, Mat. Sci. Tech. (2002) 18 79

3. H K D H Badheshia, S A David, J M Vitek and R W Reed, Mat. Sci. Tech. (191) 7 686

4. C G arcia Mateo, F G Cabellero and H K D H Bhadeshia, International Conference on Martensitic Transformations (ICOMAT '02), Helsinki, Finland, 2002 (in press).

5. J D Jorgensen, B W Veal, A P Paulikas, L J Nowicki, G W Crabtree, H Claus, W K Kwok, Phys. Rev. (1990) 41 1863

From Spinel Analysis to Micro X-ray Diffraction - A Personal View of Applications and Advances in XRD Techniques

Jo Jutson

My first encounter with XRD was in 1965 while working at Berkeley Nuclear Laboratories. Powder diffraction analysis was carried out using a Debye-Sherrer Camera - first developed in 1916 and still in use. It had low resolution compared with modern diffractometers and all measurements were manual. The work involved analysing the oxides which formed on stainless steels which were candidates for use in the Advanced Gas Cooled Reactors (AGR) being built around that time. These oxides were generally of two phases: a rhombohedral phase (Fe_xCr_2-xO₃) and a Mn-Fe-Cr spinel phase (AB₂O₄). The spinel phase was be an important part of my later work.

After a gap of 20 years I returned to Berkeley Laboratories to carry out a PhD project which included the synthesis of spinels. XRD techniques had advanced and the instrument available was a Phillips PW 1130 diffractometer with chart recorder. This was a great improvement on the camera and there was soon yet another step forwa rd as the group I worked with obtained a Siemens D500 with all the associated software. This now included search and match programmes and programmes for determining d-spacings, peak intensity and lattice parameters.

The analysis of aqueous species of zirconium salts using SAXS techniques followed. By this time it was possible to have an area detector in the laboratory and when the Cu source was insufficient trips to Daresbury to use synchotron radiation were a regular occurrence.

On to 1991 and back to a Siemens D500 diffractometer. This time with profile fitting and particle size software; texture attachments and heating stage. These enabled the structural analysis of polymers destined for cable insulations as well as compositional analysis of cable components. Software became "windows" based and processing became quicker.

My final encounter with XRD was with the micro X-ray diffractometer. Here was a very intense narrow beam (50-500microns diameter), XYZ stage to locate any area on a sample, video camera to view the sample, area detector to speed up analysis time and all the latest software available. Now it was possible to analyse a sample area as small as 50-500 microns in 2 minutes. XRD techniques have advanced considerably since I first used a camera and I am sure will continue to do so.