Autumn Meeting 9^th November 2006 at Pilkington Group Ltd, Lathom, Lancashire.

Impact of Crystallography in an Industrial Environment

Delegate joining instructions.

On-line Meeting Registration << click here. Fees: £30 (£15 concessions)
All non-members pay a £20 supplement which includes optional BCA membership for 2007.
REGISTRATION CLOSES ON FRIDAY 3rd NOVEMBER

Hotels, Transport and Maps a link to a dedicated page to help you find the venue or find somewhere to stay.

On the day of the meeting, a minibus will leave the nearest west coast main line railway station - Wigan North Western at 09:30am and return at the close of the meeting. Contact Mark Farnworth before Friday 20th October if you want to use this free service.

During the lunch break there will be an option to take a tour around the on-site Exhibition Centre which highlights the uses of glass and coated glass products in the Building and Automotive markets.

Programme Note: Abstracts are further down this page.

Download a printer friendly 28kbPDF version of the meeting programme.

10:30 - 12:30 Morning Session

10:00 Coffee & Registration

10:30 Welcome
Jeremy Cockcroft, Chair of the Industrial Group.

10:40 Introduction to Pilkington.
Mary Ormsby, Senior Manager, Head of Off Line Coatings and Science Support Group

11:00 High Throughput Screening: How to use Raman Spectroscopy and XRPD.
Gordon Barr, Department of Chemistry, University of Glasgow.

11:30 The Evolution Of FAFNIR, And The Application Of FENRIS To Crystallite Size And Strain Determinations In Pyrolytic Silicon Carbide.
Ian Ferguson, Retired (UKAEA).

12:00 Combinatorial CVD- X-ray powder diffraction mapping for the formation and quantification of new coatings on glass.
Prof Ivan P Parkin, Department of Chemistry, University College, London.

12:30 - 14:00 Lunch and tour of Pilkington Exhibition.

14:00 - 16:30 Afternoon Session

14:00 Applications of XRPD and X-ray Reflectometry in the glass industry
Mark Farnworth, Off Line Coatings and Science Support Group, Pilkington Group Ltd.

14:20 The role of XRPD at BP.
Andrew Hodge , BP Chemicals, Saltend, Hull

14:40 Dog Food ‘n Diffraction.
Richard Morris, Morris Analytical X-ray Ltd, Oldbury.

15:00 Characterisation of Advanced Semi-conductor Materials using HR XRD and how this compares with other techniques, such as TEM, PL, SIMS.
Chris Staddon, School of Physics & Astronomy, University of Nottingham.

15:20 Powder X-ray Diffraction for Process and Product Support in Shell Global Solutions.
Graham C. Smith, Shell Global Solutions UK.

15:40 Applications of X-ray Powder Diffraction (XRPD) at the Health and Safety Laboratory (HSL).
Peter Stacey HSL, Buxton.

16:00 Tea and Discussion

16:30 Close

Abstracts

High Throughput Screening: How to Use Raman Spectroscopy and XRPD Together.
Gordon Barr and Prof. Chris Gilmore, Department of Chemistry, University of Glasgow, Glasgow G12 8QQ.

High throughput screening experiments that search for salts, solvates and polymorphs traditionally use X-ray powder diffraction as the gold standard, but Raman spectroscopy is becoming increasingly important, and instruments to carry out both measurements simultaneously are now on the horizon. We have shown how cluster analysis and multivariate statistics can be used to classify data from XRPD sources [1]. In this presentation the method is extended to show how Raman spectroscopy data can be incorporated into the clustering. The method is non-trivial - merely averaging the results of the two data sources is shown not to work.

References
[1] ‘High Throughput Powder Diffraction: II Applications of Clustering Methods and Multivariate Data Analysis ’ G. Barr, W. Dong and C.J. Gilmore, J. Appl. Cryst. (2004), 37, 243-252.

The Evolution Of FAFNIR, And The Application Of FENRIS To Crystallite Size And Strain Determinations In Pyrolytic Silicon Carbide.
Ian F Ferguson, Retired (UKAEA).

The results of crystallite size and strain measurements on pyrolytic silicon carbide will be described. These results were obtained using the program FENRIS. The development of this program from FIDO will be described as well as its subsequent evolution into FAFNIR. The talk will contain various personal reminiscences from the prehistory of XRPD.

Combinatorial CVD- X-ray powder diffraction mapping for the formation and quantification of new coatings on glass
Prof Ivan P Parkin, Department of Chemistry, University College London.

This talk covers the recent work achieved at UCL at developing an area mapping strategy using X-ray powder diffraction for thin films on glass. The strategy involves using a microfocus x-ray set up so that a glass plate (8 cm x 20 cm) can be divided up into small 3x3 mm squares and the diffraction pattern measured of each square using a microfocus x-ray source. this enables an X-ray contour map of the surface to be built up. It also enables us to investigate strain, preferred orientation and phase change across a surface in a uniform and systematic way. a couple of commercially relevant coatings- self cleaning glass and electrochromic coatings will be presented as examples of the technique. In the self-cleaning glass case- the phase mapping enabled surface texturing and phase analysis of rutile/ anatase mixtures. this mapping technique provided a very useful guide to the functional properties of the coating.

Applications of XRPD and X-ray Reflectometry in the glass industry
Mark Farnworth, Off Line Coatings and Science Support Group, Pilkington Group Ltd.

Glass is not traditionally thought of as a good material for analysis by XRPD due to its amorphous nature. However, the glass making raw materials and the refractory materials that make up parts of the Float Glass Process are crystalline and their nature needs to be understood. The presentation will begin by showing how refractory materials are measured by XRPD, how the silica polymorphs quartz, tridymite and cristobalite are quantified and how the glassy phase contents are determined. Attention will then be turned to the XRPD analysis of thin coatings applied to the glass surface by Chemical Vapour Deposition (CVD) and Physical Vapour Deposition (PVD). Of particular interest is the measurement of crystallite size, strain and crystallographic texture within coatings and the presentation will cover how these various parameters are measured. The technique of X-ray Reflectometry (XRR) will also be discussed in which the layer thicknesses, densities and surface/interface roughnesses in multi-layer coatings stacks are measured.

The role of XRPD at BP.
Andrew Hodge , BP Chemicals, Saltend, Hull.

A brief background to BP will be given as context to the chronology of the PXRD capability in BP, and how it fits in with other analytical techniques. The D8-TXS (rotating anode) and Vantec detector are an incredibly fast combination useful for catalyst work, including insitu studies. Work typically includes detailed catalyst studies, mineral semiquantitative analysis of exploration cores, marine engine deposits, and various unknown solids. These require various degrees of crystallographic skill, but where the operator is inexperienced then it is very beneficial to have easy to use, reliable, current software (PDF4+, Topas, EVA).

Dog Food ‘n Diffraction.
Richard Morris, Morris Analytical X-ray Ltd.

This presentation will describe the use of X-ray powder diffraction in the development of a crystalline form of anhydrous trisodium pyrophosphate – Na₃P₂O₇ – as used in the industrial preparation of meat based pet-food products.

Characterisation of Advanced Semi-conductor Materials using HR XRD and how this compares with other techniques, such as TEM, PL, SIMS.
Chris Staddon, School of Physics & Astronomy, University of Nottingham, NG7 2RD.

As the demand for cheaper, faster, smaller, electronic devices increases there is a requirement for more precise control over device fabrication and hence a need for more sophisticated characterisation techniques to assess the quality of new materials for f uture device manufacture. In this talk several examples of advanced electronic materials grown at Nottingham University will be given, showing how HR XRD can provide detailed information about crystal quality and orientation as well as thickness, strain and composition. Data from complementary techniques such as Transmission Electron Microscopy (TEM), Photo Luminescence (PL) and Secondary Ion Mass Spectroscopy (SIMS) will be given as a comparison.

References
Determination of the Mn concentration in GaMnAs. LX Zhao, RP Campion, PF Fewster, et al. Semicond.Sci.Technol. 20 (2005) 369-373.
X-ray studies of As-doped GaN grown by plasma-assisted molecular beam Epitaxy.T.Li, CR Staddon, SV Novikov, PF Fewster, et al. Journal of Crystal Growth, 235 (2002) 103-110.
X-ray Scattering from Semiconductors (2nd edition) PF Fewster, World Scientific Press, Singapore, 2003.

Powder X-ray Diffraction for Process and Product Support in Shell Global Solutions.
Graham C. Smith, Shell Global Solutions UK,

The Analytical Technology group within Shell Global Solutions provides consultancy, analytical services and support to R&D for customers within and external to the Shell group. Powder X-ray diffraction is used widely in support of product quality, process R&D, product development and in the provision of data to enable rapid solution of production issues. A very wide range of sample types are analysed, covering suspended particulates in fuels, lubricants, industrial fluids and process streams through to solids and deposits on engine components and process plant. The talk will outline the facilities available and the sample preparation methods used. Examples will be taken from applied R&D, product development and rapid-response problem solving.

Applications of X-ray Powder Diffraction (XRPD) at the Health and Safety Laboratory (HSL)
Peter R Stacey, Health and Safety Laboratory, Harpur Hill, Buxton, SK17 9JN.

The talk will discuss the wide range of applications for XRPD in health and safety work with an emphasis on how XRPD is used within HSL to assess the risk of the exposure of workers to respirable crystalline silica, and to suppor the investigative work of the Health and Safety Executive. In addition, the talk will describe XRPD's increased use to characterise roofing materials from fatal accidents and give an example of some recent commercial work to quantify hydroxyapatite in sprayed coatings involving the application of internal s tandard and external standard and external standard relative intensity ratio (RIR) ASTM 2024-00 methods.