Neutron and X-Ray Scattering in Materials Science and Biology
Indonesia, July 23 – 31, 2007 /
PLM01
Application of X-ray and Neutron Scattering Techniques in Materials Research: Lithium Batteries and Electronic Ceramics
A. R. West1
1 University of Sheffield, Department of Engineering Materials, Sir Robert Hadfield Building, Mappin
Street, Sheffield, S1 3JD. UK
X-ray and neutron powder diffraction provide complementary information on the structures of inorganic complex oxides, primarily because of the different dependence of atomic scattering power, or scattering length, on atomic number. Neutron diffraction is particularly useful for characterising novel lithium transition metal oxides which have applications in prototype advanced lithium battery systems. Thus, it is possible to establish conduction pathways for mobile Li+ ions and to distinguish between transition metal ions in ordered spinel structures such as Li2NiMn3O8, which has a charge-discharge potential of 4.7V. An additional feature of such materials is oxygen non-stoichiometry in which their oxygen content depends on sample preparation conditions and temperature. This oxygen non-stoichiometry may be analysed by thermogravimetry and the transition metal oxidation states determined, in the solid state, by the X-ray absorption technique, XANES. Structural changes as a function of temperature may be followed by high temperature diffraction methods and as a function of lithium content during charging/discharging of lithium batteries by in situ synchrotron XRD. A range of examples of the applications of these techniques will be presented.
References
1. Inorganic functional materials: Optimization of properties by structural and compositional control, A R West, The Chemical Record, 6, 206-216 (2006).
2. Crystallography of Ni-doped Zn7Sb2O12 and phase equilibria in the system ZnO-Sb2O5-NiO, R Harrington, G C Miles and A R West, J Eur Ceram Soc, 26, 2307-2311 (2006).
3. Structural characterisation of REBaCo2O6-δ phases (RE-Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho), P S Anderson, C A Kirk, J Knudsen, I M Reaney and A R West, Solid State Sciences, 7, 1149-1156 (2003).
4. Temperature-dependent crystal structure of ferroelectric Ba2LaTi2Nb3O15, G C Miles, M C Stennett, I M Reaney and A R West, J Mater Chem, 15, 798-802 (2005).
5. Oxygen content and electrochemical activity of LiCoMnO4-δ, D Pasero, S de Souza, N Reeves and A R West, J Mat Chem, 15, 4435-4440 (2005).
Keywords: powder diffraction, synchrotron, lithium battery
Corresponding author:
PLM02
Early Years of Neutron Scattering and Its Manpower Development in Indonesia
Marsongkohadi1,2
1 Former Professor of Physics, ITB, Bandung, Indonesia
2 Director of Materials Science Research Centre, BATAN, Serpong, Indonesia from 1987 - 1996
In this paper I shall give a short history of development of neutron scattering at the Research Centre for Nuclear Technique (PPTN), in Bandung, and the early development of more advanced facilities at the Neutron Scattering Laboratory (NSL BATAN), Centre for Technology of Nuclear Industrial materials, in Serpong.
The first research reactor in Indonesia was the TRIGA MARK II in Bandung, which became operational in 1965, with a power of 250 KW, upgraded to 1 MW in 1971, and to 2 MW in 2000. The neutron scattering activities were started in 1967, with the design and construction of the first powder diffractometer, and put in operation in 1970. It was followed by the second instrument, the filter spectrometer built in 1975 in collaboration with the Bhabba Atomic Research Centre (BARC), India.
A powder diffractometer for magnetic studies was built in 1980, and finally, a modification of the filter detector spectrometer to measure texture was made in 1986. A brief description of the design and construction of the instruments, and a highlight of some activities at the 30 MW, RSG-GAS reactor in Serpong in choosing a suitable research program, which will be mainly centered around materials testing/characterization, and materials/condensed matter researches has been agreed. Instrument planning and lay-out which were appropriate to carry out the program had been decided. Manpower development for the neutron scattering laboratory is a severe problem. The efforts to overcome this problem have been solved. International Cooperation through workshops and on-the-job trainings also support the supply of qualified manpower.
Keywords: neutron scattering, powder diffractometer, magnetic studies.
Corresponding author:
PLM03
Opportunities for Materials Science and Biological Research at the OPAL Research Reactor
S. J. Kennedy1
1 Bragg Institute, ANSTO, Australia
Neutron scattering techniques have evolved over more than ½ century into a powerful set of tools for determination of atomic and molecular structures. Modern facilities offer the possibility to determine complex structures over length scales from ~0.1 nm to ~500 nm. They can also provide information on atomic and molecular dynamics, on magnetic interactions and on the location and behaviour of hydrogen in a variety of materials.
The OPAL Research Reactor is a 20 megawatt pool type reactor using low enriched uranium fuel, and cooled by water. OPAL is a multipurpose neutron factory with modern facilities for neutron beam research, radioisotope production and irradiation services. The neutron beam facility has been designed to compete with the best beam facilities in the world. After six years in construction, the reactor and neutron beam facilities are now being commissioned, and we will commence scientific experiments later this year.
The presentation will include an outline of the strengths of neutron scattering and a description of the OPAL research reactor, with particular emphasis on it’s scientific infrastructure. It will also provide an overview of the opportunities for research in materials science and biology that will be possible at OPAL, and mechanisms for accessing the facilities. The discussion will emphasize how researchers from around the world can utilize these exciting new facilities.
Keywords: neutron beam facilities, research reactor, atomic and molecular dynamics.
Corresponding author:
PLM04
J-PARC and Prospective Neutron Science
M. Arai1
1 J-PARC Centre, Japan Atomic Energy Agency, Tokai, Ibaraki, 319-1195, Japan
J-PARC is interdisciplinary facility with high power proton accelerator complex to be completed by 2008 after 7 years construction. Materials-Life Science Facility (MLF) will be very intensive pulsed neutron and muon facility at 1MW of the accelerated proton power. The neutron peak flux will be as high as several hundred times of existing high flux reactors. It is highly expected that new science will be opened up by using MLF. In the presentation I will explain the present status of J-PARC, strategy of user programme and prospective neutron science to be performed with it.
Keywords: proton accelerator, pulsed neutron, muon.
Corresponding author:
PLM05
Current Status and Future Works of Neutron Scattering Laboratory at BATAN in Serpong
A. Ikram1
1 Center of Technology for Nuclear Industrial Materials, National Nuclear Energy Agency of Indonesia
(BATAN)
Current status of neutron beam instruments using neutrons produced by the Multi Purpose Research Reactor – 30MWth (MPR 30, RSG GA Siwabessy) located in Serpong is presented. Description of the reactor as the neutron source is mentioned briefly. There are six neutron beam tubes coming from the beryllium reflector surrounding half of the reactor core providing neutrons in the experimental hall of the reactor (XHR). Four of them are dedicated to R&D in materials science using neutron scattering techniques. Neutron Radiography Facility (NRF), Triple Axis Spectrometer (TAS) and Residual Stress Measurement (RSM) Diffractometer are installed respectively at beam tubes S2, S4 and S6. The largest neutron beam tube (S5) is exploited to accommodate two neutron guide tubes that transfer the neutrons to a neighbouring building called neutron guide hall (NGH). There are three other neutron beam instruments installed at this building, namely Small Angle Neutron Scattering (SANS) Spectrometer (SMARTer), High Resolution SANS (HRSANS) Spectrometer and High Resolution Powder Diffractometer (HRPD). In the XHR, a Four Circle and Texture Diffractometer (FCD/TD) is attached to one of the neutron guide tubes. These seven instruments were installed to utilize the neutrons for materials and life sciences research, and recently the RSM diffractometer has shown its capabilities in identifying different amount of stress left due to different treatments of welding in fuel cladding, while the SANS spectrometer is now gaining capabilities in identifying different sizes and shapes of macromolecules in polymers, biomacromolecules as well as investigations of magnetic samples. In the mean time, non-destructive tests using the NRF is gathering more confidence from some latest real time measurements eventhough there are still some shortcomings in the components and their alignments. Future works including improvement of each facility and its components, even replacement of some parts are necessary and have to be carried out carefully. A plan for developing a neutron reflectometer at one of the neutron guide in the Neutron Guide Hall is also part of the near future activities.
Keywords: neutron beam instruments, fuel cladding, polymers, biomacromolecules
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PLM06
Magnetic Excitations in Transition-metal Oxides Studied by Inelastic Neutron Scattering
M. Braden1
1 Institute of Physics, University of Cologne, Germany
Inelastic neutron scattering using a triple axis spectrometer is a very efficient tool to analyze magnetic excitations. We will discuss several recent experiments on transition-metal oxides where orbital degrees of freedom play an important role. Different kinds of experimental techniques including longitudinal and spherical polarization analysis were used in order to determine not only magnon frequencies but also polarization vectors.
In layered ruthenates bands of different orbital character contribute to the magnetic excitations which are of both, ferromagnetic and antiferromagnetic, character. The orbital dependent magnetic excitations seem to play different roles in the superconducting pairing as well as in the metamagnetism .
In manganates the analysis of the magnon dispersion in the charge and orbital ordered phase yields direct insight into the microscopic coupling of orbital and magnetic degrees of freedom and helps understanding, how the switching between metallic and insulating phases in manganates may occur. In multiferroic TbMnO3 the combination of our polarized neutron scattering results with the infrared measurements identifies a soft collective excitation of hybridized magnon-phonon character.
Keywords: inelastic neutron scattering, magnetic excitations
Corresponding author:
PLM07
Pulsed Neutron Powder Diffraction for Materials Science
T. Kamiyama1,2
1 Materials and Life Science Facility, J-PARC Center, High Energy Accelerator Research Organization,
Tsukuba, Ibaraki 305-0801 JAPAN
The accelerator-based neutron diffraction began in the end of 60’s at Tohoku University which was succeeded by the four spallation neutron facilities with proton accelerators at the High Energy Accelerator Research Organization (Japan), Argonne National Laboratory and Los Alamos Laboratory (USA), and Rutherford Appleton Laboratory (UK). Since then, the next generation source has been pursued for 20 years, and 1MW-class spallation neutron sources will be appeared in about three years at the three parts of the world: Japan, UK and USA. The joint proton accelerator project (J-PARC), a collaborative project between KEK and JAEA, is one of them. The aim of the talk is to describe about J-PARC and the neutron diffractometers being installed at the materials and life science facility of J-PARC.
The materials and life science facility of J-PARC has 23 neutron beam ports and will start delivering the first neutron beam of 25 Hz from 2008 May. Until now, more than 20 proposals have been reviewed by the review committee, and accepted proposal groups have started to get fund. Those proposals include five polycrystalline diffractometers: a super high resolution powder diffractometer (SHRPD), a 0.2 %-resolution powder diffractometer of Ibaraki prefecture (IPD), an engineering diffractometers (Takumi), a high intensity S(Q) diffractometer (VSD), and a high-pressure dedicated diffractometer. SHRPD, Takumi and IPD are being designed and constructed by the joint team of KEK, JAEA and Ibaraki University, whose member are originally from the KEK powder group. These three instruments are expected to start in 2008. VSD is a super high intensity diffractometer with the highest resolution of Dd/d = 0.3%. VSD can measure rapid time-dependent phenomena of crystalline materials as well as glass, liquid and amorphous materials. The pair distribution function will be routinely obtained by the Fourier transiformation of S(Q) data. Q range of VSD will be as wide as 0.01Å-1 < Q < 100Å-1.
IPD is fully funded by Ibaraki prefecture for the promotion of new industries based on advanced science and technologies. It is for the first time in neutron facilities in Japan that a prefecture owns neutron instruments as well as neutron beam will be provided widely to industrial users. To make it successful, the user system is quite important because those users are expected to use IPD like chemical analyzers in their materials development process. Based on questionnaire data to several hundreds industries, IPD is designed as a versatile diffractometer including texture measurement, small angle scattering and total scattering as well as usual powder diffraction. IPD covers d range 0.15 < d (Å) < 4 with Dd/d = 0.15 %, and covers 4 < d (Å) < 60 with gradually changing resolution. Q range of IPD will be as wide as 0.01Å-1< Q < 50Å-1 to be utilized for varieties of structures: local structure, nano structure and crystal structure analyses. Typical measuring time for the typical ‘Rietveld-quality’ data is several minutes with the sample size of laboratory X-ray: 0.4 cc.
SHRPD is designed to be the world highest resolution with Dd/d = 0.03% without sacrificing intensity. The combination of the high quality data from HRPD and their high-precision analysis gives us information on tiny structural changes which have been overlooked. After careful examination with the moderator group five years ago, we have decided to develop a high-resolution & good S/N moderator to achieve the 0.03 % resolution within 100 m flight path. This development was almost successful up to now. Instrumental simulation and radiation analysis were almost completed. The d range 0.5 < d (Å) < 4 with Dd/d = 0.03 %, and covers 4 < d (Å) < 45 with gradually changing resolution.
Takumi is the first priority instrument in JAEA for stress mapping inside structure materials with the highest resolution of Dd/d = 0.2% (corresponding to 105 to 106 strain precision). The typical gauge volume will be 1 mm3. JED has transmission radiography detectors to support stress mapping.
Software group is planning so that basic software to cover data acquisition and data treatment should be common. Since 1 Gbyte data are typically obtained for single experiment in an instrument, the basic software is quite important. International TV conference between ISIS, IPNS, SNS has been held every month to exchange information on each development. KEK developed manyo-lib to help basic analysis. Analysis software development including powder diffraction is strongly related with the activity of the software group. However, users of IPD will be from various field of science and their background is different. It should cover wide topics and help both beginners and well-trained users. We have started with neutron intensity database, peak-search software, peak-match software, pattern simulation, whole pattern fitting, PDF and RDF analysis, and now start coding Rietveld software.