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Experimental station
"Diffractometry in the "hard" X-ray range"

(beam line 4, person in charge A. Ancharov, phone 329-4145)

1. PURPOSE OF THE STATION

a) conduction of diffraction studies in the course of chemical reactions;
b) conduction of diffraction studies in the course of intense physical impact (high pressure and/or temperature).

2. GENERAL VIEW AND MAIN ELEMENTS OF THE STATION


Fig. 1. General view of the experimental station.


Fig. 2. Detection system mar345.

3. MAIN PARAMETERS

  • Source of radiation: VEPP-3 and the wiggler with a magnetic field of 2 T at an electron energy of 2 GeV
  • X-ray quantum energy: 33.7 keV (at a wavelength of 0.3685 A)
  • X-ray optics: one-crystal monochromator by the Laue scheme, Si 111, dE/E = 3*10-3, a flow of 1.8*108photon/sec/mm (H)
  • Output beam size: 0.1 x 0.1 mm to 0.8 x 3 mm
  • Time for creation of a diffraction pattern : 1 sec to several hours
  • Time for reading a diffractogram: less than 150 sec
  • Monitor: Luminophor + TV Camera
  • Detector: mar-345 by Marresearch, based on image plate (the main detector);
  • Detector mar-345 resolution: 100 or 150 microns (set by software); it is possible to register diffraction patterns with a diameter of up to 345 mm; the distance from the sample to the detector is 72 mm to 426 mm.
  • Objects of study: solids, liquids, and gas hydrates. The sample mass is 1 mg to several grams.

4. MAIN EQUIPMENT OF THE STATION

  • The detection system based on the memory screen mar345 by Marresearch. A sample can be mounted on the goniometric head and adjusted with the help of the built-in television camera.
  • High-pressure chambers (diamond anvils) manufactured by institutes of SB RAS, two chambers produced by D'Anvils and a chamber with diaphragm actuator by Easy Lab.
  • A spectrometer by Betsa for measurement of pressure generated by the diamond anvil cells.
  • The high-temperature open-type chamber for diffraction studies at temperatures as high as 1200 C.
  • Equipment for temperature measurement and control.

5. MEASUREMENT TECHNIQUES

What does the combination of the radiation, which is relatively "hard" for X-ray diffractometry, and a flat two-coordinate detector give? What are the advantages of this technique as compared with the conventional X-ray analysis methods? With decreasing wavelength of the applied X-rays, the diffraction angles diminish, and all diffraction peaks move toward smaller angles. Therefore, a flat two-coordinate detector allows registering the main set of diffraction peaks. The detector mar345, installed at 400 mm from the sample, allows obtaining diffraction data in the same range of interplanar distances as with a standard diffractometer that uses the characteristic radiation of copper at scanning in the 2theta angle range of 7° to 140°.

It is known that radiation diffracted from a sample propagates in the form of so-called diffraction cones. However, a conventional diffractometer records only a small fraction of the diffracted radiation in a solid angle, which defines the angular resolution of the diffractometer. For acquiring a complete set of diffraction data it is necessary to perform scanning over the required range of angles of diffraction. A flat two-coordinate detector registers all the radiation scattered by the sample. With a two-coordinate detector one can obtain information not only on the position and intensity of the diffraction rings but also on the intensity distribution over a ring. With a stationary sample, from the appearance of the diffraction rings one can judge the size and texture of crystallites. When a sample is rotated, reflexes from small crystallites coalesce into rings; if the sample contains crystallites with dimensions commensurate with the beam size or larger, then successively passing through the reflecting positions, the diffraction planes will give high-intensity diffraction reflections, which form a symmetrical pattern; i.e. a diffraction pattern of rotation of a single crystal will divide into individual reflections.

Since 2005, the following techniques have been developed for the research conducted at the station:

  • In situ diffractometry for the study of structural changes occurring in the course of chemical reactions, including those at high temperatures
  • X-ray diffraction studies at high pressures
  • X-ray diffraction studies of the structure of substances at low temperatures
  • X-ray diffraction studies of the structure of substances at a pressure-induced shift
  • Methods of measurement for determining the interplanar spacings in substances by the method of X-ray diffraction on SR with the use of a two-coordinate detector. Certified on 29.12.2006.
  • Methods of measurement of the thermal linear expansion coefficient of crystalline substances by the method of diffraction of synchrotron radiation with the use of a two-coordinate X-ray detector. Certified on 30.04.2008.

6. LIST OF RESEARCH WORKS (2005-2010)

RFBR

  • 08-03-00 636-a "Dynamic X-ray visualization of combustion of condensed systems with the use of synchrotron radiation";
  • 07-08-00 338-a "Thermoelectric and thermomagnetic properties of new phases and states of electronic materials at ultrahigh pressures";
  • 07-05-00 113-a "Study of the stages and mechanisms of structure formation during phase transformations in multicomponent media by the methods of in situ diffraction and spectroscopy and computer modeling";
  • 06-05-64 542-a "Crystal-structure aspects of pressure modification of microporous aluminosilicates of various topologies";
  • 06-03-32 797-a "Use of synchrotron radiation methods with a nano-milli-second resolution for the investigation of the structure of "fresh", "non-contact" nanoparticles formed under extreme conditions of detonation, combustion, and mechanical activation";
  • 06-02-17 277-a "Development of the instruments and methods of investigation of kidney stones with the in vivo use of SR";
  • 04-05-64 438-a "Interatomic interactions and self-structuring in the processes of genesis of complex oxide melts and crystal structures";
  • 04-02-16 903-a "SR-method study of short-lived excited states of matter under extreme conditions of high temperatures and pressure";
  • 04-02-16 178-a "Thermomagnetic effects at ultrahigh pressures in semiconductor systems".

SB RAS integration projects in 2006-2008

  • No 43 "Powder diffraction studies with the use of synchrotron radiation of phase transitions at high pressure ";
  • No 98 "Mechanocomposite precursors to creation of materials with new properties";
  • No 4.8 "Development of membrane catalysts and sensors based on oxygen-permeable perovskites for reactions of partial oxidation of methane and oxidative dehydrogenation of hydrocarbons C3-C5".

SB RAS projects in 2009-2011 executed jointly with other scientific institutions

  • No 138 "Creation of the fundamentals of the influence of activation on the regulation of interaction of solid metals and their compounds with metal melts with the purpose of creation of functional materials of a specified structure and properties".

Analytical departmental target program "Development of the Scientific Potential of Higher Education (2008-2010 )"
–Ќѕ.2.2.2.3. 16033 "Research on the new forms of molecular crystals forming at solid-phase transformations, including those under high pressure".

7. PARTICIPANT ORGANIZATIONS

  • Institute of Solid State Chemistry and Mechanochemistry SB RAS
  • Institute of Inorganic Chemistry.
  • Institute of Catalysis SB RAS
  • Institute of Geology and Mineralogy SB RAS
  • Institute of Metallurgy, UB RAS
  • Institute of Metal Physics, UB RAS
  • Physico-Technical Institute UB RAS

8. PARTICIPATION IN MAIN CONFERENCES AND EXHIBITIONS

  1. V National Conference on the Use of X-ray, Synchrotron Radiation, Neutrons and Electrons for studies of nanomaterials and nanonosystems (Continued All-Union Conf. on the Application of X-rays for materials research, RSNE NANO-2005, November 14-19, 2005, Moscow
  2. XVI International synchrotron radiation conference: SR Ц 2006, July 10-14, 2006
  3. VI National Conference on the Use of X-ray, Synchrotron Radiation, Neutrons and Electrons for studies of nanomaterials and nanonosystems. 11 Ц 17 November 2007. Ц M.: IC RAS
  4. XVII International synchrotron radiation conference SR Ц 2008, June 16-20, 2008, Novosibirsk, Russia, Budker inst. of nucl. physics SB RAS
  5. VII National Conference on the Use of X-ray, Synchrotron Radiation, Neutrons and Electrons for studies of nanomaterials and nanonosystems RSNE-NBIC 2009, Abstracts, 16-20 November 2009 Ц ћ.: IC RAS, 2009
  6. VII All-Russian Conference "Physical chemistry of ultrafine (nano-) systems." 2005, Moscow
  7. International interdisciplinary symposiums (8-12) "Phase transformations in solid solutions and alloys", 2005-2009. Loo-Rostov-on-Don
  8. International interdisciplinary symposiums (8-12) "Order, disorder, and properties of oxides", 2005-2009. Loo-Rostov-on-Don
  9. I and II International interdisciplinary symposiums "Melting-crystallization of metals and oxides" (MCMO), 2007-2009. Loo-Rostov-on-Don
  10. II All-Russian Conference on nanomaterials (NANO2009), Yekaterinburg, 20-24 April 2009
  11. III International Conference Fundamental Bases of Mechanochemical Technologies "FBMT2009", May 25 - 30, 2009, Novosibirsk, Russia
  12. the 40th International Annual Conference of ICT, 23-26 June, 2009, Karlsruhe, Germany
  13. the 46th EHPRG Conference on High Pressure Research, 7-11 Sept 2008, Valencia, Spain
  14. the 13th International conference on High Pressure Semiconductor Physics (HPSP-13), Fortaleza, Ceara, Brazil. July, 22-25
  15. V International Conference "Materials and coatings under extreme conditions", Yalta, Ukraine, 22-26 September 2008

10. LIST OF MAIN PUBLICATIONS

See a separate file.

 

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