Preview

Fine Chemical Technologies

Advanced search

Use of a 4-circle goniometer for neutron and X-ray diffractometer in the study of single crystals

https://doi.org/10.32362/2410-6593-2021-16-4-363-371

Full Text:

Abstract

Objectives. This study described the 4-circle goniometer Syntex P1N and its possible applications in X-ray and neutron structure analysis of single crystals.
Methods. The 4-circle goniometer Syntex P1N, due to its high-precision mechanical characteristics and individual components from domestic equipment (sets of DRON type X-ray diffractometers), formed the basis for developing an instrument complex for X-ray and neutron-structure studies.
Results. The neutron diffractometer was upgraded based on the Syntex P1N goniometer. Therefore, the 10BF3-based end neutron counter, included in the diffractometer kit, was replaced by the 3He-based domestic side counter, SNM-16. Such a significant reduction in the linear dimensions of the detector allowed us to expand the range of measured angles of 2θ from 90° to 140° and increase the accuracy of the measured interplanar distances accordingly. The goniometer was adjusted relative to the primary neutron beam by placing it on a specially designed plate. Highly accurate measured parameters of the unit cell and the intensity of the reflexes were achieved by optimizing the installation geometry and the protection of the goniometer and detector. Based on the Syntex P1N goniometer, an instrument complex for X-ray diffraction studies has also been developed. Both the developed X-ray and the upgraded neutronography facilities were used to perform experiments to measure the unit cell parameters, the coordinates of atoms, and the parameters of their thermal vibrations on several crystals of domestic synthetic samples: diamond C, silicon Si, halite, or rock salt NaCl, and corundum α-Al2O3. An excellent correlation was achieved by comparing the data obtained with the corresponding chemical crystals’ parameters and reference samples recommended by the International Union of Crystallographers.
Conclusions. This paper described a neutron installation and a Syntex P1N neutron diffractometer for the study of single crystals. Based on the latter, an instrument complex for X-ray diffraction studies has also been developed. Experiments on standard samples have shown a high level of accuracy in measuring the lattice parameters, the coordinates of atoms, and the parameters of their thermal vibrations on both the X-ray and neutron diffractometers.

About the Author

V. A. Sarin
MIREA – Russian Technological University
Russian Federation

Viktor A. Sarin, Cand. Sci. (Phys.-Math.), Leading Engineer, Research Institute of Solid-State Electronics Materials

78, Vernadskogo pr., Moscow, 119454

Scopus Author ID 7005455400


Competing Interests:

The author declares no conflicts of interest.



References

1. Datt I.D. Ozerov R.P. Rannev N.V. High-resolution neutron diffraction device with variable wavelength. In: Apparatura i metody rentgenovskogo analiza = Equipment and methods of X-ray analysis. Leningrad: Mashinostroenie; 1973. V. 12. Р. 16–19 (in Russ.).

2. Prince E. (Ed.). International Tables for Crystallography. V. C: Mathematical, physical and chemical tables. Dordrecht: Springer; 2006. Р. 498–504. https://it.iucr.org/Cb/,https://doi.org/10.1107/97809553602060000103

3. Gorelik S.S., Rastorguev L.N., Skakov Yu.A. Rentgenograficheskii i elektronnoopticheskii analiz. Prilozheniya (X-ray and electron-optical analysis. Applications). Moscow: Metallurgiya; 1970. 107 p. (in Russ.).

4. Kodess B.N., Sarin V.A. A Neutron Diffractometer for Determining the Structural Characteristics of Single Crystals. Measurement Techniques. 2015;57(11):1299–1303. https://doi.org/10.1007/s11018-015-0624-3

5. Abrahams S.C., Bernstein J.L. Accuracy of an Automatic Diffractometer. Measurement of the Sodium Chloride Structure Factors. Acta Cryst. 1965;18(5):926–932. https://doi.org/10.1107/S0365110X65002244

6. Baur W.H. In search of the crystal structure of low quartz. Z. Kristallogr. 2009;224(12):580–592. http://dx.doi.org/10.1524/zkri.2009.1219

7. Le Page Y., Calvert L.D., Gabe E.J. Parameter variation in low-quartz between 94 and 298K. J. Phys. Chem. Solids. 1980;41(7):721–725. https://doi.org/10.1016/0022-3697(80)90078-5

8. Glinnemann J., King H.E. Jr., Schulz H., Hahn Th., La Placa S.J., Dacol F. Crystal structures of the low-temperature quartz-type phases of SiO2 and GeO2 at elevated pressure. Zeitsehrift fur Kristallographic. 1992;198(3–4):177–212. http://doi.org/10.1524/zkri.1992.198.3-4.177

9. Tsirelson V.G. Chemical bond and thermal motion of atoms in crystals. Itogi nauki i tekhniki. Ser. Kristallokhimiya. 1992;27;3–269 (in Russ.).


Supplementary files

1. The crystal structure of α-SiO2. Viewed along the “c” axis. The image is constructed according to the data of this study using the Diamond graphic program.
Subject
Type Исследовательские инструменты
View (126KB)    
Indexing metadata
  • This paper describes a neutron installation and a Syntex P1N neutron diffractometer for the study of single crystals. Based on the latter, an instrument complex for X-ray diffraction studies has also been developed.
  • Experiments on standard samples have shown a high level of accuracy in measuring the lattice parameters, the coordinates of atoms, and the parameters of their thermal vibrations on both X-ray and neutron diffractometers.

For citation:


Sarin V.A. Use of a 4-circle goniometer for neutron and X-ray diffractometer in the study of single crystals. Fine Chemical Technologies. 2021;16(4):363-371. https://doi.org/10.32362/2410-6593-2021-16-4-363-371

Views: 141


ISSN 2410-6593 (Print)
ISSN 2686-7575 (Online)