JY/T 0587-2020 English PDF (JYT0587-2020)

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JY/T 0587-2020: General rules for X-ray polycrystalline diffractometry
JY/T 0587-2020
EDUCATION INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 03.180
Y 51
Replacing JY/T 009-1996
General rules for X-ray polycrystalline diffractometry
ISSUED ON: SEPTEMBER 29, 2020
IMPLEMENTED ON: DECEMBER 01, 2020
Issued by: Ministry of Education of PRC
Table of Contents
Foreword ... 4 
1 Scope ... 6 
2 Normative references ... 6 
3 Terms and definitions... 6 
4 Principles of analysis methods ... 11 
4.1 Qualitative analysis of phases ... 11 
4.2 Quantitative analysis of phase ... 12 
4.3 Determination of grain size and lattice distortion ... 13 
4.4 Determination of unit cell parameters of cubic crystals ... 15 
4.5 Solving the crystal structure from ab initio polycrystalline diffraction data ... 16 
4.6 High and low temperature diffraction ... 16 
5 Reagents and materials ... 17 
5.1 Standard material ... 17 
5.2 Organic solvents ... 17 
5.3 Sieves ... 17 
5.4 Sample preparation tools ... 17 
5.5 Microscope ... 17 
5.6 Specimen plate ... 17 
6 Instruments ... 18 
6.1 Composition of the instrument ... 18 
6.2 Verification or calibration ... 18 
7 Samples ... 19 
7.1 Pretreatment of samples ... 19 
7.2 Filling of the specimen plate ... 19 
7.3 Judge whether the specimen plate is available ... 20 
8 Analysis steps ... 20 
8.1 Startup and parameter setting of the instrument ... 20 
8.2 Steps of phase qualitative analysis ... 21 
8.3 Steps for phase quantitative analysis ... 23 
8.4 Determination of grain size and lattice distortion by linewidth method ... 24 
8.5 Procedure for determination of unit cell parameters of cubic crystals ... 25 
8.6 Analysis steps for solving crystal structure by ab initio polycrystalline diffraction data
... 26 
8.7 High temperature and low temperature polycrystalline diffraction ... 27 
8.8 Crystallinity analysis procedure ... 28 
8.9 Inspection after determination ... 29 
9 Results report ... 29 
9.1 Basic information ... 29 
9.2 Presentation of analysis results ... 29 
10 Safety precautions ... 30 
10.1 X-ray protection ... 30 
10.2 Water and electricity safety protection ... 30 
10.3 Safety protection for experiment personal ... 30 
Appendix A (Informative) PDF descriptions ... 32 
Appendix B (Informative) Various standard materials and standard data ... 36 
Appendix C (Informative) Calibration of diffraction peak positions (2θ) ... 40 
Appendix D (Informative) Crystallinity analysis method ... 44 
References ... 48 
General rules for X-ray polycrystalline diffractometry
1 Scope
This standard specifies the analysis method principles, reagents and materials,
instruments, samples, analysis steps, result reports, safety precautions, for using
polycrystalline X-ray diffractometers, to analyze the phase composition of various
polycrystalline materials.
This standard applies to conventional polycrystal X-ray diffractometers. X-ray
diffractometers, which are equipped with two-dimensional surface detectors, can refer
to this method.
2 Normative references
The following documents are essential for the application of this document. For dated
references, only the dated version applies to this document. For undated references, the
latest edition (including all amendments) applies to this document.
GB/T 13869-2008 General guide for safety of electric user
GB 18871-2002 Basic standards for protection against ionizing radiation and for the
safety of radiation sources
JY/T 009-1996 General rules for X-ray polycrystalline diffractometry
3 Terms and definitions
The terms and definitions, which are defined in JY/T 009-1996, as well as the following
terms and definitions, apply to this document.
3.1
X-ray
Electromagnetic waves, which have wavelengths from 10-3 nm to 10 nm.
Note: The X-ray wavelength, which is used for crystal diffraction, is 0.05 nm ~ 0.25 nm.
3.2
Crystal
A generalized crystal is a solid, which has a definite diffraction pattern. Its atoms,
molecules or ions are arranged in the space a highly ordered manner, according to
certain rules, including traditional periodic crystals and non-periodic crystals.
3.3
Polycrystal
A solid powder or bulk object, which is formed by agglomeration of many small
grains. It is also known as polycrystalline material.
3.4
Space lattice
In crystallography, the tool used to express the periodic arrangement of structural
units in a crystal, which is a collection of periodically repeating points in three-
dimensional space.
3.5
Unit cell
The smallest building unit, in which atoms, molecules or ions are regularly arranged,
in long-range order, in three-dimensional space. Its shape is a parallelepiped.
3.6
Unit cell parameters
Parameters to describe the parallelepiped unit cell, namely the lengths of the three
sides a, b, c, as well as the included angle α (the angle between the b-side and the c-
side), β (the angle between the a-side and the c-side), γ (the angle between the a-side
and the b-side).
3.7
Lattice distortion
Inhomogeneous strains, that exist inside the lattice.
[JY/T 009-1996, Definition 3.7]
3.8
Crystal system
the horizontal and vertical divergence of the incident rays, the eccentricity of the
specimen surface, the absorption of the specimen, the degree of collimation of the
instrument, the misalignment of the 1:2 transmission relationship between the θ axis
and the 2θ axis, the zero point error, etc. Most of these influencing factors will decrease
or disappear, when θ approaches 90°. Therefore, a number of diffraction lines in the
high θ range are selected, the corresponding α is obtained according to their θhkl and hkl,
make the α-θ diagram, use the least square method to fit these points AND extrapolate
to θ = 90°, where α shall be the smallest error and closest to the true value. The cos2θ is
often used to extrapolate the abscissa; other trigonometric functions of θ can also be
used, such as cos2θ/sinθ, cos2θ/θ or their combinations.
4.4.3 Recommended method
It is recommended to use the full spectrum fitting method, to obtain the unit cell
parameters.
Note: The content is quoted from references [19 ~ 24].
4.5 Solving the crystal structure from ab initio polycrystalline
diffraction data
For many materials, it is impossible to obtain complete small crystals, that can be used
to measure the bulk structure, by the single crystal method. The polycrystalline
diffraction spectrum loses the three-dimensional characteristics of single crystal
diffraction AND degenerates into a one-dimensional diffraction pattern. The essence of
solving the crystal structure from ab initio powder diffraction data, is to restore the one-
dimensional diffraction pattern to three-dimensional information; then use the ab initio
single crystal method, to solve the structure to obtain the crystal structure.
Note: The content is quoted from references [4, 24 ~ 25].
4.6 High and low temperature diffraction
Some materials often undergo phase change, when the temperature changes, so the high
and low temperature diffraction accessories of the diffractometer can be used to
dynamically test the change of the specimen diffraction pattern, which is caused by the
change of the specimen structure, during the process of heating, cooling or constant
temperature, thereby determining the process of phase transition and the result of phase
transition, meanwhile determining the phase transition temperature...