YB/T 5320-2006 PDF English
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Metal materials - Quantitative phase analysis - Value K method of X-ray diffraction
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YB/T 5320-2006: Metal materials - Quantitative phase analysis - Value K method of X-ray diffraction
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/YBT5320-2006
YB
FERROUS METALLURGY INDUSTRY STANDARD
(Adjusted from GB/T 5225-1985)
Metal materials - Quantitative phase analysis - "Value
K" method of X-ray diffraction
Issued on. JULY 27, 2006
Implemented on. OCTOBER 11, 2006
Issued by. National Development and Reform Commission of PRC
Table of Contents
1 Principles... 3
2 Requirements and preparation of specimens... 4
3 Test instruments and test conditions... 6
4 Test procedure and result calculation... 7
Appendix A (Supplementary)... 9
Appendix B (Supplementary)... 12
Additional information... 14
Metal materials - Quantitative phase analysis - "Value
K" method of X-ray diffraction
This standard applies to the measurement of phase content in polycrystalline
powders of metallic materials. It can also be used as a reference for quantitative
phase analysis of polycrystalline powder specimens of other materials.
1 Principles
The X-ray diffraction pattern of a phase is a characterization of the crystal
structure of the phase.
When using the K value method to perform X-ray diffraction quantitative
analysis on a multiphase specimen, the cumulative intensity of a phase’s
diffraction line AND the content of the phase in the specimen have the
relationship of formulas (1) and (2) (see Appendix A for derivation).
Where.
Xa - The weight content of the α phase in the powder to be tested;
- The constant of proportionality. For the same radiation, the constant is
related to the αphase to be tested AND the reference substance;
Ia(hikili) - The cumulative intensity of diffraction lines of α phase on the (hikili)
crystal plane, after adding the reference substance to the powder to be
tested;
Ir(hjkjlj) - The cumulative intensity of diffraction lines of the reference material
on the crystal plane (hjkjlj), after adding the reference substance to the
powder to be tested;
(hikili) - The cumulative intensity of diffraction lines of the α phase on the
crystal plane (hikili), in the reference specimen;
(hjkjlj) - The cumulative intensity of diffraction lines of the reference material
from the crystal plane (hjkjlj), in the reference specimen;
Wr - The weight of the reference substance, after adding the powder to be
tested into the reference substance;
Wo - The weight of the powder to be tested, when adding the powder to be
tested into the reference substance;
- The weight of the reference substance, in the reference specimen;
- The weight of the powder to be tested, in the reference specimen.
The characteristic of this method is to calculate the first AND finally
determine the Xa.
Note. The reference specimen refers to the specimen, which is prepared when the
value is calculated.
2 Requirements and preparation of specimens
2.1 Sampling
2.1.1 Weighing
When weighing the sample, the relative deviation of the weight shall not exceed
0.1%.
2.1.2 Reference materials and reference specimens
2.1.2.1 Selection of reference materials
The principles for selecting reference materials are.
2.1.2.2 The linear absorption coefficient and particle radius of the reference
material and the phase to be measured shall satisfy the formula (3).
2.1.2.3 When calculating the value, the recommended ratio of the
reference specimen, which is formed by mixing the pure reference material and
the pure phase to be measured, is as follows.
When the cumulative intensity of the measured diffraction lines of the reference
material and the phase to be measured differ greatly, it shall change the ratio,
to increase the cumulative intensity of the weak diffraction lines.
2.1.4 Mixing of sample
Use an agate mortar to grind the powders, which are prepared in 2.1.2.3 and
2.1.2.4, for 30 ~ 40 minutes; mix well.
2.2 Preparation of specimens
2.2.1 Size and thickness of reference specimen and mixed specimen
In any selected diffraction position, the X-ray's irradiation area shall not exceed
the surface area of the specimen.
The thickness of the specimen shall satisfy formula (4).
2.2.2 Sample preparation
2.2.2.1 Use a commonly used specimen frame. Place a piece of about No.300
metallographic sandpaper, which is larger than the frame, under the frame
(corresponding rough ground glass can also be used).
2.2.2.2 Pour the ground mixed powder into the specimen frame. Compact
vertically to shape it.
2.2.2.3 Turn the pressed specimen over at an angle of 180°. Remove the
sandpaper. Use the surface of the specimen, which is in contact with the
sandpaper (or ground glass), as the test surface.
3 Test instruments and test conditions
3.1 Diffractometer
The overall stability of the diffractometer1 is better than 1%.
3.2 Test conditions
3.3 Requirements for diffraction peak shape
The peak height shall be 4 times larger than the fluctuation range of the
background;
The peak height should be about 4 times the half-height width.
4 Test procedure and result calculation
Before the quantitative determination, the intensity of the diffraction lines of the
reference specimen and the mixed specimen shall first be calibrated with the
JCPDS standard card, to check whether the reference material and the phase
to be measured have a preferred orientation.
4.1 Determination of value of reference specimen
4.1.1 To calculate the pure phase to be measured of the value, it shall first
carry out qualitative analysis of the X-ray diffraction line, to check the purity;
there shall be no impurity diffraction lines.
4.1.2 For the pure reference material selected according to 2.1.2, it shall check
its purity according to 4.1.1.
4.1.7 Calculate value according to formula (2).
4.2 Determination of the content of the phase to be measured
4.2.1 According to 2.1.2.4, add a reference substance to the powder to be
tested. Prepare the sample according to 2.2.2, so that the selected diffraction
lines of the measured phase conform to 3.3.
4.2.2 According to 4.1.6, record the cumulative intensity of each corresponding
diffraction line.
4.3 If the above requirements are met, the relative deviation of Xa is ≤ 5%.
Appendix A
(Supplementary)
A.1 Derivation of formula (1) in this standard
The cumulative intensity of powder diffraction lines can be expressed as.
Appendix B
(Supplementary)
B.1 If the preferred orientation is not serious, the following formula can be used
to correct the cumulative intensity of the diffraction line.
YB/T 5320-2006
YB
FERROUS METALLURGY INDUSTRY STANDARD
(Adjusted from GB/T 5225-1985)
Metal materials - Quantitative phase analysis - "Value
K" method of X-ray diffraction
Issued on. JULY 27, 2006
Implemented on. OCTOBER 11, 2006
Issued by. National Development and Reform Commission of PRC
Table of Contents
1 Principles... 3
2 Requirements and preparation of specimens... 4
3 Test instruments and test conditions... 6
4 Test procedure and result calculation... 7
Appendix A (Supplementary)... 9
Appendix B (Supplementary)... 12
Additional information... 14
Metal materials - Quantitative phase analysis - "Value
K" method of X-ray diffraction
This standard applies to the measurement of phase content in polycrystalline
powders of metallic materials. It can also be used as a reference for quantitative
phase analysis of polycrystalline powder specimens of other materials.
1 Principles
The X-ray diffraction pattern of a phase is a characterization of the crystal
structure of the phase.
When using the K value method to perform X-ray diffraction quantitative
analysis on a multiphase specimen, the cumulative intensity of a phase’s
diffraction line AND the content of the phase in the specimen have the
relationship of formulas (1) and (2) (see Appendix A for derivation).
Where.
Xa - The weight content of the α phase in the powder to be tested;
- The constant of proportionality. For the same radiation, the constant is
related to the αphase to be tested AND the reference substance;
Ia(hikili) - The cumulative intensity of diffraction lines of α phase on the (hikili)
crystal plane, after adding the reference substance to the powder to be
tested;
Ir(hjkjlj) - The cumulative intensity of diffraction lines of the reference material
on the crystal plane (hjkjlj), after adding the reference substance to the
powder to be tested;
(hikili) - The cumulative intensity of diffraction lines of the α phase on the
crystal plane (hikili), in the reference specimen;
(hjkjlj) - The cumulative intensity of diffraction lines of the reference material
from the crystal plane (hjkjlj), in the reference specimen;
Wr - The weight of the reference substance, after adding the powder to be
tested into the reference substance;
Wo - The weight of the powder to be tested, when adding the powder to be
tested into the reference substance;
- The weight of the reference substance, in the reference specimen;
- The weight of the powder to be tested, in the reference specimen.
The characteristic of this method is to calculate the first AND finally
determine the Xa.
Note. The reference specimen refers to the specimen, which is prepared when the
value is calculated.
2 Requirements and preparation of specimens
2.1 Sampling
2.1.1 Weighing
When weighing the sample, the relative deviation of the weight shall not exceed
0.1%.
2.1.2 Reference materials and reference specimens
2.1.2.1 Selection of reference materials
The principles for selecting reference materials are.
2.1.2.2 The linear absorption coefficient and particle radius of the reference
material and the phase to be measured shall satisfy the formula (3).
2.1.2.3 When calculating the value, the recommended ratio of the
reference specimen, which is formed by mixing the pure reference material and
the pure phase to be measured, is as follows.
When the cumulative intensity of the measured diffraction lines of the reference
material and the phase to be measured differ greatly, it shall change the ratio,
to increase the cumulative intensity of the weak diffraction lines.
2.1.4 Mixing of sample
Use an agate mortar to grind the powders, which are prepared in 2.1.2.3 and
2.1.2.4, for 30 ~ 40 minutes; mix well.
2.2 Preparation of specimens
2.2.1 Size and thickness of reference specimen and mixed specimen
In any selected diffraction position, the X-ray's irradiation area shall not exceed
the surface area of the specimen.
The thickness of the specimen shall satisfy formula (4).
2.2.2 Sample preparation
2.2.2.1 Use a commonly used specimen frame. Place a piece of about No.300
metallographic sandpaper, which is larger than the frame, under the frame
(corresponding rough ground glass can also be used).
2.2.2.2 Pour the ground mixed powder into the specimen frame. Compact
vertically to shape it.
2.2.2.3 Turn the pressed specimen over at an angle of 180°. Remove the
sandpaper. Use the surface of the specimen, which is in contact with the
sandpaper (or ground glass), as the test surface.
3 Test instruments and test conditions
3.1 Diffractometer
The overall stability of the diffractometer1 is better than 1%.
3.2 Test conditions
3.3 Requirements for diffraction peak shape
The peak height shall be 4 times larger than the fluctuation range of the
background;
The peak height should be about 4 times the half-height width.
4 Test procedure and result calculation
Before the quantitative determination, the intensity of the diffraction lines of the
reference specimen and the mixed specimen shall first be calibrated with the
JCPDS standard card, to check whether the reference material and the phase
to be measured have a preferred orientation.
4.1 Determination of value of reference specimen
4.1.1 To calculate the pure phase to be measured of the value, it shall first
carry out qualitative analysis of the X-ray diffraction line, to check the purity;
there shall be no impurity diffraction lines.
4.1.2 For the pure reference material selected according to 2.1.2, it shall check
its purity according to 4.1.1.
4.1.7 Calculate value according to formula (2).
4.2 Determination of the content of the phase to be measured
4.2.1 According to 2.1.2.4, add a reference substance to the powder to be
tested. Prepare the sample according to 2.2.2, so that the selected diffraction
lines of the measured phase conform to 3.3.
4.2.2 According to 4.1.6, record the cumulative intensity of each corresponding
diffraction line.
4.3 If the above requirements are met, the relative deviation of Xa is ≤ 5%.
Appendix A
(Supplementary)
A.1 Derivation of formula (1) in this standard
The cumulative intensity of powder diffraction lines can be expressed as.
Appendix B
(Supplementary)
B.1 If the preferred orientation is not serious, the following formula can be used
to correct the cumulative intensity of the diffraction line.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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