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X-ray phase analysis method of metallic materials

A metal material and phase analysis technology, applied in the field of analysis, can solve the problems of not being able to effectively eliminate the influence of the texture, not being able to reflect, etc., and achieve the effect of improving accuracy and eliminating strength measurement errors

Inactive Publication Date: 2016-04-13
武汉钢铁有限公司
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  • Description
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  • Application Information

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Problems solved by technology

However, this cannot effectively eliminate the influence of texture, because the standard does not specify a special method to measure the X-ray diffraction intensity, and still uses the conventional, fixed sample X-ray diffraction intensity measurement on the powder diffractometer mode, while the conventional fixed sample method only obtains the intensity of grains at a certain angle {hkl} with the reference direction (such as the rolling direction or transverse direction of the rolled plate), which cannot reflect the actual diffraction intensity of the phase content to be measured. Introduce experimental error, even up to several times the error

Method used

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  • X-ray phase analysis method of metallic materials
  • X-ray phase analysis method of metallic materials
  • X-ray phase analysis method of metallic materials

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Grain-oriented silicon steel sheet whose ferrite content is known to be 98% is selected as the sample to be tested.

[0029] On the D / max2500PC rotating anode X-ray diffractometer, using MoK α Radiation, rotational intensity measurement at 45Kv / 200mA voltage / current. Place the circular sample on the reference plane of the rotating sample measurement accessory, then fix the accessory in the axial plane of the goniometer according to the conventional method, and finally perform the synchronization of the sample rotation strength measurement according to the conventional θ / 2θ linkage scanning method operation, in order to calculate the strength and axial density P of the selected {hkl} measured ferrite (hkl) , measured the I of several crystal planes i(hkl) and I j(hkl) .

[0030] Calculate the axial density P of the selected {hkl} using formula (1) (hkl) .

[0031] The diffraction intensity I after secondary texture correction i(200) (c) and I j(200) (c) Substitut...

Embodiment 2

[0039] Table 3 is the austenitic stainless steel 9 measured by this method # Determination results of austenite and ferrite in the sample. It can be seen that the sum of the two phases of the result of this method is (76+27)%=103%, and the absolute error of each phase is no more than 0.03. This shows that the method is accurate. This is because this scheme adopts the first-level texture correction and the second-level texture correction, which effectively eliminates the large grain and texture effects in the X-ray diffraction intensity measurement of metal materials, thereby significantly improving the quantitative phase analysis of metal materials. accuracy.

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Abstract

The invention relates to an X-ray phase analysis method for a metal material. The method comprises the following steps: respectively carrying out rotary measurement of diffracted intensity on a sample and a guide sample of the same ingredient, carrying out rotary or non-rotary measurement of the diffracted intensity on an untextured guide sample, so as to obtain an Ii(hkl) value, Ij(hkl) value and an Ir(hkl) value; carrying out texture correction on the diffracted intensity, respectively computing the axial densities Pi(hkl) and Pj(hkl) of the sample and the guide sample {hkl} of the same ingredient; further respectively computing the diffracted intensities Ii(hkl) (c) and Ij(hkl) (c) of crystalline grains of the sample and the guide sample of the same ingredient after texture correction; and inserting the Ii(hkl) (c) and the Ij(hkl) (c) into a formula Xi=Ii(hkl) (c) / Ij(hkl) (c) Xj, so as to compute the phase content of the sample. The fixed measurement mode of the diffracted intensities is changed into a rotary measurement mode, the diffracted intensities are subjected to texture correction, and the intensity measurement error caused by large crystalline grains is effectively removed. Thus, the X-ray phase analysis accuracy is greatly improved.

Description

technical field [0001] The invention relates to an analysis method, in particular to a metal material X-ray phase analysis method. Background technique [0002] X-ray phase analysis is an important means of modern metal material research and failure analysis and other disciplines. In order to meet the needs of quantitative phase analysis of various samples, many X-ray quantitative phase analysis methods have been developed, and the success or failure of phase analysis depends on the precision and accuracy of X-ray diffraction intensity measurement. The precision and accuracy of these methods Accuracy. [0003] There are many factors that affect the precision and accuracy of X-ray diffraction intensity measurement, and the large grain effect is one of the main sources of error in X-ray intensity measurement. Because when the crystal grains are coarse or the texture is strong, the diffraction circle is composed of discontinuous or uneven spots, which is not a big error in th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N23/20
Inventor 李长一黎世德姚中海周顺兵
Owner 武汉钢铁有限公司