CN112730488A - Calibration method for measuring residual austenite of steel grade by X-ray diffraction method - Google Patents
Calibration method for measuring residual austenite of steel grade by X-ray diffraction method Download PDFInfo
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- CN112730488A CN112730488A CN202110151899.7A CN202110151899A CN112730488A CN 112730488 A CN112730488 A CN 112730488A CN 202110151899 A CN202110151899 A CN 202110151899A CN 112730488 A CN112730488 A CN 112730488A
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- ray diffraction
- residual austenite
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- 238000000034 method Methods 0.000 title claims abstract description 40
- 229910001566 austenite Inorganic materials 0.000 title claims abstract description 39
- 238000002441 X-ray diffraction Methods 0.000 title claims abstract description 31
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 28
- 239000010959 steel Substances 0.000 title claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000005259 measurement Methods 0.000 claims abstract description 10
- 238000001514 detection method Methods 0.000 claims abstract description 4
- 238000004321 preservation Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 230000000717 retained effect Effects 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 239000011651 chromium Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 238000009659 non-destructive testing Methods 0.000 abstract description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/30—Accessories, mechanical or electrical features
- G01N2223/303—Accessories, mechanical or electrical features calibrating, standardising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/624—Specific applications or type of materials steel, castings
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Analysing Materials By The Use Of Radiation (AREA)
Abstract
A calibration method for measuring the residual austenite of a steel grade by an X-ray diffraction method relates to the technical field of bearing heat treatment nondestructive testing, and comprises the following specific steps: the method comprises the following steps: preparing a bearing steel 0# sample with zero residual austenite content; step two: obtaining a zero offset value A of the measuring equipment; detecting a prepared 0# sample with zero residual austenite content by using X-ray diffraction equipment, and taking an obtained detection value A as a zero offset value; step three: detecting a sample to be detected by using the same X-ray diffraction equipment, wherein the residual austenite content Y of the sample to be detected = actual measured value B-zero offset value A; the calibration method can correct the content of the residual austenite determined by the X-ray diffraction method, so that the measurement result is more accurate.
Description
Technical Field
The invention relates to the technical field of bearing heat treatment nondestructive testing, in particular to a calibration method for determining the residual austenite of a steel grade by an X-ray diffraction method.
Background
According to the X-ray diffraction principle, the cumulative intensity of X-ray diffraction lines of a certain phase is improved along with the increase of the relative content of the phase in a sample, the content of residual austenite in steel is calculated by measuring the cumulative intensity of the diffraction lines of the martensite phase and the austenite phase of bearing steel, but equipment and calculation deviation exists in the measuring process, and the deviation is generally between 1% and 2%; the precision bearing, the rolling mill bearing and the wind power bearing have low requirements on the content of the retained austenite in steel, generally the requirement is not more than 3%, accurate measurement results cannot be obtained under the deviation, and a calibration method is needed to correct the measurement results so as to accurately obtain the content of the retained austenite of the sample.
Disclosure of Invention
In order to overcome the defects in the background art, the invention discloses a calibration method for measuring the residual austenite of a steel grade by an X-ray diffraction method, which can correct the residual austenite content measured by the X-ray diffraction method and ensure that the measurement result is more accurate.
In order to achieve the purpose, the invention adopts the following technical scheme:
a calibration method for measuring the residual austenite of a steel grade by an X-ray diffraction method comprises the following specific steps:
the method comprises the following steps: preparing a bearing steel 0# sample with zero residual austenite content; carrying out spheroidizing annealing on a high-carbon chromium bearing steel GCr15 or GCr15SiMn sample, and firstly putting the sample into a heating furnace for heating, wherein the heating temperature is as follows: 790 +/-10 ℃ and heat preservation time: 6 h-7 h; then opening a furnace cover and quickly cooling to 620 +/-10 ℃; then heating to 720 +/-10 ℃ along with the furnace, and keeping the temperature for 2-3 h; finally, the furnace is cooled to 600 +/-10 ℃ and discharged.
Step two: obtaining a zero offset value A of the measuring equipment; and (3) detecting the prepared 0# sample with zero residual austenite content by using an X-ray diffraction device, and taking the obtained detection value A as a zero offset value.
Step three: and detecting the sample to be detected by using the same X-ray diffraction equipment, wherein the residual austenite content Y of the sample to be detected = actual measured value B-zero offset value A.
Further, in step three, the absolute value of the actual measurement value of the sample to be measured is less than 6%.
Further, when the absolute value of the actual measurement value of the sample to be measured is greater than or equal to 6%, replacing the X-ray diffraction equipment, and calibrating again.
Furthermore, the material of the sample to be detected is the same as that of the 0# sample.
Further, the holding time of the sample No. 0 in the heating stage in the step one is 6.5 h.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
the calibration method for determining the residual austenite of the steel grade by the X-ray diffraction method can more accurately detect the residual austenite content in the steel, solves the problem that the X-ray diffraction method cannot accurately obtain the residual austenite content of bearing parts with low requirements on the residual austenite content such as precision bearings, rolling mill bearings, wind power bearings and the like, is convenient to provide technical support for the optimization and adjustment of the heat treatment process, and meets the requirements of users.
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Detailed Description
The present invention will be explained in detail by the following examples, which are disclosed for the purpose of protecting all technical improvements within the scope of the present invention, and are not limited to the following examples:
the first embodiment is as follows:
a calibration method for measuring the residual austenite of a steel grade by an X-ray diffraction method comprises the following specific steps:
the method comprises the following steps: preparing a bearing steel 0# sample with zero residual austenite content; firstly, spheroidizing annealing is carried out on a GCr15 or GCr15SiMn sample of high-carbon chromium bearing steel, and the sample is put into a heating furnace for heating at the following temperature: 780 ℃, heat preservation time: 6 h; then opening a furnace cover and quickly cooling to 610 ℃; then heating to 710 ℃ along with the furnace, and keeping the temperature for 2 hours; finally, furnace cooling is carried out to 590 ℃ and discharging is carried out;
step two: obtaining a zero offset value A of the measuring equipment; detecting a prepared 0# sample with zero residual austenite content by using X-ray diffraction equipment, and taking an obtained detection value A as a zero offset value;
step three: detecting a sample to be detected by using the same X-ray diffraction equipment, wherein the sample to be detected needs to be the same as the selected 0# sample in material, and the residual austenite content Y of the sample to be detected = the actual measured value B-zero offset value A; in addition, in order to ensure more accurate calibration, in step three, the absolute value of the actual measurement value of the sample to be measured needs to be less than 6%, and generally, according to the deviation requirement, the austenite of the sample to be measured only has the significance of calibration if the austenite is less than 6%; according to the requirement, when the absolute value of the actual measurement value of the sample to be measured is greater than or equal to 6%, based on the uncertainty of the measurement deviation of the X-ray diffraction equipment, the proper X-ray diffraction equipment can be selected and replaced, and calibration is carried out again.
Example two:
the difference from the first embodiment is that the first step:
the method comprises the following steps: preparing a bearing steel 0# sample with zero residual austenite content; carrying out spheroidizing annealing on a high-carbon chromium bearing steel GCr15 or GCr15SiMn sample, and firstly putting the sample into a heating furnace for heating, wherein the heating temperature is as follows: 790 ℃, heat preservation time: 6.5 h; then opening a furnace cover and quickly cooling to 620 ℃; then the temperature is raised to 720 ℃ along with the furnace, and the heat preservation time is 2.5 h; finally, the furnace is cooled to 600 ℃ and taken out of the furnace.
Example three:
the difference from the first embodiment is that the first step:
the method comprises the following steps: preparing a bearing steel 0# sample with zero residual austenite content; carrying out spheroidizing annealing on a high-carbon chromium bearing steel GCr15 or GCr15SiMn sample, and firstly putting the sample into a heating furnace for heating, wherein the heating temperature is as follows: 800 ℃, heat preservation time: 7 h; then opening a furnace cover and quickly cooling to 630 ℃; then the temperature is raised to 730 ℃ along with the furnace, and the heat preservation time is 3 hours; finally, the furnace is cooled to 610 ℃ and taken out.
Residual austenite content% by X-ray diffraction method
The present invention is not described in detail in the prior art.
Claims (5)
1. A calibration method for measuring the residual austenite of a steel grade by an X-ray diffraction method is characterized by comprising the following steps: comprises the following steps:
the method comprises the following steps: preparing a bearing steel 0# sample with zero residual austenite content;
carrying out spheroidizing annealing on a high-carbon chromium bearing steel GCr15 or GCr15SiMn sample, and firstly putting the sample into a heating furnace for heating, wherein the heating temperature is as follows: 790 +/-10 ℃ and heat preservation time: 6 h-7 h; then opening a furnace cover and quickly cooling to 620 +/-10 ℃; then heating to 720 +/-10 ℃ along with the furnace, and keeping the temperature for 2-3 h; finally, the furnace is cooled to 600 +/-10 ℃ and discharged.
Step two: obtaining a zero offset value A of the measuring equipment; and (3) detecting the prepared 0# sample with zero residual austenite content by using an X-ray diffraction device, and taking the obtained detection value A as a zero offset value.
Step three: and detecting the sample to be detected by using the same X-ray diffraction equipment, wherein the residual austenite content Y of the sample to be detected = actual measured value B-zero offset value A.
2. The calibration method for measuring the retained austenite of the steel grade by the X-ray diffraction method according to claim 1, which is characterized in that: in step three, the absolute value of the actual measurement value of the sample to be tested is less than 6%.
3. The calibration method for measuring the retained austenite of the steel grade by the X-ray diffraction method as claimed in claim 2, which is characterized in that: and when the absolute value of the actual measured value of the sample to be measured is more than or equal to 6%, replacing the X-ray diffraction equipment, and calibrating again.
4. The calibration method for measuring the retained austenite of the steel grade by the X-ray diffraction method according to claim 1, which is characterized in that: the sample to be detected is required to be the same as the 0# sample in material.
5. The calibration method for measuring the retained austenite of the steel grade by the X-ray diffraction method according to claim 1, which is characterized in that: the holding time of the sample No. 0 in the heating stage in the step one is 6.5 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110151899.7A CN112730488B (en) | 2021-02-04 | 2021-02-04 | Calibration method for measuring residual austenite in steel by X-ray diffraction method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110151899.7A CN112730488B (en) | 2021-02-04 | 2021-02-04 | Calibration method for measuring residual austenite in steel by X-ray diffraction method |
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| Publication Number | Publication Date |
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| CN112730488A true CN112730488A (en) | 2021-04-30 |
| CN112730488B CN112730488B (en) | 2023-09-22 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS563623A (en) * | 1979-06-19 | 1981-01-14 | Kawasaki Steel Corp | On-line measuring method of austenite contained in rolled steel sheet |
| US5148458A (en) * | 1990-01-18 | 1992-09-15 | Clayton Ruud | Method and apparatus for simultaneous phase composition and residual stress measurement by x-ray diffraction |
| CN101446561A (en) * | 2008-10-17 | 2009-06-03 | 武汉钢铁(集团)公司 | Method for quantitatively measuring remaining austenite in steel by X-ray diffraction polar diagram data |
| CN102135506A (en) * | 2010-01-26 | 2011-07-27 | 宝山钢铁股份有限公司 | Method for detecting residual austenite in steel plate on line |
| CN103604821A (en) * | 2013-11-27 | 2014-02-26 | 南京钢铁股份有限公司 | Method for measuring austenite content of steel |
| JP2016194158A (en) * | 2015-04-01 | 2016-11-17 | 新日鐵住金株式会社 | Hot rolled steel sheet and manufacturing method therefor |
| CN106896124A (en) * | 2017-04-24 | 2017-06-27 | 上海应用技术大学 | The assay method of corresponding residual austenite content in a kind of bearing steel material heat treatment process |
-
2021
- 2021-02-04 CN CN202110151899.7A patent/CN112730488B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS563623A (en) * | 1979-06-19 | 1981-01-14 | Kawasaki Steel Corp | On-line measuring method of austenite contained in rolled steel sheet |
| US5148458A (en) * | 1990-01-18 | 1992-09-15 | Clayton Ruud | Method and apparatus for simultaneous phase composition and residual stress measurement by x-ray diffraction |
| CN101446561A (en) * | 2008-10-17 | 2009-06-03 | 武汉钢铁(集团)公司 | Method for quantitatively measuring remaining austenite in steel by X-ray diffraction polar diagram data |
| CN102135506A (en) * | 2010-01-26 | 2011-07-27 | 宝山钢铁股份有限公司 | Method for detecting residual austenite in steel plate on line |
| CN103604821A (en) * | 2013-11-27 | 2014-02-26 | 南京钢铁股份有限公司 | Method for measuring austenite content of steel |
| JP2016194158A (en) * | 2015-04-01 | 2016-11-17 | 新日鐵住金株式会社 | Hot rolled steel sheet and manufacturing method therefor |
| CN106896124A (en) * | 2017-04-24 | 2017-06-27 | 上海应用技术大学 | The assay method of corresponding residual austenite content in a kind of bearing steel material heat treatment process |
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Address after: 471039 No. 96, Jianxi, Luoyang District, Henan, Jianshe Road Patentee after: Luoyang Bearing Group Co.,Ltd. Country or region after: China Address before: 471039 No. 96, Jianxi, Luoyang District, Henan, Jianshe Road Patentee before: LUOYANG LYC BEARING Co.,Ltd. Country or region before: China |
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