CN116593510A - Method for measuring residual austenite content in Cronidur30 high-nitrogen stainless steel - Google Patents
Method for measuring residual austenite content in Cronidur30 high-nitrogen stainless steel Download PDFInfo
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- CN116593510A CN116593510A CN202310513177.0A CN202310513177A CN116593510A CN 116593510 A CN116593510 A CN 116593510A CN 202310513177 A CN202310513177 A CN 202310513177A CN 116593510 A CN116593510 A CN 116593510A
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- 229910001566 austenite Inorganic materials 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 27
- 239000010935 stainless steel Substances 0.000 title claims abstract description 26
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 26
- 238000005498 polishing Methods 0.000 claims abstract description 34
- 238000005259 measurement Methods 0.000 claims abstract description 13
- 239000003792 electrolyte Substances 0.000 claims abstract description 9
- 229910000734 martensite Inorganic materials 0.000 claims abstract description 7
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims description 15
- 230000000717 retained effect Effects 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000007797 corrosion Effects 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 claims description 6
- 238000002441 X-ray diffraction Methods 0.000 claims description 4
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 description 10
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 229910001199 N alloy Inorganic materials 0.000 description 1
- XLZJWRNIMZGNFB-UHFFFAOYSA-N [Mo].[Cr].[N] Chemical compound [Mo].[Cr].[N] XLZJWRNIMZGNFB-UHFFFAOYSA-N 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
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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
- 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
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
-
- 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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- 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)
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Abstract
The invention provides a method for measuring the residual austenite content in Cronidur30 high-nitrogen stainless steel, which comprises the steps of firstly preparing a Cronidur30 high-nitrogen stainless steel bearing sample and a non-textured pure ferrite block sample, performing thermal mosaic on the cut sample to prepare a metallographic sample with the height of phi 30mm and the height of 10-30 mm, mechanically grinding the prepared metallographic sample by an automatic grinding and polishing machine, and polishing; taking out the embedded polished sample to be tested, and preparing for electrolytic polishing; carrying out electrolytic polishing on a sample to remove a surface deformation layer and a stress layer, preparing special electrolyte in advance, standing, selecting austenite diffraction peaks of 200, 220 and 311 and martensite diffraction peaks of 200 and 211, and obtaining a diffraction pattern of the standard sample; scanning the Cronidur30 sample to obtain a diffraction pattern of the sample to be detected; the obtained diffraction pattern is processed by adopting a five-peak six-value method, and an accurate measurement value of the residual austenite is obtained; and obtaining an accurate residual austenite measurement result by a five-peak six-value method.
Description
Technical Field
The invention relates to a method for measuring the content of retained austenite in Cronidur30 high-nitrogen stainless steel.
Background
At present, a plurality of high-end bearing materials are still first and second-generation bearing steel materials in China, wherein GCr15 bearing steel has poor high temperature resistance and corrosion resistance, 9Cr18 stainless bearing steel has poor high temperature resistance, and Cr4Mo4V high temperature bearing steel has poor corrosion resistance. The Cronidur30 material is a chromium-molybdenum-nitrogen alloy, and has excellent performances of high temperature resistance, corrosion resistance, high strength, high hardness and the like. The carbon content in the steel is reduced by nitrogen with a certain content, so that the formation of massive eutectic carbide is avoided. The Cronidur30 material is generally small in residual austenite content after deep cooling and quenching and tempering, and when the residual austenite content is increased, the phenomenon of unstable strength and service life of the material in the service process is caused, and even the failure of precision loss caused by the influence on the dimensional stability of the bearing due to martensite transformation caused by stress induction and high-temperature working conditions is caused. The priority of use as a new material in the future is higher, while the prior art is not high enough in accuracy for its retained austenite measurement.
The increase of the residual austenite content in the Cronidur30 high-nitrogen stainless steel bearing can cause unstable material strength and service life in the service process, and even the failure of precision loss caused by stress induction and martensite transformation under high-temperature working conditions, which affects the dimensional stability of the bearing. The invention can solve the problem that the prior art can not accurately measure the residual austenite content of the Cronidur30 high-nitrogen stainless steel bearing, and provides practical engineering application value.
Disclosure of Invention
Aiming at the defect that the prior art cannot accurately measure the residual austenite content of the Cronidur30 high-nitrogen stainless steel bearing, the invention provides a method for measuring the residual austenite content in the Cronidur30 high-nitrogen stainless steel. The invention improves the stability of XRD measurement peak value by preparing electrolyte solution with specific proportion and obtains the accurate residual austenite content by combining a five-peak and six-value method so as to overcome the defects in the prior art.
In order to achieve the above purpose, the invention provides a method for measuring the content of retained austenite in Cronidur30 high-nitrogen stainless steel, which comprises the following steps:
step one: preparing a Cronidur30 high-nitrogen stainless steel bearing sample and a non-textured pure ferrite block sample, cutting the samples to prepare a metallographic sample with the thickness of 20mm multiplied by 20mm, wherein the cutting thickness of the sample is 10-20 mm; performing thermal mosaic on the cut sample to prepare a metallographic sample with the height of phi 30mm and the height of 10-30 mm;
step two: mechanically grinding the prepared metallographic sample from 400, 600 and 1200 meshes of sand paper by an automatic grinding and polishing machine and polishing; taking out the embedded polished sample to be tested, and preparing for electrolytic polishing;
step three: carrying out electrolytic polishing on the sample to remove a surface deformation layer and a stress layer, preparing special electrolyte in advance, standing, carrying out electrolytic polishing for 18-20 s at a voltage of 20V, and obtaining a bright layer with a pollution-free surface, and carrying out ultrasonic washing on the sample after electrolytic polishing to remove fine stains so as to avoid influencing an X-ray diffraction scanning result;
step four: placing the treated Cronidur30 sample in the center of a specific plastic clamping groove, and fixing the back by using plasticine; selecting austenite diffraction peaks (200), (220) and (311), martensite diffraction peaks (200) and (211), selecting an X-ray diffractometer to adopt a Cu target, adopting a post-graphite monochromator to scan at a scanning range of 20-120 degrees and a scanning step rate of 0.02 degrees and a scanning speed of 1 degree/min, wherein the tube voltage is 30-35 kV;
step five: scanning the pure ferrite sample as a standard sample to obtain a diffraction pattern of the standard sample;
step six: scanning the Cronidur30 sample to obtain a diffraction pattern of the sample to be detected;
step seven: the obtained diffraction pattern is processed by adopting a five-peak six-value method, and an accurate measurement value of the residual austenite is obtained.
Further, in the first step, the cutting machine is a Struers Discotom-10 type manual-automatic cutting machine, and a linear cutting mode and the like can be adopted, and the inlaying machine is a struerscito press-1 type automatic inlaying machine.
Further, the automatic polishing machine in the second step is a Struers tegamin-25 type automatic polishing machine.
Further, in the third step, the electrolytic polishing machine is an electric 4 type electrolytic polishing corrosion machine.
Further, in the fifth step, the X-ray diffractometer is a Smartlab SE type X-ray diffractometer.
Further, in the third step, the electrolyte is prepared from potassium permanganate, absolute alcohol and water in a proportion of 7:2:1.
the beneficial effects of the invention are as follows: after the method is adopted, the surface stress layer and pollutants are removed, and a real tissue layer can be observed under a metallographic microscope. The actual residual austenite content of the Cronidur30 high-nitrogen stainless steel bearing sample is measured through XRD, misjudgment caused by sample preparation is avoided, and the surface stress of the Cronidur30 novel bearing material is removed through specially configured electrolyte compared with the traditional adaptive electrolyte, so that the surface quality of the sample is obviously improved, and the truest surface residual austenite distribution is obtained; the measuring method is convenient for the surface of an X-ray diffraction sample, can obviously improve the stability of diffraction peaks of XRD measurement, and can obtain the accurate residual austenite content of the Cronidur30 bearing; the method can perfect the conventional XRD method for measuring the residual austenite at present, and avoid the process research and judgment errors caused by inaccurate measurement of the residual austenite content of the Cronidur30 high-nitrogen stainless steel bearing. In conclusion, the method has the advantages of improving the surface quality of the Cronidur30 high-nitrogen stainless steel sample, improving the stability of XRD diffraction peaks and improving the accuracy of the residual austenite measurement result, and is suitable for other high-carbon chromium bearing materials. The sample preparation method can be used for saving more than 100 ten thousand yuan.
Drawings
FIG. 1 is a technical scheme of a residual austenite measurement method in an embodiment of the present invention;
FIG. 2 is a graph of xrd measurement results in an embodiment of the invention;
FIG. 3 is a graph showing the results of xrd treatment in the example of the present invention.
Detailed Description
Embodiments of the invention are further described below with reference to the accompanying drawings: as shown in fig. 1-3, the method for measuring the residual austenite content in the Cronidur30 high-nitrogen stainless steel is described with reference to fig. 1, and the implementation process is as follows:
step one: preparing a Cronidur30 high-nitrogen stainless steel bearing sample and a non-textured pure ferrite block sample, cutting the samples to prepare a metallographic sample with the thickness of 20mm multiplied by 20mm, wherein the cutting thickness of the sample is 10-20 mm. Performing thermal mosaic on the cut sample to prepare a metallographic sample with the height of phi 30mm and the height of 10-30 mm;
step two: and mechanically grinding and polishing the prepared metallographic sample from 400, 600 and 1200 meshes of sand paper by an automatic grinding and polishing machine. Taking out the embedded polished sample to be tested, and preparing for electrolytic polishing;
step three: carrying out electrolytic polishing on the sample to remove a surface deformation layer and a stress layer, preparing special electrolyte in advance, standing, carrying out electrolytic polishing for 18-20 s at a voltage of 20V, and obtaining a bright layer with a pollution-free surface, and carrying out ultrasonic washing on the sample after electrolytic polishing to remove fine stains so as to avoid influencing an X-ray diffraction scanning result;
step four: the treated Cronidur30 sample is placed in the center of a customized plastic clamping groove, and the back surface is fixed by using plasticine. Selecting austenite diffraction peaks (200), (220) and (311), martensite diffraction peaks (200) and (211), selecting an X-ray diffractometer to adopt a Cu target, adopting a post-graphite monochromator to scan at a scanning range of 20-120 degrees and a scanning step rate of 0.02 degrees and a scanning speed of 1 degree/min, wherein the tube voltage is 30-35 kV;
step five: scanning the pure ferrite sample as a standard sample to obtain a diffraction pattern of the standard sample;
step six: scanning the Cronidur30 sample to obtain a diffraction pattern of the sample to be detected;
step seven: the obtained diffraction pattern is processed by adopting a five-peak six-value method, and an accurate measurement value of the residual austenite is obtained.
In the first step, the cutting machine is a Struers Discotom-10 type manual-automatic integrated automatic cutting machine, and a line cutting mode and the like can be adopted, and the mosaic machine is a struerscito press-1 type automatic mosaic machine. The automatic polishing machine in the second step is a Struers tegamin-25 type automatic polishing machine. And in the third step, the electrolytic polishing machine is an Electromet 4 type electrolytic polishing corrosion machine. And in the fifth step, the X-ray diffractometer is a Smartlab SE type X-ray diffractometer. In the third step, the electrolyte is prepared from potassium permanganate, absolute alcohol and water in a proportion of 7:2:1.
raw data of diffraction patterns xrd measurement results are obtained according to the description of fig. 2; calculating diffraction integrated intensities from the five-peak diffraction profile as described in fig. 3; cronidur30 high nitrogen stainless steel xrd diffractometry results:
austenite diffraction peaks (200), (220) and (311), and martensite diffraction peaks are parameters of (200) and (211):
five-peak six-value method calculation result of Cronidur30 high-nitrogen stainless steel:
in conclusion, the method has the advantages of improving the surface quality of the Cronidur30 high-nitrogen stainless steel sample, improving the stability of XRD diffraction peaks and improving the accuracy of the residual austenite measurement result, and is suitable for other high-carbon chromium bearing materials.
The above embodiment is only one of the preferred embodiments of the present invention, and common changes and substitutions made by those skilled in the art within the scope of the technical solution of the present invention are included in the scope of the present invention.
Claims (6)
1. A method for measuring the residual austenite content in Cronidur30 high-nitrogen stainless steel is characterized by comprising the following steps: the method comprises the following steps:
step one: preparing a Cronidur30 high-nitrogen stainless steel bearing sample and a non-textured pure ferrite block sample, cutting the samples to prepare a metallographic sample with the thickness of 20mm multiplied by 20mm, wherein the cutting thickness of the sample is 10-20 mm; performing thermal mosaic on the cut sample to prepare a metallographic sample with the height of phi 30mm and the height of 10-30 mm;
step two: mechanically grinding the prepared metallographic sample from 400, 600 and 1200 meshes of sand paper by an automatic grinding and polishing machine and polishing; taking out the embedded polished sample to be tested, and preparing for electrolytic polishing;
step three: carrying out electrolytic polishing on the sample to remove a surface deformation layer and a stress layer, preparing special electrolyte in advance, standing, carrying out electrolytic polishing for 18-20 s at a voltage of 20V, and obtaining a bright layer with a pollution-free surface, and carrying out ultrasonic washing on the sample after electrolytic polishing to remove fine stains so as to avoid influencing an X-ray diffraction scanning result;
step four: placing the treated Cronidur30 sample in the center of a specific plastic clamping groove, and fixing the back by using plasticine; selecting 200, 220 and 311 austenite diffraction peaks, 200 and 211 martensite diffraction peaks, adopting a Cu target for an X-ray diffractometer, adopting a rear-mounted graphite monochromator for tube voltage of 30 kV-35 kV, and scanning at 20-120 DEG and 0.02 DEG of scanning step rate and 1 DEG/min;
step five: scanning the pure ferrite sample as a standard sample to obtain a diffraction pattern of the standard sample;
step six: scanning the Cronidur30 sample to obtain a diffraction pattern of the sample to be detected;
step seven: the obtained diffraction pattern is processed by adopting a five-peak six-value method, and an accurate measurement value of the residual austenite is obtained.
2. The method for measuring the retained austenite content in the Cronidur30 high-nitrogen stainless steel according to claim 1, characterized in that: in the first step, the cutting machine is a Struers Discotom-10 type manual and automatic integrated automatic cutting machine, and a Struers CitoPress-1 type automatic mosaic machine can also be adopted by adopting modes such as wire cutting and the like.
3. The method for measuring the retained austenite content in the Cronidur30 high-nitrogen stainless steel according to claim 1, characterized in that: the automatic polishing machine in the second step is a Struers tegamin-25 type automatic polishing machine.
4. The method for measuring the retained austenite content in the Cronidur30 high-nitrogen stainless steel according to claim 1, characterized in that: and in the third step, the electrolytic polishing machine is an Electromet 4 type electrolytic polishing corrosion machine.
5. The method for measuring the retained austenite content in the Cronidur30 high-nitrogen stainless steel according to claim 1, characterized in that: and in the fifth step, the X-ray diffractometer is a Smartlab SE type X-ray diffractometer.
6. The method for measuring the retained austenite content in the Cronidur30 high-nitrogen stainless steel according to claim 1, characterized in that: in the third step, the electrolyte is prepared from potassium permanganate, absolute alcohol and water in a proportion of 7:2:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310513177.0A CN116593510A (en) | 2023-05-05 | 2023-05-05 | Method for measuring residual austenite content in Cronidur30 high-nitrogen stainless steel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310513177.0A CN116593510A (en) | 2023-05-05 | 2023-05-05 | Method for measuring residual austenite content in Cronidur30 high-nitrogen stainless steel |
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- 2023-05-05 CN CN202310513177.0A patent/CN116593510A/en active Pending
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