CN116593510A - Measurement method of retained austenite content in Cronidur30 high nitrogen stainless steel - Google Patents
Measurement method of retained austenite content in Cronidur30 high nitrogen stainless steel Download PDFInfo
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- 229910001566 austenite Inorganic materials 0.000 title claims abstract description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 26
- 239000010935 stainless steel Substances 0.000 title claims abstract description 25
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 25
- 230000000717 retained effect Effects 0.000 title claims description 13
- 238000000691 measurement method Methods 0.000 title description 4
- 238000005498 polishing Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000005259 measurement Methods 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 229910000734 martensite Inorganic materials 0.000 claims abstract description 7
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 7
- 239000003792 electrolyte Substances 0.000 claims abstract description 4
- 238000005520 cutting process Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 238000002441 X-ray diffraction Methods 0.000 claims description 4
- 230000007797 corrosion Effects 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 claims description 4
- 239000008151 electrolyte solution Substances 0.000 claims description 4
- 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
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 description 11
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000002360 preparation method Methods 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
- 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
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 231100000719 pollutant Toxicity 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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Abstract
Description
技术领域technical field
本发明涉及一种Cronidur30高氮不锈钢中残余奥氏体含量测量方法。The invention relates to a method for measuring residual austenite content in Cronidur30 high-nitrogen stainless steel.
背景技术Background technique
目前高端轴承材料中，我国使用较多仍是第一、二代轴承钢材料，其中GCr15类轴承钢耐高温和耐腐蚀差，9Cr18类不锈轴承钢耐高温性能较差，Cr4Mo4V类高温轴承钢耐腐蚀性较差。Cronidur30材料是一种铬-钼-氮合金，具有耐高温、耐腐蚀性、高强度和高硬度等优异性能的第三代新材料轴承钢。通过一定含量氮降低钢中碳含量，避免大块共晶碳化物形成。而Cronidur30材料经过深冷及淬、回火后一般残余奥氏体含量较小，当残余奥氏体含量上升会造成服役过程材料强度和寿命不稳定现象，甚至由于应力诱发及高温工况下导致马氏体转变，影响轴承尺寸稳定性造成精度丧失的失效。作为未来新型材料的优先使用级较高，而现有技术对其残余奥氏体测量准确性的不够高。At present, among the high-end bearing materials, the first and second generation bearing steel materials are still used more in my country. Among them, 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 Corrosion resistance is poor. Cronidur30 material is a chromium-molybdenum-nitrogen alloy, a third-generation new material bearing steel with excellent properties such as high temperature resistance, corrosion resistance, high strength and high hardness. Reduce the carbon content in the steel through a certain content of nitrogen to avoid the formation of large eutectic carbides. However, Cronidur30 material generally has a small residual austenite content after cryogenic cooling, quenching and tempering. When the residual austenite content increases, the strength and service life of the material will be unstable during service, and even due to stress induction and high temperature conditions. Martensitic transformation, which affects the dimensional stability of the bearing and causes the failure of precision loss. As a new type of material in the future, the priority of use is high, but the existing technology is not high enough to measure its retained austenite.
Cronidur30高氮不锈钢轴承中残余奥氏体含量上升会造成服役过程材料强度和寿命不稳定现象，甚至由于应力诱发及高温工况下导致马氏体转变，影响轴承尺寸稳定性造成精度丧失的失效。本发明可以解决现有技术无法准确测量Cronidur30高氮不锈钢轴承的残余奥氏体含量问题，提供实际工程应用价值。The increase of residual austenite content in Cronidur30 high-nitrogen stainless steel bearings will lead to unstable material strength and life during service, and even martensite transformation due to stress induction and high temperature conditions, affecting bearing dimensional stability and resulting in failure of precision loss. The invention can solve the problem that the prior art cannot accurately measure the residual austenite content of the Cronidur30 high-nitrogen stainless steel bearing, and provides practical engineering application value.
发明内容Contents of the invention
针对现有技术无法准确测量Cronidur30高氮不锈钢轴承的残余奥氏体含量的不足，本发明提供一种Cronidur30高氮不锈钢中残余奥氏体含量测量方法。本发明的是通过配置特定比例电解液溶液制样提高XRD测量峰值稳定性，结合五峰六值法得到准确残余奥氏体的含量，以克服现有技术中存在的不足。Aiming at the deficiency that the prior art cannot accurately measure the residual austenite content of Cronidur30 high-nitrogen stainless steel bearings, the present invention provides a method for measuring the residual austenite content in Cronidur30 high-nitrogen stainless steel. The present invention improves the peak stability of XRD measurement by configuring a specific ratio of electrolyte solution sample preparation, and obtains the accurate content of retained austenite in combination with the five-peak and six-value method, so as to overcome the deficiencies in the prior art.
为实现上述目的，本发明提供一种Cronidur30高氮不锈钢中残余奥氏体含量测量方法，包括如下步骤：In order to achieve the above object, the present invention provides a method for measuring residual austenite content in Cronidur30 high nitrogen stainless steel, comprising the steps of:
步骤一：准备好Cronidur30高氮不锈钢轴承试样和无织构的纯铁素体块状试样，将他们进行切割，制备20mm×20mm的金相试样，试样切割厚度为10~20mm；切割后的试样进行热镶嵌制备为Ф30mm高度10~30mm的金相样品；Step 1: Prepare the Cronidur30 high-nitrogen stainless steel bearing sample and the non-textured pure ferrite block sample, and cut them to prepare a metallographic sample of 20mm×20mm, and the cutting thickness of the sample is 10~20mm; The cut sample is hot-mounted to prepare a metallographic sample with a height of Ф30mm and a height of 10-30mm;
步骤二： 将制备好的金相样品通过自动磨抛机从400、600、1200目砂纸进行机械研磨后抛光；把镶嵌抛光后的待测试样取出，准备电解抛光；Step 2: Mechanically grind and polish the prepared metallographic samples from 400, 600, and 1200 mesh sandpaper through an automatic grinding and polishing machine; take out the sample to be tested after inlaying and polishing, and prepare for electrolytic polishing;
步骤三：将试样进行电解抛光去除表面变形层与应力层，预先配置好专用电解液冷却静置，电解抛光参数为20V电压，电解抛光18~20s，得到表面无污染的光亮层，电解抛光后的试样进行超声洗涤细小污渍，避免影响X射线衍射扫描结果；Step 3: Electropolish the sample to remove the surface deformation layer and stress layer, pre-configure the special electrolyte to cool and let it stand, the electrolytic polishing parameter is 20V voltage, electrolytic polishing 18~20s, get a bright layer without pollution on the surface, electrolytic polishing Ultrasonic cleaning of small stains on the final sample to avoid affecting the X-ray diffraction scanning results;
步骤四：将处理好的Cronidur30试样放置于特定的塑料卡槽中心，背面用橡皮泥固定；选定奥氏体衍射峰为（200）、（220）和（311），马氏体衍射峰为（200）和（211），选定X射线衍射仪采用Cu靶，管电压为30kV~35kV，采用后置石墨单色器，扫描范围为20~120°，扫描步率0.02°，扫描速度1°/min；Step 4: Place the processed Cronidur30 sample in the center of a specific plastic card slot, and fix it with plasticine on the back; the selected austenite diffraction peaks are (200), (220) and (311), and the martensite diffraction peaks are For (200) and (211), the selected X-ray diffractometer adopts Cu target, the tube voltage is 30kV~35kV, the post graphite monochromator is used, the scanning range is 20~120°, the scanning step rate is 0.02°, and the scanning speed is 1°/min;
步骤五：将纯铁素体试样作为标样进行扫描，得到标样的衍射图谱；Step 5: Scan the pure ferrite sample as a standard sample to obtain the diffraction pattern of the standard sample;
步骤六：将Cronidur30试样进行扫描，得到待测试样的衍射图谱；Step 6: Scan the Cronidur30 sample to obtain the diffraction pattern of the sample to be tested;
步骤七：得到的衍射图谱采用五峰六值法处理，得到残余奥氏体体的准确测量值。Step 7: The obtained diffraction pattern is processed by the five-peak and six-value method to obtain the accurate measurement value of the retained austenite.
进一步地，步骤一中所述切割机为Struers Discotom-10型手自一体自动切割机，亦可采用线切割等方式，镶嵌机采用StruersCitoPress-1型自动镶嵌机。Further, the cutting machine described in step 1 is a Struers Discotom-10 manual automatic cutting machine, and wire cutting can also be used, and the mounting machine adopts a Struers CitoPress-1 automatic mounting machine.
进一步地，步骤二中所述自动磨抛机为Struers Tegramin-25型自动磨抛机。Further, the automatic grinding and polishing machine described in step 2 is a Struers Tegramin-25 automatic grinding and polishing machine.
进一步地，步骤三中所述电解抛光机为Electromet 4型电解抛光腐蚀机。Further, the electrolytic polishing machine described in step three is an Electromet 4 type electrolytic polishing and etching machine.
进一步地，步骤五中所述X射线衍射仪为Smartlab SE型X射线衍射仪。Further, the X-ray diffractometer described in step five is a Smartlab SE X-ray diffractometer.
进一步地，步骤三中所述电解液使用高锰酸钾、无水酒精和水比例为7：2：1。Further, the electrolyte solution in Step 3 uses potassium permanganate, absolute alcohol and water in a ratio of 7:2:1.
本发明的有益效果是：采用这种方法后，实现了去除表面应力层和污染物，在金相显微镜下可观察到真实的组织层。并通过XRD测量出Cronidur30高氮不锈钢轴承试样真实的残余奥氏体含量，避免了因制样而出现的误判，本发明的测量方法通过特别配置的电解液较传统适配电解液使Cronidur30新型轴承材料表面应力去除显著提高试样表面质量，得到最真实的表面残奥分布；本发明的测量方法便于X射线衍射试样表面，能够显著提高XRD测量衍射峰稳定性，得到Cronidur30轴承准确的残余奥氏体含量；该方法可以完善目前常规的XRD测量残余奥氏体的方法，避免了Cronidur30高氮不锈钢轴承残奥含量测量不准确而导致的工艺研判错误。综上所述，本发明具有提高Cronidur30高氮不锈钢试样表面质量，改善XRD衍射峰稳定性，提高残余奥氏体测量结果准确性的优点，同时适合于其他高碳铬轴承材料的优点。采用这种制样方法预计可以额外节省100万元以上的效益。The beneficial effects of the invention are: after adopting this method, the surface stress layer and pollutants are removed, and the real tissue layer can be observed under a metallographic microscope. And the real residual austenite content of the Cronidur30 high-nitrogen stainless steel bearing sample is measured by XRD, which avoids misjudgment due to sample preparation. The measurement method of the present invention makes the Cronidur30 The surface stress removal of the new bearing material significantly improves the surface quality of the sample, and obtains the most realistic surface residual distribution; the measurement method of the present invention is convenient for the surface of the X-ray diffraction sample, can significantly improve the stability of the XRD measurement diffraction peak, and obtain accurate Cronidur30 bearings. Retained austenite content; this method can improve the current conventional XRD method for measuring retained austenite, and avoid process research and judgment errors caused by inaccurate measurement of residual austenite content in Cronidur30 high-nitrogen stainless steel bearings. In summary, the present invention has the advantages of improving the surface quality of Cronidur30 high-nitrogen stainless steel samples, improving the stability of XRD diffraction peaks, improving the accuracy of retained austenite measurement results, and being suitable for other high-carbon chromium bearing materials. Using this sample preparation method is expected to save an additional benefit of more than 1 million yuan.
附图说明Description of drawings
图1为本发明实施例中的残余奥氏体测量方法技术路线图；Fig. 1 is the technical roadmap of the method for measuring retained austenite in the embodiment of the present invention;
图2为本发明实施例中xrd测量结果图谱；Fig. 2 is xrd measurement result collection of illustrative plates in the embodiment of the present invention;
图3为本发明实施例中xrd处理结果图谱。Fig. 3 is an atlas of xrd processing results in an embodiment of the present invention.
具体实施方式Detailed ways
下面结合附图对本发明实施例作进一步说明：如图1-3所示，Cronidur30高氮不锈钢中残余奥氏体含量测量方法，结合图1说明本实施过程为：Below in conjunction with the accompanying drawings the embodiment of the present invention is further described: as shown in Figure 1-3, the residual austenite content measurement method in Cronidur30 high-nitrogen stainless steel, in conjunction with Figure 1 illustrates that this implementation process is:
步骤一：准备好Cronidur30高氮不锈钢轴承试样和无织构的纯铁素体块状试样，将他们进行切割，制备20mm×20mm的金相试样，试样切割厚度为10~20mm。切割后的试样进行热镶嵌制备为Ф30mm高度10~30mm的金相样品；Step 1: Prepare the Cronidur30 high-nitrogen stainless steel bearing sample and the non-textured pure ferrite block sample, and cut them to prepare a metallographic sample of 20mm×20mm, and the cutting thickness of the sample is 10~20mm. The cut sample is hot-mounted to prepare a metallographic sample with a height of Ф30mm and a height of 10-30mm;
步骤二：将制备好的金相样品通过自动磨抛机从400、600、1200目砂纸进行机械研磨后抛光。把镶嵌抛光后的待测试样取出，准备电解抛光；Step 2: The prepared metallographic sample is mechanically ground and polished by an automatic grinding and polishing machine from 400, 600, and 1200 mesh sandpaper. Take out the sample to be tested after mosaic polishing, and prepare for electrolytic polishing;
步骤三：将试样进行电解抛光去除表面变形层与应力层，预先配置好专用电解液冷却静置，电解抛光参数为20V电压，电解抛光18~20s，得到表面无污染的光亮层，电解抛光后的试样进行超声洗涤细小污渍，避免影响X射线衍射扫描结果；Step 3: Electropolish the sample to remove the surface deformation layer and stress layer, pre-configure the special electrolyte to cool and let it stand, the electrolytic polishing parameter is 20V voltage, electrolytic polishing 18~20s, get a bright layer without pollution on the surface, electrolytic polishing Ultrasonic cleaning of small stains on the final sample to avoid affecting the X-ray diffraction scanning results;
步骤四：将处理好的Cronidur30试样放置于定制的塑料卡槽中心，背面用橡皮泥固定。选定奥氏体衍射峰为（200）、（220）和（311），马氏体衍射峰为（200）和（211），选定X射线衍射仪采用Cu靶，管电压为30kV~35kV，采用后置石墨单色器，扫描范围为20~120°，扫描步率0.02°，扫描速度1°/min；Step 4: Place the processed Cronidur30 sample in the center of the custom-made plastic card slot, and fix it with plasticine on the back. The selected austenite diffraction peaks are (200), (220) and (311), the martensite diffraction peaks are (200) and (211), the selected X-ray diffractometer uses Cu target, and the tube voltage is 30kV~35kV , using post-mounted graphite monochromator, the scanning range is 20~120°, the scanning step rate is 0.02°, and the scanning speed is 1°/min;
步骤五：将纯铁素体试样作为标样进行扫描，得到标样的衍射图谱；Step 5: Scan the pure ferrite sample as a standard sample to obtain the diffraction pattern of the standard sample;
步骤六：将Cronidur30试样进行扫描，得到待测试样的衍射图谱；Step 6: Scan the Cronidur30 sample to obtain the diffraction pattern of the sample to be tested;
步骤七：得到的衍射图谱采用五峰六值法处理，得到残余奥氏体体的准确测量值。Step 7: The obtained diffraction pattern is processed by the five-peak and six-value method to obtain the accurate measurement value of the retained austenite.
步骤一中所述切割机为Struers Discotom-10型手自一体自动切割机，亦可采用线切割等方式，镶嵌机采用StruersCitoPress-1型自动镶嵌机。步骤二中所述自动磨抛机为Struers Tegramin-25型自动磨抛机。步骤三中所述电解抛光机为Electromet 4型电解抛光腐蚀机。步骤五中所述X射线衍射仪为Smartlab SE型X射线衍射仪。步骤三中所述电解液使用高锰酸钾、无水酒精和水比例为7：2：1。The cutting machine mentioned in step 1 is a Struers Discotom-10 manual automatic cutting machine, and wire cutting can also be used. The mounting machine adopts a Struers CitoPress-1 automatic mounting machine. The automatic grinding and polishing machine described in step 2 is a Struers Tegramin-25 automatic grinding and polishing machine. The electrolytic polishing machine described in step 3 is an Electromet 4 type electrolytic polishing and etching machine. The X-ray diffractometer described in step five is a Smartlab SE X-ray diffractometer. The electrolytic solution described in Step 3 uses potassium permanganate, absolute alcohol and water in a ratio of 7:2:1.
根据图2所述的得到衍射图谱xrd测量结果原始数据；根据图3所述的根据五峰衍射分布计算衍射积分强度；Cronidur30高氮不锈钢xrd衍射法结果：Obtain the original data of the diffraction pattern xrd measurement result according to Fig. 2; Calculate the diffraction integral intensity according to the five-peak diffraction distribution described in Fig. 3; Cronidur30 high-nitrogen stainless steel xrd diffraction method result:
奥氏体衍射峰为（200）、（220）和（311），马氏体衍射峰为（200）和（211）的参数：Austenite diffraction peaks are (200), (220) and (311), martensite diffraction peaks are (200) and (211) parameters:
Cronidur30高氮不锈钢五峰六值法计算结果：Calculation results of Cronidur30 high-nitrogen stainless steel with five-peak and six-value method:
综上所述，本发明具有提高Cronidur30高氮不锈钢试样表面质量，改善XRD衍射峰稳定性，提高残余奥氏体测量结果准确性的优点，同时适合于其他高碳铬轴承材料的优点。In summary, the present invention has the advantages of improving the surface quality of Cronidur30 high-nitrogen stainless steel samples, improving the stability of XRD diffraction peaks, improving the accuracy of retained austenite measurement results, and being suitable for other high-carbon chromium bearing materials.
以上实施例，只是本发明优选地具体实施例的一种，本领域技术人员在本发明技术方案范围内进行的通常变化和替换都包含在本发明的保护范围内。The above embodiments are only one of the preferred specific embodiments of the present invention, and the usual 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 protection scope of the present invention.
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