CN118360654A - A high nitrogen austenitic stainless steel corrosive agent and corrosion method - Google Patents
A high nitrogen austenitic stainless steel corrosive agent and corrosion method Download PDFInfo
- Publication number
- CN118360654A CN118360654A CN202410399788.1A CN202410399788A CN118360654A CN 118360654 A CN118360654 A CN 118360654A CN 202410399788 A CN202410399788 A CN 202410399788A CN 118360654 A CN118360654 A CN 118360654A
- Authority
- CN
- China
- Prior art keywords
- stainless steel
- austenitic stainless
- high nitrogen
- nitrogen austenitic
- corrosion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 238000005260 corrosion Methods 0.000 title claims abstract description 58
- 230000007797 corrosion Effects 0.000 title claims abstract description 58
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 57
- 229910000963 austenitic stainless steel Inorganic materials 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000003518 caustics Substances 0.000 title claims abstract description 32
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000005498 polishing Methods 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 7
- 239000010432 diamond Substances 0.000 claims description 6
- 229910003460 diamond Inorganic materials 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000007689 inspection Methods 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 210000000085 cashmere Anatomy 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 10
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000005530 etching Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 210000001787 dendrite Anatomy 0.000 description 4
- 229910021592 Copper(II) chloride Inorganic materials 0.000 description 3
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- 101001121408 Homo sapiens L-amino-acid oxidase Proteins 0.000 description 2
- 102100026388 L-amino-acid oxidase Human genes 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910001566 austenite Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 101000827703 Homo sapiens Polyphosphoinositide phosphatase Proteins 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 102100023591 Polyphosphoinositide phosphatase Human genes 0.000 description 1
- 101100012902 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) FIG2 gene Proteins 0.000 description 1
- 101100233916 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) KAR5 gene Proteins 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- -1 dendrites Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000013386 optimize process Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
- C25F3/06—Etching of iron or steel
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
Landscapes
- Chemical & Material Sciences (AREA)
- Immunology (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Pathology (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
本发明公开了一种高氮奥氏体不锈钢腐蚀剂及腐蚀方法，高氮奥氏体不锈钢腐蚀剂由体积分数为3％～8％的高氯酸与体积分数为92％～97％的酒精配制而成。本发明的优点在于：腐蚀剂组成简单，方便配制，且无刺激性气味，腐蚀方法易于操作、精确可控、稳定高效、重现性好。腐蚀后试样表面干净整洁，无划痕污染，晶相组织清晰均匀，腐蚀效果十分良好。
The invention discloses a high nitrogen austenitic stainless steel corrosive agent and a corrosion method. The high nitrogen austenitic stainless steel corrosive agent is prepared by 3% to 8% perchloric acid and 92% to 97% alcohol. The invention has the advantages that the corrosive agent has a simple composition, is easy to prepare, and has no irritating odor. The corrosion method is easy to operate, accurately controllable, stable and efficient, and has good reproducibility. After corrosion, the surface of the sample is clean and tidy, without scratch pollution, the crystal phase structure is clear and uniform, and the corrosion effect is very good.
Description
技术领域Technical Field
本发明涉及不锈钢金属腐蚀剂技术领域，特别涉及一种高氮奥氏体不锈钢腐蚀剂及腐蚀方法。The invention relates to the technical field of stainless steel metal corrosive agents, in particular to a high-nitrogen austenitic stainless steel corrosive agent and a corrosive method.
背景技术Background technique
高氮奥氏体不锈钢是新一代先进钢铁材料之一，具有优异的力学性能，耐蚀性能和生物相容性能，在国防军工、核电工业和医疗器械等领域具有广阔的应用前景。氮作为一种重要的合金元素加入到不锈钢当中，有益于扩大并稳定奥氏体相。通过与其它元素(如Cr、Mn等)的协同作用，在显著提高不锈钢强度的同时，并不降低其韧性，还能大幅度增强其耐磨和耐腐蚀性能。High nitrogen austenitic stainless steel is one of the new generation of advanced steel materials. It has excellent mechanical properties, corrosion resistance and biocompatibility, and has broad application prospects in the fields of national defense, nuclear power industry and medical equipment. Nitrogen, as an important alloying element, is added to stainless steel, which is beneficial to expand and stabilize the austenite phase. Through the synergistic effect with other elements (such as Cr, Mn, etc.), it significantly improves the strength of stainless steel without reducing its toughness, and can also greatly enhance its wear resistance and corrosion resistance.
金相检测分析是钢种研发和生产过程中重要的基础手段，对掌握产品的微观组织(如枝晶、析出相、夹杂物、微裂纹、气孔和晶粒度等)、优化工艺参数、提升产品质量至关重要。由于氮元素的添加使高氮奥氏体不锈钢耐蚀性能变得十分优越，使用传统的不锈钢金相腐蚀剂(王水、CuCl2溶液等)的腐蚀效果不理想，不能很好地显示高氮不锈钢的原始奥氏体晶界。关于高氮奥氏体不锈钢金相腐蚀的方法鲜有报道，且现有的一些关于不锈钢的腐蚀工艺并不能适用于高氮奥氏体不锈钢金相。Metallographic testing and analysis is an important basic means in the process of steel research and development and production. It is crucial to master the microstructure of the product (such as dendrites, precipitates, inclusions, microcracks, pores and grain size, etc.), optimize process parameters, and improve product quality. The addition of nitrogen makes the corrosion resistance of high nitrogen austenitic stainless steel very superior. The corrosion effect of using traditional stainless steel metallographic etchants (aqua regia, CuCl2 solution, etc.) is not ideal and cannot well display the original austenite grain boundaries of high nitrogen stainless steel. There are few reports on the metallographic corrosion methods of high nitrogen austenitic stainless steel, and some existing corrosion processes for stainless steel are not applicable to the metallographic of high nitrogen austenitic stainless steel.
因此，探索出一种适用于高氮奥氏体不锈钢的腐蚀试剂与腐蚀方法，对高氮奥氏体不锈钢的应用具有重要意义。Therefore, exploring a corrosion reagent and corrosion method suitable for high nitrogen austenitic stainless steel is of great significance to the application of high nitrogen austenitic stainless steel.
发明内容Summary of the invention
本发明要解决的技术问题是提供一种腐蚀效果好的高氮奥氏体不锈钢腐蚀剂及腐蚀方法。The technical problem to be solved by the present invention is to provide a high nitrogen austenitic stainless steel corrosive agent and a corrosion method with good corrosion effect.
为了解决上述技术问题，本发明提供一种高氮奥氏体不锈钢腐蚀剂，其由体积分数为3％～8％的高氯酸与体积分数为92％～97％的酒精配制而成。In order to solve the above technical problems, the present invention provides a high nitrogen austenitic stainless steel corrosive agent, which is prepared by 3% to 8% perchloric acid by volume and 92% to 97% alcohol by volume.
优选的，由体积分数为5％的高氯酸与体积分数为95％的酒精配制而成Preferably, it is prepared by 5% by volume perchloric acid and 95% by volume alcohol.
优选的，所述高氮奥氏体不锈钢中N含量≥0.45％。Preferably, the nitrogen content in the high nitrogen austenitic stainless steel is ≥ 0.45%.
优选的，所述高氯酸的浓度为70％～72％。Preferably, the concentration of the perchloric acid is 70% to 72%.
优选的，所述酒精为无水乙醇。Preferably, the alcohol is anhydrous ethanol.
本发明还提供一种高氮奥氏体不锈钢腐蚀方法，包括如下步骤：The present invention also provides a high nitrogen austenitic stainless steel corrosion method, comprising the following steps:
S1、配置高氮奥氏体不锈钢腐蚀剂：依次加入92ml～98ml的酒精、2ml～8ml的高氯酸，搅拌均匀，静置2h以上；S1. Prepare high nitrogen austenitic stainless steel corrosive agent: add 92ml~98ml of alcohol and 2ml~8ml of perchloric acid in sequence, stir evenly, and let stand for more than 2h;
S2、镶嵌试样；S2, mounted specimen;
S3、打磨、抛光；S3, grinding and polishing;
S4、金相腐蚀：将试样做阳极并与电源的正极连接，用铂做阴极并与电源的阴极连接，浸入所述S1所制备的高氮奥氏体不锈钢腐蚀液中，然后接通直流稳压电源进行腐蚀，直至试样抛光面呈现银灰色时取出，依次用清水，酒精冲洗干净再吹干。S4, metallographic corrosion: the sample is used as an anode and connected to the positive electrode of the power supply, and platinum is used as a cathode and connected to the cathode of the power supply, and immersed in the high nitrogen austenitic stainless steel corrosion solution prepared in S1, and then a DC regulated power supply is connected for corrosion, until the polished surface of the sample turns silver gray, take it out, rinse it with water and alcohol in turn, and then blow it dry.
所述步骤S2镶嵌试样的具体步骤为：将试样放置在镶嵌机中使用酚醛树脂粉进行冷镶，镶嵌温度为室温、时间为15min；The specific steps of mounting the sample in step S2 are: placing the sample in a mounting machine and using phenolic resin powder for cold mounting, the mounting temperature is room temperature, and the time is 15 minutes;
进一步的，所述步骤S3打磨、抛光的具体方法为：对待测试样的检测面用砂纸依次进行打磨和抛光，直至去除掉检查面表面的划痕、凹坑及污点，使其表面光洁明亮，之后用流水冲洗抛光好的检测表面，用酒精擦洗并吹干；Furthermore, the specific method of grinding and polishing in step S3 is: grinding and polishing the inspection surface of the test sample with sandpaper in sequence until the scratches, pits and stains on the inspection surface are removed to make the surface smooth and bright, then rinsing the polished inspection surface with running water, scrubbing with alcohol and drying;
进一步的，打磨的方法为：依次使用320目、600目、1000目、1500目、2000目、3000目、5000目、7000目的砂纸在流水下进行打磨。Furthermore, the grinding method is: use 320 mesh, 600 mesh, 1000 mesh, 1500 mesh, 2000 mesh, 3000 mesh, 5000 mesh, and 7000 mesh sandpaper in sequence to grind under running water.
进一步的，抛光的方法为：先用植绒抛光布配合粒度为5μm的金刚石抛光膏进行粗抛，待抛掉磨痕且抛痕方向一致后再使用羊绒抛光布及粒度为1μm的金刚石抛光膏进行精抛，直至表面呈镜面光泽且在光学显微镜下没有观察到抛光痕。Furthermore, the polishing method is: first use a flocked polishing cloth and a diamond polishing paste with a particle size of 5μm for rough polishing, and then use a cashmere polishing cloth and a diamond polishing paste with a particle size of 1μm for fine polishing after the wear marks are removed and the directions of the polishing marks are consistent, until the surface has a mirror gloss and no polishing marks are observed under an optical microscope.
进一步的，所述步骤S4中电源为直流稳压电源，电压为3v～8v，通电时间为2s～40s。Furthermore, in step S4, the power supply is a DC regulated power supply with a voltage of 3V to 8V and a power-on time of 2s to 40s.
本发明有益效果：Beneficial effects of the present invention:
本发明提供的高氮奥氏体不锈钢腐蚀剂组成简单，方便配制，且无刺激性气味，腐蚀方法易于操作、精确可控、稳定高效、重现性好。腐蚀后试样表面干净整洁，无划痕污染，晶相组织清晰均匀，腐蚀效果十分良好，对于研究高氮奥氏体不锈钢的晶粒形貌具有重要意义。The high nitrogen austenitic stainless steel etchant provided by the present invention has a simple composition, is easy to prepare, and has no irritating odor. The corrosion method is easy to operate, accurately controllable, stable and efficient, and has good reproducibility. After corrosion, the surface of the sample is clean and tidy, without scratch pollution, the crystal phase structure is clear and uniform, and the corrosion effect is very good, which is of great significance for studying the grain morphology of high nitrogen austenitic stainless steel.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1为实施例4腐蚀得到的样品的金相组织图；FIG1 is a metallographic structure diagram of a sample obtained by etching in Example 4;
图2为实施例5腐蚀得到的样品的金相组织图；FIG2 is a metallographic structure diagram of the sample obtained by corrosion in Example 5;
图3为实施例6腐蚀得到的样品的金相组织图；FIG3 is a metallographic structure diagram of the sample obtained by corrosion in Example 6;
图4为实施例7腐蚀得到的样品的金相组织图；FIG4 is a metallographic structure diagram of the sample obtained by etching in Example 7;
图5为对比例1腐蚀得到的样品的金相组织图；FIG5 is a metallographic structure diagram of the sample obtained by corrosion in Comparative Example 1;
图6为对比例2腐蚀得到的样品的金相组织图。FIG. 6 is a metallographic structure diagram of the sample obtained by corrosion in Comparative Example 2.
具体实施方式Detailed ways
下面结合附图对本发明的具体实施方式作进一步说明。在此需要说明的是，对于这些实施方式的说明用于帮助理解本发明，但并不构成对本发明的限定。此外，下面所描述的本发明各个实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互组合。The specific embodiments of the present invention are further described below in conjunction with the accompanying drawings. It should be noted that the description of these embodiments is used to help understand the present invention, but does not constitute a limitation of the present invention. In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.
实施例1Example 1
一种高氮奥氏体不锈钢腐蚀剂，其由体积分数为3％的高氯酸与体积分数为97％的酒精配制而成。A high-nitrogen austenitic stainless steel corrosive agent is prepared from 3% by volume of perchloric acid and 97% by volume of alcohol.
进一步的，所述高氮奥氏体不锈钢中的N含量≥0.45％。Furthermore, the nitrogen content in the high nitrogen austenitic stainless steel is ≥ 0.45%.
进一步的，所述高氯酸的浓度为70％～72％。Furthermore, the concentration of the perchloric acid is 70% to 72%.
进一步的，所述酒精为无水乙醇。Furthermore, the alcohol is anhydrous ethanol.
实施例2Example 2
一种高氮奥氏体不锈钢腐蚀剂，与实施例1相比，只改变了高氯酸与酒精的比例，具体的，由体积分数为5％的高氯酸与体积分数为95％的酒精配制而成。A high nitrogen austenitic stainless steel corrosive agent, compared with Example 1, only the ratio of perchloric acid to alcohol is changed, specifically, the corrosive agent is prepared from 5% by volume perchloric acid and 95% by volume alcohol.
实施例3Example 3
一种高氮奥氏体不锈钢腐蚀剂，与实施例1相比，只改变了高氯酸与酒精的比例，具体的，由体积分数为8％的高氯酸与体积分数为92％的酒精配制而成。A high nitrogen austenitic stainless steel corrosive agent, compared with Example 1, only the ratio of perchloric acid to alcohol is changed, specifically, the corrosive agent is prepared from 8% by volume of perchloric acid and 92% by volume of alcohol.
实施例4Example 4
一种高氮奥氏体不锈钢腐蚀方法，包括如下步骤：A high nitrogen austenitic stainless steel corrosion method comprises the following steps:
S1、配置实施例1所述的高氮奥氏体不锈钢腐蚀剂：依次加入97ml的酒精、3ml的高氯酸，搅拌均匀，静置2h以上；S1. Prepare the high nitrogen austenitic stainless steel corrosive agent described in Example 1: add 97 ml of alcohol and 3 ml of perchloric acid in sequence, stir evenly, and let stand for more than 2 hours;
S2、镶嵌试样：将高氮奥氏体不锈钢试样放置在镶嵌机中使用酚醛树脂粉进行冷镶，镶嵌温度为室温、时间为15min；高氮奥氏体不锈钢试样具体的合金成分为(按重量)：21％Cr，19％Mn，2％Ni，1％Mo和余量的N；S2. Mounting sample: The high nitrogen austenitic stainless steel sample is placed in a mounting machine and cold mounted using phenolic resin powder. The mounting temperature is room temperature and the time is 15 minutes. The specific alloy composition of the high nitrogen austenitic stainless steel sample is (by weight): 21% Cr, 19% Mn, 2% Ni, 1% Mo and the balance N.
S3、打磨、抛光：对待测试样的检测面用砂纸依次进行打磨和抛光，直至去除掉检查面表面的划痕、凹坑及污点，使其表面光洁明亮，之后用流水冲洗抛光好的检测表面，用酒精擦洗并吹干；打磨的方法为：依次使用320目、600目、1000目、1500目、2000目、3000目、5000目、7000目的砂纸在流水下进行打磨；抛光的方法为：先用植绒抛光布配合粒度为5μm的金刚石抛光膏进行粗抛，待抛掉磨痕且抛痕方向一致后再使用羊绒抛光布及粒度为1μm的金刚石抛光膏进行精抛，直至表面呈镜面光泽且在光学显微镜下没有观察到抛光痕；S3, grinding and polishing: the test surface of the test sample is grinded and polished with sandpaper in sequence until the scratches, pits and stains on the surface of the test surface are removed, making the surface smooth and bright, then the polished test surface is rinsed with running water, scrubbed with alcohol and blown dry; the grinding method is: use 320 mesh, 600 mesh, 1000 mesh, 1500 mesh, 2000 mesh, 3000 mesh, 5000 mesh, 7000 mesh sandpaper to grind under running water in sequence; the polishing method is: first use flocked polishing cloth with diamond polishing paste with a particle size of 5μm for rough polishing, and after the wear marks are removed and the polishing marks are in the same direction, use cashmere polishing cloth and diamond polishing paste with a particle size of 1μm for fine polishing until the surface is mirror-like and no polishing marks are observed under an optical microscope;
S4、金相腐蚀：将试样做阳极并与电源的正极连接，用铂做阴极并与电源的阴极连接，浸入所述S1所制备的高氮奥氏体不锈钢腐蚀液中，然后接通直流稳压电源进行腐蚀，直至试样抛光面呈现银灰色时取出，依次用清水，酒精冲洗干净再吹干；电源为直流稳压电源，电压为3v，通电时间为40s。S4, metallographic corrosion: the sample is used as the anode and connected to the positive electrode of the power supply, and platinum is used as the cathode and connected to the cathode of the power supply, and immersed in the high nitrogen austenitic stainless steel corrosion liquid prepared in S1, and then connected to a DC regulated power supply for corrosion, until the polished surface of the sample turns silver gray, take it out, rinse it with clean water and alcohol in turn, and then blow it dry; the power supply is a DC regulated power supply, the voltage is 3V, and the power-on time is 40s.
将利用上述方法腐蚀得到的样品放在显微镜下进行观察，观察得到的金相组织如图1所示，可以看到，腐蚀出了一部分晶界。The sample obtained by etching using the above method was placed under a microscope for observation. The obtained metallographic structure is shown in FIG1 . It can be seen that a portion of the grain boundary has been etched out.
实施例5Example 5
一种高氮奥氏体不锈钢腐蚀方法，除步骤S1中配置的腐蚀剂和S4中通电的电压和通电时间与实施例4不同外，其余步骤均相同。具体的，配置的高氮奥氏体不锈钢腐蚀剂为实施例2中所述的高氮奥氏体不锈钢腐蚀剂：依次加入95ml的酒精、5ml的高氯酸，搅拌均匀，静置2h以上；所述步骤S4中电压为5v，通电时间为10s。A high nitrogen austenitic stainless steel corrosion method, except that the corrosive agent configured in step S1 and the voltage and power-on time in step S4 are different from those in Example 4, the remaining steps are the same. Specifically, the high nitrogen austenitic stainless steel corrosive agent configured is the high nitrogen austenitic stainless steel corrosive agent described in Example 2: 95 ml of alcohol and 5 ml of perchloric acid are added in sequence, stirred evenly, and left to stand for more than 2 hours; the voltage in step S4 is 5V, and the power-on time is 10s.
将利用上述方法腐蚀得到的样品放在显微镜下进行观察，观察得到的金相组织如图2所示，可以看到晶界较为清晰，完整，均匀，腐蚀效果较好，易于观测。The sample obtained by etching using the above method was observed under a microscope. The metallographic structure obtained by observation is shown in Figure 2. It can be seen that the grain boundaries are relatively clear, complete, and uniform, the etching effect is good, and it is easy to observe.
实施例6Example 6
一种高氮奥氏体不锈钢腐蚀方法，除步骤S1中配置的腐蚀剂和S4中通电的电压和通电时间与实施例4不同外，其余步骤均相同。具体的，配置的高氮奥氏体不锈钢腐蚀剂为实施例2中所述的高氮奥氏体不锈钢腐蚀剂：依次加入95ml的酒精、5ml的高氯酸，搅拌均匀，静置2h以上；所述步骤S4中电压为5v，通电时间为15s。A high nitrogen austenitic stainless steel corrosion method, except that the corrosive agent configured in step S1 and the voltage and power-on time in step S4 are different from those in Example 4, the remaining steps are the same. Specifically, the high nitrogen austenitic stainless steel corrosive agent configured is the high nitrogen austenitic stainless steel corrosive agent described in Example 2: 95 ml of alcohol and 5 ml of perchloric acid are added in sequence, stirred evenly, and left to stand for more than 2 hours; the voltage in step S4 is 5V, and the power-on time is 15s.
将利用上述方法腐蚀得到的样品放在显微镜下进行观察，观察得到的金相组织如图3所示，可以看到晶界清晰，完整，均匀，腐蚀效果好，易于观测，且金相比图2更加清晰。The sample obtained by etching using the above method was observed under a microscope. The metallographic structure obtained by observation is shown in Figure 3. It can be seen that the grain boundaries are clear, complete and uniform, the corrosion effect is good, and it is easy to observe. The metallographic structure is clearer than Figure 2.
实施例7Example 7
一种高氮奥氏体不锈钢腐蚀方法，除步骤S1中配置的腐蚀剂和S4中通电的电压和通电时间与实施例4不同外，其余步骤均相同。具体的，配置的高氮奥氏体不锈钢腐蚀剂为实施例3中所述的高氮奥氏体不锈钢腐蚀剂：依次加入92ml的酒精、8ml的高氯酸，搅拌均匀，静置2h以上；所述步骤S4中电压为8v，通电时间为2s。A high nitrogen austenitic stainless steel corrosion method, except that the corrosive agent configured in step S1 and the voltage and power-on time in step S4 are different from those in Example 4, the remaining steps are the same. Specifically, the high nitrogen austenitic stainless steel corrosive agent configured is the high nitrogen austenitic stainless steel corrosive agent described in Example 3: 92 ml of alcohol and 8 ml of perchloric acid are added in sequence, stirred evenly, and left to stand for more than 2 hours; the voltage in step S4 is 8V, and the power-on time is 2s.
将利用上述方法腐蚀得到的样品放在显微镜下进行观察，观察得到的金相组织如图4所示，可以看到有部分晶界被腐蚀出来了，但腐蚀不均，靠近试样边界部分腐蚀效果较好，此时，试样内部晶界较浅，效果不如实施例5和实施例6。The sample obtained by etching using the above method was observed under a microscope. The metallographic structure obtained by observation is shown in Figure 4. It can be seen that part of the grain boundary has been corroded, but the corrosion is uneven. The corrosion effect is better near the sample boundary. At this time, the grain boundary inside the sample is shallow, and the effect is not as good as that of Example 5 and Example 6.
对比例1Comparative Example 1
一种高氮奥氏体不锈钢金相腐蚀方法，除步骤S1中配置的腐蚀剂和S4腐蚀与实施例5不同外，其余步骤均相同。具体的，步骤S1为：配制CuCl2腐蚀液：依次向烧杯中加入4g硫酸铜、20mL去离子水和22mL浓度为38％的浓盐酸，用玻璃棒不断搅拌，待硫酸铜全部溶解后静置10min以上待用。步骤S4腐蚀：用脱脂棉蘸取步骤S1配置的CuCl2腐蚀液，反复擦拭试样表面8s至试样抛光面呈现银灰色，依次用清水，酒精冲洗干净再吹干。A high nitrogen austenitic stainless steel metallographic corrosion method, except that the corrosive agent configured in step S1 and S4 corrosion are different from those in Example 5, the remaining steps are the same. Specifically, step S1 is: prepare CuCl2 corrosion solution: add 4g copper sulfate, 20mL deionized water and 22mL concentrated hydrochloric acid with a concentration of 38% to a beaker in sequence, stir continuously with a glass rod, and stand for more than 10 minutes after the copper sulfate is completely dissolved. Step S4 corrosion: dip the CuCl2 corrosion solution configured in step S1 with absorbent cotton, repeatedly wipe the surface of the sample for 8s until the polished surface of the sample appears silver-gray, rinse with clean water and alcohol in sequence, and then blow dry.
将利用上述方法腐蚀得到的样品放在显微镜下进行观察，观察得到的金相组织如图5所示，可以看到腐蚀较浅，只出现了部分晶界，且随腐蚀出现了一些细微的抛痕，腐蚀效果较差。The sample obtained by the above method was observed under a microscope. The metallographic structure obtained by the observation is shown in Figure 5. It can be seen that the corrosion is shallow, only part of the grain boundary appears, and some fine polishing marks appear with the corrosion, and the corrosion effect is poor.
对比例2Comparative Example 2
一种高氮奥氏体不锈钢金相腐蚀方法，除步骤S1中配置的腐蚀剂和S4腐蚀与实施例5不同外，其余步骤均相同。具体的，步骤S1为：配制王水腐蚀液：依次向烧杯中加入60mL浓度为38％的浓盐酸和20mL浓度为68％的浓硝酸，用玻璃棒不断搅拌，待溶液混合均匀后静置10min以上待用。步骤S4腐蚀：将抛好的试样浸入步骤S1配置的王水腐蚀液中，腐蚀80s，至试样抛光面呈现银灰色，依次用清水，酒精冲洗干净再吹干。A high nitrogen austenitic stainless steel metallographic corrosion method, except that the corrosive agent configured in step S1 and S4 corrosion are different from those in Example 5, the remaining steps are the same. Specifically, step S1 is: prepare aqua regia corrosion solution: add 60mL of 38% concentrated hydrochloric acid and 20mL of 68% concentrated nitric acid to a beaker in turn, stir continuously with a glass rod, and let the solution stand for more than 10 minutes after mixing evenly. Step S4 corrosion: immerse the polished sample in the aqua regia corrosion solution configured in step S1, corrode for 80s, until the polished surface of the sample appears silver-gray, rinse with clean water and alcohol in turn, and then blow dry.
将利用上述方法腐蚀得到的样品放在显微镜下进行观察，观察得到的金相组织如图6所示，试样表面腐蚀的很不均匀，一部分枝晶发生了过腐蚀，而另一部分枝晶却未发生腐蚀；枝晶轮廓模糊不清，腐蚀效果较差。The sample obtained by the above method was observed under a microscope. The metallographic structure obtained by observation is shown in Figure 6. The surface of the sample was corroded very unevenly. Some dendrites were over-corroded while other dendrites were not corroded. The outline of the dendrites was blurred and the corrosion effect was poor.
以上结合附图对本发明的实施方式作了详细说明，但本发明不限于所描述的实施方式。对于本领域的技术人员而言，在不脱离本发明原理和精神的情况下，对这些实施方式进行多种变化、修改、替换和变型，仍落入本发明的保护范围内。The embodiments of the present invention are described in detail above with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. For those skilled in the art, various changes, modifications, substitutions and variations of these embodiments are made without departing from the principles and spirit of the present invention, and still fall within the scope of protection of the present invention.
Claims (10)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410399788.1A CN118360654A (en) | 2024-04-03 | 2024-04-03 | A high nitrogen austenitic stainless steel corrosive agent and corrosion method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410399788.1A CN118360654A (en) | 2024-04-03 | 2024-04-03 | A high nitrogen austenitic stainless steel corrosive agent and corrosion method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118360654A true CN118360654A (en) | 2024-07-19 |
Family
ID=91875992
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410399788.1A Pending CN118360654A (en) | 2024-04-03 | 2024-04-03 | A high nitrogen austenitic stainless steel corrosive agent and corrosion method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN118360654A (en) |
-
2024
- 2024-04-03 CN CN202410399788.1A patent/CN118360654A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107991161B (en) | Metallographic corrosive agent and corrosion method for super austenitic stainless steel | |
| CN104593775B (en) | Metallographic etchant for observing δ-Ni3Nb phase in nickel-iron-based superalloy structure and its application method | |
| CN105908249B (en) | The electrolytic etching method of stainless steel/carbon composite plate metallographic structure | |
| CN107340170B (en) | Corrosion method for displaying as-cast high-nitrogen austenitic stainless steel grain boundary | |
| CN103175726A (en) | Metallographic corrosion method for clearly displaying original austenite grain boundary of NiCrMoV type rotor steel | |
| CN104233301B (en) | Metallographic etchant used for HR-2 antihydrogen steel, and preparation method and corrosion method of metallographic etchant | |
| CN114295456B (en) | A GH4169 high temperature alloy grain etchant and its application | |
| CN110389129B (en) | Etching agent and etching method for displaying 690 nickel-based alloy deposited metal grain boundaries | |
| CN109991254A (en) | A kind of preparation method of pure iron EBSD sample | |
| CN107574439A (en) | Etching agent for displaying original austenite grain boundary of FB2 steel, preparation method and application | |
| CN111751184A (en) | A kind of preparation method of tantalum and tantalum-tungsten alloy metallographic sample | |
| CN112730004B (en) | Metallographic corrosion method of δ-ferrite in 1Cr13 martensitic stainless steel | |
| CN108396321B (en) | Metallographic corrosive liquid for austenitic stainless steel and preparation corrosion method thereof | |
| CN110318055A (en) | A kind of high-strength steel stainless steel dissimilar transit joint metallographic etching agent | |
| CN110749718A (en) | Dendritic crystal corrosive agent and corrosion method for maraging stainless steel | |
| CN109440181B (en) | Method for removing anodic oxidation Ni-Ti-O nano-pore disordered layer on surface of NiTi alloy | |
| CN110954388A (en) | Metallographic etchant for laser cladding layer containing rare earth titanium alloy and method for displaying structure | |
| CN118360654A (en) | A high nitrogen austenitic stainless steel corrosive agent and corrosion method | |
| CN103499480A (en) | Metallographic phase corrosion method displaying austenitic stainless steel grain boundary | |
| CN109518186A (en) | A kind of α, β two-phase brass metallographic etching agent and its display methods of metallographic structure | |
| CN115928074B (en) | Al-Mg-Si alloy grain boundary corrosive liquid | |
| CN110470525A (en) | Show the aggressive agent and corrosion method of IF steel crystal boundary | |
| CN114672808A (en) | Corrosive agent, preparation and corrosion method of γ' phase metallographic phase in nickel-based alloy | |
| CN114323887A (en) | Preparation method and corrosion method of nickel-based alloy metallographic corrosive agent | |
| CN115090875A (en) | A kind of electrolytic corrosion method of nickel-based powder superalloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |