CN106245029B - Aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel is shown, preparation method and application method - Google Patents
Aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel is shown, preparation method and application method Download PDFInfo
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- 229910000963 austenitic stainless steel Inorganic materials 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 230000002045 lasting effect Effects 0.000 title 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 45
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 24
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012153 distilled water Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 238000005260 corrosion Methods 0.000 claims description 14
- 230000007797 corrosion Effects 0.000 claims description 13
- 230000003628 erosive effect Effects 0.000 claims description 9
- 238000005530 etching Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 229920000742 Cotton Polymers 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 4
- 235000009161 Espostoa lanata Nutrition 0.000 claims description 3
- 240000001624 Espostoa lanata Species 0.000 claims description 3
- 229960004756 ethanol Drugs 0.000 claims 1
- 239000007787 solid Substances 0.000 abstract 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23F1/00—Etching metallic material by chemical means
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- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
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- 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
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Abstract
Super304H奥氏体不锈钢持久试样组织显示的侵蚀剂、制备方法及应用方法，该侵蚀剂包括：体积分数为30‑40％的蒸馏水，体积分数为35‑45％的分析纯无水乙醇，体积分数为10‑15％分析纯氢氟酸，积分数为10‑15％分析纯盐酸，和质量分数3‑5％三氯化铁；所述体积分数均为各组分占侵蚀剂总体积的百分数，质量分数为固体占侵蚀剂总质量的百分数；本发明还公开了该侵蚀剂的制备方法及应用方法；本发明解决了现有Super304H奥氏体不锈钢侵蚀剂难以显示持久试样组织中析出相和晶界的问题。
The etchant, preparation method and application method shown in the Super304H austenitic stainless steel durable sample structure, the etchant includes: distilled water with a volume fraction of 30-40%, analytical pure absolute ethanol with a volume fraction of 35-45%, volume The fraction is 10-15% of analytically pure hydrofluoric acid, the integral fraction is 10-15% of analytically pure hydrochloric acid, and the mass fraction of 3-5% ferric chloride; said volume fraction is the total volume of each component in the etchant Percentage, mass fraction is the percentage of solids accounting for the total mass of the etchant; the invention also discloses the preparation method and application method of the etchant; Phase and grain boundary issues.
Description
技术领域technical field
本发明属于金属材料金相检验方法的侵蚀剂，具体涉及到Super304H奥氏体不锈钢持久试样组织显示的侵蚀剂、制备方法及应用方法。The invention belongs to an etchant for metallographic inspection methods of metal materials, and in particular relates to an etchant for Super304H austenitic stainless steel permanent sample structure display, a preparation method and an application method.
背景技术Background technique
目前，Super304H奥氏体不锈钢金相检验最常用的化学侵蚀剂主要是王水(盐酸和硝酸体积比为3:1)和三氯化铁盐酸水溶液(5克三氯化铁+50毫升盐酸+100毫升水)。新配的王水需在24h后使用，主要应用于Super304H奥氏体不锈钢原材料，而三氯化铁盐酸水溶液可以现配现用，适用于服役后的Super304H奥氏体不锈钢。At present, the most commonly used chemical etching agents for metallographic examination of Super304H austenitic stainless steel are mainly aqua regia (the volume ratio of hydrochloric acid and nitric acid is 3:1) and ferric chloride hydrochloric acid aqueous solution (5 grams of ferric chloride + 50 ml of hydrochloric acid + 100 ml of water). The newly formulated aqua regia needs to be used after 24 hours, and is mainly used in Super304H austenitic stainless steel raw materials, while the ferric chloride hydrochloric acid aqueous solution can be prepared and used immediately, and is suitable for Super304H austenitic stainless steel after service.
Super304H奥氏体不锈钢持久试样在温度和应力的作用下，显微组织发生变化，多种析出相会发生不同程度的析出。采用王水和三氯化铁盐酸水溶液作为这种试样的侵蚀剂在使用过程中存在一定的缺陷，在显示持久试样组织中的析出相形态方面效果不理想。由于王水的强氧化性和三氯化铁盐酸酒精溶液过快的腐蚀速度，在侵蚀过程中容易侵蚀过渡，致使析出相因过腐蚀发生脱落，并且晶界很难完整清晰的显示出来，从而影响后续微观组织观察和分析的准确性，影响Super304H持久试样组织老化损伤分析的判定。Under the action of temperature and stress, the microstructure of the durable sample of Super304H austenitic stainless steel will change, and various precipitates will be precipitated to varying degrees. The use of aqua regia and ferric chloride hydrochloric acid aqueous solution as the etchant of this sample has certain defects in the use process, and the effect is not ideal in displaying the precipitated phase morphology in the durable sample structure. Due to the strong oxidation of aqua regia and the too fast corrosion rate of ferric chloride hydrochloric acid alcohol solution, it is easy to erode transition during the erosion process, resulting in the precipitation phase falling off due to over-corrosion, and it is difficult to display the grain boundary completely and clearly, thus It affects the accuracy of subsequent microstructure observation and analysis, and affects the judgment of Super304H durable sample tissue aging damage analysis.
发明内容Contents of the invention
本发明的目的在于克服现有Super304H奥氏体不锈钢组织侵蚀剂难以完整、清晰显示出Super304H持久试样晶界及析出相的缺点，保证Super304H持久试样高温老化损伤分析的准确性，提供了一种可以清晰显示Super304H奥氏体不锈钢持久试样微观组织的晶界和析出相的侵蚀剂、制备方法及应用方法。The purpose of the present invention is to overcome the shortcomings of the existing Super304H austenitic stainless steel structure etchant that it is difficult to completely and clearly show the grain boundaries and precipitated phases of the Super304H durable sample, to ensure the accuracy of the high-temperature aging damage analysis of the Super304H durable sample, and to provide a An etchant, a preparation method and an application method that can clearly display the grain boundaries and precipitated phases of the microstructure of a durable sample of Super304H austenitic stainless steel.
为达到上述目的，本发明采用如下技术方案：To achieve the above object, the present invention adopts the following technical solutions:
Super304H奥氏体不锈钢持久试样组织显示的侵蚀剂，所述侵蚀剂包括体积分数为30-40％蒸馏水、体积分数为35-45％的分析纯无水乙醇、体积分数为10-15％的分析纯盐酸、体积分数为10-15％的分析纯氢氟酸以及质量分数为3-5％三氯化铁；所述体积分数均为各组分占侵蚀剂总体积的百分数，所述质量分数为三氯化铁占侵蚀剂总质量的百分数。The corrosion agent shown by the Super304H austenitic stainless steel durable sample structure, the corrosion agent includes distilled water with a volume fraction of 30-40%, analytical pure absolute ethanol with a volume fraction of 35-45%, and distilled water with a volume fraction of 10-15%. Analytical pure hydrochloric acid, analytical pure hydrofluoric acid with a volume fraction of 10-15% and a mass fraction of 3-5% ferric chloride; the volume fractions are the percentages of each component in the total volume of the etchant, and the mass The fraction is the percentage of ferric chloride in the total mass of the etchant.
所述的Super304H奥氏体不锈钢持久试样组织显示的侵蚀剂，包括体积分数为36％蒸馏水、体积分数为36％的分析纯无水乙醇、体积分数为14％的分析纯盐酸、体积分数为14％的分析纯氢氟酸以及质量分数为4％三氯化铁。The corrosion agent shown by the permanent sample structure of the Super304H austenitic stainless steel includes a volume fraction of 36% distilled water, a volume fraction of 36% analytically pure dehydrated alcohol, a volume fraction of 14% analytically pure hydrochloric acid, and a volume fraction of 14% analytically pure hydrofluoric acid and 4% ferric chloride in mass fraction.
所述的Super304H奥氏体不锈钢持久试样组织显示的侵蚀剂，包括体积分数为33％蒸馏水、体积分数为41％的分析纯无水乙醇、体积分数为13％的分析纯盐酸、体积分数为13％的分析纯氢氟酸以及质量分数为3％的三氯化铁。The corrosion agent shown by the permanent sample structure of Super304H austenitic stainless steel includes 33% distilled water by volume fraction, 41% analytical pure dehydrated alcohol by 41% analytical pure hydrochloric acid by 13% by volume fraction, and 13% analytical pure hydrochloric acid by volume fraction. 13% analytically pure hydrofluoric acid and 3% ferric chloride.
所述的Super304H奥氏体不锈钢持久试样组织显示的侵蚀剂，包括体积分数为31％蒸馏水、体积分数为43％的分析纯无水乙醇、体积分数为13％的分析纯盐酸、体积分数为13％的分析纯氢氟酸以及质量分数为4％的三氯化铁。The corrosion agent shown by the permanent sample structure of the Super304H austenitic stainless steel includes a volume fraction of 31% distilled water, a volume fraction of 43% analytically pure absolute ethanol, a volume fraction of 13% analytically pure hydrochloric acid, and a volume fraction of 13% analytically pure hydrofluoric acid and 4% ferric chloride.
上述所述Super304H奥氏体不锈钢持久试样组织显示的侵蚀剂的制备方法，量取占侵蚀剂总体积分数为30-40％蒸馏水、35-45％无水乙醇加入烧杯中，再依次分别量取占侵蚀剂总体积分数为10-15％分析纯氢氟酸、10-15％分析纯盐酸，沿烧杯内壁缓缓加入烧杯中，并不断用玻璃棒搅拌，再加入占侵蚀剂总质量分数3-5％三氯化铁，混合均匀得到侵蚀剂。The preparation method of the etchant shown in the above-mentioned Super304H austenitic stainless steel durable sample structure is to measure 30-40% distilled water and 35-45% absolute ethanol in the beaker, and then measure them respectively Take 10-15% analytically pure hydrofluoric acid and 10-15% analytically pure hydrochloric acid that account for the total volume of the etchant, slowly add them into the beaker along the inner wall of the beaker, and keep stirring with a glass rod, then add the total mass fraction of the etchant 3-5% ferric chloride, mixed evenly to obtain the etchant.
上述所述Super304H奥氏体不锈钢持久试样组织显示的侵蚀剂用于Super304H钢持久试样微观组织显示的方法，包括如下步骤：The method that the above-mentioned Super304H austenitic stainless steel durable sample structure display corrosive agent is used for the Super304H steel durable sample microstructure display method includes the following steps:
步骤1：在Super304H持久试样上截取金相试块，对其表面进行磨平和机械抛光，用无水乙醇清洗干净，然后用吹风机吹干；Step 1: Take a metallographic test block on the Super304H durable sample, grind and mechanically polish the surface, clean it with absolute ethanol, and then dry it with a hair dryer;
步骤2：将本发明所述的侵蚀剂倒入放有脱脂棉的玻璃器皿中，将抛光好的Super304H持久试样的金相试块侵蚀面朝下浸入，侵蚀时间为1-3分钟；待到试样表面呈白灰色时取出，用水冲洗，用干净脱脂棉球擦去试样表面的腐蚀产物；Step 2: Pour the etchant of the present invention into a glass vessel with absorbent cotton, and immerse the metallographic test block erosion side of the polished Super304H durable sample downwards, and the erosion time is 1-3 minutes; When the surface of the sample is white-gray, take it out, rinse it with water, and wipe off the corrosion products on the surface of the sample with a clean absorbent cotton ball;
步骤3：用无水乙醇对经过侵蚀的Super304H持久试样的金相试块表面进行清洗，再用吹风机进行吹干，在显微镜下进行金相组织观察和拍照。Step 3: Clean the surface of the metallographic test block of the eroded Super304H durable sample with absolute ethanol, then dry it with a hair dryer, observe and take pictures of the metallographic structure under a microscope.
和现有技术相比较，本发明具有如下优点：Compared with the prior art, the present invention has the following advantages:
本发明在常用的三氯化铁盐酸水溶液配方基础上通过调整盐酸的比例，加入一定量氢氟酸，同时通过调整溶剂，加入无水乙醇配置而成。为了降低腐蚀速度，一方面通过调整溶剂以来改变侵蚀剂的挥发性，改善其稳定性；另一方面，通过降低酸的含量，或者使用一种弱酸来减缓其侵蚀性能。本发明选择了降低盐酸的含量、加入氢氟酸、使用无水乙醇来减缓所配侵蚀剂的腐蚀性能并增加其稳定性。采用本发明侵蚀剂对Super304H奥氏体不锈钢持久试样进行侵蚀，组织显示效果好，析出相和晶界显示清晰；侵蚀速度易于控制；侵蚀剂重复使用性强。The present invention is prepared by adjusting the proportion of hydrochloric acid, adding a certain amount of hydrofluoric acid, adjusting the solvent and adding absolute ethanol on the basis of the commonly used formula of ferric trichloride hydrochloric acid aqueous solution. In order to reduce the corrosion rate, on the one hand, the volatility of the etchant is changed by adjusting the solvent to improve its stability; on the other hand, the corrosion performance is slowed down by reducing the acid content or using a weak acid. The present invention chooses to reduce the content of hydrochloric acid, add hydrofluoric acid, and use absolute ethanol to slow down the corrosion performance of the matched corrosive agent and increase its stability. The etchant of the invention is used to erode the permanent sample of the Super304H austenitic stainless steel, and the microstructure display effect is good, and the precipitated phase and the grain boundary are clearly displayed; the erosion speed is easy to control; and the etchant has strong reusability.
附图说明Description of drawings
图1是用王水侵蚀剂Super304H奥氏体不锈钢持久试样金相组织(200×)。Figure 1 is the metallographic structure of a durable sample of Super304H austenitic stainless steel with aqua regia etchant (200×).
图2是用王水侵蚀剂Super304H奥氏体不锈钢持久试样金相组织(500×)。Figure 2 is the metallographic structure of a durable sample of Super304H austenitic stainless steel with aqua regia etchant (500×).
图3是用三氯化铁盐酸水溶液侵蚀剂Super304H奥氏体不锈钢持久试样金相组织(500×)。Fig. 3 is the metallographic structure (500×) of the durable sample of Super304H austenitic stainless steel with ferric chloride hydrochloric acid aqueous solution etching agent.
图4是用本发明侵蚀剂Super304H奥氏体不锈钢持久试样金相组织(200×)。Fig. 4 is the metallographic structure (200×) of the durable sample of Super304H austenitic stainless steel using the etchant of the present invention.
图5是用本发明侵蚀剂Super304H奥氏体不锈钢持久试样金相组织(500×)。Fig. 5 is the metallographic structure (500×) of the durable sample of Super304H austenitic stainless steel using the etchant of the present invention.
具体实施方式Detailed ways
下面结合附图和具体实施例对本发明作进一步详细说明。The present invention will be described in further detail below in conjunction with the accompanying drawings and specific embodiments.
实施例1：取50毫升的蒸馏水和50毫升的无水乙醇在烧杯中混合，分别量取20毫升分析纯盐酸和20分析纯氢氟酸，依次沿烧杯内壁缓缓加入烧杯中，不断搅拌，最后加入称取5克的三氯化铁，不断搅拌混合均匀得到侵蚀剂。Example 1: Mix 50 milliliters of distilled water and 50 milliliters of dehydrated ethanol in a beaker, measure 20 milliliters of analytically pure hydrochloric acid and 20 milliliters of analytically pure hydrofluoric acid, and slowly add them to the beaker along the inner wall of the beaker, stirring continuously. Finally, add and weigh 5 grams of ferric trichloride, stir and mix evenly to obtain the etchant.
实施例2：取45毫升的蒸馏水和56毫升的无水乙醇在烧杯中混合，分别量取18毫升分析纯盐酸和18分析纯氢氟酸，依次沿烧杯内壁缓缓加入烧杯中，不断搅拌，最后加入称取4.5克的三氯化铁，不断搅拌混合均匀得到侵蚀剂。Example 2: Mix 45 milliliters of distilled water and 56 milliliters of absolute ethanol in a beaker, measure 18 milliliters of analytically pure hydrochloric acid and 18 milliliters of analytically pure hydrofluoric acid, and slowly add them into the beaker along the inner wall of the beaker, stirring continuously. Finally, add and weigh 4.5 grams of ferric chloride, stir and mix evenly to obtain the etchant.
实施例3：取45毫升的水和62毫升的无水乙醇在烧杯中混合，分别量取19毫升分析纯盐酸和19分析纯氢氟酸，依次沿烧杯内壁缓缓加入烧杯中，不断搅拌，最后加入称取5.5克的三氯化铁，不断搅拌混合均匀得到侵蚀剂。Example 3: Mix 45 milliliters of water and 62 milliliters of absolute ethanol in a beaker, measure 19 milliliters of analytically pure hydrochloric acid and 19 milliliters of analytically pure hydrofluoric acid, and slowly add them to the beaker along the inner wall of the beaker, stirring constantly, Finally, add and weigh 5.5 grams of ferric trichloride, stir and mix evenly to obtain the etchant.
本发明侵蚀剂的应用方法如下：The application method of etching agent of the present invention is as follows:
1)在Super304H持久试样上截取金相试块，对其表面进行磨平和机械抛光，用无水乙醇清洗干净，然后用吹风机吹干；1) Take a metallographic test block from the Super304H durable sample, grind and mechanically polish the surface, clean it with absolute ethanol, and then dry it with a hair dryer;
2)将本发明所述的侵蚀剂倒入放有脱脂棉的玻璃器皿中，将抛光好的Super304H持久试样的金相试块侵蚀面朝下浸入，侵蚀时间为1-3分钟。待到试样表面呈白灰色时去处，用水冲洗，用干净脱脂棉球擦去试样表面的腐蚀产物；2) Pour the etching agent of the present invention into a glass vessel with absorbent cotton, and immerse the metallographic test block of the polished Super304H durable sample with the erosion side facing down, and the erosion time is 1-3 minutes. When the surface of the sample is white-gray, rinse it with water, and wipe off the corrosion products on the surface of the sample with a clean absorbent cotton ball;
3)用无水乙醇对经过侵蚀Super304H持久试样的金相试样表面进行清洗，再用吹风机进行吹干，在显微镜下进行金相组织观察和拍照。3) Clean the metallographic sample surface of the eroded Super304H durable sample with absolute ethanol, then dry it with a hair dryer, observe the metallographic structure and take pictures under a microscope.
图1-2是采用王水侵蚀剂对Super304H持久试样侵蚀后的金相组织，图1为放大倍数200×，图2为放大倍数500×，图中晶界显示较深，析出相不明显，部分析出相已脱落。Figure 1-2 is the metallographic structure of the Super304H permanent sample corroded by aqua regia etchant. Figure 1 is a magnification of 200×, and Figure 2 is a magnification of 500×. In the figure, the grain boundaries are deep and the precipitates are not obvious. , part of the analyzed phase has fallen off.
图3是采用三氯化铁盐酸水溶液侵蚀剂对Super304H持久试样侵蚀后的金相组织，图中晶界和析出相显示模糊不清。Figure 3 is the metallographic structure of the Super304H permanent sample after being corroded by an aqueous solution of ferric chloride hydrochloric acid etchant, in which the grain boundaries and precipitated phases are blurred.
图4-5为采用本发明中侵蚀剂对Super304H持久试样侵蚀后的金相组织，图4为放大倍数200×，图5为放大倍数500×，图中晶界显示完全，晶内细小的析出相显示清晰。Fig. 4-5 is the metallographic structure after adopting etchant in the present invention to the Super304H permanent sample corrosion, and Fig. 4 is magnification 200 *, and Fig. 5 is magnification 500 *, and among the figure, grain boundary shows completely, and fine intragranular The precipitated phase is clearly displayed.
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