CN111876783A - Metallographic chemical polishing solution and application thereof in field of austenitic stainless steel metallographic detection - Google Patents
Metallographic chemical polishing solution and application thereof in field of austenitic stainless steel metallographic detection Download PDFInfo
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Abstract
本发明具体涉及一种金相化学抛光液及在奥氏体不锈钢金相检测领域的应用。传统化学抛光液应用于奥氏体不锈钢表面检测难以达到理想的抛光效果,本发明提供了一种适用于18Cr‑8Ni型奥氏体不锈钢金相检测的化学抛光液,所述化学抛光液中各成分及比例如下:盐酸120ml/L~160ml/L、磷酸120ml/L~160ml/L、硝酸钠50g/L~70g/L、30%过氧化氢300ml/L、乙醇100ml/L、硫脲5g/L、盐酸抑雾剂1g/L,余量为水。该化学抛光液应用于奥氏体不锈钢能够有效抑制抛光过程中产生的酸雾、配制方法简便安全性高,能够得到清晰的金相组织表面。
The invention specifically relates to a metallographic chemical polishing liquid and its application in the field of metallographic detection of austenitic stainless steel. It is difficult to achieve the ideal polishing effect when the traditional chemical polishing liquid is applied to the surface inspection of austenitic stainless steel. The present invention provides a chemical polishing liquid suitable for the metallographic inspection of 18Cr-8Ni type austenitic stainless steel. The ingredients and proportions are as follows: hydrochloric acid 120ml/L~160ml/L, phosphoric acid 120ml/L~160ml/L, sodium nitrate 50g/L~70g/L, 30% hydrogen peroxide 300ml/L, ethanol 100ml/L, thiourea 5g /L, hydrochloric acid fog inhibitor 1g/L, the balance is water. When the chemical polishing liquid is applied to austenitic stainless steel, the acid mist generated in the polishing process can be effectively suppressed, the preparation method is simple and safe, and a clear metallographic structure surface can be obtained.
Description
技术领域technical field
本发明属于金相检测抛光技术领域,具体涉及一种金相化学抛光液、所述抛光液的配制方法以及所述金相化学抛光液在18Cr-8Ni型奥氏体不锈钢金相检测领域的应用。The invention belongs to the technical field of metallographic detection and polishing, and in particular relates to a metallographic chemical polishing liquid, a preparation method of the polishing liquid, and the application of the metallographic chemical polishing liquid in the field of metallographic detection of 18Cr-8Ni type austenitic stainless steel .
背景技术Background technique
公开该背景技术部分的信息仅仅旨在增加对本发明的总体背景的理解,而不必然被视为承认或以任何形式暗示该信息构成已经成为本领域一般技术人员所公知的现有技术。The information disclosed in this Background section is only for enhancement of understanding of the general background of the invention and should not necessarily be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
近年来,随着电站锅炉向高参数、大容量、高效率方向的快速发展,对受热部件材料的使用性能和加工性能提出了更高的要求。18Cr-8Ni型奥氏体不锈钢因其良好的组织稳定性、较高的蠕变强度、优良的抗氧化、抗高温腐蚀性能被大量应用在超临界电站锅炉的受热面管上。受热面管往往是在极为恶劣的工况下(尤其是在装机容量较大的机组上,管子外表面的烟气温度超过1000℃,管子内流动的高压蒸汽温度在540℃以上,压力达16MPa以上)运行的,随着运行时间的积累,难免会出现组织老化、腐蚀、晶间裂纹等缺陷,这些缺陷的产生严重影响了机组的安全运行,因此对奥氏体不锈钢的金相检测是电站锅炉金属监督项目中重要的一部分,而在实际的金属监督过程中需要在不损伤部件的前提下进行现场金相制备。由于现场工况的复杂性和环境条件的局限性,现场金相制备难度远远大于试验室制备。而制约现场金相制备过程中的主要难点之一就是金相抛光。In recent years, with the rapid development of high-parameter, large-capacity, and high-efficiency power plant boilers, higher requirements have been placed on the performance and processing performance of heated components. 18Cr-8Ni type austenitic stainless steel is widely used in the heating surface tubes of supercritical power plant boilers because of its good microstructure stability, high creep strength, excellent oxidation resistance and high temperature corrosion resistance. The heating surface tube is often under extremely harsh working conditions (especially in units with large installed capacity, the temperature of the flue gas on the outer surface of the tube exceeds 1000 °C, the temperature of the high-pressure steam flowing in the tube is above 540 °C, and the pressure reaches 16MPa. The above) operation, with the accumulation of operating time, it is inevitable that there will be defects such as tissue aging, corrosion, intergranular cracks, etc. The occurrence of these defects seriously affects the safe operation of the unit. Therefore, the metallographic detection of austenitic stainless steel is a power station. It is an important part of the boiler metal supervision project, and in the actual metal supervision process, it is necessary to carry out on-site metallographic preparation without damaging the components. Due to the complexity of on-site working conditions and the limitations of environmental conditions, on-site metallographic preparation is far more difficult than laboratory preparation. One of the main difficulties restricting the on-site metallographic preparation process is metallographic polishing.
在现场金相检测过程中,主要有磨光、抛光、侵蚀和观察等步骤。抛光质量的好坏将对金相组织的清晰度产生直接的影响,如果抛光质量欠佳,一些细小微小的缺陷(如碳化物的析出、晶间裂纹等)将不容易发现,形成漏检。所以目前现场最常用的抛光方式为机械抛光,是利用便携手持式电动抛光机,配合金刚石抛光液进行,但是该方法受工件形状及环境位置的限制,在抛光的过程较难控制,所需抛光时间较长,划痕不易抛掉,并容易出现局部区域过热的现象,抛光效果并不理想。In the process of on-site metallographic inspection, there are mainly steps such as polishing, polishing, erosion and observation. The quality of polishing will have a direct impact on the clarity of the metallographic structure. If the polishing quality is not good, some small and tiny defects (such as carbide precipitation, intergranular cracks, etc.) will not be easily found, resulting in missed inspections. Therefore, the most commonly used polishing method in the field is mechanical polishing, which is carried out by using a portable hand-held electric polishing machine with diamond polishing liquid. However, this method is limited by the shape of the workpiece and the location of the environment. It is difficult to control the polishing process, and the required polishing For a long time, the scratches are not easy to throw away, and the phenomenon of overheating in local areas is prone to occur, and the polishing effect is not ideal.
化学抛光是不锈钢金相检测常用的抛光工艺,可以抛光形状复杂的部件,检测效率高。就功能性而言,化学抛光除了能得到物理、化学清洁度的表面外,还能除去不锈钢金相测点表面经研磨后的机械损伤层和应力层,得到机械清洁度的表面。但是传统的化学抛光方法应用于奥氏体不锈钢存在一些不足:由于奥氏体不锈钢中Cr、Ni等合金元素的含量较高(质量分数总和往往接近30%),传统的金相化学抛光液往往由于酸度不足等因素无法对其进行化学抛光。Chemical polishing is a commonly used polishing process for metallographic inspection of stainless steel. It can polish parts with complex shapes and has high inspection efficiency. In terms of functionality, chemical polishing can not only obtain a surface with physical and chemical cleanliness, but also remove the mechanical damage layer and stress layer on the surface of the stainless steel metallographic measuring point after grinding to obtain a surface with mechanical cleanliness. However, there are some shortcomings in the application of traditional chemical polishing methods to austenitic stainless steel: due to the high content of alloying elements such as Cr and Ni in austenitic stainless steel (the total mass fraction is often close to 30%), traditional metallographic chemical polishing solutions often It cannot be chemically polished due to factors such as insufficient acidity.
发明内容SUMMARY OF THE INVENTION
针对上述背景技术中的记载,本发明的技术目的在于提供一种简化的金相检测抛光方法,提高现场检测效率。为了实现该技术目的,本发明提供了一种不锈钢金相检测化学抛光液,所述化学抛光液应用于18Cr-8Ni型奥氏体钢金相测点表面化学抛光,得到的金相组织清晰、便于观察,并且抛光效率高且速度便于控制。In view of the records in the above background art, the technical purpose of the present invention is to provide a simplified metallographic inspection and polishing method to improve the efficiency of on-site inspection. In order to achieve the technical purpose, the present invention provides a chemical polishing liquid for metallographic detection of stainless steel. It is easy to observe, and the polishing efficiency is high and the speed is easy to control.
基于上述技术效果,本发明提供以下技术方案:Based on the above technical effects, the present invention provides the following technical solutions:
本发明第一方面,提供一种金相化学抛光液,所述金相化学抛光液包括以下成分:盐酸、磷酸、硝酸钠、过氧化氢、乙醇、硫脲及盐酸抑雾剂,余量为水。In a first aspect of the present invention, a metallographic chemical polishing liquid is provided, the metallographic chemical polishing liquid includes the following components: hydrochloric acid, phosphoric acid, sodium nitrate, hydrogen peroxide, ethanol, thiourea and hydrochloric acid fog inhibitor, and the balance is water.
盐酸是一种不具有氧化性的无机强酸,是强腐蚀剂,主要起溶解金属的作用。但是单独使用盐酸,对不锈钢制品不起溶解作用,只有与硝酸和其它助剂相结合,才有一定的溶解能力,用于除去不锈钢表面上的氧化层。Hydrochloric acid is a non-oxidizing inorganic strong acid and a strong corrosive agent, mainly for dissolving metals. However, the use of hydrochloric acid alone has no dissolving effect on stainless steel products. Only in combination with nitric acid and other additives, it has a certain dissolving ability to remove the oxide layer on the surface of stainless steel.
磷酸是一种中等强度的三元无机酸,可以增加抛光液的粘度,降低抛光液的酸度,有效地抑制不锈钢的过度溶解。在化学抛光过程中起到一方面起到溶解金属表面的作用,同时还可以在表面生成一层不溶性的磷酸盐钝化膜,这种钝化膜的形成和溶解,可使金相测点表面达到平整,同时还具有抛光的功效。Phosphoric acid is a medium-strength ternary inorganic acid, which can increase the viscosity of the polishing solution, reduce the acidity of the polishing solution, and effectively inhibit the excessive dissolution of stainless steel. In the process of chemical polishing, on the one hand, it plays a role in dissolving the metal surface, and at the same time, an insoluble phosphate passivation film can be formed on the surface. The formation and dissolution of this passivation film can make the surface of metallographic measuring points To achieve flat, but also has the effect of polishing.
硝酸钠是一种强氧化剂,配合盐酸起到溶解作用,有效地去除氧化层,可在金相测点形成钝化膜。相比传统抛光液中采用硝酸作为原料,本发明采用硝酸钠作为替代,不仅可以取得同样良好的抛光效果,还可以有效避免抛光过程中产生黄烟,提高所述抛光液的配置安全性。Sodium nitrate is a strong oxidant, which can dissolve with hydrochloric acid, effectively remove the oxide layer, and form a passivation film at the metallographic measuring point. Compared with using nitric acid as a raw material in the traditional polishing liquid, the present invention adopts sodium nitrate as a substitute, which can not only achieve the same good polishing effect, but also can effectively avoid yellow smoke during the polishing process, and improve the configuration safety of the polishing liquid.
过氧化氢可消除腐蚀残渣和溶解碳及碳化物,提高不锈钢表面的光洁度,也可消除NOx的突沸。无水乙醇的加入能够提高化学抛光液体系中过氧化氢的稳定性,辅助提高不锈钢表面的光洁度。Hydrogen peroxide can eliminate corrosion residues and dissolve carbon and carbides, improve the finish of stainless steel surfaces, and also eliminate NOx bumps. The addition of anhydrous ethanol can improve the stability of hydrogen peroxide in the chemical polishing liquid system and assist in improving the smoothness of the stainless steel surface.
在化学抛光的过程中,产生酸雾的主要途径,一部分是表面金属在抛光液的腐蚀作用下,生成的氢气伴随逸出,另一部分是酸液热挥发而产生。所述盐酸抑雾剂含有表面活性剂,可以产生一定的泡沫,覆盖在抛光液表面,抑制酸的挥发,使酸液与裸露金属表面腐蚀放出的氢气大大的减少,并使得酸液降温至酸露点以下,带出的酸液减少,减少了酸的损耗。降低污染及对试验、检测人员身体的伤害。还能够清除各种油污,减缓或抑制盐酸对金属的腐蚀,与盐酸具有良好的协同效果,适用于各种温度下的盐酸使用。In the process of chemical polishing, the main way to generate acid mist is that part of the surface metal is corroded by the polishing solution, and the generated hydrogen gas is accompanied by the escape, and the other part is generated by the thermal volatilization of the acid solution. The hydrochloric acid fog suppressant contains a surfactant, which can generate a certain amount of foam, which covers the surface of the polishing liquid, inhibits the volatilization of the acid, greatly reduces the hydrogen released by the corrosion of the acid liquid and the exposed metal surface, and cools the acid liquid to an acid level. Below the dew point, the acid liquid brought out is reduced, reducing the loss of acid. Reduce pollution and physical harm to testing and testing personnel. It can also remove various oil stains, slow down or inhibit the corrosion of hydrochloric acid to metals, has a good synergistic effect with hydrochloric acid, and is suitable for the use of hydrochloric acid at various temperatures.
本发明第二方面,提供第一方面所述金相化学抛光液在奥氏体不锈钢金相检测领域的应用。The second aspect of the present invention provides the application of the metallographic chemical polishing solution described in the first aspect in the field of metallographic detection of austenitic stainless steel.
本发明第三方面,提供一种奥氏体不锈钢金相检测工具包,所述检测工具包括第一方面所述金相化学抛光液。A third aspect of the present invention provides an austenitic stainless steel metallographic detection tool kit, the detection tool includes the metallographic chemical polishing solution described in the first aspect.
以上一个或多个技术方案的有益效果是:The beneficial effects of the above one or more technical solutions are:
1.本发明提供的金相化学抛光液相比现有的化学抛光液对成分进行了简化,该化学抛光液的配置更加简单,通过加入抑雾剂,进一步提高了配置过程的安全性,降低污染风险。1. Compared with the existing chemical polishing liquid, the metallographic chemical polishing liquid provided by the present invention simplifies the composition, and the configuration of the chemical polishing liquid is simpler. contamination risk.
2.配置好的化学金相抛光液方便存储与携带,用普通塑料试剂瓶即可承装,可适用于试验室检测,也可以携带至生产现场进行金相检测。并且各成分配合之后性质稳定、不易变质,可长期使用。2. The prepared chemical metallographic polishing liquid is easy to store and carry. It can be loaded with ordinary plastic reagent bottles, which can be suitable for laboratory testing, and can also be carried to the production site for metallographic testing. In addition, the properties of the ingredients are stable, not easy to deteriorate, and can be used for a long time.
3.本发明提供的化学抛光液应用于金相表面检测的操作简单,现场适应度高,不需要借助机械设备,抛光效果好,加入硫脲作为缓蚀剂,抛光速度容易控制,得到的金相组织清晰真实。3. The chemical polishing solution provided by the present invention is easy to operate when applied to metallographic surface detection, has high on-site adaptability, does not require mechanical equipment, and has good polishing effect. The organization is clear and true.
附图说明Description of drawings
构成本发明的一部分的说明书附图用来提供对本发明的进一步理解,本发明的示意性实施例及其说明用于解释本发明,并不构成对本发明的不当限定。The accompanying drawings forming a part of the present invention are used to provide further understanding of the present invention, and the exemplary embodiments of the present invention and their descriptions are used to explain the present invention, and do not constitute an improper limitation of the present invention.
图1为实施例5中所述18Cr-8Ni型奥氏体不锈钢化学抛光后金相组织表面照片;Fig. 1 is the metallographic structure surface photo after chemical polishing of 18Cr-8Ni type austenitic stainless steel described in embodiment 5;
其中,图1a为只采用化学抛光后金相组织表面;图1b为仅采用化学抛光并进行侵蚀后的金相组织表面;图1c为仅采用机械抛光并进行侵蚀后的金相组织表面。Among them, Fig. 1a shows the metallographic structure surface after only chemical polishing; Fig. 1b shows the metallographic structure surface only after chemical polishing and etching; Fig. 1c shows the metallographic structure surface after only using mechanical polishing and etching.
具体实施方式Detailed ways
应该指出,以下详细说明都是例示性的,旨在对本发明提供进一步的说明。除非另有指明,本文使用的所有技术和科学术语具有与本发明所属技术领域的普通技术人员通常理解的相同含义。It should be noted that the following detailed description is exemplary and intended to provide further explanation of the invention. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
需要注意的是,这里所使用的术语仅是为了描述具体实施方式,而非意图限制根据本发明的示例性实施方式。如在这里所使用的,除非上下文另外明确指出,否则单数形式也意图包括复数形式,此外,还应当理解的是,当在本说明书中使用术语“包含”和/或“包括”时,其指明存在特征、步骤、操作、器件、组件和/或它们的组合。It should be noted that the terminology used herein is for the purpose of describing specific embodiments only, and is not intended to limit the exemplary embodiments according to the present invention. As used herein, unless the context clearly dictates otherwise, the singular is intended to include the plural as well, furthermore, it is to be understood that when the terms "comprising" and/or "including" are used in this specification, it indicates that There are features, steps, operations, devices, components and/or combinations thereof.
正如背景技术所介绍的,现有技术中化学抛光液应用于奥氏体不锈钢难以达到理想的效果,可能会出现灰膜、无光、研磨划痕无法去除等问题。为了解决如上的技术问题,本发明提出了一种金相化学抛光液,该抛光液应用于不锈钢表面处理,特别是奥氏体不锈钢表面处理能够获得清晰的金相组织。As described in the background art, in the prior art, it is difficult to achieve ideal results when chemical polishing liquid is applied to austenitic stainless steel, and problems such as gray film, dullness, and inability to remove grinding scratches may occur. In order to solve the above technical problems, the present invention proposes a metallographic chemical polishing liquid, which is applied to the surface treatment of stainless steel, especially the surface treatment of austenitic stainless steel, which can obtain a clear metallographic structure.
本发明第一方面,提供一种金相化学抛光液,所述金相化学抛光液包括以下成分:盐酸、磷酸、硝酸钠、过氧化氢、乙醇、硫脲及盐酸抑雾剂,余量为水。In a first aspect of the present invention, a metallographic chemical polishing liquid is provided, the metallographic chemical polishing liquid includes the following components: hydrochloric acid, phosphoric acid, sodium nitrate, hydrogen peroxide, ethanol, thiourea and hydrochloric acid fog inhibitor, and the balance is water.
优选的,所述化学抛光液中盐酸浓度为1.4~1.92mol/L。Preferably, the concentration of hydrochloric acid in the chemical polishing solution is 1.4-1.92 mol/L.
进一步优选的,本发明提供一种上述盐酸的配制方式,以市售浓盐酸为原料,1L化学抛光液中含有120ml~160ml市售的分析纯盐酸,其他盐酸浓度的化学抛光液配置方式也是如此。Further preferably, the present invention provides a preparation method of the above-mentioned hydrochloric acid, using commercially available concentrated hydrochloric acid as a raw material, 1L of chemical polishing liquid contains 120ml-160ml of commercially available analytically pure hydrochloric acid, and the configuration methods of other chemical polishing liquids of hydrochloric acid concentration are also the same. .
更进一步的,1L化学抛光液中含有130~150ml的市售的分析纯盐酸。Further, 1 L of chemical polishing solution contains 130-150 ml of commercially available analytically pure hydrochloric acid.
在效果较好的一些具体实施方案中,所述浓盐酸含量为140ml每L,即1.68mol/L。In some specific embodiments with better effects, the content of the concentrated hydrochloric acid is 140 ml per L, that is, 1.68 mol/L.
为了兼顾抛光效果及经济成本,上述盐酸采用分析纯市售浓盐酸,通常为质量分数36~38%的浓盐酸产品,经本发明验证,上述浓度偏差不影响本发明化学抛光液配置及抛光效果。In order to take into account the polishing effect and economic cost, the above-mentioned hydrochloric acid adopts analytically pure commercial concentrated hydrochloric acid, usually a concentrated hydrochloric acid product with a mass fraction of 36 to 38%. It is verified by the present invention that the above concentration deviation does not affect the chemical polishing solution configuration and polishing effect of the present invention. .
依据本发明研究,当盐酸低于1.4mol/L时,抛光液化学溶解作用小,溶解速度慢,去除氧化层不完全,抛光效果不理想;当盐酸浓度超过1.92mol/L时,使溶解腐蚀过程加剧,不锈钢表面会产生过腐蚀,抛光液的抛光性能会降低,且因挥发严重易形成酸雾,影响视线。试验结果表明,当盐酸浓度为1.68mol/L时,能够兼顾抛光速度和抛光质量,效果最佳。According to the research of the present invention, when the hydrochloric acid is lower than 1.4mol/L, the chemical dissolution effect of the polishing solution is small, the dissolution rate is slow, the removal of the oxide layer is incomplete, and the polishing effect is not ideal; when the concentration of the hydrochloric acid exceeds 1.92mol/L, the dissolution corrosion is caused. If the process is intensified, the stainless steel surface will be corroded, the polishing performance of the polishing solution will be reduced, and the acid mist will easily form due to serious volatilization, which will affect the sight. The test results show that when the concentration of hydrochloric acid is 1.68mol/L, the polishing speed and polishing quality can be taken into account, and the effect is the best.
优选的,所述磷酸浓度为1.8mol/L~2.4mol/L。Preferably, the phosphoric acid concentration is 1.8 mol/L to 2.4 mol/L.
本发明研究表明,磷酸浓度对抛光质量有较大影响,当磷酸浓度低于1.8mol/L时,金相测点表面磷酸盐转化膜不连续,不能抑制金相测点在盐酸和硝酸作用下发生过腐蚀,抛光液对金相测点只有腐蚀作用;当磷酸浓度超过2.4mol/L时,会增大不锈钢表面的磷酸盐转化膜厚度及形成速度,抑制溶解反应的进行,不能达到抛光的效果。当磷酸浓度为1.8mol/L时,抛光质量最优,既起溶解作用,又可在不锈钢表面上形成不溶性的磷酸盐转化膜,从而有效的抑制金属的过溶解。The research of the present invention shows that the concentration of phosphoric acid has a great influence on the polishing quality. When the concentration of phosphoric acid is lower than 1.8mol/L, the phosphate conversion film on the surface of the metallographic measuring point is discontinuous, which cannot inhibit the metallographic measuring point under the action of hydrochloric acid and nitric acid. If corrosion occurs, the polishing solution only has a corrosive effect on the metallographic measuring point; when the concentration of phosphoric acid exceeds 2.4mol/L, the thickness and formation speed of the phosphate conversion film on the surface of the stainless steel will be increased, the progress of the dissolution reaction will be inhibited, and the polishing effect will not be achieved. Effect. When the concentration of phosphoric acid is 1.8mol/L, the polishing quality is the best, which can not only dissolve, but also form an insoluble phosphate conversion film on the stainless steel surface, thereby effectively inhibiting the overdissolution of metals.
本发明还提供一种上述磷酸的配制方式,采用市售浓磷酸(分析纯,质量分数≥85%)作为原料进行配制,其中,所述磷酸浓度为1.8mol/L~2.4mol/L即为1L化学抛光液中加入120ml~160ml市售浓磷酸产品。市售分析纯浓磷酸产品的浓度通常为质量分数≥85%,经本发明验证,上述浓度偏差不影响本发明化学抛光液配置及抛光效果。The present invention also provides a preparation method of the above phosphoric acid, which uses commercially available concentrated phosphoric acid (analytical purity, mass fraction ≥ 85%) as a raw material for preparation, wherein the phosphoric acid concentration is 1.8mol/L~2.4mol/L, which is Add 120ml to 160ml of commercially available concentrated phosphoric acid to 1L of chemical polishing solution. The concentration of the commercially available analytically pure concentrated phosphoric acid product is usually the mass fraction ≥ 85%. It is verified by the present invention that the above concentration deviation does not affect the configuration and polishing effect of the chemical polishing solution of the present invention.
优选的,所述硝酸钠含量为50g/L~70g/L。Preferably, the sodium nitrate content is 50g/L~70g/L.
当溶液中硝酸钠浓度低于50g/L时,金相测点表面氧化层难以除去,表面会有蚀坑和麻点出现;当硝酸钠浓度超过70g/L时,对不锈钢表面会产生钝化作用,使溶解速度降低。试验结果表明,当硝酸钠浓度为60g/L时,抛光质量最优。When the concentration of sodium nitrate in the solution is less than 50g/L, the oxide layer on the surface of the metallographic measuring point is difficult to remove, and there will be pits and pits on the surface; when the concentration of sodium nitrate exceeds 70g/L, the stainless steel surface will be passivated effect, reducing the dissolution rate. The test results show that the polishing quality is the best when the concentration of sodium nitrate is 60g/L.
优选的,所述硝酸钠采用分析纯产品,质量分数≥99%。Preferably, the sodium nitrate is an analytically pure product with a mass fraction of ≥99%.
优选的,所述过氧化氢浓度为80~100ml/L。过氧化氢为粘稠的液体,本发明提供的化学抛光液中,所述过氧化氢中浓度为每L抛光液中含有纯过氧化氢80~100ml。由于本领域市售的过氧化氢通常为分析纯过氧化氢(质量分数30%)产品,采用上述市售产品配置化学抛光液时,每L化学抛光液中需要加入280~320ml的30%过氧化氢产品。Preferably, the hydrogen peroxide concentration is 80-100 ml/L. Hydrogen peroxide is a viscous liquid. In the chemical polishing liquid provided by the present invention, the concentration of the hydrogen peroxide is 80-100 ml of pure hydrogen peroxide per liter of the polishing liquid. Since the commercially available hydrogen peroxide in this field is usually analytically pure hydrogen peroxide (30% by mass), when using the above commercially available products to prepare chemical polishing solution, 280-320ml of 30% hydrogen peroxide needs to be added to each liter of chemical polishing solution. Hydrogen oxide products.
优选的,所述无水乙醇的浓度为80~120ml/L。Preferably, the concentration of the absolute ethanol is 80-120 ml/L.
优选的,所述硫脲的含量为4~6g/L。Preferably, the content of the thiourea is 4-6 g/L.
优选的,所述盐酸抑雾剂的含量为0.8~1.2g/L。Preferably, the content of the hydrochloric acid fog suppressant is 0.8-1.2 g/L.
上述优选技术方案的一些具体的实施方式中,所述每升化学抛光液溶液各组分比例如下:市售分析纯浓盐酸140ml、市售分析纯浓磷酸140ml、硝酸钠60g、30%过氧化氢300ml、无水乙醇100ml、硫脲5g、盐酸抑雾剂1g,余量为蒸馏水。In some specific embodiments of the above-mentioned preferred technical solutions, the proportions of the components of the chemical polishing solution per liter are as follows: commercially available analytically pure concentrated hydrochloric acid 140ml, commercially available analytically pure concentrated phosphoric acid 140ml, sodium nitrate 60g, 30% peroxide Hydrogen 300ml, anhydrous ethanol 100ml, thiourea 5g, hydrochloric acid fog suppressant 1g, the balance is distilled water.
上述优选技术方案的一些具体实施方式中,所述每升化学抛光液溶液各组分比例如下:市售分析纯浓盐酸130ml、市售分析纯浓磷酸160ml、硝酸钠50g、30%过氧化氢280ml、无水乙醇110ml、硫脲6g、盐酸抑雾剂0.8g,余量为蒸馏水。In some specific embodiments of the above-mentioned preferred technical solutions, the proportions of the components of the chemical polishing solution per liter are as follows: 130ml of commercially available analytically pure concentrated hydrochloric acid, 160ml of commercially available analytically pure concentrated phosphoric acid, 50g of sodium nitrate, 30% hydrogen peroxide 280ml, 110ml of absolute ethanol, 6g of thiourea, 0.8g of hydrochloric acid fog suppressant, and the balance is distilled water.
上述优选技术方案的一些具体实施方式中,所述每升化学抛光液溶液各组分比例如下:市售分析纯浓盐酸150ml、市售分析纯浓磷酸120ml、硝酸钠70g、30%过氧化氢310ml、无水乙醇80ml、硫脲4g、盐酸抑雾剂1.2g,余量为蒸馏水。In some specific embodiments of the above-mentioned preferred technical solutions, the proportions of the components of the chemical polishing solution per liter are as follows: 150ml of commercially available analytically pure concentrated hydrochloric acid, 120ml of commercially available analytically pure concentrated phosphoric acid, 70g of sodium nitrate, 30% hydrogen peroxide 310ml, 80ml of absolute ethanol, 4g of thiourea, 1.2g of hydrochloric acid fog suppressant, and the balance is distilled water.
优选的,所述化学金像抛光液的配制方法如下:量取蒸馏水、无水乙醇及过氧化氢混合均匀,之后加入盐酸、磷酸搅拌均匀,再依次加入硝酸钠、硫脲及盐酸抑雾剂。Preferably, the preparation method of the chemical gold image polishing liquid is as follows: measure distilled water, anhydrous ethanol and hydrogen peroxide and mix them evenly, then add hydrochloric acid and phosphoric acid and stir evenly, and then add sodium nitrate, thiourea and hydrochloric acid fog suppressant in sequence .
本发明第二方面,提供第一方面所述金相化学抛光液在奥氏体不锈钢金相检测领域的应用。The second aspect of the present invention provides the application of the metallographic chemical polishing solution described in the first aspect in the field of metallographic detection of austenitic stainless steel.
优选的,所述奥氏体不锈钢,钢中含Cr约18%、Ni 8%~10%,即18Cr-8Ni型奥氏体不锈钢。Preferably, the austenitic stainless steel contains about 18% of Cr and 8% to 10% of Ni, that is, 18Cr-8Ni type austenitic stainless steel.
优选的,所述金相化学抛光液的抛光方法包括以下步骤:采用吸水材料蘸取所述金相化学抛光液对金相表面进行擦拭,通过观察表面划痕情况,待划痕消失,清洗所述金相表面并干燥。Preferably, the polishing method of the metallographic chemical polishing solution includes the following steps: dipping the metallographic chemical polishing solution with a water-absorbing material to wipe the metallographic surface, and observing the scratches on the surface, after the scratches disappear, clean the surface. the metallographic surface and dried.
进一步优选的,所述清洗步骤采用无水乙醇进行清洗。Further preferably, in the cleaning step, anhydrous ethanol is used for cleaning.
优选的,所述金相化学抛光液的抛光方法包括以下步骤:将待抛光的工件加入所述金相化学抛光液中浸泡,再采用吸水材料对金相表面进行擦拭。Preferably, the polishing method of the metallographic chemical polishing solution includes the following steps: adding the workpiece to be polished into the metallographic chemical polishing solution to soak, and then wiping the metallographic surface with a water-absorbing material.
进一步优选的,所述吸水材料包括但不限于脱脂棉、无纺布、呢绒或丝绒。Further preferably, the water-absorbing material includes, but is not limited to, absorbent cotton, non-woven fabric, woolen wool or velvet.
本发明第三方面,提供一种奥氏体不锈钢金相检测工具包,所述检测工具包括第一方面所述金相化学抛光液。A third aspect of the present invention provides an austenitic stainless steel metallographic detection tool kit, the detection tool includes the metallographic chemical polishing solution described in the first aspect.
优选的,所述奥氏体不锈钢金相检测工具包中,所述金相化学抛光液的原料,盐酸、磷酸、硝酸钠、过氧化氢、乙醇、硫脲及盐酸抑雾剂及水为独立包装,使用前将其混均于容器中。Preferably, in the austenitic stainless steel metallographic detection kit, the raw materials of the metallographic chemical polishing solution, hydrochloric acid, phosphoric acid, sodium nitrate, hydrogen peroxide, ethanol, thiourea, hydrochloric acid fog inhibitor and water are independent Packaging, mix well in container before use.
优选的,所述奥氏体不锈钢金相检测工具包中,所述金相化学抛光液为各原料按配比预混合后的试剂。Preferably, in the austenitic stainless steel metallographic detection tool kit, the metallographic chemical polishing solution is a reagent pre-mixed with each raw material according to the proportions.
优选的,所述奥氏体不锈钢金相检测工具包还包括其他抛光工具,所述其他抛光工具包括但不限于竹夹、镊子、脱脂棉、抛光布、无水乙醇等。Preferably, the austenitic stainless steel metallographic detection tool kit further includes other polishing tools, including but not limited to bamboo clips, tweezers, absorbent cotton, polishing cloth, anhydrous ethanol, and the like.
为了使得本领域技术人员能够更加清楚地了解本发明的技术方案,以下将结合具体的实施例详细说明本发明的技术方案,以下实施例各成分除特别限定外均为市售产品。In order to enable those skilled in the art to understand the technical solutions of the present invention more clearly, the technical solutions of the present invention will be described in detail below with reference to specific embodiments. The components in the following examples are all commercially available products unless otherwise specified.
实施例1Example 1
本实施例中,提供一种金相化学抛光液及配制方法,所述金相化学抛光液中各成分及配比如下:盐酸130ml/L、磷酸160ml/L、硝酸钠50g/L、30%过氧化氢280ml/L、无水乙醇110ml/L、硫脲6g/L、盐酸抑雾剂0.8g/L、余量为蒸馏水。In this embodiment, a metallographic chemical polishing liquid and a preparation method are provided. The components and proportions of the metallographic chemical polishing liquid are as follows: hydrochloric acid 130ml/L, phosphoric acid 160ml/L, sodium nitrate 50g/L, 30% Hydrogen peroxide 280ml/L, absolute ethanol 110ml/L, thiourea 6g/L, hydrochloric acid fog suppressant 0.8g/L, and the balance is distilled water.
其中,所述盐酸为130ml/L配置方式如下:每L金相化学抛光液中加入质量分数36~38%的浓盐酸130ml。Wherein, the hydrochloric acid is 130ml/L and the configuration is as follows: 130ml of concentrated hydrochloric acid with a mass fraction of 36-38% is added to each L of metallographic chemical polishing solution.
所述磷酸160ml/L配置方式如下:每L金相化学抛光液中加入浓度为质量分数≥85%的浓磷酸160ml。The configuration method of the phosphoric acid 160ml/L is as follows: 160ml of concentrated phosphoric acid with a concentration of ≥85% by mass is added to each L of the metallographic chemical polishing solution.
所述30%过氧化氢280ml/L配置方式如下:每L金相化学抛光液中加入质量分数30%的过氧化氢280ml。The configuration method of the 30% hydrogen peroxide 280ml/L is as follows: 280ml of hydrogen peroxide with a mass fraction of 30% is added to each L of metallographic chemical polishing liquid.
所述盐酸抑雾剂为园泰YT-1101型。The hydrochloric acid fog inhibitor is Yuantai YT-1101 type.
本实施例中,还提供所述金相化学抛光液的配制方法,以100ml溶液配制为例,包括以下步骤:In this embodiment, a preparation method of the metallographic chemical polishing solution is also provided, taking the preparation of 100ml solution as an example, including the following steps:
步骤一:分别用量筒量取蒸馏水29ml~36ml、无水乙醇10ml和30%体积分数的过氧化氢30ml,倒入烧杯内;Step 1: Measure 29ml-36ml of distilled water, 10ml of absolute ethanol and 30ml of hydrogen peroxide with a volume fraction of 30% with a measuring cylinder, and pour them into a beaker;
步骤二:分别用量筒量取浓盐酸12~16ml和浓磷酸12~16ml,分别加入烧杯内,加入后用搅拌均匀;Step 2: Measure 12-16ml of concentrated hydrochloric acid and 12-16ml of concentrated phosphoric acid with a measuring cylinder, respectively, add them into the beaker, and stir them evenly after adding;
步骤三:分别用天平称取硝酸钠5~7g,加入烧杯内,搅拌均匀至完全溶解;Step 3: Weigh 5-7 g of sodium nitrate with a balance, add it into a beaker, and stir until it is completely dissolved;
步骤四:分别用天平称取硫脲0.5g和盐酸抑雾剂0.1g,加入烧杯内,搅拌均匀。Step 4: Weigh 0.5 g of thiourea and 0.1 g of hydrochloric acid fog suppressant with a balance, add them into a beaker, and stir evenly.
实施例2Example 2
本实施例中,提供又一种金相化学抛光液,所述金相化学抛光液中各原料及配比如下:盐酸130ml/L、磷酸160ml/L、硝酸钠50g/L、30%过氧化氢280ml/L、无水乙醇110ml/L、硫脲6g/L、盐酸抑雾剂0.8g/L、余量为蒸馏水。In this embodiment, another metallographic chemical polishing solution is provided. The raw materials and proportions of the metallographic chemical polishing solution are as follows: hydrochloric acid 130ml/L, phosphoric acid 160ml/L, sodium nitrate 50g/L, 30% peroxide Hydrogen 280ml/L, absolute ethanol 110ml/L, thiourea 6g/L, hydrochloric acid fog suppressant 0.8g/L, and the balance is distilled water.
所述盐酸抑雾剂为园泰YT-1101型。The hydrochloric acid fog inhibitor is Yuantai YT-1101 type.
所述金相化学抛光液配置方法同实施例1记载。The preparation method of the metallographic chemical polishing solution is the same as that described in Example 1.
实施例3Example 3
本实施例中,提供又一种金相化学抛光液,所述金相化学抛光液中各原料及配比如下:盐酸150ml/L、磷酸120ml/L、硝酸钠70g/L、30%过氧化氢310ml/L、无水乙醇80ml/L、硫脲4g/L、盐酸抑雾剂1.2g/L、余量为蒸馏水。In this embodiment, another metallographic chemical polishing solution is provided. The raw materials and proportions of the metallographic chemical polishing solution are as follows: hydrochloric acid 150ml/L, phosphoric acid 120ml/L, sodium nitrate 70g/L, 30% peroxide Hydrogen 310ml/L, absolute ethanol 80ml/L, thiourea 4g/L, hydrochloric acid fog suppressant 1.2g/L, and the balance is distilled water.
所述盐酸抑雾剂为园泰YT-1101型。The hydrochloric acid fog inhibitor is Yuantai YT-1101 type.
所述金相化学抛光液配置方法同实施例1记载。The preparation method of the metallographic chemical polishing solution is the same as that described in Example 1.
实施例4Example 4
本实施例中,提供一种金相化学抛光液,所述金相化学抛光液中各成分及配比如下:盐酸130ml/L、磷酸160ml/L、硝酸钠50g/L、30%过氧化氢280ml/L、硫脲6g/L、盐酸抑雾剂0.8g/L、余量为蒸馏水。In this embodiment, a metallographic chemical polishing solution is provided. The components and proportions of the metallographic chemical polishing solution are as follows: hydrochloric acid 130ml/L, phosphoric acid 160ml/L, sodium nitrate 50g/L, 30% hydrogen peroxide 280ml/L, thiourea 6g/L, hydrochloric acid fog suppressant 0.8g/L, and the balance is distilled water.
将配置完成的实施例1-4中所述金相化学抛光液装入塑料瓶中密封,放置于室温条件下保存,每隔10天对所述金相化学抛光液的pH值进行检测,pH检测结果及抛光液外观结果如下表1所示:The metallographic chemical polishing solution described in the configured examples 1-4 was put into a plastic bottle and sealed, placed at room temperature for preservation, and the pH value of the metallographic chemical polishing solution was detected every 10 days. The test results and the appearance results of the polishing liquid are shown in Table 1 below:
表1实施例1-4中所述金相化学抛光液稳定性检测结果The results of stability testing of metallographic chemical polishing solutions described in Table 1 Examples 1-4
实施例5Example 5
本实施例中,采用实施例1中配置得到的金相化学抛光液对18Cr-8Ni型奥氏体不锈钢进行抛光处理,包括以下步骤:In this embodiment, the 18Cr-8Ni type austenitic stainless steel is polished with the metallographic chemical polishing solution configured in Embodiment 1, including the following steps:
(1)按照要求的比例配置好化学抛光液;(1) Prepare the chemical polishing liquid according to the required proportion;
(2)用镊子夹住脱脂棉,蘸取3~5ml化学抛光液,在待检不锈钢金相磨面上均匀用力擦拭,不断观察试样表面划痕变化情况;(2) Hold absorbent cotton with tweezers, dip 3-5ml of chemical polishing solution, wipe evenly and forcefully on the metallographic surface of the stainless steel to be inspected, and constantly observe the change of scratches on the surface of the sample;
(3)擦拭时间控制在20~30s,当观察到金相磨面的划痕逐渐消失,用无水酒精将金相磨面冲洗干净并吹干。(3) The wiping time is controlled at 20-30s. When the scratches on the metallographic grinding surface are observed to disappear gradually, rinse the metallographic grinding surface with anhydrous alcohol and dry it.
抛光处理后的不锈钢表面如附图1所示,从图1a可以看出,仅实施例1中所述金相抛光液处理后的奥氏体不锈钢表面侵蚀平整、清晰,无凹凸不平等现象。图1b为采用实施例1中所述化学抛光液抛光并侵蚀后的金相表面,图1c为仅采用机械抛光并侵蚀后的金相表面。对比图1b和图1c可以看出,采用本发明抛光液抛光并侵蚀后获得的金相表面与机械抛光并侵蚀后获得的金相表面效果相当,证明该抛光液抛光效果基本可以媲美机械抛光效果,而机械抛光受工作场地和器械的限制应用有限,本发明中提供的化学抛光液则很好的弥补了该缺陷。The polished stainless steel surface is shown in Figure 1. It can be seen from Figure 1a that only the surface of the austenitic stainless steel treated with the metallographic polishing solution described in Example 1 is eroded flat and clear, without unevenness. Fig. 1b shows the metallographic surface after polishing and etching with the chemical polishing liquid described in Example 1, and Fig. 1c shows the metallographic surface after only mechanical polishing and etching. Comparing Fig. 1b and Fig. 1c, it can be seen that the metallographic surface obtained after polishing and eroding with the polishing liquid of the present invention is equivalent to the metallographic surface obtained after mechanical polishing and etching, which proves that the polishing effect of the polishing liquid is basically comparable to that of mechanical polishing. , and the mechanical polishing is limited by the work site and equipment, and the chemical polishing liquid provided in the present invention can make up for this defect very well.
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.
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EP0193239A1 (en) * | 1985-03-04 | 1986-09-03 | SOLVAY & Cie (Société Anonyme) | Compositions and process for chemically polishing steel surfaces |
CN104372342A (en) * | 2014-11-25 | 2015-02-25 | 湖北第二师范学院 | Chemical stainless steel polishing solution |
CN105714299A (en) * | 2016-03-28 | 2016-06-29 | 华南理工大学 | Chemical polishing liquid used for metal and polishing technology |
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EP0193239A1 (en) * | 1985-03-04 | 1986-09-03 | SOLVAY & Cie (Société Anonyme) | Compositions and process for chemically polishing steel surfaces |
CN104372342A (en) * | 2014-11-25 | 2015-02-25 | 湖北第二师范学院 | Chemical stainless steel polishing solution |
CN105714299A (en) * | 2016-03-28 | 2016-06-29 | 华南理工大学 | Chemical polishing liquid used for metal and polishing technology |
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