WO2016201936A1 - 不锈钢制品表面的一种钝化方法 - Google Patents

不锈钢制品表面的一种钝化方法 Download PDF

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WO2016201936A1
WO2016201936A1 PCT/CN2015/098071 CN2015098071W WO2016201936A1 WO 2016201936 A1 WO2016201936 A1 WO 2016201936A1 CN 2015098071 W CN2015098071 W CN 2015098071W WO 2016201936 A1 WO2016201936 A1 WO 2016201936A1
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stainless steel
passivation
steel product
citric acid
deionized water
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PCT/CN2015/098071
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English (en)
French (fr)
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马迪
李树白
李申
刘怀亮
贾传奇
张洋
狄爱俊
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海安县申菱电器制造有限公司
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    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/50—Treatment of iron or alloys based thereon

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  • the invention belongs to the technical field of stainless steel surface treatment, and in particular relates to a passivation treatment method for a stainless steel surface.
  • the stainless steel surface has a very hard oxide layer and is more difficult to remove than the oxide layer on the surface of steel.
  • various stainless steel pickling passivation pastes, pickling passivation solutions, and so on have been developed at home and abroad. They are all used to remove the oxide layer on the surface of stainless steel at room temperature and form a passivation protective film on the surface, but their passivation effect and use method are not ideal.
  • the main problems are as follows: pickling passivation paste and pickling passivation solution use a large amount of raw materials such as hydrofluoric acid, sulfuric acid, hydrochloric acid, sodium chloride, sodium alkylbenzene sulfonate, etc. Fluorine, chlorine, sulfur, sodium lamp elements can cause damage to stainless steel. If the cleaning is not clean, then in the future they will cause various types of corrosion of the stainless steel, resulting in cracking, fatigue cracking and the like of the stainless steel product.
  • the stainless steel surface passivation treatment technology is an effective method for forming a dense and uniform film layer on the surface to block the penetration and diffusion of the external corrosive medium, thereby slowing down the corrosion rate.
  • the traditional chromium salt passivation process and the strong oxidation passivation process are mature, there are serious environmental pollution problems, and even more harmful to the human body. Therefore, it is extremely urgent to find a safe and efficient stainless steel passivator to solve the above problems.
  • molybdic acid type, phytic acid type, rare earth type and citric acid type passivating agent have been studied.
  • the molybdic acid type passivating agent proposed by Chinese patent CN102762769 the tantalum type passivating agent disclosed by CN1326012A, and the citric acid type passivating agent disclosed by CN1412348A and CN101748400A.
  • the citric acid type passivation agent is gradually favored by people because of its simple process, low price, high efficiency and environmental protection.
  • the temperature of the citric acid type passivation process disclosed in CN1412348A reaches 70-80 ° C, which makes the energy consumption higher.
  • the passivation solution is composed of citric acid (40-110 g/L) and CZ-1A (10-30 g/L).
  • the reagent content is too high and the passivation process is somewhat complicated.
  • the citric acid type passivation process disclosed in CN101748400A has a simple composition of the passivating agent but a high content of the main acid and the oxidizing agent.
  • the object of the present invention is to develop a passivation method for the surface of a non-toxic and harmless stainless steel article.
  • the technical proposal of the invention is that the clean stainless steel product is subjected to purification treatment in a passivation solution composed of deionized water and citric acid, hydrogen peroxide and ethylene glycol.
  • the invention replaces the previous passivation process with strong acid and strong oxidant as the main body by the citric acid type passivation process, and the surface passivation of the stainless steel by the invention does not need to undergo a complicated acid pickling or alkali washing activation process, and only needs to be simple.
  • the oil removal pretreatment can pass through a stainless steel product having an area of about 80 cm 2 per 200 ml of the passivation solution.
  • the passivation process has the advantages of being non-toxic and non-polluting, low in price, and simple in operation.
  • the invention fully meets the requirements of sustainable development, is an environment-friendly passivation process, and the obtained passivation film is dense and uniform, and has strong corrosion resistance.
  • the advantages of the invention are as follows:
  • the passivation liquid obtained by the invention is green and environmentally friendly, and does not contain harmful substances such as strong acid and strong oxidizing agents, and meets the requirements for sustainable development. And the obtained passivation film is dense and uniform, and the corrosion resistance is good.
  • the main body of the passivation liquid of the invention has low content, low price, simple and stable operation process and high efficiency.
  • the method of the present invention has a lower operating temperature than the citric acid type passivating agent proposed by the Chinese patent document CN1412348A on the surface of the stainless steel, and the composition and process of the passivation liquid are also simpler than that of the passivating agent in the Chinese patent document CN101748400A.
  • the body content is even lower.
  • the mass of the citric acid, hydrogen peroxide and ethylene glycol in the passivation solution of the present invention are 0.5 to 2%, 0.5 to 2% and 0.5%, respectively.
  • the concentration range of the passivation solution of this formulation is low, but the passivation effect is good.
  • the deionized water is sequentially dissolved into citric acid, ethylene glycol and hydrogen peroxide in sequence, and after being uniformly stirred, the temperature is closed.
  • the characteristic is that the composition of the passivation liquid is simple, which ensures the stability of hydrogen peroxide.
  • the temperature of the passivation solution is 30 to 60 ° C and the passivation time is 60 to 120 min during the purification treatment.
  • the passivation conditions are mild and can greatly save energy.
  • the stainless steel product is cleaned in a cleaning agent at 65 ° C to obtain a clean stainless steel product, the cleaning agent.
  • a cleaning agent is mainly composed of sodium hydroxide, sulfosalicylic acid, nonionic surfactant NP-10, coconut oil fatty acid diethanolamide and sodium polyphosphate.
  • the present invention In order to remove the deposit on the surface of the film, to ensure that the surface of the stainless steel after passivation is clean, and to improve the appearance quality of the product, and to facilitate subsequent application, the present invention also ultrasonically cleans the purified stainless steel product with deionized water for 2 to 3 minutes, and then Dry by hot air.
  • Fig. 1 is a graph showing the relationship between open circuit potential and time for Examples 1, 2, and 3 and blank samples which were only subjected to pretreatment without passivation.
  • Figure 2 is a Tafel diagram of Examples 1, 2, 3 and blank samples.
  • the 304 stainless steel piece of the cutting rule is ultrasonically cleaned for 6 minutes in a cleaning agent at 65 ° C, and the surface of the steel sheet is sufficiently cleaned during the cleaning process.
  • the cleaning agent composition includes sodium hydroxide, sulfosalicylic acid, nonionic surfactant NP-10, coconut oil fatty acid diethanolamide 6501, sodium polyphosphate, etc., and then the 304 stainless steel piece is placed in deionized water for ultrasonic cleaning 2 -3min, hot air drying, ready to use.
  • citric acid C 6 H 8 O 7 , analytical grade
  • hydrogen peroxide H 2 O 2 , analytical grade
  • ethylene glycol HOCH 2 CH 2 OH, analytical grade
  • the liquefied liquid has 0.5% citric acid, 2% hydrogen peroxide, 0.5% ethylene glycol, and 97% deionized water.
  • the 304 stainless steel piece is placed obliquely into the prepared 40 ° C passivation solution to ensure sufficient contact between the stainless steel piece and the passivation solution. After 60 minutes, the 304 stainless steel piece is taken out.
  • the 304 stainless steel piece is ultrasonically cleaned with deionized water for 2 to 3 minutes, and then dried by hot air to obtain a 304 stainless steel piece with a passivation film.
  • citric acid C 6 H 8 O 7 , analytical grade
  • hydrogen peroxide H 2 O 2 , analytical grade
  • ethylene glycol HOCH 2 CH 2 OH, analytical grade
  • the citric acid has 0.5% citric acid, 0.5% hydrogen peroxide, 0.5% ethylene glycol, and 98.5% deionized water.
  • the stainless steel material is placed obliquely into the prepared 30 ° C passivation solution to ensure sufficient contact between the stainless steel sheet and the passivation solution. After 120 minutes, the stainless steel material is taken out.
  • citric acid C 6 H 8 O 7 , analytical grade
  • hydrogen peroxide H 2 O 2 , analytical grade
  • ethylene glycol HOCH 2 CH 2 OH, analytical grade
  • the liquefied liquid has 0.5% citric acid, 2% hydrogen peroxide, 0.5% ethylene glycol, and 97% deionized water.
  • the general rule of the passivation solution configuration and the temperature required for the passivation in the above examples is that the deionized water is sequentially dissolved in citric acid, ethylene glycol and hydrogen peroxide in sequence, and the mixture is uniformly heated to close the temperature.
  • Figure 1 illustrates that the open circuit potential of the sample after passivation is more positive than the blank sample, indicating that the corrosion resistance is better than the blank sample that has not been passivated.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

不锈钢制品表面的一种钝化方法，将洁净的不锈钢制品置于由去离子水和柠檬酸、双氧水、乙二醇组成的钝化液中进行钝化处理。

Description

不锈钢制品表面的一种钝化方法 技术领域
本发明属于不锈钢表面处理技术领域，具体的说是涉及不锈钢表面的钝化处理方法。
背景技术
不锈钢表面有着一层十分坚硬的氧化皮层，并且比一般钢材表面的氧化层更难以去除，目前国内外已经研制出各种各样的不锈钢酸洗钝化膏，酸洗钝化液，这类产品都是用来在常温下清除不锈钢表面氧化皮层并能在其表面形成一层钝化保护膜的试剂，但是它们的钝化效果及使用方法均不理想。问题主要表现在：酸洗钝化膏及酸洗钝化液等产品都使用了大量的氢氟酸、硫酸、盐酸、氯化钠、烷基苯磺酸钠等原料，这些原料中含有丰富的氟、氯、硫、钠灯元素，都能对不锈钢造成危害。如果清洗不净，那么日后它们便会使不锈钢产生各种类型腐蚀，从而导致不锈钢产品脆裂、疲劳裂等等。
众所周知，不锈钢表面钝化处理技术是一种在其表面生成一层致密均匀、附着力强的薄膜层来阻滞外界腐蚀介质的渗入和扩散，从而达到减缓其腐蚀速度的有效方法。然而传统的铬盐钝化工艺与强氧化型钝化工艺虽工艺技术成熟但普遍都存在着严重的环境污染问题，更甚者还会对人体造成危害。因此找到一种安全、高效的不锈钢钝化剂以解决上述问题迫在眉睫。在寻找环保型钝化剂过程中，人们研究了钼酸型、植酸型、稀土型和柠檬酸型钝化剂等。如中国专利CN102762769提出的钼酸型钝化剂、CN1326012A公布的铈酸型钝化剂和CN1412348A与CN101748400A公布的柠檬酸型钝化剂。其中柠檬酸型钝化剂因其工艺简单、价格低廉、高效环保等特点逐渐受到人们的青睐。CN1412348A公布的柠檬酸型钝化工艺中温度达到70-80℃，使得能耗较高，钝化液有柠檬酸(40-110g/L)、CZ-1A(10-30g/L)组成，主要试剂含量过高且钝化工艺稍显复杂。CN101748400A公布的柠檬酸型钝化工艺虽说钝化剂组成简单但主体酸和氧化剂含量均偏高。
发明内容
本发明的目的在于研究出一种无毒无害的不锈钢制品表面的钝化方法。
本发明的技术方案是：将洁净的不锈钢制品置于由去离子水和柠檬酸、双氧水、乙二醇组成的钝化液中进行纯化处理。
本发明以柠檬酸型钝化工艺来替代之前的以强酸，强氧化剂为主体的钝化工艺，利用本发明进行不锈钢表面钝化时不用经过繁琐酸洗或者碱洗活化过程，只需进行简单的除油预处理即可，每200ml钝化溶液可以钝化面积为80cm2左右的不锈钢制品。
另外此钝化工艺还具有无毒无污染，价格低廉，操作简单等优点。本发明完全符合可持续发展的需求，是一种环境友好型钝化工艺，且得到的钝化膜致密均匀，耐腐蚀性能强。本发明优点如下：
1、本发明得到的钝化液绿色环保，不含强酸、强氧化剂等对环境和人体有害物质，符合可持续发展要求。并且得到的钝化膜致密均匀，耐腐蚀性能好。
2、本发明钝化液主体组成含量低，价格低廉，操作工序简单稳定且效率高。
本发明要比中国专利文献CN1412348A提出的柠檬酸型钝化剂在不锈钢表面形成钝化膜的方法操作温度低，且钝化液组成与工序也更加简单，比中国专利文献CN101748400A中钝化剂的主体含量更加低。
另外，本发明所述钝化液中柠檬酸、双氧水和乙二醇质量分别为0.5～2％、0.5～2％和0.5％。该配方的钝化液的浓度范围虽较低低，但钝化效果良好。
本发明在配制钝化液时，在去离子水先后按顺序溶入柠檬酸、乙二醇和双氧水，经搅拌均匀后封闭升温。特点是：钝化液的成分简单，确保了双氧水的稳定性。
本发明在所述纯化处理时，所述纯化处理时，钝化液的温度为30～60℃，钝化时间为60～120min。该钝化条件温和，可大大节约能耗。
另外，为了取得洁净的不锈钢制品，利于在其表面形成均匀而牢固的钝化效果，本发明超声条件下，将不锈钢制品置于65℃的清洗剂中清洗取得洁净的不锈钢制品，所述清洗剂主要由氢氧化钠、磺基水杨酸、非离子表面活性剂NP-10、椰子油脂肪酸二乙醇酰胺和多聚磷酸钠组成。
为了去除膜层表面附着物，确保钝化后的不锈钢制品表面洁净，提高产品的外观质量，利于后续应用，本发明还以去离子水对纯化处理后的不锈钢制品进行超声清洗2～3min，再经热风烘干。
附图说明
图1为实施例1、2、3和只经过预处理而不经过钝化处理空白试样的开路电位与时间的关系曲线图。
图2为实施例1、2、3和空白试样的塔菲尔图。
具体实施方式
一、纯化实施例：
实施例1：
1、不锈钢表面预处理：
首先将裁剪规则的304不锈钢片放入65℃的清洗剂中超声清洗6min，清洗过程中保证钢片表面要充分清洗。清洗剂组成包括氢氧化钠、磺基水杨酸、非离子表面活性剂NP-10、椰子油脂肪酸二乙醇酰胺6501、多聚磷酸钠等，接着将304不锈钢片放入去离子水中超声清洗2-3min，热风烘干，待用。
2、配置钝化液：
由柠檬酸(C6H8O7，分析纯)、双氧水(H2O2，分析纯)和乙二醇(HOCH2CH2OH，分析纯)按比例溶于去离子水中，形成的钝化液中柠檬酸0.5％，双氧水2％，乙二醇0.5％，去离子水97％。
3、将304不锈钢片斜放入配好的40℃钝化液中，以保证不锈钢片与钝化液的充分接触，经过60min后取出304不锈钢片。
4、常温下将304不锈钢片用去离子水超声清洗2～3min，再经热风烘干后即得具有钝化膜的304不锈钢片，装袋备用。
实施例2：
1、不锈钢表面预处理：取不锈钢材以同实施例1步骤1的方法处理。
2、配置钝化溶液：
由柠檬酸(C6H8O7，分析纯)、双氧水(H2O2，分析纯)和乙二醇(HOCH2CH2OH，分析纯)按比例溶于去离子水中，形成的钝化液中柠檬酸0.5％，双氧水0.5％，乙二醇0.5％，去离子水98.5％。
3、将不锈钢材斜放入配好的30℃钝化液中，以保证不锈钢片与钝化液的充分接触，经过120min后取出不锈钢材。
4、常温下用去离子水超声清洗步骤三钝化后的不锈钢材2～3min，再经热风烘干后即得具有钝化膜的不锈钢材，装袋备用。
实施例3：
1、不锈钢零件表面预处理：取不锈钢零件以同实施例1步骤1的方法处理。
2、配置钝化溶液：
由柠檬酸(C6H8O7，分析纯)、双氧水(H2O2，分析纯)和乙二醇(HOCH2CH2OH，分析纯)按比例溶于去离子水中，形成的钝化液中柠檬酸0.5％，双氧水2％，乙二醇0.5％，去离子水97％。
3、将不锈钢零件浸入配好的60℃钝化液中，经90min后取出不锈钢零件。
4、常温下将不锈钢零件用去离子水超声清洗2～3min，再经热风烘干后即得具有钝化膜的不 锈钢零件，装袋备用。
以上各例中的钝化液配置和达到钝化要求的温度的通则是：在去离子水先后按顺序溶入柠檬酸、乙二醇和双氧水，经搅拌均匀后封闭升温。
二、效果分析：
将以上各例制成的产品和只经过预处理而不经过钝化处理空白试样分别进行试验，取得如图1、2所示的图。
图1说明：经钝化后试样的开路电位比空白试样更正，说明耐蚀性比未经钝化的空白试样好。
在实施例1、2和3的耐蚀性能比较上来看，实施例3的钝化性能较好。
从图2可见：四个试样的耐蚀性能比较为实施例3＞实施例2＞实施例1＞空白。

Claims (6)

  1. 不锈钢制品表面的一种钝化方法，其特征在于：将洁净的不锈钢制品置于由去离子水和柠檬酸、双氧水、乙二醇组成的钝化液中进行纯化处理。
  2. 根据权利要求1所述方法，其特征在于：所述钝化液中柠檬酸、双氧水和乙二醇质量分别为0.5～2％、0.5～2％和0.5％。
  3. 根据权利要求1或2所述方法，其特征在于：在去离子水先后按顺序溶入柠檬酸、乙二醇和双氧水，经搅拌均匀后封闭升温。
  4. 根据权利要求1或2所述方法，其特征在于：所述纯化处理时，钝化液的温度为30～60℃，钝化时间为60～120min。
  5. 根据权利要求1所述方法，其特征在于：超声条件下，将不锈钢制品置于65℃的清洗剂中清洗取得洁净的不锈钢制品，所述清洗剂主要由氢氧化钠、磺基水杨酸、非离子表面活性剂NP-10、椰子油脂肪酸二乙醇酰胺和多聚磷酸钠组成。
  6. 根据权利要求1所述方法，其特征在于：以去离子水对纯化处理后的不锈钢制品进行超声清洗2～3min，再经热风烘干。
PCT/CN2015/098071 2015-06-19 2015-12-21 不锈钢制品表面的一种钝化方法 WO2016201936A1 (zh)

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CN116219420A (zh) * 2022-12-07 2023-06-06 中国石油大学(华东) 一种用于13Cr不锈钢表面处理的钝化液及钝化工艺

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