CN102021570B - Treatment Method of SiO2 Coating/Ni-Si Alloyed Layer Composite Structure on Cold Rolled Low Carbon Steel Sheet Surface - Google Patents
Treatment Method of SiO2 Coating/Ni-Si Alloyed Layer Composite Structure on Cold Rolled Low Carbon Steel Sheet Surface Download PDFInfo
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Abstract
本发明涉及一种冷轧低碳钢板表面形成SiO2涂层/Ni-Si合金化层复合结构的处理方法，属金属表面处理技术领域。本发明的特点是利用纳米SiO2粉体和纳米Ni(OH)2粉体喷涂到冷轧低碳钢板表面进行加氢还原热处理；热处理温度为450～700℃通入H2的流量为100～200ml/min；最终在冷轧低碳钢板表面获得SiO2涂层/Ni-Si合金化层复合结构。经本发明方法处理过的冷轧低碳钢板，其耐蚀性有明显提高。The invention relates to a treatment method for forming a SiO2 coating/Ni-Si alloyed layer composite structure on the surface of a cold-rolled low-carbon steel plate, belonging to the technical field of metal surface treatment. The feature of the present invention is to use nano- SiO2 powder and nano-Ni(OH) 2 powder to spray on the surface of cold-rolled low - carbon steel plate to carry out hydrogenation reduction heat treatment; the heat treatment temperature is 450-700 ° C, and the flow rate of H 200ml/min; finally obtain SiO 2 coating/Ni-Si alloyed layer composite structure on the surface of cold-rolled low-carbon steel plate. The corrosion resistance of the cold-rolled low-carbon steel plate treated by the method of the invention is obviously improved.
Description
技术领域 technical field
本发明涉及一种冷轧低碳钢板表面形成SiO2涂层/Ni-Si合金化层复合结构的处理方法，属于金属表面处理技术领域。 The invention relates to a treatment method for forming a SiO2 coating/Ni-Si alloyed layer composite structure on the surface of a cold-rolled low-carbon steel plate, belonging to the technical field of metal surface treatment.
背景技术 Background technique
金属腐蚀给世界各国的国民经济带来了巨大的经济损失，我国每年由于腐蚀造成的经济损失约占当年国民生产总值的3～5%。目前常见的防腐技术有合理选材、表面保护(包括金属镀层和非金层涂层) 、环境介质处理、电化学保护和防腐蚀设计等。 Metal corrosion has brought huge economic losses to the national economies of all countries in the world. The annual economic losses caused by corrosion in my country account for about 3-5% of the gross national product of the year. At present, common anti-corrosion technologies include reasonable material selection, surface protection (including metal plating and non-gold coating), environmental medium treatment, electrochemical protection, and anti-corrosion design.
20世纪80年代，被列入世界10项关键技术之一的表面技术，经过20余年的发展，已成为一门新兴的、跨学科的、综合性强的先进基础与工程技术，形成支撑当今技术革新与技术革命发展的重要因素。在金属表面制备无机物涂层技术是近年来备受关注的金属表面处理方法,也是金属防腐技术研究的热点。利用该技术可在金属基体表面制备一层连续致密、化学惰性好的无机物涂层,以此来提高基体的抗氧化性、耐腐蚀性。人们在对TiO2 、SiO2 、ZrO2 和Al2O3 等单元体系涂层作了大量研究，它们被证明具有良好的抗氧化、耐腐蚀性能。现在人们将焦点逐渐转移到多元体系涂层上，认为多元的体系涂层与基体的结合性、抗氧化性、耐腐蚀性比单元体系涂层有较大的改善。 In the 1980s, surface technology was listed as one of the world's 10 key technologies. After more than 20 years of development, it has become an emerging, interdisciplinary, and comprehensive advanced foundation and engineering technology, forming a support for today's technology. An important factor in the development of innovation and technological revolution. The preparation of inorganic coatings on metal surfaces is a metal surface treatment method that has attracted much attention in recent years, and it is also a hot spot in the research of metal anti-corrosion technology. This technology can be used to prepare a layer of continuous dense and chemically inert inorganic coating on the surface of the metal substrate, so as to improve the oxidation resistance and corrosion resistance of the substrate. People have done a lot of research on the unit system coatings such as TiO 2 , SiO 2 , ZrO 2 and Al 2 O 3 , and they have been proved to have good oxidation resistance and corrosion resistance. Now people are gradually shifting the focus to multi-system coatings, and believe that the combination of multi-system coatings and substrates, oxidation resistance, and corrosion resistance are greatly improved compared with unit system coatings.
此外金属表面合金化也是一种重要的金属表面处理方法。金属表面合金化是指通过扩散将一些合金元素如Cr、Al、V、Ti、B、C、Zn等单一的或复合的渗入到各种金属基体或工模具的表面，获得与基体具有冶金结合的各种特殊的化合物层，从而赋予零件与工模具表面以高硬度、高耐磨性、耐蚀性、耐高温氧化性及一些特殊的电学、光学特性。金属表面合金化按实现手段可分为：1、改变金属表面的合金成分。2、金属表面覆盖技术。3、改善金属表面的金相组织，使表层组织强化。 In addition, metal surface alloying is also an important metal surface treatment method. Metal surface alloying refers to the infiltration of some alloying elements such as Cr, Al, V, Ti, B, C, Zn, etc. into the surface of various metal substrates or tools and molds by diffusion, so as to obtain a metallurgical bond with the substrate. Various special compound layers, so as to endow the surface of parts and tools with high hardness, high wear resistance, corrosion resistance, high temperature oxidation resistance and some special electrical and optical properties. Metal surface alloying can be divided into: 1. Change the alloy composition of the metal surface. 2. Metal surface covering technology. 3. Improve the metallographic structure of the metal surface and strengthen the surface structure.
冷轧低碳钢属于碳素结构钢，由于其生产工艺简单、价格低廉、工艺性能良好，在机械制造业中得到广泛的应用。在冷轧钢板退火过程中，钢中的Mn、Si等元素会向钢板表面迁移，与环境中微量的氧化性气体发生反应，在钢板表面铁素体晶界周围形成颗粒状氧化物。在退火后的冷却过程中，当钢板表面接触到空气时,表面没有颗粒氧化物的地方会形成薄层的氧化铁膜。相关研究表明:冷轧钢板表面耐蚀性能与Mn、Si等元素在冷轧钢板表面的富集程度有关。 Cold-rolled low-carbon steel belongs to carbon structural steel. Because of its simple production process, low price and good process performance, it is widely used in machinery manufacturing industry. During the annealing process of cold-rolled steel sheets, elements such as Mn and Si in the steel will migrate to the surface of the steel sheet, react with trace oxidizing gases in the environment, and form granular oxides around the ferrite grain boundaries on the surface of the steel sheet. During the cooling process after annealing, when the surface of the steel plate is in contact with air, a thin layer of iron oxide film will be formed on the surface where there is no particle oxide. Relevant studies have shown that the surface corrosion resistance of cold-rolled steel sheets is related to the enrichment of Mn, Si and other elements on the surface of cold-rolled steel sheets.
纳米科技的发展为提升传统产业技术含量提供了新的机遇。纳米粒子由于具有表面效应、小尺寸效应、量子尺寸效应、宏观量子隧道效应等特殊效应，可用于改善材料的光、磁、电、力学等性能得到提高或赋予其新的功能，可以大大提高其在应用领域中的产品质量，具有很好的理论研究价值和应用前景。此外，随着技术进步，纳米粉体及膜层的制备成本也大幅度下降，为纳米技术大规模应用奠定了扎实的物质基础。 The development of nanotechnology provides new opportunities for upgrading the technical content of traditional industries. Due to special effects such as surface effects, small size effects, quantum size effects, and macroscopic quantum tunneling effects, nanoparticles can be used to improve the optical, magnetic, electrical, and mechanical properties of materials to improve or endow them with new functions, which can greatly improve their properties. The product quality in the application field has very good theoretical research value and application prospect. In addition, with the advancement of technology, the preparation cost of nanopowder and film layer has also been greatly reduced, laying a solid material foundation for the large-scale application of nanotechnology.
在前人研究基础上，本发明紧密结合金属表面制备无机物涂层技术、钢板表面合金化、纳米科技等的热点研究领域，通过制备性能、品质、价格适当，并能够有效融入铁基固溶体的金属及其相应化合物微/纳米尺度的颗粒或膜层，将上述粉体颗粒或膜层喷涂或轧压于冷轧低碳钢表面，在强还原气氛下将部分被还原出的金属融入铁基固溶体，或将金属的相应化合物还原为金属富集于钢板表面，并保留一定的无机物涂层，以获得无机物涂层/合金化层复合的冷轧低碳钢表面层结构，以期获得良好的耐腐蚀性能以及改善其它相关的物理和化学性能。 On the basis of previous studies, the present invention is closely combined with hot research fields such as metal surface preparation inorganic coating technology, steel plate surface alloying, nanotechnology, etc., through the preparation performance, quality, price is appropriate, and can be effectively integrated into iron-based solid solution Micro/nanoscale particles or films of metals and their corresponding compounds. The above powder particles or films are sprayed or rolled on the surface of cold-rolled low-carbon steel, and part of the reduced metals are incorporated into the iron matrix under a strong reducing atmosphere. solid solution, or reduce the corresponding compound of the metal to metal enrichment on the surface of the steel plate, and retain a certain inorganic coating to obtain the surface layer structure of cold-rolled low-carbon steel composited with inorganic coating/alloying layer, in order to obtain a good Corrosion resistance and improve other related physical and chemical properties.
发明内容 Contents of the invention
本发明的目的是提提供一种冷轧低碳钢板表面形成SiO2涂层/Ni-Si合金化层复合结构的处理方法，它有效地增强冷轧低碳钢板的耐腐蚀性能。 The purpose of this invention is to provide a kind of cold-rolled low-carbon steel plate surface to form SiO 2 coating/Ni-Si alloyed layer composite structure processing method, it effectively enhances the corrosion resistance of cold-rolled low-carbon steel plate.
本发明一种冷轧低碳钢板表面形成SiO2涂层/Ni-Si合金化层复合结构的处理方法，其特征在于具有以下的过程和步骤： A kind of cold-rolled low-carbon steel plate surface of the present invention forms the processing method of SiO coating /Ni-Si alloyed layer composite structure, it is characterized in that having following process and step:
a、冷轧低碳钢板表面的预处理：将欲处理的冷轧低碳钢板经无水乙醇、丙酮依次清洗后，干燥，放置于干燥器备用； a. Pretreatment of the surface of the cold-rolled low-carbon steel plate: After the cold-rolled low-carbon steel plate to be treated is washed with absolute ethanol and acetone in sequence, dried, and placed in a desiccator for standby;
b、配置纳米SiO2- Ni(OH)2复合液，复合液的配方如下： b. Configure nano-SiO 2 -Ni(OH) 2 compound solution, the formula of the compound solution is as follows:
纳米SiO2粉体 6～20g/L，粒径为40～90nm； Nano SiO 2 powder 6~20g/L, particle size 40~90nm;
纳米Ni(OH)2粉体 1～8g/L，粒径为70～120nm； Nano Ni(OH) 2 powder 1~8g/L, particle size 70~120nm;
乙醇:丁醇 1:5～8（体积比）； Ethanol:butanol 1:5～8 (volume ratio);
将预先制备的纳米SiO2粉体和纳米Ni(OH)2粉体加入到乙醇与丁醇的混合液当中，然后超声分散30min； Add the pre-prepared nano- SiO2 powder and nano-Ni(OH) 2 powder into the mixture of ethanol and butanol, and then ultrasonically disperse for 30min;
c. 将上述配制好的纳米SiO2- Ni(OH)2复合液喷涂到上述冷轧低碳钢板表面，自然风干；SiO2- Ni(OH)2复合纳米涂层厚度为1～10μm； c. Spray the above-mentioned prepared nano-SiO 2 -Ni(OH) 2 composite liquid onto the surface of the above-mentioned cold-rolled low-carbon steel plate, and let it dry naturally; the thickness of the SiO 2 -Ni(OH) 2 composite nano-coating is 1-10 μm;
d. 将上述表面负载有SiO2- Ni(OH)2复合纳米涂层的冷轧低碳钢板在管式炉中进行通H2还原热处理；还原热处理工艺参数为： d. The above-mentioned cold-rolled low-carbon steel plate with SiO 2 -Ni(OH) 2 composite nano-coating on the surface is carried out in a tube furnace through H 2 reduction heat treatment; the reduction heat treatment process parameters are:
温度： 450～700℃ Temperature: 450～700℃
升温梯度： 2～10℃/min Heating gradient: 2～10℃/min
保温时间： 2～8h Holding time: 2～8h
降温方式： 空冷 Cooling method: Air cooling
H2气流量为： 100～300mL/min H2 gas flow: 100～300mL/min
最终在钢板表面形成SiO2涂层/Ni-Si合金化层复合结构。 Finally, a composite structure of SiO 2 coating/Ni-Si alloying layer is formed on the surface of the steel plate.
本发明的特点：本发明的特点在于利用纳米SiO2粉体和纳米Ni(OH)2粉体喷涂到冷轧低碳钢板表面进行还原热处理，使得冷轧低碳钢板表面获得SiO2涂层/Ni-Si合金化层复合结构，可利用冷轧钢板生产工序中的全氢罩式退火工艺，实现大规模连续工业化生产，提高冷轧低碳钢板的耐腐蚀性能。 Features of the present invention: the feature of the present invention is to utilize nano- SiO2 powder and nano-Ni(OH) 2 powder to spray on the surface of cold-rolled low-carbon steel plate and carry out reduction heat treatment, so that the surface of cold-rolled low-carbon steel plate obtains SiO2coating / The Ni-Si alloyed layer composite structure can utilize the full hydrogen bell annealing process in the production process of cold-rolled steel sheets to realize large-scale continuous industrial production and improve the corrosion resistance of cold-rolled low-carbon steel sheets.
具体实施方式 Detailed ways
现将本发明的具体实施叙述于后。 Now the concrete implementation of the present invention is described in the following.
实施例1：取冷轧低碳钢板10×20×1.5mm若干片，表面用金相砂纸打磨，经无水乙醇、丙酮依次清洗后，干燥，放置于干燥器中备用。 Example 1: Take cold-rolled low-carbon steel sheets of 10×20×1.5 mm, polish the surface with metallographic sandpaper, wash them in sequence with absolute ethanol and acetone, dry them, and place them in a desiccator for later use.
纳米SiO2- Ni(OH)2复合液成分为：纳米SiO2粉体13g/L，纳米Ni(OH)2粉体4g/L，乙醇:丁醇=1:5。超声分散该复合液30min。将配制好的纳米SiO2- Ni(OH)2复合液喷涂到冷轧低碳钢板表面，自然风干，SiO2- Ni(OH)2复合纳米涂层厚度为3μm。将表面负载有SiO2- Ni(OH)2复合纳米涂层的冷轧低碳钢板在管式炉中进行还原热处理，还原热处理工艺参数为：温度为680℃，升温梯度为3℃/min，保温时间为6h，降温梯度为空冷，H2气流量为160mL/min。 Nano-SiO 2 -Ni(OH) 2 composite solution consists of: nano-SiO 2 powder 13g/L, nano-Ni(OH) 2 powder 4g/L, ethanol:butanol=1:5. Ultrasonic dispersion of the complex solution for 30min. Spray the prepared nano-SiO 2 -Ni(OH) 2 composite liquid onto the surface of cold-rolled low-carbon steel plate, and let it dry naturally. The thickness of the SiO 2 -Ni(OH) 2 composite nano-coating is 3 μm. The cold-rolled low-carbon steel plate loaded with SiO 2 - Ni(OH) 2 composite nano-coating on the surface was subjected to reduction heat treatment in a tube furnace. The reduction heat treatment process parameters were: temperature 680°C, temperature gradient 3°C/min, The holding time is 6h, the cooling gradient is air cooling, and the H2 gas flow rate is 160mL/min.
将表面获得SiO2涂层/Ni-Si合金化层复合结构的冷轧低碳钢板进行盐雾实验，测得耐盐雾时间；同时浸泡在5%氯化钠溶液中30min后，测试其极化曲线，测得腐蚀电流密度。测试结果见表1.。 The cold-rolled low-carbon steel plate with SiO 2 coating/Ni-Si alloyed layer composite structure on the surface was subjected to salt spray test, and the salt spray resistance time was measured; at the same time, after soaking in 5% sodium chloride solution for 30 minutes, the extreme The corrosion curve was used to measure the corrosion current density. The test results are shown in Table 1..
实施例2：按照实施例1的方法制备冷轧低碳钢板样品。 Embodiment 2: Prepare a cold-rolled low-carbon steel plate sample according to the method of Embodiment 1.
纳米SiO2- Ni(OH)2复合液成分为：纳米SiO2粉体17g/L，纳米Ni(OH)2粉体5g/L，乙醇:丁醇=1:5。超声分散该复合液30min。将配制好的纳米SiO2- Ni(OH)2复合液喷涂到冷轧低碳钢板表面，自然风干，SiO2- Ni(OH)2复合纳米涂层厚度为3μm。将表面负载有SiO2- Ni(OH)2复合纳米涂层的冷轧低碳钢板在管式炉中进行还原热处理，还原热处理工艺参数为：温度为680℃，升温梯度为3℃/min，保温时间为6h，降温梯度为空冷，H2气流量为160mL/min。 Nano-SiO 2 -Ni(OH) 2 composite solution consists of: nano-SiO 2 powder 17g/L, nano-Ni(OH) 2 powder 5g/L, ethanol:butanol=1:5. Ultrasonic dispersion of the complex solution for 30min. Spray the prepared nano-SiO 2 -Ni(OH) 2 composite liquid onto the surface of cold-rolled low-carbon steel plate, and let it dry naturally. The thickness of the SiO 2 -Ni(OH) 2 composite nano-coating is 3 μm. The cold-rolled low-carbon steel plate loaded with SiO 2 - Ni(OH) 2 composite nano-coating on the surface was subjected to reduction heat treatment in a tube furnace. The reduction heat treatment process parameters were: temperature 680°C, temperature gradient 3°C/min, The holding time is 6h, the cooling gradient is air cooling, and the H2 gas flow rate is 160mL/min.
样品的耐腐蚀性能测试按照实施例1的方法进行。测试结果见表1.。 The corrosion resistance test of the samples was carried out according to the method of Example 1. The test results are shown in Table 1..
实施例3：按照实施例1的方法制备冷轧低碳钢板样品。 Embodiment 3: A cold-rolled low-carbon steel plate sample was prepared according to the method of Embodiment 1.
纳米SiO2- Ni(OH)2复合液成分为：纳米SiO2粉体13g/L，纳米Ni(OH)2粉体5g/L，乙醇:丁醇=1:5。超声分散该复合液30min。将配制好的纳米SiO2- Ni(OH)2复合液喷涂到冷轧低碳钢板表面，自然风干，SiO2- Ni(OH)2复合纳米涂层厚度为3μm。将表面负载有SiO2- Ni(OH)2复合纳米涂层的冷轧低碳钢板在管式炉中进行还原热处理，还原热处理工艺参数为：温度为450℃，升温梯度为3℃/min，保温时间为6h，降温梯度为空冷，H2气流量为160mL/min。 Nano-SiO 2 -Ni(OH) 2 composite solution consists of: nano-SiO 2 powder 13g/L, nano-Ni(OH) 2 powder 5g/L, ethanol:butanol=1:5. Ultrasonic dispersion of the complex solution for 30min. Spray the prepared nano-SiO 2 -Ni(OH) 2 composite liquid onto the surface of cold-rolled low-carbon steel plate, and let it dry naturally. The thickness of the SiO 2 -Ni(OH) 2 composite nano-coating is 3 μm. The cold-rolled low-carbon steel plate loaded with SiO 2 - Ni(OH) 2 composite nano-coating on the surface was subjected to reduction heat treatment in a tube furnace. The reduction heat treatment process parameters were: temperature 450 °C, temperature gradient 3 °C/min The holding time is 6h, the cooling gradient is air cooling, and the H2 gas flow rate is 160mL/min.
样品的耐腐蚀性能测试按照实施例1的方法进行。测试结果见表1.。 The corrosion resistance test of the samples was carried out according to the method of Example 1. The test results are shown in Table 1..
实施例4：按照实施例1的方法制备冷轧低碳钢板样品。 Embodiment 4: According to the method of Embodiment 1, a cold-rolled low-carbon steel plate sample was prepared.
纳米SiO2- Ni(OH)2复合液成分为：纳米SiO2粉体13g/L，纳米Ni(OH)2粉体5g/L，乙醇:丁醇=1:8。超声分散该复合液30min。将配制好的纳米SiO2- Ni(OH)2复合液喷涂到冷轧低碳钢板表面，自然风干，SiO2- Ni(OH)2复合纳米涂层厚度为3μm。将表面负载有SiO2- Ni(OH)2复合纳米涂层的冷轧低碳钢板在管式炉中进行还原热处理，还原热处理工艺参数为：温度为450℃，升温梯度为3℃/min，保温时间为6h，降温梯度为空冷，H2气流量为160mL/min。 Nano-SiO 2 -Ni(OH) 2 composite solution consists of: nano-SiO 2 powder 13g/L, nano-Ni(OH) 2 powder 5g/L, ethanol:butanol=1:8. Ultrasonic dispersion of the complex solution for 30min. Spray the prepared nano-SiO 2 -Ni(OH) 2 composite liquid onto the surface of cold-rolled low-carbon steel plate, and let it dry naturally. The thickness of the SiO 2 -Ni(OH) 2 composite nano-coating is 3 μm. The cold-rolled low-carbon steel plate loaded with SiO 2 - Ni(OH) 2 composite nano-coating on the surface was subjected to reduction heat treatment in a tube furnace. The reduction heat treatment process parameters were: temperature 450 °C, temperature gradient 3 °C/min The holding time is 6h, the cooling gradient is air cooling, and the H2 gas flow rate is 160mL/min.
样品的耐腐蚀性能测试按照实施例1的方法进行。测试结果见表1.。 The corrosion resistance test of the samples was carried out according to the method of Example 1. The test results are shown in Table 1..
实施例5：按照实施例1的方法制备冷轧低碳钢板样品。 Embodiment 5: According to the method of Embodiment 1, a cold-rolled low-carbon steel plate sample was prepared.
纳米SiO2- Ni(OH)2复合液成分为：纳米SiO2粉体13g/L，纳米Ni(OH)2粉体5g/L，乙醇:丁醇=1:5。超声分散该复合液30min。将配制好的纳米SiO2- Ni(OH)2复合液喷涂到冷轧低碳钢板表面，自然风干，SiO2- Ni(OH)2复合纳米涂层厚度为2μm。将表面负载有SiO2- Ni(OH)2复合纳米涂层的冷轧低碳钢板在管式炉中进行还原热处理，还原热处理工艺参数为：温度为680℃，升温梯度为3℃/min，保温时间为4h，降温梯度为空冷，H2气流量为160mL/min。 Nano-SiO 2 -Ni(OH) 2 composite solution consists of: nano-SiO 2 powder 13g/L, nano-Ni(OH) 2 powder 5g/L, ethanol:butanol=1:5. Ultrasonic dispersion of the complex solution for 30min. Spray the prepared nano-SiO 2 -Ni(OH) 2 composite liquid onto the surface of cold-rolled low-carbon steel plate, and let it dry naturally. The thickness of the SiO 2 -Ni(OH) 2 composite nano-coating is 2 μm. The cold-rolled low-carbon steel plate loaded with SiO 2 - Ni(OH) 2 composite nano-coating on the surface was subjected to reduction heat treatment in a tube furnace. The reduction heat treatment process parameters were: temperature 680°C, temperature gradient 3°C/min, The holding time is 4 hours, the cooling gradient is air cooling, and the H2 gas flow rate is 160mL/min.
样品的耐腐蚀性能测试按照实施例1的方法进行。测试结果见表1.。 The corrosion resistance test of the samples was carried out according to the method of Example 1. The test results are shown in Table 1..
表1. 不同处理条件下获得的冷轧低碳钢板样品的耐腐蚀性能测试结果 Table 1. Corrosion resistance test results of cold-rolled low-carbon steel plate samples obtained under different treatment conditions
实例证明利用本发明技术处理过的冷轧低碳钢板表面的腐蚀电流密度较低，盐雾试验时间较长，说明经过本发明的表面处理方法可使其耐腐蚀性能大大提高。 Examples prove that the corrosion current density on the surface of the cold-rolled low-carbon steel plate treated by the technology of the present invention is low, and the salt spray test time is long, which shows that the surface treatment method of the present invention can greatly improve its corrosion resistance.
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