CN102899644B - Method for obtaining a coating containing micronano SiO2 particles on the surface of aluminum and aluminum alloys - Google Patents
Method for obtaining a coating containing micronano SiO2 particles on the surface of aluminum and aluminum alloys Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 33
- 239000011248 coating agent Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000002245 particle Substances 0.000 title claims abstract description 18
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title abstract description 10
- 229910052681 coesite Inorganic materials 0.000 title abstract description 5
- 229910052906 cristobalite Inorganic materials 0.000 title abstract description 5
- 239000000377 silicon dioxide Substances 0.000 title abstract description 5
- 235000012239 silicon dioxide Nutrition 0.000 title abstract description 5
- 229910052682 stishovite Inorganic materials 0.000 title abstract description 5
- 229910052905 tridymite Inorganic materials 0.000 title abstract description 5
- 238000007747 plating Methods 0.000 claims abstract description 42
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 22
- 239000002105 nanoparticle Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000007772 electroless plating Methods 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005260 corrosion Methods 0.000 claims abstract description 8
- 230000007797 corrosion Effects 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005238 degreasing Methods 0.000 claims abstract description 5
- 238000007598 dipping method Methods 0.000 claims abstract description 5
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 5
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 5
- 239000011701 zinc Substances 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 11
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 10
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 6
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 6
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 6
- 239000001632 sodium acetate Substances 0.000 claims description 6
- 235000017281 sodium acetate Nutrition 0.000 claims description 6
- 239000001509 sodium citrate Substances 0.000 claims description 6
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 6
- 229940038773 trisodium citrate Drugs 0.000 claims description 6
- 235000019270 ammonium chloride Nutrition 0.000 claims description 5
- 239000004310 lactic acid Substances 0.000 claims description 5
- 235000014655 lactic acid Nutrition 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 8
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 abstract description 4
- 239000013543 active substance Substances 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000007654 immersion Methods 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
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- 229910000553 6063 aluminium alloy Inorganic materials 0.000 description 2
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- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 2
- 229940074439 potassium sodium tartrate Drugs 0.000 description 2
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- 238000004381 surface treatment Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 229910001250 2024 aluminium alloy Inorganic materials 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910018104 Ni-P Inorganic materials 0.000 description 1
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- Electroplating Methods And Accessories (AREA)
Abstract
一种在铝及铝合金表面获得含微纳米SiO2颗粒镀层的方法，试样先经酒精浸泡、化学除油、碱、酸侵蚀、水洗、浸锌、最后用丙酮、酒精超声清洗的预处理，SiO2纳米颗粒置于非离子表面活性剂OP-21中浸泡后对试样进行复合化学镀，镀后用冷水洗和后处理即得成品。本发明的方法工艺合理，操作简便，镀层致密牢固，结合性好，表面均匀，硬度高，耐磨、耐热，产品综合性能高，获得的镀层硬度性能、耐磨性能均高于单一镍磷镀层。且活性剂无毒、环保、高效，配方和操作简单，成本低，用传统的镍磷化学镀技术的设备就可以生产，具有较好的经济效益和推广前景。A method for obtaining a coating containing micro-nano SiO2 particles on the surface of aluminum and aluminum alloys. The sample is first pretreated by alcohol immersion, chemical degreasing, alkali, acid corrosion, water washing, zinc dipping, and finally ultrasonic cleaning with acetone and alcohol , SiO 2 nano-particles placed in non-ionic surfactant OP-21 after immersing composite electroless plating on the sample, washed with cold water after plating and post-treatment to get the finished product. The method of the present invention is reasonable in technology, easy to operate, dense and firm in the coating, good in bonding, uniform in surface, high in hardness, wear-resistant and heat-resistant, and has high comprehensive performance of the product. plating. In addition, the active agent is non-toxic, environmentally friendly, highly efficient, simple in formula and operation, and low in cost. It can be produced with traditional nickel-phosphorus electroless plating equipment, and has good economic benefits and popularization prospects.
Description
技术领域 technical field
本发明涉及纯铝及铝合金表面改性技术领域，特别涉及在铝及铝合金表面获得含微纳米SiO2颗粒镀层的方法。. The invention relates to the technical field of surface modification of pure aluminum and aluminum alloys, in particular to a method for obtaining a coating containing micronano SiO2 particles on the surface of aluminum and aluminum alloys. .
背景技术 Background technique
近几年来，化学镀镍作为一项重要的表面处理手段，已被广泛应用到航空、航天、电子工业、石油化工、机械、纺织、汽车工业等领域。随着纳米材料科学的发展，给表面复合镀层技术带来了新的契机。传统的化学镀层存在硬度低、耐磨性差等缺点，纳米化学复合镀是在传统的化学镀基础上发展起来的一种表面处理新技术；纳米化学复合镀层是一种具有特殊功能的复合镀层，该镀层既具有基质金属的优良特性，又具有纳米颗粒的特殊性能。它的基本原理是在Ni-P化学镀液中添加一定量的不溶性固体微粒，并通过添加表面活性剂使颗粒均匀的悬浮在镀液中，改善颗粒分布的均匀性，镀液中金属离子在被还原剂还原的同时，还可以将固体微粒嵌入金属沉积层中；由于所添加的颗粒具有良好的表面效应、体积效应、量子尺寸效应等作用，从而可以获得硬度较高、耐磨、自润滑、耐蚀及特殊的装饰外观等功能性复合镀层。 In recent years, as an important surface treatment method, electroless nickel plating has been widely used in aviation, aerospace, electronics industry, petrochemical industry, machinery, textile, automobile industry and other fields. With the development of nanomaterials science, new opportunities have been brought to surface composite coating technology. Traditional electroless plating has the disadvantages of low hardness and poor wear resistance. Nano chemical composite plating is a new surface treatment technology developed on the basis of traditional chemical plating; nano chemical composite coating is a composite coating with special functions. The coating not only has the excellent properties of matrix metal, but also has the special properties of nanoparticles. Its basic principle is to add a certain amount of insoluble solid particles to the Ni-P electroless plating solution, and to suspend the particles uniformly in the plating solution by adding a surfactant to improve the uniformity of particle distribution. While being reduced by the reducing agent, solid particles can also be embedded in the metal deposition layer; because the added particles have good surface effects, volume effects, quantum size effects, etc., it can obtain high hardness, wear resistance, self-lubricating , corrosion resistance and special decorative appearance and other functional composite coatings.
中国专利申请《金属表面化学镀镍方法》（CN102002690A）公开的技术可以在金属工件、尤其是含有深孔、深槽的金属表面镀层厚度能够达到130微米以上，且能防止金属工件表面因镍磷合金沉积在复杂金属表面的气蚀现象。但此方法需要将镀液泵入滤孔孔径为0.05微米的过滤器中进行过滤，这不仅增大了设备的投资，并且加大了操作的难度，且所得镀层表面较粗糙、硬度低。中国专利《一种低应力镀镍工艺》（ZL200910187670）公开的技术是以镍盐为主盐，通过检查镀液、去所镀材料应力、阳极电解除油、腐蚀、预镀镍、镀镍以及热处理获得内应力低、硬度高、结合力强、且具有优越的延展性的保护层。但该项工艺预处理较为繁琐，不易于维护，影响了生产效率。 The technology disclosed in the Chinese patent application "Metal Surface Electroless Nickel Plating Method" (CN102002690A) can coat metal workpieces, especially metal surfaces with deep holes and deep grooves, with a coating thickness of more than 130 microns, and can prevent the surface of metal workpieces from being damaged by nickel phosphorus. Cavitation phenomenon of alloy deposition on complex metal surfaces. However, this method needs to pump the plating solution into a filter with a filter hole diameter of 0.05 micron for filtration, which not only increases the investment in equipment, but also increases the difficulty of operation, and the resulting coating has a rough surface and low hardness. The technology disclosed in the Chinese patent "A Low Stress Nickel Plating Process" (ZL200910187670) uses nickel salt as the main salt, through inspection of the plating solution, stress removal of the plated material, anode electrolytic degreasing, corrosion, pre-nickel plating, nickel plating and Heat treatment obtains a protective layer with low internal stress, high hardness, strong bonding force and excellent ductility. However, the pretreatment of this process is cumbersome and not easy to maintain, which affects the production efficiency.
目前国内还没有一种操作简单、成本低、污染小、镀层综合性能好、特别适用于各种铝及铝合金工件的微纳米SiO2颗粒复合镀技术。 At present, there is no micro-nano SiO 2 particle composite plating technology that is simple to operate, low in cost, less polluting, and has good comprehensive performance of the coating, and is especially suitable for various aluminum and aluminum alloy workpieces.
发明内容 Contents of the invention
本发明要解决的技术问题是提供一种在铝及铝合金表面获得含微纳米SiO2颗粒镀层的方法，以提高镀层的硬度、耐磨、耐热、自润滑、耐蚀及特殊的装饰外观等性能，且操作简单，成本低，镀层性能好。 The technical problem to be solved by the present invention is to provide a method for obtaining a coating containing micro-nano SiO2 particles on the surface of aluminum and aluminum alloys, so as to improve the hardness, wear resistance, heat resistance, self-lubrication, corrosion resistance and special decorative appearance of the coating. And other performance, and simple operation, low cost, good coating performance.
本发明的工艺流程为： Process flow of the present invention is:
1.试样预处理：试样经酒精浸泡、化学除油、碱侵蚀、水洗、酸侵蚀、水洗、两次浸锌、最后分别用丙酮、酒精超声清洗； 1. Sample pretreatment: the sample is soaked in alcohol, chemical degreasing, alkali erosion, water washing, acid erosion, water washing, zinc dipping twice, and finally ultrasonic cleaning with acetone and alcohol respectively;
2 SiO2纳米颗粒处理：将SiO2纳米颗粒置于非离子表面活性剂OP-21中浸泡,SiO2纳米颗粒粒径范围为50nm~100μm； 2 SiO 2 nanoparticles treatment: Soak SiO 2 nanoparticles in non-ionic surfactant OP-21, the particle size of SiO 2 nanoparticles ranges from 50nm to 100μm;
3.进行复合化学镀：镀液配方为：硫酸镍25～35g/L、次亚磷酸钠30～40g/L、乙酸钠18～28g/L、柠檬酸三钠18～28g/L、氯化铵10～20g/L、乳酸0～6g/L、SiO2纳米颗粒10～20g/L；镀液pH为4～11，搅拌速度100～120r/min，控制温度为50～80℃，试样悬挂于镀液中施镀30分钟； 3. Composite electroless plating: The formula of the plating solution is: nickel sulfate 25-35g/L, sodium hypophosphite 30-40g/L, sodium acetate 18-28g/L, trisodium citrate 18-28g/L, chloride Ammonium 10-20g/L, lactic acid 0-6g/L, SiO 2 nanoparticles 10-20g/L; the pH of the plating solution is 4-11, the stirring speed is 100-120r/min, and the control temperature is 50-80°C. Hang in the plating solution and apply plating for 30 minutes;
4.用冷水洗去试样表面残余的镀液。 4. Wash off the remaining plating solution on the surface of the sample with cold water.
试样预处理中，先后将试样在酒精中浸泡5min；在温度为40~50℃的20g/L洗衣粉溶液中浸泡4~5min化学除油后用冷水作第一次水洗；在温度为20~30℃的质量比10%NaOH溶液中浸泡20s碱侵蚀后，再在温度为20~30℃的质量比98%H2SO4 50ml/L、质量比65%HNO3 50ml/L、质量比48%HF100ml/L的混合酸中浸泡15s后用冷水进行第二次水洗； In the pretreatment of the sample, the sample was soaked in alcohol for 5 minutes successively; soaked in 20g/L washing powder solution at a temperature of 40~50°C for 4~5 minutes and then washed with cold water for the first time after chemical degreasing; After soaking in 10% NaOH solution at 20~30℃ for 20s for alkali corrosion, then at 20~30℃ with mass ratio 98%H 2 SO 4 50ml/L, mass ratio 65%HNO 3 50ml/L, mass Soak in 48%HF100ml/L mixed acid for 15s, then wash with cold water for the second time;
试样预处理中，第一次浸锌的配方为：NaOH 45～55g/L、ZnO 3～8g/L、酒石酸钾钠1～5gL、FeCl3·6H2O 1～5g／L、NaNO3 0.5～3g／L，温度15～27℃，时间30～60s；第二次浸锌的配方为：NaOH 110～130g／L、ZnO 15～25g／L、酒石酸钾钠45～55g／L、FeCl3·6H2O 1～5g／L、NaNO3 0.5～3g／L，温度20～25℃，时间10～30s； In sample pretreatment, the formula for the first zinc dipping is: NaOH 45~55g/L, ZnO 3~8g/L, potassium sodium tartrate 1~5gL, FeCl 3 6H 2 O 1~5g/L, NaNO 3 0.5～3g/L, temperature 15～27℃, time 30～60s; the formulation of the second dipping zinc is: NaOH 110～130g/L, ZnO 15～25g/L, potassium sodium tartrate 45～55g/L, FeCl 3 6H 2 O 1～5g/L, NaNO 3 0.5～3g/L, temperature 20～25℃, time 10～30s;
在第一次浸锌后用体积比为1:1的65%HNO3浸泡30～90s后退除浸锌层，再进行第二次浸锌。 After the first galvanizing, soak in 65% HNO 3 with a volume ratio of 1:1 for 30-90s, remove the galvanizing layer, and then perform the second galvanizing.
试样预处理中，浸锌后的试样用丙酮、酒精超声清洗各10min。 In the sample pretreatment, the sample after galvanizing was ultrasonically cleaned with acetone and alcohol for 10 minutes each.
将SiO2纳米颗粒置于添加了非离子表面活性剂OP-21︰蒸馏水=0.1～1g︰100ml的溶液中浸泡10min。 Soak SiO 2 nanoparticles in a solution added with non-ionic surfactant OP-21: distilled water = 0.1 ~ 1g: 100ml for 10 minutes.
复合化学镀后的试样冷水洗3-4次。 Wash the samples after composite electroless plating with cold water for 3-4 times.
用冷水洗去试样表面残余镀液的试样，通过热处理进一步提高镀层的综合性能。 Wash the sample with cold water to remove the residual plating solution on the surface of the sample, and further improve the comprehensive performance of the coating through heat treatment.
本发明的方法具有以下优点： The method of the present invention has the following advantages:
1、本发明的方法工艺合理，操作简便，镀层致密牢固，结合性好，产品综合性能高。能很好解决SiO2因不溶于镀液而无法沉积于纯铝及铝合金表面和微纳米颗粒镀层硬度低、耐磨性差等问题。 1. The method of the present invention has reasonable technology, simple and convenient operation, dense and firm coating, good combination, and high comprehensive performance of the product. It can well solve the problems that SiO 2 cannot be deposited on the surface of pure aluminum and aluminum alloy due to insolubility in the plating solution, and the micro-nano particle coating has low hardness and poor wear resistance.
2、在铝合金表面获得的微纳米SiO2颗粒复合镀层的硬度性能、耐磨性能均高于单一镍磷镀层。 2. The hardness and wear resistance of the micro-nano SiO 2 particle composite coating obtained on the aluminum alloy surface are higher than that of the single nickel-phosphorus coating.
3、本发明采用的非离子表面活性剂作为SiO2的活性剂，无毒、环保、高效；且配方简单，操作简单，成本低，所获得复合镀层致密牢固，表面均匀，硬度高，耐磨、耐热。 3. The nonionic surfactant used in the present invention is used as the active agent of SiO2 , which is non-toxic, environmentally friendly and efficient; and the formula is simple, the operation is simple, and the cost is low. The obtained composite coating is compact and firm, with uniform surface, high hardness and wear resistance , heat resistance.
4、本发明的方法采用传统的镍磷化学镀技术的设备就可以生产，生产成本较低，具有较好的经济效益和推广前景。 4. The method of the present invention can be produced by using traditional nickel-phosphorus electroless plating technology equipment, the production cost is relatively low, and it has good economic benefits and popularization prospects.
具体实施方式 Detailed ways
微纳米SiO2颗粒复合镀工艺包括前处理、化学镀、后处理等几个主要程序。前处理是将铝合金表面的氧化膜去掉，获得与复合镀层具有良好结合力的铝合金基体表面；化学镀是将已处理好的铝合金放入镀液中，发生一系列的化学和物理反应，形成复合化学镀层；后处理主要是通过热处理工艺进一步提高镀层的综合性能。SiO2硬度高、耐磨性好、绝热性好、抗侵蚀能力强，同时在高温下仍具有高强、高韧、稳定性好等特点，而且纳米SiO2的价格低廉，在表面工程的某些领域，是A12O3、SiC等颗粒的理想替代品，能有效地降低材料成本。 The micro-nano SiO 2 particle composite plating process includes several main procedures such as pre-treatment, chemical plating, and post-treatment. Pretreatment is to remove the oxide film on the surface of the aluminum alloy to obtain an aluminum alloy substrate surface with good adhesion to the composite coating; electroless plating is to put the treated aluminum alloy into the plating solution, and a series of chemical and physical reactions occur , to form a composite electroless coating; the post-treatment is mainly to further improve the comprehensive performance of the coating through the heat treatment process. SiO 2 has high hardness, good wear resistance, good heat insulation, and strong corrosion resistance. At the same time, it still has the characteristics of high strength, high toughness, and good stability at high temperatures, and the price of nano-SiO 2 is low. It is an ideal substitute for Al 2 O 3 , SiC and other particles, which can effectively reduce material costs.
本发明采用了非离子表面活性剂与微纳米颗粒进行处理，使不溶于镀液的微纳米颗粒表面充分润湿，然后再加入已加热到施镀温度的镀液中。该复合化学镀的方法能够解决纳米颗粒由于不溶于镀液而无法沉积于铝合金表面及镀液稳定性差等问题。 The invention adopts the non-ionic surface active agent and the micronano particle to make the surface of the micronano particle insoluble in the plating solution fully wetted, and then add it into the plating solution heated to the plating temperature. The composite electroless plating method can solve the problems that the nanoparticles cannot be deposited on the surface of the aluminum alloy due to insolubility in the plating solution, the stability of the plating solution is poor, and the like.
实施例1： Example 1:
将规格为30mm×15mm×5mm的纯铝片经过预处理后置于硫酸镍30g/L、次亚磷酸钠35g/L、乙酸钠20g/L、柠檬酸三钠20g/L、氯化铵10g/L、SiO2纳米颗粒20g/L的镀液中，镀液pH为11，搅拌速度100r/min，控制温度为50℃，施镀时间为30分钟。将试样取出用冷水冲洗吹干即得到微纳米SiO2颗粒复合镀层，该镀层均匀，表面平整光滑无毛刺，致密牢固，结合性好，硬度高，耐磨性强。 Put the pure aluminum sheet with the specification of 30mm×15mm×5mm into nickel sulfate 30g/L, sodium hypophosphite 35g/L, sodium acetate 20g/L, trisodium citrate 20g/L, ammonium chloride 10g after pretreatment /L, SiO 2 In the plating solution of 20g/L of nanoparticles, the pH of the plating solution is 11, the stirring speed is 100r/min, the control temperature is 50°C, and the plating time is 30 minutes. Take out the sample and rinse it with cold water and dry it to get the composite coating of micro-nano SiO 2 particles. The coating is uniform, the surface is flat and smooth without burrs, dense and firm, good bonding, high hardness and strong wear resistance.
实施例2： Example 2:
将规格为15mm×10mm×5mm的6063铝片经过预处理后置于硫酸镍25g/L、次亚磷酸钠30g/L、乙酸钠18g/L、柠檬酸三钠18g/L、氯化铵10g/L,、乳酸2g/L、SiO2纳米颗粒10g/L的镀液中，镀液pH为4.5，搅拌速度100r/min，控制温度为80℃，施镀时间为30分钟。将试样取出用冷水冲洗吹干即得到Ni-P-SiO2复合镀层，该镀层镀层表面平整，致密牢固，结合性好，硬度高，耐磨性强。 The 6063 aluminum sheet with a size of 15mm×10mm×5mm was pretreated and placed in 25g/L of nickel sulfate, 30g/L of sodium hypophosphite, 18g/L of sodium acetate, 18g/L of trisodium citrate, and 10g of ammonium chloride. /L, lactic acid 2g/L, SiO 2 In the plating solution of nanoparticle 10g/L, the pH of the plating solution is 4.5, the stirring speed is 100r/min, the control temperature is 80°C, and the plating time is 30 minutes. The Ni-P-SiO 2 composite coating is obtained by taking out the sample and rinsing it with cold water and blowing it dry. The coating has a flat surface, is dense and firm, has good adhesion, high hardness and strong wear resistance.
实施例3： Example 3:
将规格为20mm×10mm×2mm的6063铝片经过预处理后置于硫酸镍28g/L、次亚磷酸钠32g/L、乙酸钠20g/L、柠檬酸三钠20g/L、氯化铵12g/L,、乳酸3g/L、SiO2纳米颗粒12g/L的镀液中，镀液pH为5，搅拌速度120r/min，控制温度为80℃，施镀时间为30分钟。将试样取出用冷水冲洗吹干即得到Ni-P-SiO2复合镀层，再将试样置入400℃的真空热处理炉中处理2小时后缓慢取出自然冷却至常温，所得镀层表面平整，致密牢固，结合性好，硬度更高，耐磨性更强，并具有耐热特性。 The 6063 aluminum sheet with a size of 20mm×10mm×2mm was pretreated and placed in 28g/L of nickel sulfate, 32g/L of sodium hypophosphite, 20g/L of sodium acetate, 20g/L of trisodium citrate, and 12g of ammonium chloride. /L, lactic acid 3g/L, SiO 2 In the plating solution of nanoparticles 12g/L, the pH of the plating solution is 5, the stirring speed is 120r/min, the control temperature is 80°C, and the plating time is 30 minutes. Take out the sample and rinse it with cold water to dry it to get the Ni-P-SiO 2 composite coating, then place the sample in a vacuum heat treatment furnace at 400°C for 2 hours, then slowly take it out and let it cool down to normal temperature, the surface of the obtained coating is smooth and compact Strong, good bonding, higher hardness, stronger wear resistance, and heat resistance.
实施例4： Example 4:
将规格为15mm×10mm×2mm的2024铝片经过预处理后置于硫酸镍35g/L、次亚磷酸钠40g/L、乙酸钠28g/L、柠檬酸三钠28g/L、氯化铵20g/L,、乳酸6g/L、SiO2纳米颗粒15g/L的镀液中，镀液pH为4.5，搅拌速度100r/min，控制温度为70℃，施镀时间为30分钟。将试样取出用冷水冲洗吹干即得到Ni-P-SiO2复合镀层，再将试样置入400℃的真空热处理炉中处理2小时后缓慢取出自然冷却至常温，所得镀层表面平整，致密牢固，结合性好，硬度高，耐磨性好。 The 2024 aluminum sheet with a specification of 15mm×10mm×2mm is pretreated and placed in nickel sulfate 35g/L, sodium hypophosphite 40g/L, sodium acetate 28g/L, trisodium citrate 28g/L, ammonium chloride 20g /L, lactic acid 6g/L, SiO 2 In the plating solution of nanoparticles 15g/L, the pH of the plating solution is 4.5, the stirring speed is 100r/min, the control temperature is 70°C, and the plating time is 30 minutes. Take out the sample and rinse it with cold water to dry it to get the Ni-P-SiO 2 composite coating, then place the sample in a vacuum heat treatment furnace at 400°C for 2 hours, then slowly take it out and let it cool down to normal temperature, the surface of the obtained coating is smooth and compact Strong, good combination, high hardness, good wear resistance.
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| CN105177536A (en) * | 2015-09-15 | 2015-12-23 | 广西大学 | Method for preparing micrometer-particle-contained high-temperature-oxidation-resistant composite coating on surface of niobium alloy |
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