CN101545116A - Method for electroplating inorganic molten salt on surface of magnesium and magnesium alloy with aluminum - Google Patents
Method for electroplating inorganic molten salt on surface of magnesium and magnesium alloy with aluminum Download PDFInfo
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- CN101545116A CN101545116A CN200810010794A CN200810010794A CN101545116A CN 101545116 A CN101545116 A CN 101545116A CN 200810010794 A CN200810010794 A CN 200810010794A CN 200810010794 A CN200810010794 A CN 200810010794A CN 101545116 A CN101545116 A CN 101545116A
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- electroplating
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- magnesium
- molten salt
- magnesium alloy
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 62
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 59
- 238000009713 electroplating Methods 0.000 title claims abstract description 42
- 150000003839 salts Chemical class 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 29
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000011777 magnesium Substances 0.000 title claims abstract description 21
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 21
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 42
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 22
- 238000007747 plating Methods 0.000 claims abstract description 21
- 239000011780 sodium chloride Substances 0.000 claims abstract description 21
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 19
- 239000001103 potassium chloride Substances 0.000 claims abstract description 11
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000008139 complexing agent Substances 0.000 claims abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 229910052786 argon Inorganic materials 0.000 claims description 9
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- 239000000654 additive Substances 0.000 claims description 6
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 6
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 claims description 4
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 150000004820 halides Chemical class 0.000 claims description 3
- 235000009518 sodium iodide Nutrition 0.000 claims description 3
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical group Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 230000001681 protective effect Effects 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 46
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 36
- 239000011701 zinc Substances 0.000 abstract description 36
- 229910052725 zinc Inorganic materials 0.000 abstract description 36
- 239000011248 coating agent Substances 0.000 abstract description 29
- 238000000576 coating method Methods 0.000 abstract description 29
- 238000005260 corrosion Methods 0.000 abstract description 18
- 230000007797 corrosion Effects 0.000 abstract description 12
- 239000011159 matrix material Substances 0.000 abstract description 12
- 239000000758 substrate Substances 0.000 abstract description 12
- 238000004381 surface treatment Methods 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 239000011241 protective layer Substances 0.000 abstract description 4
- 239000002346 layers by function Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 58
- 239000008367 deionised water Substances 0.000 description 33
- 229910021641 deionized water Inorganic materials 0.000 description 33
- 239000008399 tap water Substances 0.000 description 32
- 235000020679 tap water Nutrition 0.000 description 32
- 238000005406 washing Methods 0.000 description 27
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- 239000000463 material Substances 0.000 description 11
- 238000005530 etching Methods 0.000 description 10
- 230000004913 activation Effects 0.000 description 9
- 239000011734 sodium Substances 0.000 description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 7
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 7
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 7
- 229910000368 zinc sulfate Inorganic materials 0.000 description 7
- 239000011686 zinc sulphate Substances 0.000 description 7
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 6
- 239000012459 cleaning agent Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 238000005246 galvanizing Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 description 3
- 241000272186 Falco columbarius Species 0.000 description 2
- 229910017665 NH4HF2 Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 210000001787 dendrite Anatomy 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000011253 protective coating Substances 0.000 description 2
- 229910004835 Na2B4O7 Inorganic materials 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 238000005269 aluminizing Methods 0.000 description 1
- -1 anodic oxidation Chemical compound 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000010288 cold spraying Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000989 no adverse effect Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
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- Electroplating Methods And Accessories (AREA)
Abstract
The invention relates to a method for electroplating inorganic molten salt on surface of magnesium and magnesium alloy with aluminum, which belongs to the technical field of metal surface treatment. The method comprises a step of preplating a zinc layer as a substrate and a step of electroplating inorganic molten salt with aluminum. The step of preplating the zinc layer as the substrate comprises a step of immersion-plating the zinc layer and a step of electroplating the zinc layer. The step of electroplating the zinc layer is performed in an inorganic molten salt system, wherein anhydrous aluminum chloride is main salt, and sodium chloride, potassium chloride or a mixture of the two is a main complexing agent. An aluminum coating obtained by the method is complete, dense, uniform and bright, is firmly combined with a matrix, can be individually used as a protective layer, and can be prepared into a surface functional layer with better corrosion resistance, better wear resistance and high hardness through subsequent treatment. The whole process of the method has the advantages of simple process, cheap equipment, friendliness to environment, and the like.
Description
The technical field is as follows:
the invention relates to a method for electroplating inorganic molten salt on the surface of magnesium and magnesium alloy with aluminum, belonging to the technical field of metal surface treatment.
Background art:
the magnesium alloy has the advantages of small density, high specific strength, good electromagnetic shielding performance and the like, is known as a green engineering material in the 21 st century, and has wide application value in the automobile industry, the aerospace industry and the electronic industry. However, poor corrosion resistance, poor wear resistance, low hardness, etc. pose a bottleneck problem that limits the application of magnesium alloys, limiting their use in large areas. Therefore, in order to make the magnesium alloy usable in a more severe environment, it is necessary to develop a surface treatment technology for the magnesium alloy. The surface treatment technology developed on magnesium alloy at present mainly comprises chemical conversion, electrochemical anodic oxidation or micro-arc oxidation, electroplating or chemical metal coating and the like.
The chemical conversion film of the magnesium alloy has strong binding capacity with a matrix and good insulation and optical performance, but the film layer is too thin and soft and can only be used as a substrate for coating, and the chemical conversion film is rarely used alone. The coating obtained by electrochemical oxidation or micro-arc oxidation has a certain thickness, so that the corrosion resistance of the surface of the magnesium alloy is greatly improved, but the film layer is loose and porous and cannot completely and effectively prevent corrosion media from corroding the magnesium alloy; and because the brittleness of the oxide film is very high, the film layer is easy to fall off, so that the good protection effect cannot be achieved. The magnesium alloy surface is also an important protection means by implementing electroplating or chemical plating metal coating, which not only improves the corrosion resistance, wear resistance and hardness of the magnesium alloy surface, but also has conductivity and decoration. At present, the magnesium alloy surface is mainly plated with electroplating or chemical nickel plating, but because the plating layer is of negative polarity, under the condition that the plating layer has defects or is damaged in service, the risk of accelerating the corrosion of the matrix magnesium alloy exists, and the recycling of the magnesium alloy is also difficult due to the existence of the nickel plating layer.
In the preparation of the magnesium alloy surface coating, people are dedicated to research a protective coating which is suitable for various requirements of magnesium alloy such as good corrosion resistance and wear resistance, high hardness, easy recovery, environmental friendliness and the like. Among them, the application of an aluminum coating on the surface of a magnesium alloy is considered to be the most desirable coating to satisfy such a requirement for the following reasons: 1) the difference between the electrode potential of the aluminum and the magnesium is not large, so that severe galvanic corrosion can not be caused to the magnesium alloy; 2) the surface treatment of the aluminum is much more mature than that of the magnesium alloy, and the protective coating with high hardness and good wear resistance and corrosion resistance can be obtained by further treating the aluminum (such as anodic oxidation, micro-arc oxidation and the like); 3) the aluminum element is an important alloy element of the magnesium alloy, and the preparation of the aluminum coating has no adverse effect on the recycling of materials. At present, many processes for preparing an aluminum coating on the surface of a magnesium alloy are available, including physical vapor deposition, chemical vapor deposition, magnetron sputtering, cold spraying, laser surface modification, aluminizing and the like. However, these preparation techniques have various problems that the equipment is expensive and cannot be popularized and used in a large area, or the obtained coating has poor binding force, is not dense and incomplete, is difficult to perform further surface treatment, and the like, and are far from meeting the large demand of the magnesium alloy in practical application.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for preparing an aluminum coating on the surface of magnesium and magnesium alloy. The aluminum plating layer is firmly combined with the matrix, is complete and compact and has certain thickness, so that the prepared aluminum plating layer can be independently used as a protective layer and can be further converted into a film layer with higher corrosion resistance, wear resistance and high hardness through subsequent processing treatment, and the comprehensive performance of the surface of the magnesium alloy is improved.
The invention is implemented by the following technical scheme:
a method for electroplating inorganic molten salt on the surface of magnesium and magnesium alloy with aluminum comprises the following steps:
(1) after pretreatment of grinding, polishing, degreasing and the like, magnesium or magnesium alloy is etched and activated in certain etching solution or activating solution; then dip-plating zinc or electroplating zinc in certain zinc dipping solution or electroplating zinc solution, wherein the thickness of a zinc layer is 2-20um, and the zinc dipping layer or the zinc coating layer which is prepared in advance and well combined with the magnesium alloy matrix is used as a transition layer (bottom layer) before aluminum plating.
The transition zinc layer plays a role in protecting the magnesium alloy and preventing the corrosion of the magnesium alloy in the inorganic molten salt; on the other hand, the transition zinc layer replaces the oxide skin on the surface of magnesium or magnesium alloy, so that the chemical activity of the surface of the material is reduced, and the aluminum plating layer after electrodeposition is firmly combined with the substrate.
(2) The electroplating aluminum adopts an inorganic molten salt system, anhydrous aluminum chloride is used as a main salt, sodium chloride, potassium chloride or a mixture of the anhydrous aluminum chloride and the sodium chloride and the potassium chloride are used as complexing agents, halide (such as manganese chloride, tin chloride, sodium bromide, potassium bromide, sodium iodide, potassium iodide and the like) or tetramethylammonium chloride is used as an additive, and the weight ratio of the components is as follows: the main salt accounts for 65-90%; 5-30% of complexing agent; 0-5% of additive; preferred ranges are as follows: 75-85% of main salt; 15-25% of complexing agent; the additive accounts for 0-3%.
In the process of electroplating aluminum, the operation temperature is 100-250 ℃, and the current density is 0.5-5A/dm2The electroplating time is 5-180 minutes, the electroplating mode comprises direct current electroplating or pulse electroplating, and the thickness of the obtained aluminum coating is 5-60 um.
The operation temperature of the invention is 100-250 ℃, and the invention has no influence on the microstructure and mechanical property of the magnesium alloy. The aluminum coating with the required thickness is prepared by adjusting the current density and the electroplating time. And protecting the molten salt by adopting high-purity argon or nitrogen to prevent the volatilization of the anhydrous aluminum chloride. The addition of additives to the molten salt effectively inhibits the formation of aluminum dendrites and extends the range of current densities. The pulse electroplating can effectively improve the compactness of the coating. The molten salt is stirred to increase the crystallization speed and effectively prevent the growth of aluminum dendrites.
The invention relates to a method for electroplating inorganic molten salt on the surface of magnesium and magnesium alloy with aluminum, which comprises the following specific manufacturing process flows: sanding → degreasing → etching → activating → pre-galvanizing (dip galvanizing or electrogalvanizing) → light extraction → activating → molten salt electrogalvanizing → drying, and adding tap water and deionized water for cleaning in each step. Wherein, the etching and activation before the galvanization can be carried out according to the specific process; the light extraction and activation treatment of the zinc coating before aluminum plating can be selected according to requirements.
Compared with the prior art, the invention has the following remarkable advantages:
1. the aluminum plating layer is complete, compact, uniform and bright, is well combined with a substrate, can be independently used as a protective layer, and can be prepared into a surface functional layer with better corrosion resistance, wear resistance and high hardness after subsequent processing.
2. The transition layer zinc and the protective layer aluminum in the coating system are alloy elements of magnesium alloy, and the recycling of materials is facilitated.
3. The whole preparation process has the industrial practical characteristics of low equipment cost, easily obtained raw materials, simple process, convenient operation, environmental friendliness and the like.
The specific implementation mode is as follows:
the present invention will be further described with reference to the following examples.
Example 1
1. Preparing materials: after pure magnesium is cut and polished, the pure magnesium is cleaned by ultrasonic waves in acetone solution to remove oil.
2. Etching: 85% H3PO4 5ml/L，NH4HF2100g/L, and the balance of water, wherein the temperature is 10-35 ℃. Treating for 0.5-5 minutes, taking out, immediately washing for 1-2 minutes by using tap water, and then washing for 1-2 minutes by using deionized water.
3. And (3) activation: na (Na)4P2O7 40g/L，Na2B4O770g/L, 20g/L NaF and the balance of water. Treating at 70-80 ℃ for 2-5 minutes, taking out, and immediately cleaning with tap waterAnd cleaning for 1-2 minutes by using deionized water after 1-2 minutes.
4. Zinc dipping: ZnSO4·7H2O 30g/L，Na4P2O7 120g/L，NaF 5g/L，LiF 3g/L，Na2CO35g/L, and the balance of water. Treating the mixture for 30-90 minutes at the pH of 10.0-10.6 and the temperature of 75-85 ℃, immediately washing the mixture for 1-2 minutes by using tap water after taking out the mixture, and then washing the mixture for 1-2 minutes by using deionized water, wherein the thickness of a zinc layer in the embodiment is 3-10 mu m.
5. Electroplating aluminum: calculated by weight percentage, AlCl375 percent of NaCl and 25 percent of NaCl are fully melted into molten salt at 200 ℃ after being mixed under the protection of argon, and the electroplating current density is 1.5A/dm2And the time is 30 minutes, the aluminum-plated layer is immediately washed by tap water for 1-2 minutes after being taken out, then washed by deionized water for 1-2 minutes, and finally dried, wherein the thickness of the aluminum-plated layer obtained in the embodiment is about 9 um.
The relevant performance data for this example is as follows:
the bonding force between the dip coating and the substrate is more than 30 MP; the hardness of the aluminum coating is 60-70 HV, and the self-corrosion current density of the aluminum coating in 3.5 wt% sodium chloride solution is less than 1e-6A/cm2And the magnesium content is reduced by 1-2 orders of magnitude compared with that of the matrix magnesium.
Example 2
1. Preparing materials: after AZ31B magnesium alloy is cut and polished, the magnesium alloy is cleaned by ultrasonic waves in an acetone solution to remove oil.
2. Etching: 85% H3PO42-5 ml/L, 40-70 ℃, and the balance of water. Treating for 0.5-5 minutes, taking out, immediately washing for 1-2 minutes by using tap water, and then washing for 1-2 minutes by using deionized water.
3. Electrogalvanizing: ZnSO4·7H2O36g/L，Na4P2O7·10H2O 134g/L，C6H5Na3O7·2H2O10g/L，KF·2H2O10 g/L, sodium dodecyl sulfate 0.1g/L and the balance of water. pH of 9.0 to 10.0The temperature is 40-70 ℃, and the cathode current density is 0.1-0.5A/dm2And the time is 50-60 minutes, the zinc layer is immediately washed for 1-2 minutes by using tap water after being taken out, and then washed for 1-2 minutes by using deionized water, wherein the thickness of the zinc layer is 5-8 um.
4. Light emission: HNO330ml/L, HCl 10ml/L and the balance of water. And (3) treating for 5-30 seconds at the temperature of 10-35 ℃, immediately washing for 1-2 minutes by using tap water after taking out, and then washing for 1-2 minutes by using deionized water.
5. And (3) activation: 15-20 ml/L of HF, and the balance of water. The temperature is 10-35 ℃, the time is 5-30 seconds, the cleaning agent is taken out and immediately cleaned by tap water for 1-2 minutes, and then cleaned by deionized water for 1-2 minutes and dried.
6. Electroplating aluminum: calculated by weight percentage, AlCl379 percent of NaCl, 10 percent of KCl and 1 percent of NaI are mixed under the protection of argon and then fully melted into fused salt at 160 ℃, a magnetic stirrer is used for stirring the fused salt, and the cathode current density is 1.2A/dm2And the time is 60 minutes, the aluminum plate is immediately washed by tap water for 1-2 minutes after being taken out, then washed by deionized water for 1-2 minutes, and finally dried, wherein the thickness of the electroplated aluminum layer obtained in the embodiment is about 15 um.
The relevant performance data for this example is as follows:
the binding force between the zinc coating and the substrate is more than 50 MP; the hardness of the aluminum coating is 80-90 HV, and the self-corrosion current density in 3.5 wt% sodium chloride solution is less than 1e-6A/cm2And the reduction is 1-2 orders of magnitude compared with that of the matrix magnesium alloy.
Example 3
1. Preparing materials: after AZ31B magnesium alloy is cut and polished, the magnesium alloy is cleaned by ultrasonic waves in an acetone solution to remove oil.
2. Etching: na (Na)4P2O7·10H2O 40g/L，Na2CO3 3.7g/L，NaNO3 5g/L，NaH2PO4·2H205 g/L, and the balance of water. Treating at 50-70 ℃ for 0.5-5 minutes, and taking outImmediately washing with tap water for 1-2 minutes, and then washing with deionized water for 1-2 minutes.
3. And (3) activation: 30ml/L of HF, 20g/L of ZnO and the balance of water. Treating for 0.5-5 minutes at the temperature of 10-35 ℃, immediately washing for 1-2 minutes by using tap water after taking out, and then washing for 1-2 minutes by using deionized water.
4. Electrogalvanizing: ZnSO4·7H2O 35.6g/L，Na4P2O7·10H2O 134g/L，C6H5Na3O7·2H2O10g/L，KF.2H2O10 g/L, sodium dodecyl sulfate 0.1g/L and the balance of water. pH of 9.0-10.0, temperature of 40-70 deg.C, and cathode current density of 0.2-0.5A/dm2The time is 50 minutes, the zinc layer is immediately washed for 1 to 2 minutes by tap water after being taken out, and then washed for 1 to 2 minutes by deionized water, and the thickness of the zinc layer is about 6um in the embodiment.
5. Electroplating aluminum: calculated by weight percentage, AlCl385 percent, NaCl 8 percent and KCl 7 percent are fully melted into liquid molten salt at 180 ℃ after being mixed under the protection of argon, and the cathode current density is 1A/dm2And the time is 180 minutes, the aluminum-plated layer is immediately washed by tap water for 1-2 minutes after being taken out, then washed by deionized water for 1-2 minutes, and finally dried, wherein the thickness of the aluminum-plated layer obtained in the embodiment is about 40 um.
The relevant performance data for this example is as follows:
the binding force between the zinc coating and the substrate is more than 50 MP; the hardness of the aluminum coating is 60-80 HV, and the self-corrosion current density in 3.5 wt% sodium chloride solution is less than 1e-6A/cm2And the reduction is 1-2 orders of magnitude compared with that of the matrix magnesium alloy.
Example 4
1. Preparing materials: after AZ91D magnesium alloy is cut and polished, the magnesium alloy is cleaned by ultrasonic waves in an acetone solution to remove oil.
2. Etching: 85% H3PO42-5 ml/L, and the balance of water. Treating at 40-70 ℃ for 0.5-5 minutes, taking out and using immediatelyWashing with tap water for 1-2 minutes, and then washing with deionized water for 1-2 minutes.
3. Electrogalvanizing: ZnSO4·7H2O 36g/L，Na4P2O7·10H2O 134g/L，C6H5Na3O7·2H2O10g/L，KF.2H2O10 g/L, sodium dodecyl sulfate 0.1g/L and the balance of water. pH is 9.0-10.0, temperature is 40-70 ℃, and cathode current density is 0.1-0.5A/dm2And the time is 60 minutes, the zinc layer is immediately washed for 1 to 2 minutes by using tap water after being taken out, and then washed for 1 to 2 minutes by using deionized water, wherein the thickness of the zinc layer is about 6 to 8 um.
4. Light emission: HNO330ml/L, HCl 10ml/L and the balance of water. Treating for 5-30 seconds at the temperature of 16-35 ℃, immediately washing for 1-2 minutes by using tap water after taking out, and then washing for 1-2 minutes by using deionized water.
5. And (3) activation: 15-20 ml/L of HF, and the balance of water. The temperature is 16-35 ℃, the time is 5-10 seconds, the cleaning agent is taken out and immediately cleaned by tap water for 1-2 minutes, and then cleaned by deionized water for 1-2 minutes and dried.
6. Electroplating aluminum: calculated by weight percentage, AlCl379 percent of NaCl, 10 percent of KCl and 1 percent of KBr are mixed under the protection of argon and then fully melted into fused salt at 160 ℃, and the fused salt is stirred by magnetic stirring; current density 1A/dm2And the time is 60 minutes, the aluminum plate is immediately washed by tap water for 1-2 minutes after being taken out, then washed by deionized water for 1-2 minutes, and finally dried, wherein the thickness of the electroplated aluminum layer obtained in the embodiment is 15 um.
The relevant performance data for this example is as follows:
the binding force of the zinc coating and the substrate is more than 50MP, the hardness of the aluminum coating is 60-80 HV, and the self-corrosion current density in 3.5 wt% sodium chloride solution is less than 1e-6A/cm2And the reduction is 1-2 orders of magnitude compared with that of the matrix magnesium alloy.
Example 5
1. Preparing materials: after AZ91D magnesium alloy is cut and polished, the magnesium alloy is cleaned by ultrasonic waves in an acetone solution to remove oil.
2. Etching: na (Na)4P2O7·10H2O 40g/L，Na2CO3 3.7g/L，NaNO3 5g/L，NaH2PO4·2H2O5 g/L, and the balance of water. Treating for 0.5-5 minutes at 50-70 ℃, immediately washing for 1-2 minutes by using tap water after taking out, and then washing for 1-2 minutes by using deionized water.
3. And (3) activation: HF 30ml/L, ZnO 30g/L, and the balance of water. Treating for 0.5-5 minutes at the temperature of 10-35 ℃, immediately washing for 1-2 minutes by using tap water after taking out, and then washing for 1-2 minutes by using deionized water.
4. Electrogalvanizing: ZnSO4·7H2O 35.6g/L，Na4P2O7·10H2O 134g/L，C6H5Na3O7·2H2O10g/L，KF.2H2O10 g/L, sodium dodecyl sulfate 0.1g/L and the balance of water. pH is 9.0-10.0, temperature is 40-70 ℃, and cathode current density is 0.1-0.5A/dm2The time is 50 minutes, the zinc layer is immediately washed for 1 to 2 minutes by tap water after being taken out, and then washed for 1 to 2 minutes by deionized water, and the thickness of the zinc layer is about 7um in the embodiment.
5. Electroplating aluminum: calculated by weight percentage, AlCl378.5 percent of NaCl 10 percent, KCl 10 percent and 1.5 percent of tetramethylammonium chloride are mixed under the protection of argon and then fully melted into liquid molten salt at 160 ℃, pulse plating is adopted, the frequency is 1000Hz, the duty ratio is 20-35 percent, and the cathode current density is 0.8A/dm2And the time is 180 minutes, the aluminum-plated layer is immediately washed by tap water for 1-2 minutes after being taken out, then washed by deionized water for 1-2 minutes, and finally dried, wherein the thickness of the aluminum-plated layer obtained in the embodiment is about 35 um.
The relevant performance data for this example is as follows:
the binding force between the zinc coating and the substrate is more than 50 MP; the aluminum plating layer has a hardness of 70-85 HV, and is self-corroded in a 3.5 wt% sodium chloride solutionThe current is less than 1e-6A/cm2And the reduction is 1-2 orders of magnitude compared with that of the matrix magnesium alloy.
Example 6
1. Preparing materials: after cutting and polishing the AM60 magnesium alloy, the alloy is cleaned by ultrasonic waves in an acetone solution to remove oil.
2. Etching: na (Na)4P2O7·10H2O 40g/L，Na2CO3 3.7g/L，NaNO3 8g/L，NaH2PO4·2H2O5 g/L, and the balance of water. Treating for 0.5-5 minutes at 50-70 ℃, immediately washing for 1-2 minutes by using tap water after taking out, and then washing for 1-2 minutes by using deionized water.
3. And (3) activation: HF 20ml/L, NH4HF210g/L, ZnO 30g/L and the balance of water. Treating for 0.5-5 minutes at the temperature of 10-35 ℃, immediately washing for 1-2 minutes by using tap water after taking out, and then washing for 1-2 minutes by using deionized water.
4. Electrogalvanizing: ZnSO4·7H2O 20g/L，Na4P2O7·10H2100g/L of O, 5g/L of NaF, 0.1g/L of sodium dodecyl sulfate and the balance of water. pH is 9.0-9.6, temperature is 40-70 ℃, and cathode current density is 0.1-0.5A/dm2And the time is 50 minutes, the zinc layer is immediately washed for 1 to 2 minutes by using tap water after being taken out, and then washed for 1 to 2 minutes by using deionized water, wherein the thickness of the zinc layer is 6 um.
6. Electroplating aluminum: calculated by weight percentage, AlCl370 percent of NaCl, 15 percent of NaCl and 15 percent of KCl are fully melted into fused salt at 160 ℃ after being mixed under the protection of argon, and the plating current density is 1A/dm2And the time is 60 minutes, the aluminum plate is immediately washed by tap water for 1-2 minutes after being taken out, then washed by deionized water for 1-2 minutes, and finally dried, wherein the thickness of the electroplated aluminum layer obtained in the embodiment is 15 um.
The relevant performance data for this example is as follows:
the binding force between the zinc coating and the substrate is more than 50 MP; hardness of aluminum plating layer60-70 HV, and the self-corrosion current density in 3.5 wt% sodium chloride solution is less than 1e-6A/cm2And the reduction is 1-2 orders of magnitude compared with that of the matrix magnesium alloy.
Example 7
1. Preparing materials: after cutting and polishing the AM60 magnesium alloy, the alloy is cleaned by ultrasonic waves in an acetone solution to remove oil.
2. Etching: 85% H3PO42-5 ml/L, and the balance of water. Treating for 0.5-5 minutes at the temperature of 40-70 ℃, immediately washing for 1-2 minutes by using tap water after taking out, and then washing for 1-2 minutes by using deionized water.
4. Electrogalvanizing: the zinc pre-plating is carried out in two steps: ZnSO4·7H2O 36g/L，Na4P2O7·10H2O134g/L，C6H5Na3O7·2H2O 10g/L，KF.2H2O10 g/L, sodium dodecyl sulfate 0.1g/L and the balance of water. pH is 9.0-10.0, temperature is 40-70 ℃, and cathode current density is 0.1-0.5A/dm2And the time is 5-30 minutes, the cleaning agent is taken out and immediately cleaned for 1-2 minutes by using tap water, and then cleaned for 1-2 minutes by using deionized water. (2) Bright galvanizing: 17g/L of ZnO, 135g/L of NaOH, 1.0ml/L of Merlin gloss agent, 20ml/L of Merlin cylinder opening agent and the balance of water. The temperature is 10-35 ℃, and the cathode current density is 1.5-2.5A/dm2And the time is 10-60 minutes, the cleaning agent is taken out and immediately cleaned for 1-2 minutes by using tap water, and then cleaned for 1-2 minutes by using deionized water. In this embodiment, the thickness of the zinc layer is about 5-20 um.
5. Light emission: HNO330ml/L, HCl 10ml/L and the balance of water. And (3) treating for 5-30 seconds at the temperature of 10-35 ℃, immediately washing for 1-2 minutes by using tap water after taking out, and then washing for 1-2 minutes by using deionized water.
6. And (3) activation: 15-20 ml/L of HF, and the balance of water. The temperature is 10-35 ℃, the time is 5-30 seconds, the cleaning agent is taken out and immediately cleaned by tap water for 1-2 minutes, and then cleaned by deionized water for 1-2 minutes and dried.
7. Electroplating aluminum: according to the weightMeasured in percentage by weight, AlCl378.5 percent of NaCl 10 percent, KCl 10 percent and 1.5 percent of tetramethylammonium chloride are mixed under the protection of argon and then fully melted into fused salt at 190 ℃, the fused salt is stirred by magnetic stirring, and the plating current density is 1A/dm2And the time is 60 minutes, the aluminum plate is immediately washed by tap water for 1-2 minutes after being taken out, then washed by deionized water for 1-2 minutes, and finally dried, wherein the thickness of the electroplated aluminum layer obtained in the embodiment is 15 um.
The relevant performance data for this example is as follows:
the binding force of the zinc coating and the substrate is more than 50MP, the hardness of the aluminum coating is 65-75 HV, and the self-corrosion current density in 3.5 wt% sodium chloride solution is less than 1e-6A/cm2And the reduction is 1-2 orders of magnitude compared with that of the matrix magnesium alloy.
Claims (6)
1. A method for electroplating inorganic molten salt on the surface of magnesium and magnesium alloy with aluminum is characterized by comprising the following steps: the surface of magnesium or magnesium alloy is primed by a pre-galvanized layer and then is electroplated with aluminium in inorganic molten salt.
2. The method for electroplating inorganic molten salt on the surface of magnesium and magnesium alloy with aluminum according to claim 1, wherein the method comprises the following steps: the pre-galvanized layer comprises a dip-galvanized layer or an electro-galvanized layer, and the thickness of the pre-galvanized layer is 2-20 um.
3. The method for electroplating inorganic molten salt on the surface of magnesium and magnesium alloy with aluminum according to claim 1, wherein the aluminum is electroplated by adopting an inorganic molten salt system, and the inorganic molten salt system comprises the following components in percentage by weight: main salt, complexing agent and additive; wherein,
main salt: anhydrous aluminum chloride accounting for 65-90%;
complexing agent: 5-30% of sodium chloride, potassium chloride or a mixture of the sodium chloride and the potassium chloride;
additive: 0-5% of halide or tetramethylammonium chloride;
in the process of electroplating aluminum, the operation temperature is 100-250 ℃, the electroplating mode comprises direct current electroplating or pulse electroplating, the electroplating time is 5-180 minutes, and the current density is 0.5-5A/dm2The thickness of the obtained electroplated aluminum layer is 5-60 um.
4. The method for electroplating inorganic molten salt on the surface of magnesium and magnesium alloy with aluminum according to claim 3, wherein the method comprises the following steps: the halide is manganese chloride, tin chloride, sodium bromide, potassium bromide, sodium iodide or potassium iodide.
5. The method for electroplating inorganic molten salt on the surface of magnesium and magnesium alloy with aluminum according to claim 3, wherein the method comprises the following steps: the plating solution is prevented from volatilizing by adopting a protective atmosphere which is gas such as argon or nitrogen and the like which has no chemical activity to the anhydrous aluminum chloride.
6. The method for electroplating inorganic molten salt on the surface of magnesium and magnesium alloy with aluminum according to claim 3, wherein the method comprises the following steps: in the process of electroplating aluminum, the solution is adopted for stirring to improve the crystallization speed and the surface quality of the plating layer.
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