CN103334147A - Method for preparing nickel-coated aluminum powder composite coating by utilizing pulse plating - Google Patents
Method for preparing nickel-coated aluminum powder composite coating by utilizing pulse plating Download PDFInfo
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- CN103334147A CN103334147A CN2013102511878A CN201310251187A CN103334147A CN 103334147 A CN103334147 A CN 103334147A CN 2013102511878 A CN2013102511878 A CN 2013102511878A CN 201310251187 A CN201310251187 A CN 201310251187A CN 103334147 A CN103334147 A CN 103334147A
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Abstract
The invention discloses a method for preparing nickel-coated aluminum powder composite coating by utilizing pulse plating and relates to a method for preparing a composite coating. The method comprises the following steps: preparing high-yield nickel-coated aluminum powder solid powder by employing a chemical plating method; regulating technical parameters such as the average current density, temperature of a plating solution, a duty ratio, pH and plating time for performing pulsed composite plating; and finally, preparing a nickel-coated aluminum powder coating which is high-temperature-resistant, wear-resistant, high in hardness, corrosion-resistant and high in binding force on the surface of a copper sheet. In order to improve the performance of the nickel-coated aluminum powder coating, a buffer agent (boric acid), a wetting agent (lauryl sodium sulfate) and the like are utilized in the reaction process. The prepared nickel-coated aluminum powder coating is uniform in surface, dense, flat and small in grain size, and meanwhile, the metal surface is intensified, the corrosion resistance and wear resistance are improved, and the physical properties of the coating are improved. Therefore, the coating quality and performance of the pulse composite plating are superior to those of the traditional direct current plating, so that the pulse composite plating has the tendency of further replacing the traditional direct current plating.
Description
Technical field
The present invention relates to a kind of method for preparing composite deposite, particularly relate to a kind of method of utilizing pulse plating to prepare the Al contained Ni composite deposite.
Background technology
Pulse plating is a kind of novel electroplating technology that protects or decorate at metal base surface, has especially become core technology in fields such as aviation, electronics, automobiles.Pulse plating can not only improve the quality of coating, shortens the plating cycle, save energy, and can economize in raw materials, be the main direction of world today's electroplating technology development and the focus of first developing.Along with science and technology development, the electroplated coating quality is had higher requirement, thereby make the fast development of pulse composite plating.The pulse composite plating is that the method with pulse plating makes metallic matrix and solia particle codeposition obtain a kind of technological process of required coating, is a kind of metal surface enhanced technology of extremely potentialization.Concrete processing parameter should try the plating situation according to reality and carry out choose reasonable.Anticorrosion one of global scientific circles main direction of studying that become of metallic substance.Because the whole world is about 30% ~ 35% of its annual production because of the metal product amount that wearing and tearing or corrosion etc. are scrapped every year, tackles in this situation, the pulse composite plating has superiority to bring into play its effect fully.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing pulse plating to prepare the Al contained Ni composite deposite.This method uses the excellent honest and clean copper sheet of price with the method for pulse plating, its surface preparation go out high temperature resistant, wear-resisting, hardness is high, corrosion-resistant and Al contained Ni coating that bonding force is high, pollution-free in preparation process.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of utilizing pulse plating to prepare the Al contained Ni composite deposite said method comprising the steps of:
Step 1: at first remove its oxide film with NaOH solution alkali cleaning aluminium powder, the container that aluminium powder and plating bath are housed is put into agitator heating in water bath and stirring; Adopt electroless plating method in the single nickel salt system at the aluminium powder plating nickel on surface;
Step 2: the anode and cathode material for pulse plating carries out pre-treatment; Select the cathode material of copper sheet conduct for use, use sulphuric acid soln as pickle solution;
Step 3: the composition of pulse plating plating bath is specially: single nickel salt 300.0 ~ 333.0g/L, sal epsom 9.8 ~ 14.7g/L, sodium-chlor 10.0 ~ 20.0g/L, boric acid 30.0 ~ 40.0g/L, oxalic acid 18.0 ~ 26.0g/L, the preparation sodium lauryl sulphate is as wetting agent 0.5 ~ 0.8g/l; With above-mentioned medicine heating for dissolving, greeny plating bath poured in the plating tank fully stir with agitator, make that various compositions mix in the plating bath;
Step 4: use plating tank, plating bath pH is 4.7 ~ 5.8, and negative electrode connects the copper sheet of having handled, and anode connects the nickel sheet, all puts in the plating bath, picks up counting, and with the monopulse power supply opening, cathode current density is 3A/dm
2, frequency is 800Hz, and dutycycle is 2:1, pours the Al contained Ni that has plated in the step 1 into plating bath again and stirs, and timing was taken out copper sheet after 2 ~ 4 hours from plating bath, namely obtain the Al contained Ni composite deposite.
Described a kind of method of utilizing pulse plating to prepare the Al contained Ni composite deposite, the moiety of chemical plating fluid in the described step 1: single nickel salt 250g/l, inferior sodium phosphate 90g/l, Trisodium Citrate 35 g/l, citric acid 9g/l, thiocarbamide 4g/l; The pH value 11.0 of plating bath, plating bath bath temperature are 88 ℃.
Described a kind of method of utilizing pulse plating to prepare the Al contained Ni composite deposite, in the described step 2 with volume fraction be 10% sulphuric acid soln as the pickle solution of copper sheet, carry out the weak etch of chemistry with 10% dilute sulphuric acid then.
Described a kind of method of utilizing pulse plating to prepare the Al contained Ni composite deposite, the temperature of pulse plating plating bath is 40 ~ 60 ℃ in the described step 3, the stirring velocity of magnetic stirring apparatus is 200 ~ 500r/min.
Advantage of the present invention and effect are:
The present invention overcomes in the past dc electrodeposition method and prepares shortcomings such as the burning of coating, decortication, pin hole or burr, and the Al contained Ni coating surface of preparation is comparatively even, and is fine and close smooth, and crystal grain is tiny.Compare with the coating of conventional DC electrodip process preparation and to have many good qualities, low as the coating porosity, make the coating surface light fine and close, can increase the density of coating, increase hardness, improve its erosion resistance and wear resistance, improved the physicals of coating.So the quality of coating of pulse composite plating and performance thereof all are better than traditional direct current electrode position, so it has the trend of the traditional direct current electrode position of further replacement.The composite plating layer porosity is low, have high rigidity, wear resistance, self lubricity, thermotolerance, solidity to corrosion can prepare under low temperature and normal pressure, can also be by changing the matrix material that matrix metal and disperse particles method can obtain specific function.Electroplating its advantage of preparation matrix material has: the preparation process temperature is low, less investment, composite deposite are formed variation, saved material etc., and compound plating is an important method of preparation matrix material.
Embodiment
The present invention is described in detail below in conjunction with embodiment.
Aluminium powder of the present invention (13 ± 2 μ m) 10g generates Al contained Ni 85 ℃ of left and right sides electroless platings, and the product Al contained Ni output after the electroless plating is high especially, and its quality is 39g.In 50 ~ 60 ℃ electroplate liquid, add the Al contained Ni solid particulate, heat simultaneously and stir.Negative electrode is the copper sheet after the surface treatment, and anode is thin nickel sheet, begins to electroplate.In electroplating process, unavoidably can generate hydrogen on the negative electrode.Hydrogen separate out the electrodepositing speed that not only can slow down, also can make coating surface pin hole occur simultaneously.So in plating bath, add a small amount of sodium lauryl sulphate as wetting agent, thereby reduce or prevent the generation of coating pin hole.Through repetition test, thereby reached comparatively desirable effect.The present invention is main raw material with the aluminium powder.Aluminium powder exposes easy oxidation in air, the surface generates aluminum oxide, and can not carry out the plating of nickel on alumina surface, so want to remove the aluminum oxide on the surface of aluminum particle with sodium hydroxide earlier.Control the pH of solution again, use electroless plating method, the nickel content that plates on the Fine Aluminum Powder of preparing is higher, and the content of phosphorus is lower, for next step experiment is laid a good foundation.In the compound electroplating process of pulse, by the control processing parameter, successfully preparation is sent as an envoy to the substrate copper sheet wear-resistant, the Al contained Ni coating that further improves on the performances such as corrosion resistant.In order to improve the Al contained Ni coating performance, in reaction process, also utilized buffer reagent (boric acid), wetting agent (sodium lauryl sulphate) etc.The condition of pulse plating is cathode current density 3A/dm2, plating time 2 ~ 4 hours, and 40 ~ 60 ℃ of bath temperatures, stirring velocity is 200 ~ 500r/min.
Embodiment:
Step 1: be that 13 ± 2 μ m aluminium powders are removed its oxide film with NaOH solution alkali cleaning particle diameter at first, the beaker that aluminium powder and plating bath are housed is put into constant temperature blender with magnetic force heating in water bath and stirring; At the aluminium powder plating nickel on surface, the Al contained Ni of formation is done the dispersion agent of next step compound plating to the employing electroless plating method in the single nickel salt system; Plate Al contained Ni outward appearance rule, the coating even compact, thickness is moderate, the nickel al proportion meets the compound plating requirement of next stage pulse.
Step 2: the anode and cathode material for pulse plating carries out pre-treatment.Select the cathode material of copper sheet conduct for use, with the sand paper of different model it is polished, clean, with volume fraction be 10% sulphuric acid soln as pickle solution, about 2min of pickling time adopts 10% dilute sulphuric acid to carry out etch a little less than the chemistry, about 0.5min of time takes out back distilled water flushing, drying.Anode material is that purity is 99.99% pure nickel, immerses the about 60s of 10% sulphuric acid soln, takes out after washing, and acetone is washed, and dries up.
Step 3: the composition of pulse plating plating bath is specially: single nickel salt 300.0 ~ 333.0g/L, sal epsom 9.8 ~ 14.7g/L, sodium-chlor 10.0 ~ 20.0g/L, boric acid 30.0 ~ 40.0g/L, oxalic acid 18.0 ~ 26.0g/L, the preparation sodium lauryl sulphate is as wetting agent 0.5 ~ 0.8g/l.With above-mentioned medicine heating for dissolving, greeny plating bath poured in the plating tank fully stir with heat collecting type thermostatically heating magnetic stirring apparatus, make that various compositions mix in the plating bath.Before plating, earlier plating bath is heated to the temperature of regulation, Heating temperature is set at 40 ~ 60 ℃, and stirring velocity is 200 ~ 500r/min.
Step 4: use the 2.5L beaker to make plating tank, plating bath pH is 4.7 ~ 5.8.Negative electrode connects the copper sheet of having handled, and anode connects the nickel sheet, all puts in the plating bath, picks up counting, and with the monopulse power supply opening, cathode current density is 3A/dm2, and frequency is 800Hz, and dutycycle is 2:1.Pour the Al contained Ni that has plated in the step 1 into plating bath again and stir, timing was taken out copper sheet after 2 ~ 4 hours from plating bath, obtained the Al contained Ni composite deposite.
The moiety of chemical plating fluid in the step 1: single nickel salt 250g/l, inferior sodium phosphate 90g/l, Trisodium Citrate 35 g/l, citric acid 9g/l, thiocarbamide 4g/l; The pH value 11.0 of plating bath, plating bath bath temperature are 88 ℃.
Preparation by this invention paired pulses is electroplated Al contained Ni coating mainly contains two processes of electroless plating and pulse composite plating.With regard to electroless plating, if bath pH value is too high, can cause the spontaneous decomposition of plating bath easily, the reaction that the too high meeting of pH value makes hypophosphite in the plating bath be oxidized to phosphite is accelerated, and makes reaction be converted into spontaneous reaction by catalyzed reaction, makes the very fast inefficacy of plating bath.If pH is low excessively, along with the deposition of nickel-phosphorus, H+ constantly generates, and the structure of complexing agent and sedimentation rate are affected.When temperature was higher than 90 ℃, though the content of nickel plating also can increase in theory on the aluminium powder, the too high meeting of temperature caused the plating bath instability, be easy to decompose, from and can have influence on the content of aluminium powder nickel plating.So select suitable pH and bath temperature etc. very important to the nickel content of electroless plating product.
In the compound electroplating process of pulse, Al contained Ni is as the disperse phase of pulse plating Al contained Ni.In electroplate liquid, except main salt, need to add complexing agent, stablizer, conductive agent and other reagent, to guarantee carrying out smoothly of pulse plating.Al contained Ni concentration and stirring velocity etc. are different to the influence of coating fraction of coverage in different duty, frequency, current density, bath pH value, bath temperature, the plating bath.In general, under suitable processing parameter, the Al contained Ni coating after the plating and the combination of copper matrix are good, do not occur burning, defectives such as crackle, foaming, decortication, dark evil spirit, pit and striped.The wear resistance of Al contained Ni coating obviously improves, and compares with common copper sheet, and wear resistance improves more than 3 times.Obtain the Al contained Ni coating of high-quality thus.
Claims (4)
1. a method of utilizing pulse plating to prepare the Al contained Ni composite deposite is characterized in that, said method comprising the steps of:
Step 1: at first remove its oxide film with NaOH solution alkali cleaning aluminium powder, the container that aluminium powder and plating bath are housed is put into agitator heating in water bath and stirring; Adopt electroless plating method in the single nickel salt system at the aluminium powder plating nickel on surface;
Step 2: the anode and cathode material for pulse plating carries out pre-treatment; Select the cathode material of copper sheet conduct for use, use sulphuric acid soln as pickle solution;
Step 3: the composition of pulse plating plating bath is specially: single nickel salt 300.0 ~ 333.0g/L, sal epsom 9.8 ~ 14.7g/L, sodium-chlor 10.0 ~ 20.0g/L, boric acid 30.0 ~ 40.0g/L, oxalic acid 18.0 ~ 26.0g/L, the preparation sodium lauryl sulphate is as wetting agent 0.5 ~ 0.8g/l; With above-mentioned medicine heating for dissolving, greeny plating bath poured in the plating tank fully stir with agitator, make that various compositions mix in the plating bath;
Step 4: use plating tank, plating bath pH is 4.7 ~ 5.8, and negative electrode connects the copper sheet of having handled, and anode connects the nickel sheet, all puts in the plating bath, picks up counting, and with the monopulse power supply opening, cathode current density is 3A/dm
2, frequency is 800Hz, and dutycycle is 2:1, pours the Al contained Ni that has plated in the step 1 into plating bath again and stirs, and timing was taken out copper sheet after 2 ~ 4 hours from plating bath, namely obtain the Al contained Ni composite deposite.
2. a kind of method of utilizing pulse plating to prepare the Al contained Ni composite deposite according to claim 1 is characterized in that, the moiety of chemical plating fluid in the described step 1: single nickel salt 250g/l, inferior sodium phosphate 90g/l, Trisodium Citrate 35 g/l, citric acid 9g/l, thiocarbamide 4g/l; The pH value 11.0 of plating bath, plating bath bath temperature are 88 ℃.
3. a kind of method of utilizing pulse plating to prepare the Al contained Ni composite deposite according to claim 1, it is characterized in that, in the described step 2 with volume fraction be 10% sulphuric acid soln as the pickle solution of copper sheet, carry out the weak etch of chemistry with 10% dilute sulphuric acid then.
4. a kind of method of utilizing pulse plating to prepare the Al contained Ni composite deposite according to claim 1 is characterized in that, the temperature of pulse plating plating bath is 40 ~ 60 ℃ in the described step 3, and the stirring velocity of magnetic stirring apparatus is 200 ~ 500r/min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103611931A (en) * | 2013-12-18 | 2014-03-05 | 江苏科技大学 | Method for preparing nickel-coated copper composite powder in laboratory through electroplating |
| CN104278301A (en) * | 2014-10-23 | 2015-01-14 | 上海应用技术学院 | Nickel-molybdenum-aluminium coating and preparation method thereof |
| CN106077670A (en) * | 2016-08-03 | 2016-11-09 | 杭州科技职业技术学院 | Composite codeposition co-sintering prepares the method for superfine alloy powder |
| WO2018150277A1 (en) * | 2017-02-14 | 2018-08-23 | Volkswagen Ag | Electric vehicle battery cell with solid state electrolyte |
| US10797284B2 (en) | 2017-02-14 | 2020-10-06 | Volkswagen Ag | Electric vehicle battery cell with polymer frame for battery cell components |
| CN113186571A (en) * | 2021-04-29 | 2021-07-30 | 广西大学 | Al for radiation protection of stainless steel2O3Preparation method of composite coating |
| US11362371B2 (en) | 2017-02-14 | 2022-06-14 | Volkswagen Ag | Method for manufacturing electric vehicle battery cells with polymer frame support |
| US11870028B2 (en) | 2017-02-14 | 2024-01-09 | Volkswagen Ag | Electric vehicle battery cell with internal series connection stacking |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103611931A (en) * | 2013-12-18 | 2014-03-05 | 江苏科技大学 | Method for preparing nickel-coated copper composite powder in laboratory through electroplating |
| CN104278301A (en) * | 2014-10-23 | 2015-01-14 | 上海应用技术学院 | Nickel-molybdenum-aluminium coating and preparation method thereof |
| CN104278301B (en) * | 2014-10-23 | 2016-09-14 | 上海应用技术学院 | A kind of nickel molybdenum aluminium coat and preparation method thereof |
| CN106077670A (en) * | 2016-08-03 | 2016-11-09 | 杭州科技职业技术学院 | Composite codeposition co-sintering prepares the method for superfine alloy powder |
| CN106077670B (en) * | 2016-08-03 | 2018-07-24 | 杭州科技职业技术学院 | The method that composite codeposition-co-sintering prepares superfine alloy powder |
| WO2018150277A1 (en) * | 2017-02-14 | 2018-08-23 | Volkswagen Ag | Electric vehicle battery cell with solid state electrolyte |
| US10797284B2 (en) | 2017-02-14 | 2020-10-06 | Volkswagen Ag | Electric vehicle battery cell with polymer frame for battery cell components |
| US11362338B2 (en) | 2017-02-14 | 2022-06-14 | Volkswagen Ag | Electric vehicle battery cell with solid state electrolyte |
| US11362371B2 (en) | 2017-02-14 | 2022-06-14 | Volkswagen Ag | Method for manufacturing electric vehicle battery cells with polymer frame support |
| US11870028B2 (en) | 2017-02-14 | 2024-01-09 | Volkswagen Ag | Electric vehicle battery cell with internal series connection stacking |
| CN113186571A (en) * | 2021-04-29 | 2021-07-30 | 广西大学 | Al for radiation protection of stainless steel2O3Preparation method of composite coating |
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Application publication date: 20131002 |