CN102220574A - Chemical nickel-phosphorus plating method on surface of zirconium-aluminum alloy - Google Patents
Chemical nickel-phosphorus plating method on surface of zirconium-aluminum alloy Download PDFInfo
- Publication number
- CN102220574A CN102220574A CN2011101433660A CN201110143366A CN102220574A CN 102220574 A CN102220574 A CN 102220574A CN 2011101433660 A CN2011101433660 A CN 2011101433660A CN 201110143366 A CN201110143366 A CN 201110143366A CN 102220574 A CN102220574 A CN 102220574A
- Authority
- CN
- China
- Prior art keywords
- zirconium
- deionized water
- plating
- zirconium alloy
- nickel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention discloses a chemical nickel-phosphorus plating method on the surface of a zirconium-aluminum alloy. The method comprises the following steps of: (1) after preparing zirconium and aluminum according to a certain proportion, repeatedly melting to uniformize the components; (2) linearly cutting the prepared zirconium-aluminum alloy according to a certain size, polishing by using abrasive papers with the different finenesses, and carrying out alkali washing after ultrasonically cleaning by using deionized water and acetone; (3) placing a test sample in a mixed solution of HF, HNO3 and H2O for 10-30 s; (4) phosphating or performing zinc dipping; and (5) performing chemical plating, wherein the chemical plating can be neutral or acidic chemical plating. According to the method disclosed by the invention, a uniform and compact nickel-phosphorus coating with a thickness of 10-20 mum can be prepared on the surface of the zirconium-aluminum alloy, so that the abrasion corrosion resistance of the zirconium alloy is obviously improved. The method has a wide application range; and bright and compact nickel-phosphorus coatings with excellent abrasion corrosion resistance and firm combination with a substrate, can be formed on the zirconium-aluminum alloys with different components. The method disclosed by the invention is particularly suitable for strengthening parts with complex shapes.
Description
Technical field
The present invention relates to a kind of method of the surface chemical Ni-P-plating at zirconium alloy, belong to alloy surface plated film intensive treatment technical field.
Background technology
1824, emanate out the first zirconium of laboratory quantity of Berzelius, from then on zirconium enters people's the visual field and is subjected to paying close attention to widely.Zirconium has been applied to various fields at present, for example is used for electronic industry, as the absorption agent and the manufacturing valve tube part of residual gas.Its good solidity to corrosion makes it can make surgical technique and tools, chemical industry equipment, electric parts, jewelry.Zirconium powder can be used for photoflash lamp powder, flicker signal, fireworks and detonator etc.Zirconium has low thermal neutron absorption cross section, good solidity to corrosion, and higher heat conductivity, zirconium alloy is used widely as the nuclear industry fuel canning material.Zirconium is to have excellent corrosion resistance, anti-irradiation, and the coefficient of expansion is little, structure and dimensional stabilizing, reserves are abundant, are expected to replace stainless steel, GCr15 to be applied to the space operation structure unit, bear the influence of space irradiation, atomic oxygen, low temperature and alternating temperature-changing.Yet the tensile strength of pure zirconium (Zr) has only 300MPa, and corrosive nature is very unstable, can not satisfy service requirements as structural part.Add a spot of alloy element Al and prepare zirconium alloy and form the mechanical property that strengthening phase can significantly improve zirconium alloy, satisfy space structure spare performance requriements at the zirconium matrix.The corrosion of zirconium alloy in the High Temperature High Pressure deionized water is divided into two stages usually, and at the corrosion initial stage, the surface generates the black oxide film of one deck densification, and erosion rate changes more and more lower in time; Erosion rate increases suddenly subsequently, generates the white oxide film that does not have protectiveness.Therefore be necessary zirconium alloy is carried out surface treatment, improve its solidity to corrosion.As space structure spare, it also is necessary keeping certain wear resistance.
In the prior art, improve the method that the corrosion proof method of zirconium alloy normally adopts alloying, add the disadvantageous effect that an amount of Sn can suppress N, in the having influence on to a certain degree of carbon and aluminium.Adding a spot of Fe, Cr or Ni can postpone to take place the time that corrosion fast takes place.Do not appear in the newspapers and adopt surface treatment to improve its Research on Corrosion Resistance to zirconium alloy.
Summary of the invention
The purpose of this invention is to provide a kind of method, improved the wear resistance and the solidity to corrosion of zirconium alloy, and can make zirconium alloy obtain good comprehensive performances at the zirconium alloy surface chemical Ni-P-plating.
The present invention is achieved by the following technical solutions;
Method of the present invention may further comprise the steps:
(1) zirconium, aluminium are prepared in proportion the back melt back, made composition even, obtain zirconium alloy;
(2) the zirconium alloy line for preparing is cut into a certain size, polish successively, make the alloy surface smooth with 280,600,800,1000 purpose sand paper;
(3) after successively immersing in deionized water, the acetone, in ultrasonic cleaner, cleans by the zirconium alloy sample that obtains 5～10min, putting into temperature again and be 50～60 ℃, mass concentration is 40～60g/LNaOH solution alkali cleaning, 10～15min, rinses well with deionized water then;
(4) pickling alligatoring
The sample that step (3) obtains is put into HF: HNO
3: H
2O is 5 by volume: (30～45): in the mixed solution of (50～65), carry out the pickling alligatoring, time 10～30s rinses well with deionized water;
(5) phosphatization or soak zinc and handle
1. bonderizing:
Treatment solution is composed as follows: ortho-phosphoric acid 10～25g/L, zinc sulfate 20～50g/L, NaF 1～3g/L, organosulfur 0.1～0.3g/L;
Control pH 2～3,40～55 ℃ of temperature, time 1～3min; Rinse well with deionized water;
2. soaking zinc handles:
Treatment solution is composed as follows: zinc sulfate 25～35g/L, trisodium phosphate 110～130g/L, yellow soda ash 4～7g/L;
Control pH 9～11,70～85 ℃ of temperature, time 5～12min rinses well with deionized water;
(6) chemical nickel phosphorus plating
Method has following two kinds:
1. adopt neutral electroless plating:
Plating bath is composed as follows: single nickel salt 15～25g/L, reductive agent sodium hypophosphite 35～45g/L, ammonium sulfate 30～50g/L, sodium acetate 30～50g/L, lead acetate 0.5～1.5mg/L;
Control pH 6～7,70～80 ℃ of temperature, time 40～60min;
2. or adopt acid chemical plating:
Plating bath is composed as follows: main salt single nickel salt 20～35g/L, reductive agent sodium hypophosphite 20～40g/L, lactic acid 15～25g/L, sodium acetate 30～40g/L;
Control pH 4～5,70～85 ℃ of temperature, the time is 40～60min;
(7) use deionized water rinsing, dry up, obtain surface-brightening, densification, firm with matrix bond, thickness is the nickel-phosphorus coating of 10～20 μ m.
The beneficial effect that the present invention obtains is, suitability of the present invention is wide, the zirconium alloy of heterogeneity respectively by bonderizing and soak zinc handle the back electroless plating all can obtain light fine and close, with the nickel-phosphorus coating of firm, the anti-corrosion resistance to abrasion excellence of matrix bond.
Embodiment
Following examples are used to illustrate the present invention.The following examples are to be to implement under the prerequisite in technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention are not limited only to the following examples.
Embodiment 1
(1) be that 8.8% zirconium, aluminium are prepared the back melt back in proportion with the massfraction of aluminium, it is even to reach composition, obtains zirconium alloy;
(2) the zirconium alloy line for preparing is cut into 15 * 5 * 3mm size;
(3) prepare the nickel-phosphorus chemical plating bath, the chemical constitution of this plating bath is as follows:
Main salt single nickel salt 20g/L, reductive agent sodium hypophosphite 40g/L, ammonium sulfate 40g/L, sodium acetate 40g/L, lead acetate 1mg/L;
(4) zirconium alloy is carried out mechanical grinding, polish successively with 400,600,800,1000 purpose sand paper, make the surfacing light, carry out ultrasonic cleaning then, ultrasonic cleaning is zirconium alloy successively to be immersed clean 5min in deionized water, the acetone afterwards in ultrasonic cleaner, remove degrease, with deionized water rinsing and dry up;
(5) carry out alkali cleaning then, purpose is for further removing the grease on zirconium alloy surface, and alkaline wash is the sodium hydroxide solution of 60g/L, puts into zirconium alloy after being heated 60 ℃, and the time is 10min.Subsequently with deionized water rinsing and dry up;
(6) carry out pickling then, the pickle solution prescription is: hydrofluoric acid, the volume ratio of nitric acid and water are 5: 35: 60, and pickling time 20s is afterwards with deionized water rinsing and dry up;
(7) carry out bonderizing then, phosphatization liquid is composed as follows: phosphatase 11 5g/L, zinc sulfate 40g/L, Sodium Fluoride 1.5g/L, thiocarbamide 0.15g/L, 45 ℃ of temperature, pH is 2.5, time 3min, after the phosphatization with washed with de-ionized water and dry up;
(8) carry out the processing sequence of chemical nickel phosphorus plating then: above-mentioned treated zirconium alloy is put into the ready chemical plating fluid of step (3), and temperature is controlled at about 80 ℃, and the pH regulator of solution is about 6.8, and plating time is 60min;
(9) then with washed with de-ionized water and dry up, had the nickel-phosphorus alloy coating of metalluster uniformly, thickness of coating is 15～20 μ m.
Embodiment 2
(1) be that 8.0% zirconium, aluminium are prepared the back melt back in proportion with the massfraction of aluminium, it is even to reach composition;
(2) electroplate liquid formulation of present embodiment and step (2) (3) (4) (5) and (8) and above-mentioned enforcement 1 are identical, and different is step (6) and (7).
The used pickle solution of the step of present embodiment (6) is identical with example 1, and difference is that the time is 10s.
The step of present embodiment (7) is for soaking zinc, and zincate solution consists of: zinc sulfate 30g/L, and trisodium phosphate 120g/L, the aqueous solution of yellow soda ash 5g/L, pH is 10, is heated 80 ℃, puts into zirconium alloy, galvanizing time 10min.
Present embodiment can obtain to have the nickel-phosphorus alloy coating of metalluster at last on the zirconium alloy surface, thickness of coating is 15～20 μ m.
Embodiment 3
The technological process of present embodiment and step and the foregoing description 1 are identical, and different is the prescription of its chemical plating fluid.
The plating bath chemical constitution of present embodiment is:
Main salt single nickel salt 28g/L
Reductive agent sodium hypophosphite 30g/L
Lactic acid 20g/L
Sodium acetate 35g/L
Then, (2) (3) (4) (5) (6) and (7) among its technological process and step and the embodiment 1 are identical.The chemical nickel plating pH regulator is about 4.5, and temperature is controlled at 75 ℃, and plating time is 60min.Present embodiment can obtain to have the nickel-phosphorus alloy coating of metalluster at last on the zirconium alloy surface, thickness of coating is 15～20 μ m.
Embodiment 4
(1) is that 8.4% zirconium, aluminium are prepared the back melt back in proportion with the massfraction of aluminium, makes composition even;
(2) the zirconium alloy line for preparing is cut into 12 * 5 * 3mm size;
(3) prepare the nickel-phosphorus chemical plating bath, the chemical constitution of this plating bath is as follows:
Main salt single nickel salt 30g/L, reductive agent sodium hypophosphite 35g/L, lactic acid 20g/L, sodium acetate 30g/L;
(4) zirconium alloy is carried out mechanical grinding, polish successively with 400,600,800,1000 purpose sand paper, make the surfacing light, carry out ultrasonic cleaning then, ultrasonic cleaning is zirconium alloy successively to be immersed clean 5min in deionized water, the acetone afterwards in ultrasonic cleaner, remove degrease, with deionized water rinsing and dry up;
(5) carry out alkali cleaning then, purpose is for further removing the grease on zirconium alloy surface; Alkaline wash is the sodium hydroxide solution of 60g/L, puts into zirconium alloy after being heated 60 ℃, and the time is 10min.Subsequently with deionized water rinsing and dry up;
(6) carry out pickling then, the pickle solution prescription is a hydrofluoric acid, and the volume ratio of nitric acid and water is 5: 40: 55, and pickling time 10s is afterwards with deionized water rinsing and dry up;
(7) soak zinc then and handle, zincate solution is composed as follows: zinc sulfate 32g/L, and trisodium phosphate 115g/L, the aqueous solution of yellow soda ash 6g/L, pH is 9.5, is heated 75 ℃, puts into zirconium alloy, galvanizing time 10min.
(8) carry out the processing sequence of chemical nickel phosphorus plating then, above-mentioned treated zirconium alloy is put into the chemical plating fluid of step (3) preparation, temperature is controlled at about 80 ℃, and the pH regulator of solution is about 4.8, and plating time is 50min;
(9) then with washed with de-ionized water and dry up, had the nickel-phosphorus alloy coating of metalluster uniformly, thickness of coating is 15～20 μ m.
Claims (1)
1. method at the zirconium alloy surface chemical Ni-P-plating is characterized in that may further comprise the steps:
(1) zirconium, aluminium are prepared in proportion the back melt back, made composition even, obtain zirconium alloy;
(2) the zirconium alloy line for preparing is cut into a certain size, polish successively, make the alloy surface smooth with 280,600,800,1000 purpose sand paper;
(3) after successively immersing in deionized water, the acetone, in ultrasonic cleaner, cleans by the zirconium alloy sample that obtains 5～10min, putting into temperature again and be 50～60 ℃, mass concentration is 40～60g/LNaOH solution alkali cleaning, 10～15min, rinses well with deionized water then;
(4) pickling alligatoring
The sample that step (3) obtains is put into HF: HNO
3: H
2O is 5 by volume: (30～45): in the mixed solution of (50～65), carry out the pickling alligatoring, time 10～30s rinses well with deionized water;
(5) phosphatization or soak zinc and handle
1. bonderizing:
Treatment solution is composed as follows: ortho-phosphoric acid 10～25g/L, zinc sulfate 20～50g/L, NaF 1～3g/L, organosulfur 0.1～0.3g/L;
Control pH2～3,40～55 ℃ of temperature, time 1～3min; Rinse well with deionized water;
2. soaking zinc handles:
Treatment solution is composed as follows: zinc sulfate 25～35g/L, trisodium phosphate 110～130g/L, yellow soda ash 4～7g/L;
Control pH9～11,70～85 ℃ of temperature, time 5～12min rinses well with deionized water;
(6) chemical nickel phosphorus plating
Method has following two kinds:
1. adopt neutral electroless plating:
Plating bath is composed as follows: single nickel salt 15～25g/L, reductive agent sodium hypophosphite 35～45g/L, ammonium sulfate 30～50g/L, sodium acetate 30～50g/L, lead acetate 0.5～1.5mg/L;
Control pH6～7,70～80 ℃ of temperature, time 40～60min;
2. or adopt acid chemical plating:
Plating bath is composed as follows: main salt single nickel salt 20～35g/L, reductive agent sodium hypophosphite 20～40g/L, lactic acid 15～25g/L, sodium acetate 30～40g/L;
Control pH4～5,70～85 ℃ of temperature, the time is 40～60min;
(7) use deionized water rinsing, dry up, obtain surface-brightening, densification, firm with matrix bond, thickness is the nickel-phosphorus coating of 10～20 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110143366 CN102220574B (en) | 2011-05-31 | 2011-05-31 | Chemical nickel-phosphorus plating method on surface of zirconium-aluminum alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110143366 CN102220574B (en) | 2011-05-31 | 2011-05-31 | Chemical nickel-phosphorus plating method on surface of zirconium-aluminum alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102220574A true CN102220574A (en) | 2011-10-19 |
| CN102220574B CN102220574B (en) | 2013-01-09 |
Family
ID=44777270
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110143366 Expired - Fee Related CN102220574B (en) | 2011-05-31 | 2011-05-31 | Chemical nickel-phosphorus plating method on surface of zirconium-aluminum alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102220574B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586742A (en) * | 2011-11-30 | 2012-07-18 | 余姚康富特电子材料有限公司 | Manufacture method of target material structure |
| CN105937026A (en) * | 2016-06-25 | 2016-09-14 | 安徽柒柒塑业有限公司 | Chemical nickel plating process of aluminum alloy |
| CN107779713A (en) * | 2017-09-30 | 2018-03-09 | 中国科学院长春光学精密机械与物理研究所 | A kind of beryllium alumin(i)um alloy and preparation method thereof |
| CN108728854A (en) * | 2018-05-15 | 2018-11-02 | 安徽德斯兰卡铝业科技有限公司 | A kind of cleaning of aluminium section bar |
| CN110205662A (en) * | 2019-06-27 | 2019-09-06 | 安徽鼎旺环保材料科技有限公司 | A kind of aluminium alloy surface electric plating preprocess method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4284660A (en) * | 1978-05-11 | 1981-08-18 | General Electric Company | Electroless deposition process for zirconium and zirconium alloys |
| RU2415967C2 (en) * | 2009-06-08 | 2011-04-10 | Учреждение Российской Академии Наук Институт Проблем Сверхпластичности Металлов Ран | Procedure for covering work pieces out of metals and alloys with protective coating |
| CN102051604A (en) * | 2009-10-30 | 2011-05-11 | 海洋王照明科技股份有限公司 | Austenitic stainless steel surface chemical nickel-phosphorus plating method |
-
2011
- 2011-05-31 CN CN 201110143366 patent/CN102220574B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4284660A (en) * | 1978-05-11 | 1981-08-18 | General Electric Company | Electroless deposition process for zirconium and zirconium alloys |
| RU2415967C2 (en) * | 2009-06-08 | 2011-04-10 | Учреждение Российской Академии Наук Институт Проблем Сверхпластичности Металлов Ран | Procedure for covering work pieces out of metals and alloys with protective coating |
| CN102051604A (en) * | 2009-10-30 | 2011-05-11 | 海洋王照明科技股份有限公司 | Austenitic stainless steel surface chemical nickel-phosphorus plating method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586742A (en) * | 2011-11-30 | 2012-07-18 | 余姚康富特电子材料有限公司 | Manufacture method of target material structure |
| CN102586742B (en) * | 2011-11-30 | 2013-12-11 | 余姚康富特电子材料有限公司 | Manufacture method of target material structure |
| CN105937026A (en) * | 2016-06-25 | 2016-09-14 | 安徽柒柒塑业有限公司 | Chemical nickel plating process of aluminum alloy |
| CN107779713A (en) * | 2017-09-30 | 2018-03-09 | 中国科学院长春光学精密机械与物理研究所 | A kind of beryllium alumin(i)um alloy and preparation method thereof |
| CN108728854A (en) * | 2018-05-15 | 2018-11-02 | 安徽德斯兰卡铝业科技有限公司 | A kind of cleaning of aluminium section bar |
| CN110205662A (en) * | 2019-06-27 | 2019-09-06 | 安徽鼎旺环保材料科技有限公司 | A kind of aluminium alloy surface electric plating preprocess method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102220574B (en) | 2013-01-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101709459B (en) | Surface treatment method of aluminum alloy and treatment liquid | |
| CN102220574B (en) | Chemical nickel-phosphorus plating method on surface of zirconium-aluminum alloy | |
| CN100408725C (en) | Process for compound surface sheilding of metal magnesium and magnesium alloy | |
| CN100419120C (en) | Process for silver caating on surface of magnesium and magnesium alloy | |
| CN101768747B (en) | Method for carrying out surface activating treatment on surface of titanium alloy | |
| CN107779713B (en) | A kind of beryllium alumin(i)um alloy and preparation method thereof | |
| CN102220591A (en) | Pickling and passivating treatment process for stainless steel pipes | |
| CN101319316A (en) | Method for chemical nickel plating on aluminum and aluminum alloy surface | |
| JP7096422B2 (en) | How to make a graphene coating layer on a metal surface | |
| CN112410791B (en) | High-speed environment-friendly chemical stripping solution for nickel coating and preparation method thereof | |
| CN107012458A (en) | Aluminium alloy pretreatment liquid and its application method | |
| CN110117783A (en) | A kind of method of Electroless Nickel Plating of Aluminum Alloy mixed metal activation | |
| CN104120470B (en) | Steel and iron parts or zinc alloy diecasting are without the cyanogen pre-leaching copper method of monovalence copper | |
| CN101962761B (en) | Preparation method of bionic hydrophobic coating on surface of magnesium alloy | |
| CN104087927B (en) | Magnesium-alloy material surface modifying treatment | |
| CN102605358A (en) | Application of chemical plating nickel phosphorus alloy to triallyl cyanurate (TAC) film production line | |
| CN110484919A (en) | The method and surface of decoating liquid and its stripping titanium-containing film are formed with the strip method of the substrate of titanium-containing film | |
| CN103215574B (en) | Magnesium-alloy chemical nickel plating solution and nickel plating process thereof | |
| CN101173362A (en) | Magnesium alloy chemical milling and processing technique | |
| CN101748353B (en) | Method for antiseptic treatment of marine climate resistant engineering component | |
| CN102517570A (en) | Environment-friendly magnesium and magnesium alloy chemical nickel phosphor plating process | |
| CN100402699C (en) | Method for chemical plating of nickel-boron alloy on magnesium alloy surface | |
| CN105525282B (en) | A kind of alkalescence chromium-free passivation liquid and its normal temperature passivated Electroless Plating Ni P layers of method | |
| CN101812655A (en) | 0Cr17Ni14Mo2 hot dip rare earth aluminum alloy coating technology | |
| CN101831645B (en) | Cemented carbide steelwork surface electroless copper plating method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130109 Termination date: 20130531 |