CN102517547B - Method for plating aluminum film or aluminum-tin alloy film on surface of continuous aluminum rolling plate in vacuum gas phase sedimentation method - Google Patents
Method for plating aluminum film or aluminum-tin alloy film on surface of continuous aluminum rolling plate in vacuum gas phase sedimentation method Download PDFInfo
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Abstract
The invention belongs to the field of mirror finishing of aluminum rolling plates and particularly provides a method for plating an aluminum film or an aluminum-tin alloy film on the surface of a continuous aluminum rolling plate in a vacuum gas phase sedimentation method. The method comprises the following steps: substrate pretreatment, roller painting or spraying of a base coat, vacuum gas phase sedimentation plating of the aluminum film or the aluminum-tin alloy film and roller painting or spraying of a finishing coat. The method is high in production efficiency and good in film forming effect, and greatly reduces cost. Light reflection efficiency of a mirror plane plate obtained by the method is higher than 92%, and the method can be widely applied to architectural decoration, lamps and household appliance industry.
Description
Technical field
The invention belongs to the mirror finish field of aluminium roll bending, a kind of method for plating film on surface of continuous aluminium roll bending specifically is provided.
Background technology
Along with the development of economic technology, the application of aluminium plate is increasingly extensive, and especially the minute surface aluminium sheet as a kind of high-end aluminium, more and more is widely used in the fields such as upholstery, mechanical means, solar-powered heating generating.The treatment technology of surface of aluminum plate commonly used is mainly spraying, roller coat or anodic oxidation, with pursue surface of aluminum plate and different-effect.And the processing technology of minute surface aluminium sheet at present the most ripe be mainly mechanical polishing technology and chemical rightenning technology, and the domestic manufacturer that almost there is no maturation at present, this technology is mainly producer's grasps such as SUMITOMO CHEMICAL, and domestic user also mainly obtains the source of goods by import.The technology of the present invention is mainly used in the processing of specular aluminium roll bending, also can be used for the processing of stainless steel mirror board.
Acquisition minute surface aluminium sheet commonly used or the method for mirror face stainless steel plate are the treatment process that mechanical polishing and electrochemical etching combine at present.Its principle is: during mechanical polishing, polishing crop rotation high speed rotating on polishing machine, the operator with polished product surface with suitable pressure by being pressed on polishing wheel, at this moment because rubbing effect produces high temperature, make polished surface easily deform and form one deck " affected layer ".Under the frictional force effect of rotating, some boss on surface is pressed on the one hand, or inserts the position of caving in after a mobile segment distance.Thisly cut the protruding recessed flattening course of filling out, at full speed repeatedly carry out on a large scale, add that the light of rubbing paste turns use into, result just makes original more coarse product surface, becomes level and smooth and light.
Product surface by mechanical polishing is very active, is very easy in airborne oxygen generation oxidizing reaction.Therefore will obtain stable specular layer after mechanical polishing just must be auxiliary with electrochemical etching.The principle of electrochemical etching is: chemical rightenning is to utilize aluminum and its alloy to be produced on selective autolyzing solution effect in acidity or alkaline electrolyte solution, flatten the polishing product surperficial, to reduce the chemical process method of its surfaceness, while is due to the existence of concentrated nitric acid in chemical liquid or the vitriol oil, can make the bright aluminium lamination passivation on surface, be stablized thereby be exposed in air.The purity of aluminium and aluminium alloy has a great impact the quality tool of chemical rightenning, and its purity is higher, quality of finish better, otherwise just poorer.Electrochemical etching is to adopt concise and to the point viscosity liquid film theory to carry out.
The Technology that mechanical polishing adds electrochemical etching technology production aluminium mirror board or stainless steel mirror board has following weak point: (1) is because the acquisition of mirror effect mainly obtains by the mechanical friction effect, thereby production efficiency is low, and energy consumption is high.(2) need in production process to use a large amount of concentrated nitric acids, the vitriol oil or strong phosphoric acid, quantity of wastewater effluent is large, pollutes relatively serious.(3) cost is high: the auxiliary industry average cost with the electrochemical etching technology of mechanical polishing is in 30 yuan/square meter left and right.
The vacuum vapor deposition technology has been widely used in the surface treatment of plastic component at present, and main application fields is extraneous adornment spare or the structural part of the consumer electronics products such as mobile phone, digital camera.The vacuum vapor deposition technology is applied to the surface working of continuous aluminium roll bending and then obtains the specular aluminium roll bending yet there are no relevant report.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of method at continuous aluminium roll bending surface coating, the method production efficiency is high, film-formation result is good, cost significantly descends, and the mirror board reflector efficiency that obtains by method of the present invention＞92% can be widely used in architectural decoration.
Technical scheme of the present invention is:
A kind of method of continuous aluminium roll bending surface vacuum vapour deposition process plating aluminium film or Sn-Al alloy film comprises following concrete steps:
(1) substrate pre-treatment: oil removing → washing → pickling oxide film dissolving → washing → oven dry; Described substrate is aluminium sheet or aluminium roll bending;
(2) roller coat or spraying bottom coating: with pretreated substrate roller coat or spraying one deck organic coating a, then adopting energy is the ultraviolet light polymerization of 800-1200 milli Jiao/square centimeter, and the infrared rays baking 5min-8min of 50 ℃-60 ℃ is provided simultaneously;
The weight part of the main ingredient of described organic coating a is as follows: 30 parts-40 parts of single functionality epoxy resin, 20 parts-25 parts of difunctionality acrylic resins, 15 parts-20 parts of single functionality reactive thinners, 5 parts-10 parts of 1173 or 184 light triggers, 8 parts-10 parts of ethyl esters, 3 parts-5 parts of functional type auxiliary agents;
(3) vacuum vapor deposition plating aluminium film or Sn-Al alloy film: with substrate plated film in vacuum plating unit of first-class undercoat, the target that plated film adopts is aluminum metal or the Sn-Al alloy of purity 〉=99.98%; The pressure-controlling of vacuum chamber is 5 * 10
-3Below Pa, vaporizer adopts boron nitride crucible;
(4) roller coat or spray-coating surface coating: the substrate roller coat after aluminium plating film or Sn-Al alloy film or spraying one deck organic coating b, then adopting energy is the ultraviolet light polymerization of 600-1000 milli Jiao/square centimeter, and the infrared rays baking 5min-8min of 50 ℃-60 ℃ is provided simultaneously, get final product;
The weight part of the main ingredient of described organic coating b is as follows: acrylic resin modified 30 parts-40 parts of single functionality, 20 parts-25 parts of difunctionality acrylic resins, 10 parts-15 parts of difunctionality urethane acrylates, 10 parts-15 parts of single functionality reactive thinners, 4 parts-8 parts of 1173 or 184 light triggers, 5 parts-8 parts of ethyl esters, 3 parts-5 parts of functional type auxiliary agents.
Described in organic coating a and organic coating b, the single functionality reactive thinner is lauric acid methacrylic ester or iso-bornyl acrylate.Described functional type auxiliary agent is selected from second-HEMA phosphoric acid ester, BYK371 flow agent, promotor 1270 or promotor 2325.
The pretreated concrete steps of the described substrate of step (1) are:
A) oil removing: with aluminium sheet or aluminium roll bending in chemical liquid oil removing 1-2 minute, temperature was controlled at 50 ℃-65 ℃; The formula of chemical liquid is: sodium hydroxide 30-50 gram/L, and industrial detergent 0.5-1 milliliter/L, all the other are water;
B) washing: the aluminium flake after electrochemical deoiling or aluminium roll bending are inserted in warm water clean, 35 ℃-45 ℃ of water temperatures, 20 seconds-30 seconds time;
C) pickling oxide film dissolving: the substrate after washing is put into acidic solution and is removed zone of oxidation; Acidic solution is the salpeter solution of every liter of 250-300 milliliter, and the reaction times is controlled at 1min-3min;
D) washing: pickling substrate is later washed 20s-40s in the water of 35 ℃-45 ℃;
E) oven dry: 50 ℃-70 ℃ baking 5min-10min, pre-treatment is completed.
The described primer thickness of step (2) is the 10-12 micron, and hardness of film reaches 0 grade for the thickness of aluminium more than 1H.
The described aluminium film of step (3) or Sn-Al alloy film thickness are the 0.5-1 micron, insulation resistance＞2M ohm, and minute surface is to the reflecting rate of visible light＞92%.
The described finishing coat thickness of step (4) is the 6-10 micron, and hardness of film is more than 1H, and anti-bending reaches the 2T standard, and it is unchanged that salt spray resistance reaches the neutral 5%NaCl aqueous solution 48 hours, and ultraviolet aging resistance reached more than 120 hours.
Step (4) is the plastics film that shields of plating one deck more afterwards.
The below does further explanation and explanation to the present invention:
Vacuum plating unit of the present invention is existing evaporating coating equipment, as the shake ZHL-1800 type high-vacuum resistance evaporation coating machine of magnificent vacuum machine company limited of Zhaoqing.
Single functionality reactive thinner in organic coating a of the present invention and organic coating b is for existing thinner commonly used, as lauric acid methacrylic ester, iso-bornyl acrylate etc.Described functional type auxiliary agent is auxiliary agent commonly used on market, as second-HEMA phosphoric acid ester, German BYK company 371, the adhesion promoter 1270 of Di Gao company, 2325 etc.
The present invention is different from mechanical polishing and electrochemical etching technology commonly used at present fully.The aluminium sheet mirror finish technique of commonly using at present; must adopt the method for mechanical polishing and electrochemical etching combination; because mechanical polishing surface of aluminum plate later is very active; and the reflectance that pure mechanical polishing reaches is also inadequate; must auxiliaryly obtain as bright as a sixpence surface with electrochemical etching; make it reflectance and reach more than 95%, the simultaneous electrochemical polishing is also a process that passivation is stable.By the Passivation Treatment of electrochemistry liquid, the aluminium particulate on surface just is able to stable existence.The mirror board reflector efficiency that obtains by method of the present invention is generally at 92%-94%, only than the method that adopts mechanical polishing and electrochemical etching combination almost, may limit the invention in the application of photovoltaic industry, but as the architectural decoration material, this effect complete enough, and operational path is simple, and cost significantly reduces.
Compared with prior art, advantage of the present invention is:
(1) acquisition due to mirror effect obtains by vacuum gas-phase physical deposition principle, thereby production efficiency is high, and energy consumption is relatively low.Particularly aborning undercoat and finishing coat adopts UV-curing technology, makes the coating that only can complete undercoat or finishing coat about 5-7 minute, and production efficiency is very high.
(2) production process does not need to use concentrated nitric acid, the vitriol oil or the strong phosphoric acid of any component, and sewage discharge is very limited, and the traditional technology pollutant emission reduces more than 80% relatively.
(3) cost is low: the auxiliary industry average cost with the electrochemical etching technology of mechanical polishing is in 30 yuan/square meter left and right, and the vacuum vapor deposition technology obtains the cost of mirror board and can be controlled in 20 yuan/square meter.This shows, cost significantly descends more than 30%.
Embodiment
The present invention will be further explained below in conjunction with specific embodiment, and it not is exhaustive that embodiment just enumerates.
Embodiment 1:
(1) substrate pre-treatment: oil removing → washing → pickling oxide film dissolving → washing → oven dry; Described substrate is aluminium sheet;
A) oil removing: with the oil removing 2 minutes in chemical liquid of aluminium sheet or aluminium roll bending, temperature is controlled at 50 ℃; The formula of chemical liquid is: sodium hydroxide 30 grams/L, industrial detergent are the not FLK-020 type degreaser produced of Shandong cut Science and Technology Ltd. of Jinhua, and 0.5 milliliter/L, all the other are water;
B) washing: the aluminium flake after electrochemical deoiling or aluminium roll bending are inserted in warm water clean, 40 ℃ of water temperatures, 20 seconds time;
C) pickling oxide film dissolving: the substrate after washing is put into acidic solution and is removed zone of oxidation; Acidic solution is the hydrochloric acid soln of 250 milliliters every liter, and the reaction times is controlled at 1min;
D) washing: pickling substrate is later washed 20s in the water of 40 ℃;
E) oven dry: 60 ℃ of baking 7min, pre-treatment is completed.
(2) roller coat or spraying bottom coating: with pretreated substrate roller coat or spraying one deck organic coating a, the infrared rays baking 5min of 50 ℃ is provided, then adopting energy is the ultraviolet light polymerization of 800 milli Jiao/square centimeters, described primer thickness is 10 microns, hardness of film reaches 0 grade for the sticking power of aluminium more than 1H.
The weight part of the main ingredient of described organic coating a is as follows: 30 parts of single functionality epoxy resin, 20 parts of difunctionality acrylic resins, single functionality reactive thinner are 15 parts of lauric acid methacrylic esters, 7 parts of 1173 light triggers, 8 parts of ethyl esters, 12704 parts of promotor;
(3) vacuum vapor deposition plating aluminium film or Sn-Al alloy film: with substrate plated film in vacuum plating unit of first-class undercoat, the target that plated film adopts is that purity is 99.98% aluminum metal or Sn-Al alloy; The pressure-controlling of vacuum chamber is 5 * 10
-3Pa, vaporizer adopts boron nitride crucible; Described aluminium film or Sn-Al alloy film thickness are 0.6 micron, insulation resistance＞2M ohm, and minute surface is 92.8% to the reflecting rate of visible light.
(4) roller coat or spray-coating surface coating: the substrate roller coat after aluminium plating film or Sn-Al alloy film or spraying one deck organic coating b, the infrared rays baking 6min of 50 ℃ is provided, then adopting energy is the ultraviolet light polymerization of 900 milli Jiao/square centimeters, gets final product;
The weight part of the main ingredient of described organic coating b is as follows: acrylic resin modified 30 parts of single functionality, 20 parts of difunctionality acrylic resins, 10 parts of difunctionality urethane acrylates, single functionality reactive thinner are that 10 parts of lauric acid methacrylic esters, 5 parts of 1173 light triggers, 5 parts of ethyl esters, functional type auxiliary agent are 4 parts of BYK371 flow agents (German Bick chemical production).
Described finishing coat thickness is 8 microns, and hardness of film is more than the import pencil 1H of Mitsubishi, and sticking power is 0 grade, and coating is as clear as crystal.
The mirror board that obtains by this technique, the anti-bending of top coat and metal film layer reaches the 2T standard, it is unchanged that salt spray resistance reaches the neutral 5%NaCl aqueous solution 48 hours, the high temperature and humidity test result is: lower 48 hours of 95% humidity and 65 degree celsius temperature conditions are unchanged, ultraviolet aging resistance reached more than 120 hours, reflector efficiency is 92.8%, and cost is low, is about 18 yuan/square meter.
Embodiment 2:
(1) substrate pre-treatment: oil removing → washing → pickling oxide film dissolving → washing → oven dry; Described substrate is the aluminium roll bending;
A) oil removing: with the oil removing 2 minutes in chemical liquid of aluminium sheet or aluminium roll bending, temperature is controlled at 55 ℃; The formula of chemical liquid is: sodium hydroxide 45 grams/L, industrial detergent are the not 1 milliliter/L of FLK-010 type efficient degreasing powder that produces of Shandong cut Science and Technology Ltd. of Jinhua, and all the other are water;
B) washing: the aluminium flake after electrochemical deoiling or aluminium roll bending are inserted in warm water clean, 40 ℃ of water temperatures, 30 seconds time;
C) pickling oxide film dissolving: the substrate after washing is put into acidic solution and is removed zone of oxidation; Acidic solution is the hydrochloric acid soln of 300 milliliters every liter, and the reaction times is controlled at 2min;
D) washing: pickling substrate is later washed 40s in the water of 40 ℃;
E) oven dry: 65 ℃ of baking 6min, pre-treatment is completed.
(2) roller coat or spraying bottom coating: with pretreated substrate roller coat or spraying one deck organic coating a, provide the infrared rays baking 7min of 55 ℃, then adopting energy is the ultraviolet light polymerization of 900 milli Jiao/square centimeters; Described primer thickness is 12 microns, and hardness of film reaches 0 grade for the sticking power of aluminium more than 1H.
The weight part of the main ingredient of described organic coating a is as follows: 40 parts of single functionality epoxy resin, 25 parts of difunctionality acrylic resins, single functionality reactive thinner are that 20 parts of iso-bornyl acrylates, 9 parts of 1173 light triggers, 9 parts of ethyl esters, functional type auxiliary agent are 3.5 parts of 2325 type adhesion promoters (Di Gao company produce);
(3) vacuum vapor deposition plating aluminium film or Sn-Al alloy film: with substrate plated film in vacuum plating unit of first-class undercoat, the target that plated film adopts is that purity is 99.98% aluminum metal or Sn-Al alloy; The pressure-controlling of vacuum chamber is 5 * 10
-3Pa, vaporizer adopts boron nitride crucible; Described aluminium film or Sn-Al alloy film thickness are 0.8 micron, insulation resistance＞2M ohm, and minute surface is 93.5% to the reflecting rate of visible light.
(4) roller coat or spray-coating surface coating: the substrate roller coat after aluminium plating film or Sn-Al alloy film or spraying one deck organic coating b, the infrared rays baking 7min of 55 ℃ is provided, then adopting energy is the ultraviolet light polymerization of 900 milli Jiao/square centimeters, gets final product;
The weight part of the main ingredient of described organic coating b is as follows: acrylic resin modified 40 parts of single functionality, 25 parts of difunctionality acrylic resins, 15 parts of difunctionality urethane acrylates, single functionality reactive thinner are that 15 parts of iso-bornyl acrylates, 6 parts of 1173 light triggers, 6 parts of ethyl esters, functional type auxiliary agent are 4 parts of BYK333 flow agents (German Bick chemical production).
Described finishing coat thickness is 10 microns, more than the hardness of film import pencil 1H of Mitsubishi, and 0 grade of sticking power, paint film is as clear as crystal.
(5) use mechanical peritonaeum equipment to cover PE film, product is shielded.
By the mirror board that this technique obtains, the anti-bending of top coat and metal film layer reaches the 2T standard; It is unchanged that salt spray resistance reaches the neutral 5%NaCl aqueous solution 48 hours; The high temperature and humidity test result is: lower 48 hours of 95% humidity and 65 degree celsius temperature conditions are unchanged; Ultraviolet aging resistance reached more than 120 hours; Mirror board reflector efficiency after this plated film is 93.5%, and cost is low, is about 19 yuan/square meter.
Claims (8)
1. the method for a continuous aluminium roll bending surface vacuum vapour deposition process plating aluminium film or Sn-Al alloy film, is characterized in that, comprises following concrete steps:
(1) substrate pre-treatment: oil removing → washing → pickling oxide film dissolving → washing → oven dry; Described substrate is the aluminium roll bending;
(2) roller coat or spraying bottom coating: with pretreated substrate roller coat or spraying one deck organic coating a, then adopting energy is the ultraviolet light polymerization of 800-1200 milli Jiao/square centimeter, and the infrared rays baking 5min-8min of 50 ℃-60 ℃ is provided simultaneously;
The weight part of the main ingredient of described organic coating a is as follows: 30 parts-40 parts of single functionality epoxy resin, 20 parts-25 parts of difunctionality acrylic resins, 15 parts-20 parts of single functionality reactive thinners, 5 parts-10 parts of 1173 or 184 light triggers, 8 parts-10 parts of ethyl esters, 3 parts-5 parts of functional type auxiliary agents;
(3) vacuum vapor deposition plating aluminium film or Sn-Al alloy film: with substrate plated film in vacuum plating unit of first-class undercoat, the target that plated film adopts is aluminum metal or the Sn-Al alloy of purity 〉=99.98%; The pressure-controlling of vacuum chamber is 5 * 10
-3Below Pa, vaporizer adopts boron nitride crucible;
(4) roller coat or spray-coating surface coating: the substrate roller coat after aluminium plating film or Sn-Al alloy film or spraying one deck organic coating b, then adopting energy is the ultraviolet light polymerization of 600-1000 milli Jiao/square centimeter, and the infrared rays baking 5min-8min of 50 ℃-60 ℃ is provided simultaneously, get final product;
The weight part of the main ingredient of described organic coating b is as follows: acrylic resin modified 30 parts-40 parts of single functionality, 20 parts-25 parts of difunctionality acrylic resins, 10 parts-15 parts of difunctionality urethane acrylates, 10 parts-15 parts of single functionality reactive thinners, 4 parts-8 parts of 1173 or 184 light triggers, 5 parts-8 parts of ethyl esters, 3 parts-5 parts of functional type auxiliary agents.
2. the continuous method of aluminium roll bending surface vacuum vapour deposition process plating aluminium film or Sn-Al alloy film according to claim 1, is characterized in that, the pretreated concrete steps of the described substrate of step (1) are:
Oil removing: with aluminium sheet or aluminium roll bending in chemical liquid oil removing 1-2 minute, temperature was controlled at 50 ℃-65 ℃; The formula of chemical liquid is: sodium hydroxide 30-50 gram/L, and industrial detergent 0.5-1 milliliter/L, all the other are water;
Washing: the aluminium flake after electrochemical deoiling or aluminium roll bending are inserted in warm water clean, 35 ℃-45 ℃ of water temperatures, 20 seconds-30 seconds time;
The pickling oxide film dissolving: the substrate after washing is put into acidic solution and is removed zone of oxidation; Acidic solution is the salpeter solution of every liter of 250-300 milliliter, and the reaction times is controlled at 1min-3min;
Washing: pickling substrate is later washed 20s-40s in the water of 35 ℃-45 ℃;
Oven dry: 50 ℃-70 ℃ baking 5min-10min, pre-treatment is completed.
3. the continuous method of aluminium roll bending surface vacuum vapour deposition process plating aluminium film or Sn-Al alloy film according to claim 1, it is characterized in that, the described primer thickness of step (2) is the 10-12 micron, and hardness of film reaches 0 grade for the sticking power of aluminium more than 1H.
4. the continuous method of aluminium roll bending surface vacuum vapour deposition process plating aluminium film or Sn-Al alloy film according to claim 1, it is characterized in that, the described aluminium film of step (3) or Sn-Al alloy film thickness are the 0.5-1 micron, insulation resistance＞2M ohm, and minute surface is to the reflecting rate of visible light＞92%.
5. the continuous method of aluminium roll bending surface vacuum vapour deposition process plating aluminium film or Sn-Al alloy film according to claim 1, it is characterized in that, the described finishing coat thickness of step (4) is the 6-10 micron, hardness of film is more than 1H, anti-bending reaches the 2T standard, it is unchanged that salt spray resistance reaches the neutral 5%NaCl aqueous solution 48 hours, and ultraviolet aging resistance reached more than 120 hours.
6. the continuous method of aluminium roll bending surface vacuum vapour deposition process plating aluminium film or Sn-Al alloy film according to claim 1, is characterized in that, step (4) is the plastics film that shields of plating one deck more afterwards.
7. the continuous method of aluminium roll bending surface vacuum vapour deposition process plating aluminium film or Sn-Al alloy film according to claim 1, it is characterized in that, described in organic coating a and organic coating b, the single functionality reactive thinner is lauric acid methacrylic ester or iso-bornyl acrylate.
8. the continuous method of aluminium roll bending surface vacuum vapour deposition process plating aluminium film or Sn-Al alloy film according to claim 1, it is characterized in that, described in organic coating a and organic coating b, the functional type auxiliary agent is selected from second-HEMA phosphoric acid ester, BYK371 flow agent, promotor 1270 or promotor 2325.
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| CN102980162B (en) * | 2012-12-13 | 2014-10-22 | 珠海市远康企业有限公司 | Heat radiator containing vacuum-evaporated coating for LED (Light Emitting Diode) lamp and manufacture preparation method thereof |
| CN103555215B (en) * | 2013-10-11 | 2015-06-24 | 浙江海川安全防护用品有限公司 | Preparation method for solar cooker reflective membrane of acrylic surface layer |
| CN105733342A (en) * | 2016-03-11 | 2016-07-06 | 上汽大众汽车有限公司 | Film on surface of car-specification part and development method of film |
| CN105820361B (en) * | 2016-04-15 | 2018-12-04 | 宁波威霖住宅设施有限公司 | A kind of plastic item surface treatment method |
| CN108456851B (en) * | 2018-02-26 | 2019-12-24 | 蒙城繁枫真空科技有限公司 | Dry-type electroplating surface treatment method for zinc alloy |
| CN109097738B (en) * | 2018-08-13 | 2020-12-18 | 长沙中海瑞超硬材料技术有限公司 | Ceramic mirror and manufacturing method thereof |
| CN109136864B (en) * | 2018-08-21 | 2021-02-02 | 烟台正海磁性材料股份有限公司 | Method for vacuum coating of aluminum-tin composite coating on surface of magnetic steel |
| CN111604248A (en) * | 2020-06-17 | 2020-09-01 | 江苏倍科装饰材料科技有限公司 | Production process of color-coated aluminum coil |
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| CN102251213A (en) * | 2010-05-18 | 2011-11-23 | 中国科学院宁波材料技术与工程研究所 | Vapour deposition protective coating on magnesium alloy surface with corrosion resistance and wear resistance and preparation method thereof |
| CN101979703A (en) * | 2010-11-10 | 2011-02-23 | 范文波 | Method for performing surface treatment on golf head by aluminium -titanium nitride composite coating |
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