CN101210335A - Surface treatment method for light metal material - Google Patents
Surface treatment method for light metal material Download PDFInfo
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- CN101210335A CN101210335A CNA200610172604XA CN200610172604A CN101210335A CN 101210335 A CN101210335 A CN 101210335A CN A200610172604X A CNA200610172604X A CN A200610172604XA CN 200610172604 A CN200610172604 A CN 200610172604A CN 101210335 A CN101210335 A CN 101210335A
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Abstract
A surface treatment method of light metal material comprises the following steps of: forming a metal plating layer on the surface of a light metal material, wherein a micro-arc oxide film layer is formed on the surface of the light metal material before forming the metal plating layer. By sequentially carrying out micro-arc oxidization treatment and metal plating film, the invention can greatly improve the bonding force between the metal plating layer and the surface of the light metal material. For example, the bonding force of the metal film layer of a magnesium alloy material prepared by the method in the invention is over 4 B, while the bonding force of the metal film layer of a magnesium alloy material prepared by the prior art is only 2 B. Additionally, the invention is a high-quality surface treatment process and can greatly improve the corrosion resistance and appearance decoration of the material.
Description
Technical field
The invention relates to a kind of treatment process of metallic surface, especially about a kind of surface treatment method of light metal material.
Background technology
Light metal, for example aluminium, magnesium, titanium, aluminium alloy, magnesium alloy and titanium alloy etc., but have that density is little, the conductive and heat-conductive ability is strong, mechanical property is excellent and advantage such as secondary processing, therefore in national economy, obtained using widely.But light metal material itself is a kind of corrosion-prone material, therefore in order to utilize light metal material better, normally avoids Corrosion of Metallic Materials by light metal material is carried out the surface-treated method.For example, can carry out various chemical conversion processing and anodic oxidation treatment etc.Though aforesaid method can improve the erosion resistance of light metal material to a certain extent, chemical conversion is handled rete and anode oxidation membrane and is had problems such as rete approaches, wears no resistance, sight difference.
By physics vapor phase deposition method (PVD), for example formation metal plating such as electron beam evaporation plating, magnetron sputtering or ion plating method are extensive use of recently, it can deposit various metal plating on various substrate surfaces, make base material present the high metalluster of ornamental value.
For example, CN 1827839A discloses a kind of method of metal finishing, and this method comprises: a preposition finished workpiece is provided; By a vacuum metal film coating equipment, vacuum coating metallic film is in this preposition finished workpiece; And be coated with defensive dura mater on the workpiece behind this vacuum coating metallic film.Foregoing invention has reached the purpose that makes Mg alloy surface present beautiful metalluster by this method.But, by the metal plating existence of PVD method formation and the shortcoming of substrate surface bonding force difference, especially on light metal material, and many, the shape more complicated of surface imperfection of the light metal material die casting that especially forms by die casting of light metal material surface, make that the metal plating of the formation bonding force surperficial with it is poor.
Though the method that foregoing invention provides comprises that also phosphate is carried out in the metallic surface to be handled and the priming paint spray treatment, and then carries out the PVD plated film, effect still is not very good.Its reason is that priming paint and light metal material surface are relatively poor through the avidity of the rete of chemical conversion formation, can't solve metallic diaphragm in the low problem of light metal material surface bonding power.And handle if only chemical conversion is carried out on the light metal material surface, can only form the very thin rete of one deck on its surface, can't cover the defective on light metal material surface, also can't solve the low problem of metal plating bonding force, and its anti-corrosion time is shorter, and exterior decorative effect is not good.In addition, if use paint spraying separately, though can improve the surface imperfection of light metal material, also can solve the low problem of paint film avidity, chemical modification takes place in the surface but independent prime coat does not make light metal material, this simple rete covers, and can't ensure the erosion resistance that light metal material is high.
Summary of the invention
The objective of the invention is in order to overcome the shortcoming of metal plating and light metal material bonding force difference in the prior art, a kind of bonding force that can improve metal plating and light metal material is provided, can have improved the processing method of product appearance decorative effect and anti-corrosion effect again.
The invention provides a kind of surface treatment method of light metal material, this method is included in the light metal material surface and forms metal plating, wherein, before forming metal plating, forms differential arc oxidation film layer on the light metal material surface earlier.
Differential arc oxidization technique is a kind of emerging process for treating surface, it can form one deck micro-arc oxidation films by certain condition on various metallic surfaces, this rete has good wear resistance and erosion resistance, the surface treatment of the material that therefore be used for corrosion-resistant, wears no resistance.The present inventor finds, by the differential arc oxidation method light metal surface is handled earlier, and then carry out metal coating, the metallic diaphragm bonding force on the light metal material that obtains is very high, efficiently solves the problem of metallic diaphragm bonding force difference in the prior art.
The present invention handles by earlier light metal being carried out differential arc oxidation, carries out the method for metal coating again, has improved the bonding force on the surface of metal plating and light metal material greatly.For example, the bonding force of the metallic diaphragm of the magnesium alloy materials for preparing by method provided by the invention all arrives more than the 4B, and the bonding force of the metallic diaphragm of the magnesium alloy materials that the method by prior art obtains only is 2B.
The light metal material that obtains by method provided by the invention possesses the strong and advantages such as wear resistance and good corrosion resistance of metallic diaphragm bonding force, and its distinctive metalluster makes the decorative appearance of product stronger, thereby has promoted its value added greatly.
Embodiment
The surface treatment method of light metal material of the present invention is included in the light metal material surface and forms metal plating, wherein, before forming metal plating, forms differential arc oxidation film layer on the light metal material surface earlier.
Differential arc oxidation film layer of the present invention makes by the method for differential arc oxidation.The method of described differential arc oxidation is conventionally known to one of skill in the art.The method of described differential arc oxidation comprises light metal material is placed the electrolyzer that fills electrolyte solution, is anode with the light metal material, and electrolyzer carries out oxidation as negative electrode.The condition of described oxidation comprises: used electrolyte solution is for containing alkali metal hydroxide, alkali-metal silicate and the alkali-metal phosphatic aqueous solution, wherein, the content of alkali metal hydroxide is that the content of 1-20 grams per liter, alkali-metal silicate is that 5-20 grams per liter, alkali-metal phosphatic content are the 2-20 grams per liter; Electrolysis voltage is the 300-800 volt, and temperature is 20-50 ℃, and the time is 5-20 minute.It is the 3-10 micron that described electrolytic condition makes the thickness of described differential arc oxidation film layer.Can make by magnetic agitation in the process of described differential arc oxidation keeps whole system to keep the even of constant temperature and bath composition.Differential arc oxidation is washed workpiece 2-10 minute after finishing, and the workpiece drying is got final product.
Metal plating of the present invention can be formed by physics vapor phase deposition method (PVD).Described PVD method for example can be electron beam evaporation plating, magnetron sputtering or ion plating method etc.The concrete operations of aforesaid method and condition have been conventionally known to one of skill in the art.For example the condition of magnetron sputtering can be 2.0 * 10 for the base vacuum degree
-3MPa, sputtering rate be the 8000-10000 dust/minute, substrate temperature is 20-230 ℃, target-substrate distance from being that 300-600 volt, electric current are that 10-20 ampere, sputter vacuum tightness are that 0.13-1.3 pascal, sputtering time are 5 minutes for 5-30 centimetre, anode voltage.In addition, the present invention has no particular limits the kind of described metal plating, can be various metal plating known in those skilled in the art, is preferably a kind of in chromium, aluminium, tin, the nickel or contains 2 kinds or 3 kinds alloy layer in them.The thickness of metal plating is preferably the 0.2-3.0 micron, more preferably the 0.8-2 micron.
Under the preferable case, method provided by the invention also is included in and forms top coat layer on the metal plating.Described top coat layer can be the top coat layer that is formed by various finish paint paint solidifications.For example, can be by thermosetting coating or the top coat layer that solidify to form by ultraviolet-curing paint.
Because ultraviolet-curing paint only needs can solidify to form top coat layer under uviolizing, therefore, described top coat layer is preferably the top coat layer that is solidify to form by ultraviolet-curing paint.By forming top coat layer at metal coating surface, metal plating can be protected effectively, prolong the life-span of metal plating, make it keep beautiful gloss, also improved the wear resistance and the oxidation-resistance of light metal material simultaneously.Described ultraviolet-curing paint can be commercially available or obtain by prepared in various methods.For example, can make the coating of the UV of nation finish paint firmly etc.
Can adopt the whole bag of tricks of the prior art that ultraviolet-curing paint is loaded on the metal plating, for example, can adopt spraying method.It is the 5-15 micron that the amount of load makes the thickness of top coat layer.Can adopt the whole bag of tricks that ultraviolet-curing paint is cured, for example, the method that can adopt ultraviolet source such as high pressure mercury vapour lamp, Jupiter, xenon lamp, luminescent lamp to have the light metal material of ultraviolet-curing paint to shine to load, the irradiation distance of the light intensity of UV-light and irradiation time and UV-light and light metal material makes ultraviolet-curing paint solidify to form top coat layer.
In general, the light intensity of UV-light is strong more, and irradiation distance is near more, and the thickness of top coat layer is more little, then makes the required irradiation time of ultraviolet-curing paint curing short more; Otherwise irradiation time is just long.The present invention preferably uses the conventional high pressure mercury vapour lamp that uses, and the light wavelength is preferably the 380-420 nanometer; Selecting irradiation distance is 1-30 centimetre, is preferably 10-20 centimetre; The UV energy is a 400-1500 milli Jiao/square centimeter, is preferably 800-1200 milli Jiao/square centimeter.Under these conditions, can make thickness is the top coat layer curing of 5-15 micron.
In addition, the present invention can form one deck prime coat and also can not form described prime coat between described metal plating and differential arc oxidation film layer.Under the situation that does not have the direct metal cladding of prime coat, every performance of light metal material is all fine, but the luminance brightness of metal plating can reduce greatly.The present inventor further discovers, conventional primer base has good affinity to differential arc oxidation film layer, after light metal being carried out the differential arc oxidation processing, carry out the priming paint spraying again, and then carry out metal coating by the PVD method, the bonding force of metal plating is further strengthened.Therefore, under the preferable case, method provided by the invention also is included between metal plating and the differential arc oxidation film layer and forms prime coat, and the thickness of described prime coat is the 5-10 micron.Form identical that the coating of described prime coat and curing can be with top coat layer.
Under the preferable case, the present invention also is included in after the differential arc oxidation processing, mends soil and handle on differential arc oxidation film layer, and described method of mending soil is conventionally known to one of skill in the art.
Further under the preferable case, method provided by the invention also comprise in advance to light metal material polish, pre-treatment step such as polishing, degreasing, alkali cleaning.
Method provided by the invention is applicable to various light metal materials, for example can be aluminium, magnesium, titanium, aluminium alloy, magnesium alloy and titanium alloy etc.
According to a kind of preferred implementation of the present invention, the Preparation Method of magnesium alloy materials system provided by the invention comprises successively: 1. to the magnesium alloy ground polish, polishing, degreasing, alkali cleaning; 2. differential arc oxidation is handled; 3. fill artificial mend native agent, grinding; 4. form prime coat; 5. form physics vapor phase deposition metal plating; 6. form top coat layer.
The following examples will the present invention is further illustrated.
Wherein, the light metal material preferred dimension is 80 millimeters * 50 millimeters * 2 millimeters a diecast magnesium alloy.
Embodiment 1
Present embodiment illustrates the surface treatment method of light metal material provided by the invention.
(1) the magnesium alloy base material is polished, polishing, degreasing, alkali cleaning.
Adopt the method for artificial polishing that the magnesium alloy base material is polished, remove unnecessary stub bar of magnesium alloy base material and burr, polish with sand paper again, up to smoothly getting final product with 1200 purpose sand paperings, magnesium alloy base material after process being polished, polished as degreasing solvent with acetone then cleans 2 times repeatedly.Degreasing finishes, and to adopt sodium hydrate content be that 30 grams per liters, sodium phosphate content are that 40 grams per liters, water glass are that the basic solution of 20 grams per liters cleans the magnesium alloy ground in the back.The temperature of cleaning is 85 ℃, and the time of cleaning is 10 minutes.Washed then 5 minutes
(2) differential arc oxidation is handled
With NaOH content is 20 grams per liters, Na
2SiO
3Content is 20 grams per liters, Na
3PO
4Content is that the electrolyte solution of 20 grams per liters joins in the electrolyzer, makes electrolyte solution keep getting final product at normal temperatures.With the magnesium alloy base material is anode, and electrolyzer is a negative electrode, carries out differential arc oxidation and handle under 400 volts voltage, with magnetic stirring apparatus electrolyte solution is stirred therebetween, and the treatment time is 10 minutes.After processing finishes, with clear water washing 2 minutes, the magnesium alloy base material is dried up with ion wind gun again, obtain comprising the alloy of micro-arc oxidation films, (German PHYNIX company, Pocket-Surfix) thickness that records micro-arc oxidation films is 5 microns with the coated layer thickness tester.
(3) finishing plane
The benefit soil agent 20 of producing with Ji Tong company restrains the micropore of repairing on the magnesium alloy, and baking is 15 minutes in 160 ℃ baking oven, and it is solidified, and polishes with the sand paper of 1000# or 1500# then.
(4) form prime coat
Ultraviolet-curing paint (Aksu UV primer base) is sprayed on the differential arc oxidation film layer, is that the high pressure mercury vapour lamp of 400 nanometers shines with ultraviolet wavelength then, and the distance of lamp and base material is 15 centimetres, and the UV energy is 1000 milli Jiao/square centimeters.Obtain prime coat.(German PHYNIX company, Pocket-Surfix) recording prime coat thickness is 8 microns with the coated layer thickness tester.
(5) form metal plating
Adopt magnetron sputtering equipment to carry out metal coating, the processing parameter that magnetron sputtering is established is as follows: base vacuum degree: 2.0 * 10
-3Below the handkerchief; Rotating speed: 5/ minute; Substrate temperature: 50 ℃; Target-substrate distance from: 12 centimetres; Voltage between negative electrode and the anode: 400 volts; Electric current: 12 amperes; Sputter vacuum tightness: 0.5 pascal; Sputtering time: 5 minutes/sheet; Target is an aluminium.Obtain aluminum metal layer.(German PHYNIX company, Pocket-Surfix) thickness that records aluminum metal layer is 2.0 microns with the coated layer thickness tester.
(6) form top coat layer
Ultraviolet-curing paint (UV of power nation finish paint) is sprayed on the metal plating, is that the high pressure mercury vapour lamp of 400 nanometers shines with ultraviolet wavelength then, and lamp is apart from being 15 centimetres, and the UV energy is 1000 milli Jiao/square centimeters.Obtain top coat layer.(German PHYNIX company, Pocket-Surfix) recording top coat layer thickness is 10 microns with the coated layer thickness tester.
Finally obtain magnesium alloy materials A1 by above-mentioned steps.
Comparative Examples 1
The surface treatment method of the light metal material that this Comparative Examples explanation prior art provides.
Method according to embodiment 1 is carried out surface treatment to the magnesium alloy base material, different is, described step (2) is adjusted agent MD-420 for epithelium liquid 161 gram PZ-610A, 1 gram PZ-610B, 3.5 gram PZ-610C, 15 gram activator M3-410 and 30 grams that JASCO company is produced and is mixed, the magnesium alloy base material that step (1) is obtained changes in said mixture then, the temperature that changes into is 60 ℃, and the time is 30 seconds, changes into the back and cleans with clear water, take out, toasted 25 minutes down at 150 ℃.Finally obtain magnesium alloy materials D1.
Embodiment 2
Method according to embodiment 1 is carried out surface treatment to the magnesium alloy base material, and different is after carrying out the differential arc oxidation processing, directly to carry out the magnetic control sputtering plating metal plating.Finally obtain magnesium alloy materials A2.
Embodiment 3
Method according to embodiment 1 is carried out surface treatment to the magnesium alloy base material, and different is after carrying out the differential arc oxidation processing, directly to carry out the magnetic control sputtering plating metal plating.And spray paint layer not.Finally obtain magnesium alloy materials A3.
Embodiment 4
Present embodiment illustrates the performance of magnesium alloy materials provided by the invention.
The magnesium alloy materials A1 that respectively embodiment 1 is obtained according to following method carries out bonding force test, the wear-resisting test of RCA paper tape, pencil hardness test and SaltSprayTest, and the result is as shown in table 1.
(1) bonding force test (ASTMD 3359-93)
Instrument: hundred lattice cutter L500001;
The method of inspection: ASTM D3359, spacing: 1 millimeter, the pull-up angle: 90 °, adhesive tape: 3M600
(2) the wear-resisting test of RCA paper tape
Use the RCA paper tape wear resistant instrument of model as F350008, friction magnesium alloy materials top coat under 175 gram forces, magnesium alloy materials top coat are milled to when show-through, the number of turns that the record rubber wheel rotates;
(3) pencil hardness test (ASTMD 3363-74)
Instrument: pencil hardness meter F130027
The method of inspection: ASTM D3363, load: 750 grams, pencil: the UNI of Mitsubishi
(4) SaltSprayTest
The magnesium alloy materials sample is placed in the salt fog cabinet, sodium chloride brine with 5 ± 0.5 weight % under 35 ℃ sprayed sample after 8 hours, taking out and placing the another one temperature is that 22.5 ℃, relative humidity are the climatic chamber of 47.3%RH, place after 8 hours, observation sample, the corroded area of record sample surfaces accounts for the percentage composition of the coating total area (the coating total area is pressed metal coating and calculated).
Comparative Examples 2
According to the method for embodiment 4 the magnesium alloy materials D1 of Comparative Examples 1 is carried out performance test.The result is as shown in table 1.
Embodiment 5-6
These embodiment illustrate the performance of magnesium alloy materials provided by the invention.
According to the method for embodiment 4 the magnesium alloy materials A1-A2 of embodiment 2-3 is carried out performance test.The result is as shown in table 1.
Table 1
| The magnesium alloy materials source | The magnesium alloy materials numbering | Bonding force (B) | RCA paper tape wear resistance (circle) | Pencil hardness (H) | Salt spray corrosion area (area %) |
| Embodiment 1 | A1 | 5 | 450 | 6 | 1 |
| Comparative Examples 1 | D1 | 2 | 430 | 5 | 1 |
| Embodiment 2 | A2 | 4 | 447 | 6 | 1 |
| Embodiment 3 | A3 | 4 | 82 | 1 | 3 |
| Fair receipts standard | - | ≥2 | ≥300 | ≥2 | ≤5 |
As can be seen from Table 1, the metal plating of the magnesium alloy materials A1-A3 that embodiment of the invention 1-3 makes and the bonding force of substrate surface all arrive more than the 4B, the metal plating of the magnesium alloy materials D1 that Comparative Examples 1 makes and the bonding force of substrate surface only are 2B, therefore, method provided by the invention can improve the bonding force on the surface of metal plating and light metal material greatly.Wherein, embodiment 2 is poor with the magnesium alloy materials A2 that embodiment 3 makes compares magnesium alloy materials A1 with A3 metal plating bonding force, illustrates that prime coat can further improve the bonding force of metal plating and substrate surface.
In addition,, therefore, do not having under the situation of top coat layer among the embodiment 3 because wear resistance of PVD plated film own and hardness are relatively poor, though the metal plating bonding force is stronger,, wear resistance and hardness are bad.Therefore, the present invention is spray paint layer on top coat layer preferably, to obtain all good light metal material of metal plating bonding force, wear resistance, hardness, erosion resistance.
Claims (10)
1. the surface treatment method of a light metal material, this method are included in the light metal material surface and form metal plating, it is characterized in that, before forming metal plating, form differential arc oxidation film layer on the light metal material surface earlier.
2. method according to claim 1, wherein, described differential arc oxidation film layer the formation method comprise light metal material placed the electrolyzer that fills electrolyte solution, with the light metal material is anode, electrolyzer is as negative electrode, with the light metal material oxidation, it is the 3-10 micron that described oxidizing condition makes the thickness of the differential arc oxidation film layer that obtains.
3. method according to claim 2, wherein, used electrolyte solution is for containing alkali metal hydroxide, alkali-metal silicate, the alkali-metal phosphatic aqueous solution, and the content of alkali metal hydroxide is that the content of 1-20 grams per liter, alkali-metal silicate is that 5-20 grams per liter, alkali-metal phosphatic content are the 2-20 grams per liter; Electrolysis voltage is the 300-800 volt, and temperature is 20-50 ℃, and the time is 5-20 minute.
4. method according to claim 1, wherein, this method also is included in and forms top coat layer on the metal plating, and the thickness of described top coat layer is the 5-15 micron.
5. method according to claim 4, wherein, described top coat layer is formed by ultraviolet light polymerization finish paint coating or thermofixation finish paint coating.
6. method according to claim 1, wherein, this method also is included between metal plating and the differential arc oxidation film layer and forms prime coat, and the thickness of described prime coat is the 5-10 micron.
7. method according to claim 6, wherein, described prime coat is formed by ultraviolet cured primer coating or thermofixation primer base.
8. according to claim 1,4 or 6 described methods, wherein, described metal plating is the coating of a kind of in chromium, aluminium, the tin or the alloy that contains in them 2 kinds or 3 kinds, and the thickness of coating is the 0.2-2 micron.
9. method according to claim 1, wherein, described metal plating is formed by physics vapor phase deposition method.
10. method according to claim 1, wherein, described light metal is magnesium, aluminium, titanium, magnesium alloy, aluminium alloy or titanium alloy.
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| CN101974711A (en) * | 2010-09-28 | 2011-02-16 | 蔡乐勤 | Aluminum magnesium alloy material with wear resistance and corrosion resistance, and preparation method thereof |
| CN102634796A (en) * | 2012-04-28 | 2012-08-15 | 桂林电子科技大学 | Preparation method of composite ceramic layer with antibacterial properties |
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| CN103668394A (en) * | 2013-12-13 | 2014-03-26 | 中国航空工业集团公司金城南京机电液压工程研究中心 | Novel magnesium alloy surface protection process |
| CN104674322A (en) * | 2015-03-23 | 2015-06-03 | 重庆电讯职业学院 | Magnesium alloy component differential arc oxidization ceramic membrane, preparation method and electrolyte |
| CN104746072A (en) * | 2015-03-30 | 2015-07-01 | 创金美科技（深圳）有限公司 | Magnesium alloy microarc ion plating surface treatment method |
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| CN101974711B (en) * | 2010-09-28 | 2012-10-31 | 蔡乐勤 | Preparation method of aluminum magnesium alloy material with wear resistance and corrosion resistance |
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| CN102634796A (en) * | 2012-04-28 | 2012-08-15 | 桂林电子科技大学 | Preparation method of composite ceramic layer with antibacterial properties |
| CN103266338A (en) * | 2013-05-21 | 2013-08-28 | 沈阳理工大学 | TC4 titanium alloy anodizing chromium-free blackening method |
| CN103668394A (en) * | 2013-12-13 | 2014-03-26 | 中国航空工业集团公司金城南京机电液压工程研究中心 | Novel magnesium alloy surface protection process |
| CN105874100A (en) * | 2013-12-26 | 2016-08-17 | Posco公司 | Surface-treated substrate and substrate surface treatment method for same |
| CN105874100B (en) * | 2013-12-26 | 2018-09-21 | Posco公司 | The base material of surface treatment and method for treating surface of base for it |
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| CN105983836A (en) * | 2015-02-13 | 2016-10-05 | 汉达精密电子(昆山)有限公司 | Manufacturing method for magnesium alloy appearance and product with magnesium alloy appearance |
| CN104674322A (en) * | 2015-03-23 | 2015-06-03 | 重庆电讯职业学院 | Magnesium alloy component differential arc oxidization ceramic membrane, preparation method and electrolyte |
| CN104746072B (en) * | 2015-03-30 | 2017-06-13 | 创金美科技（深圳）有限公司 | A kind of magnesium alloy differential arc ion plating surface treatment method |
| CN104746072A (en) * | 2015-03-30 | 2015-07-01 | 创金美科技（深圳）有限公司 | Magnesium alloy microarc ion plating surface treatment method |
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