CN104593786A - Method for microporous treatment of metal surface - Google Patents
Method for microporous treatment of metal surface Download PDFInfo
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- CN104593786A CN104593786A CN201510074449.7A CN201510074449A CN104593786A CN 104593786 A CN104593786 A CN 104593786A CN 201510074449 A CN201510074449 A CN 201510074449A CN 104593786 A CN104593786 A CN 104593786A
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Abstract
The invention belongs to the technical field of material treatment and particularly relates to a method for microporous treatment of a metal surface. The method comprises the following steps: (1) performing anodic oxidation on a preprocessed metal base material to obtain a metal base material provided with an anodic oxide film layer on the surface; (2) soaking the metal base material obtained in the step (1) in etching liquor for treatment; (3) putting the metal base material obtained in the step (2) into an anodic oxidation groove with sulfur acid and ammonium chloride for modification treatment; (4) soaking the metal base material obtained in the step (3) in a phosphate anion solution, washing with water, soaking in a washing regulating agent at a room temperature, washing with water, and baking for 0.5-1 hour. The purpose of pore size expansion is achieved in a condition-controllable AAO (anodic aluminum oxide) film production mode, a problem that a conventional pore-forming method cannot obtain ordered controllable micropores is solved, and strict requirements on various aspects of product size, structure and the like are avoided from a macroscopic perspective.
Description
Technical field
The invention belongs to material processing technical field, the method for particularly a kind of metallic surface microporous process.
Background technology
In fields such as mobile communication equipment, electronic and electrical equipment, automobile mechanicals, often need to spray metallic surface, bond, injection moulding etc., in order to improve the bonding strength of surface attachments, usually effects on surface is needed to process, as common phosphatization, passivation and treatment process such as manufacture hole, back-off etc., in brief, all metal and dirt settling bonding strength is improved by increase corrosion resistance of surface and roughness.Traditional is adopt phosphatization, the mode of passivation is corroded metallic surface by the method for chemical solution immersion treatment, reach and not only metallic surface to be protected but also effects on surface carries out roughening to improve the object of metal and dirt settling bonding strength, it is uneven irregular that this method obtains uneven surface, only be applicable to more rough simple protection, its surface attachments bonding strength of metal is after treatment lower, conventional manufacture micropore makes the method kind of surface roughening more, such as patent CN102537066A, CN102145331A, CN1584119A, the laser micromachining process that CN101578018A etc. propose, assembling coating, the methods such as design fillet back-off is embedded, all refer to from all angles the method improving metallic surface and dirt settling bonding strength, but these class methods all in various degree there is complicated operation, cost is higher, the each side problems such as applicable surface is narrow, make it apply and receive certain limitation.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, and the method for a kind of metallic surface microporous process is provided, the present invention proposes the mode adopting electrochemistry and chemical process to combine makes metallic surface produce controllability micropore, reaches the object improving metallic surface dirt settling bonding strength at microcosmic level.Specifically, it makes metal formation have the nanometer three-dimensional cover pore structure of certain rule by the anodic oxidation of special shape, again by the growth pattern of nano aluminium oxide AAO film, controllability reaming is carried out to the nanometer micropore formed, metallic surface is reached there is the controlled roughness of size, thus reach the object that metallic surface microporous improves dirt settling bonding strength.
In order to can above-mentioned purpose be realized, the present invention by the following technical solutions:
A method for metallic surface microporous process, comprises the steps: 1) anodic oxidation: the metal base through pre-treatment is obtained the metal base of surface containing anode oxidation membrane by anodic oxidation, and described metal base is aluminum alloy base material or aluminium base.
2) anode oxide film is moved back: metal base step 1) gained being contained anode oxidation membrane immerses in etching liquid and processes, the metal base of the anode oxidation membrane that is removed, H in described etching liquid
+/ OH
-concentration is 0.55 ~ 5.5mol/L, and containing fluorion and/or phosphate anion in described etching solution, and described etching solution is also containing aluminium inhibiter.
Move back anode oxide film step to its object is to make metallic surface form " hole core " by chemical corrosion oxide film, for the growth of secondary anode micropore metal matrix provides basic point, because the hole degree of order of the nano metal matrix micropore that an anodic oxidation produces is not high, pore size is inconsistent, along with the formation of " hole core ", the strength of electric field being originally distributed in surface is made to concentrate at the bottom of hole, dissolution rate and the rate of oxidation of causing hole bottom barrier improve greatly, final dissolution rate and growth velocity reach a running balance, nanometer micropore metallic matrix is able to stable growth, during subsequent treatment process, dirt settling evenly can enter micropore, reach and improve the bonding strength object consistent with ensureing each position bonding strength.
The basic procedure that anodic oxidation can produce micropore is that metallic matrix (as aluminium) loses electronics and becomes Al under impressed voltage
3+, it is to external migration, O
2-and OH
-inside migration, metal/oxide interface constantly forms new barrier layer, increase along with aluminum oxide thickness increases voltage, electrochemical reaction slows down, now temperature raises, electrolytic solution produces dissolved corrosion to aluminum oxide, and due to the dispersiveness of corrosive fluid, the thinner position of aluminum oxide is to recessed, resistance reduces, loss of voltage, aluminum oxide continues to generate, along with the carrying out of reaction, the aluminum oxide of recess generates and dissolving reaches balance, reaction is carried out always, and thickness of aluminum alloy does not increase, and recess recessed final formation nanoporous gradually.Because produce the position that recessed position is aluminum oxide film at first, the position of aluminum oxide film is because aluminium base surface microscopic uneven distribution, and the thin and thick of aluminium base surface microscopic and size itself are uneven, therefore the nanometer micropore produced is uneven, by moving back the rough polishing of anode oxide film, make surface only residual atomic little " hole core ", thus the nanoporous that basic guarantee secondary anode produces has good homogeneity.
3) modification anodic oxidation: by step 2) gained metal base puts into sulfur acid, ammonium chloride anodizing tank carries out modification, obtains the metal base of modification anode oxidation membrane.
Wherein said modification anodic oxidation is in the anodizing solution of routine, introduce the negatively charged ion that can produce pitting attack to aluminum alloy surface; Described modification anodic oxidation is in the anodizing solution of routine, introduce the negatively charged ion that can produce pitting attack to metallic surface, make in anode oxidation process, produce little anode hole while produce large corrosion hole, and the micropore now produced above grows in first time anodic oxidation residual " hole core ", what grow thus nanometer level microporously has good order, and because the existence of pitting attack generates large micropore, both are interweaved, the final three dimensional topology forming large borehole jack aperture.
4) surface adjustment: metal base described in step 3) gained is put into H
+concentration is in the phosphate radical solution of 0.1 ~ 1mol/L, soaks 1 ~ 30 minute at 40 ~ 60 DEG C, and washing is clean, then puts it in cleaning adjustment, and soak 1 ~ 30 minute under joint room temperature, washing is clean, baking 0.5 ~ 1 hour at the temperature of 65 DEG C.Wherein the special micropore control methods described in the adjustment of surface is the growth rhythm control methods utilizing nanometer anodised aluminium AAO film, specifically, is the aperture being controlled nanoporous by phosphoric acid corrosion method.
The present invention is that the micropore utilizing short period of time anodic oxidation to produce generates the porous oxygen film with suitable spatial aperture structure in the method improved, again through reaming extremely required aperture, utilize the crab-bolt effect of micropore, ensure there is higher bonding strength between metal and dirt settling.
Carry out two-step anodization, comprise conventional anodes oxidation, move back anode oxide film and modification anodic oxidation three step, after surface treatment, in acid solution, carry out oxidation at metal and comprise sulphuric acid anodizing method, phosphate anodizing, oxalic acid anodizing method and mixed acid anodic oxidation method, its object is to generate in metallic surface a large amount of nanometer level microporous, about 1 ~ the 15nm of diameter of micropore, again through surface adjustment, obtain the three-dimensional micropore making surface have a certain size, surface micropore is made to reach required aperture by the mode of reaming again, directly can improve the metallic matrix of the bonding strength of its surface and dirt settling.
As a modification of the present invention, described step 1) in, the metal base of pre-treatment is, some pieces of metal bases to be soaked in grease-removing agent 300 seconds, temperature is set to 60 DEG C; To be soaked in the aqueous sodium hydroxide solution of 20 ~ 80g/l 40 seconds after washing is clean again, temperature is set to 65 DEG C; Again through wash clean after to be soaked in concentration under normal temperature be obtain in the aqueous nitric acid of 25% 40 seconds.
As a modification of the present invention, in described step 1), the metal base through pre-treatment is put into the sulphuric acid anodizing groove containing 190g/l, temperature remains on 17 DEG C, the lower oxidation of voltage 18V 8 minutes.
As a modification of the present invention, described step 2) comprise step 2) the gained metal base that contains anode oxidation membrane repeatedly immerses in etching liquid and process, the time processed in each immersion etching liquid is 2 ~ 10min, and each immersion in etching liquid washes after process.
As a modification of the present invention, the number of times of described immersion is 2 to 10 times.
As a modification of the present invention, in described step 3), comprise and carry out surface cleaning to the metal base of modification anode oxidation membrane, described cleaning is adjusted and is made up of weakly alkaline salt, organic amine and tensio-active agent, and cleaning micropore cleans 1 ~ 10 minute at every turn.
Described surface cleaning adopts the weakly alkaline solution of easier rinsing to carry out neutralizing the negatively charged ion cleaning and remain in micropore, as its settling mode can adopt room temperature to porous-film almost the weakly alkaline salt of corrosion-free destruction, organic amine, tensio-active agent clean 1-10 minute to clean micropore at every turn, clean 1-10 time.Because anode oxidation process is the process of Anion-adsorption in doped solution, what wherein have is then be adsorbed on the hole wall of porous-film, what have is then exist with the form of chemical bond, and its concentration in gradient distributes, the process of cleaning be for prevent the negatively charged ion that remains can in subsequent technique, dirt settling invades nanometer micropore time its bonding properties produced destroy.
As a modification of the present invention, described organic amine is made up of one or more of trolamine, triethylene diamine, dimethyl amine, pyridine, piperidines and quinoline.
As a modification of the present invention, described weakly alkaline salt is made up of one or more of Sunmorl N 60S, Sodium Benzoate, Sodium Glutamate, Seignette salt and sodium bicarbonate.
As a modification of the present invention, described tensio-active agent by palmityl trimethyl ammonium chloride, octyltrimethylammonium chloride, dihydroxy ethyl oleic imidazolinone one or more form.
As a modification of the present invention, by step 1) ~ 4) surface of metallic matrix of preparing forms the three-dimensional structure of large borehole jack aperture, macropore diameter 0.1-1 μm, small aperture 1-15nm, and reaming speed meets the linear relationship of Y=a*X+b substantially, wherein: Y represents the aperture of aluminum oxide micropore, and X represents etching time, a and b is constant, and at different concns, temperature, the value of constant is different.
Beneficial effect of the present invention: the present invention utilizes with upper type anodic oxidation, the micropore of generation is made to have good order, and add by introducing the micropore that ion forms cover well format, solve the problem that conventional chemical corrosion and passivation methods combining intensity is not high, the object of borehole enlargement is reached again by the aluminum oxide AAO film mode of production that condition is controlled, solve the problem that conventional pore forming method can not obtain orderly controlled micropore, avoid many-sided rigors such as product size, structure from the angle of macroscopic view.
Accompanying drawing explanation
Linear relationship chart to nano aluminium oxide reaming when Fig. 1 is phosphoric acid quality concentration 5%, temperature is 40 DEG C.
Fig. 2 be after anodic oxidation of the present invention through 100,000 times of electron microscope observations to picture.
Fig. 3 be after method process described in the embodiment of the present invention 1 through 100,000 times of electron microscope observations to picture.
Fig. 4 be after method process described in the embodiment of the present invention 2 through 100,000 times of electron microscope observations to picture.
Embodiment
Below in conjunction with accompanying drawing 1 to 4 and specific embodiment, the present invention will be described.
embodiment 1
A method for metallic surface microporous process, comprises the steps: 1) anodic oxidation: the metal base through pre-treatment is obtained the metal base of surface containing anode oxidation membrane by anodic oxidation, and described metal base is aluminum alloy base material or aluminium base; 2) anode oxide film is moved back: metal base step 1) gained being contained anode oxidation membrane immerses in etching liquid and processes, the metal base of the anode oxidation membrane that is removed, H in described etching liquid
+/ OH
-concentration is 0.55 ~ 5.5mol/L, and containing fluorion and/or phosphate anion in described etching solution, and described etching solution is also containing aluminium inhibiter; 3) modification anodic oxidation: by step 2) gained metal base puts into sulfur acid, ammonium chloride anodizing tank carries out modification, obtains the metal base of modification anode oxidation membrane; 4) surface adjustment: metal base described in step 3) gained is put into H
+concentration is in the phosphate radical solution of 0.1 ~ 1mol/L, soaks 1 ~ 30 minute at 40 ~ 60 DEG C, and washing is clean, then puts it in cleaning adjustment, and soak 1 ~ 30 minute under joint room temperature, washing is clean, baking 0.5 ~ 1 hour at the temperature of 65 DEG C.
Particularly, a. pre-treatment: the small pieces 6063 thick for commercially available 1.0mm Aluminum Cuttings being become many 15mm × 50mm, gets ten at random and firmly hangs on titanium alloy hanger by it; Then to be soaked in aluminium grease-removing agent 300 seconds, temperature is set to 60 DEG C; To be soaked in the aqueous sodium hydroxide solution of 70g/l 40 seconds after washing is clean again, temperature is set to 65 DEG C; Again through wash clean after to be soaked in volumetric concentration be in the aqueous nitric acid of 25% 40 seconds, normal temperature;
B. anodic oxidation: (1) step aluminum alloy sheet is put into the sulphuric acid anodizing groove containing 190g/l, at 18 DEG C, the oxidation at voltages of 18V 8 minutes, washing is clean;
C. move back anode oxide film: by the volumetric concentration that (2) step aluminium flake is put into be 5% phosphoric acid and 3g/l chromic trioxide the aqueous solution in soak 20 minutes at 70 DEG C, washing is clean;
D. modification anodic oxidation: (3) step aluminum alloy sheet is put into containing in the sulfuric acid of 190g/l, 0.5g/l ammonium chloride anodizing tank, at 18 DEG C, the oxidation at voltages of 18V 8 minutes, washing is clean;
E. surface adjustment: put in the phosphate aqueous solution of 50g/l by (4) step aluminium alloy, soaks 6 minutes at 40 DEG C, and washing is clean;
F. surface cleaning: put in the sodium gluconate solution of 5g/l by the aluminium alloy that (5) step obtains, at room temperature soaks 6 minutes, and washing is clean, toasts 30 minutes at the temperature of 65 DEG C.
And adopt SU-70 thermal field emission scanning electron microscopic observation through surface-treated aluminium flake, observing surface uniform, to be dispersed with mean pore size (macropore diameter and small aperture average) be 40nm(R
2=0.9941) aluminum oxide micropore, according to the experience using phosphoric acid corrosion method to grow nano aluminium oxide AAO film, its concentration and temperature-resistant time, change soak time (i.e. etching time) in the adjustment of surface, select 3 ~ 21 minutes, every sampling in three minutes once, utilize SU-70 thermal field emission scanning electron microscopic observation through surface-treated aluminium flake, obtain taking aperture as ordinate zou, take etching time as the concrete numerical value of X-coordinate, as shown in Figure 1, the reaming speed of phosphoric acid meets Y=a*X+b substantially, wherein, a=3.369, b=11, as Fig. 1 linear relationship, its reaming speed is about 3.369nm/min, as can be seen from trend map, only need to adjust the nano aluminium oxide micropore that etching time can obtain required pore size.Because the concentration of phosphoric acid, temperature, time all have controllability operation to aluminium alloy micropore.
embodiment 2
Adopt step process ten aluminum alloy sheets identical in embodiment 1, difference is: c. moves back anode oxide film, 20g/l sodium hydroxide, 2g/l vinylthiourea and 2g/l Xylitol is adopted to soak 3 minutes at 40 DEG C, in the adjustment of e. surface, phosphoric acid dip time lengthening to 15 minute.Adopt SU-70 thermal field emission scanning electron microscopic observation through surface-treated aluminium flake, observe surface uniform and be dispersed with the aluminum oxide micropore that mean pore size is 70nm.Other are identical with experimental example 1, repeat no more herein, and it obtains the linear relationship meeting Y=a*X+b equally.
comparative example 1
Adopt step process ten aluminum alloy sheets identical in embodiment 1, separately get ten aluminium alloys and only do (1) pre-treatment step, respectively last layer terminal hydroxy group vinylformic acid baking vanish resin is coated with to 20 aluminium alloys, dry rear employing paint film adhesion assay method (GB1720-79) to evaluate ten aluminum alloy surface paint film adhesions through surface micropore process and have seven to be 1 grade, three is 2 grades, evaluating ten aluminum alloy surface paint film adhesions merely through pre-treatment has a slice to be 1 grade, eight is 2 grades, and a slice is 3 grades.
comparative example 2
Adopt step process ten aluminum alloy sheets identical in embodiment 1, separately get ten aluminium alloys and only do (1) pre-treatment step, the mode of injection moulding is adopted to make polyphenylene sulfoether resin mixture be bonded to aluminum alloy surface to 20 aluminium alloys respectively, tensile load method is adopted to measure the shearing force being subject to the standard test methods (ASTM D2919-2000) of the gluing bonding strength of shearing force to measure 20 aluminium alloys and resin-bonded thing, measure the bonding strength average out to 24.6MPa of ten aluminium alloys through surface micropore process and resin, the bonding strength mean value of ten aluminium alloys merely through pre-treatment and resin only has 4.6MPa.Other, with embodiment 3, repeat no more herein.
With comparative example as can be seen from above-described embodiment, the metallic matrix of the rule controllability micropore gained using the present invention to obtain, its surface is made to have some micropores, improve sticking power greatly, the bonding strength between metal and surface attachments (as painted, ink, coating, dyestuff, resin and sizing agent etc.) can being significantly improved.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also carry out suitable change and amendment to above-mentioned embodiment.Therefore, the present invention is not limited to embodiment disclosed and described above, also should fall in the protection domain of claim of the present invention modifications and changes more of the present invention.In addition, although employ some specific terms in this specification sheets, these terms just for convenience of description, do not form any restriction to the present invention.
Claims (10)
1. a method for metallic surface microporous process, is characterized in that, comprises the steps:
1) anodic oxidation: the metal base through pre-treatment is obtained the metal base of surface containing anode oxidation membrane by anodic oxidation, and described metal base is aluminum alloy base material or aluminium base;
2) anode oxide film is moved back: metal base step 1) gained being contained anode oxidation membrane immerses in etching liquid and processes, the metal base of the anode oxidation membrane that is removed, H in described etching liquid
+/ OH
-concentration is 0.55 ~ 5.5mol/L, and containing fluorion and/or phosphate anion in described etching solution, and described etching solution is also containing aluminium inhibiter;
3) modification anodic oxidation: by step 2) gained metal base puts into sulfur acid, ammonium chloride anodizing tank carries out modification, obtains the metal base of modification anode oxidation membrane;
4) surface adjustment: metal base described in step 3) gained is put into H
+concentration is in the phosphate radical solution of 0.1 ~ 1mol/L, soaks 1 ~ 30 minute at 40 ~ 60 DEG C, and washing is clean, then puts it in cleaning adjustment, and at room temperature soak 1 ~ 30 minute, washing is clean, toasts 0.5 ~ 1 hour at the temperature of 65 DEG C.
2. the method for metallic surface according to claim 1 microporous process, is characterized in that: described step 1) in, the metal base of pre-treatment is, some pieces of metal bases to be soaked in grease-removing agent 300 seconds, temperature is set to 60 DEG C; To be soaked in the aqueous sodium hydroxide solution of 20 ~ 80g/l 40 seconds after washing is clean again, temperature is set to 65 DEG C; Again through wash clean after to be soaked in volumetric concentration under normal temperature be obtain in the aqueous nitric acid of 25% 40 seconds.
3. the method for metallic surface according to claim 1 microporous process, it is characterized in that, in described step 1), the metal base through pre-treatment is put into the sulphuric acid anodizing groove containing 190g/l, temperature remains on 17 DEG C, the lower oxidation of voltage 18V 8 minutes.
4. the method for metallic surface according to claim 1 microporous process, it is characterized in that: described step 2) comprise step 2) the gained metal base that contains anode oxidation membrane repeatedly immerses in etching liquid and process, the time processed in each immersion etching liquid is 2 ~ 10min, and each immersion in etching liquid washes after process.
5. the method for metallic surface according to claim 4 microporous process, is characterized in that: the number of times of described immersion is 2 to 10 times.
6. the method for metallic surface according to claim 1 microporous process, it is characterized in that: in described step 3), comprise and surface cleaning is carried out to the metal base of modification anode oxidation membrane, described cleaning is adjusted and is made up of weakly alkaline salt, organic amine and tensio-active agent, and cleaning micropore cleans 1 ~ 10 minute at every turn.
7. the method for metallic surface according to claim 6 microporous process, is characterized in that: described organic amine is made up of one or more of trolamine, triethylene diamine, dimethyl amine, pyridine, piperidines and quinoline.
8. the method for metallic surface according to claim 6 microporous process, is characterized in that: described weakly alkaline salt is made up of one or more of Sunmorl N 60S, Sodium Benzoate, Sodium Glutamate, Seignette salt and sodium bicarbonate.
9. the method for metallic surface according to claim 6 microporous process, is characterized in that: described tensio-active agent is made up of one or more of palmityl trimethyl ammonium chloride, octyltrimethylammonium chloride and dihydroxy ethyl oleic imidazolinone.
10. the method for metallic surface according to claim 1 microporous process, it is characterized in that: by step 1) ~ 4) surface of metallic matrix of preparing forms the three-dimensional structure of large borehole jack aperture, macropore diameter 0.1-1 μm, small aperture 1-15nm, and reaming speed meets the linear relationship of Y=a*X+b substantially, wherein: Y represents the aperture of aluminum oxide micropore, and X represents etching time, a and b is constant, and at different concns, temperature, the value of constant is different.
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| CN109338432A (en) * | 2018-11-27 | 2019-02-15 | 东莞市慧泽凌化工科技有限公司 | A kind of electroplating technology of stainless steel and aluminium alloy compound part |
| CN111549348A (en) * | 2020-05-15 | 2020-08-18 | 计锋 | Metal part surface treatment method and metal part plastic complex |
| CN112048747A (en) * | 2020-08-06 | 2020-12-08 | 浙江大华技术股份有限公司 | Surface source black body and preparation method thereof |
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