CN102560591A - Micro-arc oxidation electrolyte and micro-arc oxidation method - Google Patents
Micro-arc oxidation electrolyte and micro-arc oxidation method Download PDFInfo
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- CN102560591A CN102560591A CN2011103923043A CN201110392304A CN102560591A CN 102560591 A CN102560591 A CN 102560591A CN 2011103923043 A CN2011103923043 A CN 2011103923043A CN 201110392304 A CN201110392304 A CN 201110392304A CN 102560591 A CN102560591 A CN 102560591A
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- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000003792 electrolyte Substances 0.000 title claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 63
- 238000007789 sealing Methods 0.000 claims abstract description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 12
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 86
- 230000003647 oxidation Effects 0.000 claims description 85
- 239000008151 electrolyte solution Substances 0.000 claims description 45
- 239000006185 dispersion Substances 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 18
- 235000012239 silicon dioxide Nutrition 0.000 claims description 13
- 229960001866 silicon dioxide Drugs 0.000 claims description 12
- 230000010355 oscillation Effects 0.000 claims description 11
- 239000010935 stainless steel Substances 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 10
- 150000003016 phosphoric acids Chemical class 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 9
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 239000008139 complexing agent Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 235000019353 potassium silicate Nutrition 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical group [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 3
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 3
- 229940038773 trisodium citrate Drugs 0.000 claims description 3
- 229910000838 Al alloy Inorganic materials 0.000 claims description 2
- 239000004111 Potassium silicate Substances 0.000 claims description 2
- 101710194948 Protein phosphatase PhpP Proteins 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 claims description 2
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 2
- UGTZMIPZNRIWHX-UHFFFAOYSA-K sodium trimetaphosphate Chemical compound [Na+].[Na+].[Na+].[O-]P1(=O)OP([O-])(=O)OP([O-])(=O)O1 UGTZMIPZNRIWHX-UHFFFAOYSA-K 0.000 claims description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 2
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 13
- 230000007797 corrosion Effects 0.000 abstract description 13
- 239000000203 mixture Substances 0.000 abstract description 10
- 239000007864 aqueous solution Substances 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract 3
- 239000003637 basic solution Substances 0.000 abstract 2
- 239000002270 dispersing agent Substances 0.000 abstract 2
- 229910019142 PO4 Inorganic materials 0.000 abstract 1
- 238000005299 abrasion Methods 0.000 abstract 1
- 239000010452 phosphate Substances 0.000 abstract 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 description 16
- 238000011056 performance test Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000012528 membrane Substances 0.000 description 4
- 230000003245 working effect Effects 0.000 description 4
- 229910000737 Duralumin Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 241001504664 Crossocheilus latius Species 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a micro-arc oxidation electrolyte and a micro-arc oxidation method. The micro-arc oxidation electrolyte comprises the following components: a basic solution, a wear-resisting agent, a pore sealing agent and a dispersing agent, wherein the basic solution is phosphate and silicate aqueous solution of pH 8-12, the wear-resisting agent is graphite powder, the pore sealing agent is silica powder or alumina powder, and the dispersing agent is polyoxyethylenealkylphenol ether. The micro-arc oxidation electrolyte of the invention is simple in composition, and easy in control. Light metal parts to be plated are subjected to micro-arc oxidation using the micro-arc oxidation electrolyte of the invention, and are directly subjected to pore sealing treatment in the micro-arc oxidation process without after-treatment. The process of the invention is simple, and obtained micro-arc oxide film layer is high in hardness, and is good in abrasion resistance and corrosion resistance.
Description
Technical field
The present invention and metal covering list processing technique field especially relate to a kind of differential arc oxidation electrolytic solution and differential arc oxidation method.
Background technology
At present, light metal such as aluminium, titanium and alloy thereof, in light weight with it, specific tenacity is high, stone roller property and ductility are good, be easy to machining characteristics is widely used in aspects such as space flight and aviation, automobile and electron trade; But the surperficial matter of light metal material is soft, not wear-resistant, non-refractory, and the corrosion potential of light metal is lower, and is all unstable in most of media; Solidity to corrosion is relatively poor, though the surface of light metal can form sull under state of nature, the sull that forms naturally is loose porous; Can not protect inner metal,, therefore need carry out oxidation light metal surface for overcoming the defective of light metal surface aspect of performance; Make it form the fine and close sull of one deck; To improve its surface property, enlarge its range of application, prolong its work-ing life.
Differential arc oxidization technique is a kind of novel surface treatment technology of material that on the basis of conventional anodization, grows up, and handles through spark discharge under the high pressure, utilizes the directly growth in situ ceramic membrane in the metallic surface of differential of the arc district moment high temperature sintering effect; This membrane structure is fine and close; With the complete metallurgical binding of body, can well solve surface-treated problem in the light metal alloy practical application, excessive but the micro-arc oxidation films that differential arc oxidation obtains exists frictional coefficient; Especially in the use of friction pair; Wearing and tearing that can aggravation mill part, and the micro-arc oxidation films that produces has porousness, some hole even always extend to the surface of protected light metal from coatingsurface; Corrosive medium can pass these holes and reach protected light metal surface; The surface of corrosion light metal and at the interface cumulative corrosion product, make micro-arc oxidation films be full of cracks, come off, therefore for the performance that do not reduce micro-arc oxidation films with enlarge its application in precision high quality mechanical part; Be necessary the hole on micro-arc oxidation films surface is carried out shutoff, to improve the work-ing life on micro-arc oxidation films surface.
For example, one Chinese patent application publication No. CN102041541 discloses and has a kind ofly prepared the technology of composite ceramic film at Mg alloy surface May 4 2011 Granted publication day, and its core prescription is on colloidal sol preparation and electrolyte prescription.Electrolyte prescription is: prescription 1: water glass 20%, Potassium monofluoride 10%, sodium hydroxide %, 15-20 minute differential arc oxidation time.Prescription 2: water glass 6-15g/L, Sodium Tetraborate 2-5g/L, Pottasium Hydroxide 3-5g/L, Potassium monofluoride 3-6g/L, 15-20 minute differential arc oxidation time.The preparation prescription of colloidal sol: tetraethoxy (TEOS, SiO2 content >=28.0%); Absolute ethyl alcohol; Hydrochloric acid: deionized water.Its weak point is, before micro-arc oxidation process, needs to need earlier to adopt and flood-lift the system embrane method and form silica dioxide coating on the magnesium alloy differential arc oxidation film layer surface, and will repeatedly flood and lift, and technology is more loaded down with trivial details.
Summary of the invention
The objective of the invention is in order to overcome the above-mentioned deficiency of prior art; A kind of differential arc oxidation electrolytic solution that contains micron-sized graphite powder, nano level silicon-dioxide powdery or alumina powder jointed and dispersion agent is provided; The differential arc oxidation method of the above-mentioned differential arc oxidation electrolytic solution of a kind of usefulness also is provided; Make the differential arc oxidation film hardness that forms behind the differential arc oxidation high, wear resistance, good corrosion resistance need not to carry out follow-up sealing of hole and handle.
To achieve these goals, the present invention adopts following technical scheme:
A kind of differential arc oxidation electrolytic solution; Comprise following component: basal liquid, anti-wear agent, hole sealing agent and dispersion agent; Described basal liquid is that pH is phosphoric acid salt, the aqueous silicate solution of 8-12; Described anti-wear agent is the graphite powder, and described hole sealing agent is a silicon-dioxide powdery or alumina powder jointed, and described dispersion agent is a polyoxyethylenealkylphenol ether.
Anti-wear agent and hole sealing agent are insoluble to basal liquid, and making this differential arc oxidation electrolytic solution is a kind of suspension-s, and basal liquid is the aqueous solution of phosphoric acid salt, silicate; Phosphoric acid salt can improve the compactness of rate of film build and sull, reduce porosity, and silicate can make the micro-arc oxidation films surface ratio of formation more even; And phosphoric acid salt and silicate cost are lower, and under the effect of strong pulse electric current, micron-sized Graphite Powder 99 is known from experience dispersed deposition in micro-arc oxidation films; Make micro-arc oxidation films have lubricity, thereby can reduce the frictional coefficient of micro-arc oxidation films, produce antifriction effect; Thereby improve the wear resistance of micro-arc oxidation films, and aluminum oxide or silicon-dioxide are a kind of superhard materials, under the effect of strong pulse electric current; Nano level aluminum oxide or silicon-dioxide can form a kind of mutually compound in the ceramic film of being deposited on synchronously with the Graphite Powder 99 body again; Be filled in the hole in the ceramic film, make the differential arc oxidation membrane structure of formation fine and close more, can improve the hardness of oxidation film layer; The dispersion agent polyoxyethylenealkylphenol ether make graphite powder and aluminum oxide or silicon-dioxide can be in electrolytic solution homodisperse; The phenomenon of uniting can not occur, avoid ceramic film surface irregularity, interior porosity behind the differential arc oxidation big, influence its performance and work-ing life.
As preferably, described anti-wear agent particle diameter is 1-10 μ m, and described hole sealing agent particle diameter is 5-20nm; In the differential arc oxidation electrolytic solution, the weight percent of anti-wear agent is 3%-5%, and the weight percent of hole sealing agent is 1%-3%; The concentration of dispersion agent is 0.2-0.5g/L, and the add-on of graphite powder and alumina powder jointed or silicon-dioxide powdery is excessive, then can block discharge channel; Cause the electrolytic solution afunction, almost can not carry out differential arc oxidation, and add-on is too small; Do not reach needed effect again, simultaneously, add-on alumina powder jointed or silicon-dioxide powdery also influences the thickness of ceramic film; Polyoxyethylenealkylphenol ether had both made alumina powder jointed or silicon-dioxide powdery uniform distribution in electrolytic solution, had also improved alumina powder jointed or the sticking power of silicon-dioxide powdery in ceramic film, and the graphite diameter of particle is a micron order; And alumina powder jointed or silicon-dioxide powdery particle diameter is a micron order, is filled in the hole more easily and goes.
As preferably; Described phosphoric acid salt is one or more in Trisodium trimetaphosphate, Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, sodium polyphosphate, the sodium phosphate; Described silicate is water glass and/or potassium silicate, and in the differential arc oxidation electrolytic solution, phosphatic total concn is 8-12g/L; The total concn of silicate is 10-15g/L; Phosphoric acid salt mainly influences the porosity in differential arc oxidation film forming speed and the ceramic film, and silicate mainly influences oxidation film layer surface smooth degree, and the above-mentioned phosphoric acid salt and the concentration range of silicate are the optimum process condition scope that differential arc oxidation forms ceramic film.
As preferably, also comprise additive in the described differential arc oxidation electrolytic solution, described additive comprises stablizer, complexing agent; Described stablizer is USP Kosher and/or terepthaloyl moietie, and described complexing agent is YD 30 and/or Trisodium Citrate, in the differential arc oxidation electrolytic solution; The total concn of stablizer is 0.1-0.5g/L; The total concn of complexing agent is 0.1-0.5g/L, and stablizer can play the effect of stabilizing solution, makes the solution in the electrolytic process be difficult for splashing; The adding of complexing agent can improve the performance of light metal surface micro-arc oxidation films, and YD 30 and Trisodium Citrate all can improve the fineness and the homogeneity of light metal surface micro-arc oxidation films.
A kind of differential arc oxidation method fills the unplated piece immersion in the electrolyzer like each described differential arc oxidation electrolytic solution in the claim 1 to 4, and unplated piece is as anode; Stainless steel plate is as negative electrode; Under the differential arc oxidation condition, make the unplated piece surface form the micro-arc oxidation films of fine and close thickness, directly add anti-wear agent, hole sealing agent and dispersion agent in the differential arc oxidation electrolytic solution, when differential arc oxidation, can directly carry out sealing of hole and handle formed ceramic film; Need not to carry out follow-up sealing of hole, process step is simple.
As preferably; Add anti-wear agent, hole sealing agent and dispersion agent in the described basal liquid simultaneously; Add back sonic oscillation 20-30min, use sonic oscillation, make graphite powder, alumina powder jointed or silicon-dioxide powdery, polyoxyethylenealkylphenol ether can in basal liquid, form equally distributed suspension liquid system; Behind differential arc oxidation, can be evenly distributed in the formed ceramic film, make ceramic film have good compactness and wear resistance.
As preferably, the material of described light metal unplated piece is magnesiumalloy, aluminum or aluminum alloy, and magnesiumalloy, aluminium, duraluminum are all in light weight with it, specific tenacity is high, stone roller property and ductility are good, be easy to machining characteristics; Be widely used, but unstable, solidity to corrosion is relatively poor; Therefore need carry out differential arc oxidation to its surface, make it form one deck micro-arc oxidation films, to improve its surface property; Enlarge its range of application, prolong its work-ing life.
Adopt differential arc oxidation electrolytic solution provided by the invention and differential arc oxidation method; Can form one deck wear resistance, good corrosion resistance on the surface of unplated piece, the micro-arc oxidation films that hardness is high, and also differential arc oxidation electrolytic solution is formed simple; Micro-arc oxidation process is simple, need not to carry out follow-up sealing of hole.
Therefore, the present invention has following beneficial effect:
(1) differential arc oxidation electrolytic solution of the present invention is formed simply, is easy to control;
(2) directly in the process of differential arc oxidation, carry out sealing of hole, need not aftertreatment and carry out sealing of hole, technology is simple;
(3) the formed differential arc oxidation film hardness of differential arc oxidation method of the present invention is high, wear resistance, good corrosion resistance.
Embodiment
Below in conjunction with embodiment the present invention is done further description.
Embodiment 1
It is in 8 the basal liquid that anti-wear agent, hole sealing agent and dispersion agent add pH simultaneously; Add back sonic oscillation 20min, will immerse with the unplated piece that magnesiumalloy is processed again and fill in the electrolyzer of differential arc oxidation electrolytic solution, with unplated piece as anode; Stainless steel plate is as negative electrode; At reaction times 5min, electrolyte temperature is 15 ℃, and current density is 5A/dm
2Voltage is to carry out differential arc oxidation under the micro-arc oxidation process condition of 150V, makes the surface of unplated piece form the fine and close micro-arc oxidation films of one deck, and the composition of differential arc oxidation electrolytic solution is as shown in table 1; Resulting micro-arc oxidation films is carried out performance test, and the result is as shown in table 2.
Embodiment 2
It is in 10 the basal liquid that anti-wear agent, hole sealing agent and dispersion agent add pH simultaneously; Add back sonic oscillation 25min, will immerse with the unplated piece that magnesiumalloy is processed again and fill in the electrolyzer of differential arc oxidation electrolytic solution, with unplated piece as anode; Stainless steel plate is as negative electrode; At reaction times 25min, electrolyte temperature is 35 ℃, and current density is 12A/dm
2Voltage is to carry out differential arc oxidation under the micro-arc oxidation process condition of 300V, makes the surface of unplated piece form the fine and close micro-arc oxidation films of one deck, and the composition of differential arc oxidation electrolytic solution is as shown in table 1; Resulting micro-arc oxidation films is carried out performance test, and the result is as shown in table 2.
Embodiment 3
It is in 12 the basal liquid that anti-wear agent, hole sealing agent and dispersion agent add pH simultaneously; Add back sonic oscillation 30min, will immerse with the unplated piece that magnesiumalloy is processed again and fill in the electrolyzer of differential arc oxidation electrolytic solution, with unplated piece as anode; Stainless steel plate is as negative electrode; At reaction times 30min, electrolyte temperature is 40 ℃, and current density is 15A/dm
2Voltage is to carry out differential arc oxidation under the micro-arc oxidation process condition of 550V, makes the surface of unplated piece form the fine and close micro-arc oxidation films of one deck, and the composition of differential arc oxidation electrolytic solution is as shown in table 1; Resulting micro-arc oxidation films is carried out performance test, and the result is as shown in table 2.
Embodiment 4
It is in 10 the basal liquid that anti-wear agent, hole sealing agent and dispersion agent add pH simultaneously; Add back sonic oscillation 20min, the unplated piece that is formed from aluminium immersed fill in the electrolyzer of differential arc oxidation electrolytic solution again, with unplated piece as anode; Stainless steel plate is as negative electrode; At reaction times 25min, electrolyte temperature is 35 ℃, and current density is 12A/dm
2Voltage is to carry out differential arc oxidation under the micro-arc oxidation process condition of 550V, makes the surface of unplated piece form the fine and close micro-arc oxidation films of one deck, and the composition of differential arc oxidation electrolytic solution is as shown in table 1; Resulting micro-arc oxidation films is carried out performance test, and the result is as shown in table 2.
Embodiment 5
It is in 8 the basal liquid that anti-wear agent, hole sealing agent and dispersion agent add pH simultaneously; Add back sonic oscillation 25min, the unplated piece that is formed from aluminium immersed fill in the electrolyzer of differential arc oxidation electrolytic solution again, with unplated piece as anode; Stainless steel plate is as negative electrode; At reaction times 5min, electrolyte temperature is 20 ℃, and current density is 5A/dm
2Voltage is to carry out differential arc oxidation under the micro-arc oxidation process condition of 320V, makes the surface of unplated piece form the fine and close micro-arc oxidation films of one deck, and the composition of differential arc oxidation electrolytic solution is as shown in table 1; Resulting micro-arc oxidation films is carried out performance test, and the result is as shown in table 2.
Embodiment 6
It is in 10 the basal liquid that anti-wear agent, hole sealing agent and dispersion agent add pH simultaneously; Add back sonic oscillation 30min, the unplated piece that is formed from aluminium immersed fill in the electrolyzer of differential arc oxidation electrolytic solution again, with unplated piece as anode; Stainless steel plate is as negative electrode; At reaction times 15min, electrolyte temperature is 15 ℃, and current density is 12A/dm
2Voltage is to carry out differential arc oxidation under the micro-arc oxidation process condition of 400V, makes the surface of unplated piece form the fine and close micro-arc oxidation films of one deck, and the composition of differential arc oxidation electrolytic solution is as shown in table 1; Resulting micro-arc oxidation films is carried out performance test, and the result is as shown in table 2.
Embodiment 7
It is in 12 the basal liquid that anti-wear agent, hole sealing agent and dispersion agent add pH simultaneously; Add back sonic oscillation 30min, will immerse with the unplated piece that duraluminum is processed again and fill in the electrolyzer of differential arc oxidation electrolytic solution, with unplated piece as anode; Stainless steel plate is as negative electrode; At reaction times 5min, electrolyte temperature is 40 ℃, and current density is 5A/dm
2Voltage is to carry out differential arc oxidation under the micro-arc oxidation process condition of 150V, makes the surface of unplated piece form the fine and close micro-arc oxidation films of one deck, and the composition of differential arc oxidation electrolytic solution is as shown in table 1; Resulting micro-arc oxidation films is carried out performance test, and the result is as shown in table 2.
Embodiment 8
It is in 10 the basal liquid that anti-wear agent, hole sealing agent and dispersion agent add pH simultaneously; Add back sonic oscillation 20min, will immerse with the unplated piece that duraluminum is processed again and fill in the electrolyzer of differential arc oxidation electrolytic solution, with unplated piece as anode; Stainless steel plate is as negative electrode; At reaction times 30min, electrolyte temperature is 30 ℃, and current density is 15A/dm
2Voltage is to carry out differential arc oxidation under the micro-arc oxidation process condition of 300V, makes the surface of unplated piece form the fine and close micro-arc oxidation films of one deck, and the composition of differential arc oxidation electrolytic solution is as shown in table 1; Resulting micro-arc oxidation films is carried out performance test, and the result is as shown in table 2.
Performance test comprises:
(1) surfaceness test: with roughness tester (Shanghai Cai Kang opticinstrument ltd; JB-3C) scriber moves a segment distance at workpiece surface; The waveform of scriber being walked out through the computer processor that is connected with scriber amplifies and measures the spacing of its crest and trough, and by the surface roughness Ra value that indicating gauge is read workpiece, Ra is more little; The roughness that oxide ceramic membrane is described is more little, and the surface is smooth more.
(2) wearability test: with RCA paper tape wear resistant instrument (F350008), the differential arc oxidation film layer of friction workpiece surface under 180 gram forces is milled to and exposes workpiece material when surface, and the number of turns that the record rubber wheel rotates, the number of turns bright ceramic film wear resistance of speaking more more is good more.
(3) pencil hardness test: according to ASTM D3363; Load: 80 grams, pencil: the UNI of Mitsubishi, with pencil hardness meter F13002; Mounted pencil hardness meter is placed on the ceramic film surface to be promoted forward; According to the order of pencil hardness by hard to soft progressively test, scratch is not till nib fully can scratch workpiece ceramic film surface with the visual inspection sample surface, the hardness of pencil is promptly represented the hardness of ceramic film at this moment.
(4) neutral salt spray corrosion test: workpiece is placed (the positive laboratory apparatus in source, Shanghai ltd in the salt air corrosion case; FQY050); 35 ℃ use down concentration be the sodium chloride aqueous solution of 5 ± 0.5 weight % in the spraying 48 hours continuously of the differential arc oxidation film layer of workpiece surface, takes out then and observe, and the percentage composition that the corroded area of recording surface accounts for the rete total area is as the salt air corrosion ratio; Ratio is more little, explains that erosion resistance is good more.
Each component and content thereof in the differential arc oxidation electrolytic solution of each embodiment of table 1
The data results that each embodiment of table 2 carries out performance test
Can find out from the The performance test results of table 2; The surfaceness of the micro-arc oxidation films on the light metal unplated piece surface of adopting differential arc oxidation electrolytic solution provided by the invention and differential arc oxidation method and obtaining is low; Wear resistance, good corrosion resistance, hardness is high, need not to carry out follow-up sealing of hole and handles.
Claims (8)
1. differential arc oxidation electrolytic solution; It is characterized in that; Comprise following component: basal liquid, anti-wear agent, hole sealing agent and dispersion agent, described basal liquid are that pH is phosphoric acid salt, the aqueous silicate solution of 8-12, and described anti-wear agent is the graphite powder; Described hole sealing agent is a silicon-dioxide powdery or alumina powder jointed, and described dispersion agent is a polyoxyethylenealkylphenol ether.
2. differential arc oxidation electrolytic solution according to claim 1; It is characterized in that described anti-wear agent particle diameter is 1-10 μ m, described hole sealing agent particle diameter is 5-20nm; In the differential arc oxidation electrolytic solution; The weight percent of anti-wear agent is 3%-5%, and the weight percent of hole sealing agent is 1%-3%, and the concentration of dispersion agent is 0.2-0.5 g/L.
3. differential arc oxidation electrolytic solution according to claim 1; It is characterized in that; Described phosphoric acid salt is one or more in Trisodium trimetaphosphate, Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, sodium polyphosphate, the sodium phosphate, and described silicate is water glass and/or potassium silicate, in the differential arc oxidation electrolytic solution; Phosphatic total concn is 8-12 g/L, and the total concn of silicate is 10-15 g/L.
4. differential arc oxidation electrolytic solution according to claim 1 is characterized in that, also comprises additive in the described differential arc oxidation electrolytic solution; Described additive comprises stablizer, complexing agent; Described stablizer is USP Kosher and/or terepthaloyl moietie, and described complexing agent is YD 30 and/or Trisodium Citrate, in the differential arc oxidation electrolytic solution; The total concn of stablizer is 0.1-0.5 g/L, and the total concn of complexing agent is 0.1-0.5 g/L.
5. differential arc oxidation method; It is characterized in that; The immersion of light metal unplated piece is filled in the electrolyzer like each described differential arc oxidation electrolytic solution in the claim 1 to 4; Unplated piece is as anode, and stainless steel plate makes the unplated piece surface form the micro-arc oxidation films of fine and close thickness under the differential arc oxidation condition as negative electrode.
6. differential arc oxidation method according to claim 5 is characterized in that, described differential arc oxidation condition is reaction times 5-30 min, and electrolyte temperature is 15-40 ℃, and current density is 5-15A/dm
2, voltage range is 150-550 V.
7. differential arc oxidation method according to claim 5 is characterized in that, described anti-wear agent, hole sealing agent and dispersion agent add in the basal liquid simultaneously, adds back sonic oscillation 20-30 min.
8. differential arc oxidation method according to claim 5 is characterized in that, the material of described light metal unplated piece is magnesiumalloy, aluminum or aluminum alloy.
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