CN103233258A - Method for preparing dense enhancement type ceramic membrane based on micro-arc oxidizing and laser remelting - Google Patents
Method for preparing dense enhancement type ceramic membrane based on micro-arc oxidizing and laser remelting Download PDFInfo
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Abstract
一种基于微弧氧化和激光重熔的致密性增强型陶瓷膜层的制备方法，它涉及一种在镁、铝、钛等轻金属及其合金表面制备致密性增强型陶瓷膜层的方法。本发明是要解决微弧氧化表面处理技术在铝、镁、钛等轻金属及其合金表面制备陶瓷膜层时不能同时具备低能耗和膜层高性能的问题。方法：一、基体材料的预处理；二、配制工作液；三、微弧氧化处理；四、激光重熔处理MAO膜层；即得具有致密性增强型陶瓷膜层的样件。本发明制备的膜层与基体结合力好、组织致密、孔隙率低、硬度高且防腐和耐磨性能好；孔隙率可降至3%以下，硬度值可提高至未经激光重熔处理的原MAO膜层的两倍。本发明可用于在镁、铝、钛等轻金属及其合金表面制备致密性增强型陶瓷膜层。
The invention discloses a preparation method of a density-enhanced ceramic film layer based on micro-arc oxidation and laser remelting, which relates to a method for preparing a density-enhanced ceramic film layer on the surface of light metals such as magnesium, aluminum, titanium and their alloys. The invention aims to solve the problem that the micro-arc oxidation surface treatment technology cannot simultaneously possess low energy consumption and high performance of the film layer when preparing ceramic film layers on the surface of aluminum, magnesium, titanium and other light metals and their alloys. Methods: 1. Pretreatment of matrix material; 2. Preparation of working solution; 3. Micro-arc oxidation treatment; 4. Laser remelting treatment of MAO film layer; that is, a sample with enhanced density ceramic film layer. The film layer prepared by the present invention has good bonding force with the substrate, dense structure, low porosity, high hardness, and good anti-corrosion and wear resistance; the porosity can be reduced to below 3%, and the hardness value can be increased to that without laser remelting treatment. Twice the original MAO film layer. The invention can be used to prepare denseness-enhanced ceramic film layers on the surface of light metals such as magnesium, aluminum, titanium and their alloys.
Description
Technical field
The present invention relates to a kind of method for preparing compactness enhancement type ceramic film at light metals such as magnesium, aluminium, titanium and alloy surface thereof.
Background technology
The Microarc Oxidation Surface Treatment technology has bonding force preferably at ceramic film and the matrix of light metal such as aluminium, magnesium, titanium and alloy surface preparation thereof, significantly improve surface hardness, can improve wear-resisting, anticorrosion, insulation and the heat-proof quality of matrix, and working fluid is environment-friendly type, be reflected under normal temperature, the normal pressure and carry out, therefore, this technology has application promise in clinical practice.At present, the major obstacle that the restriction differential arc oxidization technique is used is the high energy consumption of technology, especially particularly outstanding in high this problem performance of rete of preparation surface hardness, the differential arc oxidation process most of the time is the micro-arc discharge stage, as aluminum alloy materials micro-arc discharge voltage usually between 380V～550V, current density 8A/dm
2～20A/dm
2Between, the hard film layer treatment time is usually more than 90min, for a long time the electrion process makes differential arc oxidation energy consumption height, make its cost higher, and the rete outside stays a large amount of discharge channels, form loose porous tissue, and mainly formed by the matrix oxide compound of noncrystalline phase, interior solid layer wear-resisting, better performances such as anticorrosion, but that tight zone accounts for the ratio of whole rete usually is not high, tight zone are grown to such an extent that thicklyer need prolong the treatment time again, consume more energy, therefore, film performance and energy consumption become a pair of contradiction, and the engineering that is restricting differential arc oxidization technique is used.
Summary of the invention
The present invention will solve the Microarc Oxidation Surface Treatment technology can not possess less energy-consumption and the high performance problem of rete simultaneously when light metals such as aluminium, magnesium, titanium and alloy surface thereof prepare ceramic film, and a kind of preparation method of the compactness enhancement type ceramic film based on differential arc oxidation and laser remolten is provided.
The preparation method of a kind of compactness enhancement type ceramic film based on differential arc oxidation and laser remolten of the present invention, carry out according to the following steps:
One, the pre-treatment of body material: select 300
#Sand paper～2000
#In the sand paper two kinds or wherein two or more model sand paper body material is polished step by step, body material washing 3min～5min after will polishing again, be NaOH solution alkali cleaning 5min～10min of 20g/L～100g/L again with concentration, body material after the alkali cleaning is put into acetone or dehydrated alcohol, be ultrasonic cleaning 1min～3min of 24KHz～40KHz through frequency, after in deionized water, cleaning 2min～5min at last, air-dry or dry, obtain pretreated body material;
Two, preparation working fluid: main membrane-forming agent, pH value conditioning agent, stablizer, tinting material and uniform coloring agent are joined in the deionized water, be stirred to fully and dissolve, obtain pH and be 8～10 working fluid; The concentration of main membrane-forming agent is 5g/L～100g/L in the wherein said working fluid, the concentration of stablizer is 1g/L～10g/L in the described working fluid, the concentration of tinting material is 3g/L～15g/L in the described working fluid, and the concentration of uniform coloring agent is 1g/L～5g/L in the described working fluid;
Three, differential arc oxidation is handled: the working fluid that the pretreated body material of step 1 is placed the step 2 preparation, be positive pole with the pretreated body material of step 1, the working fluid cell body is as negative pole, adopt current constant mode or constant voltage mode to handle 20min～60min, keeping the working fluid temperature in the treating processes is 30 ℃～50 ℃, obtain the workpiece of thicknesses of layers more than 10 μ m, then workpiece is cleaned 3min～10min in deionized water, place dehydrated alcohol at last, after being ultrasonic cleaning 5min～10min of 24KHz～40KHz through frequency, naturally dry or be dry 5min～30min under 30 ℃～50 ℃ the condition in temperature, namely obtain the exemplar after differential arc oxidation is handled;
Four, laser remolten is handled the MAO rete: the exemplar after the differential arc oxidation of step 3 preparation is handled is installed to the laser machine tool worktable, with Nd:YAG laser apparatus or CO
2The exemplar that the high energy laser beam that laser apparatus produces is handled differential arc oxidation carries out surface remelting to be handled, and the laser beam flying path is single hierarchic path scan mode, grid Recycle design or spiral-line Recycle design, and it is 50J/mm that light spot energy density is set
2～400J/mm
2, obtaining the exemplar behind the laser remolten, the rete to the exemplar behind the laser remolten polishes or grinding process then, namely obtains having the exemplar of compactness enhancement type ceramic film.
Principle of work of the present invention: between workpiece anode and cell body negative electrode, adopt free of contamination conductive liquid as working fluid, apply high-voltage pulse, allow workpiece surface produce plasma discharge, in discharge channel, form high temperature and high pressure environment, after the material thawing and oxidation near the passage, grow the matrix oxide ceramics in position, make rete and matrix form bonding force preferably, but the initial stage film hardness is lower; In the laser remolten process, under the effect of laser beam high-energy radiation, it is more that surface imperfection places such as the micropore tiny crack of spot area draw laser energy, highdensity heat energy makes and forms many small molten baths herein earlier, after laser continues the input energy, the molten bath will be toward outgrowth, expansion, adjacent molten bath will be converged, form bigger reflow zone, the melts in the reflow zone undergoes phase transition under hot conditions, generates the higher ceramic phase material of hardness, melt substance flows in loose the rete interior pore and space simultaneously, loose rete begins to melt after being heated to its fusing point, forms remelted layer, and cooling back MAO tectorium becomes the remelted layer of dense structure.
Advantage of the present invention: one, the present invention is based on the preparation method of the compactness enhancement type ceramic film of differential arc oxidation and laser remolten, can prepare at matrix surface that bonding force is good, dense structure, porosity is low, hardness is high and rete anticorrosion and that wear resisting property is good; Two, improve the microscopic appearance of MAO rete behind the laser remolten of the present invention, make the tectorium tissue become fine and close, improve pyroceramic phase ratio in the rete, improve film surface hardness, strengthen the anticorrosion and wear-resisting ceramic performance that waits of rete, great reduction differential arc oxidation treatment time and energy consumption simultaneously; Three, the present invention is environment friendly and pollution-free; Four, existing Microarc Oxidation Surface Treatment technology prepares the ceramic film porosity more than 20% at light metal such as aluminium, magnesium, titanium and alloy surface thereof, and the present invention carries out laser remolten to differential arc oxidation film layer and handles the back porosity and can be down to below 3%, and hardness value can be increased to the twice of the former MAO rete of handling without laser remolten.
Description of drawings
Fig. 1 is the systematic schematic diagram that the step 4 laser remolten is handled the MAO rete in the embodiment one;
Fig. 2 is that the step 4 laser remolten is handled laser beam flying track synoptic diagram when the laser beam flying path is the single hierarchic path scan mode in the MAO rete process in the embodiment one;
Fig. 3 is that the step 4 laser remolten is handled laser beam flying track synoptic diagram when the laser beam flying path is the grid Recycle design in the MAO rete process in the embodiment one;
Fig. 4 is that the step 4 laser remolten is handled laser beam flying track synoptic diagram when the laser beam flying path is the spiral-line Recycle design in the MAO rete process in the embodiment one;
Fig. 5 is the rete cross section microscopic appearance figure of the exemplar after the differential arc oxidation of this testing sequence three preparations is handled;
Fig. 6 is the rete cross section shape appearance figure of the exemplar with compactness enhancement type ceramic film of this test preparation.
Embodiment
Embodiment one: in conjunction with Fig. 1～Fig. 4, the preparation method of a kind of compactness enhancement type ceramic film based on differential arc oxidation and laser remolten of present embodiment, carry out according to the following steps:
One, the pre-treatment of body material: select 300
#Sand paper～2000
#In the sand paper two kinds or wherein two or more model sand paper body material is polished step by step, body material washing 3min～5min after will polishing again, be NaOH solution alkali cleaning 5min～10min of 20g/L～100g/L again with concentration, body material after the alkali cleaning is put into acetone or dehydrated alcohol, be ultrasonic cleaning 1min～3min of 24KHz～40KHz through frequency, after in deionized water, cleaning 2min～5min at last, air-dry or dry, obtain pretreated body material;
Two, preparation working fluid: main membrane-forming agent, pH value conditioning agent, stablizer, tinting material and uniform coloring agent are joined in the deionized water, be stirred to fully and dissolve, obtain pH and be 8～10 working fluid; The concentration of main membrane-forming agent is 5g/L～100g/L in the wherein said working fluid, the concentration of stablizer is 1g/L～10g/L in the described working fluid, the concentration of tinting material is 3g/L～15g/L in the described working fluid, and the concentration of uniform coloring agent is 1g/L～5g/L in the described working fluid;
Three, differential arc oxidation is handled: the working fluid that the pretreated body material of step 1 is placed the step 2 preparation, be positive pole with the pretreated body material of step 1, the working fluid cell body is as negative pole, adopt current constant mode or constant voltage mode to handle 20min～60min, keeping the working fluid temperature in the treating processes is 30 ℃～50 ℃, obtain the workpiece of thicknesses of layers more than 10 μ m, then workpiece is cleaned 3min～10min in deionized water, place dehydrated alcohol at last, after being ultrasonic cleaning 5min～10min of 24KHz～40KHz through frequency, naturally dry or be dry 5min～30min under 30 ℃～50 ℃ the condition in temperature, namely obtain the exemplar after differential arc oxidation is handled;
Four, laser remolten is handled the MAO rete: the exemplar after the differential arc oxidation of step 3 preparation is handled is installed to the laser machine tool worktable, with Nd:YAG laser apparatus or CO
2The exemplar that the high energy laser beam that laser apparatus produces is handled differential arc oxidation carries out surface remelting to be handled, and the laser beam flying path is single hierarchic path scan mode, grid Recycle design or spiral-line Recycle design, and it is 50J/mm that light spot energy density is set
2～400J/mm
2, obtaining the exemplar behind the laser remolten, the rete to the exemplar behind the laser remolten polishes or grinding process then, namely obtains having the exemplar of compactness enhancement type ceramic film.
The purpose of polishing in the present embodiment step 1 is in order to remove substrate material surface cut, oxide film and spot; The purpose of washing in the step 1 is scrubbing; Be that the purpose of the NaOH solution alkali cleaning of 20g/L～100g/L is oil removing with concentration in the step 1; The purpose of in the step 1 body material after the alkali cleaning being put into acetone or dehydrated alcohol ultrasonic cleaning is in order further to remove oil stain and dirt; Purpose with washed with de-ionized water in the step 1 is in order to remove the residuals on surface.
The concentration of main membrane-forming agent is more high in the present embodiment step 2, and coating growth speed is more fast, and film forming is more thick in the certain hour, and film surface is also got over roughness, and the pore dimension of rete is also more big; Adding tinting material in the step 2 is in order to deepen the color of rete, reinforcing membrane laminar surface smooth domain is to the sorption of laser beam energy, the micropore of film surface presents high-absorbility to laser energy, film surface melanism or heighten the color and to reduce the temperature difference of film surface hole place and non-pore region, reduce the rete internal stress, and make that the uniformity consistency of remelting is good.
Exemplar thicknesses of layers after the differential arc oxidation of present embodiment step 3 preparation is handled is more than 15um, and hardness surpasses 300HV.
In the present embodiment step 4 to the rete of the exemplar behind the laser remolten with 2000
#Above sand paper carries out grinding process.
Laser remolten can change microscopic appearance and the phase composite of material in the present embodiment step 4 under the laser beam heat effect, behind the laser remolten differential arc oxidation film layer, sealing of hole is effective, especially reduces the through hole that runs through film surface and matrix in the differential arc oxidation film layer, makes the antiseptic property of rete improve; The tissue of rete becomes fine and close after the remelting, and pyroceramic phase ratio improves, and hardness promotes, and wear resistance improves.In the laser remolten process, it is air and inner ceramic rete that the heat of rete melts transmits medium, the differential arc oxidation working fluid environment that is different from the energy fast cooling, the laser remolten capacity usage ratio is higher, and is the effective efficiency rete after the outside tectorium remelting, can reduce the thickness that the differential arc oxidation stage prepares rete, therefore, can cut down the consumption of energy in conjunction with differential arc oxidation and laser remolten technology, improve the ratio of rete tight zone, rete and matrix also have bonding force preferably.In the laser remolten treating processes, laser head is according to preset path scanning MAO coating, rational laser output power, focal length and sweep velocity are set, make the laser facula energy density between coated material fusion lower threshold and coating thermal damage threshold value, both nondestructive sintering MAO coating was not because the energy shortage of input MAO coating reached the remelting effect to reflow process yet, and reflow process effect in sealing, hyperbaric environment is better.
Laser energy density is by laser output power in the present embodiment step 4, laser scanning speed and laser beam determine in three parameters of area of the hot spot that rete forms, under the situation of other parameter constants, laser output power has determined the film temperature of radiation areas, do not influence the tissue of body material again in order to reach the remelting effect, require the LASER HEATING temperature of spot area rete near its fusing point; Sweep velocity has influenced the soaking time of hot spot melt substance, suitably reduces the generation that sweep velocity is conducive to phase transformation, improves the generation of crystalline ceramic phase material; It is as follows that the laser remolten parameter is set: regulate the Z axial coordinate, make laser focal be 10mm～15mm to the film surface distance, laser power is 20W～300W, and laser scanning speed is 2mm/s～100mm/s.
The laser remolten layer thickness of the exemplar with compactness enhancement type ceramic film of present embodiment preparation is more than 5 μ m, and film hardness is greater than 800HV behind the laser remolten.
Fig. 1 is the systematic schematic diagram that present embodiment step 4 laser remolten is handled the MAO rete, and system is made up of laser apparatus, condenser lens, worktable and X/Y/Z axle and digital control system thereof.
Fig. 2 is that present embodiment step 4 laser remolten is handled laser beam flying track synoptic diagram when the laser beam flying path is the single hierarchic path scan mode in the MAO rete process; The laser beam flying path is the single hierarchic path scan mode, path planning as shown in Figure 2, laser facula scan round moves ahead according to the step pitch less than spot diameter, processed fully until default remelting surface, wherein keeping the Duplication between the adjacent scanning strip is 10～50%.
Fig. 3 is that present embodiment step 4 laser remolten is handled laser beam flying track synoptic diagram when the laser beam flying path is the grid Recycle design in the MAO rete process; The laser beam flying path is the grid Recycle design, path planning as shown in Figure 3, laser facula scan round moves ahead according to the step pitch less than spot diameter, processed fully until default remelting surface, wherein keeping the Duplication between the adjacent scanning strip is 10%～50%.
Fig. 4 is that present embodiment step 4 laser remolten is handled laser beam flying track synoptic diagram when the laser beam flying path is the spiral-line Recycle design in the MAO rete process; The laser beam flying path is the spiral-line Recycle design, path planning as shown in Figure 4, laser facula scan round moves ahead according to the step pitch less than spot diameter, processed fully until default remelting surface, wherein keeping the Duplication between the adjacent scanning strip is 10%～30%.
The principle of work of present embodiment: between workpiece anode and cell body negative electrode, adopt free of contamination conductive liquid as working fluid, apply high-voltage pulse, allow workpiece surface produce plasma discharge, in discharge channel, form high temperature and high pressure environment, after the material thawing and oxidation near the passage, grow the matrix oxide ceramics in position, make rete and matrix form bonding force preferably, but the initial stage film hardness is lower; In the laser remolten process, under the effect of laser beam high-energy radiation, it is more that surface imperfection places such as the micropore tiny crack of spot area draw laser energy, highdensity heat energy makes and forms many small molten baths herein earlier, after laser continues the input energy, the molten bath will be toward outgrowth, expansion, adjacent molten bath will be converged, form bigger reflow zone, the melts in the reflow zone undergoes phase transition under hot conditions, generates the higher ceramic phase material of hardness, melt substance flows in loose the rete interior pore and space simultaneously, loose rete begins to melt after being heated to its fusing point, forms remelted layer, and cooling back MAO tectorium becomes the remelted layer of dense structure.
Present embodiment is based on the preparation method of the compactness enhancement type ceramic film of differential arc oxidation and laser remolten, can prepare at matrix surface that bonding force is good, dense structure, porosity is low, hardness is high and rete anticorrosion and that wear resisting property is good.
Improve the microscopic appearance of MAO rete behind the present embodiment laser remolten, make the tectorium tissue become fine and close, improve pyroceramic phase ratio in the rete, improve film surface hardness, strengthen the anticorrosion and wear-resisting ceramic performance that waits of rete, great reduction differential arc oxidation treatment time and energy consumption simultaneously.
Present embodiment is environment friendly and pollution-free.
Existing Microarc Oxidation Surface Treatment technology prepares the ceramic film porosity more than 20% at light metal such as aluminium, magnesium, titanium and alloy surface thereof, and the present invention carries out laser remolten to differential arc oxidation film layer and handles the back porosity and can be down to below 3%, and hardness value can be increased to the twice of the former MAO rete of handling without laser remolten.
Embodiment two: what present embodiment and embodiment one were different is: the body material described in the step 1 is magnesium, aluminium, titanium, magnesium alloy, aluminium alloy or titanium alloy.Other is identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is: the main membrane-forming agent Na described in the step 2
2SiO
3, NaAlO
2, Na
3PO
4(NaPO
3)
6In a kind of or several mixture wherein; PH value conditioning agent described in the step 2 is KOH or NaOH; Stablizer described in the step 2 is KF or NaF; Tinting material described in the step 2 is sodium wolframate, ammonium meta-vanadate, copper sulfate or H
3BO
3Uniform coloring agent described in the step 2 is disodium ethylene diamine tetraacetate (ETDA-2Na).Other is identical with embodiment one or two.
When the described main membrane-forming agent of present embodiment is mixture, presses arbitrary proportion between each component and mix.
Embodiment four: what present embodiment was different with one of embodiment one to three is: the current constant mode specific operation process described in the step 3 is as follows: be 3A/dm in the forward current density scope
2～40A/dm
2, the negative current density range is 1A/dm
2～8A/dm
2, frequency is that 50Hz～1000Hz and dutycycle are to handle 20min～60min under 10%～70% the condition.Other is identical with one of embodiment one to three.
Embodiment five: what present embodiment was different with one of embodiment one to four is: described current constant mode is bipolarity constant current mode or unipolarity constant current mode; Described bipolarity constant current mode specific operation process is as follows: be 3A/dm at forward current density
2～30A/dm
2, negative current density is 1A/dm
2～5A/dm
2, supply frequency is 50Hz～1000Hz, the negative sense dutycycle is 10%～40%, the forward dutycycle be 10%～40% and inter-train pause be to handle 20min～60min under 10%～30% the condition; Described unipolarity constant current mode specific operation process is as follows: be 3A/dm at forward current density
2～30A/dm
2, frequency is that 50Hz～1000Hz and forward dutycycle are to handle 20min～60min under 10%～50% the condition.Other is identical with one of embodiment one to four.
Embodiment six: what present embodiment was different with one of embodiment one to three is: the constant voltage mode specific operation process described in the step 3 is as follows: be 400V～600V in the forward voltage scope, the negative voltage scope is 60V～200V, and frequency is that 50Hz～1000Hz and dutycycle are to handle 20min～60min under 10%～70% the condition.Other is identical with one of embodiment one to three.
Embodiment seven: what present embodiment was different with one of embodiment one to six is: described constant voltage mode is unipolarity constant voltage mode or bipolarity constant voltage mode.Other is identical with one of embodiment one to six.
Embodiment eight: what present embodiment and embodiment seven were different is: described unipolarity constant voltage mode specific operation process is as follows: be 50Hz～1000Hz in frequency, the forward dutycycle is 10%～50%, voltage of supply improves step by step from 300V, and voltage rises under the condition for 450V～600V and handles 20min～60min the most at last.Other is identical with embodiment seven.
Embodiment nine: what present embodiment and embodiment seven were different is: described bipolarity constant voltage mode specific operation process is as follows: be 50Hz～1000Hz in frequency, the forward dutycycle is 10%～40%, the negative sense dutycycle is 10%～40%, forward voltage improves step by step from 300V, forward voltage rises to 450V～600V the most at last, negative voltage improves step by step from 60V, and negative voltage rises under the condition of 80V～100V and handles 20min～60min the most at last.Other is identical with embodiment seven.
Adopt following verification experimental verification effect of the present invention:
Test one: in conjunction with Fig. 1 and Fig. 2, a kind of preparation method of the compactness enhancement type ceramic film based on differential arc oxidation and laser remolten, carry out according to the following steps:
One, the pre-treatment of body material: with 600
#, 1000
#With 2000
#Sand paper is polished step by step to aluminium alloy, aluminium alloy washing 5min after will polishing again, be the NaOH solution alkali cleaning 8min of 60g/L again with concentration, aluminium alloy after the alkali cleaning is put into acetone, be the ultrasonic cleaning 3min of 40KHz through frequency, after in deionized water, cleaning 5min at last, dry, obtain pretreated aluminium alloy;
Two, preparation working fluid: with Na
2SiO
3, (NaPO
3)
6, KOH, KF, sodium wolframate and disodium ethylene diamine tetraacetate join in the deionized water, is stirred to dissolving fully, obtains pH and be 8 working fluid; In the wherein said working fluid
Be 20g/L, in the described working fluid
Be 8g/L, the concentration of KF is 5g/L in the described working fluid, and the concentration of sodium wolframate is 5g/L in the described working fluid, and the concentration of disodium ethylene diamine tetraacetate is 3g/L in the described working fluid;
Three, differential arc oxidation is handled: the working fluid that the pretreated aluminium alloy of step 1 is placed the step 2 preparation, with the pretreated aluminium alloy of step 1 for connecing positive source, the stainless steel trough body that working fluid is housed connects power cathode, adopt the bipolarity constant current mode, forward current 10A wherein, negative current 4A, frequency 500Hz, negative sense dutycycle 40%, forward dutycycle 40%, inter-train pause is 20%, handle 40min, keeping the working fluid temperature in the treating processes is 30 ℃～35 ℃, obtains thicknesses of layers at the workpiece of 18 μ m, utilize wire cutting machine tool workpiece to be divided into the exemplar that is of a size of 15mm * 15mm then, exemplar cleaned 8min in deionized water after, placing dehydrated alcohol at last, is the ultrasonic cleaning 10min of 40KHz through frequency, until being dry 20min under the condition of 50 ℃ of dryings in temperature behind the surface cleaning, namely obtain the exemplar after differential arc oxidation is handled;
Four, laser remolten is handled the MAO rete: the exemplar after the differential arc oxidation of step 3 preparation is handled is installed to the laser machine tool worktable, adopting the Nd:YAG laser apparatus to carry out surface remelting to the exemplar after the differential arc oxidation processing handles, the laser beam flying path is the single hierarchic path scan mode, as shown in Figure 2, the laser remolten parameter is as follows: laser beam foucing to film surface distance is 12mm, laser power 23W, sweep velocity is 2mm/s～10mm/s, the laser scanning Duplication is 50%, obtain the little exemplar behind the laser remolten, rete to the exemplar behind the laser remolten carries out grinding process then, namely obtains having the exemplar of compactness enhancement type ceramic film.
Aluminium alloy model described in this testing sequence one is 6082, is of a size of 100mm * 50mm * 4mm.
The MAO power supply is this numerical control device company limited development of Harbin enlightening, and laser apparatus is that Britain GUS company produces, and model is LUMONICSJK700.
The surface of the exemplar rete after the differential arc oxidation that the SIRION scanning electronic microscope (SEM) that adopts U.S. FEI Co. to produce detects three preparations of this testing sequence is handled and the microscopic appearance in cross section, detected result as shown in Figure 5, Fig. 5 is the rete cross section microscopic appearance figure of the exemplar after the differential arc oxidation of this testing sequence three preparations is handled, as shown in Figure 5, the rete of the exemplar after differential arc oxidation is handled is cashed to loose porous, features such as the thin and organization internal multiple cracks of tight zone, obtaining its porosity after the analysis of ImageJ2x image processing software is 25.01%.
The SIRION scanning electronic microscope (SEM) that adopts U.S. FEI Co. to produce detects the surface of the exemplar rete with compactness enhancement type ceramic film that this test prepares and the microscopic appearance in cross section, detected result as shown in Figure 6, Fig. 6 is the rete cross section shape appearance figure of the exemplar with compactness enhancement type ceramic film of this test preparation, as shown in Figure 6, carry out pore and the crackle reduced number of the exemplar rete inside with compactness enhancement type ceramic film that obtains after laser remolten is handled, compactness obviously improves, it is smooth that film surface also becomes, and obtaining its porosity after the analysis of ImageJ2x image processing software is 2.11%.
Adopt Japanese Zhu Shi society the film hardness of the exemplar of the DUH-W201S submicroscopic sclerometer differential arc oxidation that detects three preparations of this testing sequence after handling and the film hardness of the exemplar with compactness enhancement type ceramic film that this test prepares, the detection data are as follows: the film hardness of the exemplar after the differential arc oxidation of this testing sequence three preparations is handled is 432HV, the film hardness of the exemplar with compactness enhancement type ceramic film of this test preparation is 963HV, as can be known, behind laser remolten processing MAO rete, hardness has improved 123%.
Claims (9)
1. preparation method based on the compactness enhancement type ceramic film of differential arc oxidation and laser remolten is characterized in that carrying out according to the following steps based on the preparation method of the compactness enhancement type ceramic film of differential arc oxidation and laser remolten:
One, the pre-treatment of body material: select 300
#Sand paper～2000
#In the sand paper two kinds or wherein two or more model sand paper body material is polished step by step, body material washing 3min～5min after will polishing again, be NaOH solution alkali cleaning 5min～10min of 20g/L～100g/L again with concentration, body material after the alkali cleaning is put into acetone or dehydrated alcohol, be ultrasonic cleaning 1min～3min of 24KHz～40KHz through frequency, after in deionized water, cleaning 2min～5min at last, air-dry or dry, obtain pretreated body material;
Two, preparation working fluid: main membrane-forming agent, pH value conditioning agent, stablizer, tinting material and uniform coloring agent are joined in the deionized water, be stirred to fully and dissolve, obtain pH and be 8～10 working fluid; The concentration of main membrane-forming agent is 5g/L～100g/L in the wherein said working fluid, the concentration of stablizer is 1g/L～10g/L in the described working fluid, the concentration of tinting material is 3g/L～15g/L in the described working fluid, and the concentration of uniform coloring agent is 1g/L～5g/L in the described working fluid;
Three, differential arc oxidation is handled: the working fluid that the pretreated body material of step 1 is placed the step 2 preparation, be positive pole with the pretreated body material of step 1, the working fluid cell body is as negative pole, adopt current constant mode or constant voltage mode to handle 20min～60min, keeping the working fluid temperature in the treating processes is 30 ℃～50 ℃, obtain the workpiece of thicknesses of layers more than 10 μ m, then workpiece is cleaned 3min～10min in deionized water, place dehydrated alcohol at last, after being ultrasonic cleaning 5min～10min of 24KHz～40KHz through frequency, naturally dry or be dry 5min～30min under 30 ℃～50 ℃ the condition in temperature, namely obtain the exemplar after differential arc oxidation is handled;
Four, laser remolten is handled the MAO rete: the exemplar after the differential arc oxidation of step 3 preparation is handled is installed to the laser machine tool worktable, with Nd:YAG laser apparatus or CO
2The exemplar that the high energy laser beam that laser apparatus produces is handled differential arc oxidation carries out surface remelting to be handled, and the laser beam flying path is single hierarchic path scan mode, grid Recycle design or spiral-line Recycle design, and it is 50J/mm that light spot energy density is set
2～400J/mm
2, obtaining the exemplar behind the laser remolten, the rete to the exemplar behind the laser remolten polishes or grinding process then, namely obtains having the exemplar of compactness enhancement type ceramic film.
2. the preparation method of a kind of compactness enhancement type ceramic film based on differential arc oxidation and laser remolten according to claim 1 is characterized in that the body material described in the step 1 is magnesium, aluminium, titanium, magnesium alloy, aluminium alloy or titanium alloy.
3. the preparation method of a kind of compactness enhancement type ceramic film based on differential arc oxidation and laser remolten according to claim 1 is characterized in that the main membrane-forming agent Na described in the step 2
2SiO
3, NaAlO
2, Na
3PO
4(NaPO
3)
6In a kind of or several mixture wherein; PH value conditioning agent described in the step 2 is KOH or NaOH; Stablizer described in the step 2 is KF or NaF; Tinting material described in the step 2 is sodium wolframate, ammonium meta-vanadate, copper sulfate or H
3BO
3Uniform coloring agent described in the step 2 is disodium ethylene diamine tetraacetate.
4. the preparation method of a kind of compactness enhancement type ceramic film based on differential arc oxidation and laser remolten according to claim 1 is characterized in that the current constant mode specific operation process described in the step 3 is as follows: be 3A/dm in the forward current density scope
2～40A/dm
2, the negative current density range is 1A/dm
2～8A/dm
2, frequency is that 50Hz～1000Hz and dutycycle are to handle 20min～60min under 10%～70% the condition.
5. according to the preparation method of claim 1 or 4 described a kind of compactness enhancement type ceramic films based on differential arc oxidation and laser remolten, it is characterized in that described current constant mode is bipolarity constant current mode or unipolarity constant current mode; Described bipolarity constant current mode specific operation process is as follows: be 3A/dm at forward current density
2～30A/dm
2, negative current density is 1A/dm
2～5A/dm
2, supply frequency is 50Hz～1000Hz, the negative sense dutycycle is 10%～40%, the forward dutycycle be 10%～40% and inter-train pause be to handle 20min～60min under 10%～30% the condition; Described unipolarity constant current mode specific operation process is as follows: be 3A/dm at forward current density
2～30A/dm
2, frequency is that 50Hz～1000Hz and forward dutycycle are to handle 20min～60min under 10%～50% the condition.
6. the preparation method of a kind of compactness enhancement type ceramic film based on differential arc oxidation and laser remolten according to claim 1, it is characterized in that the constant voltage mode specific operation process described in the step 3 is as follows: be 400V～600V in the forward voltage scope, the negative voltage scope is 60V～200V, and frequency is that 50Hz～1000Hz and dutycycle are to handle 20min～60min under 10%～70% the condition.
7. according to the preparation method of claim 1 or 6 described a kind of compactness enhancement type ceramic films based on differential arc oxidation and laser remolten, it is characterized in that described constant voltage mode is unipolarity constant voltage mode or bipolarity constant voltage mode.
8. the preparation method of a kind of compactness enhancement type ceramic film based on differential arc oxidation and laser remolten according to claim 7, it is characterized in that described unipolarity constant voltage mode specific operation process is as follows: be 50Hz～1000Hz in frequency, the forward dutycycle is 10%～50%, voltage of supply improves step by step from 300V, and voltage rises under the condition for 450V～600V and handles 20min～60min the most at last.
9. the preparation method of a kind of compactness enhancement type ceramic film based on differential arc oxidation and laser remolten according to claim 7, it is characterized in that described bipolarity constant voltage mode specific operation process is as follows: be 50Hz～1000Hz in frequency, the forward dutycycle is 10%～40%, the negative sense dutycycle is 10%～40%, forward voltage improves step by step from 300V, forward voltage rises to 450V～600V the most at last, negative voltage improves step by step from 60V, and negative voltage rises under the condition of 80V～100V and handles 20min～60min the most at last.
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