CN103233258B - A kind of preparation method of the compactness enhancement type ceramic film based on differential arc oxidation and laser remolten - Google Patents
A kind of preparation method of the compactness enhancement type ceramic film based on differential arc oxidation and laser remolten Download PDFInfo
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Abstract
Based on a preparation method for the compactness enhancement type ceramic film of differential arc oxidation and laser remolten, it relates to a kind of method preparing compactness enhancement type ceramic film at the light metals such as magnesium, aluminium, titanium and alloy surface thereof.The present invention will solve Microarc Oxidation Surface Treatment technology can not possess less energy-consumption and the high performance problem of rete when the light metals such as aluminium, magnesium, titanium and alloy surface thereof prepare ceramic film simultaneously.Method: one, the pre-treatment of body material; Two, working fluid is prepared; Three, differential arc oxidation process; Four, laser remolten process MAO rete; The exemplar of compactness enhancement type ceramic film must be had.Rete prepared by the present invention and basal body binding force is good, dense structure, porosity is low, hardness is high and anticorrosion and wear resisting property good; Porosity can be down to less than 3%, and hardness value can be increased to the twice of the former MAO rete without laser remolten process.The present invention is used in the light metals such as magnesium, aluminium, titanium and alloy surface prepares compactness enhancement type ceramic film.
Description
Technical field
The present invention relates to a kind of method preparing compactness enhancement type ceramic film at the light metals such as magnesium, aluminium, titanium and alloy surface thereof.
Background technology
The ceramic film that Microarc Oxidation Surface Treatment technology is prepared at the light metals such as aluminium, magnesium, titanium and alloy surface thereof and matrix have good bonding force, significantly improve surface hardness, can improve matrix wear-resisting, anticorrosion, insulation and heat-proof quality, and working fluid is environment-friendly type, reaction is carried out under normal temperature, normal pressure, therefore, this technology has good application prospect.At present, the major obstacle of restriction differential arc oxidization technique application is the high energy consumption of technique, especially particularly outstanding in this problem of rete performance that preparation table surface hardness is high, the micro-arc oxidation process most of the time is the micro-arc discharge stage, if aluminum alloy materials micro-arc discharge voltage is usually between 380V ~ 550V, current density 8A/dm
2~ 20A/dm
2between, the hard film layer treatment time is usually at more than 90min, long electrion process makes differential arc oxidation energy consumption high, make its cost higher, and rete outside leaves a large amount of discharge channels, form loose porous tissue, and form primarily of the matrix oxide compound of noncrystalline phase, interior solid layer wear-resisting, the better performances such as anticorrosion, but the ratio that tight zone accounts for overall rete is usually not high, tight zone grows thicker need again extends the treatment time, consume more energy, therefore, film performance and energy consumption become conflict, govern the engineer applied of differential arc oxidization technique.
Summary of the invention
The present invention will solve Microarc Oxidation Surface Treatment technology can not possess less energy-consumption and the high performance problem of rete when the light metals such as aluminium, magnesium, titanium and alloy surface thereof prepare ceramic film simultaneously, and provides a kind of preparation method of the compactness enhancement type ceramic film based on differential arc oxidation and laser remolten.
The preparation method of a kind of compactness enhancement type ceramic film based on differential arc oxidation and laser remolten of the present invention, carries out according to the following steps:
One, the pre-treatment of body material: select 300
#sand paper ~ 2000
#two kinds in sand paper or wherein two or more model sand paper body material is polished step by step, again by the body material washing 3min ~ 5min after polishing, be the NaOH solution alkali cleaning 5min ~ 10min of 20g/L ~ 100g/L again by concentration, body material after alkali cleaning is put into acetone or dehydrated alcohol, through ultrasonic cleaning 1min ~ 3min that frequency is 24KHz ~ 40KHz, last clean 2min ~ 5min in deionized water after, air-dry or dry, obtain pretreated body material;
Two, working fluid is prepared: join in deionized water by main membrane-forming agent, pH value regulator, stablizer, tinting material and uniform coloring agent, be stirred to and dissolve completely, obtain the working fluid that pH is 8 ~ 10; In wherein said working fluid, the concentration of main membrane-forming agent is 5g/L ~ 100g/L, in described working fluid, the concentration of stablizer is 1g/L ~ 10g/L, in described working fluid, the concentration of tinting material is 3g/L ~ 15g/L, and the concentration of uniform coloring agent in described working fluid is 1g/L ~ 5g/L;
Three, differential arc oxidation process: the working fluid pretreated for step one body material being placed in step 2 preparation, with the pretreated body material of step one for positive pole, working fluid cell body is as negative pole, adopt current constant mode or constant voltage mode process 20min ~ 60min, working fluid temperature is kept to be 30 DEG C ~ 50 DEG C in treating processes, obtain the workpiece of thicknesses of layers more than 10 μm, then workpiece is carried out cleaning 3min ~ 10min in deionized water, finally be placed in dehydrated alcohol, after ultrasonic cleaning 5min ~ 10min that frequency is 24KHz ~ 40KHz, naturally dry or be dry 5min ~ 30min under the condition of 30 DEG C ~ 50 DEG C in temperature, namely the exemplar after differential arc oxidation process is obtained,
Four, laser remolten process MAO rete: the exemplar after differential arc oxidation process step 3 prepared is installed on laser machine tool worktable, with Nd:YAG laser apparatus or CO
2the high energy laser beam that laser apparatus produces carries out surface remelting process to the exemplar of differential arc oxidation process, and laser beam flying path is single hierarchic path scan mode, grid Recycle design or spiral-line Recycle design, and arranging light spot energy density is 50J/mm
2~ 400J/mm
2, obtain the exemplar after laser remolten, then polishing or grinding process carried out to the rete of the exemplar after laser remolten, namely obtain the exemplar with compactness enhancement type ceramic film.
Principle of work of the present invention: adopt free of contamination conductive liquid as working fluid between workpiece anode and cell body negative electrode, apply high-voltage pulse, workpiece surface is allowed to produce plasma discharge, high temperature and high pressure environment is formed in discharge channel, after the material melts of passage proximate and oxidation, grow matrix oxide ceramics in position, make rete and matrix form good bonding force, but initial stage film hardness is lower, in laser re-melting process, under the effect of laser beam high-energy radiation, it is more that the surface imperfection places such as the micropore tiny crack of spot area draw laser energy, highdensity heat energy makes first to form many small molten baths herein, after laser continues input energy, molten bath will toward outgrowth, expansion, adjacent molten bath will be converged, form larger reflow zone, melts in reflow zone undergoes phase transition under the high temperature conditions, generate the ceramic phase material that hardness is higher, simultaneously melt substance flows in pore in loose rete and space, loose rete starts after being heated to its fusing point to melt, form remelted layer, after cooling, MAO tectorium becomes the remelted layer of dense structure.
At matrix surface, advantage of the present invention: the preparation method that, the present invention is based on the compactness enhancement type ceramic film of differential arc oxidation and laser remolten, can prepare that bonding force is good, dense structure, porosity is low, hardness is high and anticorrosion and that wear resisting property is good rete; Two, the microscopic appearance of MAO rete is improved after laser remolten of the present invention, make tectorium tissue become fine and close, improve pyroceramic Phase Proportion in rete, improve film surface hardness, strengthen the anticorrosion and wear-resisting of rete and wait ceramic performance, simultaneously great reduction differential arc oxidation treatment time and energy consumption; Three, the present invention is environment friendly and pollution-free; Four, existing Microarc Oxidation Surface Treatment technology prepares ceramic film porosity more than 20% at the light metals such as aluminium, magnesium, titanium and alloy surface thereof, and the present invention laser remolten process is carried out to differential arc oxidation film layer after porosity can be down to less than 3%, hardness value can be increased to the twice of the former MAO rete without laser remolten process.
Accompanying drawing explanation
Fig. 1 is the systematic schematic diagram of step 4 laser remolten process MAO rete in embodiment one;
Fig. 2 is laser beam flying track schematic diagram when laser beam flying path is single hierarchic path scan mode in step 4 laser remolten process MAO rete process in embodiment one;
Fig. 3 is laser beam flying track schematic diagram when laser beam flying path is grid Recycle design in step 4 laser remolten process MAO rete process in embodiment one;
Fig. 4 is laser beam flying track schematic diagram when laser beam flying path is spiral-line Recycle design in step 4 laser remolten process MAO rete process in embodiment one;
Fig. 5 is the rete cross-section morphology figure of the exemplar after the differential arc oxidation process of this testing sequence three preparation;
Fig. 6 is the rete Cross Section Morphology figure with the exemplar of compactness enhancement type ceramic film of this test preparation.
Embodiment
Embodiment one: composition graphs 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, carries out according to the following steps:
One, the pre-treatment of body material: select 300
#sand paper ~ 2000
#two kinds in sand paper or wherein two or more model sand paper body material is polished step by step, again by the body material washing 3min ~ 5min after polishing, be the NaOH solution alkali cleaning 5min ~ 10min of 20g/L ~ 100g/L again by concentration, body material after alkali cleaning is put into acetone or dehydrated alcohol, through ultrasonic cleaning 1min ~ 3min that frequency is 24KHz ~ 40KHz, last clean 2min ~ 5min in deionized water after, air-dry or dry, obtain pretreated body material;
Two, working fluid is prepared: join in deionized water by main membrane-forming agent, pH value regulator, stablizer, tinting material and uniform coloring agent, be stirred to and dissolve completely, obtain the working fluid that pH is 8 ~ 10; In wherein said working fluid, the concentration of main membrane-forming agent is 5g/L ~ 100g/L, in described working fluid, the concentration of stablizer is 1g/L ~ 10g/L, in described working fluid, the concentration of tinting material is 3g/L ~ 15g/L, and the concentration of uniform coloring agent in described working fluid is 1g/L ~ 5g/L;
Three, differential arc oxidation process: the working fluid pretreated for step one body material being placed in step 2 preparation, with the pretreated body material of step one for positive pole, working fluid cell body is as negative pole, adopt current constant mode or constant voltage mode process 20min ~ 60min, working fluid temperature is kept to be 30 DEG C ~ 50 DEG C in treating processes, obtain the workpiece of thicknesses of layers more than 10 μm, then workpiece is carried out cleaning 3min ~ 10min in deionized water, finally be placed in dehydrated alcohol, after ultrasonic cleaning 5min ~ 10min that frequency is 24KHz ~ 40KHz, naturally dry or be dry 5min ~ 30min under the condition of 30 DEG C ~ 50 DEG C in temperature, namely the exemplar after differential arc oxidation process is obtained,
Four, laser remolten process MAO rete: the exemplar after differential arc oxidation process step 3 prepared is installed on laser machine tool worktable, with Nd:YAG laser apparatus or CO
2the high energy laser beam that laser apparatus produces carries out surface remelting process to the exemplar of differential arc oxidation process, and laser beam flying path is single hierarchic path scan mode, grid Recycle design or spiral-line Recycle design, and arranging light spot energy density is 50J/mm
2~ 400J/mm
2, obtain the exemplar after laser remolten, then polishing or grinding process carried out to the rete of the exemplar after laser remolten, namely obtain the exemplar with compactness enhancement type ceramic film.
In present embodiment step one, the object of polishing is to remove substrate material surface cut, oxide film and spot; In step one, the object of washing is scrubbing; Be the object of the NaOH solution alkali cleaning of 20g/L ~ 100g/L by concentration in step one be oil removing; The object in step one, the body material after alkali cleaning being put into acetone or dehydrated alcohol ultrasonic cleaning is to remove oil stain and dirt further; With the residuals that the object of washed with de-ionized water is to remove surface in step one.
In present embodiment step 2, the concentration of main membrane-forming agent is higher, and coating growth speed is faster, and in certain hour, film forming is thicker, and film surface also gets over roughness, and the pore dimension of rete is also larger; Adding tinting material in step 2 is color in order to deepen rete, strengthen rete smooth surface region 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 can reduce the temperature difference of film surface hole place and non-pore region, reduce rete internal stress, and make the uniformity consistency of remelting good.
Exemplar thicknesses of layers after differential arc oxidation process prepared by present embodiment step 3 is at more than 15um, and hardness is more than 300HV.
In present embodiment step 4 to the rete of the exemplar after laser remolten with 2000
#above sand paper carries out grinding process.
In present embodiment step 4, laser remolten can change microscopic appearance and the phase composite of material under laser beam heat effect, after laser remolten differential arc oxidation film layer, sealing of hole is effective, especially reduces the through hole running through film surface and matrix in differential arc oxidation film layer, the antiseptic property of rete is improved; After remelting, the tissue of rete becomes fine and close, and pyroceramic Phase Proportion improves, and hardness promotes, and wear resistance improves.In laser re-melting process, the heat transfer media of rete melts is air and inner ceramic rete, be different from the differential arc oxidation working fluid environment of energy fast cooling, laser remolten capacity usage ratio is higher, and is effective efficiency rete after outside tectorium remelting, can reduce the thickness that the differential arc oxidation stage prepares rete, therefore, can reduce energy consumption in conjunction with differential arc oxidation and laser remolten technique, improve the ratio of rete tight zone, rete and matrix also have good bonding force.In 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 laser facula energy density between coated material melting lower threshold and coating thermal damage threshold value, reflow process both nondestructive sintering MAO coating does not reach remelting effect because of the energy shortage of input MAO coating yet, and reflow process effect in sealing, hyperbaric environment is better.
In present embodiment step 4, laser energy density is by laser output power, area three parameters of the hot spot that laser scanning speed and laser beam are formed on rete determine, when other parameter constants, laser output power determines the film temperature of radiation areas, not affecting again the tissue of body material in order to reach remelting effect, requiring that the LASER HEATING temperature of spot area rete is near its fusing point; Sweep velocity have impact on 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; Arrange laser remolten parameter as follows: regulate Z axis coordinate, make laser focal be 10mm ~ 15mm to film surface distance, laser power is 20W ~ 300W, and laser scanning speed is 2mm/s ~ 100mm/s.
Prepared by present embodiment has the laser remolten layer thickness of the exemplar of compactness enhancement type ceramic film more than 5 μm, and after laser remolten, film hardness is greater than 800HV.
Fig. 1 is the systematic schematic diagram of present embodiment step 4 laser remolten process 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 laser beam flying track schematic diagram when laser beam flying path is single hierarchic path scan mode in present embodiment step 4 laser remolten process MAO rete process; Laser beam flying path is single hierarchic path scan mode, path planning as shown in Figure 2, laser facula scan round, moves ahead according to the step pitch being less than spot diameter, until the remelting surface of presetting is completely processed, wherein the Duplication between adjacent scan bands is kept to be 10 ~ 50%.
Fig. 3 is laser beam flying track schematic diagram when laser beam flying path is grid Recycle design in present embodiment step 4 laser remolten process MAO rete process; Laser beam flying path is grid Recycle design, path planning as shown in Figure 3, laser facula scan round, moves ahead according to the step pitch being less than spot diameter, until the remelting surface of presetting is completely processed, wherein the Duplication between adjacent scan bands is kept to be 10% ~ 50%.
Fig. 4 is laser beam flying track schematic diagram when laser beam flying path is spiral-line Recycle design in present embodiment step 4 laser remolten process MAO rete process; Laser beam flying path is spiral-line Recycle design, path planning as shown in Figure 4, laser facula scan round, moves ahead according to the step pitch being less than spot diameter, until the remelting surface of presetting is completely processed, wherein the Duplication between adjacent scan bands is kept to be 10% ~ 30%.
The principle of work of present embodiment: adopt free of contamination conductive liquid as working fluid between workpiece anode and cell body negative electrode, apply high-voltage pulse, workpiece surface is allowed to produce plasma discharge, high temperature and high pressure environment is formed in discharge channel, after the material melts of passage proximate and oxidation, grow matrix oxide ceramics in position, make rete and matrix form good bonding force, but initial stage film hardness is lower, in laser re-melting process, under the effect of laser beam high-energy radiation, it is more that the surface imperfection places such as the micropore tiny crack of spot area draw laser energy, highdensity heat energy makes first to form many small molten baths herein, after laser continues input energy, molten bath will toward outgrowth, expansion, adjacent molten bath will be converged, form larger reflow zone, melts in reflow zone undergoes phase transition under the high temperature conditions, generate the ceramic phase material that hardness is higher, simultaneously melt substance flows in pore in loose rete and space, loose rete starts after being heated to its fusing point to melt, form remelted layer, after cooling, MAO tectorium becomes the remelted layer of dense structure.
At matrix surface, present embodiment, based on the preparation method of the compactness enhancement type ceramic film of differential arc oxidation and laser remolten, can be prepared that bonding force is good, dense structure, porosity is low, hardness is high and anticorrosion and that wear resisting property is good rete.
The microscopic appearance of MAO rete is improved after present embodiment laser remolten, make tectorium tissue become fine and close, improve pyroceramic Phase Proportion in rete, improve film surface hardness, strengthen the anticorrosion and wear-resisting of rete and wait ceramic performance, simultaneously great reduction differential arc oxidation treatment time and energy consumption.
Present embodiment is environment friendly and pollution-free.
Existing Microarc Oxidation Surface Treatment technology prepares ceramic film porosity more than 20% at the light metals such as aluminium, magnesium, titanium and alloy surface thereof, and the present invention laser remolten process is carried out to differential arc oxidation film layer after porosity can be down to less than 3%, hardness value can be increased to the twice of the former MAO rete without laser remolten process.
Embodiment two: present embodiment and embodiment one unlike: the body material described in step one is magnesium, aluminium, titanium, magnesium alloy, aluminium alloy or titanium alloy.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two are unlike the main membrane-forming agent Na described in step 2
2siO
3, NaAlO
2, Na
3pO
4(NaPO
3)
6in a kind of or wherein several mixtures; PH value regulator described in step 2 is KOH or NaOH; Stablizer described in step 2 is KF or NaF; Tinting material described in step 2 is sodium wolframate, ammonium meta-vanadate, copper sulfate or H
3bO
3; Uniform coloring agent described in step 2 is disodium ethylene diamine tetraacetate (ETDA-2Na).Other is identical with embodiment one or two.
When main membrane-forming agent described in present embodiment is mixture, mix in any proportion between each component.
Embodiment four: one of present embodiment and embodiment one to three unlike: the current constant mode specific operation process described in step 3 is as follows: be 3A/dm in forward current density scope
2~ 40A/dm
2, negative current density range is 1A/dm
2~ 8A/dm
2, frequency be 50Hz ~ 1000Hz and dutycycle is process 20min ~ 60min under the condition of 10% ~ 70%.Other is identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: 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, and negative sense dutycycle is 10% ~ 40%, forward dutycycle be 10% ~ 40% and inter-train pause be process 20min ~ 60min under the condition of 10% ~ 30%; Described unipolarity constant current mode specific operation process is as follows: be 3A/dm at forward current density
2~ 30A/dm
2, frequency is 50Hz ~ 1000Hz and forward dutycycle is process 20min ~ 60min under the condition of 10% ~ 50%.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to three unlike: the constant voltage mode specific operation process described in step 3 is as follows: be 400V ~ 600V in forward voltage scope, negative voltage scope is 60V ~ 200V, and frequency is 50Hz ~ 1000Hz and dutycycle is process 20min ~ 60min under the condition of 10% ~ 70%.Other is identical with one of embodiment one to three.
Embodiment seven: one of present embodiment and embodiment one to six unlike: 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: present embodiment and embodiment seven unlike: described unipolarity constant voltage mode specific operation process is as follows: be 50Hz ~ 1000Hz in frequency, forward dutycycle is 10% ~ 50%, voltage of supply improves step by step from 300V, processes 20min ~ 60min under the condition that voltage rises to as 450V ~ 600V the most at last.Other is identical with embodiment seven.
Embodiment nine: present embodiment and embodiment seven unlike: described bipolarity constant voltage mode specific operation process is as follows: be 50Hz ~ 1000Hz in frequency, forward dutycycle is 10% ~ 40%, 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 processes 20min ~ 60min under rising to the condition of 80V ~ 100V the most at last.Other is identical with embodiment seven.
Adopt following verification experimental verification effect of the present invention:
Test one: composition graphs 1 and Fig. 2, a kind of preparation method of the compactness enhancement type ceramic film based on differential arc oxidation and laser remolten, carries 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, again by the aluminium alloy washing 5min after polishing, be the NaOH solution alkali cleaning 8min of 60g/L again by concentration, aluminium alloy after alkali cleaning is put into acetone, be the ultrasonic cleaning 3min of 40KHz through frequency, after the last 5min of cleaning in deionized water, dry, obtain pretreated aluminium alloy;
Two, working fluid is prepared: by Na
2siO
3, (NaPO
3)
6, KOH, KF, sodium wolframate and disodium ethylene diamine tetraacetate join in deionized water, be stirred to and dissolve completely, obtain the working fluid that pH is 8; In wherein said working fluid
for 20g/L, in described working fluid
for 8g/L, in described working fluid, the concentration of KF is 5g/L, and in described working fluid, the concentration of sodium wolframate is 5g/L, and in described working fluid, the concentration of disodium ethylene diamine tetraacetate is 3g/L;
Three, differential arc oxidation process: the working fluid pretreated for step one aluminium alloy being placed in step 2 preparation, with the pretreated aluminium alloy of step one for connecing positive source, the stainless steel trough body that working fluid is housed connects power cathode, adopt bipolarity constant current mode, wherein forward current 10A, negative current 4A, frequency 500Hz, negative sense dutycycle 40%, forward dutycycle 40%, inter-train pause is 20%, process 40min, working fluid temperature is kept to be 30 DEG C ~ 35 DEG C in treating processes, obtain thicknesses of layers at the workpiece of 18 μm, then wire cutting machine tool is utilized workpiece to be divided into the exemplar being of a size of 15mm × 15mm, after exemplar is carried out cleaning 8min in deionized water, finally be placed in dehydrated alcohol, be the ultrasonic cleaning 10min of 40KHz through frequency, until after clean surface under temperature is 50 DEG C of dry conditions dry 20min, namely the exemplar after differential arc oxidation process is obtained,
Four, laser remolten process MAO rete: the exemplar after differential arc oxidation process step 3 prepared is installed on laser machine tool worktable, Nd:YAG laser apparatus is adopted to carry out surface remelting process to the exemplar after differential arc oxidation process, laser beam flying path is single hierarchic path scan mode, as shown in Figure 2, laser remolten parameter is as follows: laser beam foucing is 12mm to film surface distance, laser power 23W, sweep velocity is 2mm/s ~ 10mm/s, laser scanning Duplication is 50%, obtain the little exemplar after laser remolten, then grinding process is carried out to the rete of the exemplar after laser remolten, namely the exemplar with compactness enhancement type ceramic film is obtained.
Aluminium alloy model described in this testing sequence one is 6082, is of a size of 100mm × 50mm × 4mm.
MAO power supply is the development of Harbin Di Si numerical control device company limited, and laser apparatus is that GUS company of Britain produces, and model is LUMONICSJK700.
The SIRION scanning electronic microscope (SEM) adopting FEI Co. of the U.S. to produce detects the surface of exemplar rete after the differential arc oxidation process of this testing sequence three preparation and the microscopic appearance in cross section, detected result as shown in Figure 5, Fig. 5 is the rete cross-section morphology figure of the exemplar after the differential arc oxidation process of this testing sequence three preparation, as shown in Figure 5, the rete of the exemplar after differential arc oxidation process is cashed as loose porous, thin and the features such as organization internal multiple cracks of tight zone, after the analysis of ImageJ2x image processing software, obtain its porosity is 25.01%.
The SIRION scanning electronic microscope (SEM) adopting FEI Co. of the U.S. to produce detects the surface of exemplar rete with compactness enhancement type ceramic film and the microscopic appearance in cross section of this test preparation, detected result as shown in Figure 6, Fig. 6 is the rete Cross Section Morphology figure with the exemplar of compactness enhancement type ceramic film of this test preparation, as shown in Figure 6, the pore with the exemplar rete inside of compactness enhancement type ceramic film obtained after carrying out laser remolten process and crackle reduced number, compactness significantly improves, film surface also becomes smooth, after the analysis of ImageJ2x image processing software, obtain its porosity is 2.11%.
Adopt Japanese Zhu Shi society DUH-W201S ultra microhardness meter detect differential arc oxidation process prepared by this testing sequence three after the film hardness of exemplar and the film hardness with the exemplar of compactness enhancement type ceramic film prepared of this test, detection data are as follows: the film hardness of the exemplar after differential arc oxidation process prepared by this testing sequence three is 432HV, the film hardness with the exemplar of compactness enhancement type ceramic film of this test preparation is 963HV, known, after laser remolten process MAO rete, hardness improves 123%.
Claims (8)
1., based on a preparation method for the compactness enhancement type ceramic film of differential arc oxidation and laser remolten, it is characterized in that the preparation method of the compactness enhancement type ceramic film based on differential arc oxidation and laser remolten carries out according to the following steps:
One, the pre-treatment of body material: select 300
#sand paper ~ 2000
#two kinds in sand paper or wherein two or more model sand paper body material is polished step by step, again by the body material washing 3min ~ 5min after polishing, be the NaOH solution alkali cleaning 5min ~ 10min of 20g/L ~ 100g/L again by concentration, body material after alkali cleaning is put into acetone or dehydrated alcohol, through ultrasonic cleaning 1min ~ 3min that frequency is 24KHz ~ 40KHz, last clean 2min ~ 5min in deionized water after, air-dry or dry, obtain pretreated body material;
Two, working fluid is prepared: join in deionized water by main membrane-forming agent, pH value regulator, stablizer, tinting material and uniform coloring agent, be stirred to and dissolve completely, obtain the working fluid that pH is 8 ~ 10; In wherein said working fluid, the concentration of main membrane-forming agent is 5g/L ~ 100g/L, in described working fluid, the concentration of stablizer is 1g/L ~ 10g/L, in described working fluid, the concentration of tinting material is 3g/L ~ 15g/L, and the concentration of uniform coloring agent in described working fluid is 1g/L ~ 5g/L;
Three, differential arc oxidation process: the working fluid pretreated for step one body material being placed in step 2 preparation, with the pretreated body material of step one for positive pole, working fluid cell body is as negative pole, adopt current constant mode or constant voltage mode process 20min ~ 60min, working fluid temperature is kept to be 30 DEG C ~ 50 DEG C in treating processes, obtain the workpiece of thicknesses of layers more than 10 μm, then workpiece is carried out cleaning 3min ~ 10min in deionized water, finally be placed in dehydrated alcohol, after ultrasonic cleaning 5min ~ 10min that frequency is 24KHz ~ 40KHz, naturally dry or be dry 5min ~ 30min under the condition of 30 DEG C ~ 50 DEG C in temperature, namely the exemplar after differential arc oxidation process is obtained,
Four, laser remolten process MAO rete: the exemplar after differential arc oxidation process step 3 prepared is installed on laser machine tool worktable, with Nd:YAG laser apparatus or CO
2the high energy laser beam that laser apparatus produces carries out surface remelting process to the exemplar of differential arc oxidation process, and laser beam flying path is single hierarchic path scan mode, grid Recycle design or spiral-line Recycle design, and arranging light spot energy density is 50J/mm
2~ 400J/mm
2, obtain the exemplar after laser remolten, then polishing or grinding process carried out to the rete of the exemplar after laser remolten, namely obtain the exemplar with compactness enhancement type ceramic film;
Main membrane-forming agent Na described in step 2
2siO
3, NaAlO
2, Na
3pO
4(NaPO
3)
6in a kind of or wherein several mixtures; PH value regulator described in step 2 is KOH or NaOH; Stablizer described in step 2 is KF or NaF; Tinting material described in step 2 is sodium wolframate, ammonium meta-vanadate, copper sulfate or H
3bO
3; Uniform coloring agent described in step 2 is disodium ethylene diamine tetraacetate.
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 step one 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 current constant mode specific operation process described in step 3 is as follows: be 3A/dm in forward current density scope
2~ 40A/dm
2, negative current density range is 1A/dm
2~ 8A/dm
2, frequency be 50Hz ~ 1000Hz and dutycycle is process 20min ~ 60min under the condition of 10% ~ 70%.
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 or 3, 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, and negative sense dutycycle is 10% ~ 40%, forward dutycycle be 10% ~ 40% and inter-train pause be process 20min ~ 60min under the condition of 10% ~ 30%; Described unipolarity constant current mode specific operation process is as follows: be 3A/dm at forward current density
2~ 30A/dm
2, frequency is 50Hz ~ 1000Hz and forward dutycycle is process 20min ~ 60min under the condition of 10% ~ 50%.
5. 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 step 3 is as follows: be 400V ~ 600V in forward voltage scope, negative voltage scope is 60V ~ 200V, and frequency is 50Hz ~ 1000Hz and dutycycle is process 20min ~ 60min under the condition of 10% ~ 70%.
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 or 5, is characterized in that described constant voltage mode is unipolarity constant voltage mode or bipolarity constant voltage mode.
7. the preparation method of a kind of compactness enhancement type ceramic film based on differential arc oxidation and laser remolten according to claim 6, it is characterized in that described unipolarity constant voltage mode specific operation process is as follows: be 50Hz ~ 1000Hz in frequency, forward dutycycle is 10% ~ 50%, voltage of supply improves step by step from 300V, processes 20min ~ 60min under the condition that voltage rises to as 450V ~ 600V the most at last.
8. the preparation method of a kind of compactness enhancement type ceramic film based on differential arc oxidation and laser remolten according to claim 6, it is characterized in that described bipolarity constant voltage mode specific operation process is as follows: be 50Hz ~ 1000Hz in frequency, forward dutycycle is 10% ~ 40%, 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 processes 20min ~ 60min under rising to the condition of 80V ~ 100V the most at last.
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