CN109023470A - The modified aluminium alloy extrusions of a kind of aluminium alloy section surface differential arc oxidation method of modifying and surface - Google Patents
The modified aluminium alloy extrusions of a kind of aluminium alloy section surface differential arc oxidation method of modifying and surface Download PDFInfo
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- CN109023470A CN109023470A CN201811114851.3A CN201811114851A CN109023470A CN 109023470 A CN109023470 A CN 109023470A CN 201811114851 A CN201811114851 A CN 201811114851A CN 109023470 A CN109023470 A CN 109023470A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/024—Anodisation under pulsed or modulated current or potential
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/16—Pretreatment, e.g. desmutting
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
- C25D11/246—Chemical after-treatment for sealing layers
Abstract
The present invention relates to the modified aluminium alloy extrusions of a kind of aluminium alloy section surface differential arc oxidation method of modifying and surface, which comprises a) pre-treatment: aluminium alloy extrusions completes pre-treatment through purging ash disposal, cleaning oil removing, washing, drying；B) micro-arc oxidation treatment: aluminium alloy extrusions being placed in electrolyte and carries out differential arc oxidation, and electrolyte includes following components: Na2SiO3、Na2B4O7, KOH, glycerine, Na2MoO4,EDTA-2Na；It is taken out after the completion of differential arc oxidation；C) it post-processes: after being cleaned, being dried to aluminium alloy extrusions, sealing pores being carried out to micro-arc oxidation films layer surface using polyvinylidene fluoride resin.The modified aluminium alloy extrusions in gained surface of the invention, sealing pores are carried out with polyvinylidene fluoride resin after micro-arc oxidation treatment, sealing of hole effect is good and surface compact is smooth, has excellent wearability, corrosion resistance and electrical insulation capability, greatly improves the comprehensive performance of aluminium alloy extrusions.
Description
Technical field
The invention belongs to aluminium alloy section surface processing technology fields, and in particular to a kind of aluminium alloy section surface differential of the arc oxygen
Change method of modifying, also relates to a kind of above method and prepare resulting surface modification aluminium alloy extrusions.
Background technique
Aluminium is that one of big metal of most wide six is distributed in nature, accounts for about the 8.0% of earth's crust gross mass, and density is small, molten
Point is low, easy to process, can be made into various profiles；But the intensity of fine aluminium is very low, should not make structural material.By long-term production
Practice and scientific research, people gradually carry out reinforced aluminum alloying element is added and with the methods of heat treatment, obtain a series of
Aluminium alloy, aluminium alloy keep fine aluminium it is light the advantages that while can also intensity with higher, become ideal structural material.
Aluminium alloy extrusions is light with its, inexpensive, Gao Biqiang, electric-conductivity heat-conductivity high, solderability, it is recyclable the advantages that, aerospace,
It has been widely applied in communications and transportation, machine-building, building, decorations and chemical industry.
However aluminium alloy is as structural material, that there are quality is soft, wear no resistance, in particular circumstances intolerant to burn into intolerant to
The disadvantages of high temperature, although aluminium alloy spontaneous in air can form Al on surface2O3Film layer, but thin layer is very thin and defect compared with
It is more, matrix can not effectively be protected, therefore people are by various methods surface-treated aluminium alloy extrusions to mention
Rise its performance.According to the property of process characteristic and gained protective layer, aluminium alloy section surface processing technique can be divided into chemical oxidation
Processing, chemical plating, thermal spraying, common anode oxidation processes, micro-arc oxidation treatment etc..
Micro-arc oxidation treatment is also known as microplasma surface ceramic deposition technology, is that a kind of high-voltage plasma assists
Anodic oxidation new process is enhanced using arc discharge and is activated and occur on anode on the basis of common anode oxidation
Reaction makes the metal of matrix surface and electrolyte interact, thus in the valve metals such as aluminium, magnesium, titanium and its alloy material surface
Stable reinforcing ceramic film is formed in situ under the action of the factors such as high temperature, electric field in micro-arc discharge.Aluminum alloy differential arc oxidation
The main component of film is Al2O3, have the characteristics that hardness is high, wearability is good, the growth in situ mode of film layer makes matrix and film layer
Between metallurgical bonding it is secured, not easily to fall off, overall performance is good.
In the forming process of micro-arc oxidation of aluminum alloy surface film layer, micro- plasma arc constantly generates, extinguishes, micro-arc discharge
Channel part can left behind；The TRANSIENT HIGH TEMPERATURE that micro- plasma arc generates reaches 8000K, and molten oxide swashs electrolyte
Cold lower quick solidification, generates larger stress, forms micro-crack in film layer, so that there are certain holes for differential arc oxidation film layer
Rate.Micro-arc oxidation of aluminum alloy surface film layer has unconspicuous lamination, and the oxidation film close to matrix is closely knit, far from matrix
Part is loose porous, and film surface is dispersed with the irregular crateriform hole of shape size, these holes are mainly due to hitting
Wear caused by electric discharge, inner molten oxide and gas escapes outward, have plenty of the blind hole in film layer, have plenty of connection matrix with
The through-hole of external environment presents in film layer and is bent staggered distributed in three dimensions.In practical applications, these holes are corrosive medium
It penetrates into and provides channel inside micro-arc oxidation films, corrosive medium can reach matrix along these defects, lead to matrix corrosion, oxygen
Change film cracking to fall off, weakens protective effect of the film layer for matrix.In order to further enhance the hardness, anti-corrosion, resistance to of aluminium alloy
Mill and high temperature oxidation resistance also need on the basis of micro-arc oxidation process obtains ceramic of compact film layer to differential arc oxidation film layer
Sealing pores are carried out, confining surface hole improves film layer to the barrier effect of surrounding medium, prevents pitting corrosion bring negative
It influences.
Summary of the invention
The object of the present invention is to provide a kind of aluminium alloy section surface differential arc oxidation method of modifying, greatly improve aluminium alloy
Wearability, corrosion resisting property and the electrical insulation capability of Surface of profile.
A second object of the present invention is to provide a kind of above-mentioned aluminium alloy section surface differential arc oxidation method of modifying to prepare institute
The modified aluminium alloy extrusions in the surface obtained.
To achieve the goals above, the technical scheme adopted by the invention is as follows:
A kind of aluminium alloy section surface differential arc oxidation method of modifying, comprising the following steps:
A) pre-treatment: aluminium alloy extrusions completes pre-treatment through purging ash disposal, cleaning oil removing, washing, drying；
B) micro-arc oxidation treatment: aluminium alloy extrusions being placed in electrolyte and carries out differential arc oxidation, the electrolyte include with
The component of lower concentration: Na2SiO3 8-10g/L、Na2B4O72-2.4g/L, KOH 1.6-2.0g/L, glycerine 1.8-2.0ml/L,
Na2MoO42-2.4g/L,EDTA-2Na 0.5-0.8g/L；
Electrical parameter are as follows: forward current density 8-10A/dm2, negative current density is 4A/dm2, pulse frequency 400-
450Hz, duty ratio 20%-25%, in signal period it is positive/negative to the ratio between umber of pulse be 1；
It is taken out after the completion of differential arc oxidation；
C) it post-processes: to surface after the aluminium alloy extrusions of micro-arc oxidation treatment is cleaned, dried, using gathering inclined fluorine
Vinyl carries out sealing pores to micro-arc oxidation films layer surface.
In step b), the time of the differential arc oxidation is 30-90min.
It include such as using the method that polyvinylidene fluoride resin carries out sealing pores to micro-arc oxidation films layer surface in step c)
Lower step:
1) polyvinylidene fluoride resin is taken to be dissolved in n,N-Dimethylformamide, Kynoar concentration is made in filtering, deaeration
For the hole sealing solution of 6-8g/L；
2) aluminum alloy materials by surface Jing Guo micro-arc oxidation treatment are placed in pressure vessel, after pressure vessel is vacuumized
Injection step 1) gained hole sealing solution to material surface differential arc oxidation film layer all flood, after vacuum impregnation 10-15s, release
Vacuum takes out to obtain moist wood of the surface with infiltration wet film after keeping 10-15min to normal pressure；
3) moist wood obtained by step 2) is placed in sintering furnace, is to slowly warm up to 60 DEG C -70 DEG C and keeps the temperature soak moist wood surface
N,N-Dimethylformamide volatilization in excreting dampness film obtains the bole that surface has Kynoar photopolymer layer completely；
4) bole obtained by step 3) is rapidly heated melts Kynoar photopolymer layer to 190 DEG C -195 DEG C, then fastly
Speed is cooled to 150 DEG C -155 DEG C and carries out heat preservation crystallization, is finally slowly cooled to room temperature, i.e. completion micro-arc oxidation of aluminum alloy surface film
The Kynoar sealing pores of layer.
In step 2), aluminum alloy materials of the surface Jing Guo micro-arc oxidation treatment before sealing pores through over cleaning,
It is dry.It is described cleaning refer to rinsed with dehydrated alcohol after wash again.
In step 2), the heating rate slowly to heat up is 5 DEG C -8 DEG C/min.
In step 3), the sintering furnace be vacuum sintering furnace, heating and insulating process in the N volatilized, N- dimethyl
Formamide is recycled, and is recycled.
In step 4), the heating rate being rapidly heated is 40 DEG C -45 DEG C/min；The rate of temperature fall of the fast cooling
For 25 DEG C -30 DEG C/min.
In step 4), the time for keeping the temperature crystallization is 4-5min.
In step 4), described be slowly cooled to room temperature refers to and cools to room temperature with the furnace, or after being taken out in furnace it is naturally cold
But to room temperature.
A kind of above-mentioned modified aluminium alloy extrusions in aluminium alloy section surface differential arc oxidation method of modifying preparation gained surface.
Aluminium alloy section surface micro-arc oxidation films method of modifying of the invention, electrolyte used in differential arc oxidation include with the following group
Point: Na2SiO3、Na2B4O7, KOH, glycerine, Na2MoO4,EDTA-2Na；Wherein, Na2SiO3It is basic component with KOH.
Na2B4O7As main film for additive, the binding force and oxidation film layer of differential arc oxidation film layer and alloy matrix aluminum are improved
Crystallinity to improve film hardness, and makes the even pore distribution in differential arc oxidation film layer.Na2MoO4As performance improvement
Agent is added into electrolyte, is participated in oxidation reaction and is eventually entered into oxidation film layer, improves the rate of film build of differential arc oxidation film layer；Together
When, Na2MoO4There is shrinkage cavity effect to differential arc oxidation film layer, reduce the size of film layer Hole, to reduce porosity, improve
Hardness, corrosion resistance and the wearability of film layer.On the one hand glycerine improves the dispersibility of each component as auxiliary additive, so that
Electrolyte property is stablized, long service life；On the other hand it can inhibit the point discharge in micro-arc oxidation process, prevent film layer
Local macropore or defect.For EDTA-2Na as complexing agent, the metal ion for being complexed in electrolyte (comes from water distribution, aluminium alloy
Matrix etc.), the stability of electrolyte is improved, is prolonged its service life.
Aluminium alloy section surface micro-arc oxidation films method of modifying of the invention is rationally set on the basis of above-mentioned electrolyte
The electrical parameter of differential arc oxidation is set, so that forward current density is 8-10A/dm2, negative current density is 4A/dm2, pulse frequency is
400-450Hz, duty ratio 20%-25%, positive/negative in signal period to the ratio between umber of pulse is 1, is improved in differential arc oxidation film layer
Crystalline state α-Al2O3Content reduces mullite phase, to improve the accounting of compacted zone in differential arc oxidation film layer, reduces film layer hole
Gap rate improves the performances such as its hardness, corrosion resistance and electrical insulating property.
Further, aluminium alloy section surface differential arc oxidation method of modifying of the invention is with poly- when post-processing sealing of hole
Pvdf resin is main sealing material, and polyvinylidene fluoride resin is white crystalline polymer, and high mechanical strength, itself has
There are excellent corrosion resistance, heat-resisting quantity, oxidative resistance and wearability, dielectric strength is high, good insulating.Sealing of hole side of the invention
Polyvinylidene fluoride resin is first dissolved in n,N-Dimethylformamide by method, is filtered deaeration and pure hole sealing solution is made；Using
Vacuum impregnation technique, injection hole sealing solution is flooded to sealing of hole film layer under vacuum condition, is released vacuum to normal pressure, is made using pressure difference
With by the hole and micro-crack of hole sealing solution indentation micro-arc oxidation films layer surface, pass through subsequent drying and volatilizing solvent and fused junction
Brilliant process, so that Kynoar is closely linked with differential arc oxidation film layer, confining surface hole and micro-crack form table
The compound protective film of face densification.
Aluminium alloy section surface differential arc oxidation method of modifying of the invention will be from pressure vessel when post-processing sealing of hole
The surface lifted out is placed in sintering furnace with the moist wood of infiltration wet film, is to slowly warm up to 60 DEG C -70 DEG C and keeps the temperature make moist wood table
Face infiltrates the n,N-Dimethylformamide volatilization in wet film completely, and during wet film is dry, solvent volatilizees, fluororesin is formed
Dry film often because it is dry and cracked, be contracted in surface and form hole or crack, influence sealing of hole effect.Based on this, the present invention is by surface
Bole with Kynoar photopolymer layer, which is rapidly heated, melts Kynoar photopolymer layer to 190 DEG C -195 DEG C, molten state
Kynoar refills hole or the crack of dry and cracked formation, makes the continuous and complete of superficial film；Then fast cooling is extremely
150 DEG C -155 DEG C carry out heat preservation crystallization, and the crystallite dimension of formation is small and shape size is uniform, so that film surface densification and light
Sliding, coefficient of friction is small；It is finally slowly cooled to room temperature, avoids the stress influence in cooling procedure.The method for sealing is finally in aluminium
Alloy micro-arc oxidation films layer surface forms the smooth Kynoar film layer of one layer of densification, gives full play to polyvinylidene fluoride resin
Advantage and characteristic, so that the modified film layer of aluminum alloy surface has excellent mechanical strength, corrosion resistance, wearability and electrical isolation
Property, greatly it has been modified the comprehensive performance of aluminium alloy extrusions.
Through detecting, the modified aluminium alloy extrusions in present invention gained surface, the microhardness of surface recombination film layer reaches 1630-
1665HV, coefficient of friction are reduced to 0.29-0.33, and 5% salt mist experiment reaches 2500h or more, and breakdown voltage reaches 1495-
1525V, wearability, corrosion resistance and insulation performance are greatly improved.The experimental results showed that present invention gained surface modified aluminium
Alloy profile carries out sealing pores, sealing of hole effect with polyvinylidene fluoride resin after aluminium alloy section surface micro-arc oxidation treatment
Fruit is good and surface compact is smooth, has excellent wearability, corrosion resistance and electrical insulation capability, greatly improves aluminium alloy extrusions
Comprehensive performance, expand its application.
Specific embodiment
The present invention is described further With reference to embodiment.
In specific embodiment, aluminium alloy extrusions used is 6061 aluminium alloy extrusions.Polyvinylidene fluoride resin used
It (PVDF) is Solef1010, molecular weight 45000.
In specific embodiment, the specific method for carrying out pre-treatment to aluminium alloy extrusions includes:
A) aluminium alloy section surface is purged using compressed air, removes dust；The purging pressure is 0.2MPa,
Purging air flow velocity is 6m/s；
B) under ultrasound condition, aluminium alloy extrusions is immersed in 5min in 40 DEG C of cleaning agent, is degreased；
The frequency of the ultrasound is 28kHz, power density 0.5w/cm2；
Cleaning agent used is grouped as by the group of following concentration: sodium citrate 1.5g/L, sodium metasilicate 2.8g/L, Boratex
0.5g/L, dipropylene glycol 3.0g/L, EDTA-2Na 1.0g/L, fatty alcohol polyoxyethylene ether 0.7g/L, nonylphenol polyoxyethylene ether
0.7g/L, trihydroxy ethylamine oleate soap 0.3g/L, dodecyldimethylamine oxide 0.8g/L, surplus are water；
Wherein, sodium citrate used is Sodium Citrate, usp, Dihydrate Powder, and formula ratio disregards the crystallization water.Aliphatic alcohol polyethenoxy used
The carbon atom number of ether is 12；
C) it takes out flushing after impregnating 20s using 55 DEG C of water, then is dried under the conditions of 75 DEG C, i.e. completion pre-treatment.
In above-mentioned pretreatment process, cleaning agent used is prepared by following methods:
1) it takes the dipropylene glycol of formula ratio to mix with the water for accounting for total amount 1/3, obtains mixed solvent；
2) mixed solvent obtained by step 1) is heated to 50 DEG C, under heat-retaining condition, by the aliphatic alcohol polyethenoxy of formula ratio
In the mixed solvent is added in ether, nonylphenol polyoxyethylene ether, trihydroxy ethylamine oleate soap and dodecyldimethylamine oxide, and dispersion is equal
It is even, obtain mixture A；
3) it takes the sodium citrate of formula ratio and EDTA-2Na to be added in remaining water after dissolution, adds the inclined silicon of formula ratio
Sour sodium and Boratex, stirring and dissolving obtain mixture B；
4) mixture A obtained by step 2) is mixed with mixture B obtained by step 3), ultrasound makes it be uniformly dispersed to get institute
State cleaning agent.Through detecting, the pH value of gained cleaning agent is 9.5.
In specific embodiment, the vacuum refers to that absolute pressure is no more than 80mm mercury column.
Embodiment 1
The aluminium alloy section surface differential arc oxidation method of modifying of the present embodiment, comprising the following steps:
A) pre-treatment: purging ash disposal is carried out to aluminium alloy extrusions according to above-mentioned pre-treating method, cleaning oil removing, washing, is done
It is dry, complete pre-treatment；
B) micro-arc oxidation treatment: aluminium alloy extrusions being placed in electrolyte and carries out differential arc oxidation, the electrolyte include with
The component of lower concentration: Na2SiO3 8g/L、Na2B4O72.0g/L, KOH 2.0g/L, glycerine 2.0ml/L, Na2MoO4 2。0g/
L,EDTA-2Na 0.8g/L；Surplus is water；
Electrical parameter are as follows: forward current density 10A/dm2, negative current density is 4A/dm2, pulse frequency 400Hz accounts for
Sky than being 25%, in signal period it is positive/negative to the ratio between umber of pulse be 1；Oxidization time 60min；Temperature control in micro-arc oxidation process
System is at 50 DEG C or less:
It is taken out after the completion of differential arc oxidation；
C) it post-processes: to surface after the aluminium alloy extrusions of micro-arc oxidation treatment is cleaned, dried, using gathering inclined fluorine
Vinyl carries out sealing pores to micro-arc oxidation films layer surface.The cleaning is washed again after being rinsed with dehydrated alcohol, removal
Entrained electrolyte.
The method for sealing of sealing pores, including following step are carried out to micro-arc oxidation films layer surface using polyvinylidene fluoride resin
It is rapid:
1) polyvinylidene fluoride resin is taken to be dissolved in n,N-Dimethylformamide, Kynoar concentration is made in filtering, deaeration
For the hole sealing solution of 6g/L；
2) aluminum alloy materials by surface Jing Guo micro-arc oxidation treatment are placed in pressure vessel and seal, and pressure vessel is taken out
Injection step 1 after vacuum) gained hole sealing solution to material surface differential arc oxidation film layer all flood, after vacuum impregnation 15s, solution
Except vacuum to normal pressure, moist wood of the surface with infiltration wet film is taken out to obtain after keeping 10min；
3) moist wood obtained by step 2) is placed in vacuum sintering furnace, is to slowly warm up to 60 DEG C with the rate of 5 DEG C/min, heat preservation
N,N-Dimethylformamide volatilization into moist wood surface infiltration wet film obtains surface with Kynoar photopolymer layer completely
Bole；In heating and insulating process, the n,N-Dimethylformamide volatilized is recycled, is recycled；
4) bole obtained by step 3) is rapidly heated with the rate of 40 DEG C/min keeps Kynoar photopolymer layer molten to 190 DEG C
Melt, heat preservation is then carried out to 150 DEG C with the rate fast cooling of 25 DEG C/min and crystallizes 5min, it is finally naturally cold after being taken out in furnace
But to room temperature, that is, the Kynoar sealing pores of micro-arc oxidation of aluminum alloy surface film layer are completed.
Embodiment 2
The aluminium alloy section surface differential arc oxidation method of modifying of the present embodiment, comprising the following steps:
A) pre-treatment: purging ash disposal is carried out to aluminium alloy extrusions according to above-mentioned pre-treating method, cleaning oil removing, washing, is done
It is dry, complete pre-treatment；
B) micro-arc oxidation treatment: aluminium alloy extrusions being placed in electrolyte and carries out differential arc oxidation, the electrolyte include with
The component of lower concentration: Na2SiO3 9g/L、Na2B4O72.2g/L, KOH 1.8g/L, glycerine 1.9ml/L, Na2MoO4 2.2g/
L,EDTA-2Na 0.6g/L；Surplus is water；
Electrical parameter are as follows: forward current density 10A/dm2, negative current density is 4A/dm2, pulse frequency 400Hz accounts for
Sky than being 25%, in signal period it is positive/negative to the ratio between umber of pulse be 1；Oxidization time 60min；Temperature control in micro-arc oxidation process
System is at 50 DEG C or less:
It is taken out after the completion of differential arc oxidation；
C) it post-processes: to surface after the aluminium alloy extrusions of micro-arc oxidation treatment is cleaned, dried, using gathering inclined fluorine
Vinyl carries out sealing pores to micro-arc oxidation films layer surface.The cleaning is washed again after being rinsed with dehydrated alcohol, removal
Entrained electrolyte.
The method for sealing of sealing pores, including following step are carried out to micro-arc oxidation films layer surface using polyvinylidene fluoride resin
It is rapid:
1) polyvinylidene fluoride resin is taken to be dissolved in n,N-Dimethylformamide, Kynoar concentration is made in filtering, deaeration
For the hole sealing solution of 7g/L；
2) aluminum alloy materials by surface Jing Guo micro-arc oxidation treatment are placed in pressure vessel and seal, and pressure vessel is taken out
Injection step 1 after vacuum) gained hole sealing solution to material surface differential arc oxidation film layer all flood, after vacuum impregnation 12s, solution
Except vacuum to normal pressure, moist wood of the surface with infiltration wet film is taken out to obtain after keeping 15min；
3) moist wood obtained by step 2) is placed in vacuum sintering furnace, is to slowly warm up to 65 DEG C with the rate of 7 DEG C/min, heat preservation
N,N-Dimethylformamide volatilization into moist wood surface infiltration wet film obtains surface with Kynoar photopolymer layer completely
Bole；In heating and insulating process, the n,N-Dimethylformamide volatilized is recycled, is recycled；
4) bole obtained by step 3) is rapidly heated with the rate of 45 DEG C/min keeps Kynoar photopolymer layer molten to 195 DEG C
Melt, heat preservation is then carried out to 155 DEG C with the rate fast cooling of 30 DEG C/min and crystallizes 4min, it is finally naturally cold after being taken out in furnace
But to room temperature, that is, the Kynoar sealing pores of micro-arc oxidation of aluminum alloy surface film layer are completed.
Embodiment 3
The aluminium alloy section surface differential arc oxidation method of modifying of the present embodiment, comprising the following steps:
A) pre-treatment: purging ash disposal is carried out to aluminium alloy extrusions according to above-mentioned pre-treating method, cleaning oil removing, washing, is done
It is dry, complete pre-treatment；
B) micro-arc oxidation treatment: aluminium alloy extrusions being placed in electrolyte and carries out differential arc oxidation, the electrolyte include with
The component of lower concentration: Na2SiO3 10g/L、Na2B4O72.4g/L, KOH 1.6g/L, glycerine 1.8ml/L, Na2MoO4
2.4g/L,EDTA-2Na 0.5g/L；Surplus is water；
Electrical parameter are as follows: forward current density 10A/dm2, negative current density is 4A/dm2, pulse frequency 400Hz accounts for
Sky than being 25%, in signal period it is positive/negative to the ratio between umber of pulse be 1；Oxidization time 60min；Temperature control in micro-arc oxidation process
System is at 50 DEG C or less:
It is taken out after the completion of differential arc oxidation；
C) it post-processes: to surface after the aluminium alloy extrusions of micro-arc oxidation treatment is cleaned, dried, using gathering inclined fluorine
Vinyl carries out sealing pores to micro-arc oxidation films layer surface.The cleaning is washed again after being rinsed with dehydrated alcohol, removal
Entrained electrolyte.
The method for sealing of sealing pores, including following step are carried out to micro-arc oxidation films layer surface using polyvinylidene fluoride resin
It is rapid:
1) polyvinylidene fluoride resin is taken to be dissolved in n,N-Dimethylformamide, Kynoar concentration is made in filtering, deaeration
For the hole sealing solution of 8g/L；
2) aluminum alloy materials by surface Jing Guo micro-arc oxidation treatment are placed in pressure vessel and seal, and pressure vessel is taken out
Injection step 1 after vacuum) gained hole sealing solution to material surface differential arc oxidation film layer all flood, after vacuum impregnation 10s, solution
Except vacuum to normal pressure, moist wood of the surface with infiltration wet film is taken out to obtain after keeping 10min；
3) moist wood obtained by step 2) is placed in vacuum sintering furnace, is to slowly warm up to 70 DEG C with the rate of 8 DEG C/min, heat preservation
N,N-Dimethylformamide volatilization into moist wood surface infiltration wet film obtains surface with Kynoar photopolymer layer completely
Bole；In heating and insulating process, the n,N-Dimethylformamide volatilized is recycled, is recycled；
4) bole obtained by step 3) is rapidly heated with the rate of 45 DEG C/min keeps Kynoar photopolymer layer molten to 190 DEG C
Melt, heat preservation is then carried out to 150 DEG C with the rate fast cooling of 25 DEG C/min and crystallizes 4.5min, it is finally natural after being taken out in furnace
It is cooled to room temperature, that is, completes the Kynoar sealing pores of micro-arc oxidation of aluminum alloy surface film layer.
Experimental example 1
Superficiality of this experimental example to differential arc oxidation and method for sealing treated aluminium alloy extrusions by embodiment 1-3
It can be carried out detection.Testing result is as shown in table 1.
Wherein, film thickness is measured using coating thickness detector, and each sample random detection 10 times is averaged.Microhardness is adopted
It is measured with microhardness tester, load 100g, load time 10s, each sample random detection 10 times is averaged.Polishing machine
It is measured using friction wear testing machine, abrading-ball uses GCr15 steel ball, ball radius 3mm, fraze 5mm, frequency 5Hz, revolving speed
300rpm, load 2N, wearing- in period 20min.Corrosion resistance test carries out in salt-mist corrosion tester.Breakdown voltage is used and is hit
Potentiometry measurement is worn, sample to be tested is connected to voltage resistant instrument the two poles of the earth by dielectric properties and insulation performance based on film layer, is risen according to certain
It presses rate to increase voltage, is electrically shocked voltage when wearing in the instantaneous measurement film layer that electric current passes through film layer at the first time.
The mapping surface properties result of 1 aluminium alloy extrusions of table
As it can be seen from table 1 the aluminium alloy section surface differential arc oxidation method of modifying of embodiment 1-3, by the micro- of 60min
Arc oxidation processes, aluminium alloy section surface deposit differential arc oxidation film layer with a thickness of 38-40 μm, the deposition speed of differential arc oxidation film layer
Rate is 0.64-0.67 μm/min, and deposition velocity is fast, obtains micro-arc oxidation films thickness and densification.It is found through detection, micro-arc oxidation films
The microhardness of layer (before sealing of hole) is between 1540-1565HV, and between 0.71-0.78,5% salt mist experiment exists coefficient of friction
1000h or more, breakdown voltage is between 730-750V, although having preferable comprehensive performance, due to differential arc oxidation film layer
Hole existing for surface, wearability, corrosion resistance and insulation performance are not good enough.By polyvinylidene fluoride resin sealing of hole of the invention
After processing, the microhardness of composite film reaches 1630-1665HV, relative to improving about 100HV before sealing of hole；Coefficient of friction drop
Down to 0.29-0.33, about 60% is reduced；5% salt mist experiment reaches 2500h or more, is 2.5 times before sealing of hole；Breakdown voltage reaches
It is the 2 times or more before sealing of hole to 1495-1525V, wearability, corrosion resistance and insulation performance are greatly improved.Experimental result
Show aluminium alloy section surface differential arc oxidation method of modifying of the invention, after aluminium alloy section surface micro-arc oxidation treatment,
Sealing pores are carried out with polyvinylidene fluoride resin, sealing of hole effect is good and surface compact is smooth, greatly improves differential arc oxidation film layer
Wearability, corrosion resistance and insulation performance, improve the comprehensive performance of aluminium alloy extrusions, expand its application.
Claims (8)
1. a kind of aluminium alloy section surface differential arc oxidation method of modifying, it is characterised in that: the following steps are included:
A) pre-treatment: aluminium alloy extrusions completes pre-treatment through purging ash disposal, cleaning oil removing, washing, drying；
B) micro-arc oxidation treatment: aluminium alloy extrusions being placed in electrolyte and carries out differential arc oxidation, and the electrolyte includes following dense
The component of degree: Na2SiO3 8-10g/L、Na2B4O72-2.4g/L, KOH 1.6-2.0g/L, glycerine 1.8-2.0ml/L,
Na2MoO42-2.4g/L,EDTA-2Na 0.5-0.8g/L；
Electrical parameter are as follows: forward current density 8-10A/dm2, negative current density is 4A/dm2, pulse frequency 400-450Hz,
Duty ratio is 20%-25%, in signal period it is positive/negative to the ratio between umber of pulse be 1；
It is taken out after the completion of differential arc oxidation；
C) it post-processes: to surface after the aluminium alloy extrusions of micro-arc oxidation treatment is cleaned, dried, using Kynoar
Resin carries out sealing pores to micro-arc oxidation films layer surface.
2. aluminium alloy section surface differential arc oxidation method of modifying according to claim 1, it is characterised in that: in step b),
The time of the differential arc oxidation is 60-90min.
3. aluminium alloy section surface differential arc oxidation method of modifying according to claim 1, it is characterised in that: in step c),
Included the following steps: using the method that polyvinylidene fluoride resin carries out sealing pores to micro-arc oxidation films layer surface
1) polyvinylidene fluoride resin is taken to be dissolved in n,N-Dimethylformamide, filtering, deaeration, it is 6- that Kynoar concentration, which is made,
The hole sealing solution of 8g/L；
2) aluminum alloy materials by surface Jing Guo micro-arc oxidation treatment are placed in pressure vessel, are injected after pressure vessel is vacuumized
The differential arc oxidation film layer of hole sealing solution to material surface obtained by step 1) all floods, and after vacuum impregnation 10-15s, releases vacuum
To normal pressure, moist wood of the surface with infiltration wet film is taken out to obtain after keeping 10-15min；
3) moist wood obtained by step 2) is placed in sintering furnace, is to slowly warm up to 60 DEG C -70 DEG C and keeps the temperature keep the infiltration of moist wood surface wet
N,N-Dimethylformamide volatilization in film obtains the bole that surface has Kynoar photopolymer layer completely；
4) bole obtained by step 3) is rapidly heated melts Kynoar photopolymer layer to 190 DEG C -195 DEG C, then fast prompt drop
Temperature carries out heat preservation crystallization to 150 DEG C -155 DEG C, is finally slowly cooled to room temperature, i.e. completion micro-arc oxidation of aluminum alloy surface film layer
Kynoar sealing pores.
4. aluminium alloy section surface differential arc oxidation method of modifying according to claim 3, it is characterised in that: in step 2),
The heating rate slowly to heat up is 5 DEG C -8 DEG C/min.
5. aluminium alloy section surface differential arc oxidation method of modifying according to claim 3, it is characterised in that: in step 3),
The sintering furnace is vacuum sintering furnace, recycles, follows to the n,N-Dimethylformamide volatilized in heating and insulating process
Ring utilizes.
6. aluminium alloy section surface differential arc oxidation method of modifying according to claim 3, it is characterised in that: in step 4),
The heating rate being rapidly heated is 40 DEG C -45 DEG C/min；The rate of temperature fall of the fast cooling is 25 DEG C -30 DEG C/min.
7. aluminium alloy section surface differential arc oxidation method of modifying according to claim 3, it is characterised in that: in step 4),
The time of heat preservation crystallization is 4-5min.
8. a kind of as aluminium alloy section surface differential arc oxidation method of modifying of any of claims 1-7 prepares gained table
Face is modified aluminium alloy extrusions.
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| CN109811385A (en) * | 2019-02-27 | 2019-05-28 | 长安大学 | Aluminium and aluminum alloy surface polyvinylidene fluoride/aluminum oxide composite membrane and preparation method thereof |
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| CN113215636A (en) * | 2021-04-16 | 2021-08-06 | 首钢集团有限公司 | Surface treatment method for pickled plate |
| CN114277418A (en) * | 2021-11-29 | 2022-04-05 | 广东烨兴科技有限公司 | Preparation method of pore-free ceramic membrane covered wire |
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