CN103628114A - Surface treatment method of magnesium aluminum alloy - Google Patents
Surface treatment method of magnesium aluminum alloy Download PDFInfo
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- CN103628114A CN103628114A CN201310678013.XA CN201310678013A CN103628114A CN 103628114 A CN103628114 A CN 103628114A CN 201310678013 A CN201310678013 A CN 201310678013A CN 103628114 A CN103628114 A CN 103628114A
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Abstract
The invention relates to surface treatment of alloy materials and in particular to a surface treatment method of magnesium aluminum alloy. The experimental process comprises the following steps: polishing, degreasing, performing alkaline corrosion, performing chemical polishing, performing anodic oxidation, performing electrolytic coloring, and performing hole sealing. According to the surface treatment method, the design is reasonable, and a thick and dense oxide film layer is formed on the surface of the magnesium aluminum alloy by an anodic oxidation method, so that the corrosion resistance of the magnesium aluminum alloy is remarkably changed and the hardness, the wear resistance and the decorative performance of the magnesium aluminum alloy are improved; however, the anodic oxide film of the magnesium aluminum alloy is very high in porosity rate and adsorption capacity, can be easily polluted and corroded by a corrosive medium, and has to be subjected to hole sealing so as to improve the corrosion resistance and the pollution resistance and fix pigment bodies.
Description
Technical field
The present invention relates to the surface treatment of alloy material, be specially a kind of surface treatment method of magnalium.
Background technology
Magnesium-aluminium alloy material is due to its high strength/weight ratio, and easy-formation processing and excellent physics, chemical property, become the metallic substance more than use aluminium alloy in current industry.Yet magnesium-aluminium alloy material hardness is low, wear no resistance, normal that abrasion occurs is damaged, and therefore, magnalium often needs through corresponding surface treatment, to meet it to the adaptability of environment and security, to reduce abrasion before use, extends its work-ing life.
Because the surface of magnalium easily generates layer oxide film, it is very stable in atmosphere, but the wear resistance of the oxide film of natural formation and corrosion stability are strong not enough, so will carry out by artificial means anodic oxidation treatment.
The anodic oxidation treatment of magnalium is to make magnalium vessel processed or surface of the work generate the aluminum oxide film of the porous that one deck is wear-resisting according to the principle of electrolysis, to improve hardness, wear resistance, corrosion stability and the insulativity of surface of magnesium aluminium alloy, and can be at aluminum component padding and paint base.
During magnalium anodic oxidation, the growth package of the oxide film on surface contains two processes: the electrochemistry of oxide film generates and chemical dissolution process.While only having the growth rate of oxide film to be greater than dissolution rate, oxide film could be grown up, be thickeied.Common anode oxidation mainly contains sulphuric acid anodizing, chromic acid anodizing, oxalic acid anodizing and phosphoric acid anodizing etc.
Summary of the invention
The object of the present invention is to provide a kind of new surface of magnesium aluminium alloy treatment process.
The present invention adopts following technical scheme to realize:
A surface treatment method for magnalium, comprises the steps:
(1), adopt mechanical grinding that the oxide film of magnalium sheet surface self-assembling formation is removed;
(2), the magnalium sheet material after polishing is put into temperature is the degreasing fluid 3～5min of 70～75 ℃, described degreasing fluid is by Na
2cO
3solution, Na
3pO
4solution and Na
2siO
4solution be take volume ratio and is formed as 1:1:1 configuration, described Na
2cO
3the concentration of solution is 40g/ L, described Na
3pO
4the concentration of solution is 40g/ L, described Na
2siO
4the concentration of solution is 20g/ L;
(3), the magnalium sheet material after degreasing is put into temperature is the alkaline etching liquid 3～5min of 50～70 ℃, described alkaline etching liquid is that concentration is the NaOH solution of 20g/ L;
(4), the magnalium sheet material after alkaline etching is put into temperature is the polishing fluid 3～5min of 90～110 ℃, the H that described polishing fluid is 1.70 by relative density
3pO
4solution and relative density are 1.84 H
2sO
4solution be take volume ratio and is formed as 1:1 configuration;
(5), the magnalium sheet material after polishing is carried out to sulphuric acid anodizing, anodised condition is: the concentration of sulfuric acid is 1.5g/l, and temperature is 15～25 ℃, and voltage is 10～20V, time 20～30min;
(6), the magnalium sheet material after anodic oxidation is carried out to electrolytic coloring;
(7), sealing of hole: adopt burning water, keep 10～15min in the deionized water of 90～100 ℃; Or, adopt hydrolysis salts solution to seal, NiSO in described hydrolysis salts solution
47H
2the content of O is 4～5g/L, CoSO
47H
2the content of O is 0.5～0.8g/L, H
3bO
3content be 4～5g/L, NaAc3H
2the content of O is 4～6g/L, and the pH value of hydrolysis salts solution is 4～6, temperature is 80～85 ℃, and the hold-time is 15～20min.
The present invention carries out anodic oxidation by magnalium electrolysis in aqueous sulfuric acid, makes its Surface Creation oxidation film layer.Control well under the conditions such as temperature, voltage, time, concentration of electrolyte, magnalium sulphuric acid oxidation coating layer has higher adsorptive power, easily carries out sealing of hole or painted processing,
Magnalium anodizing process with sulfuric acid as major salt is simple to operate, and electrolytic solution is stable, and cost is not high yet, more improves its corrosion stability and outward appearance.The advantage of this sulphuric acid anodizing is as follows:
1, operating procedure is easy, at the temperature of 15～20 ℃, and 5-10min, easy and simple to handle;
2, very safe, can not cause environmental pollution and be harmful to operator;
3, technique medicine is cheap.
In addition, different condition is as follows on the impact of coloring effect
1, yellow
1.1, under the condition that changes of time as table 1:
Table 1
As shown in Table 1, painted time lengthening, tone is deepened.Under 15V voltage, painted 5min can obtain the golden yellow of best tone.If painted too shallow sustainable painted for some time.
1.2, under the condition of coloring liquid temperature change, when painted, with temperature, raise, specific conductivity improves.Under the condition of identical voltage, same time, same concentrations, temperature is higher, paint faster, but because temperature of reaction raises, speed of response is accelerated, and paints inhomogeneous, occurs strip or block-type tread.
1.3, under the condition that coloring liquid concentration changes as table 2:
Table 2
As shown in Table 2, in the situation that other condition is constant, coloring liquid concentration is deepened, and colouring is deepened.
1.4, under the condition that voltage changes as table 3:
Table 3
As shown in Table 2, voltage is too low, and electric current is entirely for the charging on blocking layer, there is no metal deposition, thus do not paint.10～15V is golden yellow painted voltage range, and metal deposition is many; The above painted electric current of 15V increases, and metal deposition increases, and tone increases and color burn with voltage; The excessive colouring of the above electric current of 20V is inhomogeneous, has striated to occur.
Therefore yellow in electrolysis, adopting concentration is the KMnO of 20g/l
4solution, condition is: 18～20 ℃ of temperature, voltage 15V, time 5min.
2, redness
2.1, under the condition that changes of time as table 4:
Table 4
As shown in Table 4, painted time lengthens, institute color progressively deepen.After the colouring time is surpassing 10 minutes, the red middle blackout of color of.If painted too shallow can continuation in coloring liquid painted.
2.2, under the condition of coloring liquid temperature change, under the condition of identical voltage, same time, same concentrations, temperature is higher, paint faster, but because temperature of reaction raises, speed of response is accelerated, and paints inhomogeneous, occurs strip or block-type tread.
2.3, under the condition that coloring liquid concentration changes as table 5:
Table 5
As shown in Table 5, in the situation that all conditions is constant, concentration is larger, and color is darker.
2.4, under the condition that voltage changes as table 6:
Table 6
As shown in Table 6, voltage is low, undercurrent in coloring liquid, and metal deposition is less, painted too light; Voltage is too high, and in coloring liquid, electric current is excessive, causes CuSO
4middle Cu separates out, and sticks on painted magnalium sheet, make edge have Cu and do not paint.Temperature-resistant, concentration is constant, and by time lengthening, voltage is strengthened.After voltage is strengthened, at CuSO
4in separate out Cu; By time lengthening, CuSO
4separate out more Cu, on magnalium sheet surface, all can occur Cu ion and can not enter look.
Therefore if electrolysis red coloration, adopting concentration is the CuSO of 20g/ L
4solution, condition is: 18～20 ℃ of temperature, voltage 25V, time 5min.
3, purple
3.1, under the condition that changes of time as table 7:
Table 7
3.2, under the condition that coloring liquid concentration changes as table 8:
Table 8
3.3, by H
2sO
4concentration changes, CuSO
4concentration is constant as table 9:
Table 9
As shown in Table 9, by CuSO
4, H
2sO
4concentration changes mutually, causes the change of the color of colouring.CuSO
4the many time colourings that account for are relatively red; H
2sO
4account for many time upper colour cast deep green.
3.4, under the condition that voltage changes as table 10:
Table 10
As shown in Table 10, the time of progressively strengthening at voltage, in coloring liquid, find that there is Cu and separate out, stick to the edge of aluminium flake, make the aluminium flake can not normal coloring.
Therefore if purple in electrolysis, adopting by concentration is the CuSO of 30g/ L
4with concentration be the H of 20g/ L
2sO
4the mixed solution that the volume ratio of take forms as 1:1 configuration, parameter is: 18～20 ℃ of temperature, voltage 25V, time 3min.
The roughness of magnalium sheet matrix and luminance brightness are larger on the color and luster impact of coloring film, and painted magnalium material will have higher luminance brightness, and available chemical rightenning can only obtain yellow film or inhomogeneous oxide film if surface-treated is bad.If produce the look that inhomogeneous oxide film makes, there is bar or block product.In said process, the painted time change of all colours all has a certain impact to experiment product, at voltage, concentration of electrolyte, colour temperature, all to lengthen the product that the painted time draws in immovable situation painted just darker, shortens the product that the painted time draws painted just lighter.In voltage, painted time, colour temperature, all to increase the look that the painted product drawing of concentration of painted electrolytic solution in immovable situation just darker, reduces the look that product that the concentration of painted electrolytic solution draws just lighter.
The present invention is suitable for industrial production, is applied in production in enormous quantities, can better save medicine and coloring effect is better.
The present invention is reasonable in design, adopts anodised method to form thick and fine and close oxidation film layer at surface of magnesium aluminium alloy, significantly to change the solidity to corrosion of magnalium, improves hardness, wear resistance and decorate properties.Yet magnalium anode oxide film has very high porosity and adsorptive power, easily contaminated and corrosive medium corrodes, and must carry out sealing of hole processing, to improve solidity to corrosion, contamination resistance and fixed pigment body.
China's moral standing is numerous, and Economic development is rapid, and city constantly expands, and building magnalium section bar industry must be the industry of Sustainable development.The surface treatment of building magnesium-aluminium alloy material, both can improve use properties and life-span, can improve visual appearance again, improved decoration grade, the status of first developing that therefore still can be in standing in the breach.
Embodiment
Below specific embodiments of the invention are elaborated.
embodiment 1
A surface treatment method for magnalium, comprises the steps:
(1), with sand paper, the oxide film of the surperficial self-assembling formation of magnalium sheet material (thickness is 1.5mm) is removed, and smooth;
(2), the magnalium sheet material after polishing is put into temperature is the degreasing fluid 5min of 70 ℃, described degreasing fluid is by Na
2cO
3solution, Na
3pO
4solution and Na
2siO
4solution be take volume ratio and is formed as 1:1:1 configuration, described Na
2cO
3the concentration of solution is 40g/ L, described Na
3pO
4the concentration of solution is 40g/ L, described Na
2siO
4the concentration of solution is 20g/ L;
(3), the magnalium sheet material after degreasing is put into temperature is the alkaline etching liquid 4min of 60 ℃, described alkaline etching liquid is that concentration is the NaOH solution of 20g/ L;
(4), the magnalium sheet material after alkaline etching is put into temperature is the polishing fluid 3min of 90 ℃, the H that described polishing fluid is 1.70 by relative density
3pO
4solution and relative density are 1.84 H
2sO
4solution be take volume ratio and is formed as 1:1 configuration;
(5), the magnalium sheet material after polishing is carried out to sulphuric acid anodizing, anodised condition is: the concentration of sulfuric acid is 1.5g/ L, and temperature is 20 ℃, and voltage is 10V, time 30min;
(6), the magnalium sheet material after anodic oxidation is carried out to electrolytic coloring; Yellow, adopting concentration is the KMnO of 20g/l
4solution, condition is: 18～20 ℃ of temperature, voltage 15V, time 5min;
(7), sealing of hole: adopt burning water, keep 10～15min in the deionized water of 100 ℃.
After each step, all use washed with de-ionized water magnalium sheet material.
embodiment 2
A surface treatment method for magnalium, comprises the steps:
(1), with sand paper, the oxide film of the surperficial self-assembling formation of magnalium sheet material (thickness is 1.5mm) is removed, and smooth;
(2), the magnalium sheet material after polishing is put into temperature is the degreasing fluid 4min of 75 ℃, described degreasing fluid is by Na
2cO
3solution, Na
3pO
4solution and Na
2siO
4solution be take volume ratio and is formed as 1:1:1 configuration, described Na
2cO
3the concentration of solution is 40g/ L, described Na
3pO
4the concentration of solution is 40g/ L, described Na
2siO
4the concentration of solution is 20g/ L;
(3), the magnalium sheet material after degreasing is put into temperature is the alkaline etching liquid 3min of 70 ℃, described alkaline etching liquid is that concentration is the NaOH solution of 20g/ L;
(4), the magnalium sheet material after alkaline etching is put into temperature is the polishing fluid 5min of 100 ℃, the H that described polishing fluid is 1.70 by relative density
3pO
4solution and relative density are 1.84 H
2sO
4solution be take volume ratio and is formed as 1:1 configuration;
(5), the magnalium sheet material after polishing is carried out to sulphuric acid anodizing, anodised condition is: the concentration of sulfuric acid is 1.5g/ L, and temperature is 25 ℃, and voltage is 15V, time 25min;
(6), the magnalium sheet material after anodic oxidation is carried out to electrolytic coloring; Red coloration, adopting concentration is the CuSO of 20g/l
4solution, condition is: 18～20 ℃ of temperature, voltage 25V, time 5min;
(7), sealing of hole: adopt hydrolysis salts solution to seal, NiSO in described hydrolysis salts solution
47H
2the content of O is 4g/L, CoSO
47H
2the content of O is 0.8g/L, H
3bO
3content be 4g/L, NaAc3H
2the content of O is 6g/L, and the pH value of hydrolysis salts solution is 4, temperature is 80 ℃, and the hold-time is 20min.
After each step, all use washed with de-ionized water magnalium sheet material.
embodiment 3
A surface treatment method for magnalium, comprises the steps:
(1), with sand paper, the oxide film of magnalium sheet surface self-assembling formation is removed, and smooth;
(2), the magnalium sheet material after polishing is put into temperature is the degreasing fluid 3min of 72 ℃, described degreasing fluid is by Na
2cO
3solution, Na
3pO
4solution and Na
2siO
4solution be take volume ratio and is formed as 1:1:1 configuration, described Na
2cO
3the concentration of solution is 40g/ L, described Na
3pO
4the concentration of solution is 40g/ L, described Na
2siO
4the concentration of solution is 20g/ L;
(3), the magnalium sheet material after degreasing is put into temperature is the alkaline etching liquid 5min of 50 ℃, described alkaline etching liquid is that concentration is the NaOH solution of 20g/ L;
(4), the magnalium sheet material after alkaline etching is put into temperature is the polishing fluid 4min of 110 ℃, the H that described polishing fluid is 1.70 by relative density
3pO
4solution and relative density are 1.84 H
2sO
4solution be take volume ratio and is formed as 1:1 configuration;
(5), the magnalium sheet material after polishing is carried out to sulphuric acid anodizing, anodised condition is: the concentration of sulfuric acid is 1.5g/ L, and temperature is 15 ℃, and voltage is 20V, time 20min;
(6), the magnalium sheet material after anodic oxidation is carried out to electrolytic coloring; Purple, adopting by concentration is the CuSO of 30g/ L
4with concentration be the H of 20g/ L
2sO
4the mixed solution that the volume ratio of take forms as 1:1 configuration, parameter is: 18～20 ℃ of temperature, voltage 25V, time 3min;
(7), sealing of hole: adopt hydrolysis salts solution to seal, NiSO in described hydrolysis salts solution
47H
2the content of O is 5g/L, CoSO
47H
2the content of O is 0.5g/L, H
3bO
3content be 5g/L, NaAc3H
2the content of O is 4g/L, and the pH value of hydrolysis salts solution is 6, temperature is 85 ℃, and the hold-time is 15min.
After each step, all use washed with de-ionized water magnalium sheet material.
Most common failure and being analyzed as follows in embodiment:
(1), tubercular corrosion magnalium sulphuric acid anodizing rear oxidation film is intensely dark, sometimes produces tubercular corrosion, when serious, black tubercular corrosion is remarkable, causes magnalium part to be scrapped, and causes greater loss.The generation of this class phenomenon generally has the reason of two aspects: the one, and part is in production and circular flow, the antirust work of inter process is not carried out, and part is subject to the pollution of active media, and galvanic corrosion occurs on surface, there is local aperture or " pit " in surface, obvious especially after caustic corrosion.Another reason accidentally causes, in magnalium anode oxidation process, electricity is given in power-off midway again, during power failure, part overstays at rinse bath, cleaning sink acidity is too high, and water quality is unclean, or more containing suspended substance, silt particle etc., tend to make magnalium part generation galvanic corrosion to make oxide film intensely dark, or point-like corrosive black spot etc. occurs.If at this moment add tap water in electrolytic solution, because of water Cl content overproof after chlorinated lime is processed, thereby cause part tubercular corrosion.
(2), be faint in color or the dimness of burnt hair magnalium sulphuric acid anodizing rear oxidation film local surfaces color is even turned black, have large stretch of blackspot or Dark grey spot.This phenomenon generally appears in large thicker magnalium part.The reason producing is that material Local cooling when quenching slow (as speed of cooling deficiency, local water temperature over-high) or transfer time are long, in local organization, main strengthening phase is separated out in a large number, impel alloy matrix aluminum alloying element solid solution strengthening effect to reduce, simultaneously because second-phase is separated out from a large amount of complete non-coherences in crystal grain, this will make material corrosion resisting property reduce, anodizing corrosion speed strengthens, therefore this part different zones when anodizing presents different extent of corrosions because surperficial anodic oxidation speed is different, finally because reflective function presents different surface colors.
(3), blackspot or striped part after sulfur acid anodizing is processed, there is local non-oxidation rete, present macroscopic blackspot or striped.This situation generally each several part tissue odds improper caused with inhomogeneous, the microstructure segregation of surface metal phase, micro-impurity segregation or thermal treatment etc. is relevant, will cause selective oxidation or selective dissolution.As the segregation of material local silicon content, often cause local No oxided film or be black patches striped or local selective dissolution produces hole etc.Certainly, if the metallic impurity ion content such as suspended impurity, dust, copper iron is too high in sulfuric acid electrolyte, also can causes this class phenomenon, thereby affect the corrosion resisting property of oxide film.
(4), the anodized magnesium aluminum alloy part processed of the imperfect same groove of rete, No oxided film or rete are frivolous or imperfect, or have scaling loss corrode phenomenon at fixture and part contact position.This is because the insulativity of alumite is better.Aluminum alloy part must fill securely and hang on universal or special fixture before anodic oxidation treatment, to guarantee satisfactory electrical conductivity.Current conducting rod should be selected copper or Cu alloy material and will guarantee enough contacts area.
(5), fall film, oxide film be loose efflorescence even with hand once touching, after particularly filling and sealing, piece surface occurs that bisque is that corrosion stability is inferior.This class phenomenon mostly occurs does not have the sulphuric acid anodizing groove of refrigerating unit in summer, after processing 1～2 groove part, loose powder phenomenon-tion just there will be.Because magnalium anodic oxidation membrane resistance is very large, in anode oxidation process process, can produce a large amount of joule heatings, bath voltage more high yield heat-dissipating amount is larger, thereby causes electrolyte temperature constantly to rise.So in anode oxidation process, must adopt and stir or refrigerating unit, electrolyte temperature is controlled between 10～25 ℃, to guarantee coating mass.If liquid temperature surpasses 30 ℃, the oxide film efflorescence of can loosening, has " burning " phenomenon when serious.In addition, when electrolyte temperature is constant, anodic current density also must be limited, because anodic current density is too high, temperature rise is violent, also there will be same problem.
Magnalium sulphuric acid anodizing coating mass quality, the quality of barrier propterty against corrosion depends primarily on the composition of magnalium, thicknesses of layers and anodic oxidation treatment processing condition, as filling closing process after temperature, current density, use water quality and anodic oxidation etc.Reduce or avoid anodic oxidation fault to improve the quality of products and will set about from fine, adopting an effective measure.
Claims (4)
1. a surface treatment method for magnalium, is characterized in that: comprise the steps:
(1), adopt mechanical grinding that the oxide film of magnalium sheet surface self-assembling formation is removed;
(2), the magnalium sheet material after polishing is put into temperature is the degreasing fluid 3～5min of 70～75 ℃, described degreasing fluid is by Na
2cO
3solution, Na
3pO
4solution and Na
2siO
4solution be take volume ratio and is formed as 1:1:1 configuration, described Na
2cO
3the concentration of solution is 40g/L, described Na
3pO
4the concentration of solution is 40g/ L, described Na
2siO
4the concentration of solution is 20g/ L;
(3), the magnalium sheet material after degreasing is put into temperature is the alkaline etching liquid 3～5min of 50～70 ℃, described alkaline etching liquid is that concentration is the NaOH solution of 20g/L;
(4), the magnalium sheet material after alkaline etching is put into temperature is the polishing fluid 3～5min of 90～110 ℃, the H that described polishing fluid is 1.70 by relative density
3pO
4solution and relative density are 1.84 H
2sO
4solution be take volume ratio and is formed as 1:1 configuration;
(5), the magnalium sheet material after polishing is carried out to sulphuric acid anodizing, anodised condition is: the concentration of sulfuric acid is 1.5g/ L, and temperature is 15～25 ℃, and voltage is 10～20V, time 20～30min;
(6), the magnalium sheet material after anodic oxidation is carried out to electrolytic coloring;
(7), sealing of hole: adopt burning water, keep 10～15min in the deionized water of 90～100 ℃; Or, adopt hydrolysis salts solution to seal, NiSO in described hydrolysis salts solution
47H
2the content of O is 4～5g/L, CoSO
47H
2the content of O is 0.5～0.8g/L, H
3bO
3content be 4～5g/L, NaAc3H
2the content of O is 4～6g/L, and the pH value of hydrolysis salts solution is 4～6, temperature is 80～85 ℃, and the hold-time is 15～20min.
2. the surface treatment method of magnalium according to claim 1, is characterized in that: after each step, all use washed with de-ionized water magnalium sheet material.
3. the surface treatment method of magnalium according to claim 1 and 2, is characterized in that: in step (6), if yellow in electrolysis, adopting concentration is the KMnO of 20g/ L
4solution, condition is: 18～20 ℃ of temperature, voltage 15V, time 5min; If electrolysis red coloration, adopting concentration is the CuSO of 20g/ L
4solution, condition is: 18～20 ℃ of temperature, voltage 25V, time 5min; If purple in electrolysis, adopting by concentration is the CuSO of 30g/ L
4with concentration be the H of 20g/ L
2sO
4the mixed solution that the volume ratio of take forms as 1:1 configuration, parameter is: 18～20 ℃ of temperature, voltage 25V, time 3min.
4. the surface treatment method of magnalium according to claim 3, is characterized in that: the thickness of described magnalium sheet material is 1.5mm.
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