CN102321904A - Mixed acid anodizing and hole sealing method of magnesium-containing high-silicon-content wrought aluminum alloy surface - Google Patents
Mixed acid anodizing and hole sealing method of magnesium-containing high-silicon-content wrought aluminum alloy surface Download PDFInfo
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- CN102321904A CN102321904A CN201110246085A CN201110246085A CN102321904A CN 102321904 A CN102321904 A CN 102321904A CN 201110246085 A CN201110246085 A CN 201110246085A CN 201110246085 A CN201110246085 A CN 201110246085A CN 102321904 A CN102321904 A CN 102321904A
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Abstract
The invention belongs to the technical field of alloy surface treatment, and particularly relates to a mixed acid anodizing and hole sealing method of a magnesium-containing high-silicon-content wrought aluminum alloy surface, which comprises the following steps that: after a magnesium-containing high-silicon-content wrought aluminum alloy workpiece with the silicon content of up to 10-15wt% is pre-treated, a mixed acid liquid of 150-180g/L of H2SO4 and 5-15g/L of organic acid is used as an electrolytic liquid, the magnesium-containing high-silicon-content wrought aluminum alloy workpiece is subjected to DC (direct current) anodic oxidation for 20-25min at room temperature at the current density of 1.2-1.8A/dm<2>, and then is subjected to boiling water sealing, cold sealing, nickel acetate sealing or stearic acid hole sealing. In the acid anodizing and hole sealing method, a layer of anodic oxide film is prepared on the surface of magnesium-containing high-silicon-content wrought aluminum alloy by controlling anodizing process parameters and hole sealing process conditions, thereby improving the corrosion resistance of the surface of the magnesium-containing high-silicon-content wrought aluminum alloy.
Description
Technical field
The invention belongs to the alloy surface processing technology field, be specifically related to a kind of method that contains high silicon wrought aluminium alloy surface mixed acid anodic oxidation of magnesium and sealing of hole.
Background technology
Contain the high silicon wrought aluminium alloy of magnesium, silicon content is up to 10-15wt%, is the novel aluminum alloy with complete independent intellectual property right of China's research and development, is a kind of typical resource-conserving, environmentally friendly high-performance and low-cost novel material.It has, and to be superior to 6XXX be the room temperature strength of wrought aluminium alloy and suitable with it plasticity, has wide application space civilian with industrial circle.But in aluminum substrate, add the high content silicon element, can improve its castability, increase material hardness and intensity, reduced its solidity to corrosion also.
For architectural aluminum section and other industrial aluminum profile, surface treatment is further to improve the indispensable technological process of aluminium shape surface hardness, corrosion resistance nature and aesthetic measure.The aluminium of using always in the industry and the process of surface treatment of alloy thereof are anodic oxidation, electrolytic coloring and electrophoretic painting, and be wherein general with anodic oxidation.The anodic oxidation of aluminium and alloy thereof comprises metallic aluminium simultaneously and generates two processes on the surface from surface dissolution and aluminum oxide, and net result is to generate the micron-sized aluminium sesquioxide film of one deck at material surface, plays and improves hardness and corrosion proof effect.Contain the high silicon wrought aluminium alloy of magnesium through anodize, behind the surface metal al dissolution, expose not oxidized elemental silicon, the aluminum oxide film of generation is difficult for covering elemental silicon, and corrode easily in the gap that silicon grain causes.Thereby containing the high silicon wrought aluminium alloy of magnesium material has requirements at the higher level to surface treatment.The chemistry or the physical treatment course that carry out for anode oxide film after the alumilite process are to reduce the porosity and the adsorptive power of anode oxide film.Because there is a large amount of microvoid structures unit in anode oxide film, has increased the useful area that is exposed to aluminum alloy specimen in the environment greatly, easily suffering erosion property ionic corrosion failure; Micropore adsorbs the pollutent in the environment easily, influences the outward appearance of film, for improving its erosion resistance and stain resistance, must carry out sealing of hole and handle.
Summary of the invention
Blank in order to remedy existing process for treating surface to containing the high silicon wrought aluminium alloy of magnesium surface-treated; To the weak point that contains the high silicon wrought aluminium alloy of magnesium solidity to corrosion difference; The present invention provides a kind of method that contains high silicon wrought aluminium alloy surface mixed acid anodic oxidation of magnesium and sealing of hole, contains the solidity to corrosion of the high silicon wrought aluminium alloy of magnesium in order to raising.
The preparation process of electrolytic coloring film of the present invention is: pre-treatment, mixed acid anodic oxidation and sealing of hole.
Specifically carry out according to the following steps:
(1) pre-treatment
Pre-treatment comprises treat mechanically, oil removing, alkali erosion, pickling, dedust five processes.The pre-treatment of aluminium alloy anode oxide in the past is four procedures, does not have the dedust operation.But contain the high silicon wrought aluminium alloy of magnesium because the silicon content of silumin material own is higher, form the loose grey shape thing upper layer of one deck grey black after the alkali erosion at alloy surface, still have residually after the pickling, this ash shape thing will lean on dedust technology to remove.
Choose and contain the high silicon wrought aluminium alloy of magnesium workpiece, with it successively through 300
#, 600
#, 800
#With 1000
#Liquid honing, again with polishing machine polishing, make workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 2-3min in 60-65 C alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 98-100 C constant temperature pickling 2-3 min, the composition of acid solution is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4, 5g/L Na
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 2-3s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 15 ~ 30 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
Dedust reaction more complicated, principal reaction has:
Si?+?4HNO
3?=?SiO
2↓?+?4NO
2↑?+?2H
2O (1)
SiO
2?+?6HF?=?H
2SiF
6?+?2H
2O (2)
Al?+?4HNO
3?=?Al(NO
3)
3?+?NO↑?+?2H
2O (3)
3M?+?8HNO
3?=?3M(NO
3)
2?+?2NO↑?+?4H
2O (4)
Al
2O
3?+?6HNO
3?=?2Al(NO
3)
3?+?3H
2O (5)
M represents metallic elements such as manganese in the aluminum component, copper in the reaction (4).The effect of nitric acid is oxidation elemental silicon, dissolved oxygen aluminium film and generate aluminum nitrate, plays a major role to improving the chemical rightenning quality.The effect of hydrofluoric acid is a dissolve silica, for the workpiece that blind hole is arranged, will fully clean after the pickling, makes not remaining acid solution in the blind hole.
(2) anodic oxidation
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, be negative electrode with graphite or stereotype, as cell liquid, carry out dc anodizing 20-25min with mixing acid at normal temperatures, current density is 1.2-1.8A/dm
2
The consisting of of mix acid liquor in the described electrolyzer: 150-180 g/L mass concentration is 98% H
2SO
4With the 5-15g/L organic acid; Described organic acid is Hydrocerol A, tartrate or oxalic acid.
(3) sealing of hole
The high silicon wrought aluminium alloy of magnesium that contains after the antianode oxidation of the present invention carries out boiling water sealing hole, cold sealing of hole, nickel acetate sealing of hole or Triple Pressed Stearic Acid sealing of hole.
The essence of boiling water sealing hole is hydration reaction, and when low temperature, water is adsorbed on rete with physics mode; When high temperature, water and oxide compound chemical combination generate boehmite γ-Al
2O
3NH
2O,
Al
2O
3?+?nH
2O?=?Al
2O
3·nH
2O↓?(n?=1?or?3)
(6)
Work as Al
2O
3Aquation is monohydrate alumina (Al
2O
3H
2During O, its volumetric expansion can increase about 33%; Generate hibbsite (Al
2O
33H
2O) time, its volume increases almost 100%, because the result of sull surface and hole wall aquation, volumetric expansion makes the fenestra sealing.
The step of boiling water sealing hole of the present invention is: will pass through the anodised deionized water that the high silicon wrought aluminium alloy of magnesium workpiece places pH=5.5 ~ 6.5 that contains; Keep 98 ~ 100 ° of C of temperature; Dry behind soak time 40 min, obtain containing the high silicon wrought aluminium alloy of magnesium workpiece behind the anodic oxidation boiling water sealing hole.
Cold hole-sealing technology metal-salt encapsulant commonly used in industry is NiF mostly
2, its principle is that the positively charged ion in the confining liquid gets in the fenestra, generates Ni (OH) with the reaction of hole ambient substance
2, Al
2O
3NH
2O with
The mixture of forming stops up fenestra, thereby isolates with external environment.
The step of the cold sealing of hole of the present invention is: will pass through the anodised high silicon wrought aluminium alloy of the magnesium workpiece that contains at normal temperatures and place the liquor of hole-sealing tank of pH=5.5-6.5 to soak 12-18min; Put it into 60-80 ° of C of temperature then; Dry after soaking 20min in the deionized water of pH=5.5-6.5, what obtain the cold sealing of hole of anodic oxidation contains the high silicon wrought aluminium alloy of magnesium workpiece.
Consisting of of liquor of hole-sealing tank: deionized water, 1.3-2.5g/L NiF
2
Nickel acetate sealing of hole mechanism is that hydrolysis takes place in anode oxide film nickel ion, and the nickel hydroxide precipitate of generation makes micropore be able to fill closure in micropore, and its principal reaction is:
NiAc
2?+?2H
2O?=?Ni(OH)
2↓+?2HAc (7)
The step of nickel acetate sealing of hole of the present invention is: will pass through the anodised high silicon wrought aluminium alloy of the magnesium workpiece that contains and place 85-90 ° of C liquor of hole-sealing tank to soak the oven dry of 40min after scouring, the moity of liquor of hole-sealing tank is: deionized water, NiSO
43.6-4.7g/L, the 5g/L Glacial acetic acid min. 99.5.
The organic acid hole sealing technology is to utilize sull to have porousness, and organic acid is carried out physics and chemisorption.Generated a kind of aluminium soap compounds through chemical action; Micropore in the sull is stopped up, make micropore closed, fill organic acid molecule in the sull micropore; In case the place that has fatigue or stress crack to exist aluminum substrate to expose; Organic acid just generates the aluminium soap compounds with sull, generates protective layer once more, prevents that corrosive from taking place.
The step of Triple Pressed Stearic Acid sealing of hole of the present invention is: will pass through and anodisedly contain the high silicon wrought aluminium alloy of magnesium workpiece to place temperature be 90 – 95
oSoak in the pure Triple Pressed Stearic Acid tank liquor of C behind the 40-45min with the deionized water wash oven dry, what obtain the Triple Pressed Stearic Acid sealing of hole contains the high silicon wrought aluminium alloy of magnesium workpiece.
The invention has the beneficial effects as follows:
The present invention is containing the high silicon wrought aluminium alloy of magnesium surface preparation one deck anode oxide film through control anode oxidation process parameter and hole-sealing technology condition, has improved the solidity to corrosion that contains the high silicon wrought aluminium alloy of magnesium surface;
The anode oxide film even compact of the present invention's preparation, oxide thickness 10-15 μ m.Through dripping alkaline process (JISH 8681-1-1999), phosphorus-chromic acid method (GB/T 8753.1-2005) and neutral salt spray test method standard methods such as (QB 3826-1999) check, it is qualified that the anodic oxidation film quality behind the sealing of hole is.
Embodiment
Embodiment 1
(1) pre-treatment
That chooses silicon content and be 10wt% contains the high silicon wrought aluminium alloy of magnesium workpiece, with it earlier after the liquid honing of 300# water, 600#, 800# and 1000# again with the polishing machine polishing, makes workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 3min in 60 ℃ of alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 100 ℃ of constant temperature pickling 2 min, the composition of acid solution is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4, 5g/L Na
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 2s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 15 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
(2) sulfuric acid-Hydrocerol A anodic oxidation
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, with the stereotype negative electrode, with 170 g/L mass concentrations 98% H
2SO
4With the mix acid liquor of 10g/L Hydrocerol A as cell liquid, carry out dc anodizing 22min at normal temperatures, current density is 1.5A/dm
2
(3) boiling water sealing hole
To pass through the anodised deionized water liquor of hole-sealing tank that the high silicon wrought aluminium alloy of magnesium workpiece places pH=5.5 that contains, keep temperature 100 C, soak 40min after, what oven dry obtained the mixed acid anodic oxidation boiling water sealing hole contains the high silicon wrought aluminium alloy of magnesium workpiece.
Embodiment 2
(1) pre-treatment
That chooses silicon content and be 15wt% contains the high silicon wrought aluminium alloy of magnesium workpiece, with it earlier after the liquid honing of 300#, 600#, 800# and 1000# again with the polishing machine polishing, makes workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 2min in 65 ℃ of alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 98 ℃ of constant temperature pickling 3 min, the composition of acid solution is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4, 5g/L Na
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 2s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 15 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
(2) sulfuric acid-Hydrocerol A anodic oxidation
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, with the stereotype negative electrode, with the 150g/L mass concentration 98% H
2SO
4With the mix acid liquor of 15g/L Hydrocerol A as cell liquid, carry out dc anodizing 20min at normal temperatures, current density is 1.8A/dm
2
(3) cold sealing of hole
To pass through the anodised high silicon wrought aluminium alloy of the magnesium workpiece that contains at normal temperatures places the liquor of hole-sealing tank of pH=5.5 to soak 12min; Put it into 60 ° of C of temperature then; Dry after soaking 20min in the deionized water of pH=5.5; What obtain the cold sealing of hole of anodic oxidation contains the high silicon wrought aluminium alloy of magnesium workpiece, wherein consisting of of liquor of hole-sealing tank: deionized water, 2.5g/L NiF
2
Embodiment 3
(1) pre-treatment
That chooses silicon content and be 11wt% contains the high silicon wrought aluminium alloy of magnesium workpiece, with it earlier after the liquid honing of 300#, 600#, 800# and 1000# again with the polishing machine polishing, makes workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 3min in 60 alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 99 ℃ of constant temperature pickling 3 min, the composition of acid solution is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4, 5g/L Na
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 2s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 15 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
(2) sulfuric acid-Hydrocerol A anodic oxidation
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, with the stereotype negative electrode, with 180 g/L mass concentrations 98% H
2SO
4With the mix acid liquor of 5g/L Hydrocerol A as cell liquid, carry out dc anodizing 25min at normal temperatures, current density is 1.2A/dm
2
(3) nickel acetate sealing of hole
To pass through the anodised high silicon wrought aluminium alloy of the magnesium workpiece that contains and place the liquor of hole-sealing tank of 85 ° of C to soak 40min after washing, oven dry, wherein the moity of liquor of hole-sealing tank is: deionized water, 3.6 g/L NiSO
4, the 5g/L Glacial acetic acid min. 99.5, what obtain anodic oxidation nickel acetate sealing of hole contains the high silicon wrought aluminium alloy of magnesium workpiece.
Embodiment 4
(1) pre-treatment
That chooses silicon content and be 12wt% contains the high silicon wrought aluminium alloy of magnesium workpiece, with it earlier after the liquid honing of 300#, 600#, 800# and 1000# again with the polishing machine polishing, makes workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 2 ~ 3min in 60 ~ 65 ℃ of alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 100 ℃ of constant temperature pickling 2 min, the composition of acid solution is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4, 5g/L Na
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 2s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 15 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
(2) sulfuric acid-Hydrocerol A anodic oxidation
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, with graphite negative electrode, with 170 g/L mass concentrations 98% H
2SO
4With the mix acid liquor of 12g/L Hydrocerol A as cell liquid, carry out dc anodizing 23min at normal temperatures, current density is 1.6A/dm
2
(3) Triple Pressed Stearic Acid sealing of hole
To pass through and anodisedly contain the high silicon wrought aluminium alloy of magnesium workpiece to place temperature be 90
oSoak in the pure Triple Pressed Stearic Acid tank liquor of C behind the 40min with the deionized water wash oven dry, what obtain the Triple Pressed Stearic Acid sealing of hole contains the high silicon wrought aluminium alloy of magnesium workpiece.
Embodiment 5
(1) pre-treatment
That chooses silicon content and be 13wt% contains the high silicon wrought aluminium alloy of magnesium workpiece, with it earlier after 300# liquid honing, 600# liquid honing, 800# liquid honing, 1000# liquid honing again with the polishing machine polishing, make workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 2min in 65 ℃ of alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 98 ℃ of constant temperature pickling 3 min, the composition of mix acid liquor is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4, 5g/L Na
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 3s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 20 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
(2) sulfuric acid-tartrate anodic oxidation
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, with the stereotype negative electrode, with the 170g/L mass concentration 98% H
2SO
4With the tartaric mix acid liquor of 10g/L as cell liquid, carry out dc anodizing 25min at normal temperatures, current density is 1.2A/dm
2
(3) boiling water sealing hole
To pass through the anodised deionized water liquor of hole-sealing tank that the high silicon wrought aluminium alloy of magnesium workpiece places pH=6.5 that contains, keep temperature 98 C, soak 40min after, what oven dry obtained the mixed acid anodic oxidation boiling water sealing hole contains the high silicon wrought aluminium alloy of magnesium workpiece.
Embodiment 6
(1) pre-treatment
That chooses silicon content and be 14wt% contains the high silicon wrought aluminium alloy of magnesium workpiece, with it earlier after 300#, 600#, 800# and 1000# liquid honing again with the polishing machine polishing, make workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 3min in 60 ℃ of alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 98 ℃ of constant temperature pickling 3 min, the composition of acid solution is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4, 5g/LNa
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 3s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 20 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
(2) sulfuric acid-tartrate anodic oxidation
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, with graphite negative electrode, with 180 g/L mass concentrations 98% H
2SO
4With the tartaric mix acid liquor of 5g/L as cell liquid, carry out dc anodizing 20min at normal temperatures, current density is 1.8A/dm
2
(3) cold sealing of hole
To pass through the anodised high silicon wrought aluminium alloy of the magnesium workpiece that contains at normal temperatures places the liquor of hole-sealing tank of pH=6.5 to soak 18min; Put it into 80 ° of C of temperature then; Dry after soaking 20min in the deionized water of pH=6.5; What obtain the cold sealing of hole of anodic oxidation contains the high silicon wrought aluminium alloy of magnesium workpiece, wherein consisting of of liquor of hole-sealing tank: deionized water, 1.3g/L NiF
2
Embodiment 7
(1) pre-treatment
That chooses silicon content and be 10wt% contains the high silicon wrought aluminium alloy of magnesium workpiece, with it earlier after 300# liquid honing, 600# liquid honing, 800# liquid honing, 1000# liquid honing again with the polishing machine polishing, make workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 2min in 65 ℃ of alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 100 ℃ of constant temperature pickling 2 min, the composition of acid solution is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4, 5g/L Na
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 3s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 20 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
(2) sulfuric acid-tartrate anodic oxidation
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, be negative electrode with graphite, with 150g/LH
2SO
4With the tartaric mix acid liquor of 15g/L as cell liquid, carry out dc anodizing 20min at normal temperatures, current density is 1.8A/dm
2
(3) nickel acetate sealing of hole
To pass through the anodised high silicon wrought aluminium alloy of the magnesium workpiece that contains and place the liquor of hole-sealing tank of 90 ° of C to soak 40min after washing, oven dry, wherein the moity of liquor of hole-sealing tank is: deionized water, 4.7g/L NiSO
4, the 5g/L Glacial acetic acid min. 99.5, what obtain anodic oxidation nickel acetate sealing of hole contains the high silicon wrought aluminium alloy of magnesium workpiece.
Embodiment 8
(1) pre-treatment
Choose silicon content and be 11% contain the high silicon wrought aluminium alloy of magnesium workpiece, with it earlier after 300# liquid honing, 600# liquid honing, 800# liquid honing, 1000# liquid honing again with the polishing machine polishing, make workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 2min in 65 ℃ of alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 100 ℃ of constant temperature pickling 2 min, the composition of acid solution is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H2SO4,5g/L Na
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 3s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 30 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
(2) sulfuric acid-tartrate anodic oxidation
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, with the stereotype negative electrode, with 160 g/L H
2SO
4With the tartaric mix acid liquor of 8g/L as cell liquid, carry out dc anodizing 25min at normal temperatures, current density is 1.2A/dm
2
(3) Triple Pressed Stearic Acid sealing of hole
To pass through anodised workpiece, to place temperature be 95
oSoak in the pure Triple Pressed Stearic Acid tank liquor of C behind the 45min with the deionized water wash oven dry, what obtain the Triple Pressed Stearic Acid sealing of hole contains the high silicon wrought aluminium alloy of magnesium workpiece.
Embodiment 9
(1) pre-treatment
That chooses silicon content and be 12wt% contains the high silicon wrought aluminium alloy of magnesium workpiece, with it earlier after the liquid honing of 300#, 600#, 800# and 1000# again with the polishing machine polishing, makes workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 3min in 60 ℃ of alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 98 ℃ of constant temperature pickling 3 min, the composition of acid solution is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4And 5g/L Na
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 2-3s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 20 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
(2) sulfuric acid-oxalic acid anodizing
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, with the stereotype negative electrode, with 170g/L H
2SO
4With the mix acid liquor of 10g/L oxalic acid as cell liquid, carry out dc anodizing 22min at normal temperatures, current density is 1.5A/dm
2
(3) boiling water sealing hole
To pass through the anodised deionized water liquor of hole-sealing tank that the high silicon wrought aluminium alloy of magnesium workpiece places pH=6 that contains, keep temperature 99 C, soak 40min after, what oven dry obtained the mixed acid anodic oxidation boiling water sealing hole contains the high silicon wrought aluminium alloy of magnesium workpiece.
Embodiment 10
(1) pre-treatment
That chooses silicon content and be 13wt% contains the high silicon wrought aluminium alloy of magnesium workpiece, with it earlier after the liquid honing of 300#, 600#, 800# and 1000# again with the polishing machine polishing, makes workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 3min in 60 ℃ of alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 100 ℃ of constant temperature pickling 2 min, the composition of acid solution is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4And 5g/L Na
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 3s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 20 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
(2) sulfuric acid-oxalic acid anodizing
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, with the stereotype negative electrode, with 180 g/L mass concentrations 98% H
2SO
4With the mix acid liquor of 15g/L oxalic acid as cell liquid, carry out dc anodizing 25min at normal temperatures, current density is 1.2A/dm
2
(3) cold sealing of hole
To pass through the anodised high silicon wrought aluminium alloy of the magnesium workpiece that contains at normal temperatures places the liquor of hole-sealing tank of pH=6.0 to soak 15min; Put it into 70 ° of C of temperature then; Dry after soaking 20min in the deionized water of pH=6.0; What obtain the cold sealing of hole of anodic oxidation contains the high silicon wrought aluminium alloy of magnesium workpiece, wherein consisting of of liquor of hole-sealing tank: deionized water, 2.0 g/L NiF
2
Embodiment 11
(1) pre-treatment
That chooses silicon content and be 14wt% contains the high silicon wrought aluminium alloy of magnesium workpiece, with it earlier after the liquid honing of 300#, 600#, 800# and 1000# again with the polishing machine polishing, makes workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 2min in 65 ℃ of alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 100 ℃ of constant temperature pickling 2 min, the composition of acid solution is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4And 5g/L Na
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 2s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 20 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
(2) sulfuric acid-oxalic acid anodizing
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, with the stereotype negative electrode, with 150 g/L mass concentrations 98% H
2SO
4With the mix acid liquor of 5g/L oxalic acid as cell liquid, carry out dc anodizing 20min at normal temperatures, current density is 1.8A/dm
2
(3) nickel acetate sealing of hole
To pass through the anodised high silicon wrought aluminium alloy of the magnesium workpiece that contains and place the liquor of hole-sealing tank of 88 ° of C to soak 40min after washing, oven dry, wherein the moity of liquor of hole-sealing tank is: deionized water, 4.0g/L NiSO
4With the 5g/L Glacial acetic acid min. 99.5, what obtain anodic oxidation nickel acetate sealing of hole contains the high silicon wrought aluminium alloy of magnesium workpiece.
Embodiment 12
(1) pre-treatment
Choose silicon content and be 15% contain the high silicon wrought aluminium alloy of magnesium workpiece, with it earlier after 300# liquid honing, 600# liquid honing, 800# liquid honing, 1000# liquid honing again with the polishing machine polishing, make workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove and lose 2min in 65 ℃ of alkali, the mixed alkali liquor composition in the alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 98 ℃ of constant temperature pickling 3 min, the composition of acid solution is in the acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4And 5g/L Na
2CO
3Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust handle, workpiece is soaked 2-3s at normal temperatures in the dedust tank liquor, the prescription of dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 30 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
(2) sulfuric acid-oxalic acid anodizing
So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, with the stereotype negative electrode, with 180 g/L mass concentrations 98% H
2SO
4With the mix acid liquor of 15g/L oxalic acid as cell liquid, carry out dc anodizing 25min at normal temperatures, current density is 1.2A/dm
2
(3) Triple Pressed Stearic Acid sealing of hole
To pass through and anodisedly contain the high silicon wrought aluminium alloy of magnesium workpiece to place temperature be that 92 ℃ pure Triple Pressed Stearic Acid tank liquor soaks behind the 43min with the deionized water wash oven dry, what obtain the Triple Pressed Stearic Acid sealing of hole contains the high silicon wrought aluminium alloy of magnesium workpiece.
Claims (10)
1. contain the method for the high silicon wrought aluminium alloy of magnesium surface mixed acid anodic oxidation and sealing of hole, it is characterized in that: at first choose and contain the high silicon wrought aluminium alloy of magnesium workpiece, its warp 300 successively
#, 600
#, 800
#With 1000
#Liquid honing, again with polishing machine polishing, make workpiece form finish plate; Put it into then that ultrasonic 10 min carry out oil removal treatment in the acetone; Be placed on afterwards in the alkali groove in 60-65 C alkali erosion 2-3min; Alkali erosion back workpiece is cleaned in the migration Rinsing Area in 1min, stop 1min after, put it into again in the acid tank in 98-100 C constant temperature pickling 2-3 min; Workpiece after the pickling is soaked 1min in Rinsing Area, in air, dry then; Workpiece after drying is carried out dedust to be handled; Place the dedust tank liquor to soak 2-3s at normal temperatures workpiece; So that to contain the high silicon wrought aluminium alloy of magnesium workpiece be anode through pretreated, be negative electrode with graphite or stereotype, with mixing acid as cell liquid; Carry out dc anodizing 20-25min at normal temperatures, current density is 1.2-1.8A/dm
2The high silicon wrought aluminium alloy of magnesium that contains after the antianode oxidation carries out boiling water sealing hole, cold sealing of hole, nickel acetate sealing of hole or Triple Pressed Stearic Acid sealing of hole; The described silicon content that contains the high silicon wrought aluminium alloy of magnesium is 10-15wt%.
2. the method that contains high silicon wrought aluminium alloy surface mixed acid anodic oxidation of magnesium and sealing of hole according to claim 1, it is characterized in that: the mixed alkali liquor composition in the described alkali groove is: 5g/L NaOH, 20g/L Na
3PO
4With 20g/L Na
2CO
3
3. a kind of method that contains high silicon wrought aluminium alloy surface mixed acid anodic oxidation of magnesium and sealing of hole according to claim 1, it is characterized in that: the composition of acid solution is in the described acid tank: 600 g/L mass concentrations are 85% H
3PO
4, 400 g/L mass concentrations are 98% H
2SO
4With 5g/L Na
2CO
3
4. the method that contains high silicon wrought aluminium alloy surface mixed acid anodic oxidation of magnesium and sealing of hole according to claim 1, it is characterized in that: the prescription of described dedust tank liquor is: 90 g/L mass concentrations are 98% H
2SO
4, 15 ~ 30 g/L NaF and 50 g/L mass concentrations are 68% HNO
3
5. the method that contains high silicon wrought aluminium alloy surface mixed acid anodic oxidation of magnesium and sealing of hole according to claim 1, it is characterized in that: the mixing acid of described cell liquid is by 150-180 g/L H
2SO
4Formulated with the 5-15g/L organic acid.
6. a kind of method that contains high silicon wrought aluminium alloy surface mixed acid anodic oxidation of magnesium and sealing of hole according to claim 5 is characterized in that selected organic acid is Hydrocerol A, tartrate or oxalic acid.
7. the method that contains high silicon wrought aluminium alloy surface mixed acid anodic oxidation of magnesium and sealing of hole according to claim 1; It is characterized in that: described boiling water sealing hole is with the deionized water that the high silicon wrought aluminium alloy of magnesium workpiece places pH=5.5 ~ 6.5 that contains after the process anodic oxidation; Keep 98 ~ 100 ° of C of temperature; Dry behind soak time 40 min, obtain containing the high silicon wrought aluminium alloy of magnesium workpiece behind the anodic oxidation boiling water sealing hole.
8. the method that contains high silicon wrought aluminium alloy surface mixed acid anodic oxidation of magnesium and sealing of hole according to claim 1; It is characterized in that: described cold sealing of hole is will pass through the anodised high silicon wrought aluminium alloy of the magnesium workpiece that contains at normal temperatures to place the liquor of hole-sealing tank of pH=5.5-6.5 to soak 12-18min; Put it into 60-80 ° of C of temperature then; Dry after soaking 20min in the deionized water of pH=5.5-6.5; What obtain the cold sealing of hole of anodic oxidation contains the high silicon wrought aluminium alloy of magnesium workpiece, wherein consisting of of liquor of hole-sealing tank: deionized water, 1.3-2.5g/LNiF
2
9. the method that contains high silicon wrought aluminium alloy surface mixed acid anodic oxidation of magnesium and sealing of hole according to claim 1; It is characterized in that: said nickel acetate sealing of hole is to place 85-90 ° of C liquor of hole-sealing tank to soak the oven dry of 40min after scouring the anodised high silicon wrought aluminium alloy of the magnesium workpiece that contains of process, and wherein the moity of liquor of hole-sealing tank is: deionized water, NiSO
43.6-4.7g/L and 5g/L Glacial acetic acid min. 99.5.
10. the method that contains high silicon wrought aluminium alloy surface mixed acid anodic oxidation of magnesium and sealing of hole according to claim 1, it is characterized in that: described Triple Pressed Stearic Acid sealing of hole is workpiece to be put in the process anodic oxidation place temperature 90-95
oSoak in the pure Triple Pressed Stearic Acid tank liquor of C behind the 40-45min with the deionized water wash oven dry, what obtain the Triple Pressed Stearic Acid sealing of hole contains the high silicon wrought aluminium alloy of magnesium workpiece.
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