CN108193247A - Insulation protection Chromic Acid Anodizing Process - Google Patents
Insulation protection Chromic Acid Anodizing Process Download PDFInfo
- Publication number
- CN108193247A CN108193247A CN201711211635.6A CN201711211635A CN108193247A CN 108193247 A CN108193247 A CN 108193247A CN 201711211635 A CN201711211635 A CN 201711211635A CN 108193247 A CN108193247 A CN 108193247A
- Authority
- CN
- China
- Prior art keywords
- chromic acid
- solution
- anodizing
- acid anodizing
- processing
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Classifications
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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
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
Abstract
The present invention relates to a kind of insulation protection Chromic Acid Anodizing Process, including：1) pending part is cleaned with removing oil solution；2) chromic acid anodizing is carried out using chromic anhydride solution, is handled 75~85 minutes including 40V oxidation at voltages；Oxidation processes 5~10 minutes in the case of being risen to again not higher than 55V voltages；3) Seal treatment：Including deionized water Seal treatment and closed for second time：After the completion for the treatment of deionized water Seal treatment, then closed for second time processing is carried out, solution is nickel salt or bichromate or organic salt used by closed for second time processing；4) the surface chromic acid anodizing film layer removal for carrying out hard anodizing will be needed clean；5) hard anodizing is carried out, the solution of hard anodizing is sulfuric acid solution；6) processing is dried to step 5) products therefrom.The present invention provides a kind of resistance to insulation breakdown performance height and the good insulation protection Chromic Acid Anodizing Process of corrosion resisting property.
Description
Technical field
The invention belongs to field of material surface treatment, be related to a kind of insulation protection Chromic Acid Anodizing Process more particularly to
A kind of Chromic Acid Anodizing Process for Al and Al-alloy.
Background technology
Hard Anodic Oxidation of Aluminum Alloy is widely used in aerospace, auto industry, ocean naval vessel, health care, light-duty force
The high-tech such as device leading-edge field.But there is also the surface roughness increases by 1 that can enable aluminum alloy to parts for hard anodizing processing
~2 grades of the features such as, common product are designed and are only required in the carry out part hard anodizing processing such as abrading section of workpiece, remaining
Face considers the problems such as corrosion resistance, precision and roughness, to carry out chromic acid anodizing processing.Due to general chromic acid anodizing
The anti-insulation voltage performance of film layer is weak, and breakdown, generation horniness anode oxide film layer is particularly easy in hard anode oxidation process.
Traditional process is：1) it is whole to carry out chromic acid anodizing；2) mechanical processing removal needs the chromium at hard anodizing position
Sour anode oxidation membrane；3) it carries out whole apply and protects wax or glue, and cure；4) removal needs the wax layer at hard anodizing position,
Then hard anodizing is carried out to the position；5) wax layer of piece surface is removed.The shortcomings that process is：Hard anode
Wax before oxidation/glue removal is not clean, can cause after hard anodizing locally to show without film layer be mostly white point or
Hickie, this phenomenon often occur.And waxing/glue and to go paraffin removal/glue process be manual removal, time-consuming and laborious, quality can not
Control.Existing chromic acid anodizing technology is substantially by way of once pressurizeing, and under 22V or 40V oxidation at voltages is certain
Time carries out, and the method for closing is substantially to be closed with hot water, sodium dichromate solution or nickel acetate solution, it is preferred to use
Nickel salt or bichromate are closed, but containing a large amount of heavy metal element in such solution, pollute larger after discharge, and environmental protection is controlled
It is very high to manage cost.
Invention content
In order to solve above-mentioned technical problem present in background technology, the present invention provides a kind of resistance to insulation breakdown performance is high
And the good insulation protection Chromic Acid Anodizing Process of corrosion resisting property.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of insulation protection Chromic Acid Anodizing Process, it is characterised in that：The technique includes the following steps：
1) pending part is cleaned with removing oil solution；
2) the pending part cleaned up is filled to hang and carries out chromic acid anodizing, the chromic acid anodizing uses molten
Liquid is chromic anhydride solution, and the chromic acid anodizing process is handled using secondary booster；The secondary booster processing includes 40V voltages
Lower oxidation processes 75~85 minutes；Oxidation processes 5~10 minutes in the case of being risen to again not higher than 55V voltages；
3) Seal treatment：The Seal treatment includes deionized water Seal treatment and closed for second time：The deionized water
The temperature of Seal treatment is 96 DEG C~100 DEG C, and the time of deionized water Seal treatment is 30~40 minutes；Treat that deionized water is closed
After the completion of processing, then closed for second time processing is carried out, solution is nickel salt solution or dichromic acid used by the closed for second time processing
Salting liquid or organic slat solution, the temperature of the closed for second time processing is 80 DEG C~90 DEG C, the time 10 that closed for second time is handled~
15 minutes；
4) the surface chromic acid anodizing film layer for carrying out hard anodizing will be needed to remove by the way of mechanical processing
Totally；
5) part by oil removing and after cleaning up carries out hard anodizing, and the solution of the hard anodizing is sulphur
Acid solution, the temperature of the hard anodizing is -2 DEG C~-8 DEG C；
6) processing is dried to step 5) products therefrom.
Above-mentioned steps 3) in closed for second time processing used by solution be ammonium acetate solution, nickel acetate solution or dichromic acid
Sodium solution.
Above-mentioned steps 3) in closed for second time processing used by solution be ammonium acetate solution, the ammonium acetate solution it is dense
Degree is 4~5g/L.
Above-mentioned steps 2) in secondary booster processing include 40V oxidation at voltages processing 75~85 minutes；50V voltages are risen to again
5~10 minutes of lower oxidation processes
Above-mentioned steps 2) in from 40V voltages rise to not higher than 55V voltages when, the liter rate of voltage is 2V/min.
Above-mentioned steps 6) in be dried mode for compressed air drying.
It is an advantage of the invention that：
The present invention provides a kind of insulation protection Chromic Acid Anodizing Process, should pass through the work of secondary pressurized and dual sealing
Process forms one layer of non-porous, fine and close chromic acid anodizing film layer in aluminum alloy surface, and resistance to insulation breakdown performance improves；
The phenomenon that horniness anode oxide film thickness reaches 68 microns without leaking；The thickness of chromic acid anodizing film layer can be reached 4
~6 microns；Film layer weight up to 250 milli gram/ft or more；Minimum insulation voltage reaches more than 90V；Improve the resistance to of film layer
Corrosion, film layer can be by 800 hours neutral salt spray tests before hard anodizing, and film layer remains to pass through after hard anodizing
The neutral salt spray test of 360 hours can be directly used for the insulation protection of hard anode oxidation process, substitute traditional chromic acid anodic oxygen
The method for carrying out wax/glue protection after change again.The present invention may replace traditional painting protection wax/adhesive process, shorten part processing stream
Journey, it is time saving and energy saving, and part qualification rate greatly improves, process is simple, and controllability is strong, and the lock solution green worked out
Environmental protection reduces pollution, economical and practical.
Description of the drawings
Fig. 1 is insulation protection Chromic Acid Anodizing Process flow chart provided by the present invention；
Fig. 2 is voltage and time graph；
Fig. 3 is the thickness of chromic acid anodizing film and the relation curve of oxidation voltage；
Fig. 4 is chromic acid anodizing film layer closing schematic diagram.
Specific embodiment
Referring to Fig. 1, the present invention provides a kind of insulation protection Chromic Acid Anodizing Process, include the following steps：
1) pending part is cleaned with removing oil solution；
2) the pending part cleaned up is filled to hang and carries out chromic acid anodizing, the solution that chromic acid anodizing uses is
Chromic anhydride solution, chromic acid anodizing process are handled using secondary booster；Secondary booster processing includes 40V oxidation at voltages processing 75
~85 minutes；Oxidation processes 5~10 minutes in the case of being risen to again not higher than 55V voltages preferably rise to the situation of 50V voltages
Lower carry out oxidation processes；Oxidation film layer thickness can reach 4~6 microns；When rising to from 40V voltages not higher than 55V voltages, voltage
The rate of liter is 2V/min；
3) Seal treatment：Seal treatment includes deionized water Seal treatment and closed for second time：Deionized water Seal treatment
Temperature be 96 DEG C~100 DEG C, the time of deionized water Seal treatment is 30~40 minutes；Treat that deionized water Seal treatment is completed
Afterwards, then closed for second time processing is carried out, solution is nickel salt solution or dichromate solution or organic used by closed for second time processing
Salting liquid, the temperature of closed for second time processing is 80 DEG C~90 DEG C, 10~15 minutes time of closed for second time processing；At closed for second time
The preferred ammonium acetate solution of solution, nickel acetate solution or sodium dichromate solution used by reason；Preferably ammonium acetate solution, ammonium acetate
The concentration of solution is 4~5g/L.
4) the surface chromic acid anodizing film layer for carrying out hard anodizing will be needed to remove by the way of mechanical processing
Totally；
5) part by oil removing and after cleaning up carries out hard anodizing, and the solution of hard anodizing is that sulfuric acid is molten
Liquid, the temperature of hard anodizing is -2 DEG C~-8 DEG C, and thicknesses of layers requires 50 microns or more, aoxidizes whole voltage in 80V or so；
6) processing step 5) products therefrom is dried, the mode of drying process is dried up for compressed air.
The present invention the mechanism of action be：
The film forming mechanism of aluminium alloy chromic acid anodizing：The generation of oxidation film is the knot that two kinds of differential responses are carried out at the same time
Fruit, one kind are electrochemical reactions, and oxygen is precipitated and is combined with metallic aluminium, generates oxidation film；Another kind is chemical reaction, i.e. chromic anhydride acid is right
The dissolving of film, only when electrochemical reaction rates are more than chemical reaction velocity, oxidation film can just be successfully generated and keep certain
Thickness.Oxidation carries out after a certain period of time, and due to the generation on barrier layer, film layer formation speed is less than the solution rate of film, and supercharging can
To promote formation speed, still, the influence of voltage is very big, generally the method for constant pressure need to be used to carry out, otherwise film layer is easy to molten
Solution and dusting.According to the film layer structure of aluminium alloy chromic acid anodizing, the chromic acid anodizing film layer of aluminium alloy is bilayer structure,
Barrier layer of the internal layer for dense non-porous, the porous layer that outer layer is made of hole and hole wall.Barrier layer is one layer against metal watch
The thin oxide film in face, thickness are about 0.1 micron, and the main part of chromic acid anodizing film layer is then porous layer, porosity
Greatly, fenestra opens, if directly carrying out hard anodizing in the case of no closing, the sulfuric acid solution meeting of hard anodizing
It is slowly penetrated into fenestra by hole, after hard anodizing voltage reaches certain value, chromic acid anodizing film layer is easily
It is breakdown.
Referring to Fig. 2, chromic acid anodizing after a certain period of time, when oxidation voltage increases to 50V by 40V so that anodic oxygen
Changing the growth rate of film increases, and reduces the meltage of film layer, this process thickens film layer, shown in Figure 3.When oxidation voltage is protected
It holds in 40V, oxide thickness is substantially at 3 microns, and when oxidation voltage is risen to 50V, oxide thickness rises to 5 microns of left sides
The right side, the time of this process had to control within 10 minutes, and when voltage increases 55V again, thicknesses of layers reduces instead, film layer
Even there is dusting, film quality declines, it is impossible to use.
Referring to Fig. 4, chromic acid anodizing film layer is transformed into tool through deionized water closed process, aluminium oxide by hydration reaction
There are the hydrated alumina of vigorous nurse body structure, volume increase, so as to which micropore be closed.But the oxide film protection performance after sealing of hole has
Limit, when film layer is closed through Ammonium Acetate, ammonium acetate reacts hydrolysis with hydrated alumina, can close the porous layer of oxidation film again.
Hard anode oxidation process sulfuric acid concentration and temperature are relatively low, and voltage and current density is higher, when thicknesses of layers reaches about 50 microns
When, voltage can reach 80V or so, and general chromic acid anodizing film layer is necessarily breakdown, and (50V, that is, breakdown need to use protection
Wax or glue carry out insulation protection).Chromic acid anodizing film layer has certain porosity, after deionized water is closed, some micropores
It is not fully blocked, closing efficiency is not achieved 100%, is closed again through ammonium acetate after deionized water closing, can be to not sealing
The micropore for closing or not being fully blocked is closed, and improves closing efficiency.Deionized water and ammonium acetate dual sealing technique make
Oxidation film surface forms one layer of non-porous anodization film layer.This membranous layer corrosion resistance is fine, can the resistance to hard anodizing of long-time
When sulfuric acid corrosion, while the film layer has good insulating properties again, is that have obstructed sulfuric acid completely molten in local hard anodizing
Liquid is entered in film layer micropore, substantially increases pressure-resistant performance of the oxidation film in hard anodizing.
Initiative of the invention employs ammonium acetate as closed for second time solution, and salting liquid is closed all relative to conventionally employed
It is the sodium dichromate solution or nickel acetate solution of heavily contaminated, environmental pollution is very big, and cost of sewage disposal is high, and difficulty is big.This hair
The ammonium acetate lock solution of bright use and traditional sodium dichromate solution or nickel acetate solution, effect is suitable, but environmentally friendly,
Exhaust emission is small.
Embodiment one
For the process of insulation protection chromic acid anodizing, first secondary booster carries out chromic acid anodizing, then carries out
Deionized water is closed, and ammonium acetate closing is carried out again in 2 minutes.Secondary booster is first aoxidizes 80 minutes, then in 50V electricity under 40V
Pressure oxidation 8 minutes；The temperature of deionized water closing is 98 DEG C, and the time is 35 minutes；Ammonium acetate closure temperature is 85 DEG C, the time
It is 13 minutes.The thickness of acquired chromic acid anodizing film layer reaches 5 microns；Film layer weight up to 280 milli gram/ft；It is minimum
Insulation voltage reaches 95V；Film layer can pass through 800 hours neutral salt spray tests, hard anodizing caudacoria before hard anodizing
Layer is still resistant to the neutral salt spray test of 360 hours, can be directly used for the insulation protection of hard anode oxidation process.
Embodiment two
For the process of insulation protection chromic acid anodizing, first secondary booster carries out chromic acid anodizing, then carries out
Deionized water is closed, and ammonium acetate closing is carried out again in 2 minutes.Secondary booster is first aoxidizes 75 minutes, then in 50V electricity under 40V
Pressure oxidation 5 minutes；The temperature of deionized water closing is 96 DEG C, and the time is 30 minutes；Ammonium acetate closure temperature is 80 DEG C, the time
It is 10 minutes.The thickness of acquired chromic acid anodizing film layer reaches 4 microns；Film layer weight up to 250 milli gram/ft；It is minimum
Insulation voltage reaches 90V；Film layer can pass through 800 hours neutral salt spray tests, hard anodizing caudacoria before hard anodizing
Layer is still resistant to the neutral salt spray test of 360 hours, can be directly used for the insulation protection of hard anode oxidation process.
Embodiment three
For the process of insulation protection chromic acid anodizing, first secondary booster carries out chromic acid anodizing, then carries out
Deionized water is closed, and ammonium acetate closing is carried out again in 2 minutes.Secondary booster is first aoxidizes 85 minutes, then in 50V electricity under 40V
Pressure oxidation 10 minutes；The temperature of deionized water closing is 100 DEG C, and the time is 40 minutes；Ammonium acetate closure temperature is 90 DEG C, when
Between be 15 minutes.The thickness of acquired chromic acid anodizing film layer reaches 6 microns；Film layer weight up to 260 milli gram/ft；Most
Small insulation voltage reaches 95V；Film layer can be by 824 hours neutral salt spray tests, after hard anodizing before hard anodizing
Film layer is still resistant to the neutral salt spray test of 365 hours, can be directly used for the insulation protection of hard anode oxidation process.
Compared to according to MIL-A-8625F《The anode oxide film of aluminium and aluminium alloy》The weight one of middle chromic acid anodizing film layer
As 200 milli gram/ft；And according to 914-032-093/099《Aluminium alloy anodization processing》Chromic acid anodizing film layer
Minimum insulation voltage in 50V；It can be tried according to MIL-A-8625F chromic acid membranous layer corrosion resistance by the neutral salt spray of 336 hours
It tests, HB5373-87《Aluminium and aluminium alloy chromic acid anodizing film quality are examined》Chromic acid membranous layer corrosion resistance can pass through 300 hours
Neutral salt spray test, retrieve paper and report that certain high anti-corrosion Chromic Acid Anodizing Process can be such that film layer passes through 750 hours
Neutral salt spray test.By insulation protection Chromic Acid Anodizing Process provided by the present invention not only in chromic acid anodizing film layer
Weight on and neutral salt spray test in be all greatly improved than the prior art, far superior to existing treatment process.
Insulation protection Chromic Acid Anodizing Process provided by the present invention is using secondary during chromic acid anodizing
Boosting is that thicknesses of layers increases, while through deionized water and ammonium acetate dual sealing, one layer of non-porous, cause is formed in aluminum alloy surface
Close chromic acid anodizing film layer, resistance to insulation breakdown performance improve.Reach 68 microns without sending out in horniness anode oxide film thickness
The phenomenon that raw leakage, chromic acid anodizing film layer is intact, not due to film layer is breakdown and generates stain or blackspot, chromic acid sun
There is no transition between pole oxidation film layer and horniness anode oxide film layer, boundary is apparent.The chromic acid anodizing thicknesses of layers up to 4~
6 microns, film layer weight is more than or equal to 250 millis gram/ft, and minimum insulation voltage is more than or equal to 90V, in hard anodizing
Afterwards, chromic acid anodizing film layer can be good by the neutral salt spray test of 360 hours, membranous layer corrosion resistance；Hard anodic oxygen
Film layer can be by 800 hours neutral salt spray tests before change, and film layer remains to the neutral salt spray examination of resistance to 360 hours after hard anodizing
It tests, can be directly used for the insulation protection of hard anode oxidation process, wax/glue protection is carried out again after substituting traditional chromic acid anodic oxidation
Method.
Claims (6)
1. a kind of insulation protection Chromic Acid Anodizing Process, it is characterised in that：The technique includes the following steps：
1) pending part is cleaned with removing oil solution；
2) the pending part cleaned up is filled to hang and carries out chromic acid anodizing, the solution that the chromic acid anodizing uses is
Chromic anhydride solution, the chromic acid anodizing process are handled using secondary booster；The secondary booster processing includes oxygen under 40V voltages
Change processing 75~85 minutes；Oxidation processes 5~10 minutes in the case of being risen to again not higher than 55V voltages；
3) Seal treatment：The Seal treatment includes deionized water Seal treatment and closed for second time：The deionized water closing
The temperature of processing is 96 DEG C~100 DEG C, and the time of deionized water Seal treatment is 30~40 minutes；Treat deionized water Seal treatment
After the completion, then closed for second time processing is carried out, solution is that nickel salt solution or bichromate are molten used by the closed for second time processing
Liquid or organic slat solution, the temperature of the closed for second time processing is 80 DEG C~90 DEG C, 10~15 points of the time of closed for second time processing
Clock；
4) the surface chromic acid anodizing film layer removal for carrying out hard anodizing will be needed clean by the way of mechanical processing；
5) part by oil removing and after cleaning up carries out hard anodizing, and the solution of the hard anodizing is that sulfuric acid is molten
Liquid, the temperature of the hard anodizing is -2 DEG C~-8 DEG C；
6) processing is dried to step 5) products therefrom.
2. insulation protection Chromic Acid Anodizing Process according to claim 1, it is characterised in that：Two in the step 3)
Solution is ammonium acetate solution, nickel acetate solution or sodium dichromate solution used by secondary Seal treatment.
3. insulation protection Chromic Acid Anodizing Process according to claim 2, it is characterised in that：Two in the step 3)
Solution is ammonium acetate solution used by secondary Seal treatment, and the concentration of the ammonium acetate solution is 4~5g/L.
4. insulation protection Chromic Acid Anodizing Process according to claim 3, it is characterised in that：It is secondary in the step 2)
Boosting processing includes 40V oxidation at voltages and handles 75~85 minutes；5~10 points of oxidation processes in the case of 50V voltages are risen to again
Clock.
5. the insulation protection Chromic Acid Anodizing Process according to claims 1 or 2 or 3 or 4, it is characterised in that：The step
It is rapid 2) in from 40V voltages rise to not higher than 55V voltages when, the liter rate of voltage is 2V/min.
6. insulation protection Chromic Acid Anodizing Process according to claim 5, it is characterised in that：It is dry in the step 6)
The mode of processing is dried up for compressed air.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711211635.6A CN108193247A (en) | 2017-11-28 | 2017-11-28 | Insulation protection Chromic Acid Anodizing Process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711211635.6A CN108193247A (en) | 2017-11-28 | 2017-11-28 | Insulation protection Chromic Acid Anodizing Process |
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| CN108193247A true CN108193247A (en) | 2018-06-22 |
Family
ID=62573288
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| CN201711211635.6A Pending CN108193247A (en) | 2017-11-28 | 2017-11-28 | Insulation protection Chromic Acid Anodizing Process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110408973A (en) * | 2019-08-14 | 2019-11-05 | 深圳市晋铭航空技术有限公司 | A kind of chemical method for treating surface for aviation part |
| CN112609219A (en) * | 2020-11-17 | 2021-04-06 | 中国航发西安动力控制科技有限公司 | Bath solution for red anodic oxidation of aluminum alloy material and process method |
| CN114318316A (en) * | 2021-10-28 | 2022-04-12 | 中国航发西安动力控制科技有限公司 | Aluminum alloy colorless chemical oxidation treatment solution and process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408973A (en) * | 2019-08-14 | 2019-11-05 | 深圳市晋铭航空技术有限公司 | A kind of chemical method for treating surface for aviation part |
| CN112609219A (en) * | 2020-11-17 | 2021-04-06 | 中国航发西安动力控制科技有限公司 | Bath solution for red anodic oxidation of aluminum alloy material and process method |
| CN114318316A (en) * | 2021-10-28 | 2022-04-12 | 中国航发西安动力控制科技有限公司 | Aluminum alloy colorless chemical oxidation treatment solution and process |
| CN114318316B (en) * | 2021-10-28 | 2024-01-12 | 中国航发西安动力控制科技有限公司 | Colorless chemical oxidation treatment solution and process for aluminum alloy |
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Application publication date: 20180622 |