CN104988554A - High-low-temperature composite type anodic oxidation hole sealing method - Google Patents
High-low-temperature composite type anodic oxidation hole sealing method Download PDFInfo
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Abstract
The invention relates to a high-low-temperature composite type anodic oxidation hole sealing method. The method comprises the following steps of (1), feeding; (2), atomization; (3), second-order washing; (4), light outputting; (5), third-order washing; (6), anodic oxidation; (7), third-order washing; (8), high-temperature hole sealing; (9), second-order washing; (10), weak-acid water washing; (11), passivation at room temperature; (12), third-order washing; (13), drying; and (14) discharging. Through the method, an anodic oxidation film on an aluminum alloy base material has the corrosion resistance and temperature resistance at the same time, and the excellent effect is achieved, so that the defect that a traditional technology can only meet the requirement for a certain single performance is effectively overcome; and functionality of the anodic oxidation technology is improved, and the application field of the anodic oxidation technology is effectively expanded.
Description
Technical field
The present invention relates to Al and Alalloy anodic oxidation treatment field, particularly a kind of anodic oxidation hole-sealing technology possessing high-low temperature resistant cyclic corrosion and resisting salt fog corrosion dual nature.
Background technology
Because anode oxide film is mainly divided into non-crystalline Al
2o
3, all there is larger great disparity (thermal conductivity of oxide film and thermal expansivity are about 1/10 and 1/5 of aluminum alloy base material respectively) in the thermal conductivity of this oxidation film layer and its body aluminum alloy base material and thermal expansivity.When being heated, aluminum substrate rapid temperature increases also produces expansion by a relatively large margin, and oxide film heats up slowly after being heated and thermal expansion amplitude is less, when oxide film cannot resist the stress produced because of aluminium base expansion, namely there is crazing of oxide film phenomenon, oxide film surface produces very thin tiny crack, especially more obvious under the illumination of a branch of miter angle.
Due to the generation of this tiny crack, the properties of anode oxide film especially solidity to corrosion obviously weakens thereupon, thus develop one both high-low temperature resistant alternative cycle test (Guangzhou Honda standard is: high temperature 80 DEG C, low temperature-30 DEG C, 10 cycles, add up to 80H), the anode oxidation process of resisting salt fog corrosion test (Guangzhou Honda CR-V 2WH/2XW project touchstone is CASS 80H) just becomes the focus that industry is paid close attention to again.
Conventional anodization technique often adopts the mode of high temperature hole sealing to solve oxide film temperature resistance problem, although this method effectively can improve oxide film hot cracking phenomenon, but its shortcoming is that the salt spray corrosion resistance of oxide film is undesirable, GB test can only reach CASS 24H; And the anodised resisting salt fog corrosion of car trim requires to be generally CASS 48H at present, or NSS 480H (being about as much as CASS 48H), external if the NSS test requirements document of Jaguar Land Rover is up to 1000H; Also have part factory to adopt normal temperature (or claiming " low temperature ") sealing of hole, this hole-sealing technology relative energy-saving for high temperature hole sealing, but the temperature resistance of oxide film and corrosion resistance nature all have obvious decline than the former;
Below with two
family's platformmoney enterprise anodic oxidation source mill preparation process be example so that conventional anodization technical process to be described:
A technique (true qualities): (1) material loading; (2) pre-degreasing; (3) second order washing; (4) degreasing; (5) second order washing; (6) alkaline etching; (7) second order washing; (8) chemical rightenning; (9) hot water wash; (10) second order washing; (11) neutralize; (12) three rank washings; (13) anodic oxidation; (14) three rank washings; (15) high temperature hole sealing; (16) three rank washings; (17) dry; (18) blanking.
B technique (true qualities): (1) material loading; (2) degreasing; (3) second order washing; (4) alkaline etching; (5) three rank washings; (6) plow; (7) second order washing; (8) throwing is changed; (9) three rank washings; (10) bright dipping; (11) three rank washings; (12) anodic oxidation; (13) three rank washings; (14) high temperature hole sealing; (15) three rank washings; (16) ash disposal; (17) three rank washings; (18) hot pure water is washed; (19) blanking.
Part factory additionally uses the mode of increase hot water rinsing (as B technique) to alleviate oxide film hot cracking phenomenon, its specific practice before product enters stoving oven, increases hot pure water together wash, rinsing time is not generally 30 ~ 120 seconds not etc., and water temperature controls usually at 60 ~ 80 degrees Celsius.This method has some improvement effect, but improves limited extent, and the test of high/low temperature alternative cycle is difficult to obtain gratifying result.
Summary of the invention
The object of the invention is to, provide a kind of anode oxide film preparation technology of excellence, prepared anode oxide film both can meet high/low temperature round-robin test requirement, can reach again high-level salt air corrosion requirement.
Concrete technical scheme of the present invention is as follows:
A kind of high/low temperature combined type anodic oxidation method for sealing, its processing step comprises: (1) material loading; (2) be atomized; (3) second order washing; (4) bright dipping; (5) three rank washings; (6) anodic oxidation; (7) three rank washings; (8) high temperature hole sealing; (9) second order washing; (10) weak acid pure water is washed; (11) normal temperature passivated; (12) three rank washings; (13) dry; (14) blanking.Wherein attach most importance to treatment process in operation (2), (6), (8), (11).
In the atomization procedure of described step (2), the main component of atomization is SODIUMNITRATE and sodium hydroxide, and the mass ratio of SODIUMNITRATE and sodium hydroxide is 2:1 ~ 2.5:1.Thus reach degreasing, oil removing and alkaline etching triple effect unification effect.
In described step (6) anodic oxidation operation, working concentration is the H of 180 ~ 200g/l
2sO
4, temperature 18 ~ 21 DEG C, current density 1.8 ~ 2A/dm
2, oxidization time was at 45 ~ 50 minutes, and oxide thickness controls at 17 ~ 22 μm.
In described step (8) high temperature hole sealing operation, working concentration is the nickel acetate hole sealing agent of 7 ~ 10g/l, temperature 92 ~ 98 DEG C, and the treatment time is 20 ~ 30 minutes; Solution needs circulation stirring and filters, avoid bubble or impurity be attached to product surface cause local non-sealing of hole or sealing of hole bad.
The pH value that described step (10) weak acid pure water is washed is 3.5 ~ 4.5, in order to avoid produce excessive impact to the PH value of passivation tank liquor.
In described step (11) normal temperature passivated operation, working concentration is 10 ~ 13% trivalent chromium passivation treatment agents, and temperature is 30 ~ 40 DEG C, and the treatment time is 7 ~ 10 minutes, and solution needs pure water to prepare also in use circulating filtration.
In described step (3), (5), (7), (9), (12) described washing step, washing water is ordinary tap water, wherein the last washing together of three rank washings is washing, pure water conductivity requires to be not more than 10us/cm, and all washing times are 30 ~ 60 seconds.
Temperature requirement in described step (13) described baking operation is 60 ~ 70 DEG C, and drying time controls at 10 ~ 20min.
Method of the present invention makes the anode oxide film on aluminum alloy base material possess erosion resistance and temperature resistance simultaneously, and reach excellent effect, thus effectively overcome the deficiency that traditional technology can only meet certain single performance requirement, enhance the functional of anode oxidation process, the efficient extn Application Areas of anode oxidation process.
Accompanying drawing explanation
fig. 1to the test of the method for sealing of embodiment according to Guangzhou Honda motor corporation round-robin test standard
figure.
Embodiment
Below by embodiment, the present invention is specifically described.What be necessary to herein means out is; following examples are only for the invention will be further described; can not limiting the scope of the invention be interpreted as, some nonessential improvement and adjustment that professional and technical personnel's content according to the present invention in this field is made, still belong to protection scope of the present invention.
Embodiment 1
The present embodiment have employed a kind of special Production Flow Chart order, and main points are hole-sealing technology.Specifically, adopt high/low temperature compound hole sealing technique, first carry out pyroprocessing (i.e. high temperature hole sealing), carry out subzero treatment (namely normal temperature passivated) again, anode oxide film after this art breading possesses excellent solidity to corrosion and high and low temperature resistance, the solidity to corrosion of anode oxide film can be made to reach resistance to CASS and test 80 ~ 120H, or resistance to NSS tests 1000 ~ 1200H, simultaneously can easily by the test in 10 cycles of high/low temperature alternative cycle of Guangzhou Honda motor corporation
as Fig. 1shown in.
fig. 1middle high/low temperature round-robin test, is warming up to 80 degree and constant temperature 2 hours from normal temperature, in 2 hours, is then cooled to-30 DEG C and constant temperature 2 hours, complies with
in figuremethod circulates 10 cycles in thermostat container, observes product surface with or without being out of shape, coming off totally, look becomes, wrinkling after 80 hours.
table 1for Guangzhou Honda high/low temperature round-robin test standard.
table 1
For achieving the above object, the present invention realizes like this.Its processing step comprises:
(1) material loading; (2) be atomized; (3) second order washing; (4) bright dipping; (5) three rank washings; (6) anodic oxidation; (7) three rank washings; (8) high temperature hole sealing; (9) divalence washing; (10) weak acid pure water is washed; (11) normal temperature passivated; (12) three rank washings; (13) dry; (14) blanking.Wherein operation (2) ~ (5) simply can be described as pre-treatment.
(2) ~ (5) pre-treating technology in above-mentioned process, in order to prepare satisfactory outward appearance.The main component that wherein operation (2) is atomized is SODIUMNITRATE and sodium hydroxide, mass ratio is (2 ~ 2.5): 1, add some tensio-active agents, there is the effect removing product surface greasy dirt, basic solution can be eliminated in the lump by bad to surperficial natural oxidizing layer and section bar extrusion line etc. simultaneously, and the participation of SODIUMNITRATE has and plays out light action to a certain extent, aluminum alloy surface after this operation process forms a kind of special dumb light satin face, is more finally formed through anodic oxidation treatment and have excellent handle and sheen visual effect.The main component of operation (4) bright dipping to be concentration be 30 ~ 40% nitric acid, effect is the impurity that the silicon, manganese etc. remaining in product surface after removing step (2) process is insoluble to basic solution, namely removes surperficial dust.In above-mentioned process, (7) ~ (14) are anodic oxidation aftertreatment, to improve the Functional Requirement of oxide film, as temperature resistance required in present invention process and solidity to corrosion etc.Wherein, operation (3), (5), (7), (9), (12) are washing, that chemical liquid residual in a upper procedure is cleaned up, avoid the treatment solution polluting next process, washing time about 30 ~ 60 seconds, to obtain clean surface effect for standard.Wherein the last single order washing of operation (5), (7), (12) three three rank washings is pure water and washes, time is about 30 ~ 60 seconds, but it is very high to water quality requirement, require that pure water conductivity is at 10 below μ s/cm, strict management and control impurities in water, especially calcium, magnesium ion and chlorion, provides necessary guarantee for producing the product be possessed of good qualities.Operation (16) is washed for weak acid pure water, and the time is about 30 ~ 60 seconds; The washing of this road there are certain requirements the potential of hydrogen of pure water, and usual pH value controls between 3.5 ~ 4.5, to guarantee that lower one passivating solution can the stability of pH; The pH value of the two all can adjust with dilute sulphuric acid or weak sodium hydroxide.
In above-mentioned process, operation (2), (6), (8), (11) are attached most importance to treatment process.
Below these key procedure steps are described in further detail:
In step (6) anodic oxidation operation, the rectifier power source type of use is direct current pulse power source; The H of electrolytic solution used is concentration to be concentration be 180 ~ 200g/l
2sO
4, temperature 17 ~ 20 DEG C, current density 1.8 ~ 2A/dm
2, oxidization time was at 45 ~ 50 minutes, and oxide thickness controls at 17 ~ 22 μm.
The critical processes of above-mentioned generation oxide film, when material is identical with being oxidized the parameters such as tank liquor composition, oxidization time and current density directly determine the thickness of rete.It is 17 ~ 22 μm that present invention process anodic oxidation thickness requires, rete is relatively thick, and the aluminum alloy material trade mark is 5052, therefore anodic oxidation rear oxidation film is easy to be with certain color, make true qualities appearance and should be noted that oxidizing process parameter.The temperature of electrolytic solution is the important factor affecting oxide film color, and present invention process process need controls electrolyte temperature at 17 ~ 20 DEG C.Be argenteous when entering groove temperature lower than the oxide film color produced when 14 DEG C, and to enter the oxide film outward appearance produced when groove temperature is greater than 25 DEG C be light yellow, and the more thick-skinned look of oxide film is darker.Under present invention process, the relation of electrolyte temperature and oxide film color (fixing oxide thickness) is shown in
following table 2.
table 2
At same current density and state of temperature, oxidization time is longer, and rete is thicker, and color is darker, strengthens the change of rete porosity greatly, corrosion-resistant reduction because dissolving simultaneously; Oxidization time is shorter, and rete is thinner, and the rete transparency is higher, but crosses thin because of rete so that correlated performance is not enough.Current density is larger, and become speed faster, the time of preparing needed for identical thickness is shorter, but easily causes goods " burn " or " turning white " phenomenon; Current density is less, and rate of film build is slower, and the time of preparing same thickness oxide film is longer, but similar " burn " phenomenon not easily occurs, comparatively safe.The bidirectional demand of comprehensive production efficiency and product performance, oxidization time design was at 45 ~ 50 minutes, and current density controls at 1.8 ~ 2.0A/dm
2, can prepare under this parameter meet customer requirement thickness at 17 ~ 22 microns of true qualities anode oxide films.
table 3for oxidization time under present invention process and thickness relation therebetween.
table 3
In described step (8) high temperature hole sealing operation, working concentration is the mistake acid nickel hole sealing agent of 7 ~ 10g/l, temperature 92 ~ 98 DEG C, and the treatment time is 20 ~ 30 minutes; PH value controls between 5.8 ~ 6.5, and acidity is crossed strong or alkaline mistake and is all unfavorable for sealing of hole effect by force; Solution need filter and in use through row circulation stirring, avoid bubble or impurity be attached to product surface cause local non-sealing of hole or sealing of hole bad.After this high temperature hole sealing process, again through row subzero treatment (normal temperature passivated namely in present invention process), combine this sequencing cannot put upside down, the sequencing of this combination hole-sealing technology has sealing of hole performance generation great effect, if high temperature after first low temperature, then the temperature resistance of oxide film is still poor; And if first low-temperature passivation, passive film will play the water and sealing of hole effect that hinder high temperature nickel acetate, thus reduce sealing of hole effect.
In described step (11) normal temperature passivated operation, working concentration is 10 ~ 13% trivalent chromium passivation treatment agents, temperature 30 ~ 40 DEG C, the treatment time: 7 ~ 10 minutes, and solution needs pure water to prepare also in use circulating filtration.Described passivation treating agent need be prepared with pure water, using the pH value of the last washing together before this passivation treating agent between 3.5 ~ 4.5, in order to avoid excessive on the pH impact of tank liquor; After passivation, should with 60 ~ 70 DEG C of bakings 10 ~ 20 minutes for improving effect further.Passivation adopts the mode of soaking, and the higher then soak time of concentration is shorter, and the higher then soak time of temperature is shorter.But the long product surface of passivation time can produce lime, affects passivation quality and outward appearance; And treatment time due to correspondence during passivator excessive concentration is too short, be often difficult to management and control in volume production process, and the high density short period of time also easily causes local passivation bad phenomenon; Present invention process has drawn best passivator concentration and Passivation Treatment time through lot of experiment validation, and best passivation temperature is 30 ~ 40 DEG C.
table 4list under optimum temps, the relation in passivating solution concentration and treatment time.
table 4
The present invention proposes a kind of aluminium alloy true qualities anodic oxidation treatment technique, thickness, at 17 ~ 22 microns, has excellent solidity to corrosion and high and low temperature resistance.Due to process simplification, especially pretreatment procedure have employed " triple effect unification " atomization process, thus substantially reduce CT Cycle Time, simultaneously owing to simplifying the pretreatment procedure such as degreasing, chemical rightenning, because of but a kind of environmental protection friendly technique, stop the discharge of high pollution " phosphorus ", also decrease a large amount of blowdown processing cost to enterprise.
The concrete superiority of present invention process is as follows:
1, simplify pre-treating technology flow process, eliminated degreasing process, optimized alkaline etching operation, abandoned to change and throw operation; Thus shorten the cycle of whole processing procedure, enhance productivity.
2, because pre-treatment simplifies, thus omit grease-removing agent, change throwing agent (main component is phosphoric acid+sulfuric acid) use, eliminate the use of a large amount of chemical industry medicament, for enterprise reduces material cost.Particularly change the omission of throwing operation, sewage discharge cost is declined to a great extent, becomes a kind of environmental protection friendly technique.
3, the relatively traditional A technique of present invention process, decreases 4 road washings, relative to traditional B technique, decreases 9 road washings; Save water consumption and decreased sewage discharge amount;
4, the anode oxide film prepared of present invention process, is a kind of anode oxide film having temperature resistance and resisting salt fog corrosion dual property concurrently, has captured the deficiency that traditional technology can only meet single performance;
5, the anode oxide film prepared of present invention process, enhances properties of oxide-film, can meet NSS and test 1000 ~ 1200H, or resistance to CASS tests 80 ~ 120H; And the high/low temperature instruction ring test in more than 10 cycles of Guangzhou Honda standard can be met simultaneously.
Be only preferred embodiment of the present invention in sum, be not used for limiting practical range of the present invention.Namely all equivalences done according to the content of the present patent application the scope of the claims change and modify, and all should be technology category of the present invention.
Claims (8)
1. a high/low temperature combined type anodic oxidation method for sealing, is characterized in that, comprises the steps: (1) material loading; (2) be atomized; (3) second order washing; (4) bright dipping; (5) three rank washings; (6) anodic oxidation; (7) three rank washings; (8) high temperature hole sealing; (9) second order washing; (10) weak acid pure water is washed; (11) normal temperature passivated; (12) three rank washings; (13) dry; (14) blanking.
2. method according to claim 1, is characterized in that, the propellant composition of step (2) described atomization is SODIUMNITRATE and sodium hydroxide, and wherein, the mass ratio of SODIUMNITRATE and sodium hydroxide is 2:1 ~ 2.5:1.
3. method according to claim 1, is characterized in that, in the described anodic oxidation operation of step (6), working concentration is the H of 180 ~ 200g/l
2sO
4, temperature 18 ~ 21 DEG C, current density 1.8 ~ 2A/dm
2, oxidization time was at 45 ~ 50 minutes, and oxide thickness controls at 17 ~ 22 μm.
4. method according to claim 1, is characterized in that, in the described high temperature hole sealing operation of step (8), working concentration is the nickel acetate hole sealing agent of 7 ~ 10g/l, temperature 92 ~ 98 DEG C, and the treatment time is 20 ~ 30 minutes; Solution carries out circulation stirring and filters.
5. method according to claim 1, is characterized in that, the pH value of the pure washing step of step (10) described weak acid is 3.5 ~ 4.5.
6. method according to claim 1, is characterized in that, in the described normal temperature passivated operation of step (11), working concentration is 10 ~ 13% trivalent chromium passivation treatment agents, temperature is 30 ~ 40 DEG C, and the treatment time is 7 ~ 10 minutes, and solution pure water prepares also in use circulating filtration.
7. method according to claim 1, it is characterized in that, in step (3), (5), (7), (9), (12) described washing step, washing water is ordinary tap water, wherein the last washing together of three rank washings is washing, pure water conductivity requires to be not more than 10us/cm, and all washing times are 30 ~ 60 seconds.
8. method according to claim 1, is characterized in that, the temperature requirement in step (13) described baking operation is 60 ~ 70 DEG C, and drying time controls at 10 ~ 20min.
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| CN106367791A (en) * | 2016-11-11 | 2017-02-01 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | Alkaline three-in-one grinding process capable of integrating pretreatment of aluminum with on-line recycle of aluminum hydroxide |
| CN106367792A (en) * | 2016-11-11 | 2017-02-01 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | Aluminum pretreatment alkaline three-in-one online recycling system for demolding alkaline liquor for extruding mold aluminum material heads and aluminum hydroxide |
| CN106757268A (en) * | 2016-11-11 | 2017-05-31 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | The aluminium pre-treatment three-in-one and alkali liquid regeneration of alkalescence and aluminium hydroxide online recycling technique |
| CN108796580A (en) * | 2018-08-20 | 2018-11-13 | 永臻科技（常州）有限公司 | A kind of aluminium alloy photovoltaic proximate matter anode oxide film new sealing method |
| CN109735836A (en) * | 2019-03-27 | 2019-05-10 | 珠海市玛斯特恒新铝合金加工有限公司 | The corrosion resistance technique of aluminium alloy after a kind of oxidation |
| CN113151877A (en) * | 2021-04-25 | 2021-07-23 | 攀钢集团研究院有限公司 | Preparation method of wear-resistant titanium alloy micro-arc oxidation coating |
| CN117655443A (en) * | 2023-10-07 | 2024-03-08 | 湖北秀山智能科技有限公司 | Radiator core with passivation layer, preparation method of radiator core and radiator |
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| CN106367791A (en) * | 2016-11-11 | 2017-02-01 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | Alkaline three-in-one grinding process capable of integrating pretreatment of aluminum with on-line recycle of aluminum hydroxide |
| CN106367792A (en) * | 2016-11-11 | 2017-02-01 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | Aluminum pretreatment alkaline three-in-one online recycling system for demolding alkaline liquor for extruding mold aluminum material heads and aluminum hydroxide |
| CN106757268A (en) * | 2016-11-11 | 2017-05-31 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | The aluminium pre-treatment three-in-one and alkali liquid regeneration of alkalescence and aluminium hydroxide online recycling technique |
| CN106367791B (en) * | 2016-11-11 | 2018-10-02 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | Aluminium pre-treatment and aluminium hydroxide online recycling and the three-in-one frosting technology of alkalinity |
| CN108796580A (en) * | 2018-08-20 | 2018-11-13 | 永臻科技（常州）有限公司 | A kind of aluminium alloy photovoltaic proximate matter anode oxide film new sealing method |
| CN109735836A (en) * | 2019-03-27 | 2019-05-10 | 珠海市玛斯特恒新铝合金加工有限公司 | The corrosion resistance technique of aluminium alloy after a kind of oxidation |
| CN113151877A (en) * | 2021-04-25 | 2021-07-23 | 攀钢集团研究院有限公司 | Preparation method of wear-resistant titanium alloy micro-arc oxidation coating |
| CN113151877B (en) * | 2021-04-25 | 2022-03-22 | 攀钢集团研究院有限公司 | Preparation method of wear-resistant titanium alloy micro-arc oxidation coating |
| CN117655443A (en) * | 2023-10-07 | 2024-03-08 | 湖北秀山智能科技有限公司 | Radiator core with passivation layer, preparation method of radiator core and radiator |
| CN117655443B (en) * | 2023-10-07 | 2024-05-14 | 湖北秀山智能科技有限公司 | Radiator core with passivation layer, preparation method of radiator core and radiator |
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