CN105624664A - Hole sealing method for magnesium alloy surface rare earth chemical conversion coating - Google Patents
Hole sealing method for magnesium alloy surface rare earth chemical conversion coating Download PDFInfo
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- CN105624664A CN105624664A CN201610146039.3A CN201610146039A CN105624664A CN 105624664 A CN105624664 A CN 105624664A CN 201610146039 A CN201610146039 A CN 201610146039A CN 105624664 A CN105624664 A CN 105624664A
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- magnesium alloy
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/82—After-treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
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Abstract
The invention discloses a hole sealing method for a magnesium alloy surface rare earth chemical conversion coating. The hole sealing method includes the following steps that firstly, a magnesium alloy is pretreated; secondly, a pretreated magnesium alloy workpiece is soaked in a rare earth chemical conversion coating solution to be soaked for 10 min to 60 min, and the magnesium alloy rare earth chemical conversion coating is obtained; and thirdly; the magnesium alloy workpiece obtained in the second step is soaked in an oxidized graphene supernatant solution with a certain condensation for 20 min to 30 min and is dried at the temperature of 30 DEG C to 60 DEG C for 1 h to 3 h, and the magnesium alloy surface rare earth chemical conversion coating with holes sealed by oxidized graphene is obtained. According to the hole sealing method, the magnesium alloy rare earth conversion coating layer is soaked in the oxidized graphene supernatant solution, the oxidized graphene is soaked in conversion coating microcracks, the compactness of the rare earth conversion coating layer is enhanced, the problems that the crack-like structure of the rare earth conversion coating is generated, the conversion coating is discontinuous and the degree of covering a base body is low are solved, and the corrosion resistance of the magnesium alloy rare earth chemical conversion coating is improved remarkably.
Description
Technical field
The present invention is specifically related to the method for sealing of a kind of magnesium alloy surface rare earth chemical conversion film, belongs to technical field of magnesium alloy surface treatment.
Background technology
Currently, resources and environment has become the matter of utmost importance of human kind sustainable development, and magnesium alloy is as the lightest structural metallic materials, has unique advantage in energy-saving and emission-reduction; In addition high specific tenacity, specific rigidity and the excellent properties such as good heat conduction, damping, electromagnetic shielding, have extremely wide application prospect in fields such as traffic, telecommunications, aerospace, defence and militaries. But, the chemical property of magnesium is active, electropotential very low (-2.37V), and the oxide film PB ratio formed is less than 1, causes magnesium alloy very easily to suffer corrosion failure in applied environment, and corrosion problem seriously constrains exploitation and the widespread use of magnesium alloy.
Improving the magnesium alloy the simplest method of resistance to corrosion is that it is carried out surfacecti proteon process, and chemical conversion treatment is both process for treating surface convenient, economic, effective in current all multi-methods, and can be the substrate that follow-up organic spray-on coating provides good, it is to increase the bonding force between organic spray-on coating and matrix. At present; chemical conversion process the most ripe is chromating; although it is functional and can significantly improve the conversion film of corrosion stability of magnesium alloy to form one layer at Mg alloy surface; but along with people are for the attention of environment protection; environment and people are known from experience cause very big injury owing to wherein being contained this toxic substance of chromium of sexavalence by this kind of method for transformation; therefore its application is very restricted, and the chemical conversion process of thus new green non-pollution is urgently developed. The domestic and international Chrome-free chemical conversion process for magnesium alloy has done a lot of research in recent years, wherein rare-earth conversion coatings becomes a kind of wherein comparatively noticeable method due to environmentally safe, but rare-earth conversion coatings is in typically splitting sheet structure, seriously have impact on the continuity of conversion film, reduce rete to the coverage of matrix, conversion film is loose porous simultaneously, weak with the bonding force of matrix. This kind splits the reason that sheet structure mainly contains two aspects: on the one hand due to chemical property that magnesium alloy is active, evolving hydrogen reaction violent in film process produces a large amount of gas, the attachment of gas in matrix surface and rete defines the loose structure of conversion film and low bonding force, this outer portion bubble has blocked the contact of film-forming soln and matrix in the gathering of matrix surface, reduces the film forming efficiency of conversion film; On the other hand, traditional conversion film adopts water as film forming solvent, in later stage drying process, and conversion film dehydration shrinkage. Upper strata conversion film thickness is relatively large, shrinks and produces mutually through crackle, reduces the continuity of conversion film. Patent [CN102181851A] adopts ethanol to replace water to prepare rare earth Cerium conversion film as film forming solvent, effectively prevent the cracking that the too fast and dry dehydration of reaction causes, but film formation time extends, and reduces the film forming efficiency of conversion film. Patent [CN101113518A] adopts water glass, sweet casein to carry out the crackle of method shutoff rare-earth conversion coatings of sealing of hole, it is to increase the corrosion resisting property of rare-earth conversion coatings, but effect is not obvious.
Therefore, existing magnesium alloy surface rare earth chemical conversion membrane technology is further improved.
Summary of the invention
It is an object of the invention to provide the method for sealing of a kind of magnesium alloy surface rare earth chemical conversion film, solve above-mentioned rare-earth conversion coatings and split sheet structure, conversion film discontinuity, the problem that the coverage of matrix is low.
For achieving the above object, the technical scheme of the present invention is:
The method for sealing of a kind of magnesium alloy surface rare earth chemical conversion film of the present invention, comprises the steps:
(1) magnesium alloy pre-treatment
A. sanding and polishing: adopt the sand paper of different model and polishing machine that magnesium alloy workpiece is carried out sanding and polishing;
B. degreasing: magnesium alloy workpiece is placed in acetone soln supersound process 10-30 minute, power 200-1000W;
C. deionization washing: being soaked in deionized water 10-30 minute by the magnesium alloy workpiece through skimming treatment, hot blast drying is for subsequent use;
D. acidifying: the magnesium alloy workpiece washed through deionization is soaked 1-5 minute in hydrofluoric acid, it is intended that strengthen rare-earth conversion coatings and basal body binding force;
E. deionization washing: being soaked in deionized water 10-30 minute by acidified magnesium alloy workpiece, hot blast drying is for subsequent use;
(2) magnesium alloy pre-treated workpiece step (1) obtained immerses in rare earth chemistry conversion film solution and soaks 10-60 minute, makes magnesium alloy work-piece surface obtain magnesium alloy rare-earth chemical conversion film;
(3) magnesium alloy workpiece that step (2) obtains is immersed in certain density graphene oxide aaerosol solution 20-30 minute, at temperature 30-60 DEG C, drying 1-3 hour, makes magnesium alloy work-piece surface obtain the magnesium alloy surface rare earth chemical conversion film of graphene oxide sealing of hole.
Preferably, described magnesium alloy is AZ91D magnesium alloy.
Preferably, the rare earth chemistry conversion film solution described in described step (2) is that 10-30g/L rare earth nitrate, 5-30g/L Sodium Fluoride, 1-10g/L citric acid form by concentration.
Preferably, the rare earth nitrate in described step (2) is the one in cerous nitrate, Yttrium trinitrate, samaric nitrate.
Preferably, the concentration of the graphene oxide in described step (3) is 1-5mg/L.
The useful effect of the present invention is, magnesium alloy rare-earth conversion coatings layer is immersed in graphene oxide suspension by the present invention, and graphene oxide immerses in rare-earth conversion coatings tiny crack, enhances the compactness of rare-earth conversion coatings layer. Preparation technology of the present invention is simple, and cost value is cheap, is suitable for the device of different shapes; And can significantly improving corrosion resistance of magnesium alloy energy, compared with the rare-earth conversion coatings of non-sealing of hole, the corrosion current density of rare-earth conversion coatings soaking sealing pores through graphene oxide declines more than two orders of magnitude.
Accompanying drawing explanation
Fig. 1 is the magnesium alloy surface rare earth chemical conversion film shape appearance figure of non-sealing of hole in the embodiment of the present invention 3;
Fig. 2 is magnesium alloy surface rare earth chemical conversion film shape appearance figure after graphene oxide sealing of hole in the embodiment of the present invention 3.
Embodiment
Below in conjunction with accompanying drawing and concrete embodiment, the present invention is described in further details.
Embodiment 1:
Pre-treatment: magnesium alloy workpiece is carried out sanding and polishing and is placed in acetone soln supersound process 10 minutes, power 200-1000W; Then the magnesium alloy workpiece obtained being soaked 10 minutes in deionized water, hot blast drying is for subsequent use; Again the magnesium alloy workpiece washed through deionization is soaked 1 minute in hydrofluoric acid, it is intended that strengthen rare-earth conversion coatings and basal body binding force; Finally acidified magnesium alloy workpiece being soaked 10 minutes in deionized water, hot blast drying is for subsequent use.
It is immersion 10 minutes in the rare earth chemistry conversion film solution that form of 10g/L cerous nitrate, 5g/L Sodium Fluoride, 1g/L citric acid that the magnesium alloy pre-treated workpiece that pre-treatment obtained immerses by concentration, obtains magnesium alloy rare-earth chemical conversion film;
Finally by the graphene oxide aaerosol solution of the magnesium alloy workpiece immersion 1mg/L obtained 20 minutes, drying 1 hour at temperature about 30 DEG C, obtain the magnesium alloy surface rare earth chemical conversion film of graphene oxide sealing of hole, electro-chemical test shows, the corrosion electric current density of alloy is than reduction by more than 2 orders of magnitude without graphene oxide sealing pores.
Embodiment 2:
Pre-treatment: magnesium alloy workpiece is carried out sanding and polishing and is placed in acetone soln supersound process 30 minutes, power 200-1000W; Then the magnesium alloy workpiece obtained being soaked 30 minutes in deionized water, hot blast drying is for subsequent use; Again the magnesium alloy workpiece washed through deionization is soaked 5 minutes in hydrofluoric acid, it is intended that strengthen rare-earth conversion coatings and basal body binding force; Finally acidified magnesium alloy workpiece being soaked 30 minutes in deionized water, hot blast drying is for subsequent use.
It is immersion 60 minutes in the rare earth chemistry conversion film solution that form of 30g/L cerous nitrate, 30g/L Sodium Fluoride, 5g/L citric acid that the magnesium alloy pre-treated workpiece that pre-treatment obtained immerses by concentration, obtains magnesium alloy rare-earth chemical conversion film;
Finally by the graphene oxide aaerosol solution of the magnesium alloy workpiece immersion 5mg/L obtained 30 minutes, drying 3 hours at temperature about 60 DEG C, obtain the magnesium alloy surface rare earth chemical conversion film of graphene oxide sealing of hole, electro-chemical test shows, the corrosion electric current density of alloy with compared with graphene oxide sealing pores, reduce 2 orders of magnitude.
Embodiment 3:
Pre-treatment: magnesium alloy workpiece is carried out sanding and polishing and is placed in acetone soln supersound process 20 minutes, power 200-1000W; Then the magnesium alloy workpiece obtained being soaked 20 minutes in deionized water, hot blast drying is for subsequent use; Again the magnesium alloy workpiece washed through deionization is soaked 3 minutes in hydrofluoric acid, it is intended that strengthen rare-earth conversion coatings and basal body binding force; Finally acidified magnesium alloy workpiece being soaked 20 minutes in deionized water, hot blast drying is for subsequent use.
It is immersion 20 minutes in the rare earth chemistry conversion film solution that form of 20g/L cerous nitrate, 18g/L Sodium Fluoride, 3g/L citric acid that the magnesium alloy pre-treated workpiece that pre-treatment obtained immerses by concentration, obtains the magnesium alloy rare-earth chemical conversion film shown in Fig. 1;
Finally by the graphene oxide aaerosol solution of the magnesium alloy workpiece immersion 3mg/L obtained 25 minutes, drying 2 hours at temperature about 45 DEG C, obtain the magnesium alloy surface rare earth chemical conversion film of the graphene oxide sealing of hole shown in Fig. 2, electro-chemical test shows, the corrosion electric current density of alloy is than reduction by 3 orders of magnitude without graphene oxide sealing pores.
As known by the technical knowledge, the present invention can be realized by other the embodiment not departing from its spirit or essential feature. Therefore, above-mentioned disclosed embodiment, with regard to each side, is all illustrate, is not only. Within the scope of the present invention all or in the scope being equal to the present invention change is all comprised by the present invention.
Claims (5)
1. the method for a magnesium alloy surface rare earth chemical conversion film sealing of hole, it is characterised in that, comprise the steps:
(1) magnesium alloy pre-treatment
A. sanding and polishing: adopt the sand paper of different model and polishing machine that magnesium alloy workpiece is carried out sanding and polishing;
B. degreasing: magnesium alloy workpiece is placed in acetone soln supersound process 10-30 minute, power 200-1000W;
C. deionization washing: being soaked in deionized water 10-30 minute by the magnesium alloy workpiece through skimming treatment, hot blast drying is for subsequent use;
D. acidifying: the magnesium alloy workpiece washed through deionization is soaked 1-5 minute in hydrofluoric acid, it is intended that strengthen rare-earth conversion coatings and basal body binding force;
E. deionization washing: being soaked in deionized water 10-30 minute by acidified magnesium alloy workpiece, hot blast drying is for subsequent use;
(2) magnesium alloy pre-treated workpiece step (1) obtained immerses in rare earth chemistry conversion film solution and soaks 10-60 minute, makes magnesium alloy work-piece surface obtain magnesium alloy rare-earth chemical conversion film;
(3) magnesium alloy workpiece that step (2) obtains is immersed in certain density graphene oxide aaerosol solution 20-30 minute, at temperature 30-60 DEG C, drying 1-3 hour, makes magnesium alloy work-piece surface obtain the magnesium alloy surface rare earth chemical conversion film of graphene oxide sealing of hole.
2. the method for a kind of magnesium alloy surface rare earth chemical conversion film sealing of hole according to claim 1, it is characterised in that, described magnesium alloy is AZ91D magnesium alloy.
3. the method for a kind of magnesium alloy surface rare earth chemical conversion film sealing of hole according to claim 1, it is characterized in that, the rare earth chemistry conversion film solution described in described step (2) is that 10-30g/L rare earth nitrate, 5-30g/L Sodium Fluoride, 1-10g/L citric acid form by concentration.
4. the method for a kind of magnesium alloy surface rare earth chemical conversion film sealing of hole according to claim 3, it is characterised in that, the rare earth nitrate in described step (2) is the one in cerous nitrate, Yttrium trinitrate, samaric nitrate.
5. the method for a kind of magnesium alloy surface rare earth chemical conversion film sealing of hole according to claim 1, it is characterised in that, the concentration of the graphene oxide in described step (3) is 1-5mg/L.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610146039.3A CN105624664A (en) | 2016-03-15 | 2016-03-15 | Hole sealing method for magnesium alloy surface rare earth chemical conversion coating |
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| CN201610146039.3A CN105624664A (en) | 2016-03-15 | 2016-03-15 | Hole sealing method for magnesium alloy surface rare earth chemical conversion coating |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108203821A (en) * | 2018-01-25 | 2018-06-26 | 上海应用技术大学 | A kind of environmentally friendly passivator for adulterating GO, preparation method and applications |
| CN110670054A (en) * | 2019-10-11 | 2020-01-10 | 青海民族大学 | Magnesium alloy surface cerate conversion repair film and preparation method thereof |
| CN113913803A (en) * | 2021-09-28 | 2022-01-11 | 中国人民解放军空军工程大学 | Magnesium alloy chemical conversion composite film and preparation method thereof |
| CN114622195A (en) * | 2022-02-21 | 2022-06-14 | 华鼎国联四川动力电池有限公司 | Method for passivating zinc matrix |
Citations (3)
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| CN101113518A (en) * | 2006-07-28 | 2008-01-30 | 佛山市顺德区汉达精密电子科技有限公司 | Magnesium alloy surface rare earth treatment technique |
| CN101560658A (en) * | 2009-05-26 | 2009-10-21 | 哈尔滨工业大学 | Early pre-treatment process for rare earth converting film formed on surfaces of light metal and composite material of light metal |
| CN104878377A (en) * | 2015-05-20 | 2015-09-02 | 哈尔滨工业大学 | Method for preparing graphene oxide and micro-arc oxidized ceramic composite coating on surface of magnesium alloy |
-
2016
- 2016-03-15 CN CN201610146039.3A patent/CN105624664A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113518A (en) * | 2006-07-28 | 2008-01-30 | 佛山市顺德区汉达精密电子科技有限公司 | Magnesium alloy surface rare earth treatment technique |
| CN101560658A (en) * | 2009-05-26 | 2009-10-21 | 哈尔滨工业大学 | Early pre-treatment process for rare earth converting film formed on surfaces of light metal and composite material of light metal |
| CN104878377A (en) * | 2015-05-20 | 2015-09-02 | 哈尔滨工业大学 | Method for preparing graphene oxide and micro-arc oxidized ceramic composite coating on surface of magnesium alloy |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108203821A (en) * | 2018-01-25 | 2018-06-26 | 上海应用技术大学 | A kind of environmentally friendly passivator for adulterating GO, preparation method and applications |
| CN110670054A (en) * | 2019-10-11 | 2020-01-10 | 青海民族大学 | Magnesium alloy surface cerate conversion repair film and preparation method thereof |
| CN110670054B (en) * | 2019-10-11 | 2021-06-29 | 青海民族大学 | Magnesium alloy surface cerate conversion repair film and preparation method thereof |
| CN113913803A (en) * | 2021-09-28 | 2022-01-11 | 中国人民解放军空军工程大学 | Magnesium alloy chemical conversion composite film and preparation method thereof |
| CN114622195A (en) * | 2022-02-21 | 2022-06-14 | 华鼎国联四川动力电池有限公司 | Method for passivating zinc matrix |
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