CN107142471A - Prepare the corrosion-resistant and anti-light oxidation solution and method for penetrating composite membrane of Mg alloy surface - Google Patents
Prepare the corrosion-resistant and anti-light oxidation solution and method for penetrating composite membrane of Mg alloy surface Download PDFInfo
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- CN107142471A CN107142471A CN201710316455.8A CN201710316455A CN107142471A CN 107142471 A CN107142471 A CN 107142471A CN 201710316455 A CN201710316455 A CN 201710316455A CN 107142471 A CN107142471 A CN 107142471A
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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
- C23C22/24—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 hexavalent chromium compounds
- C23C22/26—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 hexavalent chromium compounds containing also organic compounds
-
- 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
- C23C22/73—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 characterised by the process
Abstract
The corrosion-resistant and anti-light oxidation solution and method for penetrating composite membrane of Mg alloy surface is prepared the present invention relates to a kind of.The oxidation solution includes chromate, sulfate, vanadate, adjacent benzene alkyl salt, wherein, the concentration of chromate is 7 350g/L, and the concentration of sulfate is 2.2 22.5g/L, and the concentration of vanadate is 0.5 3.5g/L, the 28g/L of concentration 0.9 of adjacent benzene alkyl salt.The oxidation solution and preparation method film forming efficiency of the present invention is high, and prepared composite film thickness is uniform, quality is high, and corrosion resistance performance is good；Preparation cost is low, and oxidation solution, degreaser are formed by conventional commercial preparation of reagents, without using rare earths material and precious metal raw material；In addition, safe and environment-friendly, oxidation solution is without extremely toxic substances such as cyanides, and effect on environment is small.
Description
Technical field
The invention belongs to Magnesiumalloy surface modifying field, be related to it is a kind of prepared containing heavy metal in Mg alloy surface it is corrosion-resistant
With the anti-light chemical oxidation liquid for penetrating composite membrane, using the oxidation solution Mg alloy surface is prepared the invention further relates to one kind corrosion-resistant multiple
The method for closing film.
Background technology
Magnesium alloy is most light commercial metal structural material, and the density for commonly using magnesium alloy is about the 2/3 of aluminium alloy, steel
1/4.Compared with other structural metallic materials, magnesium alloy has specific strength, specific stiffness height, damping property, electromagnetic shielding and radioresistance
The advantages of ability is strong, Cutting free is processed, easily reclaimed, has important in fields such as automobile, electronics, electrical equipment, traffic, Aero-Space
Application value and wide application prospect.But magnesium alloy electrode potential is relatively low (about -2.34KV), easily in various media
Corrosion, significantly limit the popularization and application of magnesium alloy；Therefore, it is necessary to carry out proper treatment to improve the corrosion-resistant of magnesium alloy
Space flight and aviation performance is penetrated with anti-light.
In the technology of numerous raising Mg alloy surface decay resistances, chemical conversion less investment, yield is high, easy to operate
Advantage, obtained space flight and aviation and be widely applied.But the main stream approach of chemical conversion treatment is with common greyish white at present
Color and milky are passivated and ceramic coating is major technique, and the product surface after processing is to be mostly used in civilian goods field,
Belong to the use product that space flight and aviation is strictly limited, with the raising of defense technology application standard, original transformation membrane process will be by
Step is banned.
In view of this, it is necessary to which can be corrosion-resistant and chemical conversion treatment solution and corresponding chemistry anti-light can be penetrated by developing one kind
Convert film-forming process.
The content of the invention
In view of this, the corrosion-resistant and anti-light composite membrane penetrated of Mg alloy surface is prepared it is an object of the invention to provide a kind of
High efficiency oxidation solution, the present invention is also provided a kind of prepares the corrosion-resistant and anti-light composite membrane of penetrating of Mg alloy surface using the oxidation solution
Method.
To reach above-mentioned purpose, the technical solution adopted by the present invention is as follows：It is corrosion-resistant and anti-that one kind prepares Mg alloy surface
Light penetrates the oxidation solution of composite membrane, and the oxidation solution includes chromate, sulfate, vanadate, adjacent benzene alkyl salt, wherein, chromate
Concentration be 7-350g/L, the concentration of sulfate is 2.2-22.5g/L, and the concentration of vanadate is 0.5-3.5g/L, adjacent benzene alkyl
The concentration 0.9-28g/L of salt.
Further, the concentration of the chromate is 40-250g/L, and the concentration of sulfate is 10-20g/L, vanadate
Concentration is 1-3g/L, and the concentration of adjacent benzene alkyl salt is 5-15g/L.
Further, described chromate is the one or more in alkali metal salt, alkali salt, ammonium salt.
Preferably, the chromate is the one or more in potassium bichromate, sodium dichromate, ammonium dichromate.
Further, the sulfate is one or both of magnesium sulfate, manganese sulfate.
Further, the vanadate is the one or more in alkali metal salt, alkali salt, ammonium salt.
Preferably, the vanadate is the one or more in ammonium metavanadate, potassium metavanadate, sodium metavanadate.
Further, the adjacent benzene alkyl salt is one or both of alkali metal salt, alkali salt.
Preferably, the alkyl in the adjacent benzene alkyl salt is methyl, ethyl, propyl group, the one or more of butyl.
Preferably, the adjacent benzene alkyl salt is toluene sulfonic acide potassium, Sodium Toluene Sulphonate, ethyl phenenyl azochlorosulfonate acid potassium, ethylo benzene
One or more in sodium sulfonate.
The oxidation solution of the present invention is made up of organic salt and inorganic salts, without cyanide and fluorine ion, with fast filming and
Film hardness and it is corrosion-resistant the advantages of, environmental pollution is small；In addition, the oxidation solution of the present invention is free of rare earth or noble metal, former material
Expect that cost is low.
In the present invention, the corrosion-resistant and anti-light method for penetrating composite membrane of Mg alloy surface is prepared using above-mentioned oxidation solution, including
Following steps：
（1）Magnesium alloy is placed in degreaser, ungrease treatment is carried out；
（2）Magnesium alloy after ungrease treatment is placed in oxidation solution, the oxidation processes 10-30min under the conditions of 90-110 DEG C.
Further, step（1）Middle degreaser includes carbonate, phosphate, inorganic inhibitor and wetting agent, wherein, carbon
The concentration of hydrochlorate is 0.5-37g/L, and phosphatic concentration is 5-50g/L, and the concentration of silicate is 0.5-15g/L, inorganic inhibition
The concentration of agent is 1-3g/L, and the concentration of wetting agent is 1-3g/L.
In the present invention, the method for preparing the corrosion-resistant composite membrane of Mg alloy surface is strict from used in degreasing and oxidation step
Solution, excellent corrosion-resistant and anti-light of indices can be finally made and penetrates composite membrane, the neutral salt spray detection level of the film can
Up to more than 48h/9 grades.
Wherein, step（1）The middle ungrease treatment time is 2-10min, and temperature is 55-70 DEG C.
Further, step（2）Middle oxidation treatment time is 15-25min, and temperature is 95-110 DEG C.
Preferably, the preparation method also includes water-washing step, and the magnesium alloy after ungrease treatment or chemical oxidation treatment is entered
After water-filling is washed, subsequent processing is carried out.
Preferably, the preparation method also includes being located at step（2）Drying steps afterwards, are closed to the magnesium after chemical oxidation treatment
Processing is dried in gold, wherein, drying temperature is 80-120 DEG C, and drying time is 20-40min.
The Reasonable Regulation And Control that the present invention passes through the technological parameter to degreasing, oxidation and drying steps, it is to avoid because misoperation
The problems such as caused oxide layer too high in resistance, chemical salt fog rank difference, for obtaining the corrosion-resistant of high-quality in Mg alloy surface
Play an important roll with anti-light composite membrane of penetrating.
The present invention is relative to prior art, with following advantageous effects：
（1）Film forming efficiency is high, and prepared composite film thickness is uniform, quality is high, and corrosion resistance performance is good；
（2）Prepare that cost is low, oxidation solution, degreaser are formed by conventional commercial preparation of reagents, without using rare earths material and expensive
Raw metal；
（3）Safe and environment-friendly, oxidation solution is without extremely toxic substances such as cyanides, and effect on environment is small.
Embodiment
The preferred embodiments of the present invention will be described in detail below.
Following examples, which will be disclosed, a kind of prepares the corrosion-resistant and anti-light oxidation solution for penetrating composite membrane of Mg alloy surface, the oxygen
Change in liquid, the concentration of chromate is 7-350g/L, and the concentration of sulfate is 2.2-22.5g/L, and the concentration of vanadate is 0.5-
3.5g/L, the concentration of adjacent benzene alkyl salt is 0.9-28g/L.Particularly, the concentration of chromate is 7-50g/L, and sulfate is
2.2-22.5g/L, vanadate is 0.5-3.5g/L；Adjacent benzene alkyl salt 0.9-28g/L.
The appearance detecting method of following examples is ocular estimate/photometer, and described adhesion force test method is cross-cut methods,
Neutral salt spray test method is GJB150.11A-2009.
Embodiment 1
The present embodiment prepares the corrosion-resistant and anti-light method for penetrating composite membrane of Mg alloy surface, comprises the following steps successively：
(1) degreasing：In degreaser used in defatting step, carbonate concentration is 35g/L, and phosphate concn is 43g/L, and silicate is dense
Spend for 10g/, the concentration of inorganic inhibitor and wetting agent is 2g/L；In the present embodiment, the defatting step time is 5min, temperature
For 63 DEG C；
(2) aoxidize：Chemical oxidation is carried out to the magnesium alloy after degreasing：Wherein, in oxidation solution used, the concentration of potassium bichromate is
43g/L, the concentration of magnesium sulfate is 21g/L, and the concentration of ammonium metavanadate is 3g/L；The concentration of o-methyl-benzene sodium sulfonate is 10g/L；This
The embodiment oxidation step time is 10min, and temperature is 110 DEG C；
(3) dry：Magnesium alloy in the environment of ventilation after drying oxidation, the present embodiment drying temperature is 110 DEG C, and the time is
30min。
It should be noted that including water-washing step in the present embodiment before oxidation, drying steps, to avoid previous step
Influence of the impurity to next step.
Embodiment 2
The present embodiment prepares the corrosion-resistant and anti-light method for penetrating composite membrane of Mg alloy surface, comprises the following steps successively：
(1) degreasing：In degreaser used in the present embodiment defatting step, carbonate concentration is 35g/L, and phosphate concn is 43g/L,
Silicate concentration is 10g/ L, and the concentration of inorganic inhibitor and wetting agent is 2g/L；In the present embodiment, the defatting step time is
5min, temperature is 63 DEG C；
(2) aoxidize：Chemical oxidation is carried out to the magnesium alloy after degreasing：Potassium bichromate concentration is in oxidation solution used in the present embodiment
9g/L, magnesium sulfate concentration is 15g/L, and ammonium metavanadate salinity is 2g/L；O-methyl-benzene sulfonic acid na concn is 20g/L；This implementation
The example oxidation step time is 25min, and temperature is 110 DEG C.
(3) dry：Magnesium alloy in the environment of ventilation after drying oxidation, the present embodiment drying temperature is 120 DEG C, time
For 30min.
It should be noted that including water-washing step in the present embodiment before degreasing, oxidation, drying steps, it is to avoid upper one
Influence of the impurity of step to next step.
Embodiment 3
The present embodiment prepares the corrosion-resistant compound and anti-light method for penetrating film of Mg alloy surface, comprises the following steps successively：
(1) degreasing：In degreaser used in this implementation defatting step, carbonate concentration is 35g/L, and phosphate concn is 43g/L, silicon
Hydrochlorate concentration is 10g/, and the concentration of inorganic inhibitor and wetting agent is 2g/L；In the present embodiment, the defatting step time is
5min, temperature is 63 DEG C；
(2) aoxidize：Chemical oxidation is carried out to the magnesium alloy after degreasing：In oxidation solution used in the present embodiment, the concentration of sodium dichromate
For 23/L, the concentration of magnesium sulfate is 11g/L, and the concentration of ammonium metavanadate is 1.5g/L；The concentration of o-methyl-benzene sodium sulfonate is 9g/L；
The present embodiment oxidation step time is 30min, and temperature is 110 DEG C；
(3) dry：Magnesium alloy in the environment of ventilation after drying oxidation, the present embodiment drying temperature is 120 DEG C, and the time is
30min。
It should be noted that in the present embodiment, water-washing step is included before degreasing, oxidation, drying steps, on avoiding
Influence of the impurity of one step to next step.
Embodiment 4
The present embodiment prepares the corrosion-resistant and anti-light method for penetrating composite membrane of Mg alloy surface, comprises the following steps successively：
(1) degreasing：Degreaser carbonate containing concentration used in this implementation defatting step is 35g/L, and phosphate concn is 43g/L, silicon
Hydrochlorate concentration is 10g/, and the concentration of inorganic inhibitor and wetting agent is 2g/L；In the present embodiment, the defatting step time is
5min, temperature is 63 DEG C；
(2) aoxidize：Chemical oxidation is carried out to the magnesium alloy after degreasing：In oxidation solution used in the present embodiment, chromic acid potassium concn is
25g/L, magnesium sulfate concentration is 11g/L, and sodium metavanadate concentration is 2.5g/L, and o-methyl-benzene sulfonic acid na concn is 15g/L；This implementation
The example oxidation step time is 25min, and temperature is 110 DEG C；
(3) dry：Magnesium alloy in the environment of ventilation after drying oxidation, the present embodiment drying temperature is 120 DEG C, and the time is
30min。
It should be noted that in the present embodiment, water-washing step is included before degreasing, oxidation, drying steps, it is to avoid upper one
Influence of the impurity of step to next step.
Comparative example 1
This comparative example prepares the corrosion-resistant and anti-light method for penetrating composite membrane of Mg alloy surface, comprises the following steps successively：
(1) degreasing：Degreaser carbonate containing concentration used in this implementation defatting step is 35g/L, and phosphate concn is 43g/L, silicon
Hydrochlorate concentration is 10g/, and the concentration of inorganic inhibitor and wetting agent is 2g/L；In the present embodiment, the defatting step time is 5min,
Temperature is 63 DEG C；
(2) aoxidize：Chemical oxidation is carried out to the magnesium alloy after degreasing：In oxidation solution used in this comparative example, potassium bichromate concentration is
43g/L, magnesium sulfate concentration is 21g/L；This comparative example oxidation step time is 10min, and temperature is 110 DEG C.
(3) dry：Magnesium alloy in the environment of ventilation after drying oxidation, this comparative example drying temperature is 110 DEG C, time
For 30min.
It should be noted that including water-washing step in this comparative example before oxidation, drying steps, it is to avoid previous step
Influence of the impurity to next step.
Comparative example 2
This comparative example prepares the corrosion-resistant and anti-light method for penetrating composite membrane of Mg alloy surface, comprises the following steps successively：
(1) degreasing：In degreaser used in this comparative example defatting step, carbonate concentration is 35g/L, and phosphate concn is 43g/L,
Silicate concentration is 10g/, and the concentration of inorganic inhibitor and wetting agent is 2g/L；In the present embodiment, the defatting step time is
5min, temperature is 63 DEG C；
(2) aoxidize：Chemical oxidation is carried out to the magnesium alloy after degreasing：In oxidation solution used in the present embodiment, potassium bichromate concentration is
9g/L, magnesium sulfate concentration is 15g/L, and ammonium metavanadate salinity is 0.1g/L, and o-methyl-benzene sulfonic acid na concn is 0.1g/L；This is right
The ratio oxidation step time is 25min, and temperature is 110 DEG C.
(3) dry：Magnesium alloy in the environment of ventilation after drying oxidation, this comparative example drying temperature is 120 DEG C, time
For 30min.
It should be noted that including water-washing step in this comparative example before degreasing, oxidation, drying steps, it is to avoid upper one
Influence of the impurity of step to next step.
Embodiment 1-4 and comparative example 1-2 correlated performance detection result is as shown in table 1.As can be seen from the table, using this
The performance for the composite membrane that the oxidation solution and preparation method of invention are obtained is substantially better than the performance of the composite membrane obtained in comparative example.
Each embodiment of table 1 and comparative example performance test results situation table
| Embodiment | Outward appearance | Film adhesion | Neutral salt spray |
| 1 | Uniform aterrimus | 0 grade | 96 hours corrosion-free points |
| 2 | Uniform aterrimus | 1 grade | 96 hours corrosion-free points |
| 3 | Uniform aterrimus | 0 grade | 96 hours corrosion-free points |
| 4 | Uniform aterrimus | 0 grade | 96 hours corrosion-free points |
| Comparative example 1 | Non-homogeneous light/dark balance | 1 grade | There is hot spot within 96 hours |
| Comparative example 2 | Non-homogeneous light/dark balance | 1 grade | There is hot spot within 96 hours |
The treatment fluid of low concentration, efficient treatment effect are realized, uniformly.
Claims (10)
1. a kind of prepare the corrosion-resistant and anti-light oxidation solution for penetrating composite membrane of Mg alloy surface, it is characterised in that the oxidation solution bag
Containing chromate, sulfate, vanadate, adjacent benzene alkyl salt, wherein, the concentration of chromate is 7-350g/L, and the concentration of sulfate is
2.2-22.5g/L, the concentration of vanadate is 0.5-3.5g/L, the concentration 0.9-28g/L of adjacent benzene alkyl salt.
2. according to claim 1 prepare the corrosion-resistant and anti-light oxidation solution for penetrating composite membrane of Mg alloy surface, its feature exists
In the concentration of the chromate is 40-250g/L, and the concentration of sulfate is 10-20g/L, and the concentration of vanadate is 1-3g/L, adjacent
The concentration of benzene alkyl salt is 5-15g/L.
3. according to claim 1 prepare the corrosion-resistant and anti-light oxidation solution for penetrating composite membrane of Mg alloy surface, its feature exists
In described chromate is the one or more in alkali metal salt, alkali salt, ammonium salt, preferably potassium bichromate, dichromic acid
One or more in sodium, ammonium dichromate.
4. according to claim 1 prepare the corrosion-resistant and anti-light oxidation solution for penetrating composite membrane of Mg alloy surface, its feature exists
In the sulfate is one or both of magnesium sulfate, manganese sulfate.
5. according to claim 1 prepare the corrosion-resistant and anti-light oxidation solution for penetrating composite membrane of Mg alloy surface, its feature exists
In the vanadate is the one or more in alkali metal salt, alkali salt, ammonium salt, preferably ammonium metavanadate, metavanadic acid
One or more in potassium, sodium metavanadate.
6. according to claim 1 prepare the corrosion-resistant and anti-light oxidation solution for penetrating composite membrane of Mg alloy surface, its feature exists
In the adjacent benzene alkyl salt is one or both of alkali metal salt, alkali salt.
7. according to claim 1 prepare the corrosion-resistant and anti-light oxidation solution for penetrating composite membrane of Mg alloy surface, its feature exists
In the alkyl in the adjacent benzene alkyl salt is methyl, ethyl, propyl group, the preferably one or more of butyl, toluene sulfonic acide
One or more in potassium, Sodium Toluene Sulphonate, ethyl phenenyl azochlorosulfonate acid potassium, ethyl phenenyl azochlorosulfonate acid sodium.
It is corrosion-resistant and anti-light penetrate composite membrane that 8. the oxidation solution described in one kind application any one of claim 1 ~ 7 prepares Mg alloy surface
Method, it is characterised in that comprise the following steps：
（1）Magnesium alloy is placed in degreaser, ungrease treatment is carried out；
（2）Magnesium alloy after ungrease treatment is placed in oxidation solution, the oxidation processes 10-30min under the conditions of 90-110 DEG C.
9. according to claim 8 prepare the corrosion-resistant and anti-light method for penetrating composite membrane of Mg alloy surface, it is characterised in that
Step（1）Middle degreaser includes carbonate, phosphate, inorganic inhibitor and wetting agent, wherein, the concentration of carbonate is 0.5-
37g/L, phosphatic concentration is 5-50g/L, and the concentration of silicate is 0.5-15g/L, and the concentration of inorganic inhibitor is 1-3g/L,
The concentration of wetting agent is 1-3g/L.
10. according to claim 8 prepare the corrosion-resistant and anti-light method for penetrating composite membrane of Mg alloy surface, its feature exists
In step（2）Middle oxidation treatment time is 15-25min, and temperature is 95-110 DEG C.
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| CN107715707A (en) * | 2017-10-19 | 2018-02-23 | 谢新昇 | A kind of preparation method of corrosion-resistant type miillpore filter |
| CN110453210A (en) * | 2019-09-06 | 2019-11-15 | 北京星航机电装备有限公司 | A kind of low chromium magnesium alloy chemical oxidation solution and chemical oxidation method |
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