CN106929863A - A kind of method for lifting aluminum alloy surface silane film properties - Google Patents
A kind of method for lifting aluminum alloy surface silane film properties Download PDFInfo
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- CN106929863A CN106929863A CN201710137350.6A CN201710137350A CN106929863A CN 106929863 A CN106929863 A CN 106929863A CN 201710137350 A CN201710137350 A CN 201710137350A CN 106929863 A CN106929863 A CN 106929863A
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- aluminum alloy
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- silane
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F17/00—Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/122—Inorganic polymers, e.g. silanes, polysilazanes, polysiloxanes
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/12—Light metals
- C23G1/125—Light metals aluminium
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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
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
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- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The present invention discloses a kind of method for lifting aluminum alloy surface silane film properties, including following operating procedure：Aluminium alloy stock after polishing is put into cleaning fluid and is cleaned；By weight, after BTESPT silane couplers, ethanol, deionized water, methylpropene sodium sulfonate being mixed, 6 10min are stirred, is prepared into film liquid and completed, mixed solution is then placed on nonventilated place and is hydrolyzed, hydrolysis time is 35 hours；Aluminum alloy materials are put into prepare complete into film liquid, after 2 5min, into 0.03 0.05 times of di (isooctyl) phosphates of weight of film liquid weight are added into film liquid, continue to soak, take out aluminum alloy materials, place it in ventilation standing, finished product.In the present invention, in silane film obtained in aluminum alloy surface, adhesive force is strong, wearability is good, good corrosion resistance, and the uniformity of film is preferable with consistency, can effectively prevent the film on Al-alloy products surface during use by mechanical damage.
Description
Technical field
The invention belongs to aluminium alloy manufacture field, and in particular to a kind of method of lifting aluminum alloy surface silane film properties.
Background technology
Aluminium is one of nonferrous materials that usage amount is maximum, range of application is most wide.But due to the normal electrode electricity of aluminium
The low, chemical property in position is active, difference of hardness, wear no resistance and in corrosive medium the aspect such as corrosion resistance difference shortcoming, largely
On limit the scope of application of aluminum, shorten its service life.Therefore aluminum products are required to by strict using preceding
After surface treatment, can just come into operation.The aluminum alloy surface handling process of safer environmental protection is silanization treatment technology at present.
The general principle of silanization treatment is the reaction and the polycondensation of silane itself of silane and metal surface hydroxide
Reaction.It has been generally acknowledged that the Corrosion Protection of silane film layer is based primarily upon the hydrophobicity of silane film.When the electricity by silanization treatment
When pole is immersed in electrolyte solution, silane film plays a part of barrier layer, can effectively reduce electrolyte, water, oxygen molecule to gold
The speed of category interface zone infiltration.But, aluminium alloy silanization treatment technique also existing defects, be divided into it is following some：（1）Due to
Silane film thicknesses of layers is relatively thin, it is necessary to carry out further safeguard procedures, simply use silane coupler is carried out to aluminum alloy materials
Treatment, its barrier propterty is simultaneously bad, although silane film is well combined with alloy matrix aluminum, but because silane film film layer is relatively thin, because
This its protection effect is limited；（2）The time of silane hydrolyzate is more long, and common silane coupler hydrolysis time is at least 10 hours,
The less stable of hydrolyzate, process deviation is larger；（3）Silane film does not possess self-healing ability, once the silane film of metal surface
After suffering mechanical failure, metal locally just occurs more serious corrosion phenomenon.
The content of the invention
In order to lift the corrosion resistance of aluminium alloy, the present invention is for silane film（1）、（2）Two point defects, there is provided a kind of
The method for lifting aluminum alloy surface silane film properties.
The present invention is achieved by the following technical solutions.
A kind of method for lifting aluminum alloy surface silane film properties, including following operating procedure：
A. aluminum alloy surface cleaning treatment
Aluminium alloy stock after polishing is put into cleaning fluid and is cleaned, wherein cleaning fluid is made up of the component of following weight portion：10%
Hydrochloric acid 10-15 parts, sodium citrate 7-10 parts, sodium phosphate 1-3 parts, water 95-125 parts；
Further, by after cleaning fluid cleaning, using deionized water rinsing aluminum alloy surface, washing time is not less than aluminium alloy stock
5min。
Then the conventional cleaning method of aluminum alloy surface carries out pickling again first to be deoiled with organic solution, so not only can
Cause to waste so that production cost increases, and the serious pollution environment of meeting, the cleaning fluid that the present invention is provided, in the same of pickling
When, with the effect deoiled, cleaning performance is thorough, it is ensured that the film-formation result of silane coupler；
B. it is configured to film liquid
By weight, by 3-6 parts of BTESPT silane couplers, ethanol 28-34 parts, deionized water 19-27 parts, metering system sulphur
After sour sodium 0.1-0.3 parts of mixing, after stirring 6-10min, prepared into film liquid and completed, be then placed on mixed solution nonventilated
Place is hydrolyzed, and hydrolysis time is 3-5 hours, and wherein the initial temperature of deionized water is 55-60 DEG C；
Further, into film liquid by weight, it is made up of the component of following weight portion：4-5 parts of BTESPT silane couplers, ethanol
30-32 parts, deionized water 24-26 parts, methylpropene sodium sulfonate 0.2-0.3 parts.
Preferably, BTESPT silane couplers, by adding ammoniacal liquor or acetic acid, maintain the pH of hydrolyzate in hydrolytic process
It is 4-6.
C. film-forming process
Aluminum alloy materials are put into prepare complete into film liquid, after 2-5min, into adding into film liquid weight 0.03- in film liquid
0.05 times of di (isooctyl) phosphate of weight, after continuing to soak 4-6min, takes out aluminum alloy materials, places it in ventilation standing
After 60-80min, finished product.
Technical scheme more than, the beneficial effects of the invention are as follows：
In the present invention, in silane film obtained in aluminum alloy surface, adhesive force is strong, wearability is good, good corrosion resistance, the thickness of silane film
Degree can reach about 650nm, and the uniformity of film is preferable with consistency, can effectively prevent Al-alloy products in the process for using
The film on middle surface is by mechanical damage.The present invention adds a small amount of metering system by BTESPT silane coupler hydrolysing steps
Sodium sulfonate, effectively accelerates the speed of hydrolysis, after 3 hours, at the beginning of the electrical conductivity of hydrolysis is 1300Ms/cm or so, hydrolyzate
Beginning electrical conductivity is 360Ms/cm or so, it was demonstrated that the addition of methylpropene sodium sulfonate, effectively accelerates BTESPT silane couplers
Hydrolysis rate, overcome in background technology in silane membrane technology（1）Point defect；The present invention by immersion process,
The a small amount of di (isooctyl) phosphate of addition, effectively improves deposition of the silane film in aluminum alloy surface, and then effective lifting
The thickness of silane film so that its thickness can reach 650nm or so, and film compactness with the uniformity preferably, can have for a long time
The aluminum alloy surface of protecting of effect is not corroded.
Specific embodiment
In order that those skilled in the art can be further understood that feature of the invention and technology contents, referring to following has
Close detailed description of the invention.
Embodiment 1
A kind of method for lifting aluminum alloy surface silane film properties, including following operating procedure：
A. aluminum alloy surface cleaning treatment
Aluminium alloy stock after polishing is put into cleaning fluid and is cleaned, wherein cleaning fluid is made up of the component of following weight portion：10%
10 parts of hydrochloric acid, 7 parts of sodium citrate, 1 part of sodium phosphate, 95 parts of water；
Further, by after cleaning fluid cleaning, using deionized water rinsing aluminum alloy surface, washing time is aluminium alloy stock
7min。
B. it is configured to film liquid
By weight, by 3 parts of BTESPT silane couplers, 28 parts of ethanol, 19 parts of deionized water, methylpropene sodium sulfonate 0.1
After part mixing, after stirring 6min, prepared into film liquid and completed, mixed solution is then placed on nonventilated place and is hydrolyzed,
Hydrolysis time is 3 hours, and wherein the initial temperature of deionized water is 55 DEG C；
Further, into film liquid by weight, it is made up of the component of following weight portion：4 parts of BTESPT silane couplers, ethanol 30
Part, 24 parts of deionized water, 0.2 part of methylpropene sodium sulfonate.
Preferably, BTESPT silane couplers, by adding ammoniacal liquor or acetic acid, maintain the pH of hydrolyzate in hydrolytic process
It is 4-6.
C. film-forming process
Aluminum alloy materials are put into prepare complete into film liquid, after 2min, into adding into 0.03 times of film liquid weight in film liquid
Weight di (isooctyl) phosphate, continue soak 4min after, take out aluminum alloy materials, place it in ventilation stand 60min after, system
Obtain finished product.
Embodiment 2
A kind of method for lifting aluminum alloy surface silane film properties, including following operating procedure：
A. aluminum alloy surface cleaning treatment
Aluminium alloy stock after polishing is put into cleaning fluid and is cleaned, wherein cleaning fluid is made up of the component of following weight portion：10%
13 parts of hydrochloric acid, 9 parts of sodium citrate, 2 parts of sodium phosphate, 110 parts of water；
Further, by after cleaning fluid cleaning, using deionized water rinsing aluminum alloy surface, washing time is aluminium alloy stock
9min。
B. it is configured to film liquid
By weight, by 5 parts of BTESPT silane couplers, 32 parts of ethanol, 25 parts of deionized water, methylpropene sodium sulfonate 0.2
After part mixing, after stirring 8min, prepared into film liquid and completed, mixed solution is then placed on nonventilated place and is hydrolyzed,
Hydrolysis time is 4 hours, and wherein the initial temperature of deionized water is 57 DEG C；
Further, into film liquid by weight, it is made up of the component of following weight portion：4 parts of BTESPT silane couplers, ethanol 31
Part, 25 parts of deionized water, 0.2 part of methylpropene sodium sulfonate.
Preferably, BTESPT silane couplers, by adding ammoniacal liquor or acetic acid, maintain the pH of hydrolyzate in hydrolytic process
It is 4-6.
C. film-forming process
Aluminum alloy materials are put into prepare complete into film liquid, after 3min, into adding into 0.04 times of film liquid weight in film liquid
Weight di (isooctyl) phosphate, continue soak 5min after, take out aluminum alloy materials, place it in ventilation stand 70min after, system
Obtain finished product.
Embodiment 3
A kind of method for lifting aluminum alloy surface silane film properties, including following operating procedure：
A. aluminum alloy surface cleaning treatment
Aluminium alloy stock after polishing is put into cleaning fluid and is cleaned, wherein cleaning fluid is made up of the component of following weight portion：10%
15 parts of hydrochloric acid, 10 parts of sodium citrate, 3 parts of sodium phosphate, 125 parts of water；
Further, by after cleaning fluid cleaning, using deionized water rinsing aluminum alloy surface, washing time is aluminium alloy stock
9min。
B. it is configured to film liquid
By weight, by 6 parts of BTESPT silane couplers, 34 parts of ethanol, 27 parts of deionized water, methylpropene sodium sulfonate 0.3
After part mixing, after stirring 10min, prepared into film liquid and completed, mixed solution is then placed on nonventilated place and is hydrolyzed,
Hydrolysis time is 5 hours, and wherein the initial temperature of deionized water is 60 DEG C；
Further, into film liquid by weight, it is made up of the component of following weight portion：5 parts of BTESPT silane couplers, ethanol 32
Part, 26 parts of deionized water, 0.3 part of methylpropene sodium sulfonate.
Preferably, BTESPT silane couplers, by adding ammoniacal liquor or acetic acid, maintain the pH of hydrolyzate in hydrolytic process
It is 4-6.
C. film-forming process
Aluminum alloy materials are put into prepare complete into film liquid, after 5min, into adding into 0.05 times of film liquid weight in film liquid
Weight di (isooctyl) phosphate, continue soak 6min after, take out aluminum alloy materials, place it in ventilation stand 80min after, system
Obtain finished product.
Experiment：
5 stock material identical aluminum alloy materials are chosen respectively, are randomly divided into test group 1,2,3,4,5,1,2,3 pairs of groups of test group
Al-alloy products processed by the way of embodiment 1,2,3, test group 4 is using conventional silanization process treatment, test group 5
In aluminum alloy materials do not carry out any treatment, being carried out a little to the aluminium alloy in 5 test groups with 3mol/L copper sulphate respectively
Drop experiment, the time of the aluminium alloy sulfuric-resisting copper discoloration of test different process treatment, result of the test is as shown in table 1：
The time of the aluminum alloy surface sulfuric-resisting copper discoloration of table 1
| Project | Coloring Time/h |
| Test group 1 | 2.3 |
| Test group 2 | 2.5 |
| Test group 3 | 2.9 |
| Test group 4 | 1.6 |
| Test group 5 | 0.08 |
As shown in Table 1, by the aluminium alloy after the inventive method treatment, the decay resistance on its surface has obtained greatly carrying
Rise, extend the service life of Al-alloy products.
Certainly, described above is not limitation of the present invention, and the present invention is also not limited to the example above, the art
Those of ordinary skill, in essential scope of the invention, the change made, change, addition or replace, should all belong to the present invention
Protection domain.
Claims (4)
1. it is a kind of lifted aluminum alloy surface silane film properties method, it is characterised in that including following operating procedure：
A. aluminum alloy surface cleaning treatment
Aluminium alloy stock after polishing is put into cleaning fluid and is cleaned, wherein cleaning fluid is made up of the component of following weight portion：10%
Hydrochloric acid 10-15 parts, sodium citrate 7-10 parts, sodium phosphate 1-3 parts, water 95-125 parts；
B. it is configured to film liquid
By weight, by 3-6 parts of BTESPT silane couplers, ethanol 28-34 parts, deionized water 19-27 parts, metering system sulphur
After sour sodium 0.1-0.3 parts of mixing, after stirring 6-10min, prepared into film liquid and completed, be then placed on mixed solution nonventilated
Place is hydrolyzed, and hydrolysis time is 3-5 hours, and wherein the initial temperature of deionized water is 55-60 DEG C；
C. film-forming process
Aluminum alloy materials are put into prepare complete into film liquid, after 2-5min, into adding into film liquid weight 0.03- in film liquid
0.05 times of di (isooctyl) phosphate of weight, after continuing to soak 4-6min, takes out aluminum alloy materials, places it in ventilation standing
After 60-80min, finished product.
2. a kind of method of the lifting aluminum alloy surface silane film properties according to claim 1, it is characterised in that step
In A, by after cleaning fluid cleaning, using deionized water rinsing aluminum alloy surface, washing time is not less than 5min to aluminium alloy stock.
3. a kind of method of the lifting aluminum alloy surface silane film properties according to claim 1, it is characterised in that step
In B, into film liquid by weight, it is made up of the component of following weight portion：4-5 parts of BTESPT silane couplers, ethanol 30-32
Part, deionized water 24-26 parts, methylpropene sodium sulfonate 0.2-0.3 parts.
4. a kind of method of the lifting aluminum alloy surface silane film properties according to claim 1, it is characterised in that step
In B, in hydrolytic process, by adding ammoniacal liquor or acetic acid, the pH for maintaining hydrolyzate is 4-6 to BTESPT silane couplers.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710137350.6A CN106929863A (en) | 2017-03-09 | 2017-03-09 | A kind of method for lifting aluminum alloy surface silane film properties |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710137350.6A CN106929863A (en) | 2017-03-09 | 2017-03-09 | A kind of method for lifting aluminum alloy surface silane film properties |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110042451A (en) * | 2019-03-27 | 2019-07-23 | 祝亚琴 | Deashing agent |
| CN110527995A (en) * | 2019-09-29 | 2019-12-03 | 中国石油大学(华东) | Application of the compound silane film of MXene/ silane surfaces in metal erosion protection |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717930A (en) * | 2009-12-25 | 2010-06-02 | 华烁科技股份有限公司 | Environment-friendly nano water-based silane treatment agent capable of improving anti-corrosion performance of metal surface |
| CN104725549A (en) * | 2014-02-24 | 2015-06-24 | 长兴化学工业(中国)有限公司 | High-performance nano composite latex |
-
2017
- 2017-03-09 CN CN201710137350.6A patent/CN106929863A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717930A (en) * | 2009-12-25 | 2010-06-02 | 华烁科技股份有限公司 | Environment-friendly nano water-based silane treatment agent capable of improving anti-corrosion performance of metal surface |
| CN104725549A (en) * | 2014-02-24 | 2015-06-24 | 长兴化学工业(中国)有限公司 | High-performance nano composite latex |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110042451A (en) * | 2019-03-27 | 2019-07-23 | 祝亚琴 | Deashing agent |
| CN110527995A (en) * | 2019-09-29 | 2019-12-03 | 中国石油大学(华东) | Application of the compound silane film of MXene/ silane surfaces in metal erosion protection |
| CN110527995B (en) * | 2019-09-29 | 2021-08-10 | 中国石油大学(华东) | Application of MXene/silane surface composite silane film in metal corrosion protection |
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Application publication date: 20170707 |