CN106756950A - A kind of titanium dioxide nano thread phytic acid conversion fluid and its application method for Mg alloy surface antirust selfreparing - Google Patents
A kind of titanium dioxide nano thread phytic acid conversion fluid and its application method for Mg alloy surface antirust selfreparing Download PDFInfo
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- CN106756950A CN106756950A CN201611215844.3A CN201611215844A CN106756950A CN 106756950 A CN106756950 A CN 106756950A CN 201611215844 A CN201611215844 A CN 201611215844A CN 106756950 A CN106756950 A CN 106756950A
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- titanium dioxide
- phytic acid
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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
- C23C22/40—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 molybdates, tungstates or vanadates
- C23C22/44—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 molybdates, tungstates or vanadates containing also fluorides or complex fluorides
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Abstract
The invention discloses a kind of titanium dioxide nano thread phytic acid conversion fluid for Mg alloy surface antirust selfreparing, the conversion fluid is using phytic acid as main film-former, assistant is with sodium molybdate, sodium fluoride, the auxiliary agents such as Choline Chloride, and ultra-fine hydroxyl britesorb serpentine and titanium dioxide nano thread are added on the basis of this chemical conversion solution, both materials are added in phytic acid conversion fluid system after being made dispersion in sodium dodecyl benzene sulfonate aqueous solution in advance, make its fine dispersion in the solution, its Uniform Doped is in conversion film, the antiwear and antifriction of film layer can significantly be improved, selfreparing, resistance to corrosion, and assign alloy surface unique optics, electricity, mechanical property, significantly improve the surface property of magnesium alloy, broadening uses scope.
Description
Technical field
It is used for Mg alloy surface antirust selfreparing the present invention relates to technical field of magnesium alloy surface treatment, more particularly to one kind
Titanium dioxide nano thread-phytic acid conversion fluid and its application method.
Background technology
Magnesium alloy is the metal material of a kind of lightweight, high intensity, and the product weight of equality strength even can compare plastic cement
Also light, the ability of its load that withstands shocks is bigger than aluminium alloy, at the same magnesium alloy also have good processability, rapid heat dissipation, antidetonation,
The advantages of anti electromagnetic wave, recoverable, is widely used in fields such as Aero-Space, 3C Product, sports equipments, especially closely
3C Product gradually develops to compact direction over year so that high performance magnesium alloy is more favored by manufacturer.
Although magnesium alloy possesses above-mentioned advantage, because magnesium and its alloy activity are high, its oxide-film is loose porous,
Cause that material surface corrosion resistance is poor, environmental suitability is poor, limits the use of magnesium alloy.In order to improve these shortcomings, work
Magnesium alloy is surface-treated frequently with surface protection technique in industry application, wherein chemical conversion treatment be it is most quick, effectively,
A kind of economic processing mode, can not only improve alloy corrosion ability, go back the further protective treatment of alloy surface and lay
Good basis.The conventional chemical pretreatment solution of current magnesium alloy mainly have chromate, permanganate, phosphate, permanganate-
The technique of the solution systems such as phosphate, wherein chromate conversion coating is the most ripe, but Cr VI is carcinogen high, at present
Prohibit the use of, although the treatment fluid of other classes is more environmentally friendly to a certain extent, the conversion film for being formed exists corrosion-resistant
The problems such as poor, film layer of property is also easy to produce crackle, it is difficult to meet engineering demand.In order to improve chemical composition coating presence these lack
Fall into, researchers can significantly improve the microstructure of conversion film by adding nano-particle in conversion fluid, such as《Nanometer is hard
The influence of matter relative chemical conversion film microstructure》The result of study of one text shows a nanometer Al2O3, Nano-meter SiO_22Addition can have
The raising conversion film crystal grain quantity of effect, improves the consistency of conversion film, obtains corrosion resistance higher, but improve nano-powder and exist
Dispersiveness in conversion fluid is still more formidable problem, very high to technological operation requirement, using limited.
The content of the invention
A kind of defect in order to make up prior art of the invention, there is provided titanium dioxide for Mg alloy surface antirust selfreparing
Titanium nano wire-phytic acid conversion fluid and its application method, the magnesium alloy surface protective film more excellent to obtain performance, further widen
The use scope of magnesium alloy.
The present invention is achieved by the following technical solutions：
A kind of titanium dioxide nano thread-phytic acid conversion fluid for Mg alloy surface antirust selfreparing, the conversion fluid is by following heavy
The raw material for measuring part is formulated：Phytic acid 20-50, sodium fluoride 0.1-0.2, sodium molybdate 4-5, Choline Chloride 1-2, ultra-fine hydroxyl silicon
Sour magnesium salts serpentine 0.1-0.2, polyvinylpyrrolidone 1-2, titanium dioxide nano thread 0.3-0.5, neopelex
0.1-0.2, defoamer 0.1-0.2, appropriate deionized water, appropriate glacial acetic acid.
The a diameter of 20-50nm of described titanium dioxide nano thread, length is 30-50 μm.
Described conversion fluid is prepared by following steps：
（1）Phytic acid is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（2）Sodium fluoride is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（3）Sodium molybdate is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（4）Choline Chloride is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（5）Take 5-10 parts by weight of deionized water to mix with neopelex, be stirring evenly and then adding into ultra-fine hydroxyl silicon
Sour magnesium salts serpentine, grinding distribution 30-50min is subsequently added titanium dioxide nano thread, sonic oscillation treatment 20-30min, institute
Obtain solution for standby；
（6）Polyvinylpyrrolidone is mixed with appropriate deionized water, stirring is completely dissolved it, and resulting solution is standby；
（7）By step（1）To step（6）Deionized water regulation is added after the solution of preparation and other residual components are well mixed
Phytic acid concentration is 10-15g/L into system, then is 3.5-4 with glacial acetic acid regulation system pH value, obtains final product described conversion fluid.
A kind of user of described titanium dioxide nano thread-phytic acid conversion fluid for Mg alloy surface antirust selfreparing
Method, comprises the following steps：
（1）Mg alloy surface is dried naturally after the steps such as oil removing, water rinsing, acid attack, water rinsing, alkali activation, water rinsing
It is standby；
（2）Pretreated magnesium alloy is soaked in temperature for the 50-60 DEG C of titanium dioxide nano thread-phytic acid of antirust selfreparing turns
Taken out after 25-30min is reacted in change liquid, then workpiece is rinsed with water, dried naturally.
, using phytic acid as main film-former, assistant is helped conversion fluid prepared by the present invention with sodium molybdate, sodium fluoride, Choline Chloride etc.
Agent, and ultra-fine hydroxyl britesorb serpentine and titanium dioxide nano thread are added on the basis of this chemical conversion solution, this
Two kinds of materials are added in phytic acid conversion fluid system after being made dispersion in sodium dodecyl benzene sulfonate aqueous solution in advance, are made
Its fine dispersion in the solution, its Uniform Doped can significantly improve the antiwear and antifriction of film layer, selfreparing, anti-in conversion film
Corrosive power, and assign alloy surface unique optics, electricity, mechanical property, the surface property of magnesium alloy is significantly improved, expand
Width uses scope.
Specific embodiment
A kind of titanium dioxide nano thread phytic acid conversion fluid for Mg alloy surface antirust selfreparing, the conversion fluid is by following
The raw material of weight portion is formulated：Phytic acid 20, sodium fluoride 0.1, sodium molybdate 4, Choline Chloride 1, ultra-fine hydroxyl britesorb snake
Line stone 0.1, polyvinylpyrrolidone 1, titanium dioxide nano thread 0.3, neopelex 0.1, defoamer 0.1, go from
Sub- appropriate amount of water, appropriate glacial acetic acid.
The wherein a diameter of 20nm of titanium dioxide nano thread, length is 30 μm.
The conversion fluid is prepared by following steps：
（1）Phytic acid is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（2）Sodium fluoride is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（3）Sodium molybdate is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（4）Choline Chloride is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（5）Take 5 parts by weight of deionized water to mix with neopelex, be stirring evenly and then adding into ultra-fine hydroxyl magnesium silicate
Salt serpentine, grinding distribution 30min is subsequently added titanium dioxide nano thread, and sonic oscillation treatment 20min, resulting solution is standby；
（6）Polyvinylpyrrolidone is mixed with appropriate deionized water, stirring is completely dissolved it, and resulting solution is standby；
（7）By step（1）To step（6）Deionized water regulation is added after the solution of preparation and other residual components are well mixed
Phytic acid concentration is 10g/L into system, then is 3.5 with glacial acetic acid regulation system pH value, obtains final product described conversion fluid.
The application method of the conversion fluid is comprised the following steps：
（1）Mg alloy surface is dried naturally after the steps such as oil removing, water rinsing, acid attack, water rinsing, alkali activation, water rinsing
It is standby；
（2）Pretreated magnesium alloy sample is soaked in 60 DEG C of titanium dioxide nano thread phytic acid conversion fluids of antirust selfreparing
Taken out after reaction 25min, then workpiece is rinsed with water, dried naturally.
Conversion film to magnesium alloy sample surface carries out performance test, and test result is：
Pattern:Macroscopic view is canescence, and film forming uniform ground, microcosmic result is solid netted result, there is slight crackle, the μ of thickness 5.6
m。
Corrosion resistance：Undressed magnesium alloy substrate and sample are distinguished into salt spray test and damp heat test, it is as a result as follows：
| Project | Salt spray test | Damp heat test |
| Matrix | General corrosion after 8h, produces a large amount of erosions | Surface discolouration, a large amount of bubbles of appearance after 24h |
| Sample | There is corrosion pit in surface after 48h | Surface light discolouration after 160h, a small amount of bubble |
Claims (4)
1. a kind of titanium dioxide nano thread-phytic acid conversion fluid for Mg alloy surface antirust selfreparing, it is characterised in that this turn
Change liquid to be formulated by the raw material of following weight portion：Phytic acid 20-50, sodium fluoride 0.1-0.2, sodium molybdate 4-5, Choline Chloride 1-2,
Ultra-fine hydroxyl britesorb serpentine 0.1-0.2, polyvinylpyrrolidone 1-2, titanium dioxide nano thread 0.3-0.5,12
Sodium alkyl benzene sulfonate 0.1-0.2, defoamer 0.1-0.2, appropriate deionized water, appropriate glacial acetic acid.
2. a kind of titanium dioxide nano thread-phytic acid conversion for Mg alloy surface antirust selfreparing as claimed in claim 1
Liquid, it is characterised in that a diameter of 20-50nm of described titanium dioxide nano thread, length is 30-50 μm.
3. a kind of titanium dioxide nano thread-phytic acid for Mg alloy surface antirust selfreparing as claimed in claim 1 or 2 turns
Change liquid, it is characterised in that described conversion fluid is prepared by following steps：
（1）Phytic acid is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（2）Sodium fluoride is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（3）Sodium molybdate is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（4）Choline Chloride is mixed with a small amount of deionized water, stirring is completely dissolved it, and resulting solution is standby；
（5）Take 5-10 parts by weight of deionized water to mix with neopelex, be stirring evenly and then adding into ultra-fine hydroxyl silicon
Sour magnesium salts serpentine, grinding distribution 30-50min is subsequently added titanium dioxide nano thread, sonic oscillation treatment 20-30min, institute
Obtain solution for standby；
（6）Polyvinylpyrrolidone is mixed with appropriate deionized water, stirring is completely dissolved it, and resulting solution is standby；
（7）By step（1）To step（6）Deionized water regulation is added after the solution of preparation and other residual components are well mixed
Phytic acid concentration is 10-15g/L into system, then is 3.5-4 with glacial acetic acid regulation system pH value, obtains final product described conversion fluid.
4. a kind of titanium dioxide nano thread-phytic acid for Mg alloy surface antirust selfreparing as described in claims 1 to 3 turns
Change the application method of liquid, it is characterised in that comprise the following steps：
（1）Mg alloy surface is dried naturally after the steps such as oil removing, water rinsing, acid attack, water rinsing, alkali activation, water rinsing
It is standby；
（2）Pretreated magnesium alloy is soaked in the titanium dioxide nano thread-phytic acid of the antirust selfreparing that temperature is 50-60 DEG C
Taken out after 25-30min is reacted in conversion fluid, then workpiece is rinsed with water, dried naturally.
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| CN201611215844.3A CN106756950A (en) | 2016-12-26 | 2016-12-26 | A kind of titanium dioxide nano thread phytic acid conversion fluid and its application method for Mg alloy surface antirust selfreparing |
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| CN201611215844.3A CN106756950A (en) | 2016-12-26 | 2016-12-26 | A kind of titanium dioxide nano thread phytic acid conversion fluid and its application method for Mg alloy surface antirust selfreparing |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102380980A (en) * | 2011-07-27 | 2012-03-21 | 江南大学 | Self-purifying textile and processing method thereof |
| CN104250758A (en) * | 2013-06-28 | 2014-12-31 | 无锡杨市表面处理科技有限公司 | Aluminum alloy surface chemical conversion film forming liquid |
| CN104250788A (en) * | 2013-06-28 | 2014-12-31 | 无锡杨市表面处理科技有限公司 | Preparation method of aluminum alloy surface chemical conversion film forming liquid |
| CN104342683A (en) * | 2013-07-25 | 2015-02-11 | 无锡市石塘湾工业园区开发建设有限公司 | Magnesium alloy work-piece surface anti-corrosion conversion film treatment process |
-
2016
- 2016-12-26 CN CN201611215844.3A patent/CN106756950A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102380980A (en) * | 2011-07-27 | 2012-03-21 | 江南大学 | Self-purifying textile and processing method thereof |
| CN104250758A (en) * | 2013-06-28 | 2014-12-31 | 无锡杨市表面处理科技有限公司 | Aluminum alloy surface chemical conversion film forming liquid |
| CN104250788A (en) * | 2013-06-28 | 2014-12-31 | 无锡杨市表面处理科技有限公司 | Preparation method of aluminum alloy surface chemical conversion film forming liquid |
| CN104342683A (en) * | 2013-07-25 | 2015-02-11 | 无锡市石塘湾工业园区开发建设有限公司 | Magnesium alloy work-piece surface anti-corrosion conversion film treatment process |
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