CN105401143A - Rare earth aluminum alloy cured film forming solution and preparation method thereof - Google Patents
Rare earth aluminum alloy cured film forming solution and preparation method thereof Download PDFInfo
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- CN105401143A CN105401143A CN201510739923.3A CN201510739923A CN105401143A CN 105401143 A CN105401143 A CN 105401143A CN 201510739923 A CN201510739923 A CN 201510739923A CN 105401143 A CN105401143 A CN 105401143A
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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
- C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/56—Treatment of aluminium or alloys based thereon
Abstract
The invention discloses a rare earth aluminum alloy cured film forming solution. The solution is composed of, by weight, 0.8-1 part of potassium fluotitanate, 100-110 parts of bis(gamma-triethoxysilylpropyl)tetrasulfide, 10-12 parts of butyl titanate, 3-5 parts of multiwalled carbon nanotubes, 0.8-1 part of cerous nitrate, 0.3-1 part of trimethylolpropane, 0.08-0.1 part of polytetrafluoroethylene, 1-2 parts of zinc naphthenate, 0.5-1 part of glycerin monostearate, 1-2 parts of ammonium molybdate and 2-3 parts of hydrolytic polymaleic anhydride. The bonding performance between an aluminum alloy cured film and an aluminum alloy base material is high, the film is not prone to falling after being formed, stability is good, and a lasting protecting effect is achieved.
Description
Technical field
The present invention relates to technical field of aluminum alloy surface treatment, particularly relate to a kind of rare earth aluminium alloy cured film shaping dope and preparation method thereof.
Background technology
Silane due to its uniqueness molecular structure, asepsis environment-protecting, cost is low, consistency is good etc., and feature starts to be applied to anti-corrosion of metal field by people.Silane can be combined with metallic matrix closely through hydrolysis, forms fine and close rete, have good protected effect to metal on surface.But when the porous of silane film own, resistibility is corroded to corrosive medium more weak, in corrosive environment, Cl-etc. are easy especially to be corroded along these defects, the accumulation of corrosion product in interface can make formation stressed zone, interface, and cause the stripping of rete to come off, such silane film is once be destroyed, cannot selfreparing be carried out, be easy to the corrosion causing metallic matrix.Research finds to prepare organic and inorganic silane complex film by the inorganic nano-particle that adulterates in silane film with the material (as rare earth ions such as Ce, La) with self-repair function, effectively can prevent these defects of silane complex film.
Summary of the invention
The object of the invention is exactly the defect in order to make up prior art, provides a kind of rare earth aluminium alloy cured film shaping dope and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of rare earth aluminium alloy cured film shaping dope, it is made up of the raw material of following weight parts:
Potassium fluotitanate 0.8-1, two (the silica-based propyl group of γ-triethoxy) tetrasulfide 100-110, butyl (tetra) titanate 10-12, multi-walled carbon nano-tubes 3-5, cerous nitrate 0.8-1, TriMethylolPropane(TMP) 0.3-1, tetrafluoroethylene 0.08-0.1, zinc naphthenate 1-2, glyceryl monostearate 0.5-1, ammonium molybdate 1-2, hydrolytic polymaleic anhydride 2-3.
A preparation method for described rare earth aluminium alloy cured film shaping dope, comprises the following steps:
(1) joined in 16-20 times of deionized water by above-mentioned potassium fluotitanate, stir, add hydrolytic polymaleic anhydride, adjustment PH is 2-3, and at 70-80 DEG C, insulated and stirred stirs 6-10 minute, and cooling, obtains acid solution;
(2) above-mentioned two (the silica-based propyl group of γ-triethoxy) tetrasulfide is mixed by the volume ratio of 1-2:3-4:90-100 with deionized water, dehydrated alcohol, ultrasonic disperse 10-20 minute, add Glacial acetic acid, adjustment PH is 4-5, at 20-30 DEG C, be incubated 46-50 hour, obtain coupling agent solution;
(3) above-mentioned cerous nitrate is joined its volume 200-300 doubly, in the ethanolic soln of 4-6%, ultrasonic 1-2 minute is rare earth alcohol liquid;
(4) mixed with rare earth alcohol liquid by above-mentioned acid solution, stir, add zinc naphthenate, 300-400 rev/min is stirred 20-30 minute, obtains rare earth composite solution;
(5) above-mentioned butyl (tetra) titanate is mixed by the volume ratio of 1-2:25-30:2-3 with dehydrated alcohol, acetic acid, stir, drip above-mentioned rare earth composite solution, dropwise rear ageing 20-24 hour, obtain TiO 2 sol;
(6) being joined by glyceryl monostearate in the dehydrated alcohol of 7-10 times of weight, stir, is alcohol ester solution;
(7) be mixed to join in resistance furnace by above-mentioned tetrafluoroethylene, multi-walled carbon nano-tubes, reacting by heating 5-6 hour at 480-500 DEG C, cooling is come out of the stove, and is washed by product, dries, obtain carbon fluoride nano-tube;
(8) above-mentioned TriMethylolPropane(TMP) is joined in 80-100 times of dehydrated alcohol, stir, add carbon fluoride nano-tube, ultrasonic 17-20 minute, mix with above-mentioned coupling agent solution, TiO 2 sol, alcohol ester solution, add each raw material of residue, stir, at 75-80 DEG C, distill 1-2 hour, cool and get final product.
Described a kind of rare earth aluminium alloy cured film shaping dope, the using method of this aluminium alloy cured film shaping dope is:
(1) after aluminium alloy being polished with carborundum paper, use the diamond paste polishing of 0.5 μm again, afterwards successively with acetone, ethanol, water three kinds of solvent supersonic cleanings, cleaned sample is processed respectively in the HNO3 solution of 1.8-2%NaOH solution and 4-5%, finally use deionized water ultrasonic cleaning, nitrogen drying is for subsequent use;
(2) the aluminium alloy pickling process pulling film forming in above-mentioned solution will handled well, sends into after film forming in loft drier, solidifies 110-120min, obtain cured film at 115-120 DEG C.
Advantage of the present invention is:
The carbon nanotube chemical character that the present invention adds is highly stable, and its C-C singly-bound is the most stable chemical bond of occurring in nature, effectively can improve solidity to corrosion and the mechanical property of substrate surface film;
Present invention adds rare earth nitrate, the oxide compound formed through passivation and oxyhydroxide can be formed with the reticulated structure of organosilane and act synergistically, fine and close coating is formed with carbon nanotube, carbonic acid gas, cathodic depolarization is effectively inhibit to react and anode dissolution reaction, reduce erosion rate, play good protective effect;
In the present invention, adding of titanium dioxide makes the compactness of silane complex film increase, effectively prevent the erosion of the corrosive ions such as Cl-, H2O and O2, the diffusion of corrosion product can be suppressed, due to aperture blocking effect, stop the further generation of corrosion, this is because a part of TiOH group will react with the hydroxyl of metallic surface, Si-OH, at aluminium alloy matrix surface synergistic sorption, this just effectively enhances the bonding force of rete and matrix, overcomes the shortcoming that simple silane film is easy to peel off at matrix surface;
The present invention is C-F key at multi-walled carbon nano-tubes Surface Creation, can improve the dispersiveness in film with TiO 2 particles, effectively reduces reunion, can also improve the water resisting property of film coated surface simultaneously;
Composite membrane of the present invention has excellent protective value to alloy matrix aluminum; can anode dissolution be effectively suppressed to react; multi-walled carbon nano-tubes can with the functional groups Cheng Jian of titanium dioxide, two (the silica-based propyl group of γ-triethoxy) tetrasulfide; serve the compactness increasing film; improve the effect of the stability of film; effectively can stop the immersion of corrosive medium, thus improve corrosion resistance.
The cohesiveness of aluminium alloy cured film of the present invention and aluminum alloy base material is strong, and difficult drop-off after film forming, good stability, protected effect is lasting.
Embodiment
A kind of rare earth aluminium alloy cured film shaping dope, it is made up of the raw material of following weight parts:
Potassium fluotitanate 0.8, two (the silica-based propyl group of γ triethoxy) tetrasulfide 100, butyl (tetra) titanate 10, multi-walled carbon nano-tubes 3, cerous nitrate 0.8, TriMethylolPropane(TMP) 0.3, tetrafluoroethylene 0.08, zinc naphthenate 1, glyceryl monostearate 0.5, ammonium molybdate 1, hydrolytic polymaleic anhydride 2.
A preparation method for described rare earth aluminium alloy cured film shaping dope, comprises the following steps:
(1) joined in 16 times of deionized waters by above-mentioned potassium fluotitanate, stir, add hydrolytic polymaleic anhydride, regulate PH to be 2, at 70 DEG C, insulated and stirred stirs 6 minutes, and cooling, obtains acid solution;
(2) above-mentioned two (the silica-based propyl group of γ triethoxy) tetrasulfide is mixed by the volume ratio of 1:3:90 with deionized water, dehydrated alcohol, ultrasonic disperse 10 minutes, adds Glacial acetic acid, regulates PH to be 4, at 20 DEG C, be incubated 46 hours, obtain coupling agent solution;
(3) above-mentioned cerous nitrate is joined its volume 200 times, 4% ethanolic soln in, ultrasonic 1 minute is rare earth alcohol liquid;
(4) mixed with rare earth alcohol liquid by above-mentioned acid solution, stir, add zinc naphthenate, 300 revs/min are stirred 20 minutes, obtain rare earth composite solution;
(5) above-mentioned butyl (tetra) titanate is mixed by the volume ratio of 1:25:2 with dehydrated alcohol, acetic acid, stir, drip above-mentioned rare earth composite solution, dropwise rear ageing 20 hours, obtain TiO 2 sol;
(6) being joined by glyceryl monostearate in the dehydrated alcohol of 7 times of weight, stir, is alcohol ester solution;
(7) be mixed to join in resistance furnace by above-mentioned tetrafluoroethylene, multi-walled carbon nano-tubes, reacting by heating 5 hours at 480 DEG C, cooling is come out of the stove, and is washed by product, dries, obtain carbon fluoride nano-tube;
(8) above-mentioned TriMethylolPropane(TMP) is joined in 80 times of dehydrated alcohols, stir, add carbon fluoride nano-tube, ultrasonic 17 minutes, mix with above-mentioned coupling agent solution, TiO 2 sol, alcohol ester solution, add each raw material of residue, stir, distill 1 hour at 75 DEG C, cool and get final product.
Described a kind of rare earth aluminium alloy cured film shaping dope, the using method of this aluminium alloy cured film shaping dope is:
(1) after aluminium alloy being polished with carborundum paper, use the diamond paste polishing of 0.5 μm again, afterwards successively with acetone, ethanol, water three kinds of solvent supersonic cleanings, by cleaned sample respectively 1.8%NaOH solution and 4% HNO3 solution in process, finally use deionized water ultrasonic cleaning, nitrogen drying is for subsequent use;
(2) the aluminium alloy pickling process pulling film forming in above-mentioned solution will handled well, sends into after film forming in loft drier, solidifies 110min, obtain cured film at 115 DEG C.
Performance test:
Bending viscosity:
By cured film shaping dope process aluminum alloy sheet of the present invention, after film-forming, by bending 60 degree of aluminium flake doubling, peel off curved part 3 times with adhesive tape, under X20 magnifying glass, detect extent of exfoliation, result flawless;
Aluminum alloy sheet after film-forming is soaked 1 hour in boiling water, at room temperature places 24 hours, then by bending 60 degree of aluminium flake doubling, peel off curved part 3 times with adhesive tape, under X20 magnifying glass, detect extent of exfoliation, result flawless;
Erosion resistance:
By cured film shaping dope process aluminum alloy sheet of the present invention, after film-forming, by this material lateral dissection, carry out spray test, agents useful for same to be concentration be 5% sodium chloride solution, test period 300 hours, measure the bubbling width formed in line of cut side, result bubbling width is 0;
Aluminum alloy sheet after film-forming being immersed in concentration is in the sodium chloride solution of 5%, and soak 300 hours, material surface is substantially unchanged, and soak 400 hours, minute quantity rust staining appears in edge.
Claims (3)
1. a rare earth aluminium alloy cured film shaping dope, is characterized in that what it was made up of the raw material of following weight parts:
Potassium fluotitanate 0.8-1, two (the silica-based propyl group of γ-triethoxy) tetrasulfide 100-110, butyl (tetra) titanate 10-12, multi-walled carbon nano-tubes 3-5, cerous nitrate 0.8-1, TriMethylolPropane(TMP) 0.3-1, tetrafluoroethylene 0.08-0.1, zinc naphthenate 1-2, glyceryl monostearate 0.5-1, ammonium molybdate 1-2, hydrolytic polymaleic anhydride 2-3.
2. a preparation method for rare earth aluminium alloy cured film shaping dope as claimed in claim 1, is characterized in that comprising the following steps:
(1) joined in 16-20 times of deionized water by above-mentioned potassium fluotitanate, stir, add hydrolytic polymaleic anhydride, adjustment PH is 2-3, and at 70-80 DEG C, insulated and stirred stirs 6-10 minute, and cooling, obtains acid solution;
(2) above-mentioned two (the silica-based propyl group of γ-triethoxy) tetrasulfide is mixed by the volume ratio of 1-2:3-4:90-100 with deionized water, dehydrated alcohol, ultrasonic disperse 10-20 minute, add Glacial acetic acid, adjustment PH is 4-5, at 20-30 DEG C, be incubated 46-50 hour, obtain coupling agent solution;
(3) above-mentioned cerous nitrate is joined its volume 200-300 doubly, in the ethanolic soln of 4-6%, ultrasonic 1-2 minute is rare earth alcohol liquid;
(4) mixed with rare earth alcohol liquid by above-mentioned acid solution, stir, add zinc naphthenate, 300-400 rev/min is stirred 20-30 minute, obtains rare earth composite solution;
(5) above-mentioned butyl (tetra) titanate is mixed by the volume ratio of 1-2:25-30:2-3 with dehydrated alcohol, acetic acid, stir, drip above-mentioned rare earth composite solution, dropwise rear ageing 20-24 hour, obtain TiO 2 sol;
(6) being joined by glyceryl monostearate in the dehydrated alcohol of 7-10 times of weight, stir, is alcohol ester solution;
(7) be mixed to join in resistance furnace by above-mentioned tetrafluoroethylene, multi-walled carbon nano-tubes, reacting by heating 5-6 hour at 480-500 DEG C, cooling is come out of the stove, and is washed by product, dries, obtain carbon fluoride nano-tube;
(8) above-mentioned TriMethylolPropane(TMP) is joined in 80-100 times of dehydrated alcohol, stir, add carbon fluoride nano-tube, ultrasonic 17-20 minute, mix with above-mentioned coupling agent solution, TiO 2 sol, alcohol ester solution, add each raw material of residue, stir, at 75-80 DEG C, distill 1-2 hour, cool and get final product.
3. a kind of rare earth aluminium alloy cured film shaping dope according to claim 1, is characterized in that the using method of this aluminium alloy cured film shaping dope is:
(1) after aluminium alloy being polished with carborundum paper, use the diamond paste polishing of 0.5 μm again, afterwards successively with acetone, ethanol, water three kinds of solvent supersonic cleanings, cleaned sample is processed respectively in the HNO3 solution of 1.8-2%NaOH solution and 4-5%, finally use deionized water ultrasonic cleaning, nitrogen drying is for subsequent use;
(2) the aluminium alloy pickling process pulling film forming in above-mentioned solution will handled well, sends into after film forming in loft drier, solidifies 110-120min, obtain cured film at 115-120 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108404917A (en) * | 2018-04-04 | 2018-08-17 | 东莞市石鼓污水处理有限公司 | A kind of preparation method of NiTiO3-ZrO2 sewage disposals film |
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| CN108404917A (en) * | 2018-04-04 | 2018-08-17 | 东莞市石鼓污水处理有限公司 | A kind of preparation method of NiTiO3-ZrO2 sewage disposals film |
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