CN109234779A - Aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method - Google Patents
Aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method Download PDFInfo
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- CN109234779A CN109234779A CN201710557050.3A CN201710557050A CN109234779A CN 109234779 A CN109234779 A CN 109234779A CN 201710557050 A CN201710557050 A CN 201710557050A CN 109234779 A CN109234779 A CN 109234779A
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- fluoropolymer
- heat treatment
- high temperature
- antiplastering
- aluminium alloy
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- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 103
- 239000004446 fluoropolymer coating Substances 0.000 title claims abstract description 29
- 230000002195 synergetic effect Effects 0.000 title claims abstract description 29
- 238000003672 processing method Methods 0.000 title claims abstract description 14
- 229920002313 fluoropolymer Polymers 0.000 claims abstract description 55
- 239000004811 fluoropolymer Substances 0.000 claims abstract description 54
- 238000010438 heat treatment Methods 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 33
- 230000003647 oxidation Effects 0.000 claims abstract description 29
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002253 acid Substances 0.000 claims abstract description 20
- 238000011282 treatment Methods 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000006277 sulfonation reaction Methods 0.000 claims abstract description 12
- 238000002048 anodisation reaction Methods 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 28
- 239000011859 microparticle Substances 0.000 claims description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 15
- 238000005507 spraying Methods 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 14
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 10
- 238000007598 dipping method Methods 0.000 claims description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 6
- 239000011737 fluorine Substances 0.000 claims description 6
- 229910052731 fluorine Inorganic materials 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 230000004927 fusion Effects 0.000 claims description 5
- 239000004310 lactic acid Substances 0.000 claims description 5
- 235000014655 lactic acid Nutrition 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 4
- -1 amino phenyl sulfonyl Chemical group 0.000 claims description 4
- 230000008595 infiltration Effects 0.000 claims description 4
- 238000001764 infiltration Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000003466 welding Methods 0.000 abstract description 5
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 abstract description 3
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 239000012528 membrane Substances 0.000 abstract description 3
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 22
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 12
- 239000000839 emulsion Substances 0.000 description 8
- 238000005554 pickling Methods 0.000 description 8
- 238000007743 anodising Methods 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- 230000003628 erosive effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 235000006408 oxalic acid Nutrition 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 229910018569 Al—Zn—Mg—Cu Inorganic materials 0.000 description 3
- 229910000737 Duralumin Inorganic materials 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- ZAJAQTYSTDTMCU-UHFFFAOYSA-N 3-aminobenzenesulfonic acid Chemical compound NC1=CC=CC(S(O)(=O)=O)=C1 ZAJAQTYSTDTMCU-UHFFFAOYSA-N 0.000 description 2
- 229910001008 7075 aluminium alloy Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 235000010210 aluminium Nutrition 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013527 degreasing agent Substances 0.000 description 2
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- XTLNYNMNUCLWEZ-UHFFFAOYSA-N ethanol;propan-2-one Chemical compound CCO.CC(C)=O XTLNYNMNUCLWEZ-UHFFFAOYSA-N 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 238000006396 nitration reaction Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 2
- 238000005491 wire drawing Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001398 aluminium Chemical class 0.000 description 1
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- MRDKYAYDMCRFIT-UHFFFAOYSA-N oxalic acid;phosphoric acid Chemical compound OP(O)(O)=O.OC(=O)C(O)=O MRDKYAYDMCRFIT-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The present invention provides a kind of aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method, the mixed acid solution electrolytic preparation aluminum alloy hard anode oxidation film containing sulfonation anthracene is used first, then expanding treatment is carried out to aluminum alloy hard anodization oxidation film layer and introduces fluoropolymer, then fused fluoropolymer and aluminum alloy hard anode oxidation film by vacuum heat treatment and be formed as one the synergism coat with high temperature antiplastering performance.Aluminium alloy high temperature antiplastering synergistic fluoropolymer coating prepared by the present invention is in homogeneous black, and uniformity is very good, and still has high temperature antiplastering performance within the scope of 160-185 DEG C, meets use demand of the aluminium alloy in the anti-stick condition of high temperature；Present invention efficiently solves the high temperature adhesive problems of non-PVC bag making technique, are used for non-PVC bag making production line, can greatly improve non-PVC bag making production efficiency；In addition, the present invention, to the welding problem for solving aluminium alloy trilamellar membrane, five tunics, rosin joint film problem etc. has highly important application value.
Description
Technical field
The present invention relates to aluminium alloy high temperature antiplastering coating treatment, especially a kind of aluminium alloy high temperature antiplastering fluoropolymer synergism
Coating Processes.
Background technique
Aluminium alloy is a kind of important nonferrous materials, is widely used in Aeronautics and Astronautics, automobile, machine-building, ship
The fields such as oceangoing ship, chemical industry.During manufacturing aluminium alloy part, (such as conduction, led to improve the performance of aluminium alloy part
Hot, wear-resisting, corrosion-resistant and optical property etc.), it usually needs it is surface-treated.Aluminum alloy material surface is handled at present
Method mainly has japanning facture, common anode oxidising dyeing and Seal treatment method, hard anodizing dyeing and Seal treatment
Method；Through above-mentioned conventional method treated aluminum alloy hardness, corrosion resistance, wear-resisting property etc., there are larger defects, it is difficult to full
Sufficient wear-resisting property and the demanding part of corrosion resistance need.Have been reported that display, by aluminium alloy light metal anode oxide film with
It controls the low friction polymer penetrated into or lubricant combines, then it is modified by precision heat treatment, obtain a kind
In the fine layers of metal material integral part, this coating is also referred to as synergism coat, and the comprehensive performance of synergism coat is more than one
As composite coating in meaning, there is great application value.CN1687488A discloses a kind of aluminium alloy material and fluorine polymer
Technique for treating synergism coat uses mixed acid solution electrolytic preparation horniness anode oxide film first, then aoxidizes to hard anodized
Film layer carries out expanding treatment and introduces fluoropolymer, keeps fluoropolymer and hard anodizing horizon molten finally by vacuum heat treatment
It is integrated, forms synergism coat；Specially first pass through mixed acid solution (content be the sulfuric acid of 1-10%, 0.5-10% lactic acid,
0.5-10% citric acid, 0-5% aminobenzenesulfonic acid and 0.1-0.5% aluminium ion) electrolytic oxidation obtains horniness anode oxide film, so
Expanding treatment is carried out with sulfuric acid or phosphoric acid-oxalic acid solution afterwards, then the aluminium alloy of expanding treatment is placed in fluoropolymer aqueous emulsion
Hot dipping or electrolysis obtain fluorine-containing horniness anode oxide film, and the polymerization of aluminium alloy fluorine is finally obtained after being heat-treated in vacuum heat treatment furnace
Object synergism coat.Inventor has found that the aluminium alloy synergism coat prepared using technique disclosed in CN1687488A is hard under study for action
The performances such as degree, wearability, corrosion resistance have a degree of promotion compared with common aluminum alloy, but when aluminum alloy materials because friction is sent out
After situations such as heat, heating causes aluminium alloy synergism coat temperature to rise, after especially temperature rises to 160 DEG C or more, synergism is applied
Layer can show stronger high temperature viscometrics, and (heretofore described high temperature viscometrics refer to the coating of metal surface table in the high temperature environment
The adhesion phenomenon revealed), to seriously affect the use of aluminium alloy；Such as CN1687488A work is used in non-PVC bag making field
There is adhesion phenomenon in the aluminium alloy of skill preparation, aluminium alloy synergism coat and non-PVC bag making product, seriously affect bag making production effect
Rate.Thus, exploitation hardness is high, wear-resisting property is good, excellent corrosion-proof performance, and the aluminium alloy synergism for being provided simultaneously with high temperature antiplastering performance applies
Layer processing technique is very necessary.
Summary of the invention
In order to solve the problems in the prior art, the purpose of the present invention is to provide a kind of aluminium alloy high temperature (160-185
DEG C) antiplastering synergistic fluoropolymer coating processing method.
Unless otherwise specified, number of the present invention is parts by weight, and the percentage is mass percent.
The object of the present invention is achieved like this:
A kind of aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method uses mixed acid solution electrolytic preparation aluminium alloy first
Then horniness anode oxide film carries out expanding treatment to aluminum alloy hard anodization oxidation film and introduces fluoropolymer, finally leads to
Crossing vacuum heat treatment makes fluoropolymer and aluminum alloy hard anode oxidation film fusion be formed as one synergism coat, and feature exists
In: also contain sulfonation anthracene in the mixed acid solution.
Preferably, sulfonation anthracene content is 0.5-5% in above-mentioned mixed acid solution；More preferably 1-3%.
Above-mentioned expanding treatment can carry out chemical enlargement using sulfuric acid solution or carry out electrochemistry using phosphoric acid/oxalic acid solution
Reaming mode.Wherein, in the technique that chemical enlargement processing is carried out using sulfuric acid solution, sulfuric acid content 105-199g/l, technique
Condition is 21-25 DEG C of temperature, and pore-enlargement is 4-9 minutes；The technique that electrochemistry expanding treatment is carried out using phosphoric acid/oxalic acid solution
In, phosphorus acid content be 102~200g/l, oxalic acid content 20~30g/l of range, process conditions be 20~25 DEG C of temperature, voltage 8~
15V, 5~9min of time.
To further enhance aluminium alloy synergism coat high temperature antiplastering performance of the present invention, make in the above method in vacuum heat treatment
After fluoropolymer and aluminum alloy hard anode oxidation film fusion are formed as one synergism coat, continue on synergism coat surface primary
Or fluoropolymer is repeatedly introduced, while carrying out vacuum heat treatment modification to fuse fluoropolymer and the synergism coat of formation being one
Body.
Preferably, above-mentioned repeatedly for twice or thrice.
Further to enhance aluminium alloy synergism coat high temperature antiplastering performance, the present invention is using spray coating method in synergism coat table
Continue one or many introducing fluoropolymers and carry out vacuum heat treatment modification in face；Wherein, the fluoropolymer microparticles introduced every time
Concentration range is 105-290g/L, and vacuum heat treatment process temperature range is 310-445 DEG C, and vacuum ranges are 4-
0.02Pa, heat treatment time range are 32-79 minutes.
Preferably, the present invention is repeatedly introduced fluoropolymer on synergism coat surface and is carried out vacuum heat treatment using spray coating method
It is modified；Wherein, the fluoropolymer microparticles concentration range introduced every time is 120-280g/L, the technological temperature model of vacuum heat treatment
Enclosing is 320-440 DEG C, and vacuum ranges are 1-0.01Pa, and heat treatment time range is 32-75 minutes.
Aluminum alloy materials or components of the present invention can be conventional using this field before carrying out hard anodizing processing
Technology carries out alkaline degreasing and/or alkalinity erosion washes and goes out light processing after water cleaning through nitric acid acidwashing and then carries out hard anode again
Oxidation processes.
Further to enhance aluminium alloy high temperature antiplastering performance of the present invention, the mixed acid solution electricity containing sulfonation anthracene is used first
Solution prepares aluminum alloy hard anode oxidation film, then carries out expanding treatment to aluminum alloy hard anodization oxidation film and to introduce fluorine poly-
Object is closed, then fluoropolymer is fused with aluminum alloy hard anode oxidation film by vacuum heat treatment and is integrated, obtains synergism painting
Layer (modified for the first time) then continues to introduce fluoropolymer on aforementioned synergism coat surface, while carrying out vacuum heat treatment, obtains
Second of modified synergism coat is finally introduced back into fluoropolymer on aforementioned second of modified synergism coat surface, simultaneously
Vacuum heat treatment is carried out, the modified synergism coat of third time is obtained；Wherein, during preparing aluminum alloy hard anode oxidation film: mixed
Sulfuric acid content is 4-7%, lactic acid content 3-6%, citric acid content 4-6% in acid solution, and amino phenyl sulfonyl acid content is
0.5-2%, aluminium composition 0.2-0.4%, sulfonation anthracene content are 1-3%, and process conditions are -4-1 DEG C of temperature, current density
For 2-3A/dm2, whole voltage is 90-105V, and oxidization time is 51-88 minutes；In expanding treatment technique: using sulfuric acid solution into
The processing of row chemical enlargement, sulfuric acid content 105-199g/l, process conditions are 21-25 DEG C of temperature, and pore-enlargement is 4-9 minutes；
For the first time in modified synergism coat preparation process: introducing fluoropolymer microparticles using hot dipping, fluoropolymer microparticles concentration is 45-
65g/L, process conditions are 35-68 DEG C of infiltration temperature, and the infiltration time is 12-37 minutes；In vacuum heat treatment process: vacuum degree is
1-0.05Pa, heat treatment temperature are 320-430 DEG C, and heat treatment time is 30-79 minutes；Second of modified synergism coat prepares work
In skill: using spray coating method introduce fluoropolymer microparticles, fluoropolymer microparticles concentration be 122-280g/L, coating thickness 3-8um,
Vacuum degree is 1-0.02Pa, and heat treatment temperature is 322-435 DEG C, and heat treatment time is 31-78 minutes；The modified synergism of third time applies
In layer preparation process: introducing fluoropolymer microparticles using spray coating method, fluoropolymer microparticles concentration is 110-290g/L, coating thickness
For 3-8um, vacuum degree 1-0.1Pa, heat treatment temperature is 315-445 DEG C, and heat treatment time is 35-77 minutes.
Fluoropolymer of the present invention can be using fluoropolymers such as polytetrafluoroethylene (PTFE), tetrafluoroethylene/hexafluoropropylene copolymers
Aqueous emulsion, as Du Pont's Teflon lotion, three Ai Fu company of Shanghai produce FR301 ptfe emulsion and FR463 perfluoroethylene third
Alkene lotion, Shanghai organic chemistry research institute produce P-202, F-203 polytetrafluoroethyldispersion dispersion and FS-46 fluoroplastics dispersion emulsion
Deng.
The utility model has the advantages that
Aluminium alloy high temperature antiplastering synergistic fluoropolymer coating prepared by the present invention not only has a very high rigidity, excellent wearability,
Corrosion resistance, moisture-proof moisture resistance and self-lubricating property, and there is high temperature antiplastering performance.It is coated with high temperature antiplastering prepared by the present invention
For the aluminium alloy of synergistic fluoropolymer coating in welding and cooling procedure, aluminium alloy synergism coat is not in adhesion phenomenon；Together
When aluminium alloy high temperature antiplastering synergistic fluoropolymer coating prepared by the present invention be not in adhesion wire drawing within the scope of 160-185 DEG C
The phenomenon that, meet use demand of the aluminium alloy in the anti-stick condition of high temperature.
Present invention efficiently solves the high temperature adhesive problems of non-PVC bag making technique, are applied to non-PVC mold
Surface treatment is such as used for the surface treatment of non-PVC bag making production line particular manufacturing craft, can greatly improve non-PVC bag making production efficiency,
Mold reliability and durability are greatly improved simultaneously；In addition, the present invention is difficult to the welding for solving aluminium alloy trilamellar membrane, five tunics
Topic, rosin joint film problem etc. have highly important application value.
The present invention can also effectively control the film forming speed of aluminum alloy substrate film layer, the horniness anode oxide film toughness of formation
It is good, overcome the big disadvantage of ordinary rigid anode oxide film brittleness, and the aluminium alloy high temperature antiplastering fluoropolymer synergism prepared
Coating uniformity, compactness are very good, further improve aluminium alloy synergism coat intensity, hardness and self-lubrication.
Aluminium alloy high temperature antiplastering antiplastering synergistic fluoropolymer coating prepared by the present invention is in ater, and light shine is good, and
Coating is not faded, does not show money or valuables one carries unintentionally, is not fallen off, in photoelectric instrument such as sighting instrument, optical ranging system, electronics and IT products and computer
Etc. there is in the protective treatment of aluminums key components and parts great advantage.
Aluminium alloy high temperature antiplastering synergistic fluoropolymer coating prepared by the present invention also has low temperature antiplastering performance, in low temperature ring
Still there is preferable adhesion in border, the drag reduction component of high-altitude vehicle can be used for as drag-reducing coating.
Specific embodiment
The present invention is specifically described below by specific embodiment, it is pointed out here that following embodiment is served only for this hair
It is bright to be further described, it should not be understood as limiting the scope of the invention, those of ordinary skill in the art are according to above-mentioned
Summary of the invention makes some nonessential modifications and adaptations to the present invention, all falls in the scope of protection of the present invention.All originals of the present invention
Material and reagent are the commercial product that those of ordinary skill in the art know.
Embodiment 1
Negated PVC bag making 7075 aluminium alloys (Al-Zn-Mg-Cu 7 series extra super duralumin) mold exemplar, it is de- in 61 DEG C with alkaline degreaser
Rouge is handled 8 minutes, and water cleaning is placed on 62 DEG C of erosions in the sodium hydroxide solution of 42g/l and washes 3 minutes, removes the oxygen of aluminum alloy surface
Change film, obtains the aluminum alloy mould exemplar after erosion is washed；The nitric acid that aluminum alloy mould exemplar after aforementioned erosion is washed is placed in 21% is molten
Pickling goes out light processing 3 minutes in liquid, removes dust and residue that pickling generates, the aluminum alloy mould exemplar after obtaining pickling；
Aluminum alloy mould exemplar after aforementioned pickling is placed in progress hard anodizing processing in mixed acid solution, after water cleaning
To aluminum alloy hard anode oxidation film (inventor observes that aluminum alloy hard anode oxidation film is highly uniform)；Wherein, nitration mixture is molten
Sulfuric acid content is 5% in liquid, lactic acid content 4%, citric acid content 0.8%, and sulfonation anthracene content is 2.0%, amino phenyl sulfonyl
Acid content is 0.8%, Al3+Content is 0.25%；The technological temperature of hard anodizing is -3 DEG C, current density 2.5A/
dm2, whole voltage 95V, oxidization time 63 minutes；Aluminum alloy hard anode oxidation film thickness control is at 22 μm；
Aforementioned aluminum alloy hard anode oxidation film is placed in by carrying out chemical enlargement in 159g/l sulfuric acid (98%) reaming solution
Reason, water is cleaned and is dried up with cold wind after reaming；Wherein temperature is 22 DEG C, and pore-enlargement is 6 minutes；
Hot dipping introduces fluoropolymer (modified for the first time): the aluminum alloy hard anode oxidation film after aforementioned reaming is placed in 48g/
In the ptfe emulsion solution of l in 39 DEG C hot dipping 18 minutes, dried in air after taking-up, then place it in vacuum drying oven,
1.0 (pas) are evacuated to, is heat-treated 35 minutes in 382 DEG C, is cooled to 150 DEG C of closing vacuum systems, removes it with naval's pug
Surface residue obtains aluminium alloy synergistic fluoropolymer coating；
Spray coating method introduces fluoropolymer (second modified): by aforementioned gained aluminium alloy synergistic fluoropolymer coating naval's pug
It cleans out, is then placed in air with acetone-ethanol mixed solvent (mass ratio=1:1 of acetone and ethyl alcohol) coating cleaning
It dries, is then the ptfe emulsion (spray layer thickness is controlled at 5 μm) of 125g/l in synergism coat surface spraying concentration,
It after being dried in air, places it in vacuum drying oven, is evacuated to 0.08Pa (pa), be heat-treated 42 minutes, be cooled in 370 DEG C
150 DEG C of closing vacuum systems finally remove sample surface residue with naval's pug, obtain aluminium alloy high temperature antiplastering fluoropolymer
Synergism coat.
Embodiment 2
7A04T6 (Al-Zn-Mg-Cu 7 series extra super duralumin) aluminum alloy mould exemplar is taken, is divided with alkaline degreaser in 74 DEG C of ungrease treatments 9
Clock, water cleaning are placed on 73 DEG C of erosions in the sodium hydroxide solution of 49g/l and wash 5 minutes, remove the oxidation film of aluminum alloy surface, obtain
Lose the aluminum alloy mould exemplar after washing；Aluminum alloy mould exemplar after aforementioned erosion is washed is placed in pickling in 29% nitric acid solution and goes out
Light processing 9 minutes, remove the dust and residue that pickling generates, the aluminum alloy mould exemplar after obtaining pickling；
Aluminum alloy mould exemplar after aforementioned pickling is placed in progress hard anodizing processing in mixed acid solution, after water cleaning
To aluminum alloy hard anode oxidation film (inventor observes that aluminum alloy hard anode oxidation film is highly uniform)；Wherein, nitration mixture is molten
Sulfuric acid content is 5% in liquid, lactic acid content 6%, citric acid content 4%, and sulfonation anthracene content is 1%, and aminobenzenesulfonic acid contains
Amount is 1.5%, Al3+Content is 0.35%；The technological temperature of hard anodizing is 1 DEG C, current density 3A/dm2, whole voltage
105V, oxidization time 77 minutes；Aluminum alloy hard anode oxidation film thickness control is at 28 μm；
Aforementioned aluminum alloy hard anode oxidation film is placed in the mixed solution of 175g/l phosphoric acid (85%) and 25g/l oxalic acid and is carried out
Electrochemical ac expanding treatment, water is cleaned and is dried up with cold wind after reaming；Wherein, using workpiece as anode in chambering process, stereotype
For cathode, temperature is 24 DEG C, voltage 38V, and pore-enlargement is 8 minutes；
Hot dipping introduces fluoropolymer (modified for the first time): the aluminum alloy hard anode oxidation film after aforementioned reaming is placed in 45g/
In the ptfe emulsion solution of l in 68 DEG C hot dipping 37 minutes, dry, place it in vacuum drying oven in air after taking-up, take out
Vacuum is heat-treated 49 minutes in 390 DEG C to 0.05 (pa), is cooled to 150 DEG C of closing vacuum systems, removes its table with naval's pug
Face residue obtains aluminium alloy synergistic fluoropolymer coating；
Spray coating method introduces fluoropolymer (second modified): by aforementioned gained aluminium alloy synergistic fluoropolymer coating naval's pug
It cleans out, is then placed in air with acetone-ethanol mixed solvent (mass ratio=1:1 of acetone and ethyl alcohol) coating cleaning
It dries, is then the ptfe emulsion (spray layer thickness is controlled at 8 μm) of 250g/l in synergism coat surface spraying concentration,
It after being dried in air, places it in vacuum drying oven, is evacuated to 0.02Pa (pa), be heat-treated 70 minutes, be cooled in 410 DEG C
150 DEG C of closing vacuum systems finally remove sample surface residue with naval's pug, obtain twice-modified aluminium alloy high temperature resistance
Viscous synergistic fluoropolymer coating.
Embodiment 3-9 and comparative example
Negated PVC bag making 7075 aluminium alloys (Al-Zn-Mg-Cu 7 series extra super duralumin) mold exemplar, referring to the step of embodiment 1, root
Aluminium alloy high temperature antiplastering synergistic fluoropolymer coating is prepared according to technological parameter in table 1.5-7 of the embodiment of the present invention is introduced in spray coating method
Fluoropolymer carry out second it is modified obtain new synergism coat after, spraying again introduces fluoropolymer to carry out third time modified,
Fluoropolymer and the synergism coat of formation is fused to be integrated.
The technological parameter of table 1 embodiment 3-9 and comparative example
Performance test: the aluminium alloy synergism coat exemplar for taking comparative example and embodiment 1-9 to prepare observes exemplar table
Face, and be tested for the property according to corresponding code requirement: it is thick with micro- metallographic method test synergism coat by the regulation of GB6462
Degree；By the regulation of GB9790, synergism coat hardness is tested with micro- metallographic method；By the regulation of ASTMB117, carry out 500 hours
After 5% neutral salt spray test, is evaluated by ASTMD1654, Corrosion protection grade is carried out to it；Separately take comparative example and embodiment 1-9
The aluminium alloy synergism coat exemplar of preparation, which is assemblied on non-PVC full automatic bag making, filling and sealing machine, carries out soldering test, tests aluminium alloy
Adhesive of the synergism coat exemplar in welding and cooling procedure, test result are shown in Table 2.
2 aluminium alloy high temperature antiplastering synergistic fluoropolymer coating test result of table
As shown in Table 2, the aluminium alloy high temperature antiplastering synergistic fluoropolymer coating of 1-9 of embodiment of the present invention preparation is in uniformly black
Color, feel lubrication, surface hydrophobic hate oil, are dust-proof, and with a thickness of 27-44um, uniformity is very good, and Vickers hardness is in 500-600HV
Between, Corrosion protection grade is 8 grades of qualifications, and the phenomenon that adhesion wire drawing is not present within the scope of 160-185 DEG C, and service performance is obvious
Better than the synergism coat of comparative example preparation.Aluminium alloy high temperature antiplastering synergistic fluoropolymer coating of the present invention is at 160-185 DEG C
Adhesion, to the welding problem for solving aluminium alloy trilamellar membrane, five tunics, rosin joint film problem etc. has highly important application
Value.
Claims (9)
1. a kind of aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method is closed using mixed acid solution electrolytic preparation aluminium first
Then golden horniness anode oxide film carries out expanding treatment to aluminum alloy hard anodization oxidation film and introduces fluoropolymer, finally
Fluoropolymer and aluminum alloy hard anode oxidation film are fused by vacuum heat treatment and is formed as one synergism coat, and feature exists
In: also contain sulfonation anthracene in the mixed acid solution.
2. aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method according to claim 1, it is characterised in that: mixed
Sulfonation anthracene content is 0.5-5% in acid solution.
3. aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method according to claim 1, it is characterised in that: mixed
Sulfonation anthracene content is 1-3% in acid solution.
4. aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method according to claim 1,2 or 3, feature exist
In: after vacuum heat treatment makes fluoropolymer and aluminum alloy hard anode oxidation film fusion be formed as one synergism coat, assisting
It closes coating surface and continues one or many introducing fluoropolymers, while carrying out that vacuum heat treatment is modified to be made fluoropolymer and formed
Synergism coat fusion is integrated.
5. aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method according to claim 4, it is characterised in that: institute
It states repeatedly as twice or thrice.
6. aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method according to claim 4, it is characterised in that: this
Invention continues one or many introducing fluoropolymers and carries out vacuum heat treatment to be modified using spray coating method on synergism coat surface；Its
In, the fluoropolymer microparticles concentration range introduced every time is 105-290g/L, and vacuum heat treatment process temperature range is
310-445 DEG C, vacuum ranges are 4-0.02Pa, and heat treatment time range is 32-79 minutes.
7. aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method according to claim 4, it is characterised in that: this
Invention is repeatedly introduced fluoropolymer and carries out vacuum heat treatment and is modified using spray coating method on synergism coat surface；Wherein, draw every time
The fluoropolymer microparticles concentration range entered is 120-280g/L, and the Process temperature ranges of vacuum heat treatment are 320-440 DEG C,
Vacuum ranges are 1-0.01Pa, and heat treatment time range is 32-75 minutes.
8. aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method according to claim 1, it is characterised in that: this
Invention is repeatedly introduced fluoropolymer and carries out vacuum heat treatment and is modified using spray coating method on synergism coat surface；Wherein, draw every time
The fluoropolymer microparticles concentration range entered is 120-280g/L, and the Process temperature ranges of vacuum heat treatment are 320-440 DEG C,
Vacuum ranges are 1-0.01Pa, and heat treatment time range is 32-75 minutes.
9. aluminium alloy high temperature antiplastering synergistic fluoropolymer coating processing method according to claim 1, it is characterised in that: first
The mixed acid solution electrolytic preparation aluminum alloy hard anode oxidation film containing sulfonation anthracene is first used, then to aluminum alloy hard anodization
Oxidation film carries out expanding treatment and introduces fluoropolymer, then makes fluoropolymer and aluminum alloy hard anode by vacuum heat treatment
Oxidation film fusion is integrated, and obtains modified synergism coat for the first time, then continues to introduce fluorine polymerization on aforementioned synergism coat surface
Object, while vacuum heat treatment is carried out, second of modified synergism coat is obtained, finally in aforementioned second of modified synergism coat
Surface is introduced back into fluoropolymer, while carrying out vacuum heat treatment, obtains the modified synergism coat of third time；Wherein, aluminium conjunction is prepared
During golden horniness anode oxide film: sulfuric acid content is 4-7%, lactic acid content 3-6%, citric acid content 4- in mixed acid solution
6%, amino phenyl sulfonyl acid content is 0.5-2%, and aluminium composition 0.2-0.4%, sulfonation anthracene content is 1-3%, and process conditions are temperature
- 4-1 DEG C of degree, current density 2-3A/dm2, whole voltage is 90-105V, and oxidization time is 51-88 minutes；Expanding treatment technique
In: chemical enlargement processing, sulfuric acid content 105-199g/l are carried out using sulfuric acid solution, process conditions are 21-25 DEG C of temperature, are expanded
The hole time is 4-9 minutes；For the first time in modified synergism coat preparation process: introducing fluoropolymer microparticles using hot dipping, fluorine is poly-
Conjunction object particle concentration is 45-65g/L, and process conditions are 35-68 DEG C of infiltration temperature, and the infiltration time is 12-37 minutes；At Vacuum Heat
In science and engineering skill: vacuum degree 1-0.05Pa, heat treatment temperature are 320-430 DEG C, and heat treatment time is 30-79 minutes；Second
In modified synergism coat preparation process: introducing fluoropolymer microparticles using spray coating method, fluoropolymer microparticles concentration is 122-280g/
L, coating thickness 3-8um, vacuum degree 1-0.02Pa, heat treatment temperature are 322-435 DEG C, and heat treatment time is 31-78 points
Clock；In the modified synergism coat preparation process of third time: introducing fluoropolymer microparticles using spray coating method, fluoropolymer microparticles concentration is
110-290g/L, coating thickness 3-8um, vacuum degree 1-0.1Pa, heat treatment temperature are 315-445 DEG C, and heat treatment time is
35-77 minutes.
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