CN108611672A - Hard Anodic Oxidation of Aluminum Alloy electrolyte, preparation method and application - Google Patents
Hard Anodic Oxidation of Aluminum Alloy electrolyte, preparation method and application Download PDFInfo
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 62
- 230000003647 oxidation Effects 0.000 title claims abstract description 61
- 239000003792 electrolyte Substances 0.000 title claims abstract description 49
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 77
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 76
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical class S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000004411 aluminium Substances 0.000 claims abstract description 44
- 150000007524 organic acids Chemical class 0.000 claims abstract description 21
- 229910052582 BN Inorganic materials 0.000 claims abstract description 11
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920005862 polyol Polymers 0.000 claims abstract description 5
- 150000003077 polyols Chemical class 0.000 claims abstract description 5
- 235000005985 organic acids Nutrition 0.000 claims abstract 3
- 238000000034 method Methods 0.000 claims description 27
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 150000005846 sugar alcohols Polymers 0.000 claims description 21
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 14
- RQFQJYYMBWVMQG-IXDPLRRUSA-N chitotriose Chemical compound O[C@@H]1[C@@H](N)[C@H](O)O[C@H](CO)[C@H]1O[C@H]1[C@H](N)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)N)[C@@H](CO)O1 RQFQJYYMBWVMQG-IXDPLRRUSA-N 0.000 claims description 13
- 235000019441 ethanol Nutrition 0.000 claims description 13
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 239000007795 chemical reaction product Substances 0.000 claims description 12
- 229940074391 gallic acid Drugs 0.000 claims description 9
- 235000004515 gallic acid Nutrition 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 229920001661 Chitosan Polymers 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229920001542 oligosaccharide Polymers 0.000 claims description 6
- 150000002482 oligosaccharides Chemical class 0.000 claims description 6
- 150000003870 salicylic acids Chemical class 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 3
- 238000002390 rotary evaporation Methods 0.000 claims description 3
- 229960004889 salicylic acid Drugs 0.000 claims description 3
- 240000000203 Salix gracilistyla Species 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims 1
- 239000000956 alloy Substances 0.000 abstract description 35
- 229910045601 alloy Inorganic materials 0.000 abstract description 33
- 239000011159 matrix material Substances 0.000 abstract description 32
- 238000012545 processing Methods 0.000 abstract description 27
- 230000007797 corrosion Effects 0.000 abstract description 12
- 238000005260 corrosion Methods 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 7
- 239000004566 building material Substances 0.000 abstract description 3
- 238000007789 sealing Methods 0.000 description 26
- 239000007788 liquid Substances 0.000 description 25
- 238000012360 testing method Methods 0.000 description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 22
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 238000002156 mixing Methods 0.000 description 9
- 235000011121 sodium hydroxide Nutrition 0.000 description 8
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 7
- 239000008151 electrolyte solution Substances 0.000 description 7
- 238000005530 etching Methods 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- 235000011187 glycerol Nutrition 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000007743 anodising Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910001250 2024 aluminium alloy Inorganic materials 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000004224 protection Effects 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000007542 hardness measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000000627 alternating current impedance spectroscopy Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 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
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
-
- 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
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention discloses a kind of Hard Anodic Oxidation of Aluminum Alloy electrolyte.The formula of the Hard Anodic Oxidation of Aluminum Alloy electrolyte is：10~20 parts sulfuric acids, 2~5 parts by weight organic acids, 0.1~0.3 weight polyol, 0.05~0.5 parts by weight boron nitride, 90~110 parts by weight water.Application the invention also discloses the preparation method of Hard Anodic Oxidation of Aluminum Alloy electrolyte and its in anticorrosion aluminium ally section.Hard Anodic Oxidation of Aluminum Alloy electrolyte prepared by the present invention is applied in the processing of anticorrosion aluminium ally section, pass through anodic oxidation, fine and close oxidation film is formed on alloy matrix aluminum, microhardness, wearability and the corrosion resistance and good of obtained anticorrosion aluminium ally section, can be applied to the every field such as electronics, electric power, aviation, chemical industry, building materials, traffic.
Description
Technical field
The present invention relates to a kind of aluminium alloy anode oxide electrolyte, belong to the field of surface treatment of aluminium alloy.
Background technology
Aluminium is silvery white non-ferrous metal, and density 2.70, fusing point is 657 DEG C.Aluminium and its alloy material are due to its high intensity/weight
Amount ratio, it is easily molded process and excellent physics, chemical property, in many such as electronics, electric power, aviation, chemical industry, building materials, traffic
In industrial department and daily life, it is widely used.
Aluminum alloy materials are since surface matter is soft, wears no resistance and the defects of friction coefficient is high, so needing to carry out when in use
The tribology surface modification treatment of aluminium and aluminium alloy carries out hard anodizing in aluminum alloy surface first, then closed in aluminium
Golden film surface and the internal various lubricating substances of deposition form lubricant coatings, to enable aluminum alloy to skin-friction coefficient reduction.
The surface treatment method of aluminium alloy can substantially be divided into oxidation, plating and coating etc..And the anodic oxygen in aoxidizing
Change and chemical oxidation is presently the most common surface treatment method.Aluminum or aluminum alloy anodic oxidation rear surface, which is dispersed with, largely to be received
The hole of meter level, there is higher free energy, but the surface of solids cannot be reduced as liquid by reducing the method for surface area
The surface free energy of system can only adsorb external agency to reduce the free energy of system.However, aluminium alloy is in sulfuric acid, phosphoric acid, grass
The microhardness of the anode oxide film prepared in the single electrolyte such as acid is generally relatively low, and wearability and corrosion resistance are poor, comprehensive
It is not high to close mechanical property, cannot be satisfied industrial requirement.Therefore a kind of Hard Anodic Oxidation of Aluminum Alloy electrolyte is developed, answered
With in the processing with anticorrosion aluminium, a kind of preparation method of anticorrosion aluminium improves the microhardness, wear-resisting of aluminium alloy
Property and corrosion resistance.
Invention content
Aiming at the above shortcomings existing in the prior art, technical problem to be solved by the invention is to provide a kind of aluminium alloys
The Hard Anodic Oxidation of Aluminum Alloy electrolyte is applied to anticorrosion aluminium by hard anodizing electrolyte and preparation method thereof
In the processing of proximate matter, it is prepared that microhardness is high, anticorrosion aluminium ally section of wearability and good corrosion resistance.
Specific technical solution is as follows：
A kind of Hard Anodic Oxidation of Aluminum Alloy electrolyte, including following component：10~20 parts sulfuric acids, 2~5 parts by weight
Organic acid, 0.1~0.3 weight polyol, 90~110 parts by weight water.
Specifically, the polyalcohol is one kind in glycerine, isopropanol, pentaerythrite.
It is further preferred that the polyalcohol is pentaerythrite.
Specifically, the organic acid is modified salicylic acid and/or gallic acid.
Another technical solution of the present invention：
A kind of Hard Anodic Oxidation of Aluminum Alloy electrolyte, is grouped as by following group：10~20 parts sulfuric acids, 2~5 weight
Part organic acid, 0.1~0.3 weight polyol, 0.05~0.5 parts by weight boron nitride, 90~110 parts by weight water.
Preferably, the polyalcohol is one kind in glycerine, isopropanol, pentaerythrite.
Preferably, the polyalcohol is pentaerythrite.
Preferably, the organic acid is modified salicylic acid and/or gallic acid.
Preferably, the modified salicylic acid is prepared by following methods, and described part is parts by weight：
(1) 1-3 parts of chitosan oligosaccharides and 80-120 parts of water are mixed, obtains chitosan oligosaccharide aqueous solution, be 10% with mass fraction
Sodium hydrate aqueous solution adjust chitosan oligosaccharide aqueous solution pH value be 7.5-8.5, add 1-2 parts of salicylic acids, 60-70 DEG C with
100-300 revs/min is stirred 80-120 minutes, and reaction product is obtained；
(2) reaction product in vacuum degree is 0.05-0.2MPa by 100 revs/min of setting Rotary Evaporators rotating speed, and temperature is
60-70 DEG C of rotary evaporation obtains solid to no moisture；
(3) by solid and ethyl alcohol in mass ratio 1：(80-100) is mixed, at 15-25 DEG C with 100-300 revs/min of stirring 10-
20 minutes, then centrifuged 8-12 minutes with 3000-5000 revs/min, what is obtained is deposited in 60-70 DEG C of drying to constant weight, is modified
Salicylic acid.
The present invention also provides application of the above-mentioned Hard Anodic Oxidation of Aluminum Alloy electrolyte in anticorrosion aluminium.Tool
Body technique scheme is as follows：
A kind of preparation method of anticorrosion aluminium ally section, includes the following steps：
(1) oil removing；
(2) alkaline etching；
(3) it neutralizes；
(4) anodic oxidation；
(5) sealing of hole.
Preferably, the preparation method of the anticorrosion aluminium ally section, includes the following steps：
(1) oil removing：By alloy matrix aluminum in 15-20 DEG C, the sulfuric acid solution of a concentration of 100-140g/L 3-5 points of dipping
Clock takes out, is eluted with water；
(2) alkaline etching：In temperature it is 35-45 DEG C, the hydrogen-oxygen of a concentration of 30-50g/L by the alloy matrix aluminum of step (1) processing
Change and impregnated 3-5 minutes in sodium solution, takes out, be eluted with water；
(3) it neutralizes：By the alloy matrix aluminum of step (2) processing in 15-20 DEG C, the sulfuric acid solution of a concentration of 100-140g/L
Middle dipping 2-4 minutes takes out, is eluted with water；
(4) anodic oxidation：The alloy matrix aluminum of step (3) processing is subjected to anodic oxidation in the electrolytic solution, aluminium alloy is
Anode, aluminium sheet are cathode, and wherein oxidation voltage is 15-20V, current density 1-2A/dm2, electrolyte temperature is 15-20 DEG C,
Oxidization time 20-40 minutes；
(5) sealing of hole：The alloy matrix aluminum of step (4) processing is impregnated 15-30 minutes in 85-95 DEG C of pore-sealing liquid, is taken
Go out to drain surface moisture, it is 2-4 hours dry at 80-90 DEG C, obtain anticorrosion aluminium ally section.
Preferably, the electrolyte is prepared by following methods, and described part is parts by weight：By 10-20 parts of sulfuric acid, have
2-5 parts of machine acid, 0.1-0.3 parts of polyalcohol are added in 100 parts of water, are stirred 5-10 minutes, are electrolysed with 100-300 revs/min
Liquid.
Preferably, the electrolyte is prepared by following methods, and described part is parts by weight：By 10-20 parts of sulfuric acid, have
2-5 parts of machine acid, 0.1-0.3 parts of polyalcohol are added in 90~110 parts of water, are stirred 5-10 minutes with 100-300 revs/min, then are added
Enter 0.05-0.5 parts of boron nitride, is stirred 20-30 minutes with 100-300 revs/min, obtain electrolyte.
Preferably, the pore-sealing liquid is prepared by following methods, and described part is parts by weight：By 1-2 parts of cerous nitrate and
100 parts of mixing of water, are stirred 10-20 minutes with 100-300 revs/min, obtain pore-sealing liquid.
Preferably, the organic acid is modified salicylic acid and/or gallic acid.
It is highly preferred that the organic acid is the mixture of modified salicylic acid and gallic acid, the modified salicylic acid and do not have
The mass ratio of gallate-based is 1：(3-5).
Preferably, the polyalcohol is one kind in glycerine, isopropanol, pentaerythrite.
Preferably, the polyalcohol is pentaerythrite.
Preferably, the modified salicylic acid is prepared by following methods, and described part is parts by weight：
(1) 1-3 parts of chitosan oligosaccharides and 80-120 parts of water are mixed, obtains chitosan oligosaccharide aqueous solution, be 10% with mass fraction
Sodium hydrate aqueous solution adjust chitosan oligosaccharide aqueous solution pH value be 7.5-8.5, add 1-2 parts of salicylic acids, 60-70 DEG C with
100-300 revs/min is stirred 80-120 minutes, and reaction product is obtained；
(2) 100 revs/min of Rotary Evaporators rotating speed is set, is in vacuum degree by reaction product
0.05-0.2MPa, temperature be 60-70 DEG C of rotary evaporation to no moisture, obtain solid；
(3) by solid and ethyl alcohol in mass ratio 1：(80-100) is mixed, at 15-25 DEG C with 100-300 revs/min of stirring 10-
20 minutes, then centrifuged 8-12 minutes with 3000-5000 revs/min, what is obtained is deposited in 60-70 DEG C of drying to constant weight, is modified
Salicylic acid.
Hard Anodic Oxidation of Aluminum Alloy electrolyte of the present invention in the preparation of anticorrosion aluminium ally section by anodic oxidation,
Fine and close oxidation film, microhardness, wearability and the corrosion resistant of obtained anticorrosion aluminium ally section are formed on alloy matrix aluminum
Corrosion can be good, can be applied to the every field such as electronics, electric power, aviation, chemical industry, building materials, traffic.
Specific implementation mode
In the present invention, if not refering in particular to, all devices and raw material is commercially available or the industry is common are following
Method in embodiment is unless otherwise instructed this field conventional method.
The micro-hardness testing of oxidation film：Using FischerHM2000 types microhardness tester (German Fei Xier test equipments
Co., Ltd produces) Vickers hardness of test oxidation film, load 500mN, load time 20s, the number of parallel sample is 3
A, each parallel sample is chosen 10 equally distributed different test points and is measured, and the microhardness for sample is averaged.
The wearability of oxidation film is studied using friction wear testing machine (CSEM companies of Switzerland produce, model THT07-135),
It is 25 DEG C of tests, the ZrO that friction bead is diameter 6mm in temperature2Ceramic wear-resisting ball, friction velocity 4cm/s, load 5N,
Friction length is 8mm, and to avoid single from rubbing, revolution is excessive causes anode oxide film worn out and total friction revolution is very few makes
Be unable to measure very little at wear extent, all samples rub 2 times 350 turns, record friction test before and after quality, as follows
Calculate mass loss rate：[(m1-m2)/m1] × 100%, wherein m1For the quality of aluminium alloy extrusions before friction test, m2For friction
The quality of aluminium alloy extrusions after experiment.
Corrosion resistance is tested：With reference to Tian Lianpeng, left Yu etc.《Aluminium alloy anode oxide film Nickel acetate sealing method rotproofness is ground
Study carefully》, corrosion and protection, 2006.27 (2), 2.4 section in method tested, it is specific as follows：Using three-electrode system, with full
It is reference electrode with calomel electrode, platinum electrode is auxiliary electrode, and test oxidation film is in acid (pH=3.0) solution of 1mol/LNaCl
In ac impedance spectroscopy (test signal be amplitude 10mV sine wave, the frequency of measurement is by 100kHz to 0.01Hz, test software
For Powersine) evaluate the corrosion resisting property of oxidation film.PH value, test temperature are adjusted by the way that hydrochloric acid is added into NaCl solution
Degree is 20 DEG C.Concrete outcome evaluates the corrosion resistance of oxidation film with frequency for the impedance value of 100HZ.
Sulfuric acid wins the concentrated sulfuric acid for the purity 98wt% that chemical industry has company to produce using Tianjin enlightening.
Sodium hydroxide, forever scientific and technological (Jiangsu) Co., Ltd production of China's chemistry.
Boron nitride uses the article No. that Qinghe County Bo Zuan metal materials Co., Ltd produces for NO-N-003-1DE boron nitride,
Average grain diameter 100nm.
Cerous nitrate, No. CAS：13093-17-9, Shanghai ShuaiSun Industrial Co., Ltd.s provide.
Salicylic acid, Shanghai Mike's woods biochemical technology Co., Ltd provide, product identification：S817529.
Gallic acid, No. CAS：149-91-7, the Zhangjiajie bio tech ltd Jiu Rui provide.
Pentaerythrite, Shanghai Mike's woods biochemical technology Co., Ltd provide, product identification：P815603.
Glycerine, Shanghai Mike's woods biochemical technology Co., Ltd provide, product identification：G6201.
Isopropanol, Shanghai Mike's woods biochemical technology Co., Ltd provide, product identification：I811924.
Chitosan oligosaccharide, the production of Shaanxi Sen Lang biochemical industries Co., Ltd, molecular weight 2000, deacetylation 90.5%.
Ethyl alcohol, the absolute ethyl alcohol of use scientific and technological (Jiangsu) Co., Ltd production of China's chemistry forever.
Aluminum alloy base material, it is 50mm × 50mm × 1mm, 2024 aluminium alloyings that 2024 aluminium alloys, volume are used in embodiment
It learns component and see the table below 1：
Table 1：2024 aluminum alloy chemically component tables
| Element | Si | Fe | Cu | Mn | Mg | Zn | Ni | Cr | Al |
| Mass fraction, % | 0.5 | 0.5 | 4.5 | 0.53 | 1.4 | 0.3 | 0.1 | 0 | Surplus |
Embodiment 1
A kind of preparation method of anticorrosion aluminium ally section, includes the following steps：
(1) oil removing：Alloy matrix aluminum is impregnated 4 minutes in 18 DEG C, the sulfuric acid solution of a concentration of 120g/L, takes out, uses
Water is cleaned；
(2) alkaline etching：By step (1) processing alloy matrix aluminum temperature be 40 DEG C, the sodium hydroxide of a concentration of 40g/L it is molten
It is impregnated 4 minutes in liquid, takes out, be eluted with water；
(3) it neutralizes：The alloy matrix aluminum of step (2) processing is impregnated 3 in 18 DEG C, the sulfuric acid solution of a concentration of 120g/L
Minute, it takes out, is eluted with water；
(4) anodic oxidation：The alloy matrix aluminum of step (3) processing is subjected to anodic oxidation in the electrolytic solution, aluminium alloy is
Anode, aluminium sheet are cathode, and wherein oxidation voltage is 18V, current density 1.5A/dm2, electrolyte temperature is 18 DEG C, when oxidation
Between 30 minutes；
(5) sealing of hole：The alloy matrix aluminum of step (4) processing is impregnated 20 minutes in 90 DEG C of pore-sealing liquid, taking-up drains
Surface moisture, it is 3 hours dry at 85 DEG C, obtain anticorrosion aluminium ally section.
The electrolyte is prepared by following methods, and described part is parts by weight：By 15 parts of sulfuric acid, 3 parts of organic acid, more
0.2 part of first alcohol is added in 100 parts of water, is stirred 8 minutes with 200 revs/min, is obtained electrolyte.
The pore-sealing liquid is prepared by following methods, and described part is parts by weight：By 100 parts of 1.5 parts of cerous nitrate and water
Mixing is stirred 15 minutes with 200 revs/min, obtains pore-sealing liquid.
The polyalcohol is glycerine.
The organic acid is modified salicylic acid, and the modified salicylic acid is prepared by following methods, and described part is attached most importance to
Measure part：
(1) 2 parts of chitosan oligosaccharides and 100 parts of water are mixed, obtains chitosan oligosaccharide aqueous solution, the hydroxide for being 10% with mass fraction
The pH value that sodium water solution adjusts chitosan oligosaccharide aqueous solution is 8.0, adds 1.5 parts of salicylic acids, at 65 DEG C with 200 revs/min of stirrings 100
Minute, obtain reaction product；
(2) reaction product in vacuum degree is 0.1MPa by 100 revs/min of setting Rotary Evaporators rotating speed, and temperature is 65 DEG C of rotations
Turn to be evaporated to no moisture, obtains solid；
(3) by solid and ethyl alcohol in mass ratio 1：90 mixing are stirred 15 minutes at 20 DEG C with 200 revs/min, then with 4000
Rev/min centrifugation 10 minutes, what is obtained is deposited in 65 DEG C of dryings to constant weight, obtains modified salicylic acid.
Embodiment 2
A kind of preparation method of anticorrosion aluminium ally section, includes the following steps：
(1) oil removing：Alloy matrix aluminum is impregnated 4 minutes in 18 DEG C, the sulfuric acid solution of a concentration of 120g/L, takes out, uses
Water is cleaned；
(2) alkaline etching：By step (1) processing alloy matrix aluminum temperature be 40 DEG C, the sodium hydroxide of a concentration of 40g/L it is molten
It is impregnated 4 minutes in liquid, takes out, be eluted with water；
(3) it neutralizes：The alloy matrix aluminum of step (2) processing is impregnated 3 in 18 DEG C, the sulfuric acid solution of a concentration of 120g/L
Minute, it takes out, is eluted with water；
(4) anodic oxidation：The alloy matrix aluminum of step (3) processing is subjected to anodic oxidation in the electrolytic solution, aluminium alloy is
Anode, aluminium sheet are cathode, and wherein oxidation voltage is 18V, current density 1.5A/dm2, electrolyte temperature is 18 DEG C, when oxidation
Between 30 minutes；
(5) sealing of hole：The alloy matrix aluminum of step (4) processing is impregnated 20 minutes in 90 DEG C of pore-sealing liquid, taking-up drains
Surface moisture, it is 3 hours dry at 85 DEG C, obtain anticorrosion aluminium ally section.
The electrolyte is prepared by following methods, and described part is parts by weight：By 15 parts of sulfuric acid, 3 parts of organic acid, more
0.2 part of first alcohol is added in 100 parts of water, is stirred 8 minutes with 200 revs/min, is added 0.1 part of boron nitride, is stirred with 200 revs/min
25 minutes, obtain electrolyte.
The pore-sealing liquid is prepared by following methods, and described part is parts by weight：By 100 parts of 1.5 parts of cerous nitrate and water
Mixing is stirred 15 minutes with 200 revs/min, obtains pore-sealing liquid.
The polyalcohol is glycerine.
The organic acid is modified salicylic acid, and the modified salicylic acid is prepared by following methods, and described part is attached most importance to
Measure part：
(1) 2 parts of chitosan oligosaccharides and 100 parts of water are mixed, obtains chitosan oligosaccharide aqueous solution, the hydroxide for being 10% with mass fraction
The pH value that sodium water solution adjusts chitosan oligosaccharide aqueous solution is 8.0, adds 1.5 parts of salicylic acids, at 65 DEG C with 200 revs/min of stirrings 100
Minute, obtain reaction product；
(2) reaction product in vacuum degree is 0.1MPa by 100 revs/min of setting Rotary Evaporators rotating speed, and temperature is 65 DEG C of rotations
Turn to be evaporated to no moisture, obtains solid；
(3) by solid and ethyl alcohol in mass ratio 1：90 mixing are stirred 15 minutes at 20 DEG C with 200 revs/min, then with 4000
Rev/min centrifugation 10 minutes, what is obtained is deposited in 65 DEG C of dryings to constant weight, obtains modified salicylic acid.
Embodiment 3
It is substantially the same manner as Example 2, it differs only in, the polyalcohol is isopropanol.
Embodiment 4
It is substantially the same manner as Example 2, it differs only in：The polyalcohol is pentaerythrite.
Comparative example 1
A kind of preparation method of anticorrosion aluminium ally section, includes the following steps：
(1) oil removing：Alloy matrix aluminum is impregnated 4 minutes in 18 DEG C, the sulfuric acid solution of a concentration of 120g/L, takes out, uses
Water is cleaned；
(2) alkaline etching：By step (1) processing alloy matrix aluminum temperature be 40 DEG C, the sodium hydroxide of a concentration of 40g/L it is molten
It is impregnated 4 minutes in liquid, takes out, be eluted with water；
(3) it neutralizes：The alloy matrix aluminum of step (2) processing is impregnated 3 in 18 DEG C, the sulfuric acid solution of a concentration of 120g/L
Minute, it takes out, is eluted with water；
(4) anodic oxidation：The alloy matrix aluminum of step (3) processing is subjected to anodic oxidation in the electrolytic solution, aluminium alloy is
Anode, aluminium sheet are cathode, and wherein oxidation voltage is 18V, current density 1.5A/dm2, electrolyte temperature is 18 DEG C, when oxidation
Between 30 minutes；
(5) sealing of hole：The alloy matrix aluminum of step (4) processing is impregnated 20 minutes in 90 DEG C of pore-sealing liquid, taking-up drains
Surface moisture, it is 3 hours dry at 85 DEG C, obtain anticorrosion aluminium ally section.
The electrolyte is prepared by following methods, and described part is parts by weight：By 15 parts of sulfuric acid, 3 parts of organic acid, more
0.2 part of first alcohol is added in 100 parts of water, is stirred 8 minutes with 200 revs/min, is added 0.1 part of boron nitride, is stirred with 200 revs/min
25 minutes, obtain electrolyte.
The pore-sealing liquid is prepared by following methods, and described part is parts by weight：By 100 parts of 1.5 parts of cerous nitrate and water
Mixing is stirred 15 minutes with 200 revs/min, obtains pore-sealing liquid.
The polyalcohol is pentaerythrite.
The organic acid is salicylic acid.
Embodiment 5
A kind of preparation method of anticorrosion aluminium ally section, includes the following steps：
(1) oil removing：Alloy matrix aluminum is impregnated 4 minutes in 18 DEG C, the sulfuric acid solution of a concentration of 120g/L, takes out, uses
Water is cleaned；
(2) alkaline etching：By step (1) processing alloy matrix aluminum temperature be 40 DEG C, the sodium hydroxide of a concentration of 40g/L it is molten
It is impregnated 4 minutes in liquid, takes out, be eluted with water；
(3) it neutralizes：The alloy matrix aluminum of step (2) processing is impregnated 3 in 18 DEG C, the sulfuric acid solution of a concentration of 120g/L
Minute, it takes out, is eluted with water；
(4) anodic oxidation：The alloy matrix aluminum of step (3) processing is subjected to anodic oxidation in the electrolytic solution, aluminium alloy is
Anode, aluminium sheet are cathode, and wherein oxidation voltage is 18V, current density 1.5A/dm2, electrolyte temperature is 18 DEG C, when oxidation
Between 30 minutes；
(5) sealing of hole：The alloy matrix aluminum of step (4) processing is impregnated 20 minutes in 90 DEG C of pore-sealing liquid, taking-up drains
Surface moisture, it is 3 hours dry at 85 DEG C, obtain anticorrosion aluminium ally section.
The electrolyte is prepared by following methods, and described part is parts by weight：By 15 parts of sulfuric acid, 3 parts of organic acid, more
0.2 part of first alcohol is added in 100 parts of water, is stirred 8 minutes with 200 revs/min, is added 0.1 part of boron nitride, is stirred with 200 revs/min
25 minutes, obtain electrolyte.
The pore-sealing liquid is prepared by following methods, and described part is parts by weight：By 100 parts of 1.5 parts of cerous nitrate and water
Mixing is stirred 15 minutes with 200 revs/min, obtains pore-sealing liquid.
The polyalcohol is pentaerythrite.
The organic acid is gallic acid.
Obtain the microhardness 517Hv of anticorrosion aluminium ally section, mass loss rate 4.13%, impedance value 1.74 × 106
Ω/cm2。
Embodiment 6
A kind of preparation method of anticorrosion aluminium ally section, includes the following steps：
(1) oil removing：Alloy matrix aluminum is impregnated 4 minutes in 18 DEG C, the sulfuric acid solution of a concentration of 120g/L, takes out, uses
Water is cleaned；
(2) alkaline etching：By step (1) processing alloy matrix aluminum temperature be 40 DEG C, the sodium hydroxide of a concentration of 40g/L it is molten
It is impregnated 4 minutes in liquid, takes out, be eluted with water；
(3) it neutralizes：The alloy matrix aluminum of step (2) processing is impregnated 3 in 18 DEG C, the sulfuric acid solution of a concentration of 120g/L
Minute, it takes out, is eluted with water；
(4) anodic oxidation：The alloy matrix aluminum of step (3) processing is subjected to anodic oxidation in the electrolytic solution, aluminium alloy is
Anode, aluminium sheet are cathode, and wherein oxidation voltage is 18V, current density 1.5A/dm2, electrolyte temperature is 18 DEG C, when oxidation
Between 30 minutes；
(5) sealing of hole：The alloy matrix aluminum of step (4) processing is impregnated 20 minutes in 90 DEG C of pore-sealing liquid, taking-up drains
Surface moisture, it is 3 hours dry at 85 DEG C, obtain anticorrosion aluminium ally section.
The electrolyte is prepared by following methods, and described part is parts by weight：By 15 parts of sulfuric acid, 3 parts of organic acid, more
0.2 part of first alcohol is added in 100 parts of water, is stirred 8 minutes with 200 revs/min, is added 0.1 part of boron nitride, is stirred with 200 revs/min
25 minutes, obtain electrolyte.
The pore-sealing liquid is prepared by following methods, and described part is parts by weight：By 100 parts of 1.5 parts of cerous nitrate and water
Mixing is stirred 15 minutes with 200 revs/min, obtains pore-sealing liquid.
The organic acid is the mixture of modified salicylic acid and gallic acid, the matter of the modified salicylic acid and gallic acid
Amount is than being 1：4.
The polyalcohol is pentaerythrite.
The modified salicylic acid is prepared by following methods, and described part is parts by weight：
(1) 2 parts of chitosan oligosaccharides and 100 parts of water are mixed, obtains chitosan oligosaccharide aqueous solution, the hydroxide for being 10% with mass fraction
The pH value that sodium water solution adjusts chitosan oligosaccharide aqueous solution is 8.0, adds 1.5 parts of salicylic acids, at 65 DEG C with 200 revs/min of stirrings 100
Minute, obtain reaction product；
(2) reaction product in vacuum degree is 0.1MPa by 100 revs/min of setting Rotary Evaporators rotating speed, and temperature is 65 DEG C of rotations
Turn to be evaporated to no moisture, obtains solid；
(3) by solid and ethyl alcohol in mass ratio 1：90 mixing are stirred 15 minutes at 20 DEG C with 200 revs/min, then with 4000
Rev/min centrifugation 10 minutes, what is obtained is deposited in 65 DEG C of dryings to constant weight, obtains modified salicylic acid.
Obtain the microhardness 601Hv of anticorrosion aluminium ally section, mass loss rate 3.46%, impedance value 2.41 × 106
Ω/cm2。
Test case 1
Aluminium alloy (trade mark 7150,50mm × 50mm × 1mm) is then placed in through conventional electrochemical deoiling, cleaning, neutralization
Hard anodizing in electrolyte obtains film layer after cleaning closing again.The technological parameter of wherein hard anodizing is：Temperature 2
DEG C, anodic current density 1A/dm2, time 50min, cathode material stereotype obtains anticorrosion aluminium.The electrolyte difference
For the electrolyte being prepared in Examples 1 to 6 and comparative example 1.
Obtained anticorrosion aluminium is carried out to salt spray test respectively to carry out by GB/T10125-1997 standards.Salt spray test
Test temperature in case is 36 DEG C, and corrosive medium used is the 5wt%NaCl solution of pH=7, sample testing face and vertical direction
Angle is 20 °.To other each surface adhesive tape seal protections of the sample in addition to test surfaces.Test result is shown in Table 2.
Table 2：Electrolyte handles the anticorrosion effect table after aluminium alloy 7150
| Embodiment | Fading occurs in specimen surface, time of pitting |
| Embodiment 1 | 551h |
| Embodiment 2 | 566h |
| Embodiment 3 | 584h |
| Embodiment 4 | 632h |
| Embodiment 5 | 654h |
| Embodiment 6 | 750h |
| Comparative example 1 | 605h |
Test case 2
The microhardness of the obtained anticorrosion aluminium ally section of embodiment 1-4 and comparative example 1 is tested, it is specific to test
It the results are shown in Table 3.
Table 3：Anticorrosion aluminium ally section micro-hardness testing result table
| Microhardness, Hv | |
| Embodiment 1 | 395 |
| Embodiment 2 | 459 |
| Embodiment 3 | 467 |
| Embodiment 4 | 528 |
| Comparative example 1 | 482 |
Test case 3
The wearability of the obtained anticorrosion aluminium ally section of embodiment 1-4 and comparative example 1 is tested, specific test knot
Fruit is shown in Table 4.
Table 4：Anticorrosion aluminium ally section wearability test result table
| Mass loss rate, % | |
| Embodiment 1 | 5.24 |
| Embodiment 2 | 4.67 |
| Embodiment 3 | 4.55 |
| Embodiment 4 | 4.03 |
| Comparative example 1 | 4.21 |
Test case 4
The corrosion resistance of the obtained anticorrosion aluminium ally section of embodiment 1-4 and comparative example 1 is tested, it is specific to test
It the results are shown in Table 5.
Table 5：Anticorrosion aluminium ally section corrosion resistance test result table
| Impedance value, Ω/cm2 | |
| Embodiment 1 | 9.24×105 |
| Embodiment 2 | 1.06×106 |
| Embodiment 3 | 1.18×106 |
| Embodiment 4 | 1.87×106 |
| Comparative example 1 | 1.62×106 |
Inorganic particle silicon nitride is added in embodiment 2 in the electrolytic solution, is remarkably improved the performance of oxidation film.
Different polyalcohols is respectively adopted in embodiment 2-4 electrolyte, finds the oxygen that embodiment 4 is obtained using pentaerythrite
Change the better performances of film.This is because polyalcohol can reduce solution rate of the electrolyte to film, while improving the temperature of permission
Range, and the speed of growth of film can be accelerated, increase the consistency and thickness of film, shadow of the different polyalcohols to anodic oxidation
It rings different.Embodiment 4 is using modified salicylic acid, and the performance of obtained oxidation film is better than comparative example 1, it may be possible to modified water
Poplar acid molecular structures are changed, and the organo-functional group being grafted on molecule is more advantageous to the performance for promoting oxidation film.
It is noted that the present invention is not limited to the above embodiment, any person skilled in the art is based on this hair
Bright technical solution both falls within the protection model of the present invention to any simple modification, equivalent change and modification made by above-described embodiment
In enclosing.
Claims (8)
1. a kind of Hard Anodic Oxidation of Aluminum Alloy electrolyte, which is characterized in that including following component：10~20 parts sulfuric acids, 2
~5 parts by weight organic acids, 0.1~0.3 weight polyol, 90~110 parts by weight water.
2. a kind of Hard Anodic Oxidation of Aluminum Alloy electrolyte, which is characterized in that be grouped as by following group：10~20 parts by weight sulphur
Acid, 2~5 parts by weight organic acids, 0.1~0.3 weight polyol, 0.05~0.5 parts by weight boron nitride, 90~110 parts by weight
Water.
3. Hard Anodic Oxidation of Aluminum Alloy electrolyte as claimed in claim 1 or 2, which is characterized in that the polyalcohol is third
One kind in triol, isopropanol, pentaerythrite.
4. Hard Anodic Oxidation of Aluminum Alloy electrolyte as claimed in claim 3, which is characterized in that the polyalcohol is Ji Wusi
Alcohol.
5. Hard Anodic Oxidation of Aluminum Alloy electrolyte as claimed in claim 1 or 2, which is characterized in that the organic acid is to change
Property salicylic acid and/or gallic acid.
6. Hard Anodic Oxidation of Aluminum Alloy electrolyte as claimed in claim 5, which is characterized in that the modified salicylic acid is under
The method of stating is prepared, and described part is parts by weight：
(1) 1-3 parts of chitosan oligosaccharides and 80-120 parts of water are mixed, obtains chitosan oligosaccharide aqueous solution, the hydrogen-oxygen for being 10% with mass fraction
It is 7.5-8.5 to change sodium water solution to adjust the pH value of chitosan oligosaccharide aqueous solution, 1-2 parts of salicylic acids is added, at 60-70 DEG C with 100-
300 revs/min are stirred 80-120 minutes, and reaction product is obtained；
(2) reaction product in vacuum degree is 0.05-0.2MPa, temperature 60-70 by 100 revs/min of setting Rotary Evaporators rotating speed
DEG C rotary evaporation obtains solid to no moisture；
(3) by solid and ethyl alcohol in mass ratio 1：(80-100) is mixed, at 15-25 DEG C with 100-300 revs/min of 10-20 points of stirring
Clock, then centrifuged 8-12 minutes with 3000-5000 revs/min, what is obtained is deposited in 60-70 DEG C of drying to constant weight, obtains modified bigcatkin willow
Acid.
7. such as the preparation method of claim 2~6 any one of them Hard Anodic Oxidation of Aluminum Alloy electrolyte, feature exists
In：10~20 parts by weight of sulfuric acid, 2~5 parts by weight of organic acid, 0.1~0.3 parts by weight of polyalcohol are added to 90~110 weight
In part water, stirred 5~10 minutes with 100~300 revs/min, add 0.05~0.5 parts by weight of boron nitride, with 100~300 turns/
Divide stirring 20~30 minutes, obtains electrolyte.
8. such as claim 1~6 any one of them Hard Anodic Oxidation of Aluminum Alloy electrolyte answering in anticorrosion aluminium
With.
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| CN110438543A (en) * | 2019-06-28 | 2019-11-12 | 绍兴市上虞和盛纺器有限公司 | A kind of textile-bobbin aluminium anodes hardening oxidation surface treatment method and product |
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| CN114672684A (en) * | 2022-03-31 | 2022-06-28 | 江苏恒鑫正宏科技有限公司 | High-strength aluminum alloy section for brake chamber and processing technology thereof |
| CN114672684B (en) * | 2022-03-31 | 2022-09-13 | 江苏恒鑫正宏科技有限公司 | High-strength aluminum alloy section for brake chamber and processing technology thereof |
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