CN107268060A - Hole sealing equipment and method for sealing hole of anodic oxide film by using vacuum and jet steam - Google Patents
Hole sealing equipment and method for sealing hole of anodic oxide film by using vacuum and jet steam Download PDFInfo
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- CN107268060A CN107268060A CN201610298337.4A CN201610298337A CN107268060A CN 107268060 A CN107268060 A CN 107268060A CN 201610298337 A CN201610298337 A CN 201610298337A CN 107268060 A CN107268060 A CN 107268060A
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- 238000007789 sealing Methods 0.000 title claims abstract description 181
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000010407 anodic oxide Substances 0.000 title abstract 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 44
- 238000012545 processing Methods 0.000 claims description 41
- 239000011148 porous material Substances 0.000 claims description 38
- 238000002347 injection Methods 0.000 claims description 37
- 239000007924 injection Substances 0.000 claims description 37
- 229910052782 aluminium Inorganic materials 0.000 claims description 34
- 239000004411 aluminium Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003125 aqueous solvent Substances 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 239000004809 Teflon Substances 0.000 claims description 4
- 229920006362 Teflon® Polymers 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 229910003460 diamond Inorganic materials 0.000 claims description 4
- 239000010432 diamond Substances 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- 230000002209 hydrophobic effect Effects 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 230000007704 transition Effects 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 239000002071 nanotube Substances 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 6
- 238000004381 surface treatment Methods 0.000 abstract description 6
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 238000001771 vacuum deposition Methods 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 12
- 238000010586 diagram Methods 0.000 description 12
- 239000003792 electrolyte Substances 0.000 description 12
- 230000004888 barrier function Effects 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 9
- 238000005260 corrosion Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000006703 hydration reaction Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 150000004682 monohydrates Chemical class 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 230000036571 hydration Effects 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 235000006408 oxalic acid Nutrition 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 229910001680 bayerite Inorganic materials 0.000 description 3
- 229910001593 boehmite Inorganic materials 0.000 description 3
- 210000003850 cellular structure Anatomy 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 210000000981 epithelium Anatomy 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- -1 oxonium ion Chemical class 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- PLXMOAALOJOTIY-FPTXNFDTSA-N Aesculin Natural products OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](O)[C@H]1Oc2cc3C=CC(=O)Oc3cc2O PLXMOAALOJOTIY-FPTXNFDTSA-N 0.000 description 1
- 229910018626 Al(OH) Inorganic materials 0.000 description 1
- 229910002706 AlOOH Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000007743 anodising Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005370 electroosmosis Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 229910001679 gibbsite Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 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
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
- C25D11/246—Chemical after-treatment for sealing layers
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Pistons, Piston Rings, And Cylinders (AREA)
Abstract
The invention provides a hole sealing device and a method for sealing an anodic oxide film by using vacuum and jet steam, which comprises the following steps: firstly, residual moisture and gas in the nano tube of the anodic oxide film are pumped out by using a vacuum pump, and then the hole sealing agent is sprayed into the nano tube of the anodic oxide film placed in the hole sealing cavity by using a jet steam engine, so that the anodic oxide film achieves the hole sealing effect. The hole sealing equipment and the hole sealing method can ensure that the anodic oxide film obtains extremely high hole sealing effect. The hole sealing equipment and the hole sealing method are suitable for surface treatment of the semiconductor equipment assembly, so that the service life of the semiconductor equipment assembly in a plasma environment is prolonged, and the cost of vacuum coating is reduced.
Description
Technical field
It is used for the present invention relates to a kind of by the plugging equipment and method of anode oxide film sealing of hole, more particularly to a kind of utilization
Vacuum and plugging equipment and method of the injection steam to anode oxide film sealing of hole so that anode oxide film obtains high sealing of hole effect
Really.Anode oxide film can obtain more preferably anti-dry-and wet-type corrosivity after the sealing pores of the present invention.Vacuum evaporation is green energy production
An important ring of industry (such as light-emittingdiode, solar cell, super capacitor) manufacturing process, plugging equipment of the invention and
Method be applied to semiconductor plasma apparatus assembly is surface-treated, and then increase plasma apparatus component wait from
Service life in daughter environment, and then reduce the cost of vacuum coating.
Background technology
In recent years, it is in the ascendant in the development of field of surface treatment, and successful exploitation and application due to surface treatment
Really the quality of the life of people is improved, infinite commercial opportunities have also been started.Precision surface processing is just widely being applied to each at present
Plant in product, for example：Optical articles, electronic product, Communication Equipment and notebook personal computer, thus for surface at
Reason requires that quality is more and more harsh.For example, for vacuum plasma cavity, anodized surface processing is especially weighed
Will.In electrochemical reaction field, anode processing has been a kind of ripe conventional industries, its anti-corruption in main application such as surface
The surfaction application such as erosion, application, decoration, electric insulation, electroplating surface, wearability.
Anodised aluminium must review to earliest it is that Setoh in 1932 and the people of Miyata two propose it is assumed that they think by
In there is a barrier layer (Barrier layer) generation, thus allow that the water in epithelium pore discharges by electrode effect it is nascent
State oxygen (Nascent oxygen) passes through, and is thereby constantly combined with aluminium and generate new barrier layer.In addition, the life of pore
Into the corrosion of mainly anions, cause oxygen penetrate into pore in so that metal material because barrier layer protection and
Avoid contacting with solution.
Advanced a theory in succession in S.Wernick in 1934, he thinks a kind of colloid with negative electrical charge, after hydrolysis, in
Anode generation aluminium hydroxide (Aluminum hydroxide).This colloid can be spread on the metal surface as sponge net,
When direct current by when, electrolyte (anion) is repelled in outer due to electroosmosis (Caraphoresis)；If alternating current
If, alternatively adsorbed with change in polarity (positive or negative) and drive away electrolyte.S.Wernick is also proposed on electrolysis
Time, increasing thickness over time had a maximum for the influence of coating growth and size.When electric current leads to intermittently
Out-of-date, thickness is thinning with time increase, and particularly when using sulfuric acid as electrolyte, this phenomenon becomes apparent.1936
Year, Rummel proposed his conception, it is believed that barrier layer can allow electric current to pass through by the generation of pore, just have in the bottom of pore
A new barrier layer starts growth, so repeated growth always, until too deep pore causes existing undertension to maintain
Epithelium continued growth.
Baumann in 1936 proposes to assume there is a gas-bearing formation film on the active layer (Active layer) of pore bottom
The presence of (Vapor film)；The release of heat is still due to electric current and the relation chemically reacted at gas-electrolyte interface
It is upper to spread, because he assumes that oxonium ion is generated on an interface herein, as long as there have enough voltage to force oxygen to enter aluminium to be brilliant
Lattice, the reaction of formation of oxide scale film just occurs, and discharges a heat；Too high heat release, makes anion cannot be introduced into pore,
Electric current is transmitted by oxonium ion, when being combined electric discharge (Discharge) with aluminium, causes oxide-film to dissolve, and causes pore size
Widen.
In recent years due to the development of nanometer technology so that technically more can completely is controlled anode oxide film tracheid or received
Caliber, pipe range and the pipe density of nanotube structures.There is provided the manufacture of with low cost and quick volume production for easy anode treatment technology
Method, can be applied to the big production development of per surface area, such as DSSC, thermally conductive sheet and heat shield
The exploitation of element.Anode treatment technology, with the demand of industrial products, the anti-corruption on heavy industry works surface is directed to from early stage
The demand of the surfactions such as erosion, abrasion resisting, impact resistance and high temperature resistant, in recent years more applied in the vacuum cavity of evaporated device
The plated film absorbed layer in portion, or the barrier layer in integrated circuit, with most popular radiating material at present, heat-insulated material, green building materials, with too
The industry developments such as positive energy battery, have the anode treatment technology of automated production characteristic, certainly will be by one of process as each industry.
The application of anode processing industrially is wherein most ripe with the operating technology of aluminium, magnesium, titanium.When aluminium is placed in specific electricity
Solve in liquid and the appropriate anode processing parameter of control, the oxide-film formed has well-regulated born of the same parents' shape (cell) or nanotube knot
Structure.The interface of nanotube ends and aluminium then forms hemispheric barrier layer, and the composition of wherein nanotube and barrier layer is three
Al 2 O (Al2O3).Aluminium is main by reacting 2Al in anode processing+3+3H2O→Al2O3+6H+Form, therefore, pH need to be controlled
Value is less than under conditions of less than 4, i.e. acid solution, and applied voltage need to be higher than more than -1.8V (SHE), H in formula+H will be passed through++H+→H2, and hydrogen is generated, this hydrogen is by Al2O3Inside effusion, in turn results in porous aluminum oxide and is formed, therefore, controls hydrogen
The speed of gas effusion, then can control the hole being formed inside aluminum oxide, the anodic alumina films as pore homogeneity made.
Aluminium is when anode is handled in Surface Creation alundum (Al2O3) (Al2O3) oxide layer, the initial stage of the oxide layer growth is with hex hole
Hole is grown up toward top, increases over time the arrangement of the hexagon hole neighboring atom gradually into irregularity (disorder)
Arrangement, so hole gradually switchs to circular opening, the change in aperture in addition can be represented by C=mV, wherein C：Pore size
(nm)、V：Anode processing voltage (V), m：Constant (2~2.5).
Due to the cellular structure of anode oxide film, its subsequently need to again through sealing pores step, using when except with U.S.
The outward appearance with polychrome coloured silkization is seen, while can more increase engineering properties such as hardness, abrasion performance etc. of anode film, and it is thin to lift anode
Corrosion in chemical stability of the film in harsh environment, such as anti-wet solution and the plasma attack in anti-dry type environment
Deng.
The problem of in order to solve for surface treatment quality rigors, the present invention proposes that one kind is steamed using vacuum with injection
Vapour can make anode oxide film obtain high sealing of hole effect, and then lifted the plugging equipment and method of anode oxide film sealing of hole
Anode handles service life of the workpiece in dry-and wet-type environment.
The content of the invention
It is an object of the invention to provide a kind of utilization vacuum and plugging equipment of the injection steam to anode oxide film sealing of hole
With method, the engineering properties and chemically stable of anode oxide film are lifted by plugging equipment provided by the present invention and method
Property.Lid is pipe cell structure because of aluminium anode oxide film, in order to improve the quality and dye firm coloration, ion or colorant of aluminium workpiece surface
The fine pore of anode oxide film must be closed after coloring, the homogeneous non-porous that surface becomes after Seal treatment is formed
Fine and close oxide-film, the anode oxide film after closing no longer has adsorptivity, absorption harmful substance can be avoided and it is contaminated or
Early stage corrodes, so as to improve the performance such as anti-pollution, against corrosion of anode oxide film.Method for sealing after conventional coloring has hydration
Sealing of hole, inorganic salt solution sealing of hole, transparent organic coating sealing of hole.
Hot hole sealing technology is that in the pure water close to boiling point, by the hydration reaction of aluminum oxide, amorphous alumina is turned
Chemical conversion is referred to as the hydrated alumina of vigorous nurse body (bohmite), i.e. Al2O3·H2O(AlOOH).Due to aqua oxidation aluminum ratio Yuanyang pole
The molecular volume of oxide-film is big, and volumetric expansion causes the micropore filling of anode oxide film to close, the resistance tocrocking of anode oxide film
With corrosion resistance with raising, while impedance increase, the dielectric constant of anode oxide film also with change it is big.Anodizing of aluminium film
There is the reaction of two kinds of forms in water：One of them is compared with low temperature (less than 40 DEG C), pH<In 4 water, three water are combined into water
Close aluminum oxide (Bayerite (Al (OH)3)), its reaction equation is Al+3H2O→Al(OH)3+1.5H2, this reaction is in applied voltage
Higher anode mold growth rate can be obtained under (stream), be called anode processing.Another is at higher temperatures (more than 80 DEG C)
In neutral water, aluminum oxide synthesizes monohydrate alumina (Boehmite AlO (OH)) with aquation, and its reaction equation is Al2O3+H2O→
2AlO (OH) is here it is the usual course of reaction of signified hydration sealing of hole, due to the molecular weight (60g/mole) of monohydrate alumina
Than hibbsite molecular weight (78g/mole) it is small, therefore by hydration sealing pores after aluminium anodes membrane volume can be swollen
Swollen ((78-60)/78=23%) (2Al (OH)3+3H2O→2AlO (OH)+3H2), and plug the anodic oxidation of tracheid shape
The hole of film.
The present invention illustrates following characteristics point simultaneously：
(1) high-pressure water vapor has higher temperature and pressure compared to normal pressure water vapour, can make hydrone be easier into
Enter and sealing of hole is carried out in anode oxide film.
(2) anode oxide film soaks sealing of hole in the hot water, anode oxide film top layer is produced loose laminated structure.
(3) anode oxide film is placed in sealing of hole in steam, and anode oxide film surface can be made to keep clean structure.
(4) aluminium anode oxide film can be produced after aluminium is handled through anode, its reaction equation is:Al+3H2O→Al(OH) 3+1.5H2
(5) aluminium anode oxide film is after high-temperature-hot-water sealing of hole, and the composition of anode oxide film can be by hibbsite
(Bayerite, (Al (OH)3)) it is converted into monohydrate alumina (Boehmite, AlO (OH)).
(6) compared to Al (OH)3, AlO (OH) has preferred corrosion resistance and abrasion performance.
(7) sealing of hole reaction equation:Hibbsite → monohydrate alumina
2Al(OH)3+3H2O→2AlO(OH)+3H2
(8) molecular weight (78g/mole) of the molecular weight (60g/mole) of monohydrate alumina, hibbsite.By
The volume of aluminium anode oxide film after hydration sealing pores can expand ((78-60)/78=23%).
Some additives such as natrium carbonicum calcinatum, ammonia, triethanolamine etc. are added in high-temperature water, sealing of hole effect can be strengthened, carried
The corrosion stability of high film layer.Be hydrated sealing of hole another method be steam sealing of hole, the oxide-film corrosion stability, wearability handled by it with
Steam pressure is relevant with the sealing of hole time.It is general to be reduced with pressure rise, time lengthening, corrosion stability raising, wearability.
For up to above-mentioned purpose, the present invention provides a kind of utilization vacuum and the plugging equipment of injection steam, the plugging equipment
Comprising：One sealing of hole cavity, workpiece is handled for housing an anode with anode oxide film；One heating furnace, for by the envelope
Vestibule body maintains a specified temp；One vavuum pump, is connected with the sealing of hole cavity, for the sealing of hole inside cavity to be evacuated to
Negative pressure state；And one injection steam engine, be connected with the sealing of hole cavity, for a hole sealing agent to be injected into the sealing of hole chamber
In vivo, barotropic state will be switched to by the negative pressure state in the sealing of hole cavity, wherein the hole sealing agent fills up the anode
Handle the hole of the anode oxide film of workpiece.
In one of present invention preferred embodiment, the anode oxide film includes：By the way that aluminum or aluminum alloy is carried out into anode
The anode oxide film produced by processing, the processing of hard anode or the processing of differential of the arc anode.
In one of present invention preferred embodiment, the sealing of hole cavity inner temperature is maintained 80 DEG C extremely by the heating furnace
Between 150 DEG C.
In one of present invention preferred embodiment, the sealing of hole inside cavity is evacuated to below 0.01torr by the vavuum pump
The negative pressure state.
In one of present invention preferred embodiment, it is described injection steam engine by the sealing of hole cavity by the negative pressure state
Switch to more than the 1.1atm barotropic state.
In one of present invention preferred embodiment, the injection steam engine sprays the hole sealing agent of liquid state or gaseous state shape
Inject in the sealing of hole cavity, the anode oxide film for handling the anode workpiece carries out sealing pores.
In one of present invention preferred embodiment, the hole sealing agent comprising water, water vapour, the aqueous solvent containing ion, contain
There are the aqueous solvent of molecule or the solvent containing suspension.
In one of present invention preferred embodiment, the ion includes the ion with transition elements.
In one of present invention preferred embodiment, the molecule is included with hydrophobic alkyl molecule or with hydrophily
Polyhydroxylated molecule.
In one of present invention preferred embodiment, the suspension includes Teflon, alumina powder, titanium dioxide powder
End, ceramic pond powder, metal dust, polymeric powder or diamond powder
The present invention also provides a kind of method for sealing, comprising：The anode processing workpiece for having anode oxide film by one is positioned over
In one sealing of hole cavity；The sealing of hole cavity is set to maintain a specified temp using a heating furnace；Using a vavuum pump by the envelope
Hole inside cavity is evacuated to a negative pressure state；Close one first air pressure valve being located between the vavuum pump and the sealing of hole cavity
Door；Open and be located at one second air pressure valve between an injection steam engine and the sealing of hole cavity to connect the injection steam engine
With the sealing of hole cavity；And hole sealing agent is entered in the sealing of hole cavity using the injection steam engine, by the sealing of hole
The barotropic state is switched to by the negative pressure state in cavity, and the anode oxide film for handling workpiece to the anode enters
Row sealing pores.
Brief description of the drawings
The schematic diagram of the plugging equipment of Fig. 1 display present invention；
The flow chart of the method for sealing of Fig. 2 display present invention；
Fig. 3 A display surfaces are formed with the schematic diagram of the aluminum component of anode oxide film；
Fig. 3 B show the diagrammatic cross-section along A-A ' transversals in Fig. 3 A；
Fig. 4 A and Fig. 4 B show the schematic diagram of three-axis force balance respectively；
It is corresponding that Fig. 5 A and Fig. 5 B show that the pipe thickness of anode oxide film and pipe inner volume or pipe internal surface are accumulated respectively
Figure；
Fig. 6 A show that anode oxide film carries out the structural representation before sealing pores；
Fig. 6 B show that anode oxide film carries out the structural representation after sealing pores；
Fig. 7 A and Fig. 7 B show that the aluminium flake of the first preferred embodiment of the present invention carries out anode table by oxalic acid solution respectively
Face before processing and the micro-structural schematic diagram after processing；
Fig. 8 A and Fig. 8 B show that aluminium flake carries out anode surface by sulfuric acid solution in second preferred embodiment of the invention respectively
Before processing and the micro-structural schematic diagram after processing.
Embodiment
Hereinafter, hereby describing a kind of of correlation of the invention in detail using accompanying drawing utilizes vacuum with injection steam to anodic oxidation
The plugging equipment of film sealing of hole and each embodiment of method.In addition, in the description of the drawings, same key element or with same function
Key element uses same symbol, and the repetitive description thereof will be omitted.
Sealing of hole quality of the invention in order to lift anode oxide film, it is proposed that one kind is using vacuum with injection steam to anode
The plugging equipment and method of oxide-film sealing of hole, such a plugging equipment and method are big etc. with production simplicity and area change
Characteristic, it is adaptable in industrial production.Fig. 1 is refer to, it shows the schematic diagram of the plugging equipment 1000 of the present invention.The sealing of hole is set
Standby 1000 include sealing of hole cavity 1002, vacuum pressure mouthful 1003, malleation air pressure mouthful 1004, vacuum connection tube 1005, the first air pressure
Valve 1006, vavuum pump 1007, malleation connecting tube 1008, the second air pressure valve 1009, injection steam engine 1010 and heating furnace
1011.The sealing of hole cavity 1002 can bear malleation and/or negative pressure, for anode processing workpiece 1001 to be housed in the inner,
So that the anode oxide film of workpiece 1001 is handled the anode carry out vacuum and the sealing pores of injection steam.In sealing pores
Before, anode processing workpiece 1001 surface is formed with one layer of anode oxide film, and the anode oxide film has non-sealing of hole
Or the pipe cell structure of local sealing of hole, its chemical composition is generally hibbsite (Bayerite (Al (OH)3)).It is described true
Air presses mouth 1003 to be formed with the malleation air pressure mouthful 1004 on the surface of the sealing of hole cavity 1002.The vacuum connection tube
1005 are used to be connected between vacuum pressure mouthful 1003 and the vavuum pump 1007 so that the sealing of hole cavity 1002 and vavuum pump
1007 connections.First air pressure valve 1006 is arranged in the vacuum connection tube 1005, by controlling first air pressure
Valve 1006 is turned on and off, and then controls the connection between the sealing of hole cavity 1002 and vavuum pump 1007.In order to remove
Gas in the nanotube of the anode oxide film of the anode processing workpiece 1001, makes hole sealing agent be easier to enter in nanotube,
When the anode processing workpiece 1001 be placed in the sealing of hole cavity 1002 when, can be by described 1007 pairs of anodes of vavuum pump at
Science and engineering part 1001 carries out vacuum suction.The malleation connecting tube 1008 be used for be connected to it is described injection steam engine 1010 with it is described just
Calm the anger between mouth 1004 so that the sealing of hole cavity 1002 is connected with the injection steam engine 1010.Second air pressure valve
Door 1009 is arranged in the malleation connecting tube 1008, by controlling being turned on and off for second air pressure valve 1009, is entered
And control the connection between the sealing of hole cavity 1002 and the injection steam engine 1010.Will using the injection steam engine 1010
Hole sealing agent injects in the sealing of hole cavity 1002 at high speed, hole sealing agent is rapidly introduced into the sun that the anode handles workpiece 1001
The purpose of sealing of hole is reached in the nanotube of pole oxide-film.The heating furnace 1011 is centered around the outside of the sealing of hole cavity 1002,
For making the temperature in the sealing of hole cavity 1002 maintain the state of long-time constant temperature.
Fig. 2 is refer to, it shows the flow chart of the method for sealing of the present invention.The method for sealing of the present invention is by such as Fig. 1
Shown plugging equipment 1000 carries out sealing pores with injection steam using vacuum to anode oxide film, and its specific steps is included：
First, step S10 is carried out：Anode processing workpiece 1001 is positioned in the sealing of hole cavity 1002.Then, step is carried out
S20：The sealing of hole cavity 1002 is set to maintain the specified temp using the heating furnace 1011.Then, step S30 is carried out：
The negative pressure state will be evacuated to using the vavuum pump 1007 inside the sealing of hole cavity 1002.Then, step S40 is carried out：Close
Close positioned at first air pressure valve 1006 between the vavuum pump 1007 and the sealing of hole cavity 1002.Then, walked
Rapid S50：Open second air pressure valve 1009 being located between the injection steam engine 1010 and the sealing of hole cavity 1002.
Finally, step S60 is carried out：The hole sealing agent is set to enter in the sealing of hole cavity 1002 using the injection steam engine 1010, with
The barotropic state will be switched to by the negative pressure state in the sealing of hole cavity 1002, and workpiece 1001 is handled to the anode
The anode oxide film carry out sealing pores.This sealing pores step can be directed to by the way that aluminum or aluminum alloy is carried out at anode
What the anode oxide film produced by reason, the processing of hard anode or the processing of differential of the arc anode was carried out.During sealing of hole, by described
Heating furnace 1011 maintains the temperature in the sealing of hole cavity 1002 between 80 DEG C to 150 DEG C, passes through the vavuum pump 1007
Below 0.01torr negative pressure state will be evacuated to inside the sealing of hole cavity 1002, and will by the injection steam engine 1010
Switch to more than 1.1atm barotropic state in the sealing of hole cavity 1002 by negative pressure state.The species of the hole sealing agent of the present invention
The hole sealing agent of liquid state or gaseous state shape can be included, for example, water, water vapour, containing ion aqueous solvent (such as transition elements from
Son), aqueous solvent containing molecule (as having hydrophobic alkyl molecule, with hydrophilic polyhydroxylated molecule), contain suspension
Solvent (such as Teflon, alumina powder, titania powder, ceramic pond powder, metal dust, polymeric powder or diamond
Powder).
Fig. 3 A and Fig. 3 B are refer to, wherein Fig. 3 A display surfaces are formed with the schematic diagram of the aluminum component of anode oxide film, and
Fig. 3 B show the diagrammatic cross-section along A-A ' transversals in Fig. 3 A.As shown in Figure 3A, when aluminum component 3001 is positioned over into specific electrolysis
In liquid and the appropriate anode processing parameter of control, can be formed on the surface of the aluminum component 3001 the well-regulated born of the same parents' shape (cell) of tool or
The anode oxide film 3003 (i.e. aluminum oxide) of nano tube structure, and end and the aluminium of the nanotube of the anode oxide film 3003
Interface between 3001 can form hemispheric barrier layer 3002, wherein the nanotube of the anode oxide film 3003 and the resistance
The composition of barrier layer 3002 is hibbsite.The diameter of nanotube, pipe density, pipe thickness, with pipe range then according to anode at
Depending on reason parameter.As shown in Figure 3 B, each nanotube of the anode oxide film 3003 is the hollow structure that a upper and lower side is connected,
The size of its pore radius is R and the pipe thickness of nanotube is W.Using the pore radius R of nanotube size, pipe thickness W with
Pipe density can calculate the surface area and bulking value of the nanotube on unit sample.The theoretical value of pipe density can utilize following methods
Obtain：When the bore dia of nanotube is (a) 15nm, (b) 60nm, with (c) 500nm, its pipe density is respectively 2.6 × 1011,
1.5×1010, with 1.5 × 108pore/cm2.The bore dia of multiple anodic alumina films and pipe density value in accordance with the above, can
Area is calculated for 1cm2Volume and surface area values of the anodic alumina films of sample surfaces under different length.Volume and surface
Long-pending calculation formula is respectively π R2× D × ρ and 2 π R × D × ρ, wherein R, D, ρ be respectively the pore radius of nanotube, thickness, with
Pipe density.
In theory, the anode oxide film formed on the aluminum component of high-purity is particularly susceptible the tracheid shape to form hexangle type, its
As shown in Figure 4 A and 4 B shown in FIG., Fig. 4 A and Fig. 4 B show the schematic diagram of three-axis force balance to formation basic theory respectively.Due to anode oxide film
Hydrogen effusion can cause anode oxide film formation hexangle type tracheid structure with the dynamic balance phenomenon that film is pushed mutually during growth.Such as
Shown in Fig. 4 A and Fig. 4 B, work as γAB=γAC=γBCWhen, γACWith γBCBetween angle be represented by(Fig. 4 A, according to the law of sinesSuch as Fig. 4 B institutes
Show, when each angle is 120 °, 120 ° of angles are further considered as to the angle of tube wall, then the tube wall of three 120 ° of angles can be combined
Into the tracheid of a hexagonal structure.
Fig. 5 A and Fig. 5 B are refer to, it shows the pipe thickness and pipe inner volume or pipe internal surface of anode oxide film respectively
Numerical value in long-pending corresponding diagram, wherein Fig. 5 A and Fig. 5 B is based on 1cm2Calculated value on area.In fig. 5a, it is shown that anode
The pipe inner volume of pellumina (Anodic Aluminum Oxide, AAO) and bore dia ψ corresponding diagram, work as anodic alumina films
Pipe thickness be 100 μm when, bore dia ψ is 15nm, 60nm, pipe inner volume corresponding with 500nm difference is
0.0046cm3、0.0048cm3、0.0069cm3.Because born of the same parents' shape tube wall occupies the pipe inner volume of part, therefore when bore dia ψ is
When 15nm, 60nm and 500nm, the pipe thickness of anodic alumina films requires more than 1cm and (for example reaches 2.18cm, 2.09cm respectively
With, 1.46cm), born of the same parents' shape pipe inner volume can just reach 1cm3.Relative to the reduction of unit volume inner anode pellumina volume, anode
The pipe internal surface product of pellumina then significantly increases.As shown in Figure 5 B, when pipe thickness is 100 μm, bore dia ψ is
15nm, 60nm, the pipe internal surface product respectively 1225.2cm with 500nm anodic alumina films2、3204.4cm2And
549.7cm2.In addition, when pipe thickness is 1cm, bore dia ψ is 15nm, 60nm, the pipe with 500nm anodic alumina films
Internal surface area is respectively 1,225,220cm2、320,442cm2With 54,997cm2, i.e., relative to 1cm3(pipe internal surface is accumulated
6cm2) fine and close bulk, bore dia ψ is 15nm, 60nm, the 1cm with 500nm3Anodic alumina films, its pipe internal surface integration
204,203,53,407 and 9,166 times are not added.
Fig. 6 A and Fig. 6 B are refer to, wherein Fig. 6 A show that anode oxide film carries out the structural representation before sealing pores,
And Fig. 6 B show that anode oxide film carries out the structural representation after sealing pores.As shown in Figure 6A, the anode oxide film
There is the pipe cell structure of systematicness, the calculating that the anodic oxidation membrane tube inner volume is accumulated with pipe internal surface before sealing of hole is not carried out
Mode can be calculated according to foregoing formula.The anode oxide film of tracheid shape with hot water except with can carry out volumetric expansion
Outside sealing of hole characteristic, high surface area can be also provided with space so that the second phase chemical substance is filled so that the anode oxide film is obtained
Obtain diversified surfaction characteristic.As shown in Figure 6B, envelope of the anode oxide film of tracheid shape Jing Guo hot water volumetric expansion
Kong Hou, is presented sealing of hole shape, with fine and close anodic oxidation membrane property.
First embodiment：
In this preferred embodiment, it can react into aluminium flake after the aluminium flake of mechanical lapping is handled through anode again on surface
Porous alundum (Al2O3) film, and using applied voltage with electrolyte component come control hole density distribution and hole it is big
Small, the electrolyte of anode processing is main based on oxalic acid, is electrolyte, additional 40 volt DC using 3wt% oxalic acid aqueous solutions
Voltage, anodic treatment times 1 hour, electrolyte temperature are 25 DEG C, the reaction of metal aluminum flake surface can be made to produce porous three oxygen
Change two aluminium films.Fig. 7 A and Fig. 7 B are refer to, it shows that the aluminium flake of the first preferred embodiment of the present invention is molten by oxalic acid respectively
With the micro-structural schematic diagram after processing before liquid progress anod surface treatment.As shown in Figure 7 A, the non-sealing of hole of the anode oxide film of aluminium flake
Preceding presentation cellular structure.Then, using the plugging equipment 1000 of the invention shown in Fig. 1 for porous three oxidations
Two aluminium films carry out sealing pores.First, the anode processing test piece of non-sealing of hole is placed in the sealing of hole cavity, and makes the envelope
Vestibule body is kept between a specified temp, such as 80~150 DEG C, and the sealing of hole cavity is imposed into Negative pressure, and its vacuum is protected
Hold in below 0.1torr, and the sealing of hole cavity is continued more than 3 minutes under this vacuum and temperature conditionss, then by vacuum
Valve (that is, the first air pressure valve) is closed, and injection steam valve (that is, the second air pressure valve) will be opened by continuing, and make sealing of hole steam
(that is, hole sealing agent) enters in sealing of hole cavity carries out sealing pores to anode processing test piece, and the sealing of hole time is maintained at more than 5 minutes,
Anode oxide film after sealing pores can show the micro-structural of dense film, as shown in Figure 7 B, anode processing test piece
Anode oxide film is through short vacuum and the micro-structural that nano particle filling is presented after injection steam sealing of hole.
Second embodiment：
In this preferred embodiment, it can react into aluminium flake after the aluminium flake of mechanical lapping is handled through anode again on surface
Porous alundum (Al2O3) film, and using applied voltage with electrolyte component come control hole density distribution and hole it is big
Small, the electrolyte of anode processing is main based on sulfuric acid, is electrolyte, additional 35 volt DC using 3wt% aqueous sulfuric acids
Voltage, anodic treatment times 1 hour, electrolyte temperature are 25 DEG C, the reaction of metal aluminum flake surface can be made to produce porous three oxygen
Change two aluminium films.Please Fig. 8 A and Fig. 8 B, it shows that aluminium flake is carried out by sulfuric acid solution in second preferred embodiment of the invention respectively
With the micro-structural schematic diagram after processing before anod surface treatment.As shown in Figure 8 A, presented before the non-sealing of hole of the anode oxide film of aluminium flake
Cellular structure.Then, it is thin for porous alundum (Al2O3) using the plugging equipment 1000 of the invention shown in Fig. 1
Film carries out sealing pores.First, the anode processing test piece of non-sealing of hole is placed in sealing of hole cavity, and keeps the sealing of hole cavity
One specified temp, such as between 80~150 DEG C, impose Negative pressure, its vacuum is maintained at 0.1torr by the sealing of hole cavity
Hereinafter, and the sealing of hole cavity is continued more than 3 minutes under this vacuum and temperature conditionss, then vacuum valve is closed (i.e.,
First air pressure valve), continue unlatching injection steam valve (that is, the second air pressure valve), enters sealing of hole steam (that is, hole sealing agent)
Sealing pores are carried out to anode processing test piece in the sealing of hole cavity, the sealing of hole time is maintained at more than 1 hour, by sealing pores
Anode oxide film afterwards can show the micro-structural of shrinkage cavity.As shown in Figure 8 B, through long-time vacuum and sun after injection steam sealing of hole
The micro-structural of shrinkage cavity is presented in pole oxide-film.Anode oxide film before the bore dia average out to 50nm of anode oxide film, sealing of hole before sealing of hole
Bore dia average out to 34nm, its hole through contraction cavity ratio be 33%.
Claims (15)
1. a kind of utilization vacuum and the plugging equipment of injection steam, it is characterised in that the plugging equipment is included：
One sealing of hole cavity, workpiece is handled for housing an anode with anode oxide film；
One heating furnace, for the sealing of hole cavity to be maintained into a specified temp；
One vavuum pump, is connected with the sealing of hole cavity, for the sealing of hole inside cavity to be evacuated into negative pressure state；And
One injection steam engine, is connected with the sealing of hole cavity, for a hole sealing agent to be injected into the sealing of hole cavity, will
Barotropic state is switched to by the negative pressure state in the sealing of hole cavity, wherein the hole sealing agent fills up the anode processing workpiece
The hole of the anode oxide film.
2. plugging equipment as claimed in claim 1, it is characterised in that the anode oxide film includes：By the way that aluminium or aluminium are closed
Gold carries out the anode oxide film produced by anode processing, the processing of hard anode or the processing of differential of the arc anode.
3. plugging equipment as claimed in claim 1, it is characterised in that the heating furnace maintains the sealing of hole cavity inner temperature
Between 80 DEG C to 150 DEG C.
4. plugging equipment as claimed in claim 1, it is characterised in that the sealing of hole inside cavity is evacuated to by the vavuum pump
Below the 0.01torr negative pressure state.
5. plugging equipment as claimed in claim 1, it is characterised in that the injection steam engine by the sealing of hole cavity by institute
State the barotropic state that negative pressure state switchs to more than 1.1atm.
6. plugging equipment as claimed in claim 1, it is characterised in that the injection steam engine is by the institute of liquid state or gaseous state shape
State hole sealing agent to be injected into the sealing of hole cavity, the anode oxide film for handling the anode workpiece is carried out at sealing of hole
Reason.
7. plugging equipment as claimed in claim 1, it is characterised in that the hole sealing agent includes water, water vapour, contains ion
Aqueous solvent, the aqueous solvent containing molecule or the solvent containing suspension.
8. plugging equipment as claimed in claim 7, it is characterised in that the ion includes the ion with transition elements.
9. plugging equipment as claimed in claim 7, it is characterised in that the molecule include with hydrophobic alkyl molecule or
With hydrophilic polyhydroxylated molecule.
10. plugging equipment as claimed in claim 7, it is characterised in that the suspension comprising Teflon, alumina powder,
Titania powder, ceramic pond powder, metal dust, polymeric powder or diamond powder.
11. a kind of utilization vacuum and the method for sealing of injection steam, it is characterised in that the method for sealing is included：
The anode processing workpiece for having anode oxide film by one is positioned in a sealing of hole cavity；
The sealing of hole cavity is set to maintain a specified temp using a heating furnace；
The sealing of hole inside cavity is evacuated to a negative pressure state using a vavuum pump；
Close one first air pressure valve being located between the vavuum pump and the sealing of hole cavity；
Open and be located at one second air pressure valve between an injection steam engine and the sealing of hole cavity to connect the injection steam
Machine and the sealing of hole cavity；And
Using it is described injection steam engine make hole sealing agent enter the sealing of hole cavity in, by the sealing of hole cavity by the negative pressure
State switchs to the barotropic state, and handles the anode anode oxide film progress sealing pores of workpiece.
12. method for sealing as claimed in claim 11, it is characterised in that the anode oxide film includes：By by aluminium or aluminium
Alloy carries out the anode oxide film produced by anode processing, the processing of hard anode or the processing of differential of the arc anode.
13. method for sealing as claimed in claim 11, it is characterised in that the heating furnace ties up the sealing of hole cavity inner temperature
Hold between 80 DEG C to 150 DEG C；
The sealing of hole inside cavity is evacuated to below the 0.01torr negative pressure state by wherein described vavuum pump；And
Wherein described injection steam engine will be switched to more than the 1.1atm malleation by the negative pressure state in the sealing of hole cavity
State.
14. method for sealing as claimed in claim 11, it is characterised in that the injection steam engine is by liquid state or gaseous state shape
The hole sealing agent is injected into the sealing of hole cavity, and the anode oxide film for handling the anode workpiece is carried out at sealing of hole
Reason.
15. method for sealing as claimed in claim 14, it is characterised in that the hole sealing agent includes water, water vapour, contains ion
Aqueous solvent, the aqueous solvent containing molecule or the solvent containing suspension；
Wherein described ion includes the ion with transition elements；
Wherein described molecule is included with hydrophobic alkyl molecule or with hydrophilic polyhydroxylated molecule；And
Wherein described suspension includes Teflon, alumina powder, titania powder, ceramic pond powder, metal dust, high score
Sub- powder or diamond powder.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW105111054A TWI588300B (en) | 2016-04-08 | 2016-04-08 | Sealing equipment and method for sealing pores of anodic oxide film by using vacuum and injection steam |
| TW105111054 | 2016-04-08 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107268060A true CN107268060A (en) | 2017-10-20 |
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| CN201610298337.4A Pending CN107268060A (en) | 2016-04-08 | 2016-05-06 | Hole sealing equipment and method for sealing hole of anodic oxide film by using vacuum and jet steam |
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| JP (1) | JP6337052B2 (en) |
| CN (1) | CN107268060A (en) |
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| CN112466512A (en) * | 2020-11-16 | 2021-03-09 | 深圳市铂科新材料股份有限公司 | Inorganic coated insulated copper wire and preparation method thereof |
| CN112725860A (en) * | 2021-01-16 | 2021-04-30 | 郝云霞 | Simple micro-arc oxidation aluminum material treatment method |
| CN113122833A (en) * | 2021-04-11 | 2021-07-16 | 常龙 | Aluminum alloy passivation method |
| CN114540806A (en) * | 2021-04-11 | 2022-05-27 | 常龙 | Aluminum alloy passivation film treatment method |
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| US11312107B2 (en) * | 2018-09-27 | 2022-04-26 | Apple Inc. | Plugging anodic oxides for increased corrosion resistance |
| CN109114617B (en) * | 2018-10-12 | 2024-01-05 | 福建优净星环境科技有限公司 | Oil-sticking-free electrostatic oil smoke filtering device and manufacturing method thereof |
| CN113913897B (en) * | 2021-10-12 | 2024-01-09 | 长安大学 | Preparation method of ceramic membrane with antibacterial function based on magnesium alloy |
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Also Published As
| Publication number | Publication date |
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| JP2017186638A (en) | 2017-10-12 |
| TWI588300B (en) | 2017-06-21 |
| TW201736645A (en) | 2017-10-16 |
| JP6337052B2 (en) | 2018-06-06 |
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Application publication date: 20171020 |
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| RJ01 | Rejection of invention patent application after publication |