CN109183125A - A kind of titanium cup process for surface oxidation - Google Patents
A kind of titanium cup process for surface oxidation Download PDFInfo
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- CN109183125A CN109183125A CN201811306859.XA CN201811306859A CN109183125A CN 109183125 A CN109183125 A CN 109183125A CN 201811306859 A CN201811306859 A CN 201811306859A CN 109183125 A CN109183125 A CN 109183125A
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- China
- Prior art keywords
- titanium cup
- titanium
- cup
- solution
- pickling
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 417
- 239000010936 titanium Substances 0.000 title claims abstract description 417
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 417
- 238000000034 method Methods 0.000 title claims abstract description 69
- 230000008569 process Effects 0.000 title claims abstract description 57
- 238000010301 surface-oxidation reaction Methods 0.000 title claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 151
- 238000005554 pickling Methods 0.000 claims abstract description 139
- 238000007743 anodising Methods 0.000 claims abstract description 81
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 44
- 239000003792 electrolyte Substances 0.000 claims abstract description 38
- 238000004140 cleaning Methods 0.000 claims abstract description 24
- 238000004381 surface treatment Methods 0.000 claims abstract description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 84
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 75
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 66
- 229940053652 fluorinse Drugs 0.000 claims description 57
- 239000007788 liquid Substances 0.000 claims description 45
- 230000003647 oxidation Effects 0.000 claims description 32
- 150000002978 peroxides Chemical class 0.000 claims description 32
- 229910019142 PO4 Inorganic materials 0.000 claims description 25
- 239000010452 phosphate Substances 0.000 claims description 25
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 25
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 24
- 239000003381 stabilizer Substances 0.000 claims description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 20
- 229910017604 nitric acid Inorganic materials 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 14
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 13
- 229910052698 phosphorus Inorganic materials 0.000 claims description 13
- 239000011574 phosphorus Substances 0.000 claims description 13
- 238000002425 crystallisation Methods 0.000 claims description 12
- 230000008025 crystallization Effects 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 12
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 12
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 12
- 238000005498 polishing Methods 0.000 claims description 12
- 230000001681 protective effect Effects 0.000 claims description 12
- 238000005488 sandblasting Methods 0.000 claims description 12
- 239000001488 sodium phosphate Substances 0.000 claims description 12
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 12
- 235000011008 sodium phosphates Nutrition 0.000 claims description 12
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 12
- 239000002699 waste material Substances 0.000 claims description 12
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical group [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 11
- 235000019797 dipotassium phosphate Nutrition 0.000 claims description 11
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 230000008859 change Effects 0.000 claims description 3
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 3
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 3
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000010436 fluorite Substances 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims 1
- 239000000243 solution Substances 0.000 description 205
- 239000000203 mixture Substances 0.000 description 29
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 12
- 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 description 9
- 235000014786 phosphorus Nutrition 0.000 description 9
- 229910052708 sodium Inorganic materials 0.000 description 9
- 239000011734 sodium Substances 0.000 description 9
- 239000011775 sodium fluoride Substances 0.000 description 9
- 235000013024 sodium fluoride Nutrition 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 238000009938 salting Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010227 cup method (microbiological evaluation) Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- -1 phosphorus Potassium hydrogen phthalate Chemical group 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/106—Other heavy metals refractory metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention discloses a kind of titanium cup process for surface oxidation, comprising the following steps: is surface-treated, and is deoiled to the titanium cup after surface treatment, cleaning treatment to titanium cup；Then titanium cup is totally submerged by configuration pickling solution A by fixed device cleans in pickling solution A；20-30s is cleaned with clear water；Pickling B solution is configured, titanium cup is totally submerged in pickling B solution by fixed device, cleans 60-120s；It is cleaned with clear water；An anodizing tank is taken, titanium cup is hung on to the anode of anodizing tank, the titanium sheet for overpickling of learning from else's experience and the cathode for being set as anodizing tank；The electrolyte being placed in anodizing tank is configured, the anode, cathode are totally submerged in the electrolyte；Jointed anode, cathode and the DC voltage for applying 1 ~ 150V make titanium cup surface and water generate oxidation reaction, to form colored oxide film on titanium cup surface, the uniformity and aesthetics for the titanium cup surface film oxide that the present invention is formed are greatly improved.
Description
Technical field
The present invention relates to a kind of titanium cup more particularly to a kind of titanium cup process for surface oxidation.
Background technique
Titanium cup is the cup being made into titanium, and titanium has good heat resistance and corrosion resistance, to extend cup
Service life.But existing its color of titanium cup is more single, when use, is more uninteresting, dull, and some producers pass through thus
Oxidation technology forms different colors on titanium cup surface, increases the interest that titanium cup uses.But these existing oxidation works
Skill is also easy to produce impurity, affects the degree of purity of titanium cup surface color, and color more dimness, the color point formed on titanium cup surface
Cloth is uneven, needs to make improvements this.
Summary of the invention
The present invention is for titanium cup color existing in the prior art is single and the degree of purity of titanium cup surface color is low, darker in color
Light, the defects of being unevenly distributed, provides a kind of new titanium cup process for surface oxidation.
In order to solve the above-mentioned technical problem, the invention is realized by the following technical scheme:
A kind of titanium cup process for surface oxidation, comprising the following steps:
(a) a titanium cup is taken, titanium cup is surface-treated, and is deoiled, after cleaning treatment to the titanium cup after surface treatment；
(b) titanium cup is fixed using fixed device, titanium cup is made to keep stablizing；
(c) pickling solution A is configured, pickling is carried out to titanium cup surface, the pickling solution A includes that the nitric acid of 5% ~ 15% concentration is molten
Liquid, the hydrofluoric acid solution of 5% ~ 15% concentration, the Fluorinse of 100g/L ~ 150g/L concentration, water mix, wherein the nitre
Acid solution, hydrofluoric acid solution, Fluorinse, water mixed proportion be 5:5:10:80-15:15:15:55, by pickling solution A
It pours into descaling bath, then titanium cup is totally submerged in pickling solution A by fixed device, cleans 60-85s；
(d) titanium cup rim of a cup is taken out from pickling solution A by fixed device downward, cleans 20-30s with clear water；
(e) pickling B solution is configured, the pickling B solution includes the peroxide solutions of 100g/L-150g/L, 5% ~ 15% concentration
Hydrofluoric acid solution, 100g/L ~ 150g/L concentration Fluorinse, water mix, wherein the peroxide solutions, hydrogen
Fluorspar acid solution, Fluorinse, water mixed proportion be 5:5:10:80-15:15:15:55, pickling B solution is poured into descaling bath
In, then titanium cup is totally submerged in pickling B solution by fixed device, cleans 60-120s；
(f) titanium cup rim of a cup is taken out from pickling B solution by fixed device downward, is cleaned 2-3 times with clear water, cleaned every time
20-30s；
(g) anodizing tank is taken, titanium cup is hung on to the anode of anodizing tank, the titanium for overpickling of learning from else's experience by fixed device
Piece and the cathode for being set as anodizing tank, the titanium sheet area be 4 times or more of titanium cup surface area, the anode, cathode
Interpolar is away from for 10-35cm；
(h) configure the electrolyte that is placed in anodizing tank, the electrolyte include 80g/L ~ 150g/L acetic acid solution,
The phosphate solution of 80g/L ~ 150g/L, the Fluorinse of 100g/L ~ 150g/L, the stabilizer of 5g/L ~ 15g/L, water mixing
It forms, wherein the mixed proportion of the acetic acid solution, phosphate solution, Fluorinse, stabilizer, water is 8:8:10:0.5:
73.5-15:15:15:1.5:53.5 the anode, cathode are totally submerged in the electrolyte；
(i) jointed anode, cathode and the DC voltage for applying 1 ~ 150V form unidirectional current circuit, make titanium cup surface and aquatic products
Raw oxidation reaction, oxidation time 2-8min, to form colored oxide film on titanium cup surface；
(j) it takes out titanium cup to be cleaned, takes out and dry up after titanium cup is impregnated 5-20min in clear water, by the titanium cup after drying
Put on protective bag.
The effect of step (a) is cleaned to titanium cup surface, prevents the spot on titanium cup surface from influencing the oxygen on titanium cup surface
Change effect, step (b) is for fixing titanium cup, and convenient for carrying out pickling to titanium cup surface, the effect of step (c) is molten with pickling A
Liquid further removes the oxide layer and other impurities of titanium cup surface self-assembling formation, so that the anodic oxidation for subsequent titanium cup surface is done
It is good to prepare, oxidation effectiveness is improved, titanium cup rim of a cup is taken out from pickling solution A downward in step (d), can speed up and drain titanium cup
The pickling solution A on surface, clear water cleaning 20-30s can further remove the pickling solution A of titanium cup surface residual, step (e)
Effect is remaining with the pickling solution A on pickling B solution removal titanium cup surface, while being pre-oxidized to titanium cup surface, forms one
The very thin directive oxide film of tool of layer, improves titanium cup surface color homogeneity and vivid degree after subsequent anodic oxidation,
Titanium cup rim of a cup is taken out from pickling B solution downward in step (f), can speed up the pickling B solution for draining titanium cup surface, clear water
Cleaning 20-30s can further remove the pickling B solution of titanium cup surface residual, step (g), (h), (i) for realizing titanium cup table
The oxidation in face forms stable, uniform oxidation film, so that color is formed on titanium cup surface, wherein the titanium sheet area as cathode
It is 4 times or more of the titanium cup area as anode, can guarantees current stability in oxidation process, while reduces cathode fever speed
Degree accelerates anodic oxidation speed, guarantees the homogeneity of the titanium cup surface film oxide as anode, anode, cathode interpolar away from setting
The resistance that being set to 10-35cm can control between anode, cathode is kept in a certain range, to be further ensured that as anode
The homogeneity of titanium cup surface film oxide simplifies the operating procedure of titanium cup method for oxidation using anodized titanium cup, improves
Treatment effeciency, while the oxidation film color that titanium cup surface is formed is uniform, color is beautiful, greatly improve the beauty of titanium cup
Degree.Titanium cup is cleaned and is dried up by step (j), can be removed titanium cup electrolyte remained on surface, be avoided remaining electrolyte
Titanium cup surface after formation colored oxide film is impacted, and by the protection of protective bag, it can further protect formation
Colored oxide film, to guarantee the uniformity and aesthetics of the oxidation film on finally obtained titanium cup surface.
Preferably, a kind of titanium cup process for surface oxidation described above, in the step (a) to titanium cup carry out surface into
The method of row processing is sandblasting or polishing or crystallization.
Impact and shear action of the abrasive material to titanium cup surface can be utilized by carrying out sandblasting to titanium cup surface, obtain titanium cup surface
Cleannes and different roughness centainly are obtained, the mechanical performance on titanium cup surface is improved, polishing can be improved the light on titanium cup surface
Bright degree, so as to improve the appearance of titanium cup, crystallization treatment can strengthen the hardness on titanium cup surface, improve mechanical property.
Preferably, a kind of titanium cup process for surface oxidation described above, in the step (c), (e), cleaned in titanium cup
In the process, titanium cup is constantly moved horizontally with the speed of 5-20cm/s by fixed device repeatedly, and the descaling bath temperature is tieed up
It holds at 15-25 DEG C.
Titanium cup is constantly moved horizontally repeatedly with the speed of 5-20cm/s, and effect is that heat of reaction accumulation is avoided to lead to solution
It splashes, descaling bath temperature maintains 15-25 DEG C, can control reaction rate, avoids heat of reaction accumulation that solution is caused to splash, draws
Safety accident is sent out, and descaling bath temperature maintains 15-25 DEG C can also control the reaction rate that multiple titanium cups are put into descaling bath,
To guarantee titanium cup uniformity for the treatment of.
Preferably, a kind of titanium cup process for surface oxidation described above, the step (c), (d), (e), (f) are processed
Cheng Zhong keeps air draft state, and the gas of discharge is carried out water curtain processing, when the waste liquid pH value that water curtain processing generates is down to 3,
Clear water of the replacement for water curtain processing.
Air draft state is kept, the pickling gas generated in oxidation process can be discharged, accumulation in anodizing tank is prevented
Excessive sour gas, influences the oxidation effectiveness of titanium cup, and water curtain processing can absorb the pickling gas of discharge, guarantee operating environment
Safety, replacement pH value be down to 3 water curtain dispose waste liquid can be improved water curtain absorb pickling gas effect.
Preferably, a kind of titanium cup process for surface oxidation described above, in the step (g), the quantity of the titanium sheet
For 5 and it is located at front, rear, left side, right side, the lower section of titanium cup, the titanium cup is located in the anodizing tank
The heart.
Titanium sheet is placed on to front, rear, left side, right side, the lower section of titanium cup, the cathode and sun of different directions can be controlled
Resistance between pole guarantees titanium cup oxidation effectiveness in different directions and improves the uniformity of titanium cup surface film oxide and consistent
Property.
Preferably, a kind of titanium cup process for surface oxidation described above, in the step (i), apply direct current briquetting
Include following steps:
(1) target voltage and interference voltage are set, the interference voltage is the 110% of target voltage；
(2) power supply pressurizes, and constant current is formed in anodizing tank, while the voltage in anodizing tank gradually rises to mistake
It is full of voltage；
(3) target voltage being retreated to by interference voltage in 0.5s, when reaching target voltage, electric current is gradually reduced to current threshold,
And stop power supply pressurization when electric current is down to current threshold.
Voltage is first risen to interference voltage, then is down to target voltage, is able to extend the working time of target voltage, thus
Guarantee the time for shortening anodic oxidation while oxidation effectiveness, improves the efficiency that titanium cup surface forms oxidation film.
Preferably, a kind of titanium cup process for surface oxidation described above, in the step (j), 0.2 ~ 0.3Mpa is used
Compressed air titanium cup is dried up.
The compressed air of 0.2 ~ 0.3Mpa can speed up the evaporation of titanium cup surface moisture, while blow away the ash on titanium cup surface
Dirt guarantees the dried and clean on titanium cup surface.
Preferably, a kind of titanium cup process for surface oxidation described above, in the step (e), the peroxide is
Hydrogen peroxide.
Hydrogen peroxide can form one layer of very thin oxidation film on titanium cup surface, be conducive to improve titanium cup surface film oxide
Generate quality and brightness.
Preferably, a kind of titanium cup process for surface oxidation described above, in the step (h), the phosphate is phosphorus
Potassium hydrogen phthalate or dibastic sodium phosphate or potassium dihydrogen phosphate or sodium dihydrogen phosphate.
Phosphate good conductivity, property is stablized, while P elements can be improved the wearability of titanium cup surface film oxide, also can
The brightness of oxidation film is enough improved, wherein potassium hydrogen phosphate, dibastic sodium phosphate, potassium dihydrogen phosphate, sodium dihydrogen phosphate have more excellent
Electric conductivity can preferably realize phosphate to the promotion effect of titanium cup surface oxidation film properties.
Preferably, a kind of titanium cup process for surface oxidation described above, in the step (b), the fixed device
Material is titanium and fixes the upper end of titanium cup, lower end.
Fixed device uses titanium matter that the metal parts being located in electrolyte can be guaranteed for same material, it is ensured that conductive
The consistency of performance improves the oxidation effectiveness on titanium cup surface.
Detailed description of the invention
Fig. 1 is voltage, the curent change schematic diagram of step (i) in the present invention.
Specific embodiment
With reference to the accompanying drawing 1 and specific embodiment present invention is further described in detail, but they are not to this hair
Bright limitation:
Embodiment 1
A kind of titanium cup process for surface oxidation, comprising the following steps:
(a) a titanium cup is taken, titanium cup is surface-treated, and is deoiled, after cleaning treatment to the titanium cup after surface treatment；
(b) titanium cup is fixed using fixed device, titanium cup is made to keep stablizing；
(c) pickling solution A is configured, pickling is carried out to titanium cup surface, the pickling solution A includes the nitric acid solution of 5% concentration, 5%
The hydrofluoric acid solution of concentration, the Fluorinse of 100g/L concentration, water mix, wherein the nitric acid solution, hydrofluoric acid are molten
Liquid, Fluorinse, water mixed proportion be 5:5:10:80, pickling solution A is poured into descaling bath, fixed dress is then passed through
It sets and titanium cup is totally submerged in pickling solution A, clean 60s；
(d) titanium cup rim of a cup is taken out from pickling solution A by fixed device downward, cleans 30s with clear water；
(e) pickling B solution is configured, the pickling B solution includes that the peroxide solutions of 100g/L, the hydrofluoric acid of 5% concentration are molten
Liquid, the Fluorinse of 100g/L concentration, water mix, wherein the peroxide solutions, hydrofluoric acid solution, sodium fluoride are molten
Liquid, water mixed proportion be 5:5:10:80, pickling B solution is poured into descaling bath, it is then by fixed device that titanium cup is complete
It is immersed in pickling B solution, cleans 60s；
(f) titanium cup rim of a cup is taken out from pickling B solution by fixed device downward, is cleaned 2 times with clear water, cleans 30s every time；
(g) anodizing tank is taken, titanium cup is hung on to the anode of anodizing tank, the titanium for overpickling of learning from else's experience by fixed device
Piece and the cathode for being set as anodizing tank, the titanium sheet area be 4 times or more of titanium cup surface area, the anode, cathode
Interpolar is away from for 10cm；
(h) electrolyte being placed in anodizing tank is configured, the electrolyte includes the phosphorus of the acetic acid solution of 80g/L, 80g/L
Acid salt solution, the Fluorinse of 100g/L, the stabilizer of 5g/L, water mix, wherein the acetic acid solution, phosphate are molten
Liquid, Fluorinse, stabilizer, water mixed proportion be 8:8:10:0.5:73.5, the anode, cathode are totally submerged in institute
It states in electrolyte；
(i) jointed anode, cathode and the DC voltage for applying 1 ~ 150V form unidirectional current circuit, make titanium cup surface and aquatic products
Raw oxidation reaction, oxidation time 2min, to form colored oxide film on titanium cup surface；
(j) it takes out titanium cup to be cleaned, takes out and dry up after titanium cup is impregnated 5min in clear water, it will be on the titanium glass holder after drying
Protective bag.
Preferably, carrying out the method that surface is handled to titanium cup in the step (a) is sandblasting or polishing or crystallization.
Preferably, in the step (c), (e), in titanium cup cleaning process, by fixed device with the speed of 5cm/s
Titanium cup is constantly moved horizontally repeatedly, and the descaling bath temperature maintains 15 DEG C.
Preferably, the step (c), (d), (e), in (f) treatment process, keep air draft state, and by the gas of discharge
Body carries out water curtain processing, when the waste liquid pH value that water curtain processing generates is down to 3, clear water of the replacement for water curtain processing.
Preferably, in the step (g), the quantity of the titanium sheet be 5 and be located at the front of titanium cup, rear,
Left side, right side, lower section, the titanium cup are located at the center of the anodizing tank.
Preferably, in the step (i), apply DC voltage the following steps are included:
(1) target voltage and interference voltage are set, the interference voltage is the 110% of target voltage, such as target voltage is arranged
For 136.4V, 150V is set by interference voltage；
(2) power supply pressurizes, and constant current is formed in anodizing tank, while the voltage in anodizing tank gradually rises to mistake
It is full of voltage；
(3) target voltage being retreated to by interference voltage in 0.5s, when reaching target voltage, electric current is gradually reduced to current threshold,
And stop power supply pressurization when electric current is down to current threshold.
Preferably, titanium cup is dried up using the compressed air of 0.2Mpa in the step (j).
Preferably, the peroxide is hydrogen peroxide in the step (e).
Preferably, the phosphate is potassium hydrogen phosphate or dibastic sodium phosphate or potassium dihydrogen phosphate or phosphorus in the step (h)
Acid dihydride sodium.
Preferably, the material of the fixed device is titanium and fixes the upper end of titanium cup, lower end in the step (b).
Embodiment 2
A kind of titanium cup process for surface oxidation, comprising the following steps:
(a) a titanium cup is taken, titanium cup is surface-treated, and is deoiled, after cleaning treatment to the titanium cup after surface treatment；
(b) titanium cup is fixed using fixed device, titanium cup is made to keep stablizing；
(c) configure pickling solution A, to titanium cup surface carry out pickling, the pickling solution A include 10% concentration nitric acid solution,
The hydrofluoric acid solution of 10% concentration, the Fluorinse of 125g/L concentration, water mix, wherein the nitric acid solution, hydrofluoric acid
Solution, Fluorinse, water mixed proportion be 10:10:12.5:67.5, pickling solution A is poured into descaling bath, is then led to
It crosses fixed device titanium cup is totally submerged in pickling solution A, cleans 60s；
(d) titanium cup rim of a cup is taken out from pickling solution A by fixed device downward, cleans 25s with clear water；
(e) pickling B solution is configured, the pickling B solution includes that the peroxide solutions of 100g/L, the hydrofluoric acid of 5% concentration are molten
Liquid, the Fluorinse of 100g/L concentration, water mix, wherein the peroxide solutions, hydrofluoric acid solution, sodium fluoride are molten
Liquid, water mixed proportion be 5:5:10:80, pickling B solution is poured into descaling bath, it is then by fixed device that titanium cup is complete
It is immersed in pickling B solution, cleans 60s；
(f) titanium cup rim of a cup is taken out from pickling B solution by fixed device downward, is cleaned 2 times with clear water, cleans 25s every time；
(g) anodizing tank is taken, titanium cup is hung on to the anode of anodizing tank, the titanium for overpickling of learning from else's experience by fixed device
Piece and the cathode for being set as anodizing tank, the titanium sheet area be 4 times or more of titanium cup surface area, the anode, cathode
Interpolar is away from for 22.5cm；
(h) electrolyte being placed in anodizing tank is configured, the electrolyte includes the phosphorus of the acetic acid solution of 80g/L, 80g/L
Acid salt solution, the Fluorinse of 100g/L, the stabilizer of 5g/L, water mix, wherein the acetic acid solution, phosphate are molten
Liquid, Fluorinse, stabilizer, water mixed proportion be 8:8:10:0.5:73.5, the anode, cathode are totally submerged in institute
It states in electrolyte；
(i) jointed anode, cathode and the DC voltage for applying 1 ~ 150V form unidirectional current circuit, make titanium cup surface and aquatic products
Raw oxidation reaction, oxidation time 5min, to form colored oxide film on titanium cup surface；
(j) it takes out titanium cup to be cleaned, takes out and dry up after titanium cup is impregnated 12.5min in clear water, by the titanium cup after drying
Put on protective bag.
Preferably, carrying out the method that surface is handled to titanium cup in the step (a) is sandblasting or polishing or crystallization.
Preferably, in the step (c), (e), in titanium cup cleaning process, by fixed device with 12.5cm/s's
Speed constantly moves horizontally titanium cup repeatedly, and the descaling bath temperature maintains 20 DEG C.
Preferably, the step (c), (d), (e), in (f) treatment process, keep air draft state, and by the gas of discharge
Body carries out water curtain processing, when the waste liquid pH value that water curtain processing generates is down to 3, clear water of the replacement for water curtain processing.
Preferably, in the step (g), the quantity of the titanium sheet be 5 and be located at the front of titanium cup, rear,
Left side, right side, lower section, the titanium cup are located at the center of the anodizing tank.
Preferably, in the step (i), apply DC voltage the following steps are included:
(1) target voltage and interference voltage are set, the interference voltage is the 110% of target voltage, such as target voltage is arranged
For 130V, 143V is set by interference voltage；
(2) power supply pressurizes, and constant current is formed in anodizing tank, while the voltage in anodizing tank gradually rises to mistake
It is full of voltage；
(3) target voltage being retreated to by interference voltage in 0.5s, when reaching target voltage, electric current is gradually reduced to current threshold,
And stop power supply pressurization when electric current is down to current threshold.
Preferably, titanium cup is dried up using the compressed air of 0.2Mpa in the step (j).
Preferably, the peroxide is hydrogen peroxide in the step (e).
Preferably, the phosphate is potassium hydrogen phosphate or dibastic sodium phosphate or potassium dihydrogen phosphate or phosphorus in the step (h)
Acid dihydride sodium.
Preferably, the material of the fixed device is titanium and fixes the upper end of titanium cup, lower end in the step (b).
Embodiment 3
A kind of titanium cup process for surface oxidation, comprising the following steps:
(a) a titanium cup is taken, titanium cup is surface-treated, and is deoiled, after cleaning treatment to the titanium cup after surface treatment；
(b) titanium cup is fixed using fixed device, titanium cup is made to keep stablizing；
(c) configure pickling solution A, to titanium cup surface carry out pickling, the pickling solution A include 15% concentration nitric acid solution,
The hydrofluoric acid solution of 15% concentration, the Fluorinse of 150g/L concentration, water mix, wherein the nitric acid solution, hydrofluoric acid
Solution, Fluorinse, water mixed proportion be 15:15:15:55, pickling solution A is poured into descaling bath, then by solid
Determine device titanium cup is totally submerged in pickling solution A, cleans 60s；
(d) titanium cup rim of a cup is taken out from pickling solution A by fixed device downward, cleans 20s with clear water；
(e) pickling B solution is configured, the pickling B solution includes that the peroxide solutions of 100g/L, the hydrofluoric acid of 5% concentration are molten
Liquid, the Fluorinse of 100g/L concentration, water mix, wherein the peroxide solutions, hydrofluoric acid solution, sodium fluoride are molten
Liquid, water mixed proportion be 5:5:10:80, pickling B solution is poured into descaling bath, it is then by fixed device that titanium cup is complete
It is immersed in pickling B solution, cleans 60s；
(f) titanium cup rim of a cup is taken out from pickling B solution by fixed device downward, is cleaned 3 times with clear water, cleans 20s every time；
(g) anodizing tank is taken, titanium cup is hung on to the anode of anodizing tank, the titanium for overpickling of learning from else's experience by fixed device
Piece and the cathode for being set as anodizing tank, the titanium sheet area be 4 times or more of titanium cup surface area, the anode, cathode
Interpolar is away from for 35cm；
(h) electrolyte being placed in anodizing tank is configured, the electrolyte includes the phosphorus of the acetic acid solution of 80g/L, 80g/L
Acid salt solution, the Fluorinse of 100g/L, the stabilizer of 5g/L, water mix, wherein the acetic acid solution, phosphate are molten
Liquid, Fluorinse, stabilizer, water mixed proportion be 8:8:10:0.5:73.5, the anode, cathode are totally submerged in institute
It states in electrolyte；
(i) jointed anode, cathode and the DC voltage for applying 1 ~ 150V form unidirectional current circuit, make titanium cup surface and aquatic products
Raw oxidation reaction, oxidation time 8min, to form colored oxide film on titanium cup surface；
(j) it takes out titanium cup to be cleaned, takes out and dry up after titanium cup is impregnated 20min in clear water, by the titanium glass holder after drying
Upper protective bag.
Preferably, carrying out the method that surface is handled to titanium cup in the step (a) is sandblasting or polishing or crystallization.
Preferably, in the step (c), (e), in titanium cup cleaning process, by fixed device with the speed of 20cm/s
Degree constantly moves horizontally titanium cup repeatedly, and the descaling bath temperature maintains 25 DEG C.
Preferably, the step (c), (d), (e), in (f) treatment process, keep air draft state, and by the gas of discharge
Body carries out water curtain processing, when the waste liquid pH value that water curtain processing generates is down to 3, clear water of the replacement for water curtain processing.
Preferably, in the step (g), the quantity of the titanium sheet be 5 and be located at the front of titanium cup, rear,
Left side, right side, lower section, the titanium cup are located at the center of the anodizing tank.
Preferably, in the step (i), apply DC voltage the following steps are included:
(1) target voltage and interference voltage are set, the interference voltage is the 110% of target voltage, such as target voltage is arranged
For 110V, 121V is set by interference voltage；
(2) power supply pressurizes, and constant current is formed in anodizing tank, while the voltage in anodizing tank gradually rises to mistake
It is full of voltage；
(3) target voltage being retreated to by interference voltage in 0.5s, when reaching target voltage, electric current is gradually reduced to current threshold,
And stop power supply pressurization when electric current is down to current threshold.
Preferably, titanium cup is dried up using the compressed air of 0.2Mpa in the step (j).
Preferably, the peroxide is hydrogen peroxide in the step (e).
Preferably, the phosphate is potassium hydrogen phosphate or dibastic sodium phosphate or potassium dihydrogen phosphate or phosphorus in the step (h)
Acid dihydride sodium.
Preferably, the material of the fixed device is titanium and fixes the upper end of titanium cup, lower end in the step (b).
Embodiment 4
A kind of titanium cup process for surface oxidation, comprising the following steps:
(a) a titanium cup is taken, titanium cup is surface-treated, and is deoiled, after cleaning treatment to the titanium cup after surface treatment；
(b) titanium cup is fixed using fixed device, titanium cup is made to keep stablizing；
(c) pickling solution A is configured, pickling is carried out to titanium cup surface, the pickling solution A includes the nitric acid solution of 5% concentration, 5%
The hydrofluoric acid solution of concentration, the Fluorinse of 100g/L concentration, water mix, wherein the nitric acid solution, hydrofluoric acid are molten
Liquid, Fluorinse, water mixed proportion be 5:5:10:80, pickling solution A is poured into descaling bath, fixed dress is then passed through
It sets and titanium cup is totally submerged in pickling solution A, clean 72.5s；
(d) titanium cup rim of a cup is taken out from pickling solution A by fixed device downward, cleans 30s with clear water；
(e) pickling B solution is configured, the pickling B solution includes that the peroxide solutions of 125g/L, the hydrofluoric acid of 10% concentration are molten
Liquid, the Fluorinse of 125g/L concentration, water mix, wherein the peroxide solutions, hydrofluoric acid solution, sodium fluoride are molten
Liquid, water mixed proportion be 10:10:12.5:67.5, pickling B solution is poured into descaling bath, then by fixed device by titanium
Cup is totally submerged in pickling B solution, cleans 90s；
(f) titanium cup rim of a cup is taken out from pickling B solution by fixed device downward, is cleaned 2 times with clear water, cleans 30s every time；
(g) anodizing tank is taken, titanium cup is hung on to the anode of anodizing tank, the titanium for overpickling of learning from else's experience by fixed device
Piece and the cathode for being set as anodizing tank, the titanium sheet area be 4 times or more of titanium cup surface area, the anode, cathode
Interpolar is away from for 10cm；
(h) electrolyte being placed in anodizing tank is configured, the electrolyte includes the acetic acid solution of 115g/L, 115g/L
Phosphate solution, the Fluorinse of 125g/L, the stabilizer of 10g/L, water mix, wherein the acetic acid solution, phosphoric acid
Salting liquid, Fluorinse, stabilizer, water mixed proportion be 11.5:11.5:12.5:1:63.5, the anode, cathode are complete
It is immersed in the electrolyte entirely；
(i) jointed anode, cathode and the DC voltage for applying 1 ~ 150V form unidirectional current circuit, make titanium cup surface and aquatic products
Raw oxidation reaction, oxidation time 2min, to form colored oxide film on titanium cup surface；
(j) it takes out titanium cup to be cleaned, takes out and dry up after titanium cup is impregnated 5min in clear water, it will be on the titanium glass holder after drying
Protective bag.
Preferably, carrying out the method that surface is handled to titanium cup in the step (a) is sandblasting or polishing or crystallization.
Preferably, in the step (c), (e), in titanium cup cleaning process, by fixed device with the speed of 5cm/s
Titanium cup is constantly moved horizontally repeatedly, and the descaling bath temperature maintains 15 DEG C.
Preferably, the step (c), (d), (e), in (f) treatment process, keep air draft state, and by the gas of discharge
Body carries out water curtain processing, when the waste liquid pH value that water curtain processing generates is down to 3, clear water of the replacement for water curtain processing.
Preferably, in the step (g), the quantity of the titanium sheet be 5 and be located at the front of titanium cup, rear,
Left side, right side, lower section, the titanium cup are located at the center of the anodizing tank.
Preferably, in the step (i), apply DC voltage the following steps are included:
(1) target voltage and interference voltage are set, the interference voltage is the 110% of target voltage, such as target voltage is arranged
For 100V, 110V is set by interference voltage；
(2) power supply pressurizes, and constant current is formed in anodizing tank, while the voltage in anodizing tank gradually rises to mistake
It is full of voltage；
(3) target voltage being retreated to by interference voltage in 0.5s, when reaching target voltage, electric current is gradually reduced to current threshold,
And stop power supply pressurization when electric current is down to current threshold.
Preferably, titanium cup is dried up using the compressed air of 0.25Mpa in the step (j).
Preferably, the peroxide is hydrogen peroxide in the step (e).
Preferably, the phosphate is potassium hydrogen phosphate or dibastic sodium phosphate or potassium dihydrogen phosphate or phosphorus in the step (h)
Acid dihydride sodium.
Preferably, the material of the fixed device is titanium and fixes the upper end of titanium cup, lower end in the step (b).
Embodiment 5
A kind of titanium cup process for surface oxidation, comprising the following steps:
(a) a titanium cup is taken, titanium cup is surface-treated, and is deoiled, after cleaning treatment to the titanium cup after surface treatment；
(b) titanium cup is fixed using fixed device, titanium cup is made to keep stablizing；
(c) configure pickling solution A, to titanium cup surface carry out pickling, the pickling solution A include 10% concentration nitric acid solution,
The hydrofluoric acid solution of 10% concentration, the Fluorinse of 125g/L concentration, water mix, wherein the nitric acid solution, hydrofluoric acid
Solution, Fluorinse, water mixed proportion be 10:10:12.5:67.5, pickling solution A is poured into descaling bath, is then led to
It crosses fixed device titanium cup is totally submerged in pickling solution A, cleans 72.5s；
(d) titanium cup rim of a cup is taken out from pickling solution A by fixed device downward, cleans 25s with clear water；
(e) pickling B solution is configured, the pickling B solution includes that the peroxide solutions of 125g/L, the hydrofluoric acid of 10% concentration are molten
Liquid, the Fluorinse of 125g/L concentration, water mix, wherein the peroxide solutions, hydrofluoric acid solution, sodium fluoride are molten
Liquid, water mixed proportion be 10:10:12.5:67.5, pickling B solution is poured into descaling bath, then by fixed device by titanium
Cup is totally submerged in pickling B solution, cleans 90s；
(f) titanium cup rim of a cup is taken out from pickling B solution by fixed device downward, is cleaned 2 times with clear water, cleans 25s every time；
(g) anodizing tank is taken, titanium cup is hung on to the anode of anodizing tank, the titanium for overpickling of learning from else's experience by fixed device
Piece and the cathode for being set as anodizing tank, the titanium sheet area be 4 times or more of titanium cup surface area, the anode, cathode
Interpolar is away from for 22.5cm；
(h) electrolyte being placed in anodizing tank is configured, the electrolyte includes the acetic acid solution of 115g/L, 115g/L
Phosphate solution, the Fluorinse of 125g/L, the stabilizer of 10g/L, water mix, wherein the acetic acid solution, phosphoric acid
Salting liquid, Fluorinse, stabilizer, water mixed proportion be 11.5:11.5:12.5:1:63.5, the anode, cathode are complete
It is immersed in the electrolyte entirely；
(i) jointed anode, cathode and the DC voltage for applying 1 ~ 150V form unidirectional current circuit, make titanium cup surface and aquatic products
Raw oxidation reaction, oxidation time 5min, to form colored oxide film on titanium cup surface；
(j) it takes out titanium cup to be cleaned, takes out and dry up after titanium cup is impregnated 12.5min in clear water, by the titanium cup after drying
Put on protective bag.
Preferably, carrying out the method that surface is handled to titanium cup in the step (a) is sandblasting or polishing or crystallization.
Preferably, in the step (c), (e), in titanium cup cleaning process, by fixed device with 12.5cm/s's
Speed constantly moves horizontally titanium cup repeatedly, and the descaling bath temperature maintains 20 DEG C.
Preferably, the step (c), (d), (e), in (f) treatment process, keep air draft state, and by the gas of discharge
Body carries out water curtain processing, when the waste liquid pH value that water curtain processing generates is down to 3, clear water of the replacement for water curtain processing.
Preferably, in the step (g), the quantity of the titanium sheet be 5 and be located at the front of titanium cup, rear,
Left side, right side, lower section, the titanium cup are located at the center of the anodizing tank.
Preferably, in the step (i), apply DC voltage the following steps are included:
(1) target voltage and interference voltage are set, the interference voltage is the 110% of target voltage, such as target voltage is arranged
For 80V, 88V is set by interference voltage；
(2) power supply pressurizes, and constant current is formed in anodizing tank, while the voltage in anodizing tank gradually rises to mistake
It is full of voltage；
(3) target voltage being retreated to by interference voltage in 0.5s, when reaching target voltage, electric current is gradually reduced to current threshold,
And stop power supply pressurization when electric current is down to current threshold.
Preferably, titanium cup is dried up using the compressed air of 0.25Mpa in the step (j).
Preferably, the peroxide is hydrogen peroxide in the step (e).
Preferably, the phosphate is potassium hydrogen phosphate or dibastic sodium phosphate or potassium dihydrogen phosphate or phosphorus in the step (h)
Acid dihydride sodium.
Preferably, the material of the fixed device is titanium and fixes the upper end of titanium cup, lower end in the step (b).
Embodiment 6
A kind of titanium cup process for surface oxidation, comprising the following steps:
(a) a titanium cup is taken, titanium cup is surface-treated, and is deoiled, after cleaning treatment to the titanium cup after surface treatment；
(b) titanium cup is fixed using fixed device, titanium cup is made to keep stablizing；
(c) configure pickling solution A, to titanium cup surface carry out pickling, the pickling solution A include 15% concentration nitric acid solution,
The hydrofluoric acid solution of 15% concentration, the Fluorinse of 150g/L concentration, water mix, wherein the nitric acid solution, hydrofluoric acid
Solution, Fluorinse, water mixed proportion be 15:15:15:55, pickling solution A is poured into descaling bath, then by solid
Determine device titanium cup is totally submerged in pickling solution A, cleans 72.5s；
(d) titanium cup rim of a cup is taken out from pickling solution A by fixed device downward, cleans 20s with clear water；
(e) pickling B solution is configured, the pickling B solution includes that the peroxide solutions of 125g/L, the hydrofluoric acid of 10% concentration are molten
Liquid, the Fluorinse of 125g/L concentration, water mix, wherein the peroxide solutions, hydrofluoric acid solution, sodium fluoride are molten
Liquid, water mixed proportion be 10:10:12.5:67.5, pickling B solution is poured into descaling bath, then by fixed device by titanium
Cup is totally submerged in pickling B solution, cleans 90s；
(f) titanium cup rim of a cup is taken out from pickling B solution by fixed device downward, is cleaned 3 times with clear water, cleans 20s every time；
(g) anodizing tank is taken, titanium cup is hung on to the anode of anodizing tank, the titanium for overpickling of learning from else's experience by fixed device
Piece and the cathode for being set as anodizing tank, the titanium sheet area be 4 times or more of titanium cup surface area, the anode, cathode
Interpolar is away from for 35cm；
(h) electrolyte being placed in anodizing tank is configured, the electrolyte includes the acetic acid solution of 115g/L, 115g/L
Phosphate solution, the Fluorinse of 125g/L, the stabilizer of 10g/L, water mix, wherein the acetic acid solution, phosphoric acid
Salting liquid, Fluorinse, stabilizer, water mixed proportion be 11.5:11.5:12.5:1:63.5, the anode, cathode are complete
It is immersed in the electrolyte entirely；
(i) jointed anode, cathode and the DC voltage for applying 1 ~ 150V form unidirectional current circuit, make titanium cup surface and aquatic products
Raw oxidation reaction, oxidation time 8min, to form colored oxide film on titanium cup surface；
(j) it takes out titanium cup to be cleaned, takes out and dry up after titanium cup is impregnated 20min in clear water, by the titanium glass holder after drying
Upper protective bag.
Preferably, carrying out the method that surface is handled to titanium cup in the step (a) is sandblasting or polishing or crystallization.
Preferably, in the step (c), (e), in titanium cup cleaning process, by fixed device with the speed of 20cm/s
Degree constantly moves horizontally titanium cup repeatedly, and the descaling bath temperature maintains 25 DEG C.
Preferably, the step (c), (d), (e), in (f) treatment process, keep air draft state, and by the gas of discharge
Body carries out water curtain processing, when the waste liquid pH value that water curtain processing generates is down to 3, clear water of the replacement for water curtain processing.
Preferably, in the step (g), the quantity of the titanium sheet be 5 and be located at the front of titanium cup, rear,
Left side, right side, lower section, the titanium cup are located at the center of the anodizing tank.
Preferably, in the step (i), apply DC voltage the following steps are included:
(1) target voltage and interference voltage are set, the interference voltage is the 110% of target voltage, such as target voltage is arranged
For 70V, 77V is set by interference voltage；
(2) power supply pressurizes, and constant current is formed in anodizing tank, while the voltage in anodizing tank gradually rises to mistake
It is full of voltage；
(3) target voltage being retreated to by interference voltage in 0.5s, when reaching target voltage, electric current is gradually reduced to current threshold,
And stop power supply pressurization when electric current is down to current threshold.
Preferably, titanium cup is dried up using the compressed air of 0.25Mpa in the step (j).
Preferably, the peroxide is hydrogen peroxide in the step (e).
Preferably, the phosphate is potassium hydrogen phosphate or dibastic sodium phosphate or potassium dihydrogen phosphate or phosphorus in the step (h)
Acid dihydride sodium.
Preferably, the material of the fixed device is titanium and fixes the upper end of titanium cup, lower end in the step (b).
Embodiment 7
A kind of titanium cup process for surface oxidation, comprising the following steps:
(a) a titanium cup is taken, titanium cup is surface-treated, and is deoiled, after cleaning treatment to the titanium cup after surface treatment；
(b) titanium cup is fixed using fixed device, titanium cup is made to keep stablizing；
(c) pickling solution A is configured, pickling is carried out to titanium cup surface, the pickling solution A includes the nitric acid solution of 5% concentration, 5%
The hydrofluoric acid solution of concentration, the Fluorinse of 100g/L concentration, water mix, wherein the nitric acid solution, hydrofluoric acid are molten
Liquid, Fluorinse, water mixed proportion be 5:5:10:80, pickling solution A is poured into descaling bath, fixed dress is then passed through
It sets and titanium cup is totally submerged in pickling solution A, clean 85s；
(d) titanium cup rim of a cup is taken out from pickling solution A by fixed device downward, cleans 30s with clear water；
(e) pickling B solution is configured, the pickling B solution includes that the peroxide solutions of 150g/L, the hydrofluoric acid of 15% concentration are molten
Liquid, the Fluorinse of 150g/L concentration, water mix, wherein the peroxide solutions, hydrofluoric acid solution, sodium fluoride are molten
Liquid, water mixed proportion be 15:15:15:55, pickling B solution is poured into descaling bath, it is then by fixed device that titanium cup is complete
It is immersed in pickling B solution entirely, cleans 120s；
(f) titanium cup rim of a cup is taken out from pickling B solution by fixed device downward, is cleaned 2 times with clear water, cleans 30s every time；
(g) anodizing tank is taken, titanium cup is hung on to the anode of anodizing tank, the titanium for overpickling of learning from else's experience by fixed device
Piece and the cathode for being set as anodizing tank, the titanium sheet area be 4 times or more of titanium cup surface area, the anode, cathode
Interpolar is away from for 10cm；
(h) electrolyte being placed in anodizing tank is configured, the electrolyte includes the acetic acid solution of 150g/L, 150g/L
Phosphate solution, the Fluorinse of 150g/L, the stabilizer of 15g/L, water mix, wherein the acetic acid solution, phosphoric acid
Salting liquid, Fluorinse, stabilizer, water mixed proportion be 15:15:15:1.5:53.5, the anode, cathode soak completely
Not in the electrolyte；
(i) jointed anode, cathode and the DC voltage for applying 1 ~ 150V form unidirectional current circuit, make titanium cup surface and aquatic products
Raw oxidation reaction, oxidation time 2min, to form colored oxide film on titanium cup surface；
(j) it takes out titanium cup to be cleaned, takes out and dry up after titanium cup is impregnated 5min in clear water, it will be on the titanium glass holder after drying
Protective bag.
Preferably, carrying out the method that surface is handled to titanium cup in the step (a) is sandblasting or polishing or crystallization.
Preferably, in the step (c), (e), in titanium cup cleaning process, by fixed device with the speed of 5cm/s
Titanium cup is constantly moved horizontally repeatedly, and the descaling bath temperature maintains 15 DEG C.
Preferably, the step (c), (d), (e), in (f) treatment process, keep air draft state, and by the gas of discharge
Body carries out water curtain processing, when the waste liquid pH value that water curtain processing generates is down to 3, clear water of the replacement for water curtain processing.
Preferably, in the step (g), the quantity of the titanium sheet be 5 and be located at the front of titanium cup, rear,
Left side, right side, lower section, the titanium cup are located at the center of the anodizing tank.
Preferably, in the step (i), apply DC voltage the following steps are included:
(1) target voltage and interference voltage are set, the interference voltage is the 110% of target voltage, such as target voltage is arranged
For 50V, 55V is set by interference voltage；
(2) power supply pressurizes, and constant current is formed in anodizing tank, while the voltage in anodizing tank gradually rises to mistake
It is full of voltage；
(3) target voltage being retreated to by interference voltage in 0.5s, when reaching target voltage, electric current is gradually reduced to current threshold,
And stop power supply pressurization when electric current is down to current threshold.
Preferably, titanium cup is dried up using the compressed air of 0.3Mpa in the step (j).
Preferably, the peroxide is hydrogen peroxide in the step (e).
Preferably, the phosphate is potassium hydrogen phosphate or dibastic sodium phosphate or potassium dihydrogen phosphate or phosphorus in the step (h)
Acid dihydride sodium.
Preferably, the material of the fixed device is titanium and fixes the upper end of titanium cup, lower end in the step (b).
Embodiment 8
A kind of titanium cup process for surface oxidation, comprising the following steps:
(a) a titanium cup is taken, titanium cup is surface-treated, and is deoiled, after cleaning treatment to the titanium cup after surface treatment；
(b) titanium cup is fixed using fixed device, titanium cup is made to keep stablizing；
(c) configure pickling solution A, to titanium cup surface carry out pickling, the pickling solution A include 10% concentration nitric acid solution,
The hydrofluoric acid solution of 10% concentration, the Fluorinse of 125g/L concentration, water mix, wherein the nitric acid solution, hydrofluoric acid
Solution, Fluorinse, water mixed proportion be 10:10:12.5:67.5, pickling solution A is poured into descaling bath, is then led to
It crosses fixed device titanium cup is totally submerged in pickling solution A, cleans 85s；
(d) titanium cup rim of a cup is taken out from pickling solution A by fixed device downward, cleans 25s with clear water；
(e) pickling B solution is configured, the pickling B solution includes that the peroxide solutions of 150g/L, the hydrofluoric acid of 15% concentration are molten
Liquid, the Fluorinse of 150g/L concentration, water mix, wherein the peroxide solutions, hydrofluoric acid solution, sodium fluoride are molten
Liquid, water mixed proportion be 15:15:15:55, pickling B solution is poured into descaling bath, it is then by fixed device that titanium cup is complete
It is immersed in pickling B solution entirely, cleans 120s；
(f) titanium cup rim of a cup is taken out from pickling B solution by fixed device downward, is cleaned 2 times with clear water, cleans 25s every time；
(g) anodizing tank is taken, titanium cup is hung on to the anode of anodizing tank, the titanium for overpickling of learning from else's experience by fixed device
Piece and the cathode for being set as anodizing tank, the titanium sheet area be 4 times or more of titanium cup surface area, the anode, cathode
Interpolar is away from for 22.5cm；
(h) electrolyte being placed in anodizing tank is configured, the electrolyte includes the acetic acid solution of 150g/L, 150g/L
Phosphate solution, the Fluorinse of 150g/L, the stabilizer of 15g/L, water mix, wherein the acetic acid solution, phosphoric acid
Salting liquid, Fluorinse, stabilizer, water mixed proportion be 15:15:15:1.5:53.5, the anode, cathode soak completely
Not in the electrolyte；
(i) jointed anode, cathode and the DC voltage for applying 1 ~ 150V form unidirectional current circuit, make titanium cup surface and aquatic products
Raw oxidation reaction, oxidation time 5min, to form colored oxide film on titanium cup surface；
(j) it takes out titanium cup to be cleaned, takes out and dry up after titanium cup is impregnated 12.5min in clear water, by the titanium cup after drying
Put on protective bag.
Preferably, carrying out the method that surface is handled to titanium cup in the step (a) is sandblasting or polishing or crystallization.
Preferably, in the step (c), (e), in titanium cup cleaning process, by fixed device with 12.5cm/s's
Speed constantly moves horizontally titanium cup repeatedly, and the descaling bath temperature maintains 20 DEG C.
Preferably, the step (c), (d), (e), in (f) treatment process, keep air draft state, and by the gas of discharge
Body carries out water curtain processing, when the waste liquid pH value that water curtain processing generates is down to 3, clear water of the replacement for water curtain processing.
Preferably, in the step (g), the quantity of the titanium sheet be 5 and be located at the front of titanium cup, rear,
Left side, right side, lower section, the titanium cup are located at the center of the anodizing tank.
Preferably, in the step (i), apply DC voltage the following steps are included:
(1) target voltage and interference voltage are set, the interference voltage is the 110% of target voltage, such as target voltage is arranged
For 40V, 44V is set by interference voltage；
(2) power supply pressurizes, and constant current is formed in anodizing tank, while the voltage in anodizing tank gradually rises to mistake
It is full of voltage；
(3) target voltage being retreated to by interference voltage in 0.5s, when reaching target voltage, electric current is gradually reduced to current threshold,
And stop power supply pressurization when electric current is down to current threshold.
Preferably, titanium cup is dried up using the compressed air of 0.3Mpa in the step (j).
Preferably, the peroxide is hydrogen peroxide in the step (e).
Preferably, the phosphate is potassium hydrogen phosphate or dibastic sodium phosphate or potassium dihydrogen phosphate or phosphorus in the step (h)
Acid dihydride sodium.
Preferably, the material of the fixed device is titanium and fixes the upper end of titanium cup, lower end in the step (b).
Embodiment 9
A kind of titanium cup process for surface oxidation, comprising the following steps:
(a) a titanium cup is taken, titanium cup is surface-treated, and is deoiled, after cleaning treatment to the titanium cup after surface treatment；
(b) titanium cup is fixed using fixed device, titanium cup is made to keep stablizing；
(c) configure pickling solution A, to titanium cup surface carry out pickling, the pickling solution A include 15% concentration nitric acid solution,
The hydrofluoric acid solution of 15% concentration, the Fluorinse of 150g/L concentration, water mix, wherein the nitric acid solution, hydrofluoric acid
Solution, Fluorinse, water mixed proportion be 15:15:15:55, pickling solution A is poured into descaling bath, then by solid
Determine device titanium cup is totally submerged in pickling solution A, cleans 85s；
(d) titanium cup rim of a cup is taken out from pickling solution A by fixed device downward, cleans 20s with clear water；
(e) pickling B solution is configured, the pickling B solution includes that the peroxide solutions of 150g/L, the hydrofluoric acid of 15% concentration are molten
Liquid, the Fluorinse of 150g/L concentration, water mix, wherein the peroxide solutions, hydrofluoric acid solution, sodium fluoride are molten
Liquid, water mixed proportion be 15:15:15:55, pickling B solution is poured into descaling bath, it is then by fixed device that titanium cup is complete
It is immersed in pickling B solution entirely, cleans 120s；
(f) titanium cup rim of a cup is taken out from pickling B solution by fixed device downward, is cleaned 3 times with clear water, cleans 20s every time；
(g) anodizing tank is taken, titanium cup is hung on to the anode of anodizing tank, the titanium for overpickling of learning from else's experience by fixed device
Piece and the cathode for being set as anodizing tank, the titanium sheet area be 4 times or more of titanium cup surface area, the anode, cathode
Interpolar is away from for 35cm；
(h) electrolyte being placed in anodizing tank is configured, the electrolyte includes the acetic acid solution of 150g/L, 150g/L
Phosphate solution, the Fluorinse of 150g/L, the stabilizer of 15g/L, water mix, wherein the acetic acid solution, phosphoric acid
Salting liquid, Fluorinse, stabilizer, water mixed proportion be 15:15:15:1.5:53.5, the anode, cathode soak completely
Not in the electrolyte；
(i) jointed anode, cathode and the DC voltage for applying 1 ~ 150V form unidirectional current circuit, make titanium cup surface and aquatic products
Raw oxidation reaction, oxidation time 8min, to form colored oxide film on titanium cup surface；
(j) it takes out titanium cup to be cleaned, takes out and dry up after titanium cup is impregnated 20min in clear water, by the titanium glass holder after drying
Upper protective bag.
Preferably, carrying out the method that surface is handled to titanium cup in the step (a) is sandblasting or polishing or crystallization.
Preferably, in the step (c), (e), in titanium cup cleaning process, by fixed device with the speed of 20cm/s
Degree constantly moves horizontally titanium cup repeatedly, and the descaling bath temperature maintains 25 DEG C.
Preferably, the step (c), (d), (e), in (f) treatment process, keep air draft state, and by the gas of discharge
Body carries out water curtain processing, when the waste liquid pH value that water curtain processing generates is down to 3, clear water of the replacement for water curtain processing.
Preferably, in the step (g), the quantity of the titanium sheet be 5 and be located at the front of titanium cup, rear,
Left side, right side, lower section, the titanium cup are located at the center of the anodizing tank.
Preferably, in the step (i), apply DC voltage the following steps are included:
(1) target voltage and interference voltage are set, the interference voltage is the 110% of target voltage, such as target voltage is arranged
For 30V, 33V is set by interference voltage；
(2) power supply pressurizes, and constant current is formed in anodizing tank, while the voltage in anodizing tank gradually rises to mistake
It is full of voltage；
(3) target voltage being retreated to by interference voltage in 0.5s, when reaching target voltage, electric current is gradually reduced to current threshold,
And stop power supply pressurization when electric current is down to current threshold.
Preferably, titanium cup is dried up using the compressed air of 0.3Mpa in the step (j).
Preferably, the peroxide is hydrogen peroxide in the step (e).
Preferably, the phosphate is potassium hydrogen phosphate or dibastic sodium phosphate or potassium dihydrogen phosphate or phosphorus in the step (h)
Acid dihydride sodium.
Preferably, the material of the fixed device is titanium and fixes the upper end of titanium cup, lower end in the step (b).
In short, the foregoing is merely presently preferred embodiments of the present invention, made by all ranges according to the present patent application patent
Deng variation and modification, it is all covered by the present invention.
Claims (10)
1. a kind of titanium cup process for surface oxidation, it is characterised in that: the following steps are included:
(a) a titanium cup is taken, titanium cup is surface-treated, and is deoiled, after cleaning treatment to the titanium cup after surface treatment；
(b) titanium cup is fixed using fixed device, titanium cup is made to keep stablizing；
(c) pickling solution A is configured, pickling is carried out to titanium cup surface, the pickling solution A includes that the nitric acid of 5% ~ 15% concentration is molten
Liquid, the hydrofluoric acid solution of 5% ~ 15% concentration, the Fluorinse of 100g/L ~ 150g/L concentration, water mix, wherein the nitre
Acid solution, hydrofluoric acid solution, Fluorinse, water mixed proportion be 5:5:10:80-15:15:15:55, by pickling solution A
It pours into descaling bath, then titanium cup is totally submerged in pickling solution A by fixed device, cleans 60-85s；
(d) titanium cup rim of a cup is taken out from pickling solution A by fixed device downward, cleans 20-30s with clear water；
(e) pickling B solution is configured, the pickling B solution includes the peroxide solutions of 100g/L-150g/L, 5% ~ 15% concentration
Hydrofluoric acid solution, 100g/L ~ 150g/L concentration Fluorinse, water mix, wherein the peroxide solutions, hydrogen
Fluorspar acid solution, Fluorinse, water mixed proportion be 5:5:10:80-15:15:15:55, pickling B solution is poured into descaling bath
In, then titanium cup is totally submerged in pickling B solution by fixed device, cleans 60-120s；
(f) titanium cup rim of a cup is taken out from pickling B solution by fixed device downward, is cleaned 2-3 times with clear water, cleaned every time
20-30s；
(g) anodizing tank is taken, titanium cup is hung on to the anode of anodizing tank, the titanium for overpickling of learning from else's experience by fixed device
Piece and the cathode for being set as anodizing tank, the titanium sheet area be 4 times or more of titanium cup surface area, the anode, cathode
Interpolar is away from for 10-35cm；
(h) configure the electrolyte that is placed in anodizing tank, the electrolyte include 80g/L ~ 150g/L acetic acid solution,
The phosphate solution of 80g/L ~ 150g/L, the Fluorinse of 100g/L ~ 150g/L, the stabilizer of 5g/L ~ 15g/L, water mixing
It forms, wherein the mixed proportion of the acetic acid solution, phosphate solution, Fluorinse, stabilizer, water is 8:8:10:0.5:
73.5-15:15:15:1.5:53.5 the anode, cathode are totally submerged in the electrolyte；
(i) jointed anode, cathode and the DC voltage for applying 1 ~ 150V form unidirectional current circuit, make titanium cup surface and aquatic products
Raw oxidation reaction, oxidation time 2-8min, to form colored oxide film on titanium cup surface；
(j) it takes out titanium cup to be cleaned, takes out and dry up after titanium cup is impregnated 5-20min in clear water, by the titanium cup after drying
Put on protective bag.
2. a kind of titanium cup process for surface oxidation according to claim 1, it is characterised in that: to titanium cup in the step (a)
Carrying out the method that surface is handled is sandblasting or polishing or crystallization.
3. a kind of titanium cup process for surface oxidation according to claim 1, it is characterised in that: in the step (c), (e),
In titanium cup cleaning process, titanium cup, and the pickling are constantly moved horizontally with the speed of 5-20cm/s by fixed device repeatedly
Bath temperature degree maintains 15-25 DEG C.
4. a kind of titanium cup process for surface oxidation according to claim 1, it is characterised in that: the step (c), (d), (e),
(f) in treatment process, air draft state is kept, and the gas of discharge is subjected to water curtain processing, as the waste liquid PH that water curtain processing generates
When value is down to 3, clear water of the replacement for water curtain processing.
5. a kind of titanium cup process for surface oxidation according to claim 1, it is characterised in that: in the step (g), the titanium
The quantity of piece is 5 and is located at front, rear, left side, right side, the lower section of titanium cup, and the titanium cup is located at the anodic oxygen
Change the center of slot.
6. a kind of titanium cup process for surface oxidation according to claim 1, it is characterised in that: in the step (i), apply straight
Galvanic electricity pressure the following steps are included:
(1) target voltage and interference voltage are set, the interference voltage is the 110% of target voltage；
(2) power supply pressurizes, and constant current is formed in anodizing tank, while the voltage in anodizing tank gradually rises to mistake
It is full of voltage；
(3) target voltage being retreated to by interference voltage in 0.5s, when reaching target voltage, electric current is gradually reduced to current threshold,
And stop power supply pressurization when electric current is down to current threshold.
7. a kind of titanium cup process for surface oxidation according to claim 1, it is characterised in that: in the step (j), use
The compressed air of 0.2 ~ 0.3Mpa dries up titanium cup.
8. a kind of titanium cup process for surface oxidation according to claim 1, it is characterised in that: in the step (e), the mistake
Oxide is hydrogen peroxide.
9. a kind of titanium cup process for surface oxidation according to claim 1, it is characterised in that: in the step (h), the phosphorus
Hydrochlorate is potassium hydrogen phosphate or dibastic sodium phosphate or potassium dihydrogen phosphate or sodium dihydrogen phosphate.
10. a kind of titanium cup process for surface oxidation according to claim 1, it is characterised in that: described in the step (b)
The material of fixed device is titanium and fixes the upper end of titanium cup, lower end.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN206761285U (en) * | 2017-01-20 | 2017-12-19 | 永安市钛产业研究院 | Titanium health double-layer vacuum cup |
| CN108103553A (en) * | 2017-12-28 | 2018-06-01 | 大博医疗科技股份有限公司 | A kind of colorful anode oxidation membrane preparation method of titanium surface non-impurity-doped low defect |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN206761285U (en) * | 2017-01-20 | 2017-12-19 | 永安市钛产业研究院 | Titanium health double-layer vacuum cup |
| CN108103553A (en) * | 2017-12-28 | 2018-06-01 | 大博医疗科技股份有限公司 | A kind of colorful anode oxidation membrane preparation method of titanium surface non-impurity-doped low defect |
Non-Patent Citations (1)
| Title |
|---|
| 张永德: "钛的着色工艺原理及其应用", 《表面技术》 * |
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