CN107893232A - A kind of surface etching method before titanium plate anodic coating - Google Patents
A kind of surface etching method before titanium plate anodic coating Download PDFInfo
- Publication number
- CN107893232A CN107893232A CN201711393367.4A CN201711393367A CN107893232A CN 107893232 A CN107893232 A CN 107893232A CN 201711393367 A CN201711393367 A CN 201711393367A CN 107893232 A CN107893232 A CN 107893232A
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- CN
- China
- Prior art keywords
- titanium plate
- hcl
- titanium
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- 20min
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 239000010936 titanium Substances 0.000 claims abstract description 64
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 64
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 63
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002253 acid Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000005530 etching Methods 0.000 claims abstract description 15
- 238000009499 grossing Methods 0.000 claims abstract description 12
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 12
- 238000005488 sandblasting Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 230000003014 reinforcing effect Effects 0.000 abstract description 9
- 238000007373 indentation Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 20
- 239000000463 material Substances 0.000 description 11
- 239000007788 liquid Substances 0.000 description 9
- 239000000758 substrate Substances 0.000 description 6
- 230000000873 masking effect Effects 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- 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
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/26—Acidic compositions for etching refractory metals
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- ing And Chemical Polishing (AREA)
Abstract
A kind of surface etching method before titanium plate anodic coating, first, the fine and close and thick and heavy oxide scale layer of 8min~20min removals titanium plate in mixed acid will be immersed under the titanium plate normal temperature after sandblasting, high warm smoothing；Then, the titanium plate after scale removal layer is placed in the oxalic acid solution that mass percent concentration is 5%~10% at 80 DEG C~100 DEG C and etches 20min~30min, then rinsed well with water.The present invention improves production efficiency, saves the energy, and the titanium plate anode surface indentation after being handled using the inventive method is careful, uniform, increases face coat load capacity, and its reinforcing life improves 30% than the titanium plate anode handled using commonsense method.
Description
Technical field
The present invention relates to a kind of surface treatment method of metallic titanium plate anode, and in particular to before a kind of titanium plate anodic coating
Surface etching method.
Background technology
For titanium-based noble metal oxide coating electrode due to high with electro catalytic activity, service life length and dimensionally stable etc. are excellent
Point, has a wide range of applications in electrochemical industry.Precious metal oxide coating is coated on base material using coating-thermal decomposition method more
Surface.Because the plasticity and toughness of industrially pure titanium are good, corrosion-resistant and the features such as be easy to shaping, the base material for making electrode is often used.
The adhesion of coating and base material is to influence a critically important factor of anode performance, therefore is preparing oxide
It is preceding, it is necessary to carry out strict pretreatment to titanium-based material.The pretreatment of titanium-based material generally includes oil removing, sandblasting, heat smoothing and acid
The process such as wash.Sandblasting can cause the deformation of base material especially plate-like substrate, need to carry out high warm smoothing process.In high warm smoothing
Process, titanium substrate surface can generate one layer of densification and thick and heavy oxide skin, and existing acid etching process generally uses oxalic acid treatment oxygen
Change skin, phenomena such as efficiency is slow, and processing is not thorough be present.
The content of the invention
Fine and close and thick and heavy oxide skin can be quickly removed it is an object of the invention to provide a kind of, improves production efficiency,
Save the surface etching method before the titanium plate anodic coating of the energy.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
1) 8min~20min in mixed acid first, will be immersed under the titanium plate normal temperature after sandblasting, high warm smoothing to remove
The fine and close and thick and heavy oxide scale layer of titanium plate；
HCl that HF that the mixed acid solution is 1~20% by percent by volume, percent by volume are 1~10% and
Percent by volume is 70%~98%H2O is formed, and wherein HF uses mass concentration, and for 30%~55%HF solution, HCl uses matter
Measure the HCl solution that concentration is 36%~38%；
2) then, 80 DEG C~100 DEG C by the titanium plate after scale removal layer be placed in mass percent concentration for 5%~
20min~30min is etched in 10% oxalic acid solution, is then rinsed well with water.
The present invention compared with prior art, greatly shortens the time of acid etching oxide skin, improves treatment effeciency, using this
Titanium plate anode surface after inventive method processing has uniform grey pitted skin, and its reinforcing life, which is significantly higher than, uses commonsense method
The titanium plate anode reinforcing life of processing.
Brief description of the drawings
Fig. 1 is that titanium-based material in temperature is 80 DEG C~100 DEG C, and mass percent concentration is in 5%~10% oxalic acid solution
The SEM figures (1000 times of amplification) of etching 2 hours.
Fig. 2 soaks 10 minutes for titanium-based material in the present invention in hydrofluoric acid and mixed in hydrochloric acid acid, is then 100 in temperature
DEG C, mass percent concentration is schemed (1000 times of amplification) to etch the SEM of 30 minutes in 5% oxalic acid solution.
Embodiment
Below in conjunction with the accompanying drawings and embodiment is described in further detail to the present invention.
Temperature will be put at 80~100 DEG C through sandblasting, the high titanium plate for warming smoothing, mass percent concentration is 5%~
Etched 2 hours in 10% oxalic acid solution, be then placed in rinsed clean in water.Apply and brush in the titanium plate Jing Guo above-mentioned processing
Liquid, sintering make titanium plate anode 1.
Embodiment 1：
1) 10min in mixed acid first, will be immersed under the titanium plate normal temperature after sandblasting, high warm smoothing and remove titanium plate
Fine and close and thick and heavy oxide scale layer；
The HCl and volume basis that HF that the mixed acid solution is 10% by percent by volume, percent by volume are 5%
Than for 85%H2O is formed, and wherein HF uses mass concentration, and for 40%HF solution, HCl uses mass concentration molten for 37% HCl
Liquid；
2) titanium plate after scale removal layer then, is placed in the oxalic acid solution that mass percent concentration is 5% at 100 DEG C
Middle etching 30min, is then rinsed well with water.
It is different that the titanium-based material surface topography that two methods handle to obtain is can be seen that from Fig. 1 and Fig. 2, by grass in Fig. 1
The titanium substrate surface indentation of acid etching 2 hours is careful, and texture rule, etch depth is shallower, and such Titanium base specific surface area is small, can
Load capacity is smaller, and surface adhesion is poor；After titanium substrate surface in Fig. 2 soaks 10 minutes in mixed acid, then in mixed acid
Immersion 30 minutes, titanium substrate surface indentation is careful, uniform, so can effectively increase the specific surface area of titanium-based material, and increase surface applies
Layer load capacity, is beneficial to bottom masking liquid sticking thereon, extends the reinforcing life of titanium plate anode.
Brushing masking liquid in the titanium plate that will be handled by embodiment 1, sintering make titanium plate anode 2.In mass percent concentration
For 15% H2SO4, temperature is 40 ± 5 DEG C, current density 80000A/m2Under test condition, by titanium plate anode 1 and titanium plate sun
Pole 2 carries out reinforcing life test, and test result is：The reinforcing life of titanium plate anode 1 is 960 hours, and the reinforcing life of titanium plate anode 2 is
1392 hours, the reinforcing life of titanium plate anode 2 was than titanium plate anode 1 long 432 hour.
Embodiment 2：
1) 12min in mixed acid first, will be immersed under the titanium plate normal temperature after sandblasting, high warm smoothing and remove titanium plate
Fine and close and thick and heavy oxide scale layer；
The HCl and volume basis that HF that the mixed acid solution is 5% by percent by volume, percent by volume are 8%
Than for 87%H2O is formed, and wherein HF uses mass concentration, and for 50%HF solution, HCl uses mass concentration molten for 36.5% HCl
Liquid；
2) titanium plate after scale removal layer then, is placed in the oxalic acid solution that mass percent concentration is 8% at 80 DEG C
Middle etching 25min, is then rinsed well with water.
Embodiment 3：
1) 15min in mixed acid first, will be immersed under the titanium plate normal temperature after sandblasting, high warm smoothing and remove titanium plate
Fine and close and thick and heavy oxide scale layer；
The HCl and volume basis that HF that the mixed acid solution is 20% by percent by volume, percent by volume are 3%
Than for 77%H2O is formed, and wherein HF uses mass concentration, and for 30%HF solution, HCl uses mass concentration molten for 37.5% HCl
Liquid；
2) titanium plate after scale removal layer then, is placed in the oxalic acid solution that mass percent concentration is 10% at 90 DEG C
Middle etching 20min, is then rinsed well with water.
Embodiment 4：
1) 8min in mixed acid first, will be immersed under the titanium plate normal temperature after sandblasting, high warm smoothing and remove titanium plate
Fine and close and thick and heavy oxide scale layer；
The HCl and volume basis that HF that the mixed acid solution is 15% by percent by volume, percent by volume are 1%
Than for 84%H2O is formed, and wherein HF uses mass concentration, and for 35%HF solution, HCl uses mass concentration molten for 38% HCl
Liquid；
2) titanium plate after scale removal layer then, is placed in the oxalic acid solution that mass percent concentration is 9% at 95 DEG C
Middle etching 23min, is then rinsed well with water.
Embodiment 5：
1) 20min in mixed acid first, will be immersed under the titanium plate normal temperature after sandblasting, high warm smoothing and remove titanium plate
Fine and close and thick and heavy oxide scale layer；
The HCl and volume basis that HF that the mixed acid solution is 1% by percent by volume, percent by volume are 10%
Than for 89%H2O is formed, and wherein HF uses mass concentration, and for 55%HF solution, HCl uses mass concentration molten for 36% HCl
Liquid；
2) titanium plate after scale removal layer then, is placed in the oxalic acid solution that mass percent concentration is 7% at 85 DEG C
Middle etching 28min, is then rinsed well with water.
The titanium plate anode handled using the inventive method, its life-span using the titanium plate anode of conventional method processing than being improved
30%, and etching period is greatly shortened, production efficiency is improved, saves the energy.Titanium plate anode life is improved mainly
Because the titanium substrate surface indentation after being handled using the inventive method is careful, uniform, it so can effectively increase the ratio table of titanium-based material
Area, increase face coat load capacity, be beneficial to bottom masking liquid sticking thereon, improve anode electro catalytic activity, reduce
Voltage during anode electrolysis, electric energy is saved, improve reinforcing life.
Claims (1)
1. the surface etching method before a kind of titanium plate anodic coating, it is characterised in that comprise the following steps：
1) 8min~20min in mixed acid first, will be immersed under the titanium plate normal temperature after sandblasting, high warm smoothing and remove titanium plate
Fine and close and thick and heavy oxide scale layer；
The HCl and volume that HF that the mixed acid solution is 1~20% by percent by volume, percent by volume are 1~10%
Percentage is 70%~98%H2O is formed, and wherein HF uses mass concentration as 30%~55%HF solution, and HCl is dense using quality
Spend the HCl solution for 36%~38%；
2) it is 5%~10% that the titanium plate after scale removal layer then, is placed in into mass percent concentration at 80 DEG C~100 DEG C
20min~30min is etched in oxalic acid solution, is then rinsed well with water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711393367.4A CN107893232A (en) | 2017-12-20 | 2017-12-20 | A kind of surface etching method before titanium plate anodic coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711393367.4A CN107893232A (en) | 2017-12-20 | 2017-12-20 | A kind of surface etching method before titanium plate anodic coating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107893232A true CN107893232A (en) | 2018-04-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711393367.4A Pending CN107893232A (en) | 2017-12-20 | 2017-12-20 | A kind of surface etching method before titanium plate anodic coating |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111349961A (en) * | 2020-04-29 | 2020-06-30 | 宝鸡市昌立特种金属有限公司 | Method for cleaning waste titanium anode plate for foil forming machine and removing and recycling precious metal |
| WO2021017104A1 (en) * | 2019-07-29 | 2021-02-04 | 东北大学 | Substrate etching method for titanium-based dimension stabilization type anode |
| CN114836762A (en) * | 2022-04-12 | 2022-08-02 | 西安泰金工业电化学技术有限公司 | Acid treatment process capable of improving durability of titanium electrode |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021017104A1 (en) * | 2019-07-29 | 2021-02-04 | 东北大学 | Substrate etching method for titanium-based dimension stabilization type anode |
| CN111349961A (en) * | 2020-04-29 | 2020-06-30 | 宝鸡市昌立特种金属有限公司 | Method for cleaning waste titanium anode plate for foil forming machine and removing and recycling precious metal |
| CN111349961B (en) * | 2020-04-29 | 2021-05-07 | 宝鸡钛普锐斯钛阳极科技有限公司 | Method for cleaning waste titanium anode plate for foil forming machine and removing and recycling precious metal |
| CN114836762A (en) * | 2022-04-12 | 2022-08-02 | 西安泰金工业电化学技术有限公司 | Acid treatment process capable of improving durability of titanium electrode |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180410 |
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