CN106906472A - A kind of antimony containing platinum middle layer mixes the preparation method of stannic oxide electrode - Google Patents
A kind of antimony containing platinum middle layer mixes the preparation method of stannic oxide electrode Download PDFInfo
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- 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
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
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- 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
- C23F13/00—Inhibiting corrosion of metals by anodic or cathodic protection
- C23F13/02—Inhibiting corrosion of metals by anodic or cathodic protection cathodic; Selection of conditions, parameters or procedures for cathodic protection, e.g. of electrical conditions
- C23F13/06—Constructional parts, or assemblies of cathodic-protection apparatus
- C23F13/08—Electrodes specially adapted for inhibiting corrosion by cathodic protection; Manufacture thereof; Conducting electric current thereto
- C23F13/12—Electrodes characterised by the material
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- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
- C25B11/093—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds at least one noble metal or noble metal oxide and at least one non-noble metal oxide
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- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/10—Electrodes, e.g. composition, counter electrode
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
- C02F2001/46142—Catalytic coating
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Abstract
The invention discloses the preparation method that a kind of antimony containing platinum middle layer mixes stannic oxide electrode, it is related to the preparation field of coated titanium electrode.It is characteristic of the invention that first plating one layer of platinum middle layer on the Titanium base for having pre-processed, tin antimony active layer is coated with.The pretreatment of Titanium base includes polishing, alkali cleaning, three steps of pickling, and one layer of platinum middle layer is plated on the Titanium base handled well by methods such as magnetron sputterings, and tin antimony active layer is coated on the Titanium base of platinum plating using modes such as pyrolysismethods then.The addition of platinum middle layer greatly reduces the passivation speed of titanium substrate, the characteristics of the electrode prepared according to the described method of this invention has oxygen evolution potential and high stability.
Description
Technical field patent of the present invention belongs to the preparation field of coated titanium electrode, is related to one kind that one layer is plated in titanium substrate
The method that antimony mixes stannic oxide electrode is prepared after platinum middle layer.
Background technology coated titanium electrode, also referred to as dimensional stable anode, are widely used in chlorine industry, sewage disposal, electricity
The numerous areas such as plating, cathodic protection.Coated titanium electrode is that, with titanium as matrix, painting is covered with the metal oxide with catalysis activity and applies
Layer constitutes electrode, and conventional active layer material has ruthenium-oxide, yttrium oxide, lead oxide, tin oxide etc..Wherein tin oxide electrode is with it
High catalytic activity, non-secondary pollution, it is cheap for manufacturing cost the advantages of receive more and more attention.But tin oxide electrode has one
Individual fatal shortcoming --- working life is short, and this shortcoming seriously limits its large-scale application.It has been proved that causing oxidation
The main cause of tin electrode failure is during catalysis oxidation, one layer of TiO to be produced between active layer and matrix2Passivation
Film, passivating film hinders the carrying out of electro transfer, ultimately results in the inactivation of electrode.So adding one between matrix and active layer
The intermediate layer of oxygen atom and Titanium base contact can be prevented, the working life of tin oxide electrode can be greatly improved.Platinum is a kind ofization
The extremely strong metal of stability is learned, insoluble in strong acid and strong base, is not easy to be oxidized, so electrode material is used frequently as, but due to
Its expensive price, can only also use in the development of high cost.
The content of the invention is it is an object of the invention to provide the preparation side that a kind of antimony containing platinum middle layer mixes stannic oxide electrode
Method, by one layer of Pt film of Titanium base plated surface, then prepares tin antimony active layer with coating pyrolysismethod, and the electrode for being obtained is not
Only there is great lifting in working life, also maintain the oxygen evolution potential and activity of traditional tin antimony electrode.
Preparation method of the invention is comprised the following steps：
(1) pretreatment of titanium plate：Pretreatment include titanium plate is polished, alkali cleaning, three steps of pickling.
(2) preparation of platinum middle layer：The thick platinum coating of one layer of 50nm is deposited in titanium substrate with magnetron sputtering method.
(3) preparation of active layer：It is 100 according to tin antimony atoms ratio:6 proportional arrangement precursor liquid, the forerunner that will have been configured
Liquid is uniformly coated in the titanium plate that deposited Pt films, and high-temperature oxydation obtains required electrode after being repeated several times.
Ti/Pt/Sb-SnO obtained by the present invention2Electrode has oxygen deposition potential (2.0V vs.Ag/AgCl) higher,
The reinforcing life of the electrode is Ti/Sb-SnO225 times of electrode, are 5 times of Ti/Pt electrodes.Ti/Sb-SnO mentioned herein2
With Ti/Pt electrodes it is obtained according to the operating procedure of the corresponding painting described in following implementation method.
Specific embodiment
(1) Titanium base pretreatment：1st, titanium-based piece is polished repeatedly with 80 mesh and 400 mesh sand paper successively, until titanium plate is presented
Go out metallic luster, it is therefore an objective to remove the impurity and titanium oxide of surface attachment.
2nd, by the titanium-based piece deionized water polished ultrasound 10 minutes after be placed in the NaOH solution of 40wt%, water-bath 95
DEG C heating 1 hour.Its object is to remove the organic matter on Titanium base.
3rd, it is after alkali cleaning that titanium sheet taking-up is ultrasonic 10 minutes with deionized water, then the HCL solution that titanium sheet is placed in 50vol%
In, 90 DEG C of water-bath is kept for 1 hour.The purpose of pickling is to go out rough pitted skin in titanium-based piece surface etch, to strengthen coating
With the adhesion of matrix.It is cleaned by ultrasonic with deionized water after pickling, then is dried up with nitrogen stream.
(2) preparation in intermediate layer：By magnetron sputtering method, prepared on the substrate handled well in the middle of the thick platinum of 50nm
Layer.Base vacuum is 4.5 × 10 during deposition-4Pa, is passed through the flow of argon gas for 20sccm, and operating air pressure is controlled in 0.5Pa.Deposition
When substrate temperature be 25 DEG C.
(3) preparation of active layer：1st, 0.4373g Sb are taken2O3With 11.2825g SnCl2·2H2O is dissolved in 50mL ethanol,
A few drop saturation concentrated hydrochloric acids are instilled while stirring, until it is transparent to see that solution becomes colorless, volumetric flask is transferred the solution into, plus
Enter ethanol and be settled to 100mL.The precursor liquid sealing preserve that will be prepared 2~3 days.
2nd, appropriate precursor liquid is taken with plastic suction pipe, several drops in drop on the substrate for plated platinum middle layer treat that masking liquid uniformly covers
After covering whole titanium plate, titanium plate is placed in 5min is dried in 100 DEG C of drying box, be placed in 550 DEG C of Muffle furnace annealing after taking-up again
5min.Above-mentioned coating procedure is repeated 6 times, and last time annealing keeps 1h.Natural cooling after taking-up, that is, obtain required electrode.
Claims (7)
1. a kind of titanium-based antimony containing platinum middle layer mixes the preparation method of stannic oxide electrode, it is characterised in that in the titanium handled well
One layer of Pt film is first plated on matrix, tin antimony active layer is then coated with, required electrode is obtained final product after annealing.
2. antimony containing platinum middle layer according to claim 1 mixes stannic oxide electrode, it is characterised in that the thickness of platinum middle layer
1~106In the range of nm, the preparation hair method of platinum middle layer can be magnetron sputtering, plating, evaporation coating, chemical vapor deposition
Etc., but it is not limited only to above method.
3. electrode preparation method according to claim 1, the size shape of substrate is not fixed, it is possible to use titanium plate conduct
Substrate, it is also possible to use titanium net, or titanium rod etc., the size of electrode can determine according to actually used situation.
4. the antimony containing platinum middle layer according to claim 1,3 mixes the preparation method of stannic oxide electrode, it is characterised in that bag
Include three steps：The pretreatment of Titanium base, the preparation of platinum middle layer and the preparation of tin antimony active layer；The wherein pretreatment of Titanium base
It is divided into polishing, alkali cleaning, pickling again, grinding process can also be changed into blasting treatment.
5. Titanium base preprocess method according to claim 4, it is characterised in that successively beaten repeatedly with 40~800 mesh sand paper
Mill, until titanium plate shows metallic luster, and blasting treatment is then that titanium plate surface is got into uniform densely covered pockmark；Alkali cleaning refers to
The Titanium base polished is placed in the NaOH solution of 20~40wt% into 80~95 DEG C to heat 1~3 hour, or is placed on third
It is cleaned by ultrasonic 10~30min in ketone solution；Pickling refer to alkali cleaning after Titanium base be placed on the oxalic acid or salt of 10~40wt%
In acid solution, 80~95 DEG C are heated 1~3 hour, until its surface is in numb grey.
6. the preparation method of the tin antimony active layer according to claim 1,4, it is characterised in that antimony atoms are relative in active layer
It is 1~15% in the mol ratio of tin atom, the thickness of tin antimony active layer is 1~106Nm, the preparation method of tin antimony active layer is not yet
Drop-coating is confined to, brushing method, dip-coating method, spin-coating method etc. is can also be；Or electro-deposition, magnetron sputtering, evaporation etc.
Method.
7. the preparation method of the tin antimony active layer according to claim 1,6, during coating pyrolysis, annealing temperature can be with
Selected between 450~600 DEG C, annealing atmosphere can be under atmospheric environment, or in oxygen atmosphere.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110034273A (en) * | 2018-01-12 | 2019-07-19 | 中南大学 | The film lithium cell cathode and its preparation of a kind of Sn base sulfide and/or nitride modification tin oxide and application |
| CN110129821A (en) * | 2019-05-10 | 2019-08-16 | 上海氯碱化工股份有限公司 | Tin, Sb doped titanium-based ruthenic oxide coated electrode preparation method |
| CN110584308A (en) * | 2019-08-28 | 2019-12-20 | 安徽名扬刷业有限公司 | Spring brush |
| CN110655150A (en) * | 2018-06-28 | 2020-01-07 | 杭州睿清环保科技有限公司 | Novel titanium-based tin oxide anode and preparation method thereof |
| CN114272920A (en) * | 2021-11-22 | 2022-04-05 | 广东省科学院资源利用与稀土开发研究所 | Composite oxide coating electrode for organic pollutant degradation and preparation method thereof |
| EP4012073A4 (en) * | 2019-08-07 | 2022-11-23 | Seoul National University R & DB Foundation | Electrode structures for electrochemical reaction, and electrochemical reaction systems including same |
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| CN1896320A (en) * | 2006-06-19 | 2007-01-17 | 哈尔滨工业大学 | Rare-earth doped titanium-base SnO2 electrolytic electrode and its preparation |
| CN102304724A (en) * | 2011-09-21 | 2012-01-04 | 山东大学 | Preparation method of rare earth Pr (praseodymium)-Dy (dysprosium) doped nanometer titanium-based tin dioxide-antimony double coating electrode |
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| CN1896320A (en) * | 2006-06-19 | 2007-01-17 | 哈尔滨工业大学 | Rare-earth doped titanium-base SnO2 electrolytic electrode and its preparation |
| CN102304724A (en) * | 2011-09-21 | 2012-01-04 | 山东大学 | Preparation method of rare earth Pr (praseodymium)-Dy (dysprosium) doped nanometer titanium-based tin dioxide-antimony double coating electrode |
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| D. SANTOS ET AL: "Preparation of Ti/Pt/SnO2-Sb2O4 electrodes for anodic oxidation of pharmaceutical drugs", 《JOURNAL OF APPLIED ELECTROCHEMISTRY》 * |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110034273A (en) * | 2018-01-12 | 2019-07-19 | 中南大学 | The film lithium cell cathode and its preparation of a kind of Sn base sulfide and/or nitride modification tin oxide and application |
| CN110655150A (en) * | 2018-06-28 | 2020-01-07 | 杭州睿清环保科技有限公司 | Novel titanium-based tin oxide anode and preparation method thereof |
| CN110655150B (en) * | 2018-06-28 | 2023-10-31 | 杭州睿清环保科技有限公司 | Titanium-based tin oxide anode electrode and preparation method thereof |
| CN110129821A (en) * | 2019-05-10 | 2019-08-16 | 上海氯碱化工股份有限公司 | Tin, Sb doped titanium-based ruthenic oxide coated electrode preparation method |
| EP4012073A4 (en) * | 2019-08-07 | 2022-11-23 | Seoul National University R & DB Foundation | Electrode structures for electrochemical reaction, and electrochemical reaction systems including same |
| CN110584308A (en) * | 2019-08-28 | 2019-12-20 | 安徽名扬刷业有限公司 | Spring brush |
| CN114272920A (en) * | 2021-11-22 | 2022-04-05 | 广东省科学院资源利用与稀土开发研究所 | Composite oxide coating electrode for organic pollutant degradation and preparation method thereof |
| WO2023088398A1 (en) * | 2021-11-22 | 2023-05-25 | 广东省科学院资源利用与稀土开发研究所 | Composite oxide coating electrode for organic pollutant degradation, and preparation method therefor |
| CN114272920B (en) * | 2021-11-22 | 2023-10-03 | 广东省科学院资源利用与稀土开发研究所 | Composite oxide coating electrode for degrading organic pollutants and preparation method thereof |
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Application publication date: 20170630 |