CN1995464A - Nanocrystalline iridium series oxide coating electrode preparation method - Google Patents

Nanocrystalline iridium series oxide coating electrode preparation method Download PDF

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Publication number
CN1995464A
CN1995464A CN 200610144150 CN200610144150A CN1995464A CN 1995464 A CN1995464 A CN 1995464A CN 200610144150 CN200610144150 CN 200610144150 CN 200610144150 A CN200610144150 A CN 200610144150A CN 1995464 A CN1995464 A CN 1995464A
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iro
coating
electrode
titanium plate
nanocrystalline
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孟惠民
孙冬柏
俞宏英
樊自栓
王旭东
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Abstract

The invention discloses a making method of nanocrystalline iridium-series oxide coating electrode in the electrochemical appliance technical domain, which comprises the following steps: predisposing base; proceeding mechanic disposal; deoiling through alkaline and acid; allocating the coating liquid; coating. The solution of IrO2-Ta2O5-MO2 coating is composed of 30-95% H2IrCl6 solution and TaCl5 solution with the molar rate of Ir and Ta at 7: 6 and 5-70% third element M chloride with Sn, Mn, Ti, Nb, Pb and Si, wherein the even size of IrO2 grain is 8-15nm, which stabilizes the electrode.

Description

A kind of nanocrystalline iridium series oxide coating electrode preparation method
Technical field
The invention belongs to the electrochemical applications technical field, particularly a kind of nanocrystalline iridium series oxide coating electrode preparation method, the crystalline particle size by the refinement coating to nano level to improve the stability of electrode.
Background technology
Electrode is the core component in the electrochemical applications.3 stages have been experienced in the development of electrode materials substantially: in 1) the Graphite Electrodes stage, saline electrolysis is aqueous electrolysis industry the earliest, mainly uses natural carbon pole, natural electrode and platinum electrode in early days.This type of electrode is anti-corrosion and inexpensive, once by life-time service, but exist electrolytic efficiency relatively poor, produce in the electrode problem of unstable; 2) platinum metals and lead alloy electrode stage, improve a lot though this type of electrode is compared performance with graphite, shortcoming such as exist equally that platinum electrode costs an arm and a leg, lead electrode is yielding and conduction difference energy consumption is big requires further improvement; 3) ti-based coating anode, titanium is a valve metal, and the protection of stable oxide layer arranged, anodic current is difficult for passing through.The titanium electrode is compared with tungsten or tantalum, has the cost performance height, and machine-shaping is easy, the advantage that electrochemical stability is good.
In the ti-based coating anode, development is that ruthenium is a coated anode comparatively fully, because it is reflected at and has electro catalytic activity and stability preferably analysing chlorine, is popularized rapidly in chlorine industry.But kind electrode shows oxygen evolution potential height, short shortcoming of life-span under oxygen evolution reaction and sour environment.And be coated anode for iridium, but can satisfy various Working environments, and electrocatalysis to be better than ruthenium be coated anode, but stability also needs further raising.
Number of patent application 86106789 has proposed to have substrate material and the irdium based amorphous metal alloys coating on it, and its formula of irdium based amorphous metal alloys is IriDdEeFf, and D is a titanium, zirconium, niobium, tantalum, ruthenium, tungsten, molybdenum and composition thereof; E be carbon, boron, silicon, phosphorus, etc. material and mixture; F is rhodium, platinum, palladium and composition thereof.Produce electrode as halogen, the release rate of chlorine is roughly 100%.Patent US6210550 has also proposed iridium 55%～80%, bismuth 45～20%, and the composition of antimony and tin 2.5～7.5% is used for oxygen generator.Patent US6572758 also discloses on a kind of titanium or the graphite matrix, ruthenium, iridium or platinum, the electrode of antimony mixed oxide.Number of patent application 00119691.X discloses a kind of titanium base iridium dioxide electrode of novel band tin antimony middle layer, adds after the middle layer, and can bring up to 1255 hours work-ing life from 763 hours.(contain the anode of irdium based amorphous metal alloys and with it as halogen electrodes, application number 86106789 publication numbers 86106789, Anode with improved coating for oxygenevolution in electrolytes containing manganese, application number US19990395828 19990914 patent No. US6210550, Electrode coating and method ofuse and preparation thereof, application number US2001077844520010206 patent No. US6572758, the titanium base iridium dioxide electrode in band tin antimony middle layer, application number: 00119691.X publication number 1339618)
In a word, be that the research of coating oxidation thing mainly concentrates on 3 aspects at present to iridium: 1) add Co, Sn, Mn, Ta, elements such as Ru prepare binary or ternary oxide coating; 2) between matrix and coating, add platinum (Pt), iridium (Ir), palladium middle layer or IrO such as (Pd) 2, IrO 2-Ta 2O 5Mix the oxygen middle layer; 3) the ratio refining grain size between change preparation technology or each composition of change coating.The research of preceding 2 aspects is comparatively extensive, and less for the research of the 3rd aspect.The present invention just is based on the research of this direction, and adopting nano-crystallization to improve iridium is coated anode stability and electrocatalysis characteristic.
Summary of the invention
The object of the present invention is to provide a kind of nanocrystalline iridium series oxide coating electrode preparation method, the crystalline particle size by the refinement coating to nano level to improve the stability and the electrocatalysis characteristic of electrode.
Preparation nanocrystalline iridium series oxide coating electrode method of the present invention is traditional thermal decomposition method.With present sol-gel method, chemical complexometry etc. are compared, and it is easy, with low cost to have a preparation, particularly the life-span long advantage.
The IrO that the present invention is prepared 2-Ta 2O 5-MO 2The coated titanium base electrode, the 3rd constituent element M is Sn, Mn, Ti, Nb, Pb, Si.IrO 2-Ta 2O 5-MO 2The solution composition of coating is: H 2IrCl 6Solution and TaCl 5Ir in the solution: the Ta mol ratio is 7: 6, H 2IrCl 6And TaCl 5Account for total amount of substance 30～95%, the muriatic amount of substance of complex element M accounts for total amount of substance 5～70%.By selecting conditions such as suitable substrate pretreated coating composition ratio, sintering temperature, sintering time, the IrO that the stability of counter electrode and electrocatalysis characteristic play a major role in the electrode of preparation 2Average grain size is at 8～15nm.
The preparation of nanocrystalline iridium series oxide coating electrode comprises the steps:
1, substrate pretreated: the pre-treatment of matrix is bigger to the apparent pattern and the grain-size influence of coating.Comprise the following aspects: 1) mechanical pre-treatment: pure titanium plate cuts into the size of required usefulness through sandblast.
2) alkali cleaning oil removing is rinsed well with deionized water again, oven dry.
3) pickling: the pickling mode of employing be hydrochloric acid soln as pickle solution, put into the titanium plate after the heating, be dipped to pickle solution and be red-purple, take out the titanium plate and wash repeatedly only, at last dry for standby with deionized water.
2, coating liquid preparation: by Ir: the Ta mol ratio is 7: 6, H 2IrCl 6And TaCl 5The ratio that accounts for total amount of substance 30～95% takes by weighing desired number, mixes to be positioned in the glassware to dissolve, and then, puts into baking oven and dries 5～12 hours down in 70～100 ℃, bakes fine powder.Temperature and time is wanted suitably, and the too high and overlong time of temperature easily makes masking liquid lump again and produces insolubles, and temperature is too low then wants the longer time just can obtain powder.Then, get dehydrated alcohol and Virahol (volume ratio 3: 1～1: 3) with the gained powder dissolution.When adding the muriate of the 3rd constituent element M (M is Nb, Pb, Si, Sn, Mn, Ti), account for total amount of substance 5～70%, take by weighing desired number, be added in the former masking liquid according to the muriatic amount of substance of complex element M.
3, coating procedure: masking liquid is brushed on titanium plate surface with fur suede pen, put in the baking oven and dried 5～10 minutes down in 90 ℃～150 ℃, make organic solvent volatilization, again in retort furnace in 5～20 minutes time of 300 ℃～480 ℃ sintering temperatures, precious metal salt is decomposed generates oxide coating; Take out the back air cooling to room temperature, repeat the thickness of above step until needs.Place retort furnace sintering 0.5～1.5 hour under 300 ℃～480 ℃ oxidate temperature at last, can obtain nanocrystalline IrO 2-Ta 2O 5-MO 2The coated titanium base electrode
The nanocrystalline IrO that the present invention is prepared 2-Ta 2O 5-SnO 2Coated titanium base electrode, matrix titanium plate apply molar content SnO after the sandblast pre-treatment 210% IrO 2(63%)-Ta 2O 5(27%)-SnO 2(10%)/and the Ti coated titanium electrode, IrO 2Average crystal grain be 7.93nm: it is 1519 hours that its accelerated aging is tested in accelerated life test, and the condition of accelerated life test is: 0.5moldm -3H 2SO 4, anodic current density 20000Am -2, 50 ℃ of temperature.
The nanocrystalline IrO that the present invention is prepared 2-Ta 2O 5-SiO 2The coated titanium base electrode, SiO 2Weight percent be 7%, IrO in the coating 2Average grain size be 12.43nm.
The apparent pattern of the prepared electrode of the present invention is even, separates out the tiny dispersion of crystal grain, has high stability, is long-life advantage.Electrode of the present invention can be applicable to industrial plating, electrolysis, galvanic protection, hypochlorite generator, electrolysis treatment waste water plant etc.
Embodiment
Embodiment 1. preparation IrO 2-Ta 2O 5-SnO 2Electrode: the pure titanium plate of not sandblast and sandblast is cut into 20 * 25mm size, carry out alkali cleaning, pickling then.Extract TaCl 5-C 2H 5OH solution (Ta180g/L) 1.855ml and chloro-iridic acid (Ir119g/L) 3.48ml place weighing bottle to mix, and put into baking oven in 90 ℃ of down bakings 10 hours, become finely powdered to mixture.Add solvent, make solution become limpid.Weighing tin protochloride (SnCl 22H 2O), make SnO 2Amount of substance account for IrO 2-Ta 2O 5-SnO 2Total amount of substance 5～15% is with itself and IrO 2-Ta 2O 5Solution mixes, and is mixed with IrO 2-Ta 2O 5-SnO 2Coating solution.With fur suede pen masking liquid is brushed on titanium plate two sides, put and dry 5min in the baking oven under 90 ℃, 370 ℃ of following sintering 5min in retort furnace take out the back air cooling to room temperature then, repeat above step to applying 3 layers.Then, in 90 ℃ of following oven dry 5min, 370 ℃ of following sintering 10min in retort furnace more so repeatedly to applying 10 layers, place retort furnace 370 ℃ of following sintering 1.5 hours, promptly make nanocrystalline electrode in baking oven.
Table 1 is the IrO of coating when the X-ray diffraction analysis collection of illustrative plates is utilized different sandblast conditions that the Scherrer formula calculates gained with different Sn content 2Average grain size.At SnO 2Content 5～15% scopes, matrix titanium plate apply after the sandblast pre-treatment and contain SnO 210% IrO 2(63%)-Ta 2O 5(27%)-SnO 2(10%)/IrO of Ti electrode coating 2The grain-size minimum.Its stability is investigated by accelerated life test.The condition of accelerated life test is: 0.5moldm -3H 2SO 4, anodic current density 20000Am -2, 50 ℃ of temperature.The IrO of sandblast pre-treatment 2(63%)-Ta 2O 5(27%)-SnO 2(10%)/life-span of Ti electrode is 1519 hours.Life test under the equal conditions of relevant document place, IrO 2-Ta 2O 5Coating titanium anode is 889 hours (Zhang Zhaoxian, Tang Renheng, Zhang Jianhua, IrO 2-Ta 2O 5The research of coating titanium anode and application, Guangdong non-ferrous metal journal, 2002,12 (2)).The stanniferous antimony middle layer Ir-SnO of number of patent application: 00119691.X preparation 2-PdO electrode is at 30%H 2SO 4, current density 15000Am -2, during 40 ℃ of electrolysis of temperature, the life-span is 1255 hours.The accelerated aging of the nanocrystalline electrode that makes of the present invention is longer as can be seen, stability is better.
Table 1 IrO 2Average grain size calculates
Different matrix pre-treatment and coating composition (mol%) IrO 2Average grain size
IrO 2(70％)-Ta 2O 5(30%) (not sandblast) 10.575
IrO 2(70％)-Ta 2O 5(30%) (sandblast) 8.426
IrO 2(66.5％)-Ta 2O 5(28.5％)-SnO 2(5%) (not sandblast) 10.84
IrO 2(66.5％)-Ta 2O 5(28.5％)-SnO 2(5%) (sandblast) 9.63
IrO 2(63％)-Ta 2O 5(27％)-SnO 2(10%) (not sandblast) 8.987
IrO 2(63％)-Ta 2O 5(27％)-SnO 2(10%) (sandblast) 7.93
IrO 2(59.5％)-Ta 2O 5(25.5％)-SnO 2(15%) (not sandblast) 12.257
IrO 2(59.5％)-Ta 2O 5(25.5％)-SnO 2(15%) (sandblast) 14.187
Embodiment 2. preparation IrO 2-Ta 2O 5-SiO 2Electrode: titanium plate pretreatment mode is identical with example 1.The IrO of preparation 2-Ta 2O 5Solution is identical with example 1.Add 0.227ml concentration therein and be 25.5% acidic silicasol solution, make SiO 2Weight percent therein is 7%, makes IrO 2-Ta 2O 5-SiO 2Coating solution.With fur suede pen masking liquid is brushed on titanium plate two sides, put and dry 5min in the baking oven under 90 ℃, 350 ℃ of following sintering 5min in retort furnace take out the back air cooling to room temperature then, repeat above step to applying 3 layers.Then, in baking oven, be still in 90 ℃ of following oven dry 5min, but in retort furnace 350 ℃ of following sintering 10min, so repeatedly to applying 10 layers.Make required nanocrystalline electrode, utilize the Scherrer formula to calculate the IrO of this electrode coating by the X-ray diffraction analysis collection of illustrative plates 2Average grain size is 12.43nm.

Claims (4)

1, a kind of nanocrystalline iridium series oxide coating electrode preparation method is characterized in that, preparation process is:
(1) substrate pretreated comprises: mechanical pre-treatment, alkali cleaning oil removing, pickling;
The machinery pre-treatment: pure titanium plate cuts into the size of required usefulness through sandblast;
Alkali cleaning oil removing: an amount of washing powder and anhydrous sodium carbonate are put into the container ware by 1: 2～2: 1 mixed, add deionized water and be mixed with washing lotion, after being heated to 85～95 ℃ the titanium plate put into and boil 15～60 minutes, use hairbrush flush away oil stain simultaneously, the titanium plate is after deoiling, rinse oven dry again well with deionized water;
Pickling: the pickling mode of employing is that working concentration is 2～3.5moldm -3Hydrochloric acid soln as pickle solution, put into the titanium plate after being heated to 85～95 ℃, soak and be red-purple to pickle solution in 15～60 minutes, take out the titanium plate and wash repeatedly only with deionized water, dry;
(2) coating liquid preparation: by Ir: the Ta mol ratio is 7: 6, H 2IrCl 6And TaCl 5The ratio that accounts for total amount of substance 30～95% takes by weighing desired number, mixes to be positioned in the glassware to dissolve, and puts into baking oven then in 70～100 ℃ of oven dry 5～12 hours, bakes fine powder; Then, got dehydrated alcohol and Virahol volume ratio 3: 1～1: 3, with the gained powder dissolution; When adding the muriate of the 3rd constituent element M, account for total amount of substance 5～70%, take by weighing desired number, be added in the former masking liquid according to the muriatic amount of complex element M; M is Nb, Pb, Si, Sn, Mn, Ti.
(3) coating procedure: masking liquid is brushed on titanium plate surface with fur suede pen, put in the baking oven and dried 5～10 minutes down in 90 ℃～150 ℃, make organic solvent volatilization, again in retort furnace in 5～20 minutes time of 300 ℃～480 ℃ sintering temperatures, precious metal salt is decomposed generates oxide coating; Take out the back air cooling to room temperature, repeat the thickness of above step until needs; Place retort furnace sintering 0.5～1.5 hour under 300 ℃～480 ℃ oxidate temperature at last, obtain nanocrystalline IrO 2-Ta 2O 5-MO 2The coated titanium base electrode.
2, according to the described preparation method of claim 1,, it is characterized in that prepared nanocrystalline IrO 2-Ta 2O 5-MO 2IrO in the coated titanium base electrode coating 2Average grain size is 8～15nm.
3, according to the described preparation method of claim 1, it is characterized in that prepared nanocrystalline IrO 2-Ta 2O 5-SnO 2Coated titanium base electrode, matrix titanium plate apply molar content SnO after the sandblast pre-treatment 210% IrO 2(63%)-Ta 2O 5(27%)-SnO 2(10%)/and the Ti coated titanium electrode, IrO 2Average crystal grain be 7.93nm: it is 1519 hours that its accelerated aging is tested in accelerated life test, and the condition of accelerated life test is: 0.5moldm -3H 2SO 4, anodic current density 20000Am -2, 50 ℃ of temperature.
4, according to the described preparation method of claim 1, it is characterized in that prepared nanocrystalline IrO 2-Ta 2O 5-SiO 2The coated titanium base electrode, SiO 2Weight percent be 7%, IrO in the coating 2Average grain size be 12.43nm.
CN 200610144150 2006-11-28 2006-11-28 Nanocrystalline iridium series oxide coating electrode preparation method Pending CN1995464A (en)

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CN113957473A (en) * 2021-10-28 2022-01-21 西安泰金工业电化学技术有限公司 Preparation method of titanium anode with multilayer structure
CN113881962A (en) * 2021-10-28 2022-01-04 西安泰金工业电化学技术有限公司 Preparation method of high-conductivity Ir-Ta-Mn composite oxide coating anode
CN114351179A (en) * 2021-12-02 2022-04-15 江苏友诺环保科技有限公司 Iridium tantalum manganese coating titanium anode plate with intermediate layer and preparation method thereof
CN114395757A (en) * 2021-12-02 2022-04-26 江阴安诺电极有限公司 Multi-oxide coating titanium anode plate and preparation method thereof
CN114395757B (en) * 2021-12-02 2024-04-26 江阴安诺电极有限公司 Preparation method of multi-element oxide coating titanium anode plate

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