CN103741165B - A kind of active coating embedding ruthenium titanium oxide and preparation method thereof - Google Patents
A kind of active coating embedding ruthenium titanium oxide and preparation method thereof Download PDFInfo
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- CN103741165B CN103741165B CN201410037120.9A CN201410037120A CN103741165B CN 103741165 B CN103741165 B CN 103741165B CN 201410037120 A CN201410037120 A CN 201410037120A CN 103741165 B CN103741165 B CN 103741165B
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Abstract
The invention discloses a kind of active coating embedding ruthenium titanium oxide and preparation method thereof, described active coating is based on iridium tantalum pentoxide, which is embedded ruthenium titanium oxide.Control to obtain the yardstick nanometer ruthenium titanium oxide powder within 15nm by sintering temperature, a nanometer ruthenium titanium oxide powder is mixed in iridium tantalum pentoxide presoma, after heated solidification, in the batch-type furnace of 530 DEG C oxidation and sinter and annealing after, Embedded iridium tantalum pentoxide active coating can be obtained.The active material of the present invention has analysis oxygen and analysis chlorine performance concurrently, considerably improves iridium tantalum active oxide coatings synthetic activity, and has higher practicality.The preparation method of the present invention has simple and convenient, workable, the feature that cost performance is high.
Description
Technical field
The invention belongs to the electrode material field of Applied Electrochemistry and energy industry, relate to a kind of material with high electrocatalysis characteristic and preparation method thereof.Concrete application includes electrochemical component and the devices such as acid electrolytic solution, weak brine electrolysis, organic solution electrolysis, cathodic protection, electrochemical sensor.The particularly suitable active coating being used as electrode material in chlorine, oxygen double; two analysis electrolysis bath.
Background technology
Active electrode is parts crucial in electrochemical industry, and nineteen sixty-five Beer develops ruthenic oxide coated anode first, has opened up the anode material of a new generation, and the existence of active coating gives the analysis chlorine activity that this kind of anode is high.Through big quantity research, in active coating, with RuO2+TiO2The binary oxide being composited has advantageous combination property, is analyse the most commonly used coating material that chlorine is industrial.People recognize gradually, and ruthenic oxide coating is not appropriate in the occasion of analysis oxygen to apply.Vercesi in 1991 etc. propose the demand adopting iridio oxide can realize oxygen evolution reaction, have succeeded in developing IrO later2+Ta2O5Composite oxides anode material, this material can be suitable for more stringent electrolytic condition, and has higher oxygen evolution activity.At present, analysis chlorine and analysis oxygen electrode have become topmost two class gassing active electrode materials in electrochemical industry.Along with industrial expansion, the expansion of application, use the complexity of environment, analysis Cl single traditionally2, analysis O2Day by day highlight by the limitation of anode.In producing at electrometallurgy field, electrolytic acid aqueous solution and perchlorate, more situation is to there is oxygen-containing and chlorine-containing compound in electrolyte, makes electrolytic environments more harsh, and therefore electrode material is also affected by more acid test.For this, research and development oxygen chlorine double; two analysis electrode material has very important practical significance.For the active coating of development of new, this research team is round TiO2+RuO2And IrO2+Ta2O5Conduct in-depth research, achieve certain achievement, as in 91 volumes of 2008 " American Ceramics association journal " with " PhaseStructureandMicrostructureofaNanoscaleTiO2-RuO2-IrO2-Ta2O5AnodeCoatingonTitanium " for inscribing, disclose a kind of TiO2+RuO2+IrO2+Ta2O5The technology of preparing of active coating；Chinese patent 200810072273.1 proposes the patent of invention of the activity " preparation method with the Ni-Ti anode of alternating structure coating " adopting alternating structure, it is thus achieved that patent for invention.These coatings play obvious effect in the corrosion resistance improve Ni-Ti anode.Recently, the research of this research group finds to adopt the method embedding ruthenium titanium oxide, namely at IrO2-Ta2O5Coating oxidation thing adds RuO2-TiO2The method of oxide nanocrystalline, improves IrO2+Ta2O5Analysis chlorine characteristic, prepare the iridium tantalum active anode coating of the damascene structures of a kind of novel ruthenium titanium oxide, will can obtain the characteristic of analysis oxygen and analysis chlorine simultaneously, it is hereby achieved that the double; two analysis active coating electrode material of efficient oxygen, chlorine.
Summary of the invention
It is an object of the invention to provide a kind of active coating embedding ruthenium titanium oxide and preparation method thereof, thus obtaining the high activity electrode material having higher pervasive effect.
The thinking of the present invention is in original iridium tantalum pentoxide active coating, utilizes embedded technology to add ruthenium titanium oxide in this coating, with improve iridium tantalum pentoxide can analyse at the same time oxygen and analysis chlorine occasion in there is more superior activity.This thinking is based on iridium tantalum pentoxide and ruthenium titanium oxide is the analysis chlorine generally acknowledged at present respectively and analyses the two class active electrode materials that oxygen is the most frequently used.Along with growing industrial expansion, the expansion of application, use the complexity of environment, analysis Cl single traditionally2, analysis O2Day by day highlight by the limitation of anode.In order to adapt to this change, this team proposes employing and embeds ruthenium titanium oxide in iridium tantalum pentoxide active coating so that in electrode process under arms, except the oxygen evolution reaction of iridium tantalum pentoxide, the exposed ruthenium titanium oxide on surface can carry out analysis chlorine reaction, the effective active of the electrode of enhancing.This oxygen, chlorine double; two analysis electrode material has very important practical significance.
The operating principle of the present invention adds the nano level ruthenium titanium active oxidation composition granule of part exactly in iridium tantalum pentoxide presoma.Described damascene structures is derived from adopting particle diameter to be about the effect that the insert of < 15nm adds, and has, thus obtaining, the structure that composite is similar.Ratio again through ruthenium titanium oxidate nano yardstick with iridium tantalum pentoxide controls, it is possible to obtain the analysis oxygen of needs and the performance of analysis chlorine.Owing to the internal organizational structure of active material is produced to significantly affect by the dosage of insert, add very little, embed interface increase amount limited, then the limited efficiency that activity improves.Adding too many, the interface accounting of embedding is too high, affects the associativity of active material, corrosion resisting property is had a negative impact.It is 18～22mol% by the optimum dosage of mole total of the active substance of design.
The employing imbedding method of the present invention prepare with ruthenium titanium oxide nanocrystalline be insert the core technology of iridium tantalum active oxide coatings include, (1) first prepares ruthenium titanium oxide, and it has suitable nanoscale；(2) mix with the presoma of iridium tantalum activating oxide, on co-deposition and titanio material；(3) heat treatment of the iridium tantalum pentoxide coating containing ruthenium titanium oxide embedded structure.
The preparation method of the present invention mainly includes following four step:
(1) preparation of ruthenium titanium oxide serosity: with RuCl3And TiCl3For source material, weigh each source material in Ru: Ti ratio, will the two mix homogeneously, obtain ruthenium titanium oxide active serosity；
(2) prepared by the sintering of ruthenium titanium oxide nano particles: extract ruthenium titanium oxide active serosity, after heated solidification, and then oxidation and sinter, it is thus achieved that there is the insert of the ruthenium titanium oxide of nanoscale.
(3) preparation of iridium tantalum pentoxide serosity: with H2IrCl6And TaCl5For source material, weigh each source material in proportion, will the two mix homogeneously, obtain active slurry；
(4) preparation of active coating: be mixed into by ruthenium titanium oxide nano particles in iridium tantalum pentoxide active slurry, be sufficiently stirred for, is coated on titanio material; after heated solidification; oxidation and sinter, finally anneals, and namely obtains the iridium tantalum pentoxide active coated Ti embedding ruthenium titanium oxide.
The present invention has the remarkable advantages that:
(1) present invention efficiently utilizes the principle increasing crystal boundary ratio of nanotechnology and composite, imports substantial amounts of damascene structures by embedding grammar.Add the number of channels of proton, so that the activity raising of electrode material.
(2) owing to passing through to prepare in advance the nano-powder of the scattered fine dimension having, the crystal miniaturization of final ruthenium titanium oxide is made after embedding, add the density in active center, so that the actual bearer electric current density at electrode activity center declines, so that the activity raising of electrode material.
(3) owing to adding the nano level ruthenium titanium active oxidation composition granule of part in iridium tantalum pentoxide presoma.Can be controlled by the ratio of ruthenium titanium oxide with iridium tantalum pentoxide, it is possible to obtain the analysis oxygen of needs and the performance of analysis chlorine.Owing to the coating of the present invention is based on iridium tantalum pentoxide, so the activity of its gassing mainly analyses oxygen, secondary is analysis chlorine.
(4) due to the fact that have employed traditional ruthenium titanium oxide active slurry solidifies in advance, dispersion, the method for refinement, making and the storage of raw material are all easy to.Added in iridium tantalum active slurry, it is possible to prepare electrode material by traditional handicraft.Therefore technique is simple, easy, does not totally make processing cost increase.Owing to improving the performance of electrode material, the cost performance of electrode product is made to be obviously improved.
Accompanying drawing explanation
Fig. 1 is transmission electron microscopy (TEM) photo of ruthenium titanium oxide insert.
Detailed description of the invention
The concrete preparation process of the iridium tantalum pentoxide with original position embedded structure of the present invention is as follows:
(1) preparation of ruthenium titanium oxide serosity: with RuCl3And TiCl3For source material, weighing each source material in the ratio of Ru: Ti mol ratio 3: 7, and be dissolved in butanol respectively, concentration controls at about 0.3mol/L, after each source material fully dissolves will the two mix homogeneously, obtain ruthenium titanium oxide active serosity；
(2) prepared by the sintering of ruthenium titanium oxide nano particles: quantitatively extract ruthenium titanium oxide active serosity, after 90 DEG C are heating and curing, take out and grinds, then oxidation and sinter in the batch-type furnace of 395 DEG C, come out of the stove cooling, after grinding, it is thus achieved that there is the insert of the ruthenium titanium oxide of nanoscale.
(3) preparation of iridium tantalum pentoxide serosity: with H2IrCl6And TaCl5For source material, weighing each source material in the ratio of Ir: Ta mol ratio 7: 3, and be dissolved in butanol respectively, concentration controls at about 0.1mol/L, after each source material fully dissolves will the two mix homogeneously, obtain active slurry；
(4) preparation of active coating: extract the iridium tantalum active slurry of ruthenium titanium nm-class oxide powder and 85 ~ 75mol% by 15 ~ 25mol% of mole total amount of active substance, ruthenium titanium oxide nano particles is mixed in iridium tantalum pentoxide active slurry, it is sufficiently stirred for, it is coated on etched titanio material, after 110 DEG C are heating and curing, oxidation and sinter 10 minutes in the batch-type furnace of 530 DEG C, row coating again after cooling, heat treatment, come out of the stove cooling, repeat 10-15 time altogether, last 530 DEG C of annealing 1 hour, namely the iridium tantalum pentoxide active coated Ti embedding ruthenium titanium oxide is obtained.
The present invention obtains the iridium tantalum pentoxide active titanium anode that embedded in ruthenium titanium oxide nano structure by above-mentioned enforcement.Research shows, the refinement of crystal grain and increasing of crystal boundary, is effectively improved the active center density of activating oxide, improves the conductive capability of dispersity and proton, to such an extent as to makes activity be improved.Owing to the present invention is to having the iridium tantalum pentoxide active material embedding ruthenium titanium oxide structure, it is provided with the activity of analysis oxygen and analysis chlorine simultaneously.Carrying out contrast experiment with traditional iridium tantalum pentoxide active material of preparation under equal conditions, result shows that the combination property with the iridium tantalum pentoxide active material of ruthenium titanium oxide embedded structure is improved significantly.Table 1 for without embedded structure and the iridium tantalum pentoxide active material analysis oxygen when parallel laboratory test that has embedded structure and analyse chlorine performance.Can clearly finding out, the Ni-Ti anode of embedded structure is suitable with the oxygen evolution potential of traditional Ni-Ti anode in the performance of analysis oxygen, but the current potential of its analysis chlorine substantially reduces.This fully shows, has the iridium tantalum pentoxide active material embedding ruthenium titanium oxide nano structure and has good oxygen, chlorine double; two analysis performance.
Describe two examples of implementation of the present invention in detailed below, but the present invention is not limited to this.
Embodiment 1
The preparation of the iridium tantalum activating oxide covering electrodes material adding 18mol% insert sequentially includes the following steps:
(1) preparation of ruthenium titanium oxide serosity: with RuCl3And TiCl3For source material, weighing each source material in the ratio of Ru: Ti mol ratio 3: 7, and be dissolved in butanol respectively, concentration controls at 0.25mol/L, after each source material fully dissolves will the two mix homogeneously, obtain ruthenium titanium oxide active serosity；
(2) prepared by the sintering of ruthenium titanium oxide nano particles: quantitatively extract ruthenium titanium oxide active serosity, after 90 DEG C are heating and curing, take out and grinds, then oxidation and sinter in the batch-type furnace of 395 DEG C, come out of the stove cooling, after grinding, it is thus achieved that there is the insert of the ruthenium titanium oxide that nanoscale is 14nm.
(3) preparation of iridium tantalum pentoxide serosity: with H2IrCl6And TaCl5For source material, weighing each source material in the ratio of Ir: Ta mol ratio 7: 3, and be dissolved in butanol respectively, concentration controls at 0.15mol/L, after each source material fully dissolves will the two mix homogeneously, obtain active slurry；
(4) preparation of active coating: extract the iridium tantalum active slurry of ruthenium titanium nm-class oxide powder and 78mol% by the 18mol% of mole total amount of active substance, ruthenium titanium oxide nano particles is mixed in iridium tantalum pentoxide active slurry, it is sufficiently stirred for, it is coated on the titanio material after the 10% oxalic acid 1 hour cleaning-drying of etching that seethes with excitement, after 110 DEG C are heating and curing, oxidation and sinter 10 minutes in the batch-type furnace of 530 DEG C, row coating again after cooling, heat treatment, come out of the stove cooling, repeat 12 times altogether, last 530 DEG C of annealing 1 hour, namely the iridium tantalum pentoxide active coated Ti embedding ruthenium titanium oxide is obtained.Its analysis oxygen and analysis chlorine performance are shown in Table 1.
Embodiment 2
The preparation of the iridium tantalum activating oxide covering electrodes material adding 22% insert sequentially includes the following steps:
(1) preparation of ruthenium titanium oxide serosity: with RuCl3And TiCl3For source material, weighing each source material in the ratio of Ru: Ti mol ratio 7: 3, and be dissolved in butanol respectively, concentration controls at 0.35mol/L, after each source material fully dissolves will the two mix homogeneously, obtain ruthenium titanium oxide active serosity；
(2) prepared by the sintering of ruthenium titanium oxide nano particles: quantitatively extract ruthenium titanium oxide active serosity, after 90 DEG C are heating and curing, take out and grind, then oxidation and sinter in the batch-type furnace of 385 DEG C, come out of the stove cooling, after grinding, it is thus achieved that there is the insert of the ruthenium titanium oxide that nanoscale nanoscale is 13nm.
(3) preparation of iridium tantalum pentoxide serosity: with H2IrCl6And TaCl5For source material, weighing each source material in the ratio of Ir: Ta mol ratio 7: 3, and be dissolved in butanol respectively, concentration controls at 0.15mol/L, after each source material fully dissolves will the two mix homogeneously, obtain active slurry；
(4) preparation of active coating: extract the iridium tantalum active slurry of ruthenium titanium nm-class oxide powder and 85 ~ 75mol% by 15 ~ 25mol% of mole total amount of active substance, ruthenium titanium oxide nano particles is mixed in iridium tantalum pentoxide active slurry, it is sufficiently stirred for, it is coated on the titanio material after the 10% oxalic acid 1 hour cleaning-drying of etching that seethes with excitement, after 110 DEG C are heating and curing, oxidation and sinter 10 minutes in the batch-type furnace of 530 DEG C, row coating again after cooling, heat treatment, come out of the stove cooling, repeat 15 times altogether, last 530 DEG C of annealing 1 hour, namely the iridium tantalum pentoxide active coated Ti embedding ruthenium titanium oxide is obtained.Its analysis oxygen and analysis chlorine performance are shown in Table 1.
Table 1 has the electrochemical properties of the iridium tantalum pentoxide Ni-Ti anode embedding ruthenium titanium oxide structure
The foregoing is only presently preferred embodiments of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to the covering scope of the present invention.
Claims (1)
1. the preparation method of the active coating embedding ruthenium titanium oxide, it is characterised in that: described active coating is based on iridium tantalum pentoxide, which is embedded ruthenium titanium oxide；
In described ruthenium titanium oxide, the mol ratio of Ru and Ti is 3:7；
In described iridium tantalum pentoxide, the mol ratio of Ir and Ta is 7:3；
In described active coating, the mol ratio of Ir and Ru is 75 ~ 85:15 ~ 25；
The particle diameter of described ruthenium titanium oxide is less than 15nm；
Preparation method comprises the following steps:
(1) preparation of ruthenium titanium oxide active serosity: with RuCl3And TiCl3For source material, be that 3:7 weighs each source material by the mol ratio of Ru and Ti, and be dissolved in butanol respectively, after each source material fully dissolves will the two mix homogeneously, obtain ruthenium titanium oxide active serosity；
(2) sintering of ruthenium titanium oxide nano particles: extract ruthenium titanium oxide active serosity, after 90 DEG C are heating and curing, take out and grinds, and then oxidation and sinter in the batch-type furnace of 395 DEG C, cooling of coming out of the stove, after grinding, it is thus achieved that ruthenium titanium oxide nano particles；
(3) preparation of iridium tantalum pentoxide active slurry: with H2IrCl6And TaCl5For source material, be weigh each source material at 7: 3 by Ir and Ta mol ratio, and be dissolved in butanol respectively, after each source material fully dissolves will the two mix homogeneously, obtain iridium tantalum pentoxide active slurry；
(4) preparation of active coating: weigh ruthenium titanium oxide nano particles by the 15 ~ 25% of mole total amount of active substance, iridium tantalum pentoxide active slurry is weighed by the 85 ~ 75% of mole total amount of active substance, ruthenium titanium oxide nano particles is mixed in iridium tantalum pentoxide active slurry, it is sufficiently stirred for, it is coated on etched titanio material, after 110 DEG C are heating and curing, oxidation and sinter 10 minutes in the batch-type furnace of 530 DEG C, row coating again after cooling, heat treatment, come out of the stove cooling, repeat 10-15 time altogether, last 530 DEG C of annealing 1 hour, namely the iridium tantalum pentoxide active coated Ti embedding ruthenium titanium oxide is obtained.
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| CN104988530B (en) * | 2015-08-12 | 2018-01-26 | 海南金海浆纸业有限公司 | A kind of composite coating anode and preparation method thereof and electrolytic cell |
| CN108048895B (en) * | 2017-12-20 | 2019-12-17 | 福州大学 | nickel-based active electrode material embedded with ruthenium-zirconium composite oxide and preparation method thereof |
| CN108048870B (en) * | 2017-12-20 | 2019-12-17 | 福州大学 | Nickel-based active electrode material embedded with ruthenium-silicon composite oxide and preparation method thereof |
| CN108048869B (en) * | 2017-12-20 | 2019-08-09 | 福州大学 | A kind of Ni-based active electrode material and preparation method thereof being embedded in ruthenium hafnium composite oxides |
| CN110438527A (en) * | 2019-08-05 | 2019-11-12 | 上海氯碱化工股份有限公司 | The preparation method of the transient metal doped anode containing ruthenium coating |
| CN112010400A (en) * | 2020-07-20 | 2020-12-01 | 西安怡速安智能科技有限公司 | Anode layer formula of electrochemical electrode for water sterilization |
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