阅读说明：本技术 一种水电解用析氧电极的制备方法 (A kind of preparation method of water electrolysis analysis oxygen electrode ) 是由 王选明 于 2019-09-20 设计创作，主要内容包括：本发明公开了一种水电解用析氧电极的制备方法,包括通过通过溅射的方法制取铁合金薄膜,随后对铁合金薄膜进行脱合金处理得到纳米多孔金属基体；然后将纳米多孔金属基体置于铁钨离子混合液中进行原位生长铁钨复合氧化物处理,原位生长铁钨复合氧化物处理后即可得到所述析氧电极。上述制得的水电解析氧电极,通过原位生长得到的铁钨复合氧化物,主要组成为钨酸亚铁,同时含有少量的FeOOH纳米棒、WO<Sub>3</Sub>纳米棒,钨酸亚铁中Fe<Sup>2+</Sup>和W<Sup>6+</Sup>离子能够与O<Sup>2-</Sup>离子形成八面体配位,而且钨酸亚铁、FeOOH纳米棒、WO<Sub>3</Sub>纳米棒之间形成很好的协同作用,使得析氧电极表现出较低的产氧电势、高稳定性和高产氧效率,同时,铁钨复合氧化物的生产成本低、操作方便。(The invention discloses a kind of water electrolysis preparation methods of analysis oxygen electrode, including producing ferroalloy film by the method by sputtering, then carry out de- alloy treatment to ferroalloy film and obtain nano porous metal matrix；Then nano porous metal matrix is placed in ferrotungsten Ar ion mixing liquid and carries out the processing of growth in situ ferrotungsten composite oxides, the analysis oxygen electrode can be obtained after the processing of growth in situ ferrotungsten composite oxides.Water power obtained above parses oxygen electrode, the ferrotungsten composite oxides obtained by growth in situ, and main group becomes ferrous tungstate, contains a small amount of FeOOH nanometer rods, WO simultaneously 3 Nanometer rods, Fe in ferrous tungstate 2+ And W 6+ Ion can be with O 2‑ Ion forms octahedral coordination, and ferrous tungstate, FeOOH nanometer rods, WO 3 Synergistic effect well is formed between nanometer rods, so that analysis oxygen electrode shows lower production oxygen voltage, high stability and high yield oxygen efficiency, meanwhile, the production cost of ferrotungsten composite oxides is low, easy to operate.)

1. a kind of water electrolysis preparation method of analysis oxygen electrode, it is characterised in that: including passing through

Ferroalloy film is produced by the method for sputtering, de- alloy treatment then is carried out to ferroalloy film and obtains nano-porous gold Belong to matrix；Then nano porous metal matrix is placed in ferrotungsten Ar ion mixing liquid and is carried out at growth in situ ferrotungsten composite oxides The analysis oxygen electrode can be obtained after the processing of growth in situ ferrotungsten composite oxides in reason.

2. the water electrolysis according to claim 1 preparation method of analysis oxygen electrode, it is characterised in that: nano porous metal base Body is nanoporous platinum base body or nano-porous gold matrix.

3. the water electrolysis according to claim 1 preparation method of analysis oxygen electrode, it is characterised in that: ferrotungsten Ar ion mixing liquid It is formulated by ferrous sulfate and sodium tungstate.

4. the water electrolysis according to claim 1 preparation method of analysis oxygen electrode, which is characterized in that including operating as follows:

S1: being cleaned by ultrasonic 5min using acetone for iron foil matrix, then reuses dilute hydrochloric acid ultrasonic cleaning 5min, finally uses nothing Water-ethanol removes solion remained on surface and rapid draing；Iron foil is transferred on magnetron sputtering apparatus matrix sample platform, Magnetron sputtering reaction chamber is closed, pumping is very passed through argon gas afterwards, after iron target sputters 10min with 150W, opens platinum target with 200W and iron Target cosputtering 2h together, by obtained above-mentioned material in argon gas protection atmosphere 450 DEG C of annealing 2h, after heating anneal, both Obtain iron foil alloy firm；

S2: iron foil alloy firm is cut according to required size, is put into the hydrochloric acid solution of 1mol/L after cutting and is removed iron gold Category can be prepared by nanoporous platinum base body；

S3: ferrous sulfate solution, ammonium sulfate, sodium tungstate solution are configured with ultrapure water respectively, according to Fe²⁺ _、NH₄ ⁺、WO₄ ²It is 1: The molar ratio of 2:1.2 is taken ferrous sulfate solution, ammonium sulfate, sodium tungstate solution and is mixed, and sulfuric acid is added and adjusts PH To 2.0, mixed solution is placed in pvc response kettle, nanoporous platinum base body is lost into reaction kettle, 200 DEG C of heating are reacted 10h after reaction takes out matrix, and the analysis oxygen electrode can be obtained after cleaning-drying.

Technical field

The present invention relates to photocatalytic water electrode technology fields, and in particular to a kind of preparation method of water electrolysis analysis oxygen electrode.

Background technique

Water electrolysis hydrogen producing because its technically reliable, without separation, readily available high-purity H₂, it is easy to operate, easy to maintain, It is pollution-free, be able to achieve automatic control and be widely adopted and study.In practical water electrolysis hydrogen production, overpotential for oxygen evolution is than liberation of hydrogen Big more of overpotential, are constantly precipitated O on analysis oxygen electrode₂And itself is in high potential, this will lead to electrode surface and generates additionally Poorly conductive oxide skin(coating), considerably increase resistance, therefore, the anti-hydrogen production rate of electrolysis water depend on analysis oxygen electrode effect Rate.The thinking for reducing overpotential for oxygen evolution mainly has: improving electrolysis temperature；Study the analysis oxygen electrode of efficient stable and into electrolyte A small amount of additive is added, currently, the research emphasis of electrolyzed alkaline water hydrogen producing technology is development of new analysis oxygen anodes material, or The electrocatalysis characteristic for improving existing analysis oxygen anodes material, reduces anodic overpotential, to achieve the purpose that improve hydrogen production efficiency.

The preparation method of analysis oxygen elctro-catalyst usually has metal salt thermal decomposition method, spray heating decomposition, coprecipitation, colloidal sol Gel method, freeze-drying etc..The raw material of preparation is also various, but universal raw material used is mostly noble metal material at present Material, therefore high production cost, while the analysis oxygen electrode prepared also there is also complex process, overpotential for oxygen evolution is larger, stability compared with The defects of poor.

Summary of the invention

The object of the present invention is to provide a kind of water electrolysis preparation method of analysis oxygen electrode, water electrolysis hydrogen producing effect is good.

The technical solution that the present invention takes is specific as follows:

A kind of preparation method of water electrolysis analysis oxygen electrode, it is characterised in that: including passing through

Ferroalloy film is produced by the method for sputtering, de- alloy treatment then is carried out to ferroalloy film and obtains nano-porous gold Belong to matrix；Then nano porous metal matrix is placed in ferrotungsten Ar ion mixing liquid and is carried out at growth in situ ferrotungsten composite oxides The analysis oxygen electrode can be obtained after the processing of growth in situ ferrotungsten composite oxides in reason.

Nano porous metal matrix is nanoporous platinum base body or nano-porous gold matrix.

Ferrotungsten Ar ion mixing liquid is formulated by ferrous sulfate and sodium tungstate.

Concrete operations are as follows:

S1: being cleaned by ultrasonic 5min using acetone for iron foil matrix, then reuses the concentrated hydrochloric acid ultrasonic cleaning 5min of 20 times of dilution, Finally solion remained on surface and rapid draing are removed using dehydrated alcohol；Iron foil is transferred to magnetron sputtering apparatus matrix On sample stage, close magnetron sputtering reaction chamber, pumping is very passed through argon gas afterwards, after iron target sputters 10min with 150W, open platinum target with Obtained above-mentioned material is protected 450 DEG C of annealing 2h in atmosphere, heating anneal knot in argon gas by 200W cosputtering 2h together with iron target Shu Hou both obtains iron foil alloy firm；

S2: iron foil alloy firm is cut according to required size, is put into the hydrochloric acid solution of 1mol/L after cutting and is removed iron gold Category can be prepared by nanoporous platinum base body；

S3: ferrous sulfate solution, ammonium sulfate, sodium tungstate solution are configured with ultrapure water respectively, according to Fe²⁺ _、NH₄ ⁺、WO₄ ²For The molar ratio of 1:2:1.2 is taken ferrous sulfate solution, ammonium sulfate, sodium tungstate solution and is mixed, and sulfuric acid adjusting is added Mixed solution is placed in pvc response kettle by PH to 2.0, and nanoporous platinum base body is lost into reaction kettle, and 200 DEG C of heating are anti- 10h is answered, after reaction takes out matrix, the analysis oxygen electrode can be obtained after cleaning, 120 DEG C of dryings.

Water power obtained above parses oxygen electrode, and the ferrotungsten composite oxides obtained by growth in situ, main group becomes Ferrous tungstate contains a small amount of FeOOH nanometer rods, WO simultaneously₃Nanometer rods, Fe in ferrous tungstate²⁺And W⁶⁺Ion can be with O^2- Ion forms octahedral coordination, and ferrous tungstate and a small amount of FeOOH nanometer rods, WO₃Association well is formed between nanometer rods Same-action, so that analysis oxygen electrode shows lower production oxygen voltage, high stability and high yield oxygen efficiency, meanwhile, ferrotungsten composite oxygen The production cost of compound is low, easy to operate.

Specific embodiment

In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out specifically with reference to embodiments It is bright.It should be appreciated that following text is only used to describe one or more of specific embodiments of the invention, not to the present invention The protection scope specifically requested carries out considered critical.

In following each embodiments, unless otherwise instructed, agents useful for same and drug are commercially available by commercial sources.