CN107988617A - Water electrolysis efficiently, double-function catalyzing electrode and preparation method thereof - Google Patents
Water electrolysis efficiently, double-function catalyzing electrode and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- 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
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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
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention belongs to electrochemical catalysis electrode technology field, be specially water electrolysis efficiently, double-function catalyzing electrode and preparation method thereof.The method that the present invention uses chemical plating, pretreatment matrix is immersed in chemical plating fluid, reacts the catalysis electrode that metal boride or the covering of metal boron phosphorus compound is made.The catalysis electrode of the present invention can be used as electrolysis water hydrogen-precipitating electrode and analysis oxygen electrode at the same time, have the characteristics of overpotential is low, chemical stabilization, service life is long.The catalysis electrode preparation method process is simple, and reaction condition is gentle, and equipment requirement is low, and electro-catalysis functional membrane is fine and close, is firmly combined with matrix.This method is applicable not only to the preparation of efficient catalytic electrode, it can also be used to has assembled the upgrading of electrode, has had industrial utility value in fields such as water electrolysis, chemical industry for making chlorine and alkali liberations of hydrogen.
Description
Technical field
The invention belongs to electrochemical catalysis electrode technology field, and in particular to one kind be used for industrial high-efficient water electrolysis hydrogen production,
Electrode material of oxygen and preparation method thereof.
Background technology
Water electrolysis technology is that one kind extensively should in fields such as sewage disposal, sea water desalination, electrolysis chlor-alkali, hydrogen manufacturing, electro-catalysis
Technology, has consequence in modern industrial production.Wherein, chlorine industry is the pillar basic industry of country；
Water electrolysis hydrogen production is one of industrial technology of Production of High-purity Hydrogen, before having wide application in terms of structure cleans hydrogen energy source system
Scape.
One complete water electrolytic cell is mainly made of four parts：Solution, amberplex, cathode catalysis layer and sun
Pole Catalytic Layer.In order to improve the reaction speed of water electrolysis, respectively in cathode catalysis layer and anode catalyst layer coated cathode liberation of hydrogen
Reaction（HER）Catalysis material and Oxygen anodic evolution reaction（OER）Catalysis material.After external voltage is applied on electrode, basic reaction
It is the generation for having oxygen and hydrogen respectively on anode and cathode.In theory, it is only necessary to apply and be not less than 1.23 volts
External voltage can just water electrolysis reaction is smoothly occurred, but in actual industrial production, it is necessary to be applied more than thermodynamics
The potential that namely 1.23 volts of voltage can just promote water decomposition reaction to be smoothed out.The presence of the overpotential so that water electrolysis
During energy loss it is huge.Wherein, during water electrolysis hydrogen producing, liberation of hydrogen (HER) and analysis oxygen (OER) overpotential constitute about
The 1/3 of cell voltage, energy loss is huge.It is estimated that the voltage for the water electrolysis hydrogen producing gas equipment that China uses now is as can reduce
250mV, the energy value that can be saved every year will reach several hundred million yuans.Therefore the method that overpotential can effectively be reduced by finding has
Greatly production meaning.The research and development of novel electrode catalysis material are always the key of water electrolysis performance boost.
Following three classes can be divided into by being currently used for the element of manufacture electrode：1. noble metal electrode material (such as Pt, Ir, Ru
Deng), this is the electrode material of a kind of excellent performance, but these metal material reserves are limited, expensive, it is difficult to large-scale promotion
Use；2. non-noble metal alloy electrode, is mainly made of transition metal such as iron, cobalt, nickel, this kind of material is easily worked, and cost is fitted
In, apply, but overall performance is general；3. nonmetallic combination electrode, which contains the electrocatalysis material of high activity, mainly
It is made of the compound of the nonmetalloids such as oxygen, phosphorus, carbon, sulphur and transition metal, such material cost is relatively low, easily prepared, and
Portion of material performance is better than noble metal, has promotional value in actual production.Both at home and abroad in terms of such electrocatalysis material
Numerous studies are carried out, presently relevant research is still very active.Chinese invention patent 201210504498.6 is by the oxidation of cobalt, nickel
Thing loads to carbon base body surface, is prepared for combination electrode, greatly reduces the voltage needed for water electrolysis hydrogen producing, while be catalyzed moisture
Solution current efficiency is also improved.Chinese invention patent 201310320738.1 is cheap using cost of material, and synthesis cost is low
It is honest and clean, simple method is prepared, using nickel as matrix, by hydro-thermal reaction metal sulphide nickel, Ni/Ni has been made3S2/Ni(OH)2Multilayer
Combination electrode.The electrode has ultralow electrolysis water overpotential, high current density.Chinese invention patent 201510296779.0
By hydro-thermal reaction and self-assembling technique, cobaltosic oxide is deposited in nickel foam, and is wrapped up with graphene, is prepared for
It can be directly used for the combination electrode of three-dimensional analysis oxygen.Chinese invention patent 201610315618.6 uses Ni2P nanometer sheets, CoP receive
The transition metal phosphide such as rice noodles, NiCoP nano wires is substantially improved electro-catalysis H2-producing capacity, and point out as working electrode
Such material is the material of alternative noble metal catalyst.
Our research finds that metal boride is also the electrocatalysis material of a kind of excellent performance.This kind of chemical material
It can stablize, electric conductivity is good；In addition, this kind of material can also be used as cathode material and anode material at the same time, promote liberation of hydrogen and
Oxygen evolution reaction, the great application prospect in terms of water electrolysis catalyst electrode.The present invention will pre-process matrix using the method for chemical plating
Immerse in chemical plating fluid and react, metal boride or the catalysis electrode of metal boron phosphorus compound covering is made.The catalysis of the present invention
Electrode advantage is that the electrode can be used as electrolysis water hydrogen-precipitating electrode and analysis oxygen electrode at the same time, chemistry low with overpotential
The characteristics of stabilization, service life is long.In addition, catalysis electrode preparation method is simple, reaction condition is gentle, and equipment requirement is low, and electricity is urged
It is fine and close to change functional membrane, is firmly combined with matrix.This method cannot be only used for the preparation of efficient catalytic electrode, it can also be used to assemble
The upgrading of electrode, has industrial utility value in fields such as water electrolysis, chemical industry for making chlorine and alkali liberations of hydrogen.
The content of the invention
It is an object of the invention to provide a kind of water electrolysis is efficient, and with difunctional（Liberation of hydrogen and analysis oxygen）Catalysis electrode
And preparation method thereof.
Water electrolysis provided by the invention is efficient, and has difunctional catalysis electrode, by metal boride or metal boron phosphorus
Compound covers matrix and forms.Wherein, the metal in metal boride or metal boron phosphorus compound be selected from iron, cobalt, nickel, molybdenum,
One or more of mixtures in tungsten；Tenor 70-97% in metal boride, Boron contents 3-30%；Metal boron phosphatization
Tenor 60-95% in compound, Boron contents 3-30%, phosphorus content 2-20%, three's total amount meet 100%；Matrix refers to waiting to locate
Reason material or production line have electrode, its material matter is carbon steel, titanium, cobalt, nickel, stainless steel, copper or carbon etc..
Water electrolysis provided by the invention is efficient, and the preparation method with difunctional catalysis electrode, comprises the following steps that：
（1）Plating solution is prepared：By metal boride or metal boron phosphorus compound presoma, and reducing agent, complexing agent, buffer and
Water, is mixed by usage ratio, with obtained plating solution；
（2）Substrate pretreated：By matrix in clear water ultrasound 2-5 minutes, then with acetone, ethanol, deionized water clean remove table
Face spot, then matrix is immersed in acid solution activate, then is pre-processed with deionized water rinsing, completion；
（3）Chemical plating：By step（2）The middle matrix by pretreatment immerses step（1）It is anti-through chemical plating in the plating solution of middle preparation
Should, matrix is then taken out, with deionized water rinsing, re-dry, i.e. catalysis electrode needed for acquisition.
Step（1）In, the metal salt cation in chemical plating fluid is one or more of in iron, cobalt, nickel, molybdenum, tungsten
Mixture, anion are selected from Cl-, SO4 2-, NO3 -, PO3 3-, acetate, oxalate；Metal salt concentrations are in 5g/L-80g/L.Reduction
Agent is selected from boron hydride, hypophosphite.Wherein, boron hydride is selected from sodium borohydride, potassium borohydride, ammonia borine, amine borine
One or more of mixtures in compound；Ortho phosphorous acid salt cation is selected from ammonium, hydrogen, sodium, potassium, in magnesium, calcium, iron, cobalt, nickel
It is one or more of；Reductant concentration is in 1g/L-50g/L.Complexing agent is selected from the compound that can be coordinated with metal salt, mainly there is ammonia
Water, amine, sodium citrate, sodium acetate, sodium lactate, sodium malonate.Buffer is selected from sodium acetate, boric acid, ammonium chloride, sodium sulphate.
Step（2）In, one or more of the acid in hydrochloric acid, sulfuric acid, nitric acid, oxalic acid in pickle, sour volume
Concentration is 5-15%, acid liquor temperature 10-45oC, processing time are 2-15 minutes.
Step（3）In, electroless plating reaction temperature is 0-80oC, the reaction time for 15 minutes -12 it is small when.
Compared with existing electrode, catalysis electrode prepared by the present invention can be at the same time as electrolysis water hydrogen-precipitating electrode and analysis oxygen electrode
Use, and there is the characteristics of overpotential is low, and service life is long.
The catalysis electrode preparation method is simple, and reaction condition is gentle, and no particularization equipment requirement, cost is low, obtained electricity
Catalysis film is fine and close, and is firmly combined with matrix.This method is applicable not only to the preparation of efficient catalytic electrode, it can also be used to
The upgrading of electrode is assembled, there is the practical valency of industry in water electrolysis hydrogen production, the field such as oxygen processed, chlorine industry electrocatalytic hydrogen evolution
Value.
Brief description of the drawings
Fig. 1 is Co-B/Ni electrode photos.
Fig. 2 schemes for Co-B/Ni electrodes SEM.
Fig. 3 is Different electrodes electrolysis water Hydrogen Evolution Performance test result.
Fig. 4 is electrolysed elutriation oxygen the performance test results for Different electrodes.
Fig. 5 is Co-B-P/Ni electrode photos.
Fig. 6 schemes for Co-B-P/Ni electrodes SEM.
Fig. 7 is Ni-B/Ni electrode photos.
Fig. 8 is Ni-W-B/ carbon cloth electrode photos.
Embodiment
The present invention is further described below by specific embodiment.
Embodiment 1, the preparation of Co-B/Ni electrode catalytic materials
（1）Ni substrate pre-processes
Nickel sheet is positioned in acetone soln and is cleaned by ultrasonic 30 minutes, removes the grease of substrate surface, is then positioned over mole dense
Spend in the salpeter solution for 3 mol/L, soak 15 minutes, remove the oxide of Ni-based basal surface, finally with deionized water rinsing,
Place natural air drying；
（2）The chemical plating fluid containing Co-B is configured, the amount of each material is as shown in the table with when experiment condition：
Ni substrate will be pre-processed, will be immersed in above-mentioned solution, when chemical deposition 15 minutes -12 is small at 30 DEG C；It is different heavy to can obtain
The catalytic electrode material of product thickness, it is dry by deionized water rinsing, electrode is made.Electrode photo and SEM figures are as shown in Figure 1, Figure 2
It is shown；
（3）Electrochemistry liberation of hydrogen and analysis oxygen performance detection；
It is electric using the Co-B/Ni of above-mentioned preparation as work using the KOH of 1 mol/L as electrolyte solution using three-electrode system
Pole, using graphite carbon rod as to electrode, using saturation mercury/mercury oxide as reference electrode, 25 DEG C of room temperature in electrochemical workstation
In the environment of, carry out evolving hydrogen reaction（HER）And oxygen evolution reaction（OER）Test.The material and Pt/C（20%wt%）, IrO2Survey
Test result is as shown in Figure 3, Figure 4.
Embodiment 2, the preparation of Co-B-P/Ni electrode catalytic materials
（1）Ni substrate pre-processes
Nickel sheet is positioned in acetone soln and is cleaned by ultrasonic 30 minutes, removes the grease of substrate surface, is then positioned over mole dense
Spend in the salpeter solution for 3mol/L, soak 5 minutes, remove the oxide of Ni-based basal surface, finally with deionized water rinsing, put
Put natural air drying；
（2）Configure the chemical plating fluid containing Co-B-P, each material it is as shown in the table with when experiment condition：
Ni substrate will be pre-processed, will be immersed in above-mentioned solution, when chemical deposition 15 minutes -12 is small at 30 DEG C；It is different heavy to can obtain
The catalytic electrode material of product thickness, it is dry by deionized water rinsing, electrode is made.Electrode photo and SEM figure such as Fig. 5, Fig. 6
It is shown；
（3）Electrochemistry liberation of hydrogen and analysis oxygen performance detection；
Using three-electrode system, using the KOH of 1 mol/L as electrolyte solution, work is used as using the Co-B-P/Ni of above-mentioned preparation
Electrode, using graphite carbon rod as to electrode, using saturation mercury/mercury oxide as reference electrode, 25 DEG C in electrochemical workstation
Under environment, evolving hydrogen reaction is carried out（HER）And oxygen evolution reaction（OER）Test, its test result is as shown in Fig. 3, Fig. 4.
It is prepared by embodiment 3, Ni-B/Ti electrodes
（1）Titanium base pre-processes
Titanium sheet substrate is positioned in acetone soln and is cleaned by ultrasonic 10 minutes, the grease of substrate surface is removed, is then positioned over and rubs
Your concentration is in the salpeter solution of 3mol/L, is soaked 15 minutes, removes the oxide of titanium-based basal surface, finally uses deionized water
Rinse, place natural air drying；
（2）Configure the chemical plating fluid containing Ni-B, its each material with when experiment condition as shown in figure following table：
Pre-processing titanium matrix is immersed in above-mentioned solution, when chemical deposition 15 minutes -12 is small at 30 DEG C；It is different heavy to can obtain
The catalytic electrode material of product thickness, it is dry by deionized water rinsing, electrode is made.Electrode photo is as shown in Figure 7；
（3）The electrochemistry liberation of hydrogen of Ni-B/Ti electrode slices, analysis oxygen performance detection
It is electric using the Ni-B/Ti of above-mentioned preparation as work using the KOH of 1 mol/L as electrolyte solution using three-electrode system
Pole, using graphite carbon rod as to electrode, using saturation mercury/mercury oxide as reference electrode, 25 DEG C of the ring in electrochemical workstation
Under border, evolving hydrogen reaction is carried out（HER）And oxygen evolution reaction（OER）Test, its test result is as shown in table 1.
It is prepared by embodiment 4, Ni-W-B/ carbon cloth electrodes
（1）Carbon cloth substrate pretreatment
Carbon cloth is positioned over ultrasound 30 minutes in acetone soln, removes the grease of substrate surface, being then positioned over mass concentration is
In 65% concentrated nitric acid solution, 6h is soaked at 90 DEG C, finally with deionized water rinsing, drying；
（2）Configure the chemical plating fluid containing Ni-W-B, its each material it is as shown in the table with when experiment condition：
Carbon cloth will be pre-processed, will be immersed in above-mentioned solution, when chemical deposition 15 minutes -12 is small at 30 DEG C；Available not synsedimentary
The catalytic electrode material of thickness, it is dry by deionized water rinsing, electrode is made.Electrode photo is as shown in Figure 8；
（3）The electrochemistry liberation of hydrogen and analysis oxygen performance detection of Ni-W-B/ carbon cloth electrodes；
Using three-electrode system, using the KOH of 1 mol/L as electrolyte solution, work is used as using the Ni-W-B/ carbon cloths of above-mentioned preparation
Make electrode, using graphite carbon rod as to electrode, using saturation mercury/mercury oxide as reference electrode, 25 DEG C in electrochemical workstation
In the environment of, carry out evolving hydrogen reaction（HER）And oxygen evolution reaction（OER）Test, its test result are as shown in table 1.
It is prepared by embodiment 5, Ni-B-P/ carbon cloth electrodes
（1）Carbon cloth substrate pretreatment
Carbon cloth is positioned over ultrasound 30 minutes in acetone soln, removes the grease of substrate surface, being then positioned over mass concentration is
In 65% concentrated nitric acid solution, 6h is soaked at 90 DEG C, finally with deionized water rinsing, drying；
（2）The chemical plating fluid containing Ni-B-P is configured, its each material see the table below with when experiment condition：
Carbon cloth will be pre-processed, will be immersed in above-mentioned solution, when chemical deposition 15 minutes -12 is small at 30 DEG C；Available not synsedimentary
The catalytic electrode material of thickness, it is dry by deionized water rinsing, electrode is made；
（3）The electrochemistry liberation of hydrogen and analysis oxygen performance detection of Ni-B-P/ carbon cloth electrodes；
Using three-electrode system, using the KOH of 1 mol/L as electrolyte solution, work is used as using the Ni-B-P/ carbon cloths of above-mentioned preparation
Make electrode, using graphite carbon rod as to electrode, using saturation mercury/mercury oxide as reference electrode, the room temperature in electrochemical workstation
In the environment of 25 DEG C, evolving hydrogen reaction is carried out（HER）And oxygen evolution reaction（OER）Test, its test result is shown in Table 1.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention principle it
Interior, any modification, equivalent replacement, improvement and so on, should be included within the scope of the present invention.
Table 1:Ni-B/Ti, Ni-B-P/ carbon cloth electrode electrolysis water overpotential list
Note：HER：Evolving hydrogen reaction；OER：Oxygen evolution reaction；J：Current density.
Claims (5)
1. a kind of water electrolysis is efficient, double-function catalyzing electrode, it is characterised in that is covered by metal boride or metal boron phosphorus compound
Lid matrix and form；Wherein, the metal in metal boride or metal boron phosphorus compound in iron, cobalt, nickel, molybdenum, tungsten one
Kind or several mixtures；Tenor 70-97% in metal boride, Boron contents 3-30%；It is golden in metal boron phosphorus compound
Belong to content 60-95%, Boron contents 3-30%, phosphorus content 2-20%, three's total amount meets 100%；Matrix refer to pending material or
Production line has electrode, its material is carbon steel, titanium, cobalt, nickel, stainless steel, copper or carbon.
2. a kind of water electrolysis as claimed in claim 1 is efficient, the preparation method of double-function catalyzing electrode, it is characterised in that tool
Body step is as follows：
（1）Plating solution is prepared：By metal boride or metal boron phosphorus compound presoma, and reducing agent, complexing agent, buffer and
Water, is mixed by usage ratio, with obtained plating solution；
（2）Substrate pretreated：By matrix in clear water ultrasound 2-5 minutes, then with acetone, ethanol, deionized water clean remove table
Face spot, then matrix is immersed in acid solution activate, then is pre-processed with deionized water rinsing, completion；
（3）Chemical plating：By step（2）The middle matrix by pretreatment immerses step（1）It is anti-through chemical plating in the plating solution of middle preparation
Should, matrix is then taken out, with deionized water rinsing, re-dry, i.e. catalysis electrode needed for acquisition.
3. according to preparation method as claimed in claim 2, it is characterised in that step（1）In, the metal salt sun in chemical plating fluid
One or more of mixtures of the ion in iron, cobalt, nickel, molybdenum, tungsten, anion are selected from Cl-, SO4 2-, NO3 -, PO3 3-, acetic acid
Root, oxalate；Metal salt concentrations are in 5g/L-80g/L；Reducing agent is selected from boron hydride, hypophosphite；Wherein, boron hydride
Selected from sodium borohydride, potassium borohydride, ammonia borine, one or more of mixtures in amine borine compound；Hypophosphite sun
Ion is selected from ammonium, hydrogen, sodium, potassium, the one or more in magnesium, calcium, iron, cobalt, nickel；Reductant concentration is in 1g/L-50g/L；Complexing
Agent is the compound that can be coordinated with metal salt, selected from ammonium hydroxide, amine, sodium citrate, sodium acetate, sodium lactate, sodium malonate；Buffer
Selected from sodium acetate, boric acid, ammonium chloride, sodium sulphate.
4. according to preparation method as claimed in claim 2, it is characterised in that step（2）In, the acid in pickle is selected from salt
One or more in acid, sulfuric acid, nitric acid, oxalic acid, sour volumetric concentration are 5-15%, acid liquor temperature 10-45oC, during processing
Between be 2-15 minutes.
5. according to preparation method as claimed in claim 2, it is characterised in that step（3）In, electroless plating reaction temperature is 0-
80oC, the reaction time for 15 minutes -12 it is small when.
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| CN108624907A (en) * | 2018-04-26 | 2018-10-09 | 复旦大学 | Nonmetal basal body efficient catalytic electrode and preparation method thereof |
| CN109518217A (en) * | 2018-11-23 | 2019-03-26 | 济南大学 | A kind of preparation method of the Ni-based oxygen-separating catalyst of boronation |
| CN110104737A (en) * | 2019-05-15 | 2019-08-09 | 广东工业大学 | A kind of novel lead dioxide electrode preparation method and application with electrocatalytic oxidation property |
| CN111809196A (en) * | 2020-06-23 | 2020-10-23 | 复旦大学 | Hollow foam autocatalytic electrode and preparation method thereof |
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| CN111957323A (en) * | 2020-08-21 | 2020-11-20 | 中国地质大学（武汉） | Boron-doped core-shell structure catalyst and preparation method and application thereof |
| CN113249747A (en) * | 2021-04-12 | 2021-08-13 | 上海理工大学 | Chemical plating method for preparing metal sulfide by efficiently electrolyzing water to prepare hydrogen |
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| CN113684493A (en) * | 2021-08-20 | 2021-11-23 | 中国科学院过程工程研究所 | Method for preparing efficient electrolytic water hydrogen evolution catalyst by chemical plating method |
| US20210376332A1 (en) * | 2020-05-29 | 2021-12-02 | 2706649 Ontario Ltd | Active element for an electrochemical apparatus |
| CN114032575A (en) * | 2021-11-05 | 2022-02-11 | 上海理工大学 | Preparation method of polymer composite boron-based transition metal catalytic electrode and boron-based polymer |
| CN114214654A (en) * | 2021-12-10 | 2022-03-22 | 清华大学 | System device and method for preparing electrolytic water electrode by solution method |
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