CN108193227A - Oxygen electrode and its preparation and application are analysed in the electro-catalysis of nickel-ferric spinel base - Google Patents

Oxygen electrode and its preparation and application are analysed in the electro-catalysis of nickel-ferric spinel base Download PDF

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CN108193227A
CN108193227A CN201611122593.4A CN201611122593A CN108193227A CN 108193227 A CN108193227 A CN 108193227A CN 201611122593 A CN201611122593 A CN 201611122593A CN 108193227 A CN108193227 A CN 108193227A
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nickel
electrode
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catalysis
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黄延强
王发楠
何杨华
徐金铭
张涛
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Dalian Institute of Chemical Physics of CAS
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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
    • 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
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • 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
    • C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
    • C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
    • C25B11/031—Porous electrodes
    • 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
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention belongs to materials science field and electro-catalysis hydrogen producing technology fields, and in particular to a kind of nickel-ferric spinel base electro catalytic electrode and its preparation available for electrolysis water oxygen evolution reaction in alkaline medium.For the electrode system using nickel-ferric spinel structure as catalytic active center, nickel foam is electrode material.It efficiently electrolysis water can prepare oxygen in alkaline medium, and the entirety electricity excessively for greatly reducing electrolysis water is thrown, and show good stability.Its preparation process grows nickel-ferric spinel composite construction by electrodeposition process in situ in foam nickel base, required raw material sources are extensive, cheap, technical maturity is stable, simple and efficient to handle, controllability is strong, process is nontoxic, is reacted suitable for large-scale production and industrial electrolysis water.

Description

Oxygen electrode and its preparation and application are analysed in the electro-catalysis of nickel-ferric spinel base
Technical field
The invention belongs to materials science field and electro-catalysis hydrogen producing technology fields, and in particular to one kind is in alkaline medium The nickel-ferric spinel base electro-catalysis analysis oxygen electrode of middle high-efficient electrolytic water hydrogen manufacturing and its preparation.
Background technology
Hydrogen is a kind of important clean energy resource, it is considered to be hopeful substitute fossil energy novel energy, always with Come by mondial extensive concern.In recent years, it is continuous with the continuous development of new-generation technology and network system Optimization and upgrading, the advantage of water electrolysis hydrogen production technology are further magnified or even are described as extensively " optimal industrial hydrogen production side Method ".However in electro-catalysis water splitting processes, the dynamics of oxygen evolution reaction hinders seriously to restrict the raising of water decomposition efficiency. At present, the metal oxide containing precious metals such as iridium, ruthenium, platinum are acknowledged as most efficient and analysis oxygen elctro-catalyst, but noble metal is high Price and low amount of storage limit the length of extensive use and electrolysis hydrogen producing process of such catalyst in electrolysis water oxygen Foot development.Therefore efficient, stable, environmental-friendly and cheap elctro-catalyst is found to replace the pass that noble metal is development electrolysis water Key.
It recent studies have shown that, stratiform transition metal oxide or hydroxide show higher in electro-catalysis oxygen making reaction Activity and stabill.Hydrotalcite is the lamellar compound formed by interlayer anion and positively charged laminate ordered fabrication, Middle main layer board shares seamed edge by divalent transition metal oxide octahedron and forms.Divalent metal positioned at laminate can be The interior trivalent metal cation same order elements similar in ionic radius of certain proportional region, so as to make main board layer band part just Charge；Positive charge between object anion and laminate that interlayer can exchange balances each other, and it is in electroneutral to make hydrotalcite overall structure. In numerous hydrotalcite structures, nickel-ferric spinel and its derivative that nickelous is formed with ferric iron have high electrolysis elutriation Oxygen activity, it is considered to be the elctro-catalyst of most possible substitution noble metal.However, the synthesis side of this kind of material reported at this stage Method prepared by method and electrode has limitation, such as uses solvent-thermal method, high-temperature exercise method synthetic method, complex process, Energy consumption is big, environment is unfriendly etc.；In addition it is typically to load the elctro-catalyst prepared by the methods of spin coating, spraying, drop coating Onto two-dimentional substrate, need additional adhesives, catalyst electrode surface combine loosely, loose contact, dispersion it is uneven, lead to electricity The problems such as lotus transmission is obstructed and easily comes off, has seriously affected final catalytic activity and the service life of electrode.
Invention content
An object of the present invention is to provide one kind The electro-catalysis analysis oxygen electrode in activated centre.The electro catalytic electrode raw material sources are extensive, of low cost, shown in alkaline medium Very high catalytic activity and long-term structure and chemical stability are applicable to industrial electrolysis water oxygen.
The second object of the present invention is to provide a kind of nickel-ferric spinel base electro-catalysis for preparing high-efficient electrolytic water oxygen to analyse oxygen The method of electrode.The clear novelty of this method mentality of designing, technical maturity is stable, simple and efficient to handle, controllability is strong, suitable for big Large-scale production.
The preparation method of nickel-ferric spinel base electrocatalytic hydrogen evolution electrode provided by the invention, concrete operations are as follows：
1st, the pretreatment of nickel foam：Ultrasound is repeated in ultra-pure water ultrasound and at least with degreasing degreasing in acetone or alcohol Twice with cleaning, ultrasound acidification activation 1~20 minute in the hydrochloric acid of 1~2mol/L, finally again ultrasonic 1~20 in ultra-pure water Minute and be at least repeated twice.
2nd, the preparation of electrolyte：Ni-based soluble-salt and iron-based soluble-salt are directly dissolved in ultra-pure water.Ferronickel member The sum of plain molar concentration is 0.1mmol/L~1mol/L, and wherein ferro element molar content is 10%~80%.
3rd, the assembling of standard three electrode system：Using the foam nickel electrode handled in step (1) as working electrode and to electrode, Saturated calomel electrode is reference electrode, using prepared solution in step (2) as electrolyte, is assembled into three electrode bodies of standard System.
4th, electro-deposition：The three-electrode system assembled in step (3) is connected to electrochemical workstation, will be passed through in electrolyte Inert gas keeps flow to take out working electrode after 5~100mL/min, 10~600s of constant potential or constant current electro-deposition, Excess electrolyte is cleaned up with ultra-pure water, is dried at room temperature, obtains the electro-catalysis moisture parsing oxygen electrode.
Preferably, in step (2) Ni-based soluble-salt be nickel chloride, nickel nitrate, one or more of nickel sulfate, iron-based Soluble-salt is one or more of frerrous chloride, ferrous sulfate.
Preferably, the constant potential electro-deposition current potential of step (4) is relative to saturated calomel electrode -1~-2V, constant current electricity Deposition current is in -0.01~-0.1A/cm2。
The present invention technical principle be：With the close bivalent nickel ion of ionic radius and electro-deposition current potential and ferrous iron from Son is electro-deposition presoma, under conditions of constant potential or constant current, can in foam nickel base homoepitaxial Elemental redistribution The uniform nickel iron hydroxide film of shape from level to level.With aerial drying process, the ferrous ion on film is gradual Oxidation by air is ferric ion, and makes the body layer band part positive charge of script.At this point, had more to balance this part Positive charge, the carbon dioxide in air enter interlayer and generate carbonyl, and local laminate is strutted with hydroxyl reaction, make originally smooth Two-dimensional layered structure on growth in situ go out many small laminates straggly, form three-dimensional structure.It is this due to divalent metal original The hydrotalcite structure that position aoxidizes and is formed in situ, has special three-layer laminated structure, substantially increases the effective of catalyst Active surface area；In-situ oxidation process only carries out on the laminate of catalysis material simultaneously, remain oxidation procatalyst film with It the good contact of substrate and combines closely, makes the catalysis electrode that there is fabulous electrochemical stability and reaction service life.
The present invention has the advantages that compared with prior art：
1. the present invention grows nickel-ferric spinel layer structure electricity using electro-deposition method in situ directly in foam nickel base Catalyst.This method raw material sources are extensive, cheap, and technical maturity, simple and quick, it is only necessary to more than ten seconds to ten minutes Preparation time, process control, be suitble to large-scale industrial production.
2. the present invention forms the three-layer laminated structure of nickel-ferric spinel using divalent metal in-situ oxidation, which possesses Great electrochemical active surface considerably increases the oxygen evolution activity of the elctro-catalyst, noble metal promoted alkalinity can be replaced to be situated between The development of aqueous systems is electrolysed in matter.
3. the present invention utilizes growth in situ of the elctro-catalyst in foam nickel base, without outer adding additives, electrode and base Bottom good contact is simultaneously combined closely, and ensure that charge transfer efficiency, while substantially increases the stable structure of the electro catalytic electrode Property.
Description of the drawings
Fig. 1 is the X-ray diffraction spectrum (a) of nickel-ferric spinel and infrared spectrum (b) prepared by electrodeposition process in situ；
The transmission electron microscope picture (a) of nickel-ferric spinel prepared by Fig. 2 original positions electrodeposition process and (b) and x-ray photoelectron energy It composes (c) and (d)；
Fig. 3 is the optical photograph (a) of fresh nickel-ferric spinel catalysis electrode prepared by electrodeposition process in situ and scanning electricity Mirror figure (b) and the electrode dry optical photograph (c) and scanning electron microscope (SEM) photograph (d) after oxidation in air；
Fig. 4 is the active testing of nickel-ferric spinel catalysis electrode；
Fig. 5 is the stability test of nickel-ferric spinel catalysis electrode.
Specific embodiment
Below by specific embodiment, the present invention is described in detail, but these embodiments are not to present disclosure It is construed as limiting.
Embodiment 1
A kind of preparation method of nickel-ferric spinel base electro-catalysis analysis oxygen electrode, follows the steps below.
(1) it is nickel foam is 10 minutes ultrasonic in acetone, it is cleaned, and be repeated twice within 10 minutes in ultra-pure water ultrasound, Ultrasound 10 minutes in the hydrochloric acid of 1mol/L, finally ultrasound is cleaned, and be repeated twice for 10 minutes in ultra-pure water again.
(2) preparation of electrolyte：Nickel nitrate and ferrous sulfate are directly dissolved in ultra-pure water.Ferro-nickel element molar concentration The sum of for 50mmol/L, wherein ferro element molar content is 25%.
(3) using the foam nickel electrode handled in step (1) as working electrode and to electrode, saturated calomel electrode is reference electricity Pole using prepared solution in step (2) as electrolyte, is assembled into the three-electrode system of standard.
(4) three-electrode system assembled in step (3) is connected to electrochemical workstation, nitrogen will be passed through in electrolyte, Flow is kept in 20mL/min, the constant potential electro-deposition 300s under relative to the electrode potential that saturated calomel electrode is -1.241V Afterwards, working electrode is taken out, excess electrolyte is cleaned up with ultra-pure water, is dried at room temperature, obtains the electro-catalysis moisture Parse oxygen electrode.
Fig. 1 (a) is the catalyst being made according to the constant potential electro-deposition method in situ of embodiment 1 after air drying XRD diagram, by comparing standard spectrogram, it can be deduced that the catalyst is the nickel-ferric spinel layer structure of carbonate intercalation.This is urged The infrared spectrum (Fig. 1 (b)) of agent also further demonstrates the nickel-ferric spinel layer structure of its carbonate intercalation.Fig. 2's (a) Transmission electron microscope picture can be seen that apparent layer structure.The x-ray photoelectron spectroscopy of Fig. 2 (b) demonstrates the catalyst by divalent Nickel and ferric iron composition, it is believed that be oxidation by air during the ferrous iron added in preparation process is dried at room temperature for Into ferric iron.Fig. 3 (a) is the optical photograph of fresh catalyst electrode just prepared of method according to embodiment 1, can be with The catalyst electrode is found out in green, and the corresponding scanning electron microscope (SEM) photograph of the electrode (Fig. 3 (b)) shows that catalyst is more smooth for surface Lamellar structure composition.After catalyst electrode dries a period of time in air, as optical photograph shows the electricity in Fig. 3 (c) Pole color significantly becomes yellow, and corresponding scanning electron microscope (SEM) photograph (Fig. 3 (d)) shows that the smooth sheet surfaces of catalyst are grown perhaps Mostly small lamella, the two-dimensional structure of script become three-dimensional structure.
The electrochemical property test of nickel-ferric spinel base electro-catalysis analysis oxygen electrode obtained carries out by the following method：
(1) using three-electrode system, working electrode 1cm2The compound carbonitride foam nickel electrode of molybdenum nickel, be to electrode Platinum plate electrode, reference electrode are saturated calomel electrode.Electro-chemical test is enterprising in strong (Solarton) electrochemical workstation of defeated power Row, electrolyte are the potassium hydroxide solution of 0.1mol/L or 1mol/L, and test process is passed through high pure nitrogen and carries out saturated process, surveys It is 25 DEG C to try temperature control.
(2) linear sweep voltammetry curve is tested：Sweep speed is 1mV/s, and electrode potential carries out iR corrections, and is converted into Relative to the electrode potential of reversible hydrogen electrode (RHE), calculation formula is：Overpotential=electrode potential+0.059 × pH+ 0.2415-iR-1.23(V)。
(3) stability test is divided into two programs：Sweeping for potential-time graph is carried out first under the program of current step It retouches, current density is from 50mA/cm2To 500mA/cm2Variation, each 50mA/cm primary per 600s steps2；Secondly without Under conditions of any processing, it is subject to 50mA/cm on identical electrode2Current density, it is small that 5 are carried out to potential-time graph Current density is then directly adjusted to 100mA/cm by Shi Jilu2, then 5 hour records are carried out to potential-time graph, then Current density is adjusted to 200mA/cm again2, 5 hour records are carried out to potential-time graph.
As shown in figure 4, the electro catalytic electrode shows high oxygen evolution activity in alkaline medium, in the electricity of 0.1mol/L It solves in liquid, current density is in 50mA/cm2、100mA/cm2And 200mA/cm2Under, overpotential be respectively 280mV, 310mV and 370mV；In the electrolyte of 1mol/L, current density is in 50mA/cm2、100mA/cm2And 200mA/cm2Under, overpotential difference For 250mV, 260mV and 280mV.The oxygen evolution reaction overpotential of the catalyst is showed well below other catalyst are reported at present Go out high catalytic activity.
As shown in Fig. 5 (a) and (c), under the current density of variation, which shows in the electrolyte of various concentration Go out the stability of good anti-current fluctuation, in 500mA/cm2Current density under still show well activity and stability. Fig. 5 (b) and (d) show that under constant high current, violent gas sparging, which also shows outstanding anti-machine Tool disturbs ability and very long catalytic life.
Embodiment 2
A kind of preparation method of nickel-ferric spinel base electro-catalysis analysis oxygen electrode, follows the steps below.
(5) it is nickel foam is 10 minutes ultrasonic in acetone, it is cleaned, and be repeated twice within 10 minutes in ultra-pure water ultrasound, Ultrasound 10 minutes in the hydrochloric acid of 1mol/L, finally ultrasound is cleaned, and be repeated twice for 10 minutes in ultra-pure water again.
(6) preparation of electrolyte：Nickel nitrate and ferrous sulfate are directly dissolved in ultra-pure water.Ferro-nickel element molar concentration The sum of for 50mmol/L, wherein ferro element molar content is 25%.
(7) using the foam nickel electrode handled in step (1) as working electrode and to electrode, saturated calomel electrode is reference electricity Pole using prepared solution in step (2) as electrolyte, is assembled into the three-electrode system of standard.
(8) three-electrode system assembled in step (3) is connected to electrochemical workstation, nitrogen will be passed through in electrolyte, Flow is kept in 20mL/min, in -0.05A/cm2Current density under after constant current electro-deposition 300s, take out working electrode, use Ultra-pure water cleans up excess electrolyte, dries at room temperature, obtains the electro-catalysis moisture parsing oxygen electrode.
The electrochemical property test of nickel-ferric spinel base electro-catalysis obtained analysis oxygen electrode press with the method in embodiment 1 into Row.
The electro catalytic electrode is in the electrolyte of 0.1mol/L, and current density is in 50mA/cm2、100mA/cm2And 200mA/ cm2Under, overpotential is respectively 250mV, 290mV and 350mV；In the electrolyte of 1mol/L, current density is in 50mA/cm2、 100mA/cm2And 200mA/cm2Under, overpotential is respectively 230mV, 250mV and 270mV.
In conclusion the method for the original position electro-deposition is under conditions of constant potential or constant current, it can be in foam nickel base Homoepitaxial stratiform nickel-ferric spinel film.Due to divalent metal in-situ oxidation, it has been formed in situ with special three-layer laminated Hydrotalcite structure substantially increases the effective active surface area of catalyst；In-situ oxidation process is only in catalysis material simultaneously It carries out, remain the good contact of oxidation procatalyst film and substrate and combines closely on laminate, there is the catalysis electrode Fabulous electrochemical stability and reaction service life.
The above is only the basic explanation under present inventive concept, and any made by technical solution according to the present invention Equivalent transformation is within the scope of protection of the invention.

Claims (7)

1. oxygen electrode is analysed in a kind of nickel-ferric spinel base electro-catalysis, which is characterized in that the catalyst activity component is nickel-ferric spinel, Its electrode basement is nickel foam；Nickel-ferric spinel compound structure film is grown in foam nickel base by electrodeposition process in situ.
A kind of 2. nickel-ferric spinel base electro-catalysis analysis oxygen electrode as described in claim 1, which is characterized in that the electrode basement For the three-dimensional porous foams nickel of purity 99.99%, porosity is 90~98%.
A kind of 3. preparation method of the nickel-ferric spinel base electro-catalysis analysis oxygen electrode described in claims 1 or 2, it is characterised in that system Standby step is as follows：
(1) pretreatment of nickel foam：Ultrasound is repeated twice in ultra-pure water ultrasound and at least with degreasing degreasing in acetone or alcohol With cleaning, ultrasound acidification activation 1~20 minute in the hydrochloric acid of 1~2mol/L is finally 1~20 minute ultrasonic in ultra-pure water again And it is at least repeated twice；
(2) preparation of electrolyte：Ni-based soluble-salt and iron-based soluble-salt are directly dissolved in ultra-pure water；Ferro-nickel element is rubbed The sum of your concentration is 0.1mmol/L~1mol/L, and wherein ferro element molar content is 10%~80%；
(3) assembling of standard three electrode system：Using the foam nickel electrode handled in step (1) as working electrode and to electrode, satisfy It is reference electrode with calomel electrode, using prepared solution in step (2) as electrolyte, is assembled into the three-electrode system of standard；
(4) electro-deposition in situ：The three-electrode system assembled in step (3) is connected to electrochemical workstation, will be led in electrolyte Enter inert gas, keep flow after 5~100mL/min, 10~600s of constant potential or constant current electro-deposition, take out work electricity Excess electrolyte with ultra-pure water is cleaned up, dried at room temperature by pole, obtains the electro-catalysis moisture parsing oxygen electrode.
4. preparation method according to claim 3, it is characterised in that：Ni-based soluble-salt is nickel chloride, nitre in step (2) One or more of sour nickel, nickel sulfate, iron-based soluble-salt is frerrous chloride, ferrous nitrate, ferrous sulfate, iron chloride, nitre One or more of sour iron, ferric sulfate.
5. preparation method according to claim 3, it is characterised in that：The constant potential electro-deposition current potential of step (4) is opposite In saturated calomel electrode -1~-2V, constant current electro-deposition electric current is in -0.01~-0.1A/cm2。
A kind of 6. application of the compound carbonitride electrocatalytic hydrogen evolution electrode of molybdenum nickel described in claim 1, which is characterized in that the electricity Catalytic hydrogen evolution electrode can be used as anode electrolysis water decomposition oxygen in alkaline medium.
7. according to the application described in claim 6, which is characterized in that alkaline medium is in potassium hydroxide or sodium hydroxide solution One or more, a concentration of 0.1~10mol/L.
CN201611122593.4A 2016-12-08 2016-12-08 Oxygen electrode and its preparation and application are analysed in the electro-catalysis of nickel-ferric spinel base Pending CN108193227A (en)

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