CN105977467A - Preparation method for preparing Co3O4@CoP composite electrode based on MOF template - Google Patents

Preparation method for preparing Co3O4@CoP composite electrode based on MOF template Download PDF

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CN105977467A
CN105977467A CN201610515711.1A CN201610515711A CN105977467A CN 105977467 A CN105977467 A CN 105977467A CN 201610515711 A CN201610515711 A CN 201610515711A CN 105977467 A CN105977467 A CN 105977467A
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cop
porous
electrode
zif
combination electrode
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李建荣
周健
豆义波
赵敏坚
谢亚勃
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Beijing University of Technology
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Beijing University of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5805—Phosphides
    • 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
    • Y02E60/10—Energy storage using batteries

Abstract

The invention provides a preparation method for preparing a Co3O4@CoP composite electrode based on an MOF template and belongs to the technical field of energy conversion. The preparation method comprises the following steps: uniformly growing Co(CO3)0.5OH 0.11H2O on a nickel plate substrate by virtue of simple hydrothermal reaction, and further growing favorable-appearance ZIF-67 in situ on the surface of Co(CO3)0.5OH 0.11H2O, thereby obtaining a Co(CO3)0.5OH 0.11H2O@ZIF-67 composite material; and furthermore, performing bonderizing so as to obtain Co3O4@CoP derivates. Compared with a single Co(CO3)0.5OH 0.11H2O electrode, the derivate electrode material has relatively low oxygen evolution potential and relatively high corresponding current density under same electric potential, and can be applied to the fields of hydrogen production based on electrocatalysis and decomposition of water and conversion of new energy resources such as fuel cells.

Description

One prepares Co based on MOF template3O4The preparation method of@CoP combination electrode
Technical field
The invention belongs to the technical field of electrochemical energy storage and conversion, technology relates to metal-oxide and zeolite miaow Azoles ester frame structure material (ZIFs) composite and the preparation method of derivant thereof, be based particularly on nickel sheet base The cobalt base oxide nano-array of basal surface modifies growth ZIF and the Co constructed thereof3O4@ZIF derivant electrode Construct.
Background technology
Along with people to the exhaustive exploitation of fossil energy (coal, oil, natural gas) and constantly consume, cause Energy crisis and thing followed environmental pollution attract attention, and the most in recent years, day is increasingly Acute haze environmental problem has beaten alarm bell to the mankind especially.Therefore exploitation substitutes the novel energy-storing of fossil energy And required electrode material becomes one of widely studied focus of people.Hydrogen energy source is considered as a kind of excellent Good energy storage and conversion carrier, because of its have that energy density is high, reusable edible and green friendly etc. excellent Point.The following exploitation economic for " Hydrogen Energy " is one of emphasis of Future New Energy Source development.We may utilize The electric energy excessively that generation of electricity by new energy produces is electrolysed water and prepares hydrogen, and prepared hydrogen can be as Gas Energy Source Directly burning heat production stores and utilizes, it is possible to is converted into electric energy as the fuel recirculation in fuel cell and carries out profit With.
Zeolite imidazole ester frame structure material (ZIFs) is by metal ion or metal cluster and imidazoles or imidazoles The framing structure that derivant is coordinated and is formed, it is similar to that common zeolite molecular sieve.This series compound Structure there is multiformity, pore volume can be in harmonious proportion duct can the advantage such as functionalization.And have the most thermally-stabilised Property and chemical stability.In recent years, the electrode that prepared by ZIFs (such as ZIF-8 and ZIF-67 etc.) and derivant Material is gradually applied to electrochemical energy storage field, such as lithium-sky battery, fuel cell and solaode etc.. But, such material is generally modified at electrode surface with the form of powder body, and the interface binding power of its difference makes The electrode material electrochemical stability obtained eventually is poor, has adverse effect its actual application.Therefore, as What is constructed has the ZIFs of rock-steady structure and derivant electrode material still suffers from many problems.
Summary of the invention
Object of the present invention is to provide a kind of multistage knot at nickel sheet substrate grown basic cobaltous carbonate@ZIF Structure, carries out derivation process to multilevel hierarchy simultaneously and obtains porous C o3O4@CoP club shaped structure array, Co3O4The cross section of@CoP club shaped structure is polygon.
The Co of the present invention3O4The preparation method of@CoP combination electrode, by hydro-thermal reaction in nickel/platinized platinum substrate Upper homoepitaxial Co (CO3)0.5OH·0.11H2O thin film, and then at Co (CO3)0.5OH·0.11H2O surface is former The ZIF-67 of position growth crystal form, constructs and obtains Co (CO3)0.5OH·0.11H2O@ZIF-67 composite, finally Bonderizing obtains the Co of loose structure3O4@CoP electrode.
Present disclosure is broadly divided into three steps: the first step is to be grown by hydro-thermal reaction in nickel sheet substrate Co(CO3)0.5OH·0.11H2O array；Second step is at Co (CO3)0.5OH·0.11H2O array surface is further Growth ZIF-67 thin film；3rd step is by Co (CO3)0.5OH·0.11H2O@ZIF-67 multilevel hierarchy bonderizing Finally give Co3O4@CoP combination electrode.
The synthetic method of the above-mentioned composite of the present invention, comprises the following steps:
The nickel sheet (length, width and height=2cm × 1cm × 0.1cm) cleaned is immersed solution A, hydro-thermal reaction system by the first step Obtain Co (CO3)0.5OH·0.11H2O electrode, wherein solution A cabaltous nitrate hexahydrate and carbamide are dissolved in deionized water The solution obtained, preferably every 5mmol cabaltous nitrate hexahydrate correspondence 20-30mmol carbamide, 20-80ml go from Sub-water；The most every 5mmol cabaltous nitrate hexahydrate correspondence 25mmol carbamide, 50ml deionized water； Its hydrothermal reaction condition is 90 DEG C-110 DEG C, preferably 90 DEG C, constant temperature 8-12 hour, preferably 10 hours.
Second step is by Co (CO3)0.5OH·0.11H2O electrode immersion mother solution B carries out reaction obtain Co(CO3)0.5OH·0.11H2O@ZIF-67 combination electrode；Mother solution B is 2-methylimidazole, deionized water and three The mixed liquor of ethamine, preferably every 1-3g2-Methylimidazole. correspondence 10ml deionized water and three second of 0.5-1.5ml Amine, reaction temperature keeps 50-75 DEG C, preferably 70 DEG C, 0.5-3 hour time, preferably 1 hour.
3rd step is by Co (CO3)0.5OH·0.11H2Tube furnace put into by O@ZIF-67 combination electrode and sodium hypophosphite Bonderizing in porcelain boat, obtains porous C o3O4@CoP, phosphatization atmosphere is N2Or Ar atmosphere, phosphatization temperature For 270-350 DEG C, preferably 300 DEG C, heating rate is 1-3 DEG C/min, preferably 2 DEG C/min, and phosphating time is 2-4 hour, preferably 3 hours.
Preferably Co (CO3)0.5OH·0.11H2The O@every 0.2cm of ZIF-67 combination electrode2Corresponding 0.1-0.5g phosphorus Acid sodium.
Gained Co of the present invention3O4@CoP is used for electrocatalytic decomposition water and fuel cell field.
Co (the CO of the present invention3)0.5OH·0.11H2The composite that O and ZIF constructs is novel, obtains simultaneously Porous C o3O4@CoP has well-regulated pattern and orderly array, and has good electro catalytic activity, Electrolysis water is widely used；Preparation method technique of the present invention is simple, easy to implement, productivity is high, is beneficial to Batch prepares high performance electrode material.
Accompanying drawing explanation
Fig. 1 is this Co (CO3)0.5OH·0.11H2The scanning electron microscope schematic diagram of O electrode.
Fig. 2 is this Co (CO3)0.5OH·0.11H2The scanning electron microscope schematic diagram of O@ZIF-67 combination electrode.
Fig. 3 is this porous C o3O4The scanning electron microscope schematic diagram of@CoP combination electrode.
Fig. 4 is this Co (CO3)0.5OH·0.11H2O electrode and Co3O4The electrocatalytic decomposition of@CoP combination electrode The performance schematic diagram of water.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but the present invention is not limited to following example.
Embodiment 1
The first step: 50ml deionized water stirring and dissolving 5mmol cabaltous nitrate hexahydrate and 25mmol carbamide, system The homogeneous phase solution obtained is poured in reactor, by clean nickel sheet (length, width and height=2cm × 1cm × 0.1cm) submergence State solution, 100 DEG C of Water Under thermal response constant temperature 8 hours, takes out Co (CO3)0.5OH·0.11H2O electrode.
Second step: 10ml water stirring and dissolving 1.25g 2-methylimidazole, adds 1.0ml triethylamine, pours into anti- Answer in still and by Co (CO3)0.5OH·0.11H2O electrode immerses, constant temperature 2 hours under the conditions of 70 DEG C, prepares Co(CO3)0.5OH·0.11H2O@ZIF-67 combination electrode.
3rd step is by Co (CO3)0.5OH·0.11H2O ZIF-67 combination electrode is (long generous =2cm × 1cm × 0.1cm) put into bonderizing in tube furnace porcelain boat with 0.1g sodium hypophosphite.Reaction atmosphere is N2Atmosphere, phosphatization temperature is 300 DEG C, and heating rate is 2 DEG C/min, and phosphating time is 2 hours, prepares many Hole Co3O4@CoP combination electrode, wherein mass area ratio is 1mg/cm-2。
Embodiment 2
The first step: 50ml deionized water stirring and dissolving 5mmol cabaltous nitrate hexahydrate, 25mmol carbamide, system The homogeneous phase solution obtained is poured in reactor, by clean nickel sheet (length, width and height=2cm × 1cm × 0.1cm) submergence State solution, 90 DEG C of Water Under thermal response constant temperature 12 hours, takes out Co (CO3)0.5OH·0.11H2O electrode.
Second step: 10ml water stirring and dissolving 1.25g 2-methylimidazole, adds 1.5ml triethylamine, pours into anti- Answer in still and by Co (CO3)0.5OH·0.11H2O electrode immerses, constant temperature 2 hours under the conditions of 70 DEG C, prepares Co(CO3)0.5OH·0.11H2O@ZIF-67 combination electrode.
3rd step is by Co (CO3)0.5OH·0.11H2O@ZIF-67 combination electrode (length, width and height =2cm × 1cm × 0.1cm) put into bonderizing in tube furnace porcelain boat with 0.5g sodium hypophosphite.Reaction atmosphere is Ar atmosphere, phosphatization temperature is 350 DEG C, and heating rate is 2 DEG C/min, and phosphating time is 2 hours, prepares many Hole Co3O4@CoP electrode, wherein mass area ratio is 1mg/cm-2。
The test result of the material of above-described embodiment gained is identical, is specifically shown in following:
(1) material morphology characterizes:
Take this Co (CO respectively3)0.5OH·0.11H2O electrode, Co (CO3)0.5OH·0.11H2O@ZIF-67 is combined Electrode and porous C o3O4One fritter of@CoP derivant electrode, selects Zeiss SIGMA 500/VP model field Launch scanning electron microscope it is characterized.Structure and morphology figure is shown in Fig. 1, Fig. 2 and Fig. 3.
(2) material charge-discharge performance characterizes:
Fig. 4 is Co (CO3)0.5OH·0.11H2O electrode and Co3O4@CoP derivant electrode is in 1M hydroxide In potassium, scanning speed is the linear sweep voltammetry curve (LSV) of 20mV/s.

Claims (9)

1. porous C o3O4The preparation method of@CoP combination electrode, it is characterised in that pass through Hydro-thermal reaction is homoepitaxial Co (CO in nickel/platinized platinum substrate3)0.5OH·0.11H2O thin film, enters And at Co (CO3)0.5OH·0.11H2The ZIF-67 of O surface in situ growth crystal form, constructs and obtains Co(CO3)0.5OH·0.11H2O@ZIF-67 composite, final bonderizing obtains porous knot The Co of structure3O4@CoP electrode.
2. according to a kind of porous C o described in claim 13O4The system of@CoP combination electrode Preparation Method, it is characterised in that specifically include following steps:
The nickel sheet cleaned is immersed solution A by the first step, and hydro-thermal reaction prepares Co(CO3)0.5OH·0.11H2O electrode, wherein solution A cabaltous nitrate hexahydrate is dissolved in carbamide The solution that ionized water obtains, preferably every 5mmol cabaltous nitrate hexahydrate correspondence 20-30mmol Carbamide, 20-80ml deionized water；
Second step is by Co (CO3)0.5OH·0.11H2O electrode immerses in mother solution B and carries out reacting To Co (CO3)0.5OH·0.11H2O@ZIF-67 combination electrode；Mother solution B be 2-methylimidazole, Deionized water and the mixed liquor of triethylamine, every 1-3g 2-methylimidazole correspondence 10ml deionized water With the triethylamine of 0.5-1.5ml, reaction temperature keeps 50-75 DEG C, 0.5-3 hour time；
3rd step is by Co (CO3)0.5OH·0.11H2O@ZIF-67 combination electrode is put with sodium hypophosphite Enter bonderizing in tube furnace porcelain boat, obtain porous C o3O4@CoP, phosphatization atmosphere is N2Or Ar atmosphere, phosphatization temperature is 270-350 DEG C, and heating rate is 1-3 DEG C/min, preferably 2 DEG C/min, Phosphating time is 2-4 hour.
3. according to a kind of porous C o described in claim 23O4The system of@CoP combination electrode Preparation Method, it is characterised in that the first step, the preferably every 5mmol cabaltous nitrate hexahydrate of solution A Corresponding 25mmol carbamide, 50ml deionized water；Hydrothermal reaction condition is 90 DEG C-110 DEG C, Constant temperature 8-12 hour.
4. according to a kind of porous C o described in claim 33O4The system of@CoP combination electrode Preparation Method, it is characterised in that hydrothermal reaction condition is 90 DEG C, constant temperature 10 hours.
5. according to a kind of porous C o described in claim 23O4The system of@CoP combination electrode Preparation Method, it is characterised in that second step reaction temperature keeps 70 DEG C, 1 hour time.
6. according to a kind of porous C o described in claim 23O4The system of@CoP combination electrode Preparation Method, it is characterised in that the 3rd step Co (CO3)0.5OH·0.11H2O@ZIF-67 compound electric Extremely every 0.2cm2Corresponding 0.1-0.5g sodium hypophosphite.
7. according to a kind of porous C o described in claim 23O4The system of@CoP combination electrode Preparation Method, it is characterised in that the 3rd step phosphatization temperature is 300 DEG C, heating rate is 2 DEG C/min, Phosphating time is 3 hours.
8. porous C o prepared according to the arbitrary phase method of claim 1-73O4@CoP is multiple Composite electrode, it is characterised in that porous C o3O4@CoP combination electrode is porous C o3O4@CoP Club shaped structure array, Co3O4The cross section of@CoP club shaped structure is polygon.
9. porous C o prepared according to the arbitrary phase method of claim 1-73O4@CoP is multiple The application of composite electrode, it is characterised in that for electrocatalytic decomposition water and fuel cell.
CN201610515711.1A 2016-07-01 2016-07-01 Preparation method for preparing Co3O4@CoP composite electrode based on MOF template Pending CN105977467A (en)

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CN106450200A (en) * 2016-10-25 2017-02-22 福建师范大学 Cos@carbon nano-cage as well as preparation method and application thereof
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CN107029792A (en) * 2017-04-07 2017-08-11 三峡大学 A kind of metal organic frame and graphene electro-catalysis composite and preparation method thereof
CN107275639A (en) * 2017-06-30 2017-10-20 武汉理工大学 CoP/C classifying nano lines of nano particle assembling and its preparation method and application
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