CN108400346A - A kind of preparation method of the overmolded carbon material of cuprous oxide - Google Patents
A kind of preparation method of the overmolded carbon material of cuprous oxide Download PDFInfo
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- CN108400346A CN108400346A CN201810197420.1A CN201810197420A CN108400346A CN 108400346 A CN108400346 A CN 108400346A CN 201810197420 A CN201810197420 A CN 201810197420A CN 108400346 A CN108400346 A CN 108400346A
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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
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5072—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with oxides or hydroxides not covered by C04B41/5025
- C04B41/5074—Copper oxide or solid solutions thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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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
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/96—Carbon-based electrodes
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/16—Biochemical fuel cells, i.e. cells in which microorganisms function as catalysts
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- 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
- Y02E60/50—Fuel cells
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The present invention relates to new energy and sewage treatment field, it is desirable to provide a kind of preparation method of the overmolded carbon material of cuprous oxide.Including：By molding carbon material after polishing, cleaning, it is immersed in the mixed solution of copper nitrate and stabilizer；Then electroreduction processing is carried out；It is rinsed with deionized water, soaking at room temperature in deionized water；It is dried in vacuo to get to the molding carbon material for having coated cuprous oxide under the conditions of being protected from light.The present invention uses molding carbon material as cuprous oxide base material for the first time, more meets practical application request；Under visible light illumination, there are significant photoelectric respones for the product of preparation；It can be by regulating and controlling current density and electrodeposition time, to adjust the thickness of cuprous oxide film；Preparation method is simple, and film-formation result is stablized, and is conducive to produce in enormous quantities.This method carries out at low temperature, and current density is small, and current utilization rate is high, and energy cost is low.In electrolyte after use, content of beary metal is low, disposable.
Description
Technical field
The present invention relates to a kind of preparation methods of the quick controllable overmolded carbon material of cuprous oxide.The material can be applied
In directions such as rechargeable battery, photocatalysis, electro-catalysis, microbiological fuel cell, solar cell, ultracapacitors, belong to new energy
Source and sewage treatment field.
Background technology
With the fast development of human society, the energy lacks and environmental pollution the problem of bringing seems and becomes increasingly conspicuous, and develops
Reproducible new energy and relevant energy and material are cleaned, efficient, non-secondary pollution novel environmental treatment technology is found, becomes
One hot issue urgently to be resolved hurrily.
Cuprous oxide is a kind of energy and environment material of great interest in recent years, it can be applied to photocatalysis,
The multiple fields such as electro-catalysis, microbiological fuel cell, rechargeable battery, solar cell, ultracapacitor.Cuprous oxide (Cu2O)
Semiconductive thin film is a kind of non-stoichiometry semiconductor few in number, and semiconductor type is usually p-type, and direct band gap is
1.9~2.1eV is a kind of novel photoelectric converting material.Cu2O semiconductive thin films have good gas sensing property and piezoelectricity, can
By the excited by visible light in 800~400nm wave-length coverages.Cu2The photoelectric conversion efficiency of O theoretically can reach 20%, report at present
The highest energy transfer efficiency in road is more than 2%.The conduction band current potential of cuprous oxide is -0.28V vs.NHE, less than hydrogen-evolution overpotential and
Carbon dioxide reduction current potential, therefore the photoelectron of the strong reducing property generated after being excited using cuprous oxide light, can be applied to produce
The fields such as hydrogen, carbon trapping (Carbon capture and storage, CCS), methane phase.And the photohole tool of cuprous oxide
There is extremely strong oxidisability (valence band current potential is 1.92V vs.NHE), the organic pollution of the degradable overwhelming majority, cuprous oxide exists
Photocatalysis treatment field of sewage has a large amount of reports.In addition, since cuprous oxide material has the spies such as cheap and easy to get, high specific capacitance
Property, have in terms of substituting conventional graphite material as the negative material of the equipment such as lithium battery, sode cell, ultracapacitor very big
Potentiality.Microbiological fuel cell (Microbial Fuel Cell, abbreviation MFC) be it is a kind of using microorganism be catalyst, directly
Convert the chemical energy being stored in waste water in the device of electric energy.Pass through the cathode or anode modification oxygen in microbiological fuel cell
Change the cuprous research to promote the wastewater treatment efficiency and electricity generation performance of battery and is also seen in report.
In general, the grain diameter of cuprous oxide is smaller, and specific surface area is bigger, and surface reactant adsorbance is bigger, anti-
Answer active site exposure more.Cuprous oxide micro-nano granules can be prepared by the methods of hydro-thermal method, agglutinating nature yeast, still
Discrete cuprous oxide particle there is a problem of being unevenly distributed in practical applications, it is common to be difficult to recycling, usually need
Carrier is wanted to load cuprous oxide particle.The load of overwhelming majority cuprous oxide is all made of electro-conductive glass (including Fluorin doped at present
Fin oxide condutire glass, FTO；With indium tin oxide electro-conductive glass, ITO) it is substrate.
Molding carbon material includes graphite cake, graphite rod, carbon cloth, carbon paper, carbon felt or carbon fiber brush, since it has height
Conductance, high capacitance, corrosion-resistant, biocompatibility be good, easily modification, there are the characteristics such as certain flexibility, microbiological fuel cell,
The fields such as photocatalysis, electro-catalysis, battery, ultracapacitor have application ripe extensively.Using molding carbon material as oxygen
Change cuprous supporting substrate, is an ideal selection.However, the carbon materials that can be used as cuprous oxide substrate reported at present
Material, only graphene, carbon nanotube, carbon nanohorn, graphite particle etc. be micro-, nano level discrete form, wider in application
The simple controllable technology for preparing cuprous oxide particle has not been reported in molding carbon material substrate.Currently, being received in graphene, carbon
Mitron, carbon nanohorn, graphite particle etc. dispersion carbon material on load cuprous oxide, mostly use greatly chemical vapor deposition, hydro-thermal method,
The methods of sol-gel method, pyrolysismethod in situ, these preparation methods process is complicated, generally requires special installation majority and needs height
Temperature, loss rate of raw materials is high in preparation process, and energy cost and cost of material are high；The cuprous oxide usually prepared is in granular form point
It dissipates, it is difficult to form a film, the density and thickness of stratum granulosum are not easy to control；Preparation process processed remaining heavy metallic salt solution, is received organic matter
Rice material etc. can cause environmental pollution, it is difficult to meet the needs of large-scale application.
Invention content
The technical problem to be solved by the present invention is to overcome deficiency in the prior art, provide a kind of cuprous oxide and be overmolding to
The preparation method of type carbon material.
To solve technical problem, inventive solution is：
A kind of preparation method of the overmolded carbon material of cuprous oxide is provided, is included the following steps：
(1) by the sample for being molded carbon material after polishing, cleaning, it is immersed in 0.05~0.2M that pH value is 9.0~12.0
In the mixed solution of (abbreviation of mol/L, the same below) copper nitrate and 2~4M stabilizers；Then in 0.5~2.0mAcm-2Electric current
Density or under conditions of relative to silver/silver chloride reference -0.3~-0.5V of electrode potential carry out electroreduction processing 0.5~
2.0h, the temperature that should control mixed solution in the process is 40~60 DEG C；
(2) after rinsing the sample that is handled through electroreduction 4~8 times with deionized water, it is placed in soaking at room temperature in deionized water
20min；Then 2~4h is dried in vacuo at 60~100 DEG C and under the conditions of being protected from light to get to the molding carbon materials for having coated cuprous oxide
Material.
In the present invention, the molding carbon material be it is following any one：Graphite cake, graphite rod, carbon cloth, carbon paper, carbon
Felt or carbon fiber brush.
In the present invention, the stabilizer is lactic acid, acetic acid or tartaric acid.Stabilizer is used to generate complex compound with copper ion,
Promote cuprous oxide slowly to stablize to be precipitated.
In the present invention, the pH value adjustment of mixed solution is real by the way that 1M sodium hydroxide solutions are added dropwise into mixed solution
Existing.
In the present invention, the temperature control in electro-reduction process is to heat to realize by water bath with thermostatic control.
In the present invention, current density and current potential in electro-reduction process are by potentiostat, constant-current supply or electrification
Learn test cabinet control.
In the present invention, the vacuum condition is realized in vacuum drying chamber or tube-type atmosphere furnace.
In the present invention, it is described be protected from light condition be by using lighttight container contain sample, with aluminium-foil paper package sample,
Or the vacuum drying chamber equipped with sample is placed in and is realized in darkroom.
Compared with prior art, present invention has the advantages that：
(1) in the cuprous oxide cladding carbon material reported, the carbon material used is the carbon material of dispersing type, including stone
Black alkene, carbon nanohorn, carbon nanotube, graphite particle etc., the present invention use molding carbon material as cuprous oxide substrate material for the first time
Material, specifically includes graphite cake, graphite rod, carbon cloth, carbon paper, carbon felt or carbon fiber brush, more meets practical application request；
(2) cuprous oxide prepared by this method coats carbon material, and under visible light illumination, there are significant photoelectric respones；
(3) cuprous oxide prepared by this method coats carbon material, can be come by regulating and controlling current density and electrodeposition time
Adjust the thickness of cuprous oxide film；
(4) compared with untreated carbon material, to have coated the carbon material of cuprous oxide as the moon of microorganism electrolysis cell
Pole substrate can greatly improve the kinetic current of reactor, promote the hydrogen output of reactor.
(5) method for belonging to electrochemical deposition does not need complicated equipment and operation.Preparation method is simple, film-formation result
Stablize, is conducive to produce in enormous quantities.
(6) this method carries out at low temperature, and current density is small, and current utilization rate is high, and energy cost is low.Electrolysis after use
In liquid, content of beary metal is low, disposable.
Description of the drawings
Fig. 1 coats the surface scan electromicroscopic photograph (SEM) of carbon material for cuprous oxide obtained in embodiment 1,2.
The X ray diffracting spectrum (XRD) of cuprous oxide obtained cladding carbon material surface in the positions Fig. 2 embodiment 1,2.
Fig. 3 is that cuprous oxide coated graphite plate electrode obtained is electric in -0.3V vs. silver/silver chloride reference in embodiment 1
Photoelectric current under electrode potential.
Fig. 4 is cuprous oxide coated graphite plate electrode obtained in embodiment 1 in -0.3~-0.65V vs. silver/silver chlorate
Photocurrent variations trend in reference electrode potential range.
Fig. 5 is the cuprous oxide graphite plate electrode obtained under different electrodeposition times, in -0.3V using in embodiment 2
Vs. the photoelectric current under silver/silver chloride reference electrode potential.
Fig. 6 is cuprous oxide coated graphite plate electrode obtained under different electrodeposition times in embodiment 2, -0.3~-
Photocurrent variations trend within the scope of 0.65V vs. silver/silver chloride reference electrode potential.
Specific implementation mode
Below in conjunction with attached drawing and specific example, the invention will be further described, and its object is to preferably explain the present invention
Rather than limitation of the present invention.
Specific embodiment 1
It is prepared by cuprous oxide coated graphite plate electrode：
It is 4cm that high temperature pyrolysis graphite cake, which is cut into area,2Square, successively use P400 sand paper, P1500 sand paper and 0.05
Each face of high temperature pyrolysis graphite cake is polishing to smooth by μm aluminium powder, removes an area 4cm2Side outside, graphite cake other faces are used
Waterproof insulation tape is pasted.By a piece of suspended electrode in 50mL pH=12.0, T=40 DEG C of 0.1M copper nitrates and 3M lactic acid
In mixed solution, a piece of area of exposed surface face is 9cm2Square platinized platinum, electrode spacing 2cm.By graphite cake and electrification
The working electrode connection for learning work station, platinized platinum with reference electrode and connect electrode, structure dual-electrode electrolysis cell system.Xiang Gong
Make electrode conveying 1mAcm-2Electric current (total current by graphite cake bare area calculate), be persistently powered 1h；After taking-up, by gained
After sample is rinsed 5 times with deionized water, it is placed in soaking at room temperature 20min in deionized water, is coated with aluminium foil, the vacuum at 100 DEG C
Dry 3h coats carbon material to get to the cuprous oxide handled well.
The photoelectric conversion performance test of cuprous oxide coated graphite plate electrode：
Using cuprous oxide coated graphite plate obtained as working electrode, platinum plate electrode is to electrode, with silver/silver chloride electrode
For reference electrode three-electrode electrochemical test system is built using 0.2M metabisulfite solutions as electrolyte.Nitrogen is exposed to electrolyte in advance
Gas 20min, and nitrogen is persistently roused during the test.To controlling working electrode potential in -0.3V, to work using potentiostat
Electrode apply intermittent illumination (be intermittent illumination described in this specification unless otherwise stated, visible light wave range, light intensity=
100mW·cm-2, light application time=15s, interlunation=15s), monitoring current, the changing value of electric current under light illumination is photoelectricity
Stream.Linear voltammetric scan is done using potentiostat control working electrode, scanning voltage range is from -0.3V to -0.65V, scanning speed
Rate is 5mV/s, while applying indirect illumination to working electrode, detects photocurrent response.
The SEM of cuprous oxide coated graphite plate is shown in that Fig. 1, cuprous oxide obtained are regular micro/nano level cubic
Grain.Relative to crumby cuprous oxide, the active site exposure of cubic cuprous oxide is more, and reaction rate is usually more
Greatly.Fig. 2 is the XRD spectra of cuprous oxide coated graphite plate surface, the powder diffraction standard card phase with graphite and cuprous oxide
Symbol, and without extra diffraction maximum, illustrate that cuprous oxide purity obtained is very high.Cuprous oxide coated graphite plate electrode obtained-
Photoelectric current under 0.3V vs. silver/silver chloride reference electrode potential is as shown in Figure 3.Under the current potential, by 100mWcm-2It can be seen that
Light irradiates, and cuprous oxide coated graphite plate electrode can generate 0.527Am-2Photoelectric current.Cuprous oxide coated graphite obtained
Photoelectric current of the plate electrode within the scope of -0.3~-0.65V vs. silver/silver chloride reference electrode potential is as shown in Figure 4.With current potential
Decline, photoelectric current is obviously improved.When current potential is in -0.65V, photoelectric current is about 11.2Am-2。
Specific embodiment 2
For the cuprous oxide coated graphite plate electrode of multiple sample preparation difference electrodeposition times：
It is 4cm that high temperature pyrolysis graphite cake, which is cut into 4 areas,2Square, and carry out following processing：P400 sand is used successively
Paper, P1500 sand paper and 0.05 μm of aluminium powder each face of high temperature pyrolysis graphite cake is polishing to it is smooth, remove an area 4cm2Side
Outside, graphite cake other faces are pasted with waterproof insulation tape.By a piece of suspended electrode in 50mL pH=12.0, T=40 DEG C
In the mixed solution of 0.1M copper nitrates and 3M lactic acid, a piece of area of exposed surface face is 9cm2Square platinized platinum, electrode spacing
For 2cm.The working electrode of graphite cake and electrochemical workstation is connected, platinized platinum with reference electrode and connect electrode, structure
Dual-electrode electrolysis cell system.1mAcm is conveyed to working electrode-2Electric current (total current by graphite cake bare area calculate),
For in the experiment of different samples, be persistently powered 0.5h respectively, 1h, 1.5h, 2.0h；After taking-up, by gained sample spend from
After sub- water rinses 5 times, be placed in soaking at room temperature 20min in deionized water, coated with aluminium foil, be dried in vacuo at 100 DEG C 3h to get
Carbon material is coated to the cuprous oxide handled well.
Test the opto-electronic conversion performance of the cuprous oxide coated graphite plate electrode of different electrodeposition times：
Respectively using the cuprous oxide coated graphite plate of different electrodeposition times obtained as working electrode, platinum plate electrode is pair
Electrode, using silver/silver chloride electrode as reference electrode, using 0.2M metabisulfite solutions as electrolyte, structure three-electrode electro Chemical test
System.Nitrogen 20min is exposed to electrolyte in advance, and persistently rouses nitrogen during the test.Utilize potentiostat control work electricity
(intermittent illumination described in this specification unless otherwise stated, electrode potential applies intermittent illumination in -0.3V, to working electrode
It is visible light wave range, light intensity=100mWcm-2, light application time=15s, interlunation=15s), monitoring current, electric current exists
Changing value under illumination is photoelectric current.Linear voltammetric scan, scanning voltage range are done using potentiostat control working electrode
From -0.3V to -0.65V, sweep speed 5mV/s, while indirect illumination is applied to working electrode, detect photocurrent response.
Compare photocurrent response of the cuprous oxide graphite plate electrode under different potentials made from different electrodeposition times.
Cuprous oxide graphite plate electrode obtained under different electrodeposition times, photoelectric current such as Fig. 5 institutes under -0.3V current potentials
Show.As can be seen that when electrodeposition time is 1.0h, the photoelectric current of cuprous oxide film obtained is maximum, and decaying is most slow.It is different
Cuprous oxide graphite plate electrode obtained under electrodeposition time, photoelectric current such as Fig. 6 institutes in -0.3~-0.65V potential ranges
Show.As can be seen that when electrodeposition time is 1.0h, the photoelectric current of cuprous oxide film obtained, in -0.3~-0.65V electricity
Photoelectric current in the range of position is noticeably greater than other；When current potential is more negative, this otherness is more apparent.
Specific embodiment 3
In addition to following adjusted parameters, the preparation method of the overmolded carbon material of cuprous oxide of present embodiment with
Specific embodiment 1 is identical, and adjusted design parameter is：
Using graphite rod as base material, the mixed solution with pH=9.0, T=60 DEG C of 0.2M copper nitrates and 4M acetic acid is
Electrolyte, in 0.5mAcm-2Current density under reductase 12 h, deionized water rinse 4 times, deionized water impregnate 20min, use aluminium
Foil coats, and 4h is dried in vacuo at 60 DEG C.
Specific embodiment 4
In addition to following adjusted parameters, the preparation method of the overmolded carbon material of cuprous oxide of present embodiment with
Specific embodiment 1 is identical, and adjusted design parameter is：
Using carbon cloth as base material, with the mixing of pH=11.0, T=50 DEG C of 0.05M copper nitrates and 2M tartaric acid
Solution is electrolyte, in 2mAcm-2Current density under restore 0.5h, deionized water is rinsed 8 times, and deionized water is impregnated
10min is coated with aluminium foil, and 2h is dried in vacuo at 80 DEG C.
Specific embodiment 5
In addition to following adjusted parameters, the preparation method of the overmolded carbon material of cuprous oxide of present embodiment with
Specific embodiment 1 is similar, and adjusted design parameter is：
Using carbon paper as base material, the mixed solution with pH=10.0, T=45 DEG C of 0.15M copper nitrates and 2M lactic acid is
Electrolyte, electro-deposition 1h (scans the reduction electricity for determining cuprous oxide in Carbon felt surface by cyclic voltammetry under -0.4V current potentials
Position is about -0.38V, and electro-deposition current potential should be slightly less than the current potential), deionized water is rinsed 6 times, and deionized water impregnates 10min, uses aluminium
Foil coats, and 2.5h is dried in vacuo at 70 DEG C.
Specific embodiment 6
In addition to following adjusted parameters, the preparation method of the overmolded carbon material of cuprous oxide of present embodiment with
Specific embodiment 1 is similar, and adjusted design parameter is：
It is molten with the mixing of pH=10.5, T=55 DEG C of 0.125M copper nitrates and 3.5M tartaric acid using carbon felt as base material
Liquid is electrolyte, and electro-deposition 2h (is scanned by cyclic voltammetry and determined cuprous oxide going back in Carbon felt surface under -0.3V current potentials
Former current potential is about -0.28V, and electro-deposition current potential should be slightly less than the current potential), deionized water is rinsed 7 times, and deionized water impregnates 20min,
It is coated with aluminium foil, the vacuum drying time 3.5h at 90 DEG C.
Specific embodiment 7
In addition to following adjusted parameters, the preparation method of the overmolded carbon material of cuprous oxide of present embodiment with
Specific embodiment 1 is similar, and adjusted design parameter is：
Using carbon fiber brush as base material, with the mixing of pH=9.5, T=40 DEG C of 0.175M copper nitrates and 2.5M acetic acid
Solution is electrolyte, and electro-deposition 1.5h (is scanned by cyclic voltammetry and determined cuprous oxide in Carbon felt surface under -0.5V current potentials
Reduction potential be about -0.47V, electro-deposition current potential should be slightly less than the current potential), deionized water is rinsed 8 times, and deionized water is impregnated
20min is coated with aluminium foil, the vacuum drying time 4h at 85 DEG C.
In above-described embodiment, the pH value adjustment of mixed solution can be molten by the way that 1M sodium hydroxides are added dropwise into mixed solution
What liquid was realized.Temperature control in electro-reduction process can heat realization by water bath with thermostatic control.Electric current in electro-reduction process is close
Degree can be controlled with current potential by potentiostat, constant-current supply or electro-chemical test cabinet.Vacuum condition can be in vacuum drying chamber
Or realized in tube-type atmosphere furnace.The condition of being protected from light can be contained sample by using lighttight container, wrap up sample with aluminium-foil paper
What product or be placed in the vacuum drying chamber equipped with sample were realized in darkroom.
Claims (8)
1. a kind of preparation method of the overmolded carbon material of cuprous oxide, which is characterized in that include the following steps：
(1) by the sample for being molded carbon material after polishing, cleaning, it is immersed in 0.05~0.2M nitric acid that pH value is 9.0~12.0
In the mixed solution of copper and 2~4M stabilizers；Then in 0.5~2.0mAcm-2Current density or relative to silver/chlorination
Electroreduction is carried out under conditions of -0.3~-0.5V of silver-colored reference electrode current potential and handles 0.5~2.0h, should control mixed solution in the process
Temperature be 40~60 DEG C；
(2) after rinsing the sample that is handled through electroreduction 4~8 times with deionized water, it is placed in soaking at room temperature 20min in deionized water；
Then 2~4h is dried in vacuo at 60~100 DEG C and under the conditions of being protected from light to get to the molding carbon material for having coated cuprous oxide.
2. according to the method described in claim 1, it is characterized in that, the molding carbon material be it is following any one：Graphite cake,
Graphite rod, carbon cloth, carbon paper, carbon felt or carbon fiber brush.
3. according to the method described in claim 1, it is characterized in that, the stabilizer is lactic acid, acetic acid or tartaric acid.
4. according to the method described in claims 1 to 3 any one, which is characterized in that the pH value adjustment of mixed solution is logical
It crosses and the realization of 1M sodium hydroxide solutions is added dropwise into mixed solution.
5. according to the method described in claims 1 to 3 any one, which is characterized in that the temperature control in electro-reduction process
It is to heat to realize by water bath with thermostatic control.
6. according to the method described in claims 1 to 3 any one, which is characterized in that the current density in electro-reduction process
With current potential controlled by potentiostat, constant-current supply or electro-chemical test cabinet.
7. according to the method described in claims 1 to 3 any one, which is characterized in that the vacuum condition is dry in vacuum
It is realized in dry case or tube-type atmosphere furnace.
8. according to the method described in claims 1 to 3 any one, which is characterized in that it is described be protected from light condition be by using
Lighttight container contains sample, sample is wrapped up with aluminium-foil paper or the vacuum drying chamber equipped with sample is placed in darkroom and is realized
's.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110302783A (en) * | 2019-08-07 | 2019-10-08 | 浙江理工大学 | A kind of flexible easily recycling carbon cloth@Cu2O optic catalytic composite material and preparation method thereof |
| CN111200134A (en) * | 2020-02-18 | 2020-05-26 | 金陵科技学院 | Cuprous oxide film and application thereof in fuel cell |
| CN112607969A (en) * | 2020-12-18 | 2021-04-06 | 张家港市山牧新材料技术开发有限公司 | Dye wastewater treatment process |
| CN112678922A (en) * | 2020-12-18 | 2021-04-20 | 张家港市山牧新材料技术开发有限公司 | Electrochemical water treatment device and system |
| CN112723492A (en) * | 2020-12-18 | 2021-04-30 | 张家港市山牧新材料技术开发有限公司 | Preparation method and application of cuprous oxide loaded activated carbon |
| CN113584517A (en) * | 2021-06-30 | 2021-11-02 | 合肥工业大学 | Preparation method of non-noble metal Ni-Mo-P-B efficient electro-catalytic hydrogen evolution electrode |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110302783A (en) * | 2019-08-07 | 2019-10-08 | 浙江理工大学 | A kind of flexible easily recycling carbon cloth@Cu2O optic catalytic composite material and preparation method thereof |
| CN111200134A (en) * | 2020-02-18 | 2020-05-26 | 金陵科技学院 | Cuprous oxide film and application thereof in fuel cell |
| CN111200134B (en) * | 2020-02-18 | 2022-05-20 | 金陵科技学院 | Cuprous oxide film and application thereof in fuel cell |
| CN112607969A (en) * | 2020-12-18 | 2021-04-06 | 张家港市山牧新材料技术开发有限公司 | Dye wastewater treatment process |
| CN112678922A (en) * | 2020-12-18 | 2021-04-20 | 张家港市山牧新材料技术开发有限公司 | Electrochemical water treatment device and system |
| CN112723492A (en) * | 2020-12-18 | 2021-04-30 | 张家港市山牧新材料技术开发有限公司 | Preparation method and application of cuprous oxide loaded activated carbon |
| CN112607969B (en) * | 2020-12-18 | 2023-10-31 | 湖北紫诺新材料科技股份有限公司 | Dye wastewater treatment process |
| CN113584517A (en) * | 2021-06-30 | 2021-11-02 | 合肥工业大学 | Preparation method of non-noble metal Ni-Mo-P-B efficient electro-catalytic hydrogen evolution electrode |
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