CN106783213A - Metal and the mesoporous carbon nano-composite material preparation method of metal oxide quantum dot - Google Patents
Metal and the mesoporous carbon nano-composite material preparation method of metal oxide quantum dot Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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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
- Y02E60/13—Energy storage using capacitors
Abstract
It is an object of the present invention to provide a kind of metal with excellent capacity and cycle performance and the preparation method of the mesoporous carbon nano-composite material of metal oxide quantum dot.The inventive method does carbon source, maceration extract immersion stalk particle, then the composite is obtained through drying, roasting, grinding to prepare maceration extract as solvent with metal M salt as solute, with absolute ethyl alcohol and distilled water with sponginess straw high.The inventive method process is simple, it is with low cost, quantum point grain diameter is in 2 10nm or so and is evenly distributed, favorable reproducibility, metal and the metal oxide quantum dot/mesoporous carbon composite material of preparation show excellent capacity and cycle performance for electrode material for super capacitor, and good catalytic performance is also shown for methanol catalytic oxidation.
Description
(1) technical field
The present invention relates to a kind of metal and the preparation method of metal oxide quantum dot-mesoporous carbon nano-composite material.
(2) background technology
Quantum dot (quantum dots, QDs), is also called semiconductor nanocrystals body, i.e., by hundreds of to few thousand atoms
Composition, radius is less than or close to bohr exciton radii, and size is less thanZero-dimension nano metal or semi-conducting material.By
In its unique structure, quantum dot have quantum size effect, skin effect, macro quanta tunnel effect, Dielectric confinement effect,
The fundamental characteristics such as quantum confined effect, skin effect.Therefore compared to macroscopic material, CdS quantum dots show many spies
Different physics and chemical property, wide application prospect is showed in fields such as optics, energy storage, catalysis and new materials.
Ultracapacitor is a kind of electrochemical energy storage device between traditional capacitor and secondary cell, with power
Density is high, have extended cycle life, temperature in use wide ranges, it is environmentally safe the advantages of, be widely used in portable electronic
Equipment, electric automobile field and standby power system.According to energy storage mechnism, ultracapacitor can be divided into double based on carbon material
Electric layer capacitor and the pseudocapacitors based on conducting polymer, metal oxide, and pseudocapacitors are with higher than carbon material
Specific capacitance.One great development direction of ultracapacitor is exactly comprehensive raising energy density and power density, the counterfeit electricity of this aspect
Have very big advantage, but fake capacitance has the limitation of cycle life and high rate performance.Nowadays, the starting point of researcher
Reduction particle size is focused primarily on, increases specific surface area or compound with other materials to improve its capacity and stability.Quantum
The super-small of point, can effectively increase the specific surface area of active material, and electrolyte can be more abundant with surface of active material
Contact, beneficial to the generation of electrochemical reaction, reduce current density and reduce polarization, so as to increase capacity, show more preferable electricity
Chemism and stability.
Metallic catalyst has good catalytic performance, the study hotspot as catalytic chemistry.By metal quantum point
For catalyst, because its size is minimum, specific surface area is big, surface atom ligancy wretched insufficiency existing defects, thus with very
Surface-active high, the characteristic causes that quantum dot shows many excellent catalysis activity and selectivity in catalytic field, is to pass
System catalyst is incomparable.
Though quantum dot is with above-mentioned many advantages, because its surface can be higher, easily reunite and deteriorate, and storage capacity
The organic solvent toxicity of son point is larger, and these all limit the application of quantum dot.Research shows, by being combined other base materials
The performance of quantum dot can be effectively improved.Meso-porous carbon material has larger specific surface area (up to 2000m2/ g) and specific pore volume
(up to 1.5m3/ g), the pore passage structure of high-sequential (or unordered), it is easy to the pattern of regulation and control, narrow and small pore-size distribution is good
Micro-nano structure, outstanding physical and chemical stability is a kind of ideal carrier material.Quantum dot is answered with meso-porous carbon material
Close, on the one hand the pore structure of mesoporous carbon rich can increase the dispersion of quantum dot, effectively prevent the reunion of quantum dot particle
Larger reaction interface and outstanding chemically and thermally stability is provided simultaneously, is on the other hand had in itself due to carbon material good
Electric conductivity, so it can also improve the electric conductivity and ion transport capability of active material.The nano combined material of quantum dot-mesoporous carbon
Material not only possesses the quantum size effect of quantum dot special construction generation, and the electronic transmission performance high with mesoporous carbon, two
In the great application potential in field such as energy storage and catalysis after person is compound.In conventional report, in terms of being applied to energy storage and catalysis
The report of metal and metal oxide quantum dot/mesoporous carbon composite material is less, and preparation method is required for greatly some costlinesses, has
The raw material and reagent and special device of toxicity, the harm to human body are larger.
(3) content of the invention
It is an object of the present invention to provide a kind of metal with excellent capacity and cycle performance and metal oxide quantum dot-
The preparation method of mesoporous carbon nano-composite material.
The technical solution adopted by the present invention is:
A kind of preparation method of metal and metal oxide quantum dot-mesoporous carbon nano-composite material, methods described includes:
(1) with metal M salt as solute, with absolute ethyl alcohol and distilled water as solvent, the leaching of 10~100mmol/L of compound concentration
Stain liquid, metal M is Co, Mn, Cu, Zn, Fe or W, absolute ethyl alcohol:Distilled water volume ratio is 1:5~8;It is general using inclined when M is W
Ammonium tungstate when M is other metals, then typically uses its acetate as solute as solute;
(2) carbon source is done with sponginess straw high, is removed the peel, remove interior stem, crushed, 50~60 DEG C of 4~5h of drying obtain stalk
Particle;The sponginess straw high is maize straw, Jerusalem artichoke stalk or broomcorn straw;Using sponginess straw plants straw high
Stalk, autologous tissue's structure mesoporous gap rate is higher, and high porosity can make a large amount of maceration extract absorption on stalk particle.Stalk goes
Skin, interior flesh is only stayed after removing interior stem, is in fine granularity after crushing.
(3) step (1) maceration extract soaking step (2) stalk particle is used, solid-to-liquid ratio is 1g:150~250mL, normal temperature ultrasound
After (100~200W) processes 10~30min, 10~30min of application of vacuum under 0.08~0.1MPa;The cavitation of ultrasonic wave can
To realize the uniform mixing between heterogeneous reaction thing, accelerate diffusion of the maceration extract to stalk particle hole.Meanwhile, ultrasonic wave
Plant cell wall can be destroyed, the crystallinity of cellulose is reduced, increases surface area, improve accessibility of the solution to cellulose, with
This increases load capacity.Application of vacuum can remove the air in hole, and relative more solution that can make enter, and increase negative
Carrying capacity.
(4) stalk particle after immersion is filtered, 60~80 DEG C of dryings;
(5) stalk particle that step (4) is obtained is placed in tube furnace, heat up heating under inert gas atmosphere, 600~
1000 DEG C of 3~6h of roasting, grind after taking-up, obtain the composite.
Preferably, the metal M is Co, Mn, Cu or W.
Preferably, impregnation concentration is 50mmol/L in step (1).
Inert gas is usually argon gas or nitrogen, preferably argon gas in step (5).
Preferably, heating rate is 1~10 DEG C/min, most preferably 5 DEG C/min in step (5).Roasting time is preferably
4h。
Sintering temperature temperature according to selected by the difference of maceration extract species described in step (5) is different.For the acetic acid of metal M
Salt makees presoma, and it is 600 DEG C that temperature is optimal, and presoma is made for ammonium metatungstate, and it is 1000 DEG C that temperature is optimal.
Metal of the present invention and metal oxide quantum dot-mesoporous carbon nano-composite material are used as electrode of super capacitor reality
With it is high to show capacity, steady performance.In acidic methanol solution, as the catalyst of methanol oxidation electroxidation, table
Reveal good catalytic performance.
Compared with prior art, the advantage of the invention is that:
(1) method of the present invention does carbon using sponginess straw high (such as maize straw, Jerusalem artichoke stalk, broomcorn straw)
Source, low raw-material cost is easy to get.Metal and metal oxide quantum dot/mesoporous carbon composite wood are prepared by high-temperature roasting
Material, the method is prepared and is simple and convenient to operate, favorable reproducibility, without strong acid, highly basic or toxic reagent in preparation process, also not
The accessory substance of easily pollution environment can be produced, it is environmentally friendly.
(2) the quantum dot particle that obtains of the present invention can be uniformly dispersed in mesoporous carbon skeleton, Average Particle Diameters 2~
10nm, mesoporous carbon can effectively prevent the reunion of quantum dot, while the electric conductivity and ion transport capability of material can be increased.Will
To material show high power capacity, long-life advantage for electrode of super capacitor, also shown for methanol catalytic oxidation
Good catalytic performance.
(4) illustrate
Fig. 1 schemes for the TEM of manganous oxide quantum dot obtained in embodiment 1-mesoporous carbon nano-composite material.
Fig. 2 schemes for the TEM of cobalt oxide quantum dot obtained in embodiment 2-mesoporous carbon nano-composite material.
Fig. 3 schemes for the TEM of copper quantum dot obtained in embodiment 3-mesoporous carbon nano-composite material.
Fig. 4 schemes for the TEM of manganous oxide quantum dot obtained in embodiment 4-mesoporous carbon nano-composite material.
Fig. 5 schemes for the TEM of tungsten carbide quantum dot obtained in embodiment 5-mesoporous carbon nano-composite material.
Fig. 6 is the XRD of tungsten carbide quantum dot obtained in embodiment 5-mesoporous carbon nano-composite material.
Fig. 7 is tungsten carbide quantum dot obtained in embodiment 5-mesoporous carbon nano-composite material in acidic methanol solution
Cyclic voltammetry curve.
(5) specific embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This:
Embodiment 1:
Maize straw is removed into interior stem, interior flesh is taken and is crushed, 60 DEG C dry 5h, standby.0.49g manganese acetates are weighed, is added
35mL distilled water, 5mL ethanol is configured to the acetic acid manganese solution of 50mmol/L.Flesh in the corn after 0.2g treatment is weighed to be put into
In 100mL round-bottomed flasks, the acetic acid manganese solution that addition is prepared, ultrasound 30min, application of vacuum 30min under normal temperature.Once take out
Filter, 80 DEG C of dryings.Flesh in corn after impregnation drying is inserted in tube furnace, argon gas atmosphere, be calcined 4h, sintering temperature is 600
DEG C, heating rate is 5 DEG C/min.Grinding obtains product after cooling.
Transmission electron microscope detection is carried out to resulting manganous oxide quantum dot-mesoporous carbon nano-composite material, is tied
As a result fruit as shown in figure 1, show:Quantum dot high uniformity is dispersed in mesoporous carbon, and particle size is in 5nm or so.
Embodiment 2:
Maize straw is removed into interior stem, interior flesh is taken and is crushed, 60 DEG C dry 5h, standby.0.498g cobalt acetates are weighed, is added
35mL distilled water, 5mL ethanol is configured to the acetic acid cobalt liquor of 50mmol/L.Flesh in the corn after 0.2g treatment is weighed to be put into
In 100mL round-bottomed flasks, the acetic acid cobalt liquor that addition is prepared, ultrasound 30min, application of vacuum 30min under normal temperature.Once take out
Filter, 80 DEG C of dryings.Flesh in corn after impregnation drying is inserted in tube furnace, argon gas atmosphere, be calcined 4h, sintering temperature is 600
DEG C, heating rate is 5 DEG C/min.Grinding obtains product after cooling.
Transmission electron microscope detection is carried out to resulting cobalt oxide quantum dot-mesoporous carbon nano-composite material, as a result
As shown in Fig. 2 as a result showing:Quantum dot high uniformity is dispersed in mesoporous carbon, and particle size is in 5nm or so.
Embodiment 3:
Maize straw is removed into interior stem, interior flesh is taken and is crushed, 60 DEG C dry 5h, standby.0.799g copper acetates are weighed, is added
35mL distilled water, 5mL ethanol is configured to the copper acetate solution of 100mmol/L.Flesh in the corn after 0.2g treatment is weighed to be put into
In 100mL round-bottomed flasks, the copper acetate solution that addition is prepared, ultrasound 30min, application of vacuum 30min under normal temperature.Once take out
Filter, 80 DEG C of dryings.Flesh in corn after impregnation drying is inserted in tube furnace, argon gas atmosphere, be calcined 4h, sintering temperature is 600
DEG C, heating rate is 5 DEG C/min.Grinding obtains product after cooling.
Transmission electron microscope detection is carried out to resulting copper quantum dot-mesoporous carbon nano-composite material, as a result such as Fig. 3
It is shown, as a result show:Quantum dot high uniformity is dispersed in mesoporous carbon, and particle size is in 10nm or so.
Embodiment 4:
Jerusalem artichoke stalk is removed into interior stem, interior flesh is taken and is crushed, 60 DEG C dry 5h, standby.0.49g manganese acetates are weighed, is added
35mL distilled water, 5mL ethanol is configured to the acetic acid manganese solution of 50mmol/L.Flesh in the Jerusalem artichoke after 0.2g treatment is weighed to be put into
In 100mL round-bottomed flasks, the acetic acid manganese solution that addition is prepared, ultrasound 30min, application of vacuum 30min under normal temperature.Once take out
Filter, 80 DEG C of dryings.Flesh in Jerusalem artichoke after impregnation drying is inserted in tube furnace, argon gas atmosphere, be calcined 4h, sintering temperature is 600
DEG C, heating rate is 5 DEG C/min.Grinding obtains product after cooling.
Transmission electron microscope detection is carried out to resulting manganous oxide quantum dot-mesoporous carbon nano-composite material, is tied
As a result fruit as shown in figure 4, show:Quantum dot high uniformity is dispersed in mesoporous carbon, and particle size is in 2nm or so.
Embodiment 5:
Maize straw is removed into interior stem, interior flesh is taken and is crushed, 60 DEG C dry 5h, standby.5.912g ammonium metatungstates are weighed, plus
Enter 35mL distilled water, 5mL ethanol is configured to the ammonium metatungstate solution of 50mmol/L.Flesh in the corn after 0.2g treatment is weighed to be put into
In 100mL round-bottomed flasks, the ammonium metatungstate solution that addition is prepared, ultrasound 30min, application of vacuum 30min under normal temperature.Once take out
Filter, 80 DEG C of dryings.Flesh in corn after impregnation drying is inserted in tube furnace, argon gas atmosphere, be calcined 4h, sintering temperature is 1000
DEG C, heating rate is 5 DEG C/min.Grinding obtains product after cooling.
Transmission electron microscope detection is carried out to resulting tungsten carbide quantum dot-mesoporous carbon nano-composite material, as a result
As shown in figure 5, as a result showing:Quantum dot high uniformity is dispersed in mesoporous carbon, and particle size is in 5nm or so.
X-ray powder diffraction test is carried out to resulting tungsten carbide quantum dot-mesoporous carbon nano-composite material, as a result
As shown in fig. 6, as a result showing:Material is made up of tungsten carbide and agraphitic carbon.
Resulting materials are prepared into electrode, material:Acetylene black:PTFE=8:1:1, nickel foam does collector, pole piece size
It is 1cm × 1cm.With three-electrode system come test material capacitive property, prepared electrode is working electrode, platinized platinum (1.5cm ×
1.5cm) it is auxiliary electrode, mercury oxidation mercury electrode is reference electrode, and electrolyte is 6mol/L KOH solutions.Electro-chemical test exists
Carried out on land battery test systems, voltage range is 0~0.5V, current density is 1A/g, 2A/g.Result shows the composite wood
Expect to show high power capacity, long-life advantage for electrode of super capacitor.The composite following in acidic methanol solution
Ring volt-ampere curve is shown in Fig. 7, as a result shows that composite also shows good catalytic performance for methanol catalytic oxidation.
Claims (6)
1. a kind of preparation method of metal and metal oxide quantum dot-mesoporous carbon nano-composite material, methods described includes:
(1) with metal M salt as solute, with absolute ethyl alcohol and distilled water as solvent, the dipping of 10~100mmol/L of compound concentration
Liquid, metal M is Co, Mn, Cu, Zn, Fe or W, absolute ethyl alcohol:Distilled water volume ratio is 1:5~8;
(2) carbon source is done with sponginess straw high, is removed the peel, remove interior stem, crushed, 50~60 DEG C of 4~5h of drying obtain stalk
Grain;The sponginess straw high is maize straw, Jerusalem artichoke stalk or broomcorn straw;
(3) step (1) maceration extract soaking step (2) stalk particle is used, solid-to-liquid ratio is 1g:150~250mL, normal temperature is ultrasonically treated
After 10~30min, 10~30min of application of vacuum under 0.08~0.1MPa;
(4) stalk particle after immersion is filtered, 60~80 DEG C of dryings;
(5) stalk particle that step (4) is obtained is placed in tube furnace, heat up heating, 600~1000 under inert gas atmosphere
DEG C roasting 3~6h, after taking-up grind, obtain the composite.
2. the method for claim 1, it is characterised in that metal M is Co, Mn, Cu or W in step (1).
3. the method for claim 1, it is characterised in that impregnation concentration is 50mmol/L in step (1).
4. the method for claim 1, it is characterised in that inert gas is argon gas in step (5).
5. the method for claim 1, it is characterised in that heating rate is 1~10 DEG C/min in step (5).
6. the method for claim 1, it is characterised in that in step (5), presoma for M metals acetate when, roasting
Temperature is 600 DEG C;When presoma is ammonium metatungstate, sintering temperature is 1000 DEG C.
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CN109516507A (en) * | 2017-09-18 | 2019-03-26 | 浙江工业大学 | A kind of preparation method of porous cobaltosic oxide nano piece |
CN111180745A (en) * | 2019-12-30 | 2020-05-19 | 浙江工业大学 | CeO (CeO)xPreparation method and application of/MC nanosheet material |
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CN109516507A (en) * | 2017-09-18 | 2019-03-26 | 浙江工业大学 | A kind of preparation method of porous cobaltosic oxide nano piece |
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CN111180745A (en) * | 2019-12-30 | 2020-05-19 | 浙江工业大学 | CeO (CeO)xPreparation method and application of/MC nanosheet material |
CN111180745B (en) * | 2019-12-30 | 2021-11-23 | 浙江工业大学 | CeO (CeO)xPreparation method and application of/MC nanosheet material |
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