CN115490211A - Method for preparing nitrogen-doped porous carbon nickel diselenide nanocomposite by nesting doll type microwave method - Google Patents
Method for preparing nitrogen-doped porous carbon nickel diselenide nanocomposite by nesting doll type microwave method Download PDFInfo
- Publication number
- CN115490211A CN115490211A CN202211246343.7A CN202211246343A CN115490211A CN 115490211 A CN115490211 A CN 115490211A CN 202211246343 A CN202211246343 A CN 202211246343A CN 115490211 A CN115490211 A CN 115490211A
- Authority
- CN
- China
- Prior art keywords
- nickel
- nitrogen
- diselenide
- microwave
- porous carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 29
- -1 carbon nickel diselenide Chemical compound 0.000 title claims abstract description 9
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 24
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 20
- 150000002815 nickel Chemical class 0.000 claims abstract description 19
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 5
- 239000011669 selenium Substances 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 229910052799 carbon Inorganic materials 0.000 claims description 24
- IJUKXQRCJABGNO-UHFFFAOYSA-N [Se].[Ni]=[Se] Chemical compound [Se].[Ni]=[Se] IJUKXQRCJABGNO-UHFFFAOYSA-N 0.000 claims description 22
- 238000005303 weighing Methods 0.000 claims description 19
- 229910001415 sodium ion Inorganic materials 0.000 claims description 11
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 10
- 239000011358 absorbing material Substances 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 229940078487 nickel acetate tetrahydrate Drugs 0.000 claims description 4
- OINIXPNQKAZCRL-UHFFFAOYSA-L nickel(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Ni+2].CC([O-])=O.CC([O-])=O OINIXPNQKAZCRL-UHFFFAOYSA-L 0.000 claims description 4
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 3
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 claims description 3
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims description 3
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 3
- DOLZKNFSRCEOFV-UHFFFAOYSA-L nickel(2+);oxalate Chemical compound [Ni+2].[O-]C(=O)C([O-])=O DOLZKNFSRCEOFV-UHFFFAOYSA-L 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 239000004570 mortar (masonry) Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000013354 porous framework Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- 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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
-
- 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
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of novel energy materials, and particularly relates to a method for preparing a nitrogen-doped porous carbon nickel diselenide nanocomposite by using a nesting doll type microwave method. The method comprises the following steps: fully mixing a selenium source, a nickel salt and a polyacrylonitrile material, then placing the mixture into a small crucible with a cover, then placing the small crucible with the cover into a large crucible with a cover and filled with copper oxide powder, then placing the whole nesting doll system into a microwave reactor, and successfully synthesizing the nitrogen-doped carbon nickel diselenide nano composite material by controlling the mass ratio, the microwave power and the microwave heating time of the polyacrylonitrile, the selenium source and the nickel salt. The preparation method has the advantages of high efficiency, low production cost and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of novel energy materials, and particularly relates to a method for preparing nickel selenide grown on a nitrogen-doped carbon porous skeleton by using a nesting doll type microwave method.
Background
In terms of large-scale energy storage, sodium ion batteries are considered to be promising substitutes for lithium ionEnergy storage product for a sub-cell. However, due to the ionic radius of sodium
Ionic radius of specific lithium
Large, resulting in slow reaction kinetics, which in turn hinders large-scale application of sodium ion batteries. Therefore, it is necessary to find suitable electrode materials having high capacity and good cycle stability.
In recent years, nitrogen-doped carbon porous frameworks can improve electrical conductivity, accelerate ion transport, increase active sites, and reduce volume expansion. NiSe 2 Has good conductivity (resistivity is lower than 10) -3 Ω cm) is a promising electrode material. Nickel diselenide grows on the nitrogen-doped carbon porous skeleton, and has synergistic effect on improving the storage performance of sodium ions. However, the conventional manufacturing process of the composite material is very time-consuming and requires complicated post-treatments such as templating, hydrothermal and chemical vapor deposition. Therefore, a simple method for manufacturing the porous composite material must be found. Microwave nanotechnology has several advantages over traditional methods of preparation, including ease of handling, uniform heating, and short processing times.
The nesting doll type microwave method adopted for preparing the nickel diselenide nano composite material of the nitrogen-doped porous carbon has the advantages of simple and quick operation and no need of a solvent. In microwave synthesis, microwave absorbing materials are heated through dielectric loss, and the unique heating mechanism can be adopted to accelerate the synthesis speed of the porous composite material and reduce the manufacturing time and energy consumption. The copper oxide powder is used as a microwave absorbing material, so that the nickel diselenide nano composite material of nitrogen-doped porous carbon prepared by the method has the advantages of simplicity, rapidness, environmental friendliness and low price, and the nano composite material has wide application prospect in the field of energy storage.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a nickel diselenide nanocomposite material of nitrogen-doped porous carbon and a method for preparing the nickel diselenide nanocomposite material of nitrogen-doped porous carbon by using a nesting doll type microwave method. The porous carbon doped nickel diselenide nano composite material is successfully synthesized by controlling the mass ratio of polyacrylonitrile to nickel salt and sulfur source, the microwave power and the microwave heating time.
In order to achieve the purpose, the invention adopts the following technical scheme:
the nickel diselenide nano composite material of the nitrogen-doped porous carbon has a nitrogen-doped porous graphite carbon skeleton, and nickel diselenide particles are uniformly distributed on the graphite carbon skeleton.
A method for preparing a nickel diselenide nano composite material of nitrogen-doped porous carbon by using a nesting doll type microwave method comprises the following steps:
(1) Weighing 0.01-200g of polyacrylonitrile by mass;
(2) Weighing selenium powder with the mass part of 0.01-500 g;
(3) Weighing 0.01-500g of nickel salt by mass, putting the nickel salt and the polyacrylonitrile in the step (1) and the selenium powder in the step (2) into a mortar together, fully mixing, uniformly grinding, and putting into a small container with a cover inside, wherein the nickel salt is one or a mixture of nickel nitrate hexahydrate, nickel chloride hexahydrate, nickel acetate tetrahydrate, nickel oxalate and nickel sulfate hexahydrate;
(4) Placing the small container with the inner cover in the step (3) into a large container with an outer cover and copper oxide powder to form a nesting doll system, wherein the copper oxide powder is used as a microwave absorbing material, and the height of the powder needs to reach 1/2-2/3 of the height of the outer wall of the small container with the inner cover;
(5) The whole nesting doll system is put into a microwave reactor, and the nitrogen-doped carbon nickel diselenide nano composite material can be obtained after certain microwave power and heating time, wherein the microwave power is 100-1000W, and the microwave heating time is 1-180min.
According to the method for preparing the nitrogen-doped porous carbon nickel diselenide nanocomposite by using the nesting doll type microwave method, the small container with the inner cover is a 10-milliliter crucible, and the large container with the outer cover is a 50-milliliter crucible.
According to the method for preparing the nitrogen-doped porous carbon nickel diselenide nanocomposite by using the nesting doll type microwave method, the mass ratio of the selenium source to the nickel salt is 1:4-4:1; the mass ratio of polyacrylonitrile to nickel salt is 1.
The nickel diselenide nanocomposite of nitrogen-doped porous carbon prepared by the method for preparing the nickel diselenide nanocomposite of nitrogen-doped porous carbon by using the nesting doll type microwave method is used for preparing electrode plates and assembling sodium ion batteries, the prepared battery capacitance is 290-360mAh/g, and the charging and discharging cycle is still stable for 500-1600 circles.
The invention provides a method for preparing a nickel diselenide nano composite material of nitrogen-doped porous carbon by using a nesting doll type microwave method. Polyacrylonitrile is used as a nitrogen-doped carbon source, the carbonization temperature of the polyacrylonitrile is below 300 ℃, and the polyacrylonitrile can react under the action of microwaves; selenium powder is used as a selenium source; the method adopts a solid phase microwave method, takes copper oxide as a microwave heating layer and polyacrylonitrile as a nitrogen-doped carbon source, and synthesizes the nickel diselenide nano composite material of nitrogen-doped porous carbon in one step. The method has the advantages of rapidness, simplicity, environmental friendliness, low price and the like. The material synthesis method is simple, easy to operate and has good application prospect.
Drawings
Fig. 1 is an X-ray diffraction pattern (XRD pattern) of the nickel diselenide nanocomposite of nitrogen-doped porous carbon prepared in example 1.
Fig. 2 is a scanning electron micrograph (SEM image) of a nickel diselenide nanocomposite of nitrogen-doped porous carbon prepared in example 1.
Detailed Description
The present invention will be described in detail with reference to examples, but the scope of the present invention is not limited to the following examples.
Example 1
(1) 0.10g of nickel nitrate hexahydrate is weighed;
(2) Weighing 0.035g of polyacrylonitrile and 0.20g of selenium powder, uniformly mixing with the nickel salt in the step (1), and placing in a 10 ml small crucible with a cover;
(3) 25g of copper oxide powder was weighed and placed in a 50 ml large crucible with a lid;
(4) And (3) placing the small crucible with the cover in the step (2) in the large crucible with the cover in the step (3) to form a nesting doll system.
(5) And (3) putting the whole nesting doll system into a microwave reactor, wherein the microwave power is 1000W, and the microwave heating time is 20min, so as to obtain a sample.
(6) Preparing an electrode plate from the sample, assembling the sodium ion battery, measuring the capacitance value of 360mAh/g under the current density of 0.2A/g, and keeping the stability after 1000 cycles of charge-discharge cycle.
Example 2
(1) Weighing 10g of nickel acetate tetrahydrate;
(2) Weighing 50g of polyacrylonitrile and 40g of selenium powder, uniformly mixing the polyacrylonitrile and the selenium powder with the nickel salt in the step (1), and placing the mixture in a crucible of 50 ml;
(3) Weighing 100g of copper oxide powder, and placing the copper oxide powder in a 100 ml crucible;
(4) And (3) placing the crucible of 50 ml in the step (2) in the crucible of 100 ml in the step (3) to form a nesting doll system.
(5) And (3) putting the whole nesting doll system into a microwave reactor, wherein the microwave power is 800W, and the microwave heating time is 60min, so as to obtain a sample.
(6) Preparing an electrode plate from the sample, assembling the sodium ion battery, measuring the capacitance value of 300mAh/g under the current density of 1A/g, and keeping the charge-discharge cycle stable for 1600 circles.
Example 3
(1) Weighing 300mg of nickel sulfate hexahydrate;
(2) Weighing 200mg of polyacrylonitrile and 1000mg of selenium powder, uniformly mixing the polyacrylonitrile and the 1000mg of selenium powder with the nickel salt in the step (1), and placing the mixture in a 10 ml crucible;
(3) Weighing 50g of copper oxide powder, and placing the copper oxide powder in a crucible of 50 ml;
(4) And (3) placing the 10 ml crucible in the step (2) in the 50 ml crucible in the step (3) to form a nesting doll system.
(5) And (3) putting the whole nesting doll system into a microwave reactor, wherein the microwave power is 600W, and the microwave heating time is 40min, so as to obtain a sample.
(6) Preparing an electrode plate from the sample, assembling the sodium ion battery, and measuring the capacitance value of 324mAh/g under the current density of 0.2A/g, wherein the charge-discharge cycle is 1400 circles and still keeps stable.
Example 4
(1) 1.0g of nickel acetate tetrahydrate is weighed;
(2) Weighing 0.5g of polyacrylonitrile and 2.0g of selenium powder, uniformly mixing the polyacrylonitrile and the selenium powder with the nickel salt in the step (1), and placing the mixture in a 50 ml small crucible with a cover;
(3) Weighing 50g of copper oxide powder, and placing the copper oxide powder in a 100 ml large crucible with a cover;
(4) And (3) placing the small crucible with the cover in the step (2) in the large crucible with the cover in the step (3) to form a nesting doll system.
(5) And (3) putting the whole nesting doll system into a microwave reactor, wherein the microwave power is 1000W, and the microwave heating time is 40min, so as to obtain a sample.
(6) Preparing electrode plates from the samples, assembling the sodium ion battery, and measuring the capacitance value of 308mAh/g under the current density of 0.2A/g, wherein the stability is still kept after 800 cycles of charge-discharge circulation.
Example 5
(1) 0.05g of nickel oxalate is weighed;
(2) Weighing 0.01g of polyacrylonitrile and 0.40g of selenium powder, uniformly mixing the polyacrylonitrile and the selenium powder with the nickel salt in the step (1), and placing the mixture in a 10 ml small crucible with a cover;
(3) Weighing 25g of copper oxide powder, and placing the copper oxide powder in a 50 ml large crucible with a cover;
(4) And (3) placing the small crucible with the cover in the step (2) in the large crucible with the cover in the step (3) to form a nesting doll system.
(5) And (3) putting the whole nesting doll system into a microwave reactor, wherein the microwave power is 200W, and the microwave heating time is 35min, so as to obtain a sample.
(6) Preparing an electrode plate from the sample, assembling the sodium ion battery, measuring the capacitance value of 290mAh/g under the current density of 1A/g, and keeping the stability after 500 cycles of charge and discharge.
Example 6
(1) 0.03g of nickel chloride hexahydrate is weighed;
(2) Weighing 0.6g of polyacrylonitrile and 0.12g of selenium powder, uniformly mixing the polyacrylonitrile and the selenium powder with the nickel salt in the step (1), and placing the mixture in a 10 ml small crucible with a cover;
(3) Weighing 25g of copper oxide powder, and placing the copper oxide powder in a 50 ml large crucible with a cover;
(4) And (3) placing the small crucible with the cover in the step (2) in the large crucible with the cover in the step (3) to form a nesting doll system.
(5) And (3) putting the whole nesting doll system into a microwave reactor, wherein the microwave power is 800W, and the microwave heating time is 20min, so as to obtain a sample.
Preparing an electrode plate from the sample, assembling the sodium ion battery, and measuring the capacitance value of 321mAh/g under the current density of 0.1A/g, wherein the charge-discharge cycle is still stable for 1200 circles.
Claims (5)
1. The nitrogen-doped porous carbon nickel diselenide nano composite material is characterized by having a nitrogen-doped porous graphite carbon skeleton, and nickel diselenide particles are uniformly distributed on the graphite carbon skeleton.
2. A method for preparing a nickel diselenide nano composite material of nitrogen-doped porous carbon by a nesting doll type microwave method is characterized by comprising the following steps:
(1) Weighing 0.01-200g of polyacrylonitrile in parts by mass;
(2) Weighing selenium powder with the mass part of 0.01-500 g;
(3) Weighing 0.01-500g of nickel salt by mass, putting the nickel salt and the polyacrylonitrile in the step (1) and the selenium powder in the step (2) into a mortar together, fully mixing, uniformly grinding, and putting into a small container with a cover inside, wherein the nickel salt is one or a mixture of nickel nitrate hexahydrate, nickel chloride hexahydrate, nickel acetate tetrahydrate, nickel oxalate and nickel sulfate hexahydrate;
(4) Placing the small container with the inner cover in the step (3) into a large container with an outer cover and copper oxide powder to form a nesting doll system, wherein the copper oxide powder is used as a microwave absorbing material, and the height of the powder needs to reach 1/2-2/3 of the height of the outer wall of the small container with the inner cover;
(5) Putting the whole nesting doll system into a microwave reactor, and obtaining the nitrogen-doped carbon nickel diselenide nano composite material after certain microwave power and heating time, wherein the microwave power is 100-1000W, and the microwave heating time is 1-180min.
3. The method for preparing the nickel diselenide nanocomposite of nitrogen-doped porous carbon by using the nesting doll type microwave method as claimed in claim 1, wherein the small container with the inner cover is a 10 ml crucible, and the large container with the outer cover is a 50 ml crucible.
4. The method for preparing the nickel diselenide nanocomposite material of nitrogen-doped porous carbon by using the nesting doll type microwave method according to claim 1, wherein the mass ratio of the selenium source to the nickel salt is 1:4-4:1; the mass ratio of polyacrylonitrile to nickel salt is 1.
5. The method for preparing the nickel diselenide nanocomposite of nitrogen-doped porous carbon according to any one of claims 2 to 4, wherein the nickel diselenide nanocomposite of nitrogen-doped porous carbon prepared by the method for preparing the nickel diselenide nanocomposite of nitrogen-doped porous carbon by using the nesting doll type microwave method is used for preparing electrode plates and assembling sodium ion batteries, the prepared battery capacitance is 290-360mAh/g, and the charging and discharging cycle is still stable for 500-1600 circles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211246343.7A CN115490211B (en) | 2022-10-12 | 2022-10-12 | Method for preparing nitrogen-doped porous carbon nickel diselenide nanocomposite by using nested doll type microwave method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211246343.7A CN115490211B (en) | 2022-10-12 | 2022-10-12 | Method for preparing nitrogen-doped porous carbon nickel diselenide nanocomposite by using nested doll type microwave method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115490211A true CN115490211A (en) | 2022-12-20 |
| CN115490211B CN115490211B (en) | 2024-01-09 |
Family
ID=84473688
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211246343.7A Active CN115490211B (en) | 2022-10-12 | 2022-10-12 | Method for preparing nitrogen-doped porous carbon nickel diselenide nanocomposite by using nested doll type microwave method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115490211B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106025244A (en) * | 2016-07-30 | 2016-10-12 | 复旦大学 | Nickel selenide/graphene/carbon nanotube composite material and preparation method thereof |
| CN113511647A (en) * | 2021-04-22 | 2021-10-19 | 广东工业大学 | Preparation method of nickel diselenide/reduced graphene oxide composite material derived from nickel-based metal organic framework |
-
2022
- 2022-10-12 CN CN202211246343.7A patent/CN115490211B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106025244A (en) * | 2016-07-30 | 2016-10-12 | 复旦大学 | Nickel selenide/graphene/carbon nanotube composite material and preparation method thereof |
| CN113511647A (en) * | 2021-04-22 | 2021-10-19 | 广东工业大学 | Preparation method of nickel diselenide/reduced graphene oxide composite material derived from nickel-based metal organic framework |
Non-Patent Citations (2)
| Title |
|---|
| JIAQI LI ET AL.: "Microwave synthesis of Sb2Se3/polyacrylonitrilebased carbon fiber mat electrodes for high performance flexible capacitors and hydrogen evolution reaction", INTERNATIONAL JOURNAL OF HYDROGEN ENERGY, vol. 47, no. 73, XP087174796, DOI: 10.1016/j.ijhydene.2022.07.059 * |
| 黄招娣: "硒化镍@氮掺杂碳复合材料的可控合成及电催化性能", 中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑, pages 52 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115490211B (en) | 2024-01-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105895886B (en) | A kind of sodium-ion battery transition metal phosphide/porous anode composite and preparation method thereof | |
| CN113410440B (en) | Cobalt diselenide @ porous nitrogen-doped carbon nanocomposite, potassium ion battery and preparation method of cobalt diselenide @ porous nitrogen-doped carbon nanocomposite | |
| CN113725432B (en) | ZIF-67 and preparation method of cobalt selenide/carbon electrode material derived from ZIF-67 | |
| CN110734097B (en) | ZIF 67-containing derived composite carbon material lithium-sulfur battery positive electrode material, preparation method thereof, positive electrode plate containing positive electrode material and lithium-sulfur battery | |
| CN111933933A (en) | Novel lithium ion battery cathode material and preparation method thereof | |
| CN104860349B (en) | Titanium dioxide hollow ball that a kind of nanometer rods are constructed and preparation method and application | |
| CN111933934A (en) | Battery negative electrode material and preparation method thereof | |
| CN106252630A (en) | A kind of lithium-sulfur cell rich nitrogen hollow carbon balls/sulfur composite positive pole and preparation method thereof | |
| CN110518188A (en) | A kind of selenium-phosphorus-carbon composite and the preparation method and application thereof | |
| CN114388814A (en) | Preparation method of Co0.85Se nanoparticle @3D carbon network composite material and application of composite material in lithium-sulfur battery | |
| CN116936771A (en) | Hollow spherical shell structure ferric sodium sulfate composite positive electrode material, preparation method and sodium ion battery | |
| CN106920937A (en) | A kind of preparation method of electrode composite material | |
| CN111463406B (en) | Preparation method of cobalt-doped zinc-based metal selenide composite electrode for lithium ion battery | |
| CN115490211B (en) | Method for preparing nitrogen-doped porous carbon nickel diselenide nanocomposite by using nested doll type microwave method | |
| CN114759188B (en) | Potassium ion battery negative electrode material and preparation method and application thereof | |
| CN114068904B (en) | Carbon-coated tin-based chalcogenide composite material and preparation method and application thereof | |
| CN106611846B (en) | Negative electrode of lithium ion battery α-LiFeO2The synthetic method of/porous carbon composite | |
| CN115207344B (en) | Preparation of FexSey@CN composite material and electrochemical energy storage application thereof | |
| CN113690422B (en) | Hollow nanocube multi-element metal compound composite material with layered structure, preparation method and application in lithium ion battery | |
| CN115472797A (en) | Porous carbon supported interlamellar spacing expansion molybdenum disulfide compound and preparation method and application thereof | |
| CN109786728B (en) | NbOPO4 nanosheet/rGO composite material and preparation method and application thereof | |
| CN108963214B (en) | Preparation method of lithium ion battery negative electrode material | |
| CN114725356B (en) | Mn-based heterogeneous compound/carbon composite material with limited domain structure and preparation method and application thereof | |
| CN113871587B (en) | Preparation method of silicon @ carbon nanotube @ carbon composite negative electrode material of lithium ion battery | |
| CN115490213B (en) | VSe derived from metal-organic frameworks 2 Material, preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |