CN111547705B - Preparation method of porous carbon electrode material - Google Patents
Preparation method of porous carbon electrode material Download PDFInfo
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- CN111547705B CN111547705B CN202010395395.5A CN202010395395A CN111547705B CN 111547705 B CN111547705 B CN 111547705B CN 202010395395 A CN202010395395 A CN 202010395395A CN 111547705 B CN111547705 B CN 111547705B
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/18—Conductive material dispersed in non-conductive inorganic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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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
- H01G11/44—Raw materials therefor, e.g. resins or coal
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a porous carbon electrode material, which takes manganese salt and tartrate as raw materials, and prepares the porous carbon electrode material by hydrothermal reaction carbonization and nitrogen-sulfur doping; the manganese salt is one of manganese chloride, manganese bromide and manganese nitrate; the tartrate is one of potassium sodium tartrate, ammonium sodium tartrate and antimony sodium tartrate; the nitrogen source is one of urea, biuret, N-methylurea, N-ethylurea, N-propylurea and N-isopropylurea; the sulfur source is one of thiourea, methyl thiourea, ethyl thiourea, propyl thiourea and butyl thiourea; the molar ratio of the manganese salt to the tartrate is 0.8-1.2; the nitrogen source is 0-20 wt% of the porous carbon electrode material in percentage by mass; the sulfur source is 0-15 wt% of the porous carbon electrode material. After the porous carbon is compounded with electrode materials such as selenium, sulfur, silicon and the like, the lithium storage performance is very excellent, and the application prospect is good. The porous carbon electrode material has simple and controllable preparation process and convenient operation, and is suitable for industrial production.
Description
Technical Field
The invention relates to a preparation method of an electrode material, in particular to a preparation method of a porous carbon electrode material.
Background
The carbon material has the characteristics of high conductivity, good hydrothermal stability, large comparative area, porous structure and the like, and is widely applied to new energy devices such as lithium ion batteries, supercapacitors and the like; particularly as a carrier, the electrochemical performance of electrode materials such as sulfur, selenium, silicon and the like is effectively improved.
Gao et al adopt sea sedge as raw material, firstly carbonizing at 500 deg.C, then mixing the product with sodium aluminate, and reacting at 500-900 deg.C to obtain 1-2 nm microporous-mesoporous carbon material with BET specific surface area and pore volume up to 1374m2G and 1.15cm3/g.(Gao Y,et al.Chemical Engineering J,2015,274:76-83.)
Yang et al utilize calcium citrate to crack at a high temperature of 700-. The calcium carbonate and calcium oxide materials can be recycled, and the problems of chemical resource waste and potential environmental pollution caused by the removal of other templates such as silicon dioxide and the like are solved. (Yang J, et al, Microporous Mesoporus Mater.,2014,183(1):91-98.)
A Sanche-sanchez synthesizes nitrogen-doped mesoporous carbon by using SBA-15 as a template and acetonitrile as a carbon source and a nitrogen source, wherein the average size of the carbon material is 3.36 nanometers. (A.Sanche-sanchez, et al.J. Colloid and Interface Science,2015,450:91-100)
However, the methods all require the adjustment of the pore structure of the carbon material by a template, and the yield of the mesoporous carbon product is low, so that the industrial production is difficult to realize.
Disclosure of Invention
Aiming at the defects of the prior art scheme, the invention aims to provide a preparation method of a porous carbon electrode material.
A preparation method of a porous carbon electrode material comprises the steps of taking manganese salt and tartrate as raw materials, carbonizing through a hydrothermal reaction, and doping nitrogen and sulfur to prepare the porous carbon electrode material; the manganese salt is one of manganese chloride, manganese bromide and manganese nitrate; the tartrate is one of potassium sodium tartrate, ammonium sodium tartrate and antimony sodium tartrate; the nitrogen source is one of urea, biuret, N-methylurea, N-ethylurea, N-propylurea and N-isopropylurea; the sulfur source is one of thiourea, methyl thiourea, ethyl thiourea, propyl thiourea and butyl thiourea;
a preparation method of a porous carbon electrode material comprises the following steps:
1) weighing tartrate and manganese salt in a certain molar ratio, dissolving the tartrate and the manganese salt in water, violently stirring for 1-2 hours, and reacting the obtained product at 120-240 ℃ for 10-20 hours; washing and drying the obtained product;
2) mixing the product obtained in the step 1) with a nitrogen source according to a certain proportion, dispersing in water, and reacting the obtained product at 120-240 ℃ for 5-10 hours; washing and drying the obtained product, and carrying out heat treatment on the dried product at 400-900 ℃ for 5-10 hours in an inert atmosphere;
3) mixing the product obtained in the step 2) with a sulfur source according to a certain proportion, dispersing in water, and reacting the obtained product for 5-10 hours at 120-240 ℃; washing and drying the obtained product, and annealing the dried product at 400-900 ℃ for 1-2 hours to prepare a porous carbon electrode material;
the molar ratio of the manganese salt to the tartrate is 0.8-1.2;
the nitrogen source is 0-20 wt% of the porous carbon electrode material in percentage by mass;
the sulfur source is 0-15 wt% of the porous carbon electrode material in percentage by mass.
The porous carbon material produced by the method can be applied to the negative electrode of a lithium ion battery and can also be used as a super capacitor material;
the porous carbon material produced by the method can be applied to carriers and conductive agents of selenium, sulfur and silicon electrode materials.
Compared with the prior art, the preparation method of the porous carbon electrode material provided by the invention has the following advantages:
1) the preparation process is simple, the raw material cost is low, and the industrial production can be realized;
2) the manganese salt reacts with tartrate, and the carbonization temperature is reduced; the nitrogen source and the sulfur source are doped, so that the pore structure of the carbon material is enlarged; the porous carbon size is nanoscale.
3) The porous carbon prepared by the method is of an ant nest-shaped structure and has rich nano gaps; the three-dimensional nano structure and the synergistic effect of nitrogen and sulfur doping enable the carbon material to be more beneficial to stable deposition of electrode materials such as sulfur, selenium, silicon and the like on the surface of the electrode materials.
4) After the porous carbon prepared by the method is compounded with electrode materials such as selenium, sulfur, silicon and the like, the electrochemical performance of the electrode materials such as selenium, sulfur, silicon and the like is obviously improved.
Detailed Description
In order to further understand the contents, features and effects of the present invention, the following embodiments are described in detail as follows:
example 1
A preparation method of a porous carbon electrode material comprises the following steps:
1) weighing tartrate and manganese salt with a certain molar ratio, dissolving in water, stirring vigorously for 2 hours, and reacting the obtained product at 180 ℃ for 10 hours; washing and drying the obtained product;
2) mixing the product obtained in the step 1) with a nitrogen source according to a certain proportion, dispersing in water, and reacting the obtained product for 5 hours at 180 ℃; washing and drying the obtained product, and carrying out heat treatment on the dried product for 5 hours at 600 ℃ in an inert atmosphere;
3) mixing the product obtained in the step 2) with a sulfur source according to a certain proportion, dispersing the mixture in water, and reacting the obtained product for 5 hours at 180 ℃; and washing and drying the obtained product, and annealing the dried product at 600 ℃ for 2 hours to obtain the porous carbon electrode material.
A compositional design of a porous carbon electrode material, comprising:
1) the molar ratio of manganese chloride to potassium sodium tartrate is 1: 1; the urea accounts for 10 wt% of the carbonized products of manganese chloride and potassium sodium tartrate; thiourea accounts for 8 wt% of the carbonized product of manganese chloride and potassium sodium tartrate;
the porous carbon electrode material and selenium powder are uniformly mixed according to the mass ratio of 3.5:6.5, then ball milling is carried out for 6 hours, and ball milling products are placed into a tube furnace to be annealed for 6 hours at 300 ℃ to obtain the nitrogen-doped porous carbon loaded selenium electrode material. The charging and discharging voltage range is 1-3V, the current density is 200mA/g, the discharging specific capacity of the porous carbon load selenium electrode material after 50 cycles is larger than 400mAh/g, and the charging and discharging capacity is far larger than 206mAh/g of the selenium electrode under the same condition.
Example 2
The procedure is as in example 1.
A compositional design of a porous carbon electrode material, comprising:
2) the molar ratio of manganese nitrate to sodium ammonium tartrate is 1.1: 1; the biuret accounts for 8 wt% of the mass percentage of the carbonized products of the manganese nitrate and the ammonium sodium tartrate; the methylthiourea accounts for 12 wt% of the carbonization products of the manganese nitrate and the ammonium sodium tartrate;
the porous carbon electrode material and selenium powder are uniformly mixed according to the mass ratio of 3.5:6.5, then ball milling is carried out for 6 hours, and ball milling products are placed into a tube furnace to be annealed for 6 hours at 300 ℃ to obtain the nitrogen-doped porous carbon loaded selenium electrode material. The charging and discharging voltage range is 1-3V, the current density is 200mA/g, the discharging specific capacity of the porous carbon load selenium electrode material after 50 cycles is larger than 400mAh/g, and the charging and discharging capacity is far larger than 206mAh/g of the selenium electrode under the same condition.
Example 3
The procedure is as in example 1.
A compositional design of a porous carbon electrode material, comprising:
3) the molar ratio of the manganese bromide to the potassium sodium tartrate is 0.9: 1; the N-methylurea accounts for 15 wt% of the mass percentage of the carbonized products of the manganese nitrate and the ammonium sodium tartrate; the ethyl thiourea is 9 wt% of the carbonized product of the manganese bromide and the potassium sodium tartrate in percentage by mass;
the porous carbon electrode material and selenium powder are uniformly mixed according to the mass ratio of 3.5:6.5, then ball milling is carried out for 6 hours, and ball milling products are placed into a tube furnace to be annealed for 6 hours at 300 ℃ to obtain the nitrogen-doped porous carbon loaded selenium electrode material. The charging and discharging voltage range is 1-3V, the current density is 200mA/g, the discharging specific capacity of the porous carbon load selenium electrode material after 50 cycles is larger than 400mAh/g, and the charging and discharging capacity is far larger than 206mAh/g of the selenium electrode under the same condition.
The above-described embodiments of the patent are intended to be illustrative, but not limiting, of the scope of the patent, which is included for the purpose of better understanding the patent by those skilled in the art; any equivalent alterations or modifications made according to the spirit of the disclosure of this patent are intended to be included in the scope of this patent.
Claims (4)
1. A preparation method of a porous carbon electrode material is characterized by comprising the following steps: manganese salt and tartrate are used as raw materials, and carbonization and nitrogen-sulfur doping are carried out through hydrothermal reaction to prepare the porous carbon electrode material; the manganese salt is one of manganese chloride, manganese bromide and manganese nitrate; the tartrate is one of potassium sodium tartrate, ammonium sodium tartrate and antimony sodium tartrate; the nitrogen source is one of urea, biuret, N-methylurea, N-ethylurea, N-propylurea and N-isopropylurea; the sulfur source is one of thiourea, methyl thiourea, ethyl thiourea, propyl thiourea and butyl thiourea; a preparation method of a porous carbon electrode material comprises the following steps:
1) weighing tartrate and manganese salt in a certain molar ratio, dissolving the tartrate and the manganese salt in water, violently stirring for 1-2 hours, and reacting the obtained product at 120-240 ℃ for 10-20 hours; washing and drying the obtained product;
2) mixing the product obtained in the step 1) with a nitrogen source according to a certain proportion, dispersing in water, and reacting the obtained product at 120-240 ℃ for 5-10 hours; washing and drying the obtained product, and carrying out heat treatment on the dried product at 400-900 ℃ for 5-10 hours in an inert atmosphere;
3) mixing the product obtained in the step 2) with a sulfur source according to a certain proportion, dispersing in water, and reacting the obtained product for 5-10 hours at 120-240 ℃; and washing and drying the obtained product, and annealing the dried product at 400-900 ℃ for 1-2 hours to obtain the porous carbon electrode material.
2. The method for preparing a porous carbon electrode material according to claim 1, wherein the molar ratio of the manganese salt to the tartrate is 0.8 to 1.2.
3. The preparation method of the porous carbon electrode material, as recited in claim 1, characterized in that the nitrogen source is 8-20 wt% of the carbonized product of manganese salt and tartrate.
4. The preparation method of the porous carbon electrode material, as recited in claim 1, characterized in that the sulfur source is 8-15 wt% of the manganese salt and tartrate carbonized product in mass percent.
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2020
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