CN103730638A - Preparation method of nitrogen-doped carbon material - Google Patents
Preparation method of nitrogen-doped carbon material Download PDFInfo
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- CN103730638A CN103730638A CN201310478193.7A CN201310478193A CN103730638A CN 103730638 A CN103730638 A CN 103730638A CN 201310478193 A CN201310478193 A CN 201310478193A CN 103730638 A CN103730638 A CN 103730638A
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a nitrogen-doped carbon material. The carbon material has a mesoporous structure and is doped with nitrogen, and the doping content of the nitrogen in the carbon material is controllable; a composite of the carbon material is modified by the carbon material; and the preparation method selects egg white as a raw material to form the nitrogen-doped carbon material through high-temperature calcination and carbonization in the inert atmosphere, and comprises steps as follows: (1), an egg white solution is taken as a solvent for material composition; (2), the egg white is steamed in boiling water and forms tin dioxide jelly similar to yellow cake; and (3), calcination is performed in the inert atmosphere to obtain the nitrogen-doped carbon material. with the adoption of the method, the nitrogen-doped carbon composite material with a carbon coating structure can be prepared, and the content of the nitrogen in the carbon material is controllable; and the prepared nitrogen-doped carbon composite material is suitable for being taken as a Li-ion electrode material, and is simultaneously applicable to the fields of corrosion resistance, gas absorption and the like.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic functional material, particularly relate to a kind of method that adopts high-temperature calcination under inert atmosphere to prepare nitrogenous material with carbon element, belong to inorganic advanced nano material fabricating technology field.
Background technology
It is high that lithium ion battery has voltage, and specific capacity is large, and the plurality of advantages such as discharging voltage balance and fail safe height have become one of the focus of the research and development of novel secondary field of chemical power source, and the improvement of its performance mainly depends on anode and cathode active materials.At present, the negative material of commercial applications is mainly graphitized carbon material, but the theoretical capacity of material with carbon element is only 372mAh/g, along with social progress, traditional graphitized carbon material has been difficult to meet the demand of people to cathode material for high capacity lithium ion battery.
With graphite-phase ratio, the interlamellar spacing of amorphous carbon is larger, can accelerate lithium ion diffusion, simultaneously the isotropic architectural feature of amorphous carbon also makes the lithium ion therein can free diffusing, the amorphous carbon on graphite granule top layer can guide lithium ion to enter the interlayer of graphite fast, and this is all conducive to improve the high rate during charging-discharging of electrode.Amorphous carbon can carry out modification by several different methods, to reach different effects.Doping is a kind of conventional method, by doping nitrogen or boron element, can change the electronic property of semi-conducting material.Graphitic carbon material band structure after doping changes, and conductivity improves, and therefore the graphitic carbon material after doping has larger development space than original graphitic carbon material.In protein, contain carbon and nitrogen element, therefore by calcining protein under high temperature inert atmosphere, can make it that carburizing reagent occurs, the last only amorphous carbon of remaining nitrogen doping.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of nitrogenous material with carbon element, this preparation method's technique is simple, cost is low, the material with carbon element of preparation has meso-hole structure, in material with carbon element doped with nitrogen element, and can control nitrogen element content in material with carbon element, the composite material of its composite material for modifying through this kind of material with carbon element, is suitable as lithium ion battery negative material.
Above-mentioned purpose of the present invention is achieved through the following technical solutions: take egg solution as raw material high-temperature calcination carbonization formation nitrogen-doped carbon material under anaerobic condition, concrete preparation process comprises:
(1) get after fresh-laid egg clear liquid stirs homogeneous processing in 1-48 hour and filter removal impurity, add in proportion deionized water and be uniformly mixed, the content of controlling water is 0-500%;
(2) in egg white solution, add powder tin ash, stir after 0.1-12 hour ultrasonic to being uniformly dispersed;
(3) with steam heating, make egg molecule degeneration shrink pack be layed onto tin ash surface;
(4) centrifugal, washing, dry after under inert atmosphere 300-700 ℃ of calcining 1-6 hour, obtain nitrogen-doped carbon and tin ash composite material;
The described egg of step (1) also can adopt the aqueous solution of other oroteins or peptide matters to replace, and product material with carbon element is still rich in nitrogen, and the preparation method of its composite material still has applicability;
The egg white solution that step (1) is described, can by add glucose and regulate and control egg white and glucose between mass ratio, reach in regulation and control product the content of nitrogen element in material with carbon element;
The described nitrogenous material with carbon element of step (4) has meso-hole structure, and when not adding tin ash, this material with carbon element can be for composite sulfur simple substance, elementary silicon as li-ion electrode materials;
The described nitrogenous carbon composite of step (4) can be removed metal oxide by subsequent corrosion means, and residue has the nitrogenous material with carbon element of hollow-core construction.
Technique scheme of the present invention has the following advantages:
1) reaction mechanism of the present invention is to utilize in protein molecule the nitrogen element of self, forms the amorphous carbon of nitrogen doping by inert atmosphere high-temperature calcination.
2) albumen water soluble used of the present invention, is convenient to the synthetic of composite material; And during protein generation sex change, shrink and compound phase can be wrapping to the composite material that forms clad structure in protein, be conducive to alleviate the volumetric expansion of compound phase.
3) the present invention, by albumen is mixed in proportion with glucose, can realize the regulation and control of the doping content of nitrogen element in amorphous carbon.
4) the present invention does not need special process equipment, can utilize rotten egg and other protein etc., and waste material recycling can reduce production costs, and Technology for Heating Processing is simple.
Accompanying drawing explanation
Fig. 1 is the field transmitting low power morphology observation of the nitrogen doped amorphous carbon prepared of the present invention
Fig. 2 is the coated Fe of nitrogen doped amorphous carbon prepared by the present invention
3o
4the field transmitting morphology observation of composite material
Embodiment
Below in conjunction with example, further illustrate particular content of the present invention.
The invention discloses a kind of preparation method of nitrogen-doped carbon material, described material with carbon element has meso-hole structure, in material with carbon element, doped with nitrogen element, and can control nitrogen-doping content in material with carbon element, the composite material of its composite material for modifying through this kind of material with carbon element; Preparation method selects the high-temperature calcination carbonization under inert atmosphere of egg raw material to form nitrogen-doped carbon material, comprises the following steps: (1) be take egg solution and carried out the compound of material as solvent; (2) boiling water cooks egg, forms the jelly of similar sponge cake tin ash; (3) under inert atmosphere, calcining obtains nitrogen-doped carbon composite material.This method can make has the coated structural composite material of nitrogen-doped carbon, and in material with carbon element, nitrogen element content is controlled; The nitrogen-doped carbon composite material making is suitable as li-ion electrode materials, is also applicable to the fields such as anticorrosive and gas absorption simultaneously.
Embodiment mono-
(1) get egg white solution stirring and carry out homogeneous processing in 24 hours, then by filtration, remove impurity, 40 grams of egg white solutions join in 30 ml deionized water and are uniformly mixed;
(2) egg white solution is heated in the steam of boiling water, egg molecule generation sex change is shunk, form the colloid that is similar to sponge cake;
(3) under nitrogen protection, 500 ℃ of calcinings can obtain the amorphous carbon that nitrogen adulterates for 3 hours;
Embodiment bis-
(1) get egg white solution stirring and carry out homogeneous processing in 12 hours, then by filtration, remove impurity, 20 grams of egg white solutions join in 20 ml deionized water and are uniformly mixed;
(2) in egg white solution, add 0.5 gram of tin ash, stir after 1 hour ultrasonic to being uniformly dispersed;
(3) suspension is heated in the steam of boiling water, egg molecule generation sex change is shunk, form the colloid that is similar to sponge cake;
(4) centrifugal, washing, dry after under inert atmosphere 500 ℃ of calcinings within 6 hours, can obtain the coated tin ash composite material of nitrogen-doped carbon;
Embodiment tri-
(1) get egg white solution stirring and carry out homogeneous processing in 48 hours, then by filtration, remove impurity, 30 grams of egg white solutions are added in 30 ml deionized water and are uniformly mixed;
(2) in egg white solution, add 1 gram of glucose, 0.5 gram of tin ash, stirs after 1 hour ultrasonic to being uniformly dispersed;
(3) suspension is heated in the steam of boiling water, egg molecule generation sex change is shunk, form the colloid that is similar to sponge cake;
(4) after dry, under inert atmosphere, 600 ℃ of calcinings can obtain the coated tin ash composite material of nitrogen-doped carbon for 6 hours;
Embodiment tetra-
(1) get egg white solution stirring and carry out homogeneous processing in 48 hours, then by filtration, remove impurity, 20 grams of egg white solutions are added in 20 ml deionized water and are uniformly mixed;
(2) in egg white and glucose mixed solution, add 2.16 grams of iron chloride, after ultrasonic 30 minutes, stir 2 hours; Add 20 milliliters of hydrazine hydrates;
(3) suspension is incubated to 20 hours under 140 degree in reactor, prepares Fe
3o
4composite material with protein;
(4) after dry, under inert atmosphere, 500 ℃ of calcinings can obtain the coated Fe of nitrogen-doped carbon for 3 hours
3o
4composite material;
Embodiment five
(1) get egg white solution and stir and to carry out homogeneous processing in 10 hours, then by filtration, remove impurity, 30 grams of egg white solutions and glucose in mass ratio 50:1 are mixed to join in 80 ml deionized water and are uniformly mixed;
(2) in egg white and glucose mixed solution, add iron chloride, stir 1 hour to dissolving, add sodium hydroxide solution to generate FeOOH suspension;
(3) make egg molecule degeneration shrink pack overlay on hydroxyl oxidize iron surface 100 ℃ of heating of suspension;
(4) centrifugal, washing, dry after under inert atmosphere 500 ℃ of calcinings within 6 hours, can obtain nitrogen-doped carbon and Fe
3o
4composite material;
(5) in composite material, add hydrochloric acid, by the Fe in composite material
3o
4erosion removal, obtains hollow nitrogen doped amorphous carbon, to high temperature in amorphous carbon material, injects sulphur simple substance, can be used for the electrode of lithium-sulfur cell.
Embodiment six
(1) get egg white solution stirring and carry out homogeneous processing in 20 hours, then by filtration, remove impurity, 30 grams of egg white solutions mix with deionized water for stirring;
(2) 100 ℃ of heating of suspension are made egg molecule degeneration shrink;
(3) after dry, under inert atmosphere, 500 ℃ of calcinings can obtain nitrogen doped amorphous carbon in 6 hours;
(4) to high temperature in nitrogen doped amorphous carbon, inject sulphur simple substance, can be used for the electrode of lithium-sulfur cell.
Claims (5)
1. a preparation method for nitrogen-doped carbon material, is characterized in that:
Described material with carbon element is meso-hole structure, in material with carbon element, doped with nitrogen element, and can control nitrogen-doping content in material with carbon element, and its composite material is this kind of composite material that material with carbon element is coated; Take egg solution as raw material high-temperature calcination carbonization formation nitrogen-doped carbon material under anaerobic condition, and concrete preparation process comprises:
(1) get fresh-laid egg clear liquid and stir 1-48 hour, homogeneous filters and removes impurity after processing, and adds in proportion deionized water and is uniformly mixed, and the content of controlling water is 0-500%;
(2) in egg white solution, add powder tin ash, stir after 0.1-12 hour ultrasonic to being uniformly dispersed;
(3) with steam heating, make egg molecule degeneration shrink pack be layed onto tin ash surface;
(4) centrifugal, washing, dry after under inert atmosphere 300-700 ℃ of calcining 1-6 hour, obtain nitrogen-doped carbon and tin ash composite material.
2. the preparation method of a kind of nitrogen-doped carbon material according to claim 1, is characterized in that:
The aqueous solution of the egg white described in step (1) or employing other oroteins or peptide matters replaces, and product material with carbon element is still rich in nitrogen, and the preparation method of its composite material still has applicability.
3. the preparation method of a kind of nitrogen-doped carbon material according to claim 1, is characterized in that:
Egg white solution described in step (1), or by add glucose and regulate and control egg white and glucose between mass ratio, reach in regulation and control product the content of nitrogen element in material with carbon element.
4. the preparation method of a kind of nitrogen-doped carbon material according to claim 1, is characterized in that:
Nitrogenous material with carbon element described in step (4) has meso-hole structure, and when not adding tin ash, this material with carbon element is used for composite sulfur simple substance, elementary silicon as li-ion electrode materials.
5. the preparation method of a kind of nitrogen-doped carbon material according to claim 1, is characterized in that:
Nitrogenous carbon composite described in step (4), or remove metal oxide by subsequent corrosion means, residue has the nitrogenous material with carbon element of hollow-core construction.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103979530A (en) * | 2014-06-11 | 2014-08-13 | 安徽工业大学 | Method for preparing porous carbon for electrochemical capacitor from egg white used as raw material |
| CN103992144A (en) * | 2014-05-20 | 2014-08-20 | 中国科学技术大学 | Method for preparing nitrogen/carbon-containing material by biomass pyrolysis and carbonization |
| CN105655154A (en) * | 2016-01-11 | 2016-06-08 | 河南师范大学 | Preparation method for preparing electrode material of super capacitor made of graphene-active carbon compounds |
| CN105977491A (en) * | 2016-06-08 | 2016-09-28 | 北京化工大学 | Nitrogen-doped hierarchical porous carbon electrode material and application thereof |
| CN106410215A (en) * | 2016-09-20 | 2017-02-15 | 福建农林大学 | Preparation method of N-doped hematite electrode material |
| CN106996946A (en) * | 2017-03-31 | 2017-08-01 | 温州大学 | N doping circle carbon plate and tin-oxide composite and its preparation method and application |
| CN108063254A (en) * | 2017-11-14 | 2018-05-22 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of nitrogen carbon coating niobium pentaoxide material |
| CN108400300A (en) * | 2018-02-11 | 2018-08-14 | 长沙理工大学 | A kind of titanium dioxide/nitrogen-doped carbon cladding SnO2Combination electrode material and preparation method thereof |
| CN108598411A (en) * | 2018-04-20 | 2018-09-28 | 湖北工程学院 | Carbon adulterates nitrogen cladding tin oxide/ferric oxide composite material and preparation method thereof, lithium battery material |
| CN108690677A (en) * | 2018-06-20 | 2018-10-23 | 深圳烯创美科技有限公司 | A kind of modified graphene lubricating oil and preparation method |
| CN108987719A (en) * | 2018-07-27 | 2018-12-11 | 盐城市新能源化学储能与动力电源研究中心 | A kind of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material and preparation method thereof |
| CN110600719A (en) * | 2019-09-12 | 2019-12-20 | 河南电池研究院有限公司 | Porous silicon-carbon lithium ion battery cathode material with high rate performance and preparation method thereof |
| CN115050945A (en) * | 2022-07-15 | 2022-09-13 | 湖北工业大学 | Preparation method of biomass nitrogen-doped carbon-coated lithium-rich lithium iron phosphate positive electrode material |
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Cited By (18)
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| CN103992144A (en) * | 2014-05-20 | 2014-08-20 | 中国科学技术大学 | Method for preparing nitrogen/carbon-containing material by biomass pyrolysis and carbonization |
| CN103992144B (en) * | 2014-05-20 | 2016-03-30 | 中国科学技术大学 | A kind of method being prepared nitrogenous carbon material by biomass pyrolytic carbonization |
| CN103979530A (en) * | 2014-06-11 | 2014-08-13 | 安徽工业大学 | Method for preparing porous carbon for electrochemical capacitor from egg white used as raw material |
| CN105655154A (en) * | 2016-01-11 | 2016-06-08 | 河南师范大学 | Preparation method for preparing electrode material of super capacitor made of graphene-active carbon compounds |
| CN105655154B (en) * | 2016-01-11 | 2018-05-01 | 河南师范大学 | A kind of preparation method of graphene-activity Carbon composites electrode material for super capacitor |
| CN105977491A (en) * | 2016-06-08 | 2016-09-28 | 北京化工大学 | Nitrogen-doped hierarchical porous carbon electrode material and application thereof |
| CN106410215A (en) * | 2016-09-20 | 2017-02-15 | 福建农林大学 | Preparation method of N-doped hematite electrode material |
| CN106996946A (en) * | 2017-03-31 | 2017-08-01 | 温州大学 | N doping circle carbon plate and tin-oxide composite and its preparation method and application |
| CN108063254A (en) * | 2017-11-14 | 2018-05-22 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of nitrogen carbon coating niobium pentaoxide material |
| CN108400300A (en) * | 2018-02-11 | 2018-08-14 | 长沙理工大学 | A kind of titanium dioxide/nitrogen-doped carbon cladding SnO2Combination electrode material and preparation method thereof |
| CN108400300B (en) * | 2018-02-11 | 2019-08-02 | 长沙理工大学 | A kind of titanium dioxide/nitrogen-doped carbon cladding SnO2Combination electrode material and preparation method thereof |
| CN108598411A (en) * | 2018-04-20 | 2018-09-28 | 湖北工程学院 | Carbon adulterates nitrogen cladding tin oxide/ferric oxide composite material and preparation method thereof, lithium battery material |
| CN108690677A (en) * | 2018-06-20 | 2018-10-23 | 深圳烯创美科技有限公司 | A kind of modified graphene lubricating oil and preparation method |
| CN108987719A (en) * | 2018-07-27 | 2018-12-11 | 盐城市新能源化学储能与动力电源研究中心 | A kind of three-dimensional sulfur doping porous carbon/stannic oxide combination electrode material and preparation method thereof |
| CN108987719B (en) * | 2018-07-27 | 2020-11-03 | 盐城市新能源化学储能与动力电源研究中心 | Three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material and preparation method thereof |
| CN110600719A (en) * | 2019-09-12 | 2019-12-20 | 河南电池研究院有限公司 | Porous silicon-carbon lithium ion battery cathode material with high rate performance and preparation method thereof |
| CN115050945A (en) * | 2022-07-15 | 2022-09-13 | 湖北工业大学 | Preparation method of biomass nitrogen-doped carbon-coated lithium-rich lithium iron phosphate positive electrode material |
| CN115050945B (en) * | 2022-07-15 | 2023-09-22 | 湖北工业大学 | Preparation method of biomass nitrogen-doped carbon-coated lithium-rich lithium iron phosphate positive electrode material |
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