CN105390672A - Preparation method for three-dimensional nitrogen-doped mesoporous carbon ultra-thin nanosheet material - Google Patents
Preparation method for three-dimensional nitrogen-doped mesoporous carbon ultra-thin nanosheet material Download PDFInfo
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- CN105390672A CN105390672A CN201510687699.8A CN201510687699A CN105390672A CN 105390672 A CN105390672 A CN 105390672A CN 201510687699 A CN201510687699 A CN 201510687699A CN 105390672 A CN105390672 A CN 105390672A
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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
- H01M4/362—Composites
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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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- 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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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 provides a preparation method for a three-dimensional nitrogen-doped mesoporous carbon ultra-thin nanosheet material. The preparation method comprises the steps of preparing a 15-30% water solution based on mass percentage from sodium chloride and sodium silicate at the mass ratio of (1-10):100; adding glucose and urea into the water solution, wherein the mass ratio of glucose to urea to sodium chloride is (1-2): (1-2): (10-20), and stirring the mixture to obtain a settled solution; performing vacuum freezing and drying on the settled solution to obtain precursor powder; heating the precursor powder under protection of argon or nitrogen to be 600-750 DEG C, performing a carbonization and nitrogen-doping process, and then performing furnace cooling to reduce temperature to room temperature; and preparing the three-dimensional nitrogen-doped mesoporous carbon ultra-thin nanosheet. The three-dimensional nitrogen-doped mesoporous carbon ultra-thin nanosheet prepared by the method is relatively large in the specific surface area, optimized in the porous structure and relatively high in nitrogen doping amount.
Description
Technical field
The present invention relates to a kind of three-dimensional N doping mesoporous carbon ultrathin nanometer sheet and preparation method thereof, belong to advanced material with carbon element technology of preparing.
Background technology
Along with the development in the market of electronic product and new-energy automobile, advanced energy storage device receives people and more and more pays close attention to.Wherein, lithium ion battery has long circulation life because of it, the advantages such as high power capacity, high-energy-density, clean and safe, becomes the focus that people fall over each other to develop.But the capacity of traditional negative material graphite only has 372mAh/g.In order to obtain good lithium electrical property, negative material is needed to have higher specific area.For this reason, people constantly reduce the thickness of material with carbon element, the stratiform material with carbon element from the block material with carbon element of micron level to Nano grade.But when the nanoscale twins of carbon is very thin, Van der Waals force therebetween can make carbon-coating reunite, thus greatly affects the performance of its performance.For overcoming this problem, researcher tends to transfer the laminar structured of two dimension to three-dimensional network-like structure.Meanwhile, the introducing of meso-hole structure is also the method for common optimization material with carbon element structure.Abundant mesoporously can improve material specific surface area further, be conducive to the diffusion of electrolyte.Especially, as lithium cell negative pole material, the existence of meso-hole structure can alleviate the swelling that Lithium-ion embeding deviates from material with carbon element in process, thus promotes the useful life of electrode material.
Impurity element is also the means effectively promoting material with carbon element physical and chemical performance.Such as common, by the doping of nitrogen element, the chemical property of carbon base body can be improved, comprise raising conductance.Meanwhile, the introducing of N element, also can expand carbon-coating spacing, and introduce defect, and these can promote the avtive spot of carbon adsorption lithium atom, thus promotes lithium storage content.
In sum, desirable lithium cell negative pole material should possess: 1) three-dimensional net structure; 2) abundant mesoporous distribution; 3) the impurity element doping of high level.But the material report meeting as above condition is less, or preparation technology is too complicated, is difficult to realize large-scale production simultaneously.Therefore, use resourceful raw material, the Novel lithium battery negative material meeting above-mentioned condition by comparatively simple technique preparation has become significant challenge.
Summary of the invention
The present invention aims to provide a kind of three-dimensional N doping mesoporous carbon ultrathin nanometer sheet material preparation method being applied to lithium ion battery negative, this the three-dimensional N doping mesoporous carbon ultrathin nanometer sheet adopting this kind of method to prepare has larger specific surface knot, the hierarchical porous structure of optimization and higher N doping amount.Its Stability Analysis of Structures, excellent electrochemical performance is one of ideal material of the negative pole of lithium ion battery, and preparation method is simple, abundant raw material environmental protection.
A kind of three-dimensional N doping mesoporous carbon ultrathin nanometer sheet material preparation method, is characterized in that comprising following process:
1) be (1 ~ 10) by sodium chloride and sodium metasilicate according to mass ratio: 100 are mixed with the aqueous solution that sodium chloride mass fraction is 15 ~ 30%, glucose and urea are added in this aqueous solution, wherein glucose, the mass ratio of urea and sodium chloride is (1 ~ 2): (1 ~ 2): (10 ~ 20), obtains settled solution through stirring;
2) by step 1) in gained settled solution carry out vacuum freeze drying, obtain precursor powder;
3) precursor powder being placed in tube furnace, is 100 ~ 300mLmin at flow
-1argon gas or nitrogen protection under, with 5 ~ 10 DEG C of min
-1heating rate be heated to 600 DEG C ~ 750 DEG C, insulation 1 ~ 3h, carrying out carbonization and nitrating process, is 100 ~ 300mLmin at flow
-1argon gas or nitrogen under, cool to room temperature with the furnace, by sample take out, grinding, obtain black powder;
4) by step 3) gained black powder joins in deionized water, and obtained concentration is 20 ~ 50gL
-1suspension-turbid liquid, use deionized water filtering and washing subsequently, obtain black powder, it is dry in 50 ~ 100 DEG C of drying boxes, obtain three-dimensional N doping mesoporous carbon ultrathin nanometer sheet.
Compared with prior art, the invention has the beneficial effects as follows: the microscopic appearance of obtained material is the three-dimensional network-like structure that ultrathin nanometer sheet (< 5nm) is made, and the surperficial dense distribution of nanometer sheet mesoporous in a large number.Wherein, three-dimensional communicating structure increases specific area and effectively prevent the reunion of ultra-thin carbon nanosheet, thus improves the cyclical stability as lithium cell negative pole material; Equally distributed meso-hole structure is conducive to electrolytical transmission and diffusion, and deviates from for Lithium-ion embeding the change in volume that process causes and have certain pooling feature.The nitrogen-doping of high-load can improve the chemical property of carbon base body, and introduces the avtive spot of more storage lithium ions.In addition, the method is simple, and cheaper starting materials environmental protection, is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 three-dimensional N doping mesoporous carbon ultrathin nanometer sheet material SEM obtained by the embodiment of the present invention one schemes
Fig. 2 three-dimensional N doping mesoporous carbon ultrathin nanometer sheet material TEM obtained by the embodiment of the present invention one schemes
Fig. 3 three-dimensional N doping mesoporous carbon ultrathin nanometer sheet material XPS obtained by the embodiment of the present invention one schemes
Fig. 4 is three-dimensional N doping mesoporous carbon ultrathin nanometer sheet material pore size distribution figure obtained by the embodiment of the present invention one
Fig. 5 is three-dimensional N doping mesoporous carbon ultrathin nanometer sheet material cyclic voltammetry curve obtained by the embodiment of the present invention one
Embodiment
Below in conjunction with embodiment, the invention will be further described, and these embodiments, just for illustration of the present invention, do not limit the present invention.
Embodiment one
Weigh quality 25g sodium chloride respectively, 0.5g sodium metasilicate, 1.25g glucose, the beaker of 300mL put into by 1.25g urea, adds the deionized water of 100mL respectively, 200rmin
-1mechanical agitation 15min obtains settled solution.This solution is carried out vacuum freeze drying (condenser temperature of drying machine is-50 DEG C, air pressure <20Pa), obtain precursor powder; Precursor powder being placed in corundum tube furnace, is 200mLmin at flow
-1argon gas atmosphere under, with 5 DEG C of min
-1heating rate be heated to 650 DEG C, insulation 2h, carry out carburizing reagent.Be 200mLmin at flow
-1argon gas atmosphere under cool to room temperature with the furnace, by sample take out, grinding, obtain black powder; Gained black powder is joined obtained suspension-turbid liquid in 400mL deionized water, 15min is stirred under the speed of 200rpm, suction filtration (filter paper aperture is 0.22 μm) washing subsequently, 400mL deionized water is added again to obtaining powder, stir 15min, again suction filtration, obtain black powder, by its in drying box in 80 DEG C of dry 10h, obtain three-dimensional N doping mesoporous carbon ultrathin nanometer sheet material.Resulting materials macropore diameter is about 2 μm, and mesoporous average diameter is 5nm, micro content 0.15cm
3/ g, nitrogen content is 5.87%.
Three-dimensional N doping mesoporous carbon ultrathin nanometer sheet material and PVDF binding agent, conductive carbon black are obtained the slurry of dark thick according to mass ratio magnetic agitation 4h in nmp solvent of 80:10:10, then slurry is evenly coated on Copper Foil, the thickness of coating is 100 μm, be placed in vacuum drying chamber 80 DEG C of dry 12h again, after being cooled to room temperature, obtain battery pole piece.The button cell model adopted in battery assembling is CR2025, and prepared electrode is Electrode, and metal lithium sheet is auxiliary electrode, and electrolyte is for containing 1molmL
-1liPF
6eC+DEC+EMC mixed system (volume ratio is 1:1:1).The barrier film of work electrode, the full electrolyte of leaching, auxiliary electrode and nickel foam are put into battery case in order successively.All operations all being full of argon gas, humidity is less than in the glove box of 4% and carries out, and makes the Spherical Carbon coated iron oxide half-cell that Li/ is graphene-supported, for test.
Cyclic voltammetry adopts the Electrochemical Comprehensive Tester that model is CHI660D, Shanghai Chen Hua company produces.Experiment employing two electrode test system is at room temperature carried out, and Electrode is active sample electrode, and auxiliary and reference electrode is Li
+/ Li, sweep speed is 0.1mVs
-1, sweep limits is 0.01 ~ 3.0V.Charge-discharge test adopts computer-controlled indigo plant electric CT2001A high accuracy battery Performance Test System to test.Charge-discharge procedures is: first leave standstill 5s, and after constant-current discharge to 0.005V, then leave standstill 5s, constant current charge is to 3.0V afterwards, with Li in test process
+/ Li is auxiliary and reference electrode.
Embodiment two
Weigh quality 25g sodium chloride respectively, 1.5g sodium metasilicate, 1.25g DEXTROSE ANHYDROUS, the beaker of 300mL put into by 1.25g urea, adds the deionized water of 100mL respectively, 200rmin
-1mechanical agitation 15min obtains settled solution.This solution is carried out vacuum freeze drying (condenser temperature of drying machine is-50 DEG C, air pressure <20Pa), obtain precursor powder; Precursor powder being placed in corundum tube furnace, is 200mLmin at flow
-1argon gas atmosphere under, with 10 DEG C of min
-1heating rate be heated to 650 DEG C, insulation 2h, make glucose carbonization, urea decomposition.Be 200mLmin at flow
-1argon gas atmosphere under cool to room temperature with the furnace, by sample take out, grinding, obtain the mixture of material with carbon element and salt; Gained mixture is joined obtained suspension-turbid liquid in 400mL deionized water, 15min is stirred under the speed of 200rpm, suction filtration (filter paper aperture is 0.22 μm) washing subsequently, 400mL deionized water is added again to obtaining powder, stir 15min, again suction filtration, obtain black powder, by its in drying box in 80 DEG C of dry 10h, obtain three-dimensional N doping mesoporous carbon ultrathin nanometer sheet material.Resulting materials macropore diameter is about 2 μm, and mesopore diameter is 15-20nm, and micro content is lower than 0.1cm
3/ g, nitrogen content is 5%.
Embodiment three
Weigh quality 10g sodium chloride respectively, 0.5g sodium metasilicate, 1.25g glucose, the beaker of 300mL put into by 1.25g urea, adds the deionized water of 100mL respectively, 200rmin
-1mechanical agitation 15min obtains settled solution.This solution is carried out vacuum freeze drying (condenser temperature of drying machine is-50 DEG C, air pressure <20Pa), obtain precursor powder; Precursor powder being placed in corundum tube furnace, is 200mLmin at flow
-1argon gas atmosphere under, with 5 DEG C of min
-1heating rate be heated to 750 DEG C, insulation 2h, make glucose carbonization, urea decomposition.Be 200mLmin at flow
-1argon gas atmosphere under cool to room temperature with the furnace, by sample take out, grinding, obtain the mixture of material with carbon element and salt; Gained mixture is joined obtained suspension-turbid liquid in 400mL deionized water, 15min is stirred under the speed of 200rpm, suction filtration (filter paper aperture is 0.22 μm) washing subsequently, 400mL deionized water is added again to obtaining powder, stir 15min, again suction filtration, obtain black powder, by its in drying box in 80 DEG C of dry 10h, obtain three-dimensional N doping mesoporous carbon ultrathin nanometer sheet material.Resulting materials macropore diameter is about 5 μm, and mesopore diameter is 5nm, and nitrogen content is 6%.
The nitrogen element mass fraction adulterated in obtained material is 3 ~ 8%, and overall pattern presents three-dimensional sequential like macroporous structure, diameter macropores is 1 ~ 5 μm, and the hole wall of macropore is all the meso-hole structure of 5 ~ 10nm with a large amount of diameter that distributes.
Claims (1)
1. a three-dimensional N doping mesoporous carbon ultrathin nanometer sheet material preparation method, is characterized in that comprising following process:
1) be (1 ~ 10) by sodium chloride and sodium metasilicate according to mass ratio: 100 are mixed with the aqueous solution that sodium chloride mass fraction is 15 ~ 30%, glucose and urea are added in this aqueous solution, wherein glucose, the mass ratio of urea and sodium chloride is (1 ~ 2): (1 ~ 2): (10 ~ 20), obtains settled solution through stirring;
2) by step 1) in gained settled solution carry out vacuum freeze drying, obtain precursor powder.
3) precursor powder being placed in tube furnace, is 100 ~ 300mLmin at flow
-1argon gas or nitrogen protection under, with 5 ~ 10 DEG C of min
-1heating rate be heated to 600 DEG C ~ 750 DEG C, insulation 1 ~ 3h, carrying out carbonization and nitrating process, is 100 ~ 300mLmin at flow
-1argon gas or nitrogen under, cool to room temperature with the furnace, by sample take out, grinding, obtain black powder;
4) by step 3) gained black powder joins in deionized water, and obtained concentration is 20 ~ 50gL
-1suspension-turbid liquid, use deionized water filtering and washing subsequently, obtain black powder, it is dry in 50 ~ 100 DEG C of drying boxes, obtain three-dimensional N doping mesoporous carbon ultrathin nanometer sheet.
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517133A (en) * | 2016-10-09 | 2017-03-22 | 华中科技大学 | Nitrogen-doped three-dimensional bicontinuous porous structure ultrathin carbon layer and preparation method and application thereof |
| CN107768645A (en) * | 2017-11-28 | 2018-03-06 | 吉林大学 | A kind of porous nitrogen-doped carbon nanometer sheet composite negative pole material and preparation method thereof |
| CN107919461A (en) * | 2016-10-09 | 2018-04-17 | 南京工业大学 | The preparation method of a kind of porous carbon cathode material of N doping and application |
| CN108469483A (en) * | 2018-03-23 | 2018-08-31 | 福州大学 | A kind of ultra-thin two-dimension carbonoxide nitrogen nanometer sheet and its preparation and application |
| CN109802114A (en) * | 2019-01-11 | 2019-05-24 | 武汉工程大学 | A kind of method that step complexes ira situ prepares uniform ternary cathode material of lithium ion battery |
| CN110002425A (en) * | 2019-04-22 | 2019-07-12 | 天津大学 | A kind of preparation method of the three-dimensional porous carbon material of ionic liquid super capacitor |
| CN110148733A (en) * | 2019-05-30 | 2019-08-20 | 中南大学 | A kind of exotic atom doped porous carbon material and its preparation method and application |
| CN110155980A (en) * | 2019-05-20 | 2019-08-23 | 北京化工大学 | A kind of preparation method of the three-dimensional porous carbon material of honeycomb |
| CN110386626A (en) * | 2018-04-16 | 2019-10-29 | 中国科学技术大学 | A kind of cobalt protoxide thin slice, preparation method and its decompose the application in water entirely in visible light catalytic |
| CN110449149A (en) * | 2019-06-27 | 2019-11-15 | 天津大学 | A kind of preparation method of carbon network supported noble metals nano-particle material |
| CN110649254A (en) * | 2019-09-06 | 2020-01-03 | 成都新柯力化工科技有限公司 | Lithium battery silicon-carbon negative electrode composite material and preparation method thereof |
| CN111825074A (en) * | 2019-04-15 | 2020-10-27 | 中国科学院福建物质结构研究所 | Preparation method and application of sulfur-nitrogen co-doped three-dimensional porous carbon nanosheet |
| CN111883754A (en) * | 2020-07-21 | 2020-11-03 | 合肥国轩高科动力能源有限公司 | Iron nitride-ordered mesoporous carbon composite material and preparation method and application thereof |
| CN112713280A (en) * | 2020-12-25 | 2021-04-27 | 河南师范大学 | Preparation method of noble metal platinum-based redox catalyst carrier |
| CN113061933A (en) * | 2021-02-25 | 2021-07-02 | 南京师范大学 | Ultrathin hierarchical structure Co @ N-C nanosheet and preparation method and application thereof |
| CN113430537A (en) * | 2021-07-20 | 2021-09-24 | 兰州大学 | Preparation method of N-doped carbon-based material for oxygen evolution electrocatalyst |
| CN113772655A (en) * | 2021-09-18 | 2021-12-10 | 河北零点新能源科技有限公司 | Heteroatom-doped hard carbon material and preparation method thereof |
| CN115000370A (en) * | 2022-06-02 | 2022-09-02 | 烟台大学 | Molybdenum dioxide confinement growth and modification three-dimensional porous carbon composite electrode material and preparation method thereof |
| CN115020723A (en) * | 2022-06-20 | 2022-09-06 | 巢湖学院 | Ultrathin vanadium nitride/nitrogen-doped carbon composite material and preparation method thereof |
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Cited By (21)
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| CN106517133A (en) * | 2016-10-09 | 2017-03-22 | 华中科技大学 | Nitrogen-doped three-dimensional bicontinuous porous structure ultrathin carbon layer and preparation method and application thereof |
| CN107919461A (en) * | 2016-10-09 | 2018-04-17 | 南京工业大学 | The preparation method of a kind of porous carbon cathode material of N doping and application |
| CN107768645A (en) * | 2017-11-28 | 2018-03-06 | 吉林大学 | A kind of porous nitrogen-doped carbon nanometer sheet composite negative pole material and preparation method thereof |
| CN107768645B (en) * | 2017-11-28 | 2020-07-14 | 吉林大学 | Porous nitrogen-doped carbon nanosheet composite negative electrode material and preparation method thereof |
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| CN110148733B (en) * | 2019-05-30 | 2022-06-07 | 中南大学 | Hetero-atom doped porous carbon material and preparation method and application thereof |
| CN110449149A (en) * | 2019-06-27 | 2019-11-15 | 天津大学 | A kind of preparation method of carbon network supported noble metals nano-particle material |
| CN110649254A (en) * | 2019-09-06 | 2020-01-03 | 成都新柯力化工科技有限公司 | Lithium battery silicon-carbon negative electrode composite material and preparation method thereof |
| CN111883754A (en) * | 2020-07-21 | 2020-11-03 | 合肥国轩高科动力能源有限公司 | Iron nitride-ordered mesoporous carbon composite material and preparation method and application thereof |
| CN112713280A (en) * | 2020-12-25 | 2021-04-27 | 河南师范大学 | Preparation method of noble metal platinum-based redox catalyst carrier |
| CN113061933A (en) * | 2021-02-25 | 2021-07-02 | 南京师范大学 | Ultrathin hierarchical structure Co @ N-C nanosheet and preparation method and application thereof |
| CN113430537A (en) * | 2021-07-20 | 2021-09-24 | 兰州大学 | Preparation method of N-doped carbon-based material for oxygen evolution electrocatalyst |
| CN113772655A (en) * | 2021-09-18 | 2021-12-10 | 河北零点新能源科技有限公司 | Heteroatom-doped hard carbon material and preparation method thereof |
| CN115000370A (en) * | 2022-06-02 | 2022-09-02 | 烟台大学 | Molybdenum dioxide confinement growth and modification three-dimensional porous carbon composite electrode material and preparation method thereof |
| CN115020723A (en) * | 2022-06-20 | 2022-09-06 | 巢湖学院 | Ultrathin vanadium nitride/nitrogen-doped carbon composite material and preparation method thereof |
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