CN104795565A - Porous graphene powder rich in heteroatom and preparation method and application thereof - Google Patents
Porous graphene powder rich in heteroatom and preparation method and application thereof Download PDFInfo
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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
- 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
- H01G11/42—Powders or particles, e.g. composition thereof
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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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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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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- 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 porous graphene powder rich in heteroatom. The porous graphene powder is formed by gathering graphene doped with heteroatom, and the heteroatom comprises at least one of nitrogen, boron, oxygen and phosphorus, wherein the chemical bond type of the carbon comprises graphitized sp<2>C, sp<3> hybridized C, oxygen-bridged C, and heterocyclic ring C, the sp<3> hybridized C comprises C-N or C-O, and the heterocyclic ring C comprises C=N or C=O. A natural high polymer material and carbohydrate are used as a biomass resource model, urea is used as a solid-state nitrogen source, graphene, which is high in specific surface area, has a microporous-mesoporous structure and contains nitrogen atoms, oxygen atoms and boron atoms, is prepared through a free-standing pyrolysis one-step method under the condition of normal pressure and without protection atmosphere, the graphene has a good battery energy storage function. The graphene powder disclosed by the invention has the characteristics of being low in cost, recyclable, small in environment influence, free from secondary pollution and the like, and is suitable for actual production practice.
Description
Technical field
One of the present invention is rich in hetero-atom porous graphene powder and self-supporting pyrolysis preparation and electrochemical energy storage application thereof and belongs to Graphene two-dimension nano materials technical field.
Background technology
Graphene (Graphene, G) is a kind of by sp
2the two dimensional crystal material of hydbridized carbon atoms composition, has slightly wavy layered structure, is considered to the basic composition unit forming the allotropes such as graphite, carbon nano-tube, fullerene.The intensity of Graphene, up to 130GPa, is one of mechanical property best material found so far, and the thermal conductivity of Graphene reaches 5000W/ (mK), is good heat carrier.The carrier properties of Graphene uniqueness, makes its electron mobility reach 2 × 10
5cm
2/ (Vs), exceedes silicon 100 times, and varies with temperature hardly and change.Current graphene preparation method mainly contains: (1) crystal epitaxy method, this method is, under high vacuum degree, single crystal silicon carbide substrate is heated to 1200 ~ 1600 DEG C, silicon atom distillation in substrate is separated out, excessive carbon atom stays substrate and reconstruct generates Graphene, (2) chemical vapour deposition technique (CVD), the carbon compounds such as methane are carried out pyrolysis and reconstruct generation Graphene by this method in substrate, then remove metallic substrates and obtain Graphene, (3) chemical oxidation-reduction method, at present with the standby i.e. Brodie method of this legal system, Staudenmaier method and Hummers method.
Nitrogen-doped graphene (N-doped G) is containing very important one in hetero-atom Graphene, wherein the introducing of nitrogen-atoms can change spin density and the charge distribution state of electronics in around carbon atom, thus makes it have the potentiality of the application such as electro-catalysis, sensing and electronic device.At present, the synthetic method of nitrogen-doped graphene has two kinds: the chemical synthesis of (1) (bottom-up) from bottom to top, as CVD and solvent-thermal method, (2) under nitrogen or ammonia atmosphere, high temperature reprocessing Graphene or graphite oxide (graphite oxide).
Solid phase pyrolysis synthesis (Solid-state pyrolysis) belongs to chemical synthesis process from bottom to top, uses Nitrogen element carbon compound as precursors, certain atmosphere and catalyst auxiliary under react.Synthesis as, nitrogen-doped carbon nanometer pipe (N-doped Carbon nanotube) utilizes metal organic complex containing carbon, nitrogen and metal catalytic source as presoma, obtained in sealing system by solid phase pyrolytic reaction.
Carbon and nitrogen solid precursor compound can friendly, the cheap and agricultural biomass resource that is easy to get of environment for use and natural macromolecular materials, as cellulose, leaf, glucose, shitosan, starch etc.
As positive electrode, elemental sulfur has higher theoretical specific capacity 1675mAh/g, theoretical specific energy 2600Wh/Kg, is 3 ~ 5 times of lithium rechargeable battery, and in addition, elemental sulfur also has the advantages such as hypotoxicity, memory space be large, cheap.
In sulphur lithium battery, the electrochemical reaction process of sulfur-bearing positive pole complexity and the physical property such as non-conductive thereof determine the research and development difficult point of lithium-sulfur cell mainly at positive electrode, for realizing the application of lithium-sulfur cell, the conductivity of positive electrode will be improved on the one hand, improve the utilance of positive active material, improve the high rate performance of battery; Also to suppress can not losing of capacity, to improve the cycle performance of battery on the other hand.
And research in recent years mainly concentrates on organosulfur compound material and carbon composite material two kinds of positive electrodes.And the present invention is exactly the carrier using the Graphene of high-specific surface area, microcellular structure and nitrogenous, oxygen atom as sulphur (S), it is positive electrode that chemical deposition prepares sulphur/porous graphene composite material, apply its oxygen functional group and large specific area to sulphur load, and then the non-constant of the conductivity overcoming sulphur greatly, be unfavorable for that the high rate capability of battery and sulphur are in discharge process, the expansion of volume is reduced very large, likely causes cell expansion and the shortcoming damaged.
Summary of the invention
This research contents is for biomass resource model with cellulose, leaf, maize straw, glucose, shitosan, starch, gelatin (natural macromolecular material); urea is solid-state nitrogenous source; under the condition of normal pressure and unprotect atmosphere, prepare high-specific surface area, microcellular structure and containing heteroatomic Graphene by self-supporting pyrolysis one-step method.
To achieve these goals, technical scheme of the present invention is as follows:
One is rich in heteroatomic porous graphene powder, it forms by assembling doped with heteroatomic Graphene, the microscopic pattern of powder contains hetero-atom described in micropore-mesopore compound pore passage structure and comprises at least one in nitrogen, boron, oxygen and phosphorus, and wherein, the chemical bond types of carbon comprises: graphitization sp
2c, sp
3hydridization C, oxo bridge connection C, heterocycle C, described sp
3hydridization C comprises C-N or C-O, and described heterocycle C comprises C=N or C=O, and the chemical bond of nitrogen comprises pyridine N, pyrroles N or pyridone N, graphitization N, pyridine oxide N.
One is rich in heteroatomic porous graphene raw powder's production technology as described in the present invention, it is characterized in that, be with biomass resource and solid-state nitrogenous source for raw material, at ambient pressure, prepared by self-supporting pyrolysis one-step method.
Specifically comprise the steps:
By biomass resource with solid-state nitrogenous source with (0 ~ 2): the mass ratio of 20 mixes, and is ground to after granularity is less than 500 orders, obtains mixed powder;
Described mixed powder is dried at 85 DEG C to water content lower than 500ppm after, at 500 ~ 1300 DEG C, carry out pyrolysis 3 hours, obtain being rich in heteroatomic porous graphene powder;
Preferably, described biomass resource is natural macromolecular material; Described solid-state nitrogenous source is urea, melamine or thiocarbamide.
Preferably, described natural macromolecular material is at least one in cellulose, glucose, shitosan, starch, leaf, maize straw.
A kind ofly be rich in the application of heteroatomic porous graphene powder in electrochemical energy storage as described in the present invention.
Preferably, the electrode of the positive pole of lithium-sulfur cell, lithium ion battery negative, super capacitor is comprised.
Porous comprises micropore and mesoporous;
Content 1 ~ the 30wt% of what the present invention obtained be rich in hetero-atom porous graphene powder nitrogen, oxygen content 10 ~ 20wt%; Specific area 485.146 ~ 737.793m
2/ g, micropore pore volume 0 ~ 0.31cm
3/ g, average pore size is distributed as 2.2nm ~ 10.8nm.
To be rich in the carrier of heteroatomic porous graphene powder as sulphur (S), chemical deposition prepares sulphur/porous graphene composite material, with water-soluble LAX132 for binding agent makes sulphur positive pole.With lithium metal (Li) for negative pole, electrolyte is 1M lithium bis-(trifl uoromethanesulfonyl) imide (LiTFSI) in 1,3-dioxolane and 1,2-dimethoxy-ethane (volume ratio 1:1) processes lithium-sulphur electricity.
The present invention utilizes this nitrogenous exactly, the conductivity that the graphene carbon material of oxygen atom is superior, good chemical stability and thermal stability, large specific area, abundant pore structure and surface functional group, carried out on a microscopic scale carbon sulphur composite material design (nitrogen containing oxygen Graphene as the carrier of sulphur (S), chemical deposition prepares sulphur/porous graphene composite material) sulphur is limited in the micropore of carbon nano-material, defect and Adsorption, with 1M lithium bis-(trifl uoromethanesulfonyl) imide (LiTFSI) in 1, 3-dioxolane and 1, 2-dimethoxy-ethane (volume ratio 1:1) is electrolyte, effectively increase the conductivity of sulphur and limit the dissolving of many sulphions, significantly improve the performance of lithium-sulfur cell at electric automobile power battery, the application in the fields such as intelligent grid and the extensive energy-storage battery of clean energy resource, there is potential using value widely.
Content of the present invention is for biomass resource model with cellulose, leaf, maize straw, glucose, shitosan, starch, gelatin (natural macromolecular material); urea is solid-state nitrogenous source; under the condition of normal pressure and unprotect atmosphere; prepare high-specific surface area, microcellular structure and Graphene that is nitrogenous, oxygen atom by self-supporting pyrolysis one-step method, this Graphene has the function of good battery energy storage.And possess with low cost, recyclable recycling, have fewer environmental impacts, the feature such as non-secondary pollution, be suitable for actual production practices.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph that hetero-atom porous graphene is rich in the present invention.
Fig. 2 is nitrogen adsorption-desorption curve figure that hetero-atom porous graphene is rich in the present invention.
Fig. 3 is that the cycle performance figure of hetero-atom porous graphene as Lithium-sulphur battery anode material is rich in the present invention.
Embodiment
For setting forth practical function of the present invention, below by reaction better and have the example of feature to be discussed.This process uses six kinds of natural products such as cellulose, leaf, maize straw, glucose, shitosan, starch, gelatin, there is wide material sources, renewable, wide variety, excellent performance, there are excellent biocompatibility, environmental friendliness, are easy to modification, broad-spectrum advantage.
Embodiment 1
Weigh urea 20g respectively, glucose 2g is in agate mortar, Homogeneous phase mixing, identical hand trituration is about 1h, till not having crystal to occur, by ground mixture in still, 85 DEG C without water oven in pyrolysis dry burning more than 3 days, the mixture be baked is placed in muffle furnace, and at the temperature of 900 DEG C and 1000 DEG C, carry out pyrolysis respectively, the time is about 10 ~ 12h.Black solid (Graphene) after pyrolysis is weighed, carries out the sign mensuration of XRD, SEM projection scanning, specific area respectively.
Embodiment 2
Weigh urea 20g respectively, cellulose 2g is in agate mortar, Homogeneous phase mixing, identical hand trituration is about 1h, till not having crystal to occur, by ground mixture in still, 85 DEG C without water oven in pyrolysis dry burning more than 3 days, the mixture be baked is placed in muffle furnace, and at the temperature of 900 DEG C and 1000 DEG C, carry out pyrolysis respectively, the time is about 10h ~ 12h.Black solid (Graphene) after pyrolysis is weighed, carries out the sign mensuration of XRD, SEM projection scanning, specific area respectively.
Embodiment 3
Weigh urea 20g respectively, shitosan 2g is in agate mortar, Homogeneous phase mixing, identical hand trituration is about 1h, till not having crystal to occur, by ground mixture in still, 85 DEG C without water oven in pyrolysis dry burning more than 3 days, the mixture be baked is placed in muffle furnace, and at the temperature of 900 DEG C and 1000 DEG C, carry out pyrolysis respectively, the time is about 10h ~ 12h.Black solid (Graphene) after pyrolysis is weighed, carries out the sign mensuration of XRD, SEM projection scanning, specific area respectively.
Embodiment 4
Weigh urea 20g respectively, edible corn starch 2g is in agate mortar, Homogeneous phase mixing, identical hand trituration is about 1h, till not having crystal to occur, by ground mixture in still, 85 DEG C without water oven in pyrolysis dry burning more than 3 days, the mixture be baked is placed in muffle furnace, and at the temperature of 900 DEG C and 1000 DEG C, carry out pyrolysis respectively, the time is about 10h ~ 12h.Black solid (Graphene) after pyrolysis is weighed, carries out the sign mensuration of XRD, SEM projection scanning, specific area respectively.
Embodiment 5
Weigh urea 20g respectively, gelatin 2g is in agate mortar, Homogeneous phase mixing, identical hand trituration is about 1h, till not having crystal to occur, by ground mixture in still, 85 DEG C without water oven in pyrolysis dry burning more than 3 days, the mixture be baked is placed in muffle furnace, and at the temperature of 900 DEG C and 1000 DEG C, carry out pyrolysis respectively, the time is about 10h ~ 12h.
Embodiment 6
Weigh urea 20g respectively, leaf powder 2g is in agate mortar, Homogeneous phase mixing, identical hand trituration is about 1h, till not having crystal to occur, by ground mixture in still, 85 DEG C without water oven in pyrolysis dry burning more than 3 days, the mixture be baked is placed in muffle furnace, and at the temperature of 900 DEG C and 1000 DEG C, carry out pyrolysis respectively, the time is about 10h ~ 12h.
Embodiment 7
It is nitrogenous that containing the carrier of oxygen Graphene as sulphur (S), chemical deposition prepares sulphur/porous graphene composite material, with water-soluble LAX132 for binding agent makes sulphur positive pole.With lithium metal (Li) for negative pole, electrolyte is 1M lithium bis-(trifl uoromethanesulfonyl) imide (LiTFSI) in 1,3-dioxolaneand 1,2-dimethoxy-ethane (volume ratio 1:1) processes lithium-sulfur cell.
Embodiment 8
Electrode preparation does not need binding agent and conductive filler, and 2mg powder sample is directly pressed onto (0.5cm*0.5cm) in nickel sheet and makes electrochemical capacitance electrode under 5MPa pressure.In 6M potassium hydroxide aqueous solution, be the electrochemical capacitance performance that reference electrode measures porous graphene electrode to electrode, saturated dry mercury electrode with Pt dish (1.5cm*1.5cm).
In sum, be only preferred embodiment of the present invention, not be used for limiting scope of the invention process, all equalizations of doing according to shape, structure, feature and the spirit described in the claims in the present invention scope change and modify, and all should be included in right of the present invention.
Claims (7)
1. be rich in a heteroatomic porous graphene powder, it is characterized in that, form by assembling doped with heteroatomic Graphene, described hetero-atom comprises at least one in nitrogen, boron, oxygen and phosphorus, and wherein, the chemical bond types of carbon comprises: graphitization sp
2c, sp
3hydridization C, oxo bridge connection C, heterocycle C, described sp
3hydridization C comprises C-N or C-O, and described heterocycle C comprises C=N or C=O, and the chemical bond of nitrogen comprises pyridine N, pyrroles N, pyridone N, graphitization N or pyridine oxide N.
2. be rich in a heteroatomic porous graphene raw powder's production technology as claimed in claim 1, it is characterized in that, be with biomass resource and solid-state nitrogenous source for raw material, at ambient pressure, prepared by self-supporting pyrolysis one-step method.
3. preparation method as claimed in claim 2, is characterized in that, specifically comprise the steps:
By biomass resource with solid-state nitrogenous source with (0 ~ 2): the mass ratio of 20 mixes, and is ground to after granularity is less than 500 orders, obtains mixed powder;
Described mixed powder is dried at 85 DEG C to water content lower than 500ppm after, at 500 ~ 1300 DEG C, carry out pyrolysis 3 hours, obtain being rich in heteroatomic porous graphene powder.
4. preparation method as claimed in claim 2 or claim 3, it is characterized in that, described biomass resource is natural macromolecular material; Described solid-state nitrogenous source is urea, melamine, thiocarbamide.
5. preparation method as claimed in claim 4, is characterized in that, described natural macromolecular material is cellulose, shitosan, leaf, maize straw, carbohydrate are at least one in starch, glucose.
6. one kind is rich in the application of heteroatomic porous graphene powder in electrochemical energy storage as claimed in claim 1.
7. apply as claimed in claim 6, it is characterized in that, comprise the electrode of the positive pole of lithium-sulfur cell, lithium ion battery negative, super capacitor.
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| US20150141666A1 (en) * | 2012-07-30 | 2015-05-21 | Zhongwei Chen | Low Cost Synthesis of Single Material Bifunctional Nonprecious Catalyst for Electrochemical Devices |
| CN105032469A (en) * | 2015-08-11 | 2015-11-11 | 中国人民解放军国防科学技术大学 | Biomass base nitrogen-doped graphene/carbon fiber electrocatalyst and preparation method thereof |
| CN105217613A (en) * | 2015-10-15 | 2016-01-06 | 田野 | A kind of preparation method of Graphene dopant material and application |
| CN105562050A (en) * | 2015-12-15 | 2016-05-11 | 华南理工大学 | Porous graphene-like structure doped carbon material as well as preparation method and application of porous graphene-like structure doped carbon material |
| CN105609324A (en) * | 2015-12-25 | 2016-05-25 | 哈尔滨工业大学 | Preparation method and application of N-P-dopted carbon fiber/graphene/bacterial cellulose conducting film material |
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| CN108172795A (en) * | 2017-12-27 | 2018-06-15 | 肇庆市华师大光电产业研究院 | A kind of preparation method of lithium sulfur battery anode material |
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| CN108172795A (en) * | 2017-12-27 | 2018-06-15 | 肇庆市华师大光电产业研究院 | A kind of preparation method of lithium sulfur battery anode material |
| CN108172795B (en) * | 2017-12-27 | 2020-05-12 | 肇庆市华师大光电产业研究院 | Preparation method of lithium-sulfur battery positive electrode material |
| ES2678079A1 (en) * | 2018-02-12 | 2018-08-08 | Depuración De Aguas Del Mediterráneo, S.L. | PROCEDURE FOR OBTAINING GRAFÉNICOS MATERIALS FROM LANDS FROM THE TREATMENT OF WASTEWATER (Machine-translation by Google Translate, not legally binding) |
| CN108695515A (en) * | 2018-03-20 | 2018-10-23 | 中原大学 | Method for manufacturing negative electrode material for secondary battery |
| CN110562961A (en) * | 2019-08-26 | 2019-12-13 | 广西大学 | Method for in-situ synthesis of nitrogen and sulfur co-doped stereo graphene |
| CN111029530A (en) * | 2019-11-21 | 2020-04-17 | 合肥国轩高科动力能源有限公司 | Nitrogen and sulfur co-doped hollow biomass carbon material, preparation method thereof, and lithium-sulfur battery positive pole piece and battery prepared from same |
| CN111029530B (en) * | 2019-11-21 | 2022-04-12 | 合肥国轩高科动力能源有限公司 | Nitrogen and sulfur co-doped hollow biomass carbon material, preparation method thereof, and lithium-sulfur battery positive pole piece and battery prepared from same |
| CN111517306B (en) * | 2020-04-29 | 2021-12-14 | 内蒙古民族大学 | Graphene-like/biomass carbon fiber aerogel and preparation method and application thereof |
| CN111517306A (en) * | 2020-04-29 | 2020-08-11 | 内蒙古民族大学 | Graphene-like/biomass carbon fiber aerogel and preparation method and application thereof |
| CN111540618A (en) * | 2020-05-07 | 2020-08-14 | 安徽大学 | Non-hydroformylation preparation method of nitrogen-oxygen co-doped carbon-based supercapacitor electrode material |
| CN111540618B (en) * | 2020-05-07 | 2021-10-22 | 安徽大学 | Non-hydroformylation preparation method of nitrogen-oxygen co-doped carbon-based supercapacitor electrode material |
| CN114497598A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | Sulfur-nitrogen-phosphorus doped carbon material, platinum-carbon catalyst, and preparation methods and applications thereof |
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