CN106517162A - Preparation method of nitrogen/ sulphur co-doping three-dimensional graphene sponge - Google Patents
Preparation method of nitrogen/ sulphur co-doping three-dimensional graphene sponge Download PDFInfo
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- CN106517162A CN106517162A CN201611161316.4A CN201611161316A CN106517162A CN 106517162 A CN106517162 A CN 106517162A CN 201611161316 A CN201611161316 A CN 201611161316A CN 106517162 A CN106517162 A CN 106517162A
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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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- 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
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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
- 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 relates to a preparation method of a nitrogen/ sulphur co-doping three-dimensional graphene sponge. The preparation method of the nitrogen/ sulphur co-doping three-dimensional graphene sponge comprises the steps of firstly, fully dispersing a graphene oxide and thiourea mixture through an ultrasonic oscillating way, then filling the mixture into a hydrothermal reaction kettle, reducing the graphene oxide into graphene through high temperature and high pressure, meanwhile, self-assembling the graphene into a three-dimensional graphene macroscopic body, and doping a nitrogen element and a sulphur element into a graphene substrate; and finally, repetitively cleaning the three-dimensional graphene macroscopic body, and freeze drying to obtain the nitrogen/ sulphur co-doping three-dimensional graphene sponge. The three-dimensional graphene sponge synthesized through hydrothermal reaction has the advantages of light weight and porosity, and is applied in a lithium-sulfur battery so as to be capable of improving the electrical conductivity of an anode material and solving the problem of big volume change during an electrode reaction process. The preparation method of the nitrogen/ sulphur co-doping three-dimensional graphene sponge provided by the invention is simple and easy to implement, and is very applicable to engineering production.
Description
Technical field
The present invention is the preparation method that a kind of nitrogen/sulfur is co-doped with three-dimensional grapheme sponge, belongs to a kind of graphene macroform
Preparation method.
Background technology
Lithium-sulfur cell is the redox reaction of a kind of dependence lithium and sulfur, and the fracture/generation and electronics for causing sulfur-sulfide linkage turns
Move, realize the secondary cell mutually changed between chemical energy and electric energy.Lithium-sulfur cell theory specific energy is 2600Wh/Kg, is current
Lithium ion battery theory specific energy (500WhKg-1) 5 times, be acknowledged as the lithium secondary battery of most prospect of future generation.It is expected to
The fields such as portable type electronic product, electric automobile, aerospace craft and electrical grid transmission are used widely, today's society,
Huge effect is played in the development of economic and science and technology, with very bright application prospect.
But under room temperature condition, elemental sulfur electrical conductivity is low, many sulfur of solubility are generated in lithium-sulfur cell charge and discharge process
Compound, causes various side reactions and change in volume, cause that lithium-sulphur cell positive electrode active material utilization rate is low, high rate performance is poor and
Cycle life is short, restricts sulfur as the development of positive electrode material of lithium secondary cell battery.Thus, improve lithium-sulphur cell positive electrode active matter
Matter utilization rate and cycle life and improve high rate performance to become lithium-sulfur cell be prior development direction from now on.
Graphene is a kind of New Two Dimensional nano material, and its nanometer sheet is by sp2The monoatomic layer of hydbridized carbon atoms composition
The two-dimensional material of thickness, is most thin, the most hard nano material in known world, and intensity is up to 1.01TPa, is structural steel
100 times, density is but the 1/5 of structural steel.Heat conductivity is up to 5300W/m K, higher than CNT and diamond, under room temperature
Electron mobility is more than 200000cm2/ V S, higher than CNT or silicon crystal, resistivity only about 1 Ω m, than copper or silver more
It is low, it is the minimum material of world resistivity.
Graphene has very high electrical conductivity, and using it for lithium sulfur battery anode material, can to solve element sulphur non-conductive
Problem, improve positive electrode electric conductivity.Graphene belongs to nanometer materials, with surface activity, easily with other materials particle
With reference to, it is easy to fixed polysulfide, prevent shuttle effect.Due to the toughness and intensity of Graphene, using Graphene as lithium
Sulphur cell positive electrode material skeleton, can effectively solving lithium sulfur battery anode material change in volume problem.But conventional two-dimensional Graphene is just
Pole material is difficult to improve its own specific surface area, and the contribution to fixed polysulfide is limited.Three-dimensional grapheme has loose structure,
High-specific surface area, high conductivity and high mechanical properties, therefore become lithium sulfur battery anode material ideal skeleton.
The content of the invention
The present invention is exactly directed to above-mentioned problems of the prior art and designs and be co-doped with three-dimensional stone there is provided a kind of nitrogen/sulfur
The preparation method of black alkene sponge, its objective is, in the way of hydro-thermal reaction, by High Temperature High Pressure, graphene oxide to be reduced into stone
Black alkene, forms three-dimensional sponge shape Graphene, solves the problems, such as lithium sulfur battery anode material.
The purpose of the present invention is achieved through the following technical solutions：
This kind of nitrogen/sulfur is co-doped with the preparation method of three-dimensional grapheme sponge, it is characterised in that：The step of the method, is as follows：
The preparation of step one, graphene oxide/compound
Graphene oxide is dissolved in deionized water, graphene oxide water solution is obtained, graphene oxide in the solution
Concentration is 2.6mg/ml～15.6mg/ml；
Step 2, thiourea is added to graphene oxide it is water-soluble in, recycle sonic oscillation carry out it is dispersed, formed oxygen
Graphite alkene/thiourea mixed solution, graphene oxide are 1 with the mass ratio of thiourea:4～1:10；
Step 3, graphene oxide/thiourea mixed solution is imported in hydrothermal reaction kettle, then hydrothermal reaction kettle is put into dry
Hydro-thermal reaction is carried out in dry stove, hydrothermal temperature is 150～200 DEG C, and heat time heating time is 12～24h, obtains nitrogen/sulfur and is co-doped with three
Dimension Graphene；
In the step, graphene oxide is reduced into Graphene, while Graphene is self-assembled into three-dimensional grapheme macroscopic body,
And in graphene base body nitrogen doped and element sulphur；
After step 4, deionized water clean remaining thiourea repeatedly, nitrogen/sulfur is co-doped with three-dimensional grapheme, and to carry out freezing dry
Dry, lyophilization temperature is -55 DEG C, and the time is 72h.
Graphene oxide is lamellar, and its contour dimension is 10 μm～20 μm.
Technical solution of the present invention is to introduce containing nitrogen and sulfur with the difference of conventional three-dimensional grapheme sponge preparation method
Functional group, these functional groups replace surface of graphene oxide or the original hydroxyl in edge and carboxylic group.These nitrogenous and sulfur
Functional group produce with polysulfide in lithium sulfur electrode course of reaction it is strong interact, polysulfide is consolidated so as to strengthen
It is set for using.Jing electrochemical property tests, using the three-dimensional grapheme sponge as the lithium-sulfur cell of positive electrode under 0.2C multiplying powers,
Initial specific capacities are up to 1200mAh/g.
Nitrogen/the sulfur obtained by above-mentioned technical proposal is co-doped with clear advantage.Graphene is co-doped with as lithium using nitrogen/sulfur
Sulphur cell positive electrode material, can play following advantage：First, the high conductivity of Graphene is conducive to improving lithium-sulphur cell positive electrode material
The electric conductivity of material；Secondly, the functional group of the loose structure, high-specific surface area and surface of three-dimensional grapheme can effectively fix many
Sulfide；Finally, the high intensity and high tenacity of Graphene can effectively adjust polysulfide and produce in electrode process
Change in volume.Three-dimensional grapheme sponge is co-doped with using nitrogen/sulfur lithium-sulfur cell can be effectively improved as lithium sulfur battery anode material
Chemical property.
Specific embodiment
Technical solution of the present invention is further described below with reference to embodiment：
Embodiment
Prepared using the inventive method as follows the step of nitrogen/sulfur is co-doped with three-dimensional grapheme sponge：
Step 1：Prepare graphene oxide and thiourea mixed solution；
(1) 260mg graphene oxides are dissolved in 100ml deionized waters；
(2) the thiourea 1.52g thiourea for weighing is dissolved in graphene oxide solution；
(3) graphene oxide solution prepared in step b is put in ultrasonic wave concussion device and stirs 30min；
Step 2：Graphene oxide is imported in hydrothermal reaction kettle with thiourea mixed solution；
Step 3：Step 2 gained hydrothermal reaction kettle is placed in drying oven, 180 DEG C, 24 hours, carries out hydro-thermal reaction；
Step 4：Step 3 gained nitrogen/nitrogen is co-doped with into three-dimensional grapheme sponge deionized water and cleans repeatedly remaining thiourea；
Step 5：Step 4 gained carbon/nitrogen is co-doped with into sponge Graphene lyophilization.
By said method, realize Graphene to be self-assembled into is three-dimensional grapheme sponge and nitrogen/sulfur functional group in stone
The doping on black alkene surface, can more accurately control the density of three-dimensional grapheme sponge by this technique, while this process is simple,
The preparation that large batch of nitrogen/sulfur is co-doped with graphene sponge is easily achieved, is conducive to engineer applied.
Claims (2)
1. a kind of nitrogen/sulfur is co-doped with the preparation method of three-dimensional grapheme sponge, it is characterised in that：The step of the method, is as follows：
The preparation of step one, graphene oxide/compound
Graphene oxide is dissolved in deionized water, graphene oxide water solution is obtained, the concentration of graphene oxide in the solution
For 2.6mg/ml～15.6mg/ml；
Step 2, thiourea is added to graphene oxide it is water-soluble in, recycle sonic oscillation carry out it is dispersed, formed oxidation stone
Black alkene/thiourea mixed solution, graphene oxide are 1 with the mass ratio of thiourea:4～1:10；
Step 3, graphene oxide/thiourea mixed solution is imported in hydrothermal reaction kettle, then hydrothermal reaction kettle is put into into drying oven
In carry out hydro-thermal reaction, hydrothermal temperature is 150～200 DEG C, and heat time heating time is 12～24h, obtains nitrogen/sulfur and is co-doped with three-dimensional stone
Black alkene；
After step 4, deionized water clean remaining thiourea repeatedly, nitrogen/sulfur is co-doped with three-dimensional grapheme carries out lyophilization, cold
It is -55 DEG C to freeze baking temperature, and the time is 72h.
2. nitrogen/sulfur according to claim 1 is co-doped with the preparation method of three-dimensional grapheme sponge, it is characterised in that：Oxidation stone
Black alkene is lamellar, and its contour dimension is 10 μm～20 μm.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106876685A (en) * | 2017-04-12 | 2017-06-20 | 河北工业大学 | A kind of preparation method of lithium sulfur battery anode material |
| CN107118386A (en) * | 2017-05-27 | 2017-09-01 | 华南理工大学 | A kind of super-hydrophobic sponge and its preparation method and application |
| CN107732202A (en) * | 2017-10-16 | 2018-02-23 | 河源广工大协同创新研究院 | A kind of preparation method of lithium sulfur battery anode material |
| CN107887586A (en) * | 2017-11-06 | 2018-04-06 | 陈少华 | A kind of preparation method of ion cathode material lithium |
| CN108123126A (en) * | 2017-12-20 | 2018-06-05 | 厦门紫阳科技产业发展有限公司 | A kind of preparation method of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material |
| CN108376772A (en) * | 2018-02-05 | 2018-08-07 | 西安理工大学 | A kind of richness N, S Based on Dual-Aperture meso-hole structure carbon carrier, preparation method and application |
| CN108493422A (en) * | 2018-04-02 | 2018-09-04 | 清华大学深圳研究生院 | A kind of sulfur functionalization porous graphene macroscopic view block materials and preparation method thereof |
| CN108722347A (en) * | 2017-04-21 | 2018-11-02 | 无锡市惠诚石墨烯技术应用有限公司 | A kind of preparation of graphene oil suction sponge |
| CN108963215A (en) * | 2018-07-03 | 2018-12-07 | 陕西科技大学 | The fixed porous MoS of N doped graphene flexible substrates with three-dimensional structure2Nano material and its preparation method and application |
| CN109037678A (en) * | 2018-06-15 | 2018-12-18 | 陕西科技大学 | A kind of preparation method of nitrogen sulphur codope three-dimensional graphene foam electrode active material |
| CN109709189A (en) * | 2019-02-27 | 2019-05-03 | 山东理工大学 | A kind of preparation method of the interlayer type electrochemical immunosensor of cardiac troponin |
| CN109709188A (en) * | 2019-02-27 | 2019-05-03 | 山东理工大学 | A kind of preparation method and application of the interlayer type immunosensor of nitrogen sulphur codope graphene oxide label |
| CN110294470A (en) * | 2018-03-22 | 2019-10-01 | 中国科学院上海硅酸盐研究所 | It is a kind of to vulcanize three-dimensional porous grapheme material and preparation method thereof |
| CN112670479A (en) * | 2020-12-24 | 2021-04-16 | 惠州亿纬锂能股份有限公司 | Sulfur and nitrogen co-doped coaxial core-shell silicon-carbon negative electrode material, preparation method thereof and lithium ion battery |
| US11437199B1 (en) * | 2022-04-08 | 2022-09-06 | King Fahd University Of Petroleum And Minerals | Layered dual hydroxide (LDH) composite |
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| CN106876685B (en) * | 2017-04-12 | 2019-05-14 | 河北工业大学 | A kind of preparation method of lithium sulfur battery anode material |
| CN106876685A (en) * | 2017-04-12 | 2017-06-20 | 河北工业大学 | A kind of preparation method of lithium sulfur battery anode material |
| CN108722347A (en) * | 2017-04-21 | 2018-11-02 | 无锡市惠诚石墨烯技术应用有限公司 | A kind of preparation of graphene oil suction sponge |
| CN107118386A (en) * | 2017-05-27 | 2017-09-01 | 华南理工大学 | A kind of super-hydrophobic sponge and its preparation method and application |
| CN107732202A (en) * | 2017-10-16 | 2018-02-23 | 河源广工大协同创新研究院 | A kind of preparation method of lithium sulfur battery anode material |
| CN107732202B (en) * | 2017-10-16 | 2020-11-03 | 河源广工大协同创新研究院 | Preparation method of lithium-sulfur battery positive electrode material |
| CN107887586A (en) * | 2017-11-06 | 2018-04-06 | 陈少华 | A kind of preparation method of ion cathode material lithium |
| CN108123126A (en) * | 2017-12-20 | 2018-06-05 | 厦门紫阳科技产业发展有限公司 | A kind of preparation method of high-capacity lithium ion cell stannic oxide/nitrogen-doped graphene composite negative pole material |
| CN108376772A (en) * | 2018-02-05 | 2018-08-07 | 西安理工大学 | A kind of richness N, S Based on Dual-Aperture meso-hole structure carbon carrier, preparation method and application |
| CN110294470A (en) * | 2018-03-22 | 2019-10-01 | 中国科学院上海硅酸盐研究所 | It is a kind of to vulcanize three-dimensional porous grapheme material and preparation method thereof |
| CN110294470B (en) * | 2018-03-22 | 2022-10-14 | 中国科学院上海硅酸盐研究所 | Vulcanized three-dimensional porous graphene material and preparation method thereof |
| CN108493422A (en) * | 2018-04-02 | 2018-09-04 | 清华大学深圳研究生院 | A kind of sulfur functionalization porous graphene macroscopic view block materials and preparation method thereof |
| CN109037678B (en) * | 2018-06-15 | 2022-02-01 | 陕西科技大学 | Preparation method of nitrogen and sulfur co-doped three-dimensional graphene foam electrode active material |
| CN109037678A (en) * | 2018-06-15 | 2018-12-18 | 陕西科技大学 | A kind of preparation method of nitrogen sulphur codope three-dimensional graphene foam electrode active material |
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| CN108963215B (en) * | 2018-07-03 | 2021-04-30 | 陕西科技大学 | N-doped graphene flexible substrate fixed porous MoS with three-dimensional structure2Nano material and preparation method and application thereof |
| CN109709188B (en) * | 2019-02-27 | 2020-08-11 | 山东理工大学 | Preparation method and application of sandwich type immunosensor marked by nitrogen-sulfur double-doped graphene oxide |
| CN109709188A (en) * | 2019-02-27 | 2019-05-03 | 山东理工大学 | A kind of preparation method and application of the interlayer type immunosensor of nitrogen sulphur codope graphene oxide label |
| CN109709189A (en) * | 2019-02-27 | 2019-05-03 | 山东理工大学 | A kind of preparation method of the interlayer type electrochemical immunosensor of cardiac troponin |
| CN112670479A (en) * | 2020-12-24 | 2021-04-16 | 惠州亿纬锂能股份有限公司 | Sulfur and nitrogen co-doped coaxial core-shell silicon-carbon negative electrode material, preparation method thereof and lithium ion battery |
| CN112670479B (en) * | 2020-12-24 | 2022-08-09 | 惠州亿纬锂能股份有限公司 | Sulfur and nitrogen co-doped coaxial core-shell silicon-carbon negative electrode material, preparation method thereof and lithium ion battery |
| US11437199B1 (en) * | 2022-04-08 | 2022-09-06 | King Fahd University Of Petroleum And Minerals | Layered dual hydroxide (LDH) composite |
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Address after: 100095 Haidian District, Beijing, box 81, Applicant after: China Hangfa Beijing Institute of Aerial Materials Address before: 100095 Haidian District, Beijing, box 81, Applicant before: Beijing Institute of Aeronautical Materials, China Aviation Industry Group Corporation |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170322 |