CN106129351A - A kind of RGO/In2s3the preparation method of composite - Google Patents

A kind of RGO/In2s3the preparation method of composite Download PDF

Info

Publication number
CN106129351A
CN106129351A CN201610516561.6A CN201610516561A CN106129351A CN 106129351 A CN106129351 A CN 106129351A CN 201610516561 A CN201610516561 A CN 201610516561A CN 106129351 A CN106129351 A CN 106129351A
Authority
CN
China
Prior art keywords
composite
rgo
ultrasonic
preparation
graphene
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610516561.6A
Other languages
Chinese (zh)
Inventor
何丹农
卢静
张彦鹏
尹桂林
葛美英
金彩虹
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai National Engineering Research Center for Nanotechnology Co Ltd
Original Assignee
Shanghai National Engineering Research Center for Nanotechnology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai National Engineering Research Center for Nanotechnology Co Ltd filed Critical Shanghai National Engineering Research Center for Nanotechnology Co Ltd
Priority to CN201610516561.6A priority Critical patent/CN106129351A/en
Publication of CN106129351A publication Critical patent/CN106129351A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • H01M4/364—Composites as mixtures
    • 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
    • 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
    • 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
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • 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
    • 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 present invention relates to a kind of RGO/In2S3The preparation method of composite, it is specifically related to use simple hydro-thermal method, under conditions of not using strong reductant and noxious substance, synchronize to carry out in hydro-thermal reaction by the growth course of redox graphene and indium sulfide, first by graphene oxide ultrasonic disperse in deionized water, the rear indium chloride adding equal in quality and the thioacetamide of 5 times of quality, continue ultrasonic, mixed solution after ultrasonic is put into autoclave reaction, is cooled to product clean dry after room temperature, finally at N2High annealing in atmosphere, can obtain the good Graphene of electric property/indium sulfide composite.The present invention uses hydro-thermal method one step to generate so that reduced graphene and In2S3The generation of nano-particle synchronizes to carry out, under conditions of without strong reductant or poisonous reactant, it is possible to quickly and stably obtain the RGO/In that chemical property is good2S3Composite, preparation process repeatability is high, simply and without Large expensive instrument supports.

Description

A kind of RGO/In2S3The preparation method of composite
Technical field
The invention belongs to field of composite material preparation, relate to a kind of RGO/In with good electrical chemical property2S3Composite wood The preparation method of material.The method specifically uses simple hydro-thermal method, synchronizes to carry out the reduction process of graphene oxide in the solution With the growth course of indium sulfide, under conditions of not using poisonous or strong reductant, obtain the RGO/In that electric property is good2S3Multiple Condensation material.
Background technology
Carbon-based material such as block graphite, CNT, Graphene etc. are because having abundant raw material, green non-poisonous, with low cost Etc. advantage, because being with a wide range of applications in terms of the field of batteries in energy industry.Particularly Graphene, good because having Good dynamic performance and electric property, closest to the requirement of battery anode material in carbon-based material.But circulation volume damages Mistake rate is higher is the subject matter limiting its application.Coloured glaze race metallic compound@C matrix composite is to reducing cycle capacity loss tool Improve significantly.
2012, Sathish M et al. used SnS2Greatly improve lithium electricity after nano-particle modified ultra-thin graphene film to deposit Storage.(J Phys. Chem. C 116,12475-12481,2012).But process is complex, and repeatability is the best.
2013, Gu Y et al. have employed the CoS RGO composite construction lithium battery of then limit for height capacity to be prepared.(ACS Appl. Mater Interfaces 5,801-806,2013), equally exist expensive and relatively costly the asking of apparatus for preparation Topic.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of simple RGO/In2S3The preparation side of composite Method, under conditions of not using strong reductant, in hydrothermal reaction process so that reduced graphene and In2S3The life of nano-particle Become synchronization to carry out, be effectively simplified preparation process.And prepared composite electric property is well, repeatable high, cost Cheap, to realizing, batch production is significant.
A kind of RGO/In2S3The preparation method of composite, it is characterised in that specifically include following steps:
(1) dispersion soln was formed by the most ultrasonic for graphene oxide 1 hour；
(2) add appropriate indium chloride and thioacetyl in step (1), continue ultrasonic 1 hour；
(3) mixed solution of the ultrasonic mistake in step (2) is transferred in autoclave, keeps 24 hours at 120 DEG C after sealing, Use ethanol and deionized water rinsing clean after being cooled to room temperature, be dried 6 hours at 70 DEG C in vacuum drying oven；
(4) by products therefrom in step (3) at N2Carry out high annealing in atmosphere, the RGO/ that chemical property is good can be obtained In2S3Composite.
The mass ratio of graphene oxide, indium sulfide and thioacetamide is 1:1:5.
When 0.1g graphene oxide is scattered in deionized water, the content of deionized water is at 10-40mL.
N2Under atmosphere, the temperature of annealing should control at 300-400 DEG C, and annealing time is 2 hours.
With prior art, the invention has the beneficial effects as follows:
The present invention uses hydro-thermal method one step to generate so that reduced graphene and In2S3The generation of nano-particle synchronizes to carry out, not Under conditions of adding strong reductant or poisonous reactant, it is possible to quickly and stably obtain the RGO/In that chemical property is good2S3 Composite, preparation process repeatability is high, simply and without Large expensive instrument supports.
Accompanying drawing explanation
The charging and discharging curve of Fig. 1 embodiment sample 1.
Detailed description of the invention
Elaborating embodiments of the invention below, the present embodiment is carried out under premised on technical solution of the present invention Implement, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following enforcement Example.
Embodiment 1:
0.1g graphene oxide is placed in 10 ml deionized waters ultrasonic 1 hour；By 0.1g indium chloride and 0.5g thioacetyl Amine is added in the graphene solution after ultrasonic disperse, continues ultrasonic 1 hour；Mixed solution after ultrasonic is transferred to high pressure anti- Answer in still, keep 24 hours at 120 DEG C after sealing；Ethanol and deionized water is used repeatedly to rinse well, in vacuum after cooling Drying baker is dried 6 hours at 70 DEG C；By dried product at N2The lower 400 DEG C of high annealings of atmosphere 2 hours, the product of gained Thing products therefrom is RGO/In2S3Composite.
Embodiment 2:
0.1g graphene oxide is placed in 20 ml deionized waters ultrasonic 1 hour；By 0.1g indium chloride and 0.5g thioacetyl Amine is added in the graphene solution after ultrasonic disperse, continues ultrasonic 1 hour；Mixed solution after ultrasonic is transferred to high pressure anti- Answer in still, keep 24 hours at 120 DEG C after sealing；Ethanol and deionized water is used repeatedly to rinse well, in vacuum after cooling Drying baker is dried 6 hours at 70 DEG C；By dried product at N2The lower 350 DEG C of high annealings of atmosphere 2 hours, the product of gained Thing products therefrom is RGO/In2S3Composite.
Embodiment 3:
0.1g graphene oxide is placed in 25ml deionized water ultrasonic 1 hour；By 0.1g indium chloride and 0.5g thioacetyl Amine is added in the graphene solution after ultrasonic disperse, continues ultrasonic 1 hour；Mixed solution after ultrasonic is transferred to high pressure anti- Answer in still, keep 24 hours at 120 DEG C after sealing；Ethanol and deionized water is used repeatedly to rinse well, in vacuum after cooling Drying baker is dried 6 hours at 70 DEG C；By dried product at N2The lower 300 DEG C of high annealings of atmosphere 2 hours, the product of gained Thing products therefrom is RGO/In2S3Composite.
Embodiment 4:
0.1g graphene oxide is placed in 40ml deionized water ultrasonic 1 hour；By 0.1g indium chloride and 0.5g thioacetyl Amine is added in the graphene solution after ultrasonic disperse, continues ultrasonic 1 hour；Mixed solution after ultrasonic is transferred to high pressure anti- Answer in still, keep 24 hours at 120 DEG C after sealing；Ethanol and deionized water is used repeatedly to rinse well, in vacuum after cooling Drying baker is dried 6 hours at 70 DEG C；By dried product at N2The lower 400 DEG C of high annealings of atmosphere 2 hours, the product of gained Thing products therefrom is RGO/In2S3Composite.
Case study on implementation sample carries out the electrochemical property test of discharge and recharge, and accompanying drawing 1 gives the charge and discharge of case study on implementation 1 sample Electricity cyclic curve.

Claims (4)

1. a RGO/In2S3The preparation method of composite, it is characterised in that specifically include following steps:
(1) dispersion soln was formed by the most ultrasonic for graphene oxide 1 hour；
(2) add appropriate indium chloride and thioacetyl in step (1), continue ultrasonic 1 hour；
(3) mixed solution of the ultrasonic mistake in step (2) is transferred in autoclave, keeps 24 hours at 120 DEG C after sealing, Use ethanol and deionized water rinsing clean after being cooled to room temperature, be dried 6 hours at 70 DEG C in vacuum drying oven；
(4) by products therefrom in step (3) at N2Carry out high annealing in atmosphere, the RGO/ that chemical property is good can be obtained In2S3Composite.
A kind of RGO/In2S3The preparation method of composite, it is characterised in that graphene oxide, The mass ratio of indium sulfide and thioacetamide is 1:1:5.
A kind of RGO/In2S3The preparation method of composite, it is characterised in that 0.1g graphite oxide When alkene is scattered in deionized water, the content of deionized water is at 10-40mL.
A kind of RGO/In2S3The preparation method of composite, it is characterised in that N2Anneal under atmosphere Temperature should control at 300-400 DEG C, annealing time is 2 hours.
CN201610516561.6A 2016-07-04 2016-07-04 A kind of RGO/In2s3the preparation method of composite Pending CN106129351A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610516561.6A CN106129351A (en) 2016-07-04 2016-07-04 A kind of RGO/In2s3the preparation method of composite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610516561.6A CN106129351A (en) 2016-07-04 2016-07-04 A kind of RGO/In2s3the preparation method of composite

Publications (1)

Publication Number Publication Date
CN106129351A true CN106129351A (en) 2016-11-16

Family

ID=57468195

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610516561.6A Pending CN106129351A (en) 2016-07-04 2016-07-04 A kind of RGO/In2s3the preparation method of composite

Country Status (1)

Country Link
CN (1) CN106129351A (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108816249A (en) * 2018-05-18 2018-11-16 盐城师范学院 The preparation method of indium trisulfide@stannic oxide/graphene nano composite material
CN108993554A (en) * 2018-07-09 2018-12-14 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of three-dimensional sheet nano wire and products thereof and application
CN111554886A (en) * 2020-04-02 2020-08-18 中南林业科技大学 Lamellar Sb @ Sb-In-S @ rGO sodium ion battery anode material and preparation method thereof
CN112209367A (en) * 2019-07-12 2021-01-12 哈尔滨理工大学 Preparation of indium sulfide nanosphere/foam graphene and electrochemical detection of levodopa
CN112209369A (en) * 2019-07-12 2021-01-12 哈尔滨理工大学 Preparation and application of indium oxide nanosheet array/foamed graphene electrode
CN112209368A (en) * 2019-07-12 2021-01-12 哈尔滨理工大学 Preparation and application of indium sulfide nanosheet array/foamed graphene electrode

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001351611A (en) * 2000-06-02 2001-12-21 Mitsubishi Chemicals Corp Positive electrode material for lithium secondary battery, positive electrode for lithium secondary battery and lithium secondary battery
CN104253269A (en) * 2013-06-29 2014-12-31 华为技术有限公司 Lithium ion secondary cell negative electrode active material, preparation method of lithium ion secondary cell negative electrode active material, lithium ion secondary cell negative electrode piece and lithium ion secondary cell

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001351611A (en) * 2000-06-02 2001-12-21 Mitsubishi Chemicals Corp Positive electrode material for lithium secondary battery, positive electrode for lithium secondary battery and lithium secondary battery
CN104253269A (en) * 2013-06-29 2014-12-31 华为技术有限公司 Lithium ion secondary cell negative electrode active material, preparation method of lithium ion secondary cell negative electrode active material, lithium ion secondary cell negative electrode piece and lithium ion secondary cell

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
XIA YANG,等: ""One-pot synthesis of graphene/In2S3 nanoparticle"", 《CRYSTENGCOMM》 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108816249A (en) * 2018-05-18 2018-11-16 盐城师范学院 The preparation method of indium trisulfide@stannic oxide/graphene nano composite material
CN108993554A (en) * 2018-07-09 2018-12-14 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of three-dimensional sheet nano wire and products thereof and application
CN108993554B (en) * 2018-07-09 2021-03-23 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of three-dimensional sheet nanowire, product and application thereof
CN112209367A (en) * 2019-07-12 2021-01-12 哈尔滨理工大学 Preparation of indium sulfide nanosphere/foam graphene and electrochemical detection of levodopa
CN112209369A (en) * 2019-07-12 2021-01-12 哈尔滨理工大学 Preparation and application of indium oxide nanosheet array/foamed graphene electrode
CN112209368A (en) * 2019-07-12 2021-01-12 哈尔滨理工大学 Preparation and application of indium sulfide nanosheet array/foamed graphene electrode
CN111554886A (en) * 2020-04-02 2020-08-18 中南林业科技大学 Lamellar Sb @ Sb-In-S @ rGO sodium ion battery anode material and preparation method thereof
CN111554886B (en) * 2020-04-02 2021-05-18 中南林业科技大学 Lamellar Sb @ Sb-In-S @ rGO sodium ion battery anode material and preparation method thereof

Similar Documents

Publication Publication Date Title
CN106129351A (en) A kind of RGO/In2s3the preparation method of composite
CN102664103B (en) Zinc cobaltate nanorod/foam nickel composite electrode, preparation method thereof and application thereof
CN103440998B (en) A kind of cobalt acid zinc nanometer sheet array/nickel foam combination electrode, preparation method and application thereof
CN106745323B (en) A kind of preparation method of iron sulphur compound and its composite material
CN107275587B (en) A kind of lithium ion silicon-carbon composite cathode material and preparation method thereof
CN102544479B (en) Preparation method of zinc cobaltate array/carbon cloth composite anode material of lithium ion battery
CN104157876B (en) A kind of lithium cell negative pole porous carbon-sijna nano composite material preparation method
CN107146915B (en) A kind of preparation method of porous bismuth-carbon composite
CN103441246B (en) The preparation method of the graphene-based tin dioxide composite material of three-dimensional N doping and application thereof
CN104835963B (en) Lithium ion battery composite anode material and preparation method thereof
CN105244191A (en) Manganese cobalt oxide porous nanometer sheet/foam nickel compound electrode material preparation method
CN110581026B (en) Transition metal selenide/ordered porous graphene aerogel composite electrode material and preparation method thereof
CN105460917A (en) Nitrogen-doped carbon nanotube adopting hierarchical structure and preparation method
CN106784654A (en) A kind of preparation method of graphene coated cobalt acid lithium material
CN104733716A (en) Molybdenum oxide/nitrogen-doped carbon composite electrode material and preparation method thereof
CN103730638A (en) Preparation method of nitrogen-doped carbon material
CN103390752A (en) Graphene-based composite material, preparation method of same and application of same in lithium-sulfur battery
CN106673655A (en) Preparation method of self-supporting thin film of graphene enhanced three-dimensional porous carbon
CN103274385B (en) A kind of lithium ion battery negative material carbon microballoon and preparation method thereof
CN107317001A (en) A kind of artificial gold/N doping carbonization bacteria cellulose lithium ion battery negative material and preparation method thereof
CN110357100A (en) A kind of method and application preparing carbon material using waste tire
CN107959017A (en) A kind of solid carbon ball lithium ion battery negative material of graphene/oxide coated by zinc and preparation method thereof
CN105514375A (en) Carbon-coated Na0.55 Mn2O4.1.5H2O nanocomposite and preparation method thereof
CN111403718A (en) Titanium niobium oxide/vertical graphene/titanium carbide-carbon composite material and preparation method and application thereof
CN110311133A (en) A kind of three-dimensional carbon negative pole material and preparation method thereof, application

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20161116