CN105140513A - MoS2/C lithium ion battery cathode composite material synthesized by taking carbohydrate as carbon source, and preparation method for MoS2/C lithium ion battery cathode composite material - Google Patents

MoS2/C lithium ion battery cathode composite material synthesized by taking carbohydrate as carbon source, and preparation method for MoS2/C lithium ion battery cathode composite material Download PDF

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Publication number
CN105140513A
CN105140513A CN201510439773.4A CN201510439773A CN105140513A CN 105140513 A CN105140513 A CN 105140513A CN 201510439773 A CN201510439773 A CN 201510439773A CN 105140513 A CN105140513 A CN 105140513A
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China
Prior art keywords
lithium ion
ion battery
carbohydrate
carbon source
composite material
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CN201510439773.4A
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Inventor
蔡亚菱
康健
高琍玲
张玉岁
朱文浩
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JIANGSU XINGUANG ENVIRONMENTAL PROTECTION ENGINEERING Co Ltd
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JIANGSU XINGUANG ENVIRONMENTAL PROTECTION ENGINEERING Co Ltd
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Priority to CN201510439773.4A priority Critical patent/CN105140513A/en
Publication of CN105140513A publication Critical patent/CN105140513A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/581Chalcogenides or intercalation compounds thereof
    • H01M4/5815Sulfides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/04Processes of manufacture in general
    • H01M4/0471Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/583Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/5835Comprising fluorine or fluoride salts
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses an MoS2/C lithium ion battery cathode composite material synthesized by taking carbohydrate as a carbon source, and a preparation method for the MoS2/C lithium ion battery cathode composite material. The MoS2/C lithium ion battery cathode composite material is prepared from sodium molybdate, thiourea carbohydrate and deionized water through a hydrothermal reaction. Compared with the conventional lithium ion battery cathode composite material, the MoS2/C lithium ion battery cathode composite material has the following obvious advantages: a), the preparation raw materials are low in cost, easy to purchase and high in cost performance; b), the preparation process reduces the raw material losses, and is easy to operate and realize industrial production; and c) the energy transformation ratio of the prepared battery is higher.

Description

A kind of MoS taking carbohydrate as carbon source and synthesize 2/ C composite cathode material of lithium ion battery and preparation method thereof
Technical field
The present invention relates to electrochemical field, particularly relate to a kind of MoS taking carbohydrate as carbon source and synthesize 2/ C composite cathode material of lithium ion battery and preparation method thereof.
Background technology
Chemical power source realizes the device that electric energy and chemical energy change mutually, is can the important medium of more reasonable energy utilization.The excellent properties such as the lithium ion battery of a new generation has that operating voltage is high, volume is little, specific capacity is high, lightweight, memory-less effect.Commercial Li-ion battery many employings material with carbon element is as negative pole, what material with carbon element use was more is graphite, graphite is good cyclical stability because design feature has, but its shortcoming also can not be ignored, first the restriction of theoretical capacity can not adapt to the requirement of height ratio capacity, secondly intercalation potential is close with lithium metal sedimentation potential, and lithium metal may produce dendrite precipitation at electrode surface, concerning battery, have safety issue.In recent years about negative material large quantity research also round raising battery capacity, strengthen battery cyclical stability and improve security performance launch, how to seek a kind of good negative material and require study with the demand of satisfied society.
Summary of the invention
Goal of the invention: in order to overcome the defect in prior art existing for traditional lithium cell cathode material, the first object of the present invention be propose a kind of with low cost, prepare easy, energy conversion efficiency high take carbohydrate as the MoS of carbon source synthesis 2/ C composite cathode material of lithium ion battery.
The second object of the present invention is the preparation method proposing above-mentioned composite material.
Technical scheme: in order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of MoS taking carbohydrate as carbon source and synthesize 2/ C composite cathode material of lithium ion battery, comprises the raw materials of following component:
The ratio of amount of substance is sodium molybdate, thiocarbamide, the carbohydrate of 1:4.1-4.3:1.17-1.19, deionized water; Wherein the addition of deionized water is the deionized water of the corresponding 60mL of sodium molybdate of 1mol.
Further, described carbohydrate is the one in glucose, sucrose and soluble starch.
The above-mentioned MoS taking carbohydrate as carbon source and synthesize 2the preparation method of/C composite cathode material of lithium ion battery, comprises the following steps:
(1) get out the raw materials of aequum, after mixing, put into hydrothermal reaction kettle, at 180-220 DEG C, carry out hydro-thermal reaction 24h;
(2) after above-mentioned product being filtered at 70-80 DEG C vacuumize 24h, obtain black powder;
(3) mist of argon gas and hydrogen will be full of in tube furnace, the black powder that step (2) obtains be placed in tube furnace with the temperature 2-2.5h of 700-800 DEG C; Be incubated rear cool to room temperature and can obtain required MoS 2/ C composite cathode material of lithium ion battery.
Further, the argon gas in described step (3) in tube furnace and the volume ratio of hydrogen are 9:1.
More preferred, in described step (4), the temperature ramp of tube furnace is 16-20 DEG C/min.
Beneficial effect: a kind of MoS taking carbohydrate as carbon source and synthesize provided by the invention 2/ C composite cathode material of lithium ion battery and preparation method thereof, be prepared from by hydro-thermal reaction by sodium molybdate, thiocarbamide, carbohydrate and deionized water, there is compared with traditional composite cathode material of lithium ion battery following obviously advantage: a) raw materials is with low cost, easy purchase, cost performance is high; B) decrease the significant loss in preparation process, be easy to operation and suitability for industrialized production; C) the cell power conversion rate be prepared from is higher.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1:
A kind of MoS taking carbohydrate as carbon source and synthesize 2/ C composite cathode material of lithium ion battery, comprises the raw materials of following component:
Sodium molybdate 0.300g, thiocarbamide 0.400g and glucose 1.000g, deionized water 60mL; The above-mentioned MoS taking carbohydrate as carbon source and synthesize 2the preparation method of/C composite cathode material of lithium ion battery, comprises the following steps:
(1) get out the raw materials of aequum, after mixing, put into hydrothermal reaction kettle, at 200 DEG C, carry out hydro-thermal reaction 24h;
(2) after above-mentioned product being filtered at 70 DEG C vacuumize 24h, obtain black powder;
(3) will be full of the mist of argon gas and hydrogen in tube furnace, its volume ratio is 9:1, the black powder that step (2) obtains is placed in tube furnace with the temperature 2h of 800 DEG C; Be incubated rear cool to room temperature and can obtain required MoS 2/ C composite cathode material of lithium ion battery, wherein the heating rate of temperature is 20 DEG C/min.
Embodiment 2:
A kind of MoS taking carbohydrate as carbon source and synthesize 2/ C composite cathode material of lithium ion battery, comprises the raw materials of following component:
Sodium molybdate 0.300g, thiocarbamide 0.400g and sucrose 0.951g, deionized water 60mL; The above-mentioned MoS taking carbohydrate as carbon source and synthesize 2the preparation method of/C composite cathode material of lithium ion battery, comprises the following steps:
(1) get out the raw materials of aequum, after mixing, put into hydrothermal reaction kettle, at 180 DEG C, carry out hydro-thermal reaction 24h;
(2) after above-mentioned product being filtered at 80 DEG C vacuumize 24h, obtain black powder;
(3) will be full of the mist of argon gas and hydrogen in tube furnace, its volume ratio is 9:1, the black powder that step (2) obtains is placed in tube furnace with the temperature 2.5h of 700 DEG C; Be incubated rear cool to room temperature and can obtain required MoS 2/ C composite cathode material of lithium ion battery, wherein the heating rate of temperature is 16 DEG C/min.
Embodiment 3:
A kind of MoS taking carbohydrate as carbon source and synthesize 2/ C composite cathode material of lithium ion battery, comprises the raw materials of following component:
Sodium molybdate 0.300g, thiocarbamide 0.400g and soluble starch 0.900g, deionized water 60mL; The above-mentioned MoS taking carbohydrate as carbon source and synthesize 2the preparation method of/C composite cathode material of lithium ion battery, comprises the following steps:
(1) get out the raw materials of aequum, after mixing, put into hydrothermal reaction kettle, at 220 DEG C, carry out hydro-thermal reaction 24h;
(2) after above-mentioned product being filtered at 75 DEG C vacuumize 24h, obtain black powder;
(3) will be full of the mist of argon gas and hydrogen in tube furnace, its volume ratio is 9:1, the black powder that step (2) obtains is placed in tube furnace with the temperature 2.25h of 750 DEG C; Be incubated rear cool to room temperature and can obtain required MoS 2/ C composite cathode material of lithium ion battery, wherein the heating rate of temperature is 18 DEG C/min.
To sum up, can find out from embodiment 1-3, the present invention take carbohydrate as the MoS of carbon source synthesis 2/ C composite cathode material of lithium ion battery and preparation method thereof, be prepared from by hydro-thermal reaction by sodium molybdate, thiocarbamide, carbohydrate and deionized water, there is compared with traditional composite cathode material of lithium ion battery following obviously advantage: a) raw materials is with low cost, easy purchase, cost performance is high; B) decrease the significant loss in preparation process, be easy to operation and suitability for industrialized production; C) the cell power conversion rate be prepared from is higher.
Should be understood that, above embodiment is only not used in for illustration of the present invention and limits the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.

Claims (5)

1. one kind is the MoS that carbon source is synthesized with carbohydrate 2/ C composite cathode material of lithium ion battery, is characterized in that the raw materials comprising following component:
The ratio of amount of substance is sodium molybdate, thiocarbamide, the carbohydrate of 1:4.1-4.3:1.17-1.19, deionized water, and wherein the addition of deionized water is the deionized water of the corresponding 60mL of sodium molybdate of 1mol.
2. the MoS taking carbohydrate as carbon source and synthesize according to claim 1 2/ C composite cathode material of lithium ion battery, is characterized in that: described carbohydrate is the one in glucose, sucrose and soluble starch.
3. the MoS taking carbohydrate as carbon source and synthesize as claimed in claim 1 2the preparation method of/C composite cathode material of lithium ion battery, is characterized in that comprising the following steps:
(1) get out the raw materials of aequum, after mixing, put into hydrothermal reaction kettle, at 180-220 DEG C, carry out hydro-thermal reaction 24h;
(2) after above-mentioned product being filtered at 70-80 DEG C vacuumize 24h, obtain black powder;
(3) mist of argon gas and hydrogen will be full of in tube furnace, the black powder that step (2) obtains be placed in tube furnace with the temperature 2-2.5h of 700-800 DEG C; Be incubated rear cool to room temperature and can obtain required MoS 2/ C composite cathode material of lithium ion battery.
4. the MoS taking carbohydrate as carbon source and synthesize according to claim 3 2the preparation method of/C composite cathode material of lithium ion battery, is characterized in that: the argon gas in described step (3) in tube furnace and the volume ratio of hydrogen are 9:1.
5. the MoS taking carbohydrate as carbon source and synthesize according to claim 3 2the preparation method of/C composite cathode material of lithium ion battery, is characterized in that: in described step (4), the temperature ramp of tube furnace is 16-20 DEG C/min.
CN201510439773.4A 2015-07-23 2015-07-23 MoS2/C lithium ion battery cathode composite material synthesized by taking carbohydrate as carbon source, and preparation method for MoS2/C lithium ion battery cathode composite material Pending CN105140513A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105742602A (en) * 2016-03-27 2016-07-06 华南理工大学 Sn/MoS<2>/C composite material for sodium ion battery negative electrode and preparation method therefor
CN106848228A (en) * 2017-01-24 2017-06-13 同济大学 A kind of method for preparing molybdenum bisuphide/carbon combined multi-stage Porous materials
CN107188230A (en) * 2017-05-24 2017-09-22 岭南师范学院 A kind of molybdenum disulfide carbon is combined bouquet and its preparation method and application
CN108212178A (en) * 2018-02-02 2018-06-29 郑州大学 The preparation method of molybdenum disulfide/carbon composite, catalyst and preparation method thereof
CN110165173A (en) * 2019-05-17 2019-08-23 华南理工大学 A kind of preparation method of sodium-ion battery flexible transition metal sulfide negative electrode material
CN111235602A (en) * 2018-11-28 2020-06-05 中国科学院大连化学物理研究所 High-performance hydrogen evolution electrode and preparation and application thereof
CN111902975A (en) * 2017-12-06 2020-11-06 汉阳大学校产学协力团 Anode active material for lithium-sulfur secondary battery and method for preparing same
KR20210094375A (en) * 2020-01-21 2021-07-29 한국과학기술연구원 Nitrogen-doped molybdenum sulfide/carbon composite for sodium ion battery of core-shell structure, manufacturing method thereof and sodium ion battery comprising the same

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CN102683039A (en) * 2012-05-15 2012-09-19 中国科学院长春应用化学研究所 Electrochemical capacitor

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CN102683039A (en) * 2012-05-15 2012-09-19 中国科学院长春应用化学研究所 Electrochemical capacitor

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KUN CHANG等: ""Graphene-like MoS2/amorphous carbon composites with high capacity and excellent stability as anode materials for lithium ion batteries"", 《J. MATER. CHEM》 *

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105742602A (en) * 2016-03-27 2016-07-06 华南理工大学 Sn/MoS<2>/C composite material for sodium ion battery negative electrode and preparation method therefor
CN105742602B (en) * 2016-03-27 2018-07-20 华南理工大学 A kind of sodium-ion battery cathode Sn/MoS2/ C composite and preparation method thereof
CN106848228A (en) * 2017-01-24 2017-06-13 同济大学 A kind of method for preparing molybdenum bisuphide/carbon combined multi-stage Porous materials
CN107188230A (en) * 2017-05-24 2017-09-22 岭南师范学院 A kind of molybdenum disulfide carbon is combined bouquet and its preparation method and application
CN107188230B (en) * 2017-05-24 2019-04-26 岭南师范学院 A kind of compound bouquet of molybdenum disulfide-carbon and its preparation method and application
CN111902975A (en) * 2017-12-06 2020-11-06 汉阳大学校产学协力团 Anode active material for lithium-sulfur secondary battery and method for preparing same
CN108212178B (en) * 2018-02-02 2020-12-22 郑州大学 Preparation method of molybdenum disulfide/carbon composite material, catalyst and preparation method thereof
CN108212178A (en) * 2018-02-02 2018-06-29 郑州大学 The preparation method of molybdenum disulfide/carbon composite, catalyst and preparation method thereof
CN111235602A (en) * 2018-11-28 2020-06-05 中国科学院大连化学物理研究所 High-performance hydrogen evolution electrode and preparation and application thereof
CN111235602B (en) * 2018-11-28 2021-08-31 中国科学院大连化学物理研究所 High-performance hydrogen evolution electrode and preparation and application thereof
CN110165173A (en) * 2019-05-17 2019-08-23 华南理工大学 A kind of preparation method of sodium-ion battery flexible transition metal sulfide negative electrode material
CN110165173B (en) * 2019-05-17 2022-03-29 华南理工大学 Preparation method of flexible transition metal sulfide negative electrode material of sodium ion battery
KR20210094375A (en) * 2020-01-21 2021-07-29 한국과학기술연구원 Nitrogen-doped molybdenum sulfide/carbon composite for sodium ion battery of core-shell structure, manufacturing method thereof and sodium ion battery comprising the same
KR102304760B1 (en) 2020-01-21 2021-09-28 한국과학기술연구원 Nitrogen-doped molybdenum sulfide/carbon composite for sodium ion battery of core-shell structure, manufacturing method thereof and sodium ion battery comprising the same

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