CN108390042A - A kind of carbon packet SnS2Composite material and preparation method and application - Google Patents

A kind of carbon packet SnS2Composite material and preparation method and application Download PDF

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Publication number
CN108390042A
CN108390042A CN201810170239.1A CN201810170239A CN108390042A CN 108390042 A CN108390042 A CN 108390042A CN 201810170239 A CN201810170239 A CN 201810170239A CN 108390042 A CN108390042 A CN 108390042A
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sns
composite material
ion battery
carbon
hollow
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官轮辉
赵毅
吴初新
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Fujian Institute of Research on the Structure of Matter of CAS
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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
    • H01M4/366—Composites as layered products
    • 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
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
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  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention belongs to new energy field, more particularly to a kind of carbon packet SnS2Composite material and preparation method and application.The present invention provides a kind of carbon packet SnS2Composite material, the material have hollow core-shell structure, shell be hollow carbon shell, it is interior be SnS2Nanometer sheet, SnS2Spatial joint clearance is remained between hollow carbon shell.The material can be applied to lithium ion battery, sodium-ion battery or kalium ion battery as negative material.

Description

A kind of carbon packet SnS2Composite material and preparation method and application
Technical field
The invention belongs to new energy field, more particularly to a kind of carbon packet SnS2Composite material and preparation method and application.
Background technology
In lithium ion battery, sodium-ion battery and kalium ion battery, there is stratiform CdI2The SnS of type structure2Frequently as Cell negative electrode material shows potential using value.However huge volume when low intrinsic conductivity and insertion/deintercalation sodium ion Change the storing up electricity performance for causing its poor.Construct nanostructure SnS2 and with the carbon material of high conductivity (carbon nanotube, graphite Alkene, hard carbon etc.) it is compound be the effective ways to solve the above problems.
Wang Jingjing et al. are prepared for carbon packet SnS by the method for vacuum-sintering2Composite material, the composite material For nucleocapsid, as anode material of lithium-ion battery, in 50mA g-1Current density under, 50 times cycle after capacity protect It holds in 570mAh g-1.(ACS Applied Materials＆Interfaces 2015,7,11476-11481.) is this compound The design feature of material is carbon packet SnS2, but there is no spatial joint clearance between SnS2 and carbon ball, therefore can not be in SnS2Embedding sodium/de- Cushion space is provided during the volume change of sodium so that the promotion of the cycle performance and high rate performance of entire composite material by To restriction.
Li Haomiao et al. are prepared for SnS by the method for sintering2The structure of/C composite, the composite material is carbon Material is wrapped SnS2, as anode material of lithium-ion battery, in 100mA g-1Current density under, 300 times cycle after Capacity is maintained at 758mAh g-1.The SnS of (RSC Advanced, 2016,6,35197-35202) this structure2Composite material Certain cushion space can be provided for the volume change of embedding sodium/removing sodium, but the cushion space is uncontrollable, in long-term cycle Composite material meeting electrode slice because volume change fall off, to influence the cycle performance of battery.
In view of the problems of the existing technology, the present invention devises a kind of carbon packet SnS2Composite material, SnS in the material2 It for nanometer sheet, and is covered by among hollow carbon shell, and SnS2Spatial joint clearance is remained between hollow carbon sphere.This structure Material is as lithium ion battery, sodium-ion battery or kalium ion battery cathode, due to SnS2It is pre- between nanometer sheet and hollow carbon shell Space is stayed, the volume change caused by ion deinsertion can be buffered effectively, and the battery of material can be effectively promoted Cycle performance.It is the SnS of nano-sheet in addition, compared with block2Deintercalation ion can be reduced in charge and discharge process in material The transmission range in portion and storing up electricity capacity is improved, cycle performance and high rate performance are followed to improve battery.
Invention content
In view of the problems of the existing technology, the present invention provides a kind of carbon packet SnS2Composite material and preparation method and Using.
The technical scheme is that：
A kind of carbon packet SnS2Composite material, SnS in the material2For nanometer sheet, and it is covered by among hollow carbon shell, and SnS2Spatial joint clearance is remained between hollow carbon shell.
The size of the hollow carbon shell is 10nm~100um, preferably 100nm~1000nm；
The SnS2The thickness of nanometer sheet is 1~35nm, SnS2The planar dimension of nanometer sheet is 10nm~100um, excellent It is 100nm~1000nm to select planar dimension.
A kind of carbon packet SnS2Composite material application, as negative material be applied to lithium ion battery, sodium-ion battery Or kalium ion battery.
One kind includes the carbon packet SnS2Composite material secondary cell, the secondary cell includes lithium-ion electric Pond, sodium-ion battery or kalium ion battery, the lithium ion battery, sodium-ion battery or kalium ion battery include positive, negative Pole and electrolyte；The cathode includes：Collector and the negative material being supported on the collector；Wherein, the negative material Contain the composite material.
A kind of carbon packet SnS2Composite material preparation method, include the following steps：
By the hollow SnO of carbon packet that size is 10nm~100um2Ball and thiocarbamide press SnO2:CH4N2S=(0.01~0.99)： 1 mass ratio is sealed in glass tube with vacuum together, and is positioned in 350~550 DEG C of Muffle furnaces naturally cold after heat preservation 6~for 24 hours But to room temperature, by product filtering, deionized water washing, it is dried to obtain the carbon packet SnS2Composite material.
Compared with prior art, carbon packet SnS of the invention2Composite material, the SnS coated inside hollow carbon shell2's Structure is nano-sheet, on the one hand this structure is conducive to SnS2Enough spaces are reserved between hollow carbon shell, are conducive to delay The variation for rushing volume caused by battery intermediate ion deintercalation, be on the other hand beneficial to reduce ion active material internal transmission away from From quickening ionic conduction speed, to improve battery high rate performance.
Compared with prior art, carbon packet SnS of the invention2Composite material preparation method, further improve be, By the hollow SnO of carbon packet2Ball and thiocarbamide are sealed in glass tube with vacuum by a certain percentage to be reacted, and two reactants are placed in one In a closed space, can enable the thiocarbamide of decomposition fully with SnO2Adequately chemical reaction occurs for ball contact, while It will not be lost because of the decomposition of thiocarbamide, thiocarbamide dosage will not be caused uncontrollable, and then realize the SnS of nanometer chip architecture2's Controllable growth.The displacement reaction decomposed using thiocarbamide in confined space can also avoid directly making using hydrogen sulfide toxic gas At danger.
Beneficial effects of the present invention are：
The carbon packet SnS of the present invention2Composite material have hollow core-shell structure, outer cladding layer be hollow carbon shell, it is hollow It is SnS in carbon shell2Nanometer sheet, SnS2Spatial joint clearance is remained between hollow carbon shell.The material of this structure is as lithium-ion electric Pond, sodium-ion battery or kalium ion battery cathode, due to SnS2Space has been reserved between nanometer sheet and hollow carbon shell, it is de- in ion Volume change can be buffered effectively caused by embedding, can effectively promote the cycle performance of battery of material.In addition, with block Body is compared, and is the SnS of nano-sheet2Transmission range and raising of the deintercalation ion in material internal in charge and discharge process can be reduced Storing up electricity capacity, to improve the cycle performance and high rate performance of battery.The composite material of the present invention is born as sodium-ion battery Pole material shows excellent cycle performance, in 1A g-1Current density under, 150 times cycle after capacity be maintained at 435mAh g-1, while in charging and discharging currents from 0.1A g-1Increase to 10A g-1High rate performance test is carried out, in 10Ag-1Descend it Capacity is maintained at 230mAh g-1, return to 0.1A g-1When, capacity remains at 760 mAh g-1, show excellent multiplying power Performance.
Description of the drawings
Fig. 1 is carbon packet SnS prepared by embodiment 12The transmission electron microscope photo of composite material.
Fig. 2 is carbon packet SnS prepared by embodiment 12The X-ray diffractogram of composite material.
Fig. 3 is the carbon packet SnS prepared with embodiment 12Composite material is the battery charging and discharging of anode material of lithium-ion battery Cycle performance figure.
Fig. 4 is the carbon packet SnS prepared with embodiment 12Composite material is the battery charging and discharging of anode material of lithium-ion battery High rate performance figure.
Specific implementation mode
Embodiment 1：
1) silicon ball that diameter is about 400nm being added in the mixed solution of deionized water and ethyl alcohol, ultrasonic disperse is uniform, Obtain mixed liquor A；Urea and K is added to mixed liquor A2SnO3·3H2O, ultrasonic disperse is uniform, obtains mixed liquid B；Wherein, ethyl alcohol Volume ratio with water is 37.5ml：12.5ml, silicon ball, urea and K2SnO3·3H2The mass ratio of O is 360mg：1.8g：240mg；
2) mixed liquid B is transferred in 100ml water heating kettles, is placed in 170 DEG C of hydro-thermal case, it is naturally cold after heat preservation 2h But it is then repeated once operation above, is obtained after filtration, washing and drying with water and ethyl alcohol respectively washing three times to room temperature SnO2Coated Si O2Ball compound (SiO2@SnO2)；
3) by SiO2@SnO2It is added in 2M NaOH solutions, is placed on and is set as in 60 DEG C of heating plate, stirred at 60 DEG C of constant temperature 12h obtains hollow SnO after filtration, washing and drying2Ball；
4) by hollow SnO2Ball is added into Tris-buffer solution (10mM；PH=8.5 it in), is uniformly dispersed, is mixed Liquid C；Dopamine hydrochloride is added into mixed liquor C, reaction is stirred at room temperature for 24 hours.Through being filtered, washed, being dried to obtain macromolecule/SnO2 It is heated to 500 DEG C by compound in argon gas, keeps the temperature cooled to room temperature after 3h, obtains the hollow SnO of carbon coating2It is compound Object (SnO2@C)；Wherein Tris-buffer solution, SnO2The ratio of ball and Dopamine hydrochloride is 75ml：120mg：240mg；
5) by SnO2It is sealed in glass tube with vacuum together with@C compounds and thiocarbamide, and is positioned in 350 DEG C of Muffle furnaces and protects Temperature 6~for 24 hours after cooled to room temperature, by product filtering, deionized water washing, be dried to obtain carbon coating SnS2Nanometer sheet is compound Object, i.e., carbon packet SnS of the present invention2Composite material.Wherein, the SnO in this step in SnO2@C compounds2With the matter of thiocarbamide Amount is than being (0.28：1)；
Fig. 1 is carbon packet SnS manufactured in the present embodiment2The transmission electron microscope photo of composite material, it is observed that having in figure The SnS of nano-sheet2It is coated on hollow ball inside, SnS2There are spatial joint clearance, SnS between hollow carbon shell2The thickness of nanometer sheet Degree is 1-35nm, and plane sizes are less than 400nm.
6) product of step 5) (70wt%), conductive black (15wt%) and carboxymethyl cellulose (CMC 15wt%) are added Enter and crush grinding in agate mortar, wherein deionized water is as dispersant.The nickel foam of the drying flattened is got out, and right It is weighed.The slurry obtained after grinding uniformly is applied in foamed nickel current collector, 80 DEG C of vacuum drying 12h, after drying Electrode slice weighs, and the front and back stock quality of poor quality that can be obtained on each electrode slice is smeared according to collector.It, will after weighing 80 DEG C of vacuum drying 2h of electrode slice, the electrode slice after drying is put into glove box, with button cell to be assembled.
7) assembling that button cell is carried out in the glove box full of argon gas, using metallic sodium piece as cathode, glass fibre For diaphragm, made electrode slice is anode.
8) constant current charge-discharge test mainly investigates charging and discharging capacity of the sodium ion half-cell under different electric currents, cyclicity Energy and high rate performance.Sodium ion half-cell in the initial state anode in be not present sodium ion, so battery most proceeds by perseverance Electricity is banished, the sodium ion in metallic sodium piece is made to be embedded in positive electrode；After electric discharge, positive electrode is in rich sodium state, charging Test starts, with this loop test.Button cell test voltage is 0.05-2.8V, and charging and discharging currents density is according to experiment condition It is set as 100mA g-1~10A g-1Differ.
Embodiment 2
The present embodiment difference from example 1 is that：About 100 nm of the diameter using silicon ball in step 1)；Step 5) SnO in2Mass ratio with thiocarbamide is (0.99：1), the temperature of Muffle furnace is 550 DEG C.
Embodiment 3
The present embodiment difference from example 1 is that：About 1000 nm of the diameter using silicon ball in step 1)；Step It is rapid 5) in SnO2Mass ratio with thiocarbamide is (0.1：1).
Embodiment 4
The present embodiment difference from example 1 is that：The about 10nm of the diameter using silicon ball in step 1)；Step 5) Middle SnO2Mass ratio with thiocarbamide is (0.01：1), the temperature of Muffle furnace is 250 DEG C.
Embodiment 5
The present embodiment difference from example 1 is that：About 100 um of the diameter using silicon ball in step 1)；Step 5) SnO in2Mass ratio with thiocarbamide is (0.1：1).

Claims (6)

1. a kind of carbon packet SnS2Composite material, which is characterized in that the carbon packet SnS2Composite material has hollow core-shell structure, I.e. outer shell is hollow carbon shell, kernel SnS2Nanometer sheet, and hollow carbon shell and SnS2Spatial joint clearance is remained between nanometer sheet.
2. composite material according to claim 1, which is characterized in that the size of the hollow carbon shell be 10nm~ 100um, the SnS2The thickness of nanometer sheet is 1~35nm, SnS2The planar dimension of nanometer sheet is 10nm~100um.
3. composite material according to claim 1 or 2, which is characterized in that the size of the hollow carbon shell be 100nm~ 1000nm, the SnS2The planar dimension of nanometer sheet is 100nm~1000nm.
4. a kind of carbon packet SnS2The preparation method of composite material, which is characterized in that include the following steps：
By the hollow SnO of carbon packet that size is 10nm~100um2Ball and thiocarbamide press SnO2:CH4N2S=(0.01~0.99):1 matter Amount ratio be sealed in together in glass tube with vacuum, and be positioned in 250~550 DEG C of Muffle furnaces keep the temperature 6~naturally cool to room afterwards for 24 hours Temperature by product filtering, deionized water washing, is dried to obtain the carbon packet SnS2Composite material.
5. a kind of any one of claim 1-3 composite materials are in primary or secondary electrochemical electric organ, high-energy power generation device With the application in electrochemical luminescence modulating system, which is characterized in that in secondary lithium battery, secondary sodium-ion battery or two As the application of cell negative electrode material in secondary kalium ion battery.
6. a kind of including any one of claim the 1-3 secondary lithium battery of the composite material, secondary sodium-ion battery Or kalium ion battery, which is characterized in that the secondary lithium battery, secondary sodium-ion battery or kalium ion battery include：Just Pole, cathode and electrolyte；The cathode includes：Collector and the negative material being supported on the collector；Wherein, the cathode Material contains the composite material.
CN201810170239.1A 2018-03-01 2018-03-01 A kind of carbon packet SnS2Composite material and preparation method and application Pending CN108390042A (en)

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CN109301229A (en) * 2018-11-12 2019-02-01 陕西科技大学 A kind of preparation method and application of kalium ion battery negative electrode material graphene coated tin oxide/stannic disulfide nano flower
CN109304187A (en) * 2018-10-16 2019-02-05 安徽师范大学 A kind of hollow nanocomposite, preparation method and applications
CN110684507A (en) * 2019-10-09 2020-01-14 中国科学院宁波材料技术与工程研究所 Core-shell structure type wave-absorbing material and preparation method and application thereof
CN110844933A (en) * 2019-11-29 2020-02-28 河北省科学院能源研究所 Preparation method of stannous sulfide composite negative electrode material
CN111092211A (en) * 2019-12-31 2020-05-01 青岛科技大学 Micro-cavity liquid state vulcanization preparation method of carbon and sulfide composite electrode material
CN111584845A (en) * 2020-05-20 2020-08-25 信阳师范学院 Preparation method and application of N, S co-doped carbon/tin disulfide composite material
CN111682184A (en) * 2020-06-23 2020-09-18 欣旺达电动汽车电池有限公司 Tin-based composite material and preparation method thereof, negative plate and lithium ion battery
CN111785967A (en) * 2020-06-30 2020-10-16 北京高压科学研究中心 Core-shell structure chalcogenide negative electrode material and preparation method thereof
CN113206225A (en) * 2021-04-12 2021-08-03 华南理工大学 Hollow carbon sphere anchored with metal sulfide, preparation method thereof and application of hollow carbon sphere in preparation of potassium ion battery cathode
CN113880130A (en) * 2021-12-06 2022-01-04 中博龙辉装备集团股份有限公司 Stannous sulfide carbon composite material and preparation method and application thereof
US11417877B1 (en) 2021-04-14 2022-08-16 Guangdong University Of Technology Carbon quantum dot/carbon coated VSe2 composite material (VSe2@CQD) for potassium ion battery and preparation method thereof

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CN109304187A (en) * 2018-10-16 2019-02-05 安徽师范大学 A kind of hollow nanocomposite, preparation method and applications
CN109304187B (en) * 2018-10-16 2021-05-14 安徽师范大学 Hollow nano composite material, preparation method and application thereof
CN109301229A (en) * 2018-11-12 2019-02-01 陕西科技大学 A kind of preparation method and application of kalium ion battery negative electrode material graphene coated tin oxide/stannic disulfide nano flower
CN109301229B (en) * 2018-11-12 2021-02-05 陕西科技大学 Preparation method and application of graphene-coated tin oxide/tin disulfide nanoflower serving as negative electrode material of potassium ion battery
WO2021068660A1 (en) * 2019-10-09 2021-04-15 中国科学院宁波材料技术与工程研究所 Core-shell structure wave-absorbing material, preparation method therefor, and application thereof
CN110684507A (en) * 2019-10-09 2020-01-14 中国科学院宁波材料技术与工程研究所 Core-shell structure type wave-absorbing material and preparation method and application thereof
CN110684507B (en) * 2019-10-09 2021-06-29 中国科学院宁波材料技术与工程研究所 Core-shell structure type wave-absorbing material and preparation method and application thereof
CN110844933A (en) * 2019-11-29 2020-02-28 河北省科学院能源研究所 Preparation method of stannous sulfide composite negative electrode material
CN110844933B (en) * 2019-11-29 2022-02-11 河北省科学院能源研究所 Preparation method of stannous sulfide composite negative electrode material
CN111092211A (en) * 2019-12-31 2020-05-01 青岛科技大学 Micro-cavity liquid state vulcanization preparation method of carbon and sulfide composite electrode material
CN111584845A (en) * 2020-05-20 2020-08-25 信阳师范学院 Preparation method and application of N, S co-doped carbon/tin disulfide composite material
CN111584845B (en) * 2020-05-20 2022-04-29 信阳师范学院 Preparation method and application of N, S co-doped carbon/tin disulfide composite material
CN111682184A (en) * 2020-06-23 2020-09-18 欣旺达电动汽车电池有限公司 Tin-based composite material and preparation method thereof, negative plate and lithium ion battery
CN111682184B (en) * 2020-06-23 2023-07-14 欣旺达电动汽车电池有限公司 Tin-based composite material, preparation method thereof, negative plate and lithium ion battery
CN111785967A (en) * 2020-06-30 2020-10-16 北京高压科学研究中心 Core-shell structure chalcogenide negative electrode material and preparation method thereof
CN113206225A (en) * 2021-04-12 2021-08-03 华南理工大学 Hollow carbon sphere anchored with metal sulfide, preparation method thereof and application of hollow carbon sphere in preparation of potassium ion battery cathode
US11417877B1 (en) 2021-04-14 2022-08-16 Guangdong University Of Technology Carbon quantum dot/carbon coated VSe2 composite material (VSe2@CQD) for potassium ion battery and preparation method thereof
CN113880130A (en) * 2021-12-06 2022-01-04 中博龙辉装备集团股份有限公司 Stannous sulfide carbon composite material and preparation method and application thereof

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