CN106876702A - A kind of sodium-ion battery negative pole coal tar pitch resin base amorphous carbon coats the preparation method and application of few layer molybdenum disulfide nano box - Google Patents
A kind of sodium-ion battery negative pole coal tar pitch resin base amorphous carbon coats the preparation method and application of few layer molybdenum disulfide nano box Download PDFInfo
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Abstract
The present invention relates to nano material production technical field, a kind of sodium-ion battery negative pole coal tar pitch resin base amorphous carbon coats the preparation method and application of few layer molybdenum disulfide nano box.Preparation method includes procedure below：Saturated aqueous sodium chloride is added dropwise in absolute ethyl alcohol, dry cake is obtained sodium chloride template after suction filtration, coal tar pitch resin, four thio ammonium molybdate, pore creating material polymethyl methacrylate and sodium chloride template are added in N-methyl pyrrolidones by a certain percentage, agitating heating solvent evaporated carries out carbonization treatment, it is cooled to room temperature taking-up, adopt and sodium chloride template is washed with deionized, obtain target material after drying and be applied particularly in sodium-ion battery.The method have the advantages that：It is the carbon source and pore creating material wide material sources that use, cheap；Sodium chloride template and N-methyl pyrrolidinone solvent can be recycled, low cost；Target material shows reversible storage sodium capacity and preferable high rate performance higher as anode material of lithium-ion battery.
Description
Technical field
Wataru of the present invention and a kind of few layer molybdenum bisuphide of sodium-ion battery negative pole coal tar pitch resin base amorphous carbon cladding are received
The preparation method and application of rice box, belongs to nano material production technical field.
Background technology
Electric energy is the critical energy for maintaining human society operation and development, and substantial amounts of storage is needed during the utilization of electric energy
Can device.Lithium ion battery possesses the excellent properties such as high voltage, high-energy-density and long circulation life, obtains in daily life
Extensive use.But lithium resource content in the earth's crust is limited and skewness, in the case where not considering to reclaim, lithium has been verified
Resource reserve is only capable of meeting the demand of human future decades.Thus make using lithium ion battery as extensive energy storage device
With, however it remains some are difficult to the problem for overcoming.There is similar physicochemical properties and similar storage in view of sodium and lithium
Mechanism, and rich reserves, the cost of raw material are cheap in nature, sodium-ion battery has huge for large-scale energy storage system
Potentiality.
Electrode material is the key issue in sodium-ion battery technology, for negative material, new sodium-ion battery master
Will be using amorphous carbon, metal sulfide, tin, antimony etc..Wherein the conductive good, structure of amorphous carbon is easy to regulation and control, cost
The advantages of low, good cycling stability, but its storage sodium specific capacity is limited.Laminated metal sulfide has specific capacity higher, but
Substantially, capacity attenuation is rapid for Volume Changes in poorly conductive, and cyclic process.Xie X[Xie X,Makaryan T,Zhao M,
et al.MoS2Nanosheets Vertically Aligned on Carbon Paper:A Freestanding
Electrode for Highly Reversible Sodium‐Ion Batteries[J].Advanced Energy
Materials,2015,DOI:10.1002/aenm.201502161] molybdenum disulfide nano sheet vertical-growth is made on carbon paper
For carbon/molybdenum bisuphide composite, but because molybdenum disulfide nano sheet is not coated by carbon base body, and nanometer sheet is multilayer knot
The reasons such as structure, the specific capacity and high rate performance of material is still not ideal enough.The few layer molybdenum bisuphide structure of carbon coating can substantially suppress
Volume Changes in charge and discharge process, while carbon substrate ensure that the good electric conductivity of composite, be expected to obtain specific capacity it is high,
The anode material of lithium-ion battery of good cycling stability.
The microscopic appearance and structure of C-base composte material can influence material and electrolyte contacts area, sodium ion diffusion path
Deng finally influenceing material electrochemical performance.Nanometer box be the nanostructured assembled by two-dimensional nano piece, with electrolysis
Liquid contact area is big, the advantages of sodium ion transmission path is short, is expected to prepare high performance electrode material.Traditional carbon-based nano box with
Di-iron trioxide nano particle etc. is template, needs pickling to remove removing template after carbonization, and preparation technology is complicated and easily pollutes environment, no
Beneficial to large-scale production.
The content of the invention
In order to overcome the deficiencies in the prior art, dripped with coal it is an object of the present invention to provide a kind of sodium-ion battery negative pole
The preparation method and application of the blue or green few layer molybdenum disulfide nano box of resin base amorphous carbon cladding.Preparation method preparation process letter
Single, raw material sources enrich, and prepared composite has specific capacity high as sodium-ion battery negative pole, good rate capability with follow
The advantages of ring excellent performance.
In order to realize foregoing invention purpose, in the presence of solving the problems, such as prior art, the technical scheme that the present invention takes
It is：A kind of sodium-ion battery negative pole coal tar pitch resin base amorphous carbon coats the preparation side of few layer molybdenum disulfide nano box
Method, comprises the following steps：
Step 1, at room temperature, saturated aqueous sodium chloride is added dropwise in absolute ethyl alcohol, and dry cake is obtained after suction filtration
Sodium chloride template, the saturated aqueous sodium chloride is 1 with absolute ethyl alcohol mass ratio:5-30, filtration cakes torrefaction temperature control is in 80-
120 DEG C, drying time is controlled in 2-10h；
Step 2, coal tar pitch resin is dissolved in N-methyl pyrrolidones, adds four thio ammonium molybdate and the poly- first of pore creating material
Base methyl acrylate, is added thereto to as sodium chloride template obtained in step 1 after being completely dissolved, and the lower solvent evaporated of stirring is described
At 150-210 DEG C, coal tar pitch resin is 1 with the mass ratio of N-methyl pyrrolidones to the control of solvent vapo(u)rizing temperature:5-50, coal tar pitch
Resin is 1 with the mass ratio of pore creating material polymethyl methacrylate:The quality of 0.1-2, coal tar pitch resin and four thio ammonium molybdate
Than being 1:0.5-5, coal tar pitch resin is 1 with the mass ratio of sodium chloride template:1-20；
Step 3, the mixture for obtaining step 2 carry out carbonization treatment under inert gas shielding, temperature with 2~10 DEG C/
Min heating rates rise to 600-900 DEG C, and constant temperature 1-3h, the inert gas is selected from the one kind in nitrogen or argon gas；
Step 4, the sample after step 3 carbonization treatment is cooled to room temperature, adopts and sodium chloride template is washed with deionized simultaneously
It is dried, at 90-120 DEG C, time control obtains target material coal tar pitch resin base amorphous carbon to temperature control in 3-10h
The few layer molybdenum disulfide nano box of cladding.
The preparation method, prepares the few layer molybdenum disulfide nano box of coal tar pitch resin base amorphous carbon cladding in sodium ion
Application in battery.
Present invention has the advantages that：A kind of sodium-ion battery negative pole coal tar pitch resin base amorphous carbon coats few sulphur of layer two
Change the preparation method and application of molybdenum nanometer box, wherein, preparation method is comprised the following steps：(1) at room temperature, by sodium chloride saturation
The aqueous solution is added dropwise in absolute ethyl alcohol, and dry cake is obtained sodium chloride template after suction filtration, and coal tar pitch resin is dissolved in nitrogen by (2)
In methyl pyrrolidone, four thio ammonium molybdate and pore creating material polymethyl methacrylate are added, be added thereto to after being completely dissolved
As sodium chloride template obtained in step 1, the lower solvent evaporated of stirring, the mixture that (3) obtain step 2 is under inert gas shielding
Carbonization treatment is carried out, the sample after step 3 carbonization treatment is cooled to room temperature by (4), adopt and sodium chloride template is washed with deionized
And be dried, obtain the few layer molybdenum disulfide nano box of target material coal tar pitch resin base amorphous carbon cladding.With existing skill
Art is compared, and the present invention has advantages below：One is, carbon source used in the present invention and pore creating material wide material sources, cheap；Two
It is that preparation method is simple and easy to apply, using water-soluble sodium chloride template, environmental protection；Three are, sodium chloride template and N-methyl pyrroles
Alkanone solvent can be recycled, and production cost is relatively low, it is easy to accomplish large-scale production；Four are, molybdenum bisuphide is with few layer of dispersion
In carbon substrate, be conducive to fully suppressing Volume Changes in charge and discharge process；Five are, the present invention prepare coal tar pitch resin base without
The few layer molybdenum disulfide nano box of setting carbon coating shows reversible storage sodium capacity higher as anode material of lithium-ion battery,
Preferable high rate performance and excellent cycle performance.
Brief description of the drawings
Fig. 1 is the few layer molybdenum disulfide nano box of coal tar pitch resin base amorphous carbon cladding prepared by the embodiment of the present invention 1
Stereoscan photograph figure.
Fig. 2 is the few layer molybdenum disulfide nano box of coal tar pitch resin base amorphous carbon cladding prepared by the embodiment of the present invention 1
Transmission electron microscope photo figure.
Fig. 3 is the few layer molybdenum disulfide nano box of coal tar pitch resin base amorphous carbon cladding prepared by the embodiment of the present invention 1
X ray diffracting spectrum.
Fig. 4 is the few layer molybdenum disulfide nano box of coal tar pitch resin base amorphous carbon cladding prepared by the embodiment of the present invention 1
Charge-discharge performance curve map under different current densities in sodium ion half-cell.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
At room temperature, 100g saturated aqueous sodium chlorides are added dropwise in 500g absolute ethyl alcohols, suction filtration and by filter cake 100
DEG C dry 2h and sodium chloride template is obtained；2g coal tar pitch resins are dissolved in 60g N-methyl pyrrolidones, 3g tetra- is added thereto to
Ammonium thiomolybdate, 1g pore creating material polymethyl methacrylates, add 20g sodium chloride templates after being completely dissolved, stirred in 205 DEG C of oil baths
Mix heating and be evaporated N-methyl pyrrolidones；The mixture carbonization that will be obtained, is warming up under argon gas protection in tube furnace with 5 DEG C/min
700 DEG C, constant temperature 2h is taken out after being cooled to room temperature, then sodium chloride template is washed with deionized, and 8h is dried at 90 DEG C, and mesh is obtained
The few layer molybdenum disulfide nano box of mark material coal tar pitch resin base amorphous carbon cladding.Its stereoscan photograph figure as shown in figure 1,
Transmission electron microscope photo figure is as shown in Fig. 2 X ray diffracting spectrum is as shown in Figure 3.By target material and acetylene black, PVDF (poly- inclined two
PVF) according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, and sodium-ion battery is assembled in glove box.
Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage scope is 0.01-3V, measures this
Material is in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 552.9mAh g-1, its charge-discharge performance curve map such as Fig. 4
It is shown.
Embodiment 2
At room temperature, 150g saturated aqueous sodium chlorides are added dropwise in 1000g absolute ethyl alcohols, suction filtration simultaneously exists filter cake
100 DEG C dry 2h and sodium chloride template are obtained；2g coal tar pitch resins are dissolved in 40g N-methyl pyrrolidones, are added thereto to
3g four thio ammonium molybdates, 2g pore creating material polymethyl methacrylates, add 20g sodium chloride templates, 200 DEG C of oil baths after being completely dissolved
Middle agitating heating is evaporated N-methyl pyrrolidones；The mixture carbonization that will be obtained, with 5 DEG C/min liters under argon gas protection in tube furnace
To 800 DEG C, constant temperature 1h is taken out temperature after being cooled to room temperature, then sodium chloride template is washed with deionized, and 10h is dried at 90 DEG C, is made
Obtain the few layer molybdenum disulfide nano box of target material coal tar pitch resin base amorphous carbon cladding.By target material and acetylene black,
PVDF (polyvinylidene fluoride) is according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, in glove box assemble sodium from
Sub- battery.Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage scope is 0.01-
3V, measures the material in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 514.3mAh g-1。
Embodiment 3
At room temperature, 130g saturated aqueous sodium chlorides are added dropwise in 700g absolute ethyl alcohols, suction filtration and by filter cake 80
DEG C dry 10h and sodium chloride template is obtained；2g coal tar pitch resins are dissolved in 80g N-methyl pyrrolidones, 2g is added thereto to
Four thio ammonium molybdate, 1g pore creating material polymethyl methacrylates, add 20g sodium chloride templates, in 200 DEG C of oil baths after being completely dissolved
Agitating heating is evaporated N-methyl pyrrolidones；The mixture carbonization that will be obtained, is heated up under argon gas protection in tube furnace with 5 DEG C/min
To 700 DEG C, constant temperature 2h is taken out after being cooled to room temperature, then sodium chloride template is washed with deionized, and 8h is dried at 90 DEG C, is obtained
The few layer molybdenum disulfide nano box of target material coal tar pitch resin base amorphous carbon cladding.By target material and acetylene black, PVDF
(polyvinylidene fluoride) is according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, and sodium ion electricity is assembled in glove box
Pond.Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage scope is 0.01-3V,
The material is measured in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 473.1mAh g-1。
Embodiment 4
At room temperature, 90g saturated aqueous sodium chlorides are added dropwise in 500g absolute ethyl alcohols, suction filtration and by filter cake at 90 DEG C
Dry 2h and sodium chloride template is obtained；2g coal tar pitch resins are dissolved in 60g N-methyl pyrrolidones, the sulphur of 4g tetra- is added thereto to
For ammonium molybdate, 1g pore creating material polymethyl methacrylates, 20g sodium chloride templates are added after being completely dissolved, stirred in 200 DEG C of oil baths
Heating is evaporated N-methyl pyrrolidones；The mixture carbonization that will be obtained, is warming up under argon gas protection in tube furnace with 5 DEG C/min
700 DEG C, constant temperature 3h is taken out after being cooled to room temperature, then sodium chloride template is washed with deionized, and 4h is dried at 100 DEG C, and mesh is obtained
The few layer molybdenum disulfide nano box of mark material coal tar pitch resin base amorphous carbon cladding.Target material and acetylene black, PVDF is (poly-
Vinylidene fluoride) according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, and sodium-ion battery is assembled in glove box.
Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage scope is 0.01-3V, is measured
The material is in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 546.8mAh g-1。
Embodiment 5
At room temperature, 100g saturated aqueous sodium chlorides are added dropwise in 500g absolute ethyl alcohols, suction filtration and by filter cake 100
DEG C dry 5h and sodium chloride template is obtained；2g coal tar pitch resins are dissolved in 60g N-methyl pyrrolidones, 3g tetra- is added thereto to
Ammonium thiomolybdate, 2g pore creating material polymethyl methacrylates, add 20g sodium chloride templates after being completely dissolved, stirred in 205 DEG C of oil baths
Mix heating and be evaporated N-methyl pyrrolidones；The mixture carbonization that will be obtained, is warming up under argon gas protection in tube furnace with 5 DEG C/min
900 DEG C, constant temperature 1h is taken out after being cooled to room temperature, then sodium chloride template is washed with deionized, and 5h is dried at 100 DEG C, and mesh is obtained
The few layer molybdenum disulfide nano box of mark material coal tar pitch resin base amorphous carbon cladding.Target material and acetylene black, PVDF is (poly-
Vinylidene fluoride) according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, and sodium-ion battery is assembled in glove box.
Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage scope is 0.01-3V, is measured
The material is in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 533.7mAh g-1。
Embodiment 6
At room temperature, 130g saturated aqueous sodium chlorides are added dropwise in 700g absolute ethyl alcohols, suction filtration and by filter cake 90
DEG C dry 5h and sodium chloride template is obtained；2g coal tar pitch resins are dissolved in 50g N-methyl pyrrolidones, 3g tetra- is added thereto to
Ammonium thiomolybdate, 1g pore creating material polymethyl methacrylates, add 10g sodium chloride templates after being completely dissolved, stirred in 200 DEG C of oil baths
Mix heating and be evaporated N-methyl pyrrolidones；The mixture carbonization that will be obtained, is warming up under argon gas protection in tube furnace with 5 DEG C/min
800 DEG C, constant temperature 2h is taken out after being cooled to room temperature, then sodium chloride template is washed with deionized, and 10h is dried at 90 DEG C, and mesh is obtained
The few layer molybdenum disulfide nano box of mark material coal tar pitch resin base amorphous carbon cladding.Target material and acetylene black, PVDF is (poly-
Vinylidene fluoride) according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, and sodium-ion battery is assembled in glove box.
Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage scope is 0.01-3V, is measured
The material is in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 548.2mAh g-1。
Comparative example 1
At room temperature, 100g saturated aqueous sodium chlorides are added dropwise in 500g absolute ethyl alcohols, suction filtration and by filter cake 100
DEG C dry 2h and sodium chloride template is obtained；2g coal tar pitch resins are dissolved in 60g N-methyl pyrrolidones, 1g are added thereto to and are made
Hole agent polymethyl methacrylate, adds 20g sodium chloride templates after being completely dissolved, agitating heating is evaporated n-formyl sarcolysine in 200 DEG C of oil baths
Base pyrrolidones；The mixture carbonization that will be obtained, 700 DEG C are warming up in tube furnace under argon gas protection with 5 DEG C/min, constant temperature 2h,
Taken out after being cooled to room temperature, then sodium chloride template is washed with deionized, 5h is dried at 100 DEG C, composite is obtained.Will be compound
Material is with acetylene black, PVDF (polyvinylidene fluoride) according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, in hand
Sodium-ion battery is assembled in casing.Battery performance, discharge and recharge are tested on Land CT2001A type battery test systems
Voltage range is 0.01-3V, measures the material in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 276.4mAh g-1。
Comparative example 2
At room temperature, 90g saturated aqueous sodium chlorides are added dropwise in 500g absolute ethyl alcohols, suction filtration and by filter cake 100
DEG C dry 2h and sodium chloride template is obtained；2g coal tar pitch resins are dissolved in 60g N-methyl pyrrolidones, 3g tetra- is added thereto to
Ammonium thiomolybdate, adds 20g sodium chloride templates after being completely dissolved, agitating heating is evaporated N-methyl pyrrolidones in 200 DEG C of oil baths；
The mixture carbonization that will be obtained, 700 DEG C, constant temperature 2h, after being cooled to room temperature are warming up in tube furnace under argon gas protection with 5 DEG C/min
Take out, then sodium chloride template is washed with deionized, 5h is dried at 100 DEG C, composite is obtained.By composite and acetylene
Black, PVDF (polyvinylidene fluoride) is according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, is assembled in glove box
Sodium-ion battery.Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage scope is
0.01-3V, measures the material in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 432.7mAh g-1。
From comparative example 1 (being added without four thio ammonium molybdate), comparative example 2 (being added without pore creating material polymethyl methacrylate) system
The composite for obtaining finds out that test battery is electrochemical on Land CT2001A type battery test systems compared with embodiment 1 to 6
Performance is learned, charging/discharging voltage scope is 0.01-3V, measures the material in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity it is bright
Reduce aobviously.
Claims (2)
1. a kind of sodium-ion battery negative pole coal tar pitch resin base amorphous carbon coats the preparation of few layer molybdenum disulfide nano box
Method, it is characterised in that comprise the following steps：
Step 1, at room temperature, saturated aqueous sodium chloride is added dropwise in absolute ethyl alcohol, and dry cake is obtained chlorination after suction filtration
Sodium template, the saturated aqueous sodium chloride is 1 with absolute ethyl alcohol mass ratio:5-30, filtration cakes torrefaction temperature control is in 80-120
DEG C, drying time is controlled in 2-10h；
Step 2, coal tar pitch resin is dissolved in N-methyl pyrrolidones, adds four thio ammonium molybdate and the poly- methyl-prop of pore creating material
E pioic acid methyl ester, is added thereto to as sodium chloride template obtained in step 1 after being completely dissolved, stirring lower solvent evaporated, the solvent
At 150-210 DEG C, coal tar pitch resin is 1 with the mass ratio of N-methyl pyrrolidones for vapo(u)rizing temperature control:5-50, coal tar pitch resin
It is 1 with the mass ratio of pore creating material polymethyl methacrylate:0.1-2, coal tar pitch resin is with the mass ratio of four thio ammonium molybdate
1:0.5-5, coal tar pitch resin is 1 with the mass ratio of sodium chloride template:1-20；
Step 3, the mixture for obtaining step 2 carry out carbonization treatment under inert gas shielding, and temperature is with 2~10 DEG C/min liters
Warm speed rises to 600-900 DEG C, and constant temperature 1-3h, the inert gas is selected from the one kind in nitrogen or argon gas；
Step 4, the sample after step 3 carbonization treatment is cooled to room temperature, adopts and sodium chloride template is washed with deionized and carries out
Dry, at 90-120 DEG C, time control obtains target material coal tar pitch resin base amorphous carbon cladding to temperature control in 3-10h
Few layer molybdenum disulfide nano box.
2. preparation method according to claim 1, prepares the few layer molybdenum disulfide nano of coal tar pitch resin base amorphous carbon cladding
Application of the box in sodium-ion battery.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108163832A (en) * | 2017-12-08 | 2018-06-15 | 大连理工大学 | A kind of preparation method and applications of pitch base carbon nanometer sheet |
| CN110127654A (en) * | 2019-05-31 | 2019-08-16 | 天津大学 | A kind of preparation method of uniform micron pore size three-dimensional carbon network |
| CN110518228A (en) * | 2019-09-17 | 2019-11-29 | 安徽大学 | It is a kind of embed inorganic nano-particle three-dimensional grapheme carbon nano-composite material and its application |
| CN111048752A (en) * | 2019-11-25 | 2020-04-21 | 珠海冠宇电池有限公司 | Negative electrode material, preparation method thereof and sodium ion battery |
| WO2020124394A1 (en) * | 2018-12-18 | 2020-06-25 | 深圳先进技术研究院 | Transition metal chalcogenide nanosheet material, preparation method thereof, negative electrode material for battery, secondary battery and use thereof |
| CN114715936A (en) * | 2022-04-18 | 2022-07-08 | 鸡西市唯大新材料科技有限公司 | Negative electrode NaSbS of lithium or sodium ion battery2Preparation method of @ C composite material |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104681815A (en) * | 2015-02-11 | 2015-06-03 | 深圳新宙邦科技股份有限公司 | Spherical molybdenum disulfide composite material and preparation method and application thereof |
| CN104934602A (en) * | 2015-06-19 | 2015-09-23 | 上海交通大学 | Molybdenum disulfide/carbon composite material and preparation method thereof |
| CN105161692A (en) * | 2015-10-23 | 2015-12-16 | 西南大学 | Preparation method for C-MoS2 composite material and products and electrochemical application thereof |
| CN106058189A (en) * | 2016-07-19 | 2016-10-26 | 天津师范大学 | Method for synthesizing high-capacity anode material of lithium ion battery |
| CN106099109A (en) * | 2016-06-22 | 2016-11-09 | 大连理工大学 | A kind of preparation method and applications of asphaltic base hard charcoal nanometer sheet |
| CN106299304A (en) * | 2016-09-27 | 2017-01-04 | 华南理工大学 | A kind of carbon cladding molybdenum sulfide composite and preparation method and application and a kind of sodium-ion battery |
-
2017
- 2017-02-08 CN CN201710069960.7A patent/CN106876702B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104681815A (en) * | 2015-02-11 | 2015-06-03 | 深圳新宙邦科技股份有限公司 | Spherical molybdenum disulfide composite material and preparation method and application thereof |
| CN104934602A (en) * | 2015-06-19 | 2015-09-23 | 上海交通大学 | Molybdenum disulfide/carbon composite material and preparation method thereof |
| CN105161692A (en) * | 2015-10-23 | 2015-12-16 | 西南大学 | Preparation method for C-MoS2 composite material and products and electrochemical application thereof |
| CN106099109A (en) * | 2016-06-22 | 2016-11-09 | 大连理工大学 | A kind of preparation method and applications of asphaltic base hard charcoal nanometer sheet |
| CN106058189A (en) * | 2016-07-19 | 2016-10-26 | 天津师范大学 | Method for synthesizing high-capacity anode material of lithium ion battery |
| CN106299304A (en) * | 2016-09-27 | 2017-01-04 | 华南理工大学 | A kind of carbon cladding molybdenum sulfide composite and preparation method and application and a kind of sodium-ion battery |
Cited By (8)
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|---|---|---|---|---|
| CN108163832A (en) * | 2017-12-08 | 2018-06-15 | 大连理工大学 | A kind of preparation method and applications of pitch base carbon nanometer sheet |
| CN108163832B (en) * | 2017-12-08 | 2020-11-20 | 大连理工大学 | Preparation method and application of asphalt-based carbon nanosheet |
| WO2020124394A1 (en) * | 2018-12-18 | 2020-06-25 | 深圳先进技术研究院 | Transition metal chalcogenide nanosheet material, preparation method thereof, negative electrode material for battery, secondary battery and use thereof |
| CN110127654A (en) * | 2019-05-31 | 2019-08-16 | 天津大学 | A kind of preparation method of uniform micron pore size three-dimensional carbon network |
| CN110518228A (en) * | 2019-09-17 | 2019-11-29 | 安徽大学 | It is a kind of embed inorganic nano-particle three-dimensional grapheme carbon nano-composite material and its application |
| CN111048752A (en) * | 2019-11-25 | 2020-04-21 | 珠海冠宇电池有限公司 | Negative electrode material, preparation method thereof and sodium ion battery |
| CN114715936A (en) * | 2022-04-18 | 2022-07-08 | 鸡西市唯大新材料科技有限公司 | Negative electrode NaSbS of lithium or sodium ion battery2Preparation method of @ C composite material |
| CN114715936B (en) * | 2022-04-18 | 2023-10-03 | 鸡西市唯大新材料科技有限公司 | Negative electrode NaSbS of lithium or sodium ion battery 2 Preparation method of @ C composite material |
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