CN108598406A - Carbon coating MoS2The preparation method and application of/silicon composite - Google Patents
Carbon coating MoS2The preparation method and application of/silicon composite Download PDFInfo
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- 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
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- 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
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Abstract
The invention belongs to field of lithium ion battery, disclose a kind of carbon coating MoS for lithium ion battery2The preparation method of/silicon composite cathode material.This approach includes the following steps：(1) nano-silicon is added in the solution containing molybdenum source, reducing agent is added, MoS is obtained by liquid phase reduction2/ silicon composite；(2) product of step (1) is subjected to carbon coating, obtains carbon-coated MoS2/ silicon composite cathode material.There is the composite material of the present invention high electrochemical lithium storage content, excellent cycle performance to have potential application prospect in high performance lithium ion battery field.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of carbon-coated MoS2The system of/silicon composite
Preparation Method and its application in lithium ion battery.
Background technology
Currently, commercial lithium ion battery mainly uses graphite negative electrodes material, however the storage lithium gram volume of this material
It is low, cannot meet the needs of lithium ion battery with high energy density.It is urgent to develop a kind of negative material with high-energy density
In the eyebrows and eyelashes.
Molybdenum disulfide is a kind of two-dimentional transient metal sulfide having with graphite-like quasi-lamellar structure.Its interlayer mainly has
Weak van der Waals interaction has the covalent bond effect of molybdenum and sulphur atom in layer.Ontology molybdenum disulfide is received by the molybdenum disulfide of multilayer
Rice piece is constituted.The structure feature of molybdenum disulfide enables it to the material of main part as storage foreign ion and molecule, such as Li+, Mg2+,
Na+, K+Deng.Lemmon etc. reports the MoS of (DOI.10.1021/cm101254j) stripping2Nano material, lithium storage content play
Up to 1131mAh/g.
As the silicon materials of the same clan with graphite, there is high specific discharge capacity (4200mAh/g).In addition, silicon is also with low
Removal lithium embedded voltage platform (be less than 0.5V vs Li+/ Li), and it is its rich reserves, cheap, therefore be that current high-energy is close
Spend the research hot topic of negative material.However, due to the characteristic of its own, silicon materials can be along with larger body in cyclic process
Product expansion and contraction, the stress effect thus brought lead to the active material on electrode and easy to produce between active material to split
Line, active material are easily separated from collector, and it is serious to ultimately cause capacity attenuation.
Invention content
The present invention obtains MoS by being introduced into nano-silicon in the solution containing molybdenum source, using liquid phase reduction2/ silicon is compound
Material.During liquid-phase reduction, there is the MoS with graphite-like plate like structure2Be grown in nano silicon material surface, formed by
MoS2Nano-silicon (the MoS of nanometer sheet protection2/ silicon) composite material.Then it by chemical vapour deposition technique, obtains carbon-coated
MoS2/ silicon composite.Composite material obtained shows high electrochemical lithium storage content and excellent cycle performance.This method
The carbon coating MoS of preparation2/ silicon composite has potential application prospect in field of lithium ion battery.
The object of the present invention is to provide a kind of high power capacity and the preparation method of the negative material with excellent cycling performance, tool
Preparation process is as follows：
(1) nano-silicon is added in the aqueous solution containing molybdenum source, reducing agent is added, MoS is obtained by Liquid reduction reaction process2/
Silicon composite；
(2) carbon coating is carried out to the composite material obtained by step (1), obtains carbon-coated MoS2/ silicon composite.
Further, the molybdenum source described in step (1) is sodium molybdate, ammonium thiomolybdate, phosphomolybdic acid, molybdenum pentachloride, three oxidations
One or more of molybdenum.
Further, the grain size of the nano-silicon described in step (1) is 50-100nm.If the grain size of silicon is too small, i.e. silicon
Specific surface area is too big, then will increase the contact area of electrolyte and material, in charge and discharge process side reaction increase, reduce battery
Coulombic efficiency for the first time；If the grain size of silicon is too big, although can reduce the contact area of electrolyte and material, lithium ion exists
The path migrated in particle increases, and causes lithium ion diffusion rate relatively slow, is unfavorable for the performance of capacity, therefore, the present invention
Select the grain size of nano-silicon for 50-100nm.
Further, the molar ratio of the nano-silicon described in step (1) and molybdenum source is 0.01-1:1.
Further, the reducing agent described in step (1) is hydrazine hydrate, thiocarbamide, L-cysteine, thioacetamide, hydrochloric acid
The molar ratio of one or more of azanol, reducing agent and molybdenum source is 3:1-6:1.
Further, the Liquid reduction reaction process temperature described in step (1) is 60-120 DEG C, reaction time 3-15h.
Further, the carbon coating process described in step (2) is one kind in liquid phase coating, chemical vapor deposition cladding,
Preferably chemical vapor deposition coats, and the carbon source used in vapor deposition processes is acetylene gas/nitrogen, acetylene gas/argon gas or acetylene
One or more in gas/helium, temperature of plate are 400-1000 DEG C, and the cladding time is 1-12h.
Chemical vapor deposition coating equipment is relatively easy, and process is few, and carbon structure is controllable, and covered effect is uniform.
Using the preparation process provides a kind of carbon coating MoS2/ silicon composite, carbon coating MoS obtained2/ silicon
Composite material is used as the negative electrode active material of lithium ion battery.
Beneficial effects of the present invention are as follows：
(a) raw material that the present invention uses is simple and easy to get, and preparation method is simple, low for equipment requirements, using chemical vapor deposition
Area method has obtained uniform cladding carbon-coating；
(b) present invention forms MoS during liquid-phase reduction in nanometer silicon face2The protective layer of nanometer sheet composition, then
Using chemical vapor deposition method in MoS2/ silicon composite surface coats amorphous carbon layer, and covered effect is uniform.Amorphous carbon
Layer can not only improve MoS2The electric conductivity of/silicon composite, moreover it is possible to as protection medium, further buffer nano Si material and fill
Volumetric expansion in discharge process.The carbon coating MoS being prepared2/ silicon composite combines MoS2, silicon and amorphous
The advantages of carbon, shows high power capacity and excellent cycle performance.
Description of the drawings
Fig. 1 is protected using circulation volume when composite material is as lithium ion battery negative pole active materials made from embodiment 5
Holdup and cycle-index relational graph.
Specific implementation mode
To make those skilled in the art more fully understand technical scheme of the present invention, With reference to embodiment to this
Invention is described in further detail.
Embodiment 1
12g sodium molybdates are dissolved under conditions of ultrasonic agitation in 120ml deionized waters, 0.7g grain sizes are then slowly added into
For the nano-silicon of 100nm, continuously adds 24.2g biomolecule L-cysteines and shift acquired solution after it is completely dissolved
Into the round-bottomed flask of 250ml, under stirring conditions in 80 DEG C of back flow reaction 12h.The product for collecting gained, after vacuum drying
Obtain MoS2/ silicon composite.The MoS that will be obtained2/ silicon composite is put in tube furnace, is passed through nitrogen as protectiveness gas
Body, gas flow rate is 200 ml/mins, and after being warming up to 800 DEG C, it is 1 to be passed through volume ratio:10 acetylene/nitrogen mixed gas is made
For carbon-coated carbon source, flow control is 50 ml/mins, and the control cladding time is 6h at 800 DEG C.After deposition, obtain
To carbon-coated MoS2/ silicon composite.
Embodiment 2
12g sodium molybdates are dissolved under conditions of ultrasonic agitation in 120ml deionized waters, are then slowly added into 0.84g
Diameter is the nano-silicon of 80nm, continuously adds 15g thioacetamides, after it is completely dissolved, acquired solution is transferred to 250ml's
In round-bottomed flask, under stirring conditions in 80 DEG C of back flow reaction 12h.The product for collecting gained, MoS is obtained after vacuum drying2/
Silicon composite.The MoS that will be obtained2/ silicon composite is put in tube furnace, is passed through nitrogen as protective gas, gas stream
Speed is 200 ml/mins, and after being warming up to 800 DEG C, it is 1 to be passed through volume ratio:10 acetylene/nitrogen mixed gas is as carbon coating
Carbon source, flow control be 50 ml/mins, at 800 DEG C control cladding the time be 6h.After deposition, carbon coating is obtained
MoS2/ silicon composite.
Embodiment 3
13g ammonium thiomolybdates are dissolved under conditions of ultrasonic agitation in 120ml deionized waters, are then slowly added into
1.12g grain sizes are the nano-silicon of 80nm, continuously add 10g hydrazine hydrates, acquired solution is transferred in the round-bottomed flask of 250ml,
Under stirring conditions in 80 DEG C of back flow reaction 8h.The product for collecting gained, MoS is obtained after vacuum drying2/ silicon composite.
The MoS that will be obtained2/ silicon composite is put in tube furnace, is passed through nitrogen as protective gas, and gas flow rate is 200 milliliters/
Minute, after being warming up to 700 DEG C, it is 1 to be passed through volume ratio:10 acetylene/nitrogen mixed gas is as carbon-coated carbon source, flow control
50 ml/mins are made as, the control cladding time 9h at 700 DEG C.After deposition, carbon-coated MoS is obtained2/ silicon composite wood
Material.
Embodiment 4
7.2g molybdenum trioxides are dissolved under conditions of ultrasonic agitation in 120ml deionized waters, 1.4g is then slowly added into
Grain size is the nano-silicon of 60nm, continuously adds 15.2g thiocarbamides, acquired solution is transferred in the round-bottomed flask of 250ml, stirring
Under conditions of in 100 DEG C of back flow reaction 10h.The product for collecting gained, MoS is obtained after vacuum drying2/ silicon composite.Will
The MoS arrived2/ silicon composite is put in tube furnace, is passed through nitrogen as protective gas, gas flow rate is 200 ml/mins
Clock, after being warming up to 900 DEG C, it is 1 to be passed through volume ratio:10 acetylene/nitrogen mixed gas is as carbon-coated carbon source, flow control
For 50 ml/mins, the control cladding time 4h at 900 DEG C.After deposition, carbon-coated MoS is obtained2/ silicon composite.
Embodiment 5
12g sodium molybdates are dissolved under conditions of ultrasonic agitation in 120ml deionized waters, 1.4g grain sizes are then slowly added into
For the nano-silicon of 100nm, 15.2g thiocarbamides are continuously added, acquired solution is transferred in the round-bottomed flask of 250ml, in stirring
Under the conditions of in 90 DEG C of back flow reaction 8h.The product for collecting gained, MoS is obtained after vacuum drying2/ silicon composite.By what is obtained
MoS2/ silicon composite is put in tube furnace, is passed through nitrogen as protective gas, gas flow rate is 200 ml/mins, is risen
Temperature is 1 to volume ratio after 800 DEG C, is passed through:10 acetylene/nitrogen mixed gas is as carbon-coated carbon source, flow control 50
Ml/min, the control cladding time 8h at 800 DEG C.After deposition, carbon-coated MoS is obtained2/ silicon composite.
Fig. 1 is protected using circulation volume when composite material is as lithium ion battery negative pole active materials made from embodiment 5
Holdup and cycle-index relational graph.The data of Fig. 1 show using negative material made from embodiment 5 as negative electrode of lithium ion battery and live
Property substance when good cycling stability, 100 times cycle after capacity retention ratio still be up to 91.8%.Excellent stability is attributed to Si
Material surface forms MoS2The protective layer of nanometer sheet composition and the agraphitic carbon of cladding, have effectively buffered silicon materials in charge and discharge
The Volumetric expansion generated in the process improves the cyclical stability of battery.
Embodiment 6
13g ammonium thiomolybdates are dissolved under conditions of ultrasonic agitation in 120ml deionized waters, are then slowly added into
1.12g grain sizes are the nano-silicon of 80nm, continuously add 13.9g thiocarbamides, acquired solution is transferred in the round-bottomed flask of 250ml,
Under stirring conditions in 80 DEG C of back flow reaction 8h.The product for collecting gained, MoS is obtained after vacuum drying2/ silicon composite.
The MoS that will be obtained2/ silicon composite is put in tube furnace, is passed through nitrogen as protective gas, and gas flow rate is 200 milliliters/
Minute, after being warming up to 800 DEG C, it is 1 to be passed through volume ratio:10 acetylene/nitrogen mixed gas is as carbon-coated carbon source, flow control
It is made as 50 milliliters/min, the control cladding time 6h at 800 DEG C.After deposition, carbon-coated MoS is obtained2/ silicon composite wood
Material.
Comparative example 1
12g sodium molybdates are dissolved under conditions of ultrasonic agitation in 120ml deionized waters, 0.7g grain sizes are then slowly added into
For the nano-silicon of 100nm, continuously adds 24.2g biomolecule L-cysteines and shift acquired solution after it is completely dissolved
Into the round-bottomed flask of 250ml, under stirring conditions in 80 DEG C of back flow reaction 12h.The product for collecting gained, after vacuum drying
Obtain MoS2/ silicon composite.
Comparative example 2
13g ammonium thiomolybdates are dissolved under conditions of ultrasonic agitation in 120ml deionized waters, then proceed to that 10g is added
Acquired solution is transferred in the round-bottomed flask of 250ml by hydrazine hydrate, under stirring conditions in 80 DEG C of back flow reaction 8h.It collects
The product of gained obtains a nanometer MoS after vacuum drying2Material.The nanometer MoS that will be obtained2Material is put in tube furnace, is passed through nitrogen
For gas as protective gas, gas flow rate is 200 ml/mins, and after being warming up to 700 DEG C, it is 1 to be passed through volume ratio:10 acetylene/
Nitrogen mixed gas is 50 ml/mins as carbon-coated carbon source, flow control, the control cladding time 9h at 700 DEG C.It is heavy
After product, carbon-coated nanometer MoS is obtained2Material.
Comparative example 3
13g ammonium thiomolybdates are dissolved under conditions of ultrasonic agitation in 120ml absolute ethyl alcohols, are then slowly added into
1.12g grain sizes are the nano-silicon of 80nm, continuously add 13.9g thiocarbamides, dry under room temperature until solution volatilizees completely.Collect institute
The product obtained, is put in tube furnace, is passed through nitrogen as protective gas, gas flow rate is 200 ml/mins, is warming up to 800
After DEG C, it is 1 to be passed through volume ratio:10 acetylene/nitrogen mixed gas as carbon-coated carbon source, flow control is 50 milliliters/
Min, the control cladding time 6h at 800 DEG C.It is combined by thermal reduction and chemical deposition and obtains carbon-coated MoS2/ silicon composite wood
Material.
It is prepared by negative plate：Slurry is prepared by stirring, then automatic film applicator is used to be coated on copper foil, is done at 80 DEG C
It is dry to form.Slurry solvent is deionized water, and conductive agent is acetylene black, and binder is sodium carboxymethylcellulose, prepared by the present invention
Composite negative pole material is 8 as the weight ratio control of active material, conductive agent, binder:1:1, copper thickness is 10 μm.Drying
Pole piece first through twin rollers (pressure 15MPa) roll-in, then cut into the sequin of a diameter of 16mm.
Button cell assembles：Using metal lithium sheet as cathode, electrolyte is the EC/DMC (v/v=1/ of the LiPF6 containing 1.0M
1) electrolyte, diaphragm use polyethylene diagrams, by anode cover, positive plate, diaphragm, lithium piece, nickel foam, stainless steel in glove box
Gasket, negative plate sequence be assembled into button cell.
Battery testing：Using the chemical property of Wuhan indigo plant electrical testing system thinking button cell, charge-discharge magnification is
0.1C, charge voltage range 5mV-3.0V.The button prepared as negative material by the composite material of each embodiment and comparative example
The charge-discharge performance of formula battery the results are shown in Table 1.
Table 1, embodiment and comparative example buckle electrical test results compared with
1 data result of table shows：The carbon-coated MoS prepared using the method for the present invention2/ silicon composite is due in nanometer
Silicon face forms MoS2The protective layer of nanometer sheet composition, then uses chemical vapor deposition method in MoS2/ silicon composite surface
Amorphous carbon layer is coated, MoS can not only be improved2The electric conductivity of/silicon composite, moreover it is possible to as protection medium, further buffer
Volumetric expansion of the nano Si material in charge and discharge process.Pass through carbon coating compared to comparative example, without adding
The composite material for entering silicon materials and thermal reduction and chemical vapor deposition being combined to be prepared, the carbon packet that embodiment is prepared
Cover MoS2/ silicon composite combines MoS2, silicon and the advantages of amorphous carbon, show high power capacity, high coulombic efficiency for the first time and excellent
Different cycle performance.The liquid phase reduction reaction condition that the present invention uses is mild, simple for process, and preparing on a large scale, silicon substrate is compound
Material Field has potential application prospect.
Claims (9)
1. a kind of carbon coating MoS2The preparation method of/silicon composite, it is characterised in that：The preparation method comprises the following steps：
(1) nano-silicon is added in the aqueous solution containing molybdenum source, adds reducing agent, MoS is obtained by Liquid reduction reaction process2/ silicon is multiple
Condensation material；
(2) carbon coating is carried out to the composite material obtained by step (1), obtains carbon-coated MoS2/ silicon composite.
2. carbon coating MoS as described in claim 12The preparation method of/silicon composite, it is characterised in that：Step (1) is described
Molybdenum source be sodium molybdate, ammonium thiomolybdate, phosphomolybdic acid, molybdenum pentachloride, one or more of molybdenum trioxide.
3. carbon coating MoS as described in claim 12The preparation method of/silicon composite, it is characterised in that：Step (1) is described
Nano-silicon grain size be 50-100nm.
4. carbon coating MoS as described in claim 12The preparation method of/silicon composite, it is characterised in that：Step (1) is described
Nano-silicon and molybdenum source molar ratio be 0.1-1：1.
5. carbon coating MoS as described in claim 12The preparation method of/silicon composite, it is characterised in that：Step (1) is described
Reducing agent be one or more of hydrazine hydrate, thiocarbamide, L-cysteine, thioacetamide or hydroxylamine hydrochloride, reducing agent with
The molar ratio of molybdenum source is 3:1-6：1.
6. carbon coating MoS as described in claim 12The preparation method of/silicon composite, it is characterised in that：Step (1) is described
Liquid reduction reaction process temperature be 60-120 DEG C, reaction time 3-15h.
7. carbon coating MoS as described in claim 12The preparation method of/silicon composite, it is characterised in that：Step (2) is described
Carbon coating process be liquid phase coating, chemical vapor deposition coat one or more of.
8. carbon coating MoS as described in claim 12The preparation method of/silicon composite, it is characterised in that：The carbon coating
Process coats for chemical vapor deposition, wherein the carbon source used in vapor deposition cladding process is acetylene gas/nitrogen, acetylene gas/argon
One kind in gas or acetylene gas/helium, temperature of plate are 400-1000 DEG C, and the cladding time is 1-12h.
9. a kind of carbon coating MoS prepared such as any one of claim 1-7 the methods2The application of/silicon composite, feature
It is：The composite material is used as the negative electrode active material of lithium ion battery.
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Cited By (6)
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| CN110061206A (en) * | 2019-03-28 | 2019-07-26 | 华南师范大学 | A kind of SiO based nano composite material, cathode and preparation method thereof |
| CN111422906A (en) * | 2020-02-29 | 2020-07-17 | 合肥国轩高科动力能源有限公司 | Preparation method of silylene and molybdenum disulfide lithium battery cathode composite material |
| CN113629230A (en) * | 2021-08-05 | 2021-11-09 | 合肥国轩电池材料有限公司 | Lithium ion battery cathode material and preparation method thereof |
| CN116072879A (en) * | 2023-04-07 | 2023-05-05 | 河南工学院 | Electrode material of lithium ion battery and preparation method thereof |
| CN116253360A (en) * | 2023-03-16 | 2023-06-13 | 青岛新泰和纳米科技有限公司 | Molybdenum sulfide doped amorphous carbon coated silicon-based composite material and preparation method thereof |
| WO2024074353A1 (en) * | 2022-10-03 | 2024-04-11 | Northvolt Ab | A silicon-based particulate material for use in an anode active material for a lithium-ion battery cell |
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| CN111422906A (en) * | 2020-02-29 | 2020-07-17 | 合肥国轩高科动力能源有限公司 | Preparation method of silylene and molybdenum disulfide lithium battery cathode composite material |
| CN113629230A (en) * | 2021-08-05 | 2021-11-09 | 合肥国轩电池材料有限公司 | Lithium ion battery cathode material and preparation method thereof |
| CN113629230B (en) * | 2021-08-05 | 2022-12-27 | 合肥国轩电池材料有限公司 | Lithium ion battery cathode material and preparation method thereof |
| WO2024074353A1 (en) * | 2022-10-03 | 2024-04-11 | Northvolt Ab | A silicon-based particulate material for use in an anode active material for a lithium-ion battery cell |
| CN116253360A (en) * | 2023-03-16 | 2023-06-13 | 青岛新泰和纳米科技有限公司 | Molybdenum sulfide doped amorphous carbon coated silicon-based composite material and preparation method thereof |
| CN116072879A (en) * | 2023-04-07 | 2023-05-05 | 河南工学院 | Electrode material of lithium ion battery and preparation method thereof |
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