CN107069035A - A kind of preparation method of molybdenum disulfide/carbosphere lithium ion battery negative material - Google Patents
A kind of preparation method of molybdenum disulfide/carbosphere lithium ion battery negative material Download PDFInfo
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- CN107069035A CN107069035A CN201710208739.5A CN201710208739A CN107069035A CN 107069035 A CN107069035 A CN 107069035A CN 201710208739 A CN201710208739 A CN 201710208739A CN 107069035 A CN107069035 A CN 107069035A
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- lithium ion
- carbosphere
- molybdenum disulfide
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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
- H01M4/58—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
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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
- 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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of preparation method of molybdenum disulfide/carbosphere lithium ion battery negative material, is related to battery material technical field.Preparation method of the present invention is：Polystyrene microsphere, two molybdic acid hydrate sodium, thiocarbamide and glucose are dissolved in deionized water, mixed solution is obtained, mixed solution is placed in reactor, 8 24 hours are incubated at 180 230 DEG C, cooling, centrifuge washing, drying, sintering are carried out by reacted mixed solution, you can.The preparation method that the present invention is provided is simple, it is easy to industrialized production, and molybdenum disulfide/carbosphere can be uniformly distributed in the molybdenum disulfide prepared/carbosphere lithium ion battery negative material, with excellent chemical property.
Description
Technical field
The present invention relates to battery material technical field, it is related to a kind of molybdenum disulfide/carbosphere lithium ion battery negative material
Preparation method Preparation Method.
Background technology
Lithium ion battery is gradually applied to electric automobile and energy storage device, however, the theoretical capacity of business graphite is only
There is 372mAhg-1, seriously limit its application in terms of electric automobile and energy storage device.Have the two of similar structures with graphite
Molybdenum sulfide nanometer sheet, due to being subjected to extensive concern, theoretical capacity in lithium ion battery with higher theoretical capacity
Height, substantial amounts of lithium ion can be stored mainly due in the lamella of two dimension.But its poorly conductive and in electrochemical process
The shortcomings of middle Volume Changes are big, causes poor as the cycle performance and high rate performance of electrode material.
The material of Nano grade has the new physical phenomenons such as quantum size effect, small-size effect, surface quantum effect,
The pattern and structure on performance of material have large effect.As having the zero-dimension structural accumulated compared with small specific surface with good thermal stability
(such as nanosphere, nano dot) material, can be used for the micron devices of one-dimentional structure (such as nanotube, nano wire) material prepared；
Two-dimensional structure (such as nanometer sheet) material with big exposure crystal face and special high preferred orientation, can be instructed by mould material
Synthesis or the three-dimensional structure material for the self assembly preparation for passing through low-dimensional materials.But for two-dimensional structure, research finds its tool
There are the structure and surface features of uniqueness, there is potential application value in terms of catalysis and the energy.Pattern and structure are to electrode
The Electrochemical Performances of material are very big, because active material and electrolyte solution have good contact and sufficiently large contact surface
Product, it is ensured that insertion abjection of the lithium ion between electrolyte solution and active material smoothly and can be rapidly performed by, from
And improve the fast charging and discharging performance of battery.
In recent years, research of the metal oxide/sulfide of central hole structure in terms of functional material causes people very
Big interest.Particularly, the shell of intact inner space and functionalization imparts the ability that there is energy to convert and store for they.
In the prior art, the chemical preparation of the metal oxide/sulfide material of pore structure mainly uses template and nothing
Template is carried out, and still, template is expensive, and process is complicated and yields poorly, it is difficult to industrialized production, and template-free method is to anti-
The condition answered is more harsh and material structure morphology controllable is poor.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of system of molybdenum disulfide/carbosphere lithium ion battery negative material
Preparation Method Preparation Method, solves technical problem of the prior art.
To realize object above, the present invention is achieved by the following technical programs：
A kind of preparation method of molybdenum disulfide/carbosphere lithium ion battery negative material, comprises the following steps：
S1, polystyrene microsphere, two molybdic acid hydrate sodium, thiocarbamide and glucose is dissolved in deionized water, obtains mixing molten
Liquid；
S2, mixed solution made from step S1 inserted into reactor, reacted 8-24 hours at 180-230 DEG C, natural cooling
To room temperature, reacted mixed solution is subjected to centrifuge washing, drying obtains powder thing；
S3, powder thing made from step S2 sintered under an inert atmosphere, you can.
It is preferred that, quality-volumetric concentration that the polystyrene microsphere accounts for the mixed solution is 1-100mg/mL；It is described
The molar concentration that two molybdic acid hydrate sodium, thiocarbamide and glucose account for the mixed solution respectively is 5-100mmol/L, 20-
200mmol/L and 5-100mmol/L.
It is preferred that, a diameter of 200-1000nm of the polystyrene microsphere.
It is preferred that, mixed solution is inserted reactor by the step S2, is reacted 10-24 hours at 200-220 DEG C.
It is preferred that, the heating schedule sintered described in step S3 is：With 2-10 DEG C/min of heating rate, 100-300 is warming up to
DEG C, soaking time 1-5 hours, then it is warming up to 700-1000 DEG C, soaking time 1-10 hours.
It is preferred that, the inert atmosphere is at least one of nitrogen, helium, argon gas.
The present invention provides a kind of preparation method Preparation Method of molybdenum disulfide/carbosphere lithium ion battery negative material, with showing
There is technology to be compared to advantage：
Preparation method of the present invention is simple, it is easy to industrialized production, prepared that molybdenum disulfide/carbosphere lithium ion battery is born
Molybdenum disulfide/carbosphere can be uniformly distributed in the material of pole, and external diameter reaches 220nm-1200nm, and wall thickness is 10nm-1000nm, this
Invention molybdenum disulfide/carbosphere lithium ion battery negative material is prepared into lithium ion half-cell, electric performance test with excellent
Chemical property and cycle performance；
Molybdenum disulfide prepared by the present invention/carbosphere lithium ion battery negative material cost is low, and process simple condition is gentle,
Material structure morphology controllable system, and yield is high, can realize industrialized production.
Brief description of the drawings
The SEM figures of Fig. 1 molybdenum disulfide of the present invention/carbosphere lithium ion battery negative material.
Fig. 2 schemes for the TEM of molybdenum disulfide of the present invention/carbosphere lithium ion battery negative material.
Fig. 3 is the XRD of molybdenum disulfide of the present invention/carbosphere lithium ion battery negative material.
Fig. 4 is CV figure of the molybdenum disulfide of the present invention/carbosphere lithium ion battery negative material in lithium ion half-cell.
Fig. 5 is molybdenum disulfide of the present invention/cyclicity of the carbosphere lithium ion battery negative material in lithium ion half-cell
Can figure.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, with reference to embodiment to the present invention
Technical scheme in embodiment is clearly and completely described, it is clear that described embodiment is that a part of the invention is implemented
Example, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creativeness
The every other embodiment obtained under the premise of work, belongs to the scope of protection of the invention.
In embodiment, filled in the battery constant current prepared by 2 molybdenum disulfide of embodiment/carbosphere lithium ion battery negative material
In discharge measuring, the preparation method of electrode is：By electrode material, Ketjen black, and polyvinylidene fluoride according to mass ratio 80：
10：10 in 1-METHYLPYRROLIDONE mixed pulp, and slurry is coated on copper foil, is dried, preparation work electrode of cutting into slices.It is multiple
Composite electrode material surface density is 1mgcm-2.Method of testing：Lithium piece is used as reference electrode, electrolyte selection 1M in lithium ion half-cell
Ethylene carbonate/dimethyl carbonate (mass ratio 1 of lithium hexafluoro phosphate:1) mixed liquor；Battery charging and discharging is tested in Arbin BT-1
Carried out on battery test system, voltage range selection 0-3V (vs Li+/ Li), charge-discharge magnification according to nano composite material matter
Amount is calculated.
Embodiment 1：
The preparation method of the present embodiment molybdenum disulfide/carbosphere lithium ion battery negative material is：By 0.1g polystyrene
Microballoon, the molybdic acid hydrate sodium of 0.1g bis-, 0.14g thiocarbamides and 0.05g glucose are dissolved in 40mL deionized waters, obtain mixed solution
(wherein, quality-volumetric concentration of polystyrene microsphere is 2.5mg/mL, two molybdic acid hydrate sodium, thiocarbamide and glucose it is mole dense
Degree is respectively 10.33mmol/L, 45.98mmol/L and 6.95mmol/L), mixed solution is inserted into 50mL reactors, at 200 DEG C
Lower reaction 10 hours, naturally cools to room temperature, and reacted solution carries out centrifuge washing, and drying obtains the powder of black.
Obtained black powder carries out heating sintering in a nitrogen atmosphere, and heating rate is 2 DEG C/min, is first warming up to 200
DEG C, 2 hours are incubated, then it is warming up to 700 DEG C, 2 hours are incubated, molybdenum disulfide/carbosphere lithium ion battery negative material is obtained.
300nm is respectively adopted in the diameter of polystyrene microsphere, and 500nm, 1000nm is tested.It is respectively 1Ag in electric current-1
Discharge capacity and first efficiency are determined during electric discharge, when circulating 500 circle, discharge capacity is determined again, it is shown that good circulation
Performance.The performance parameter of the molybdenum disulfide prepared/carbosphere lithium ion battery negative material is as shown in table 1.
The performance parameter of the lithium ion battery negative material of table 1
As can be seen from the table, when the diameter of polystyrene microsphere uses 500nm, the electric discharge of the negative material prepared
Performance is better than the diameter of other polystyrene microspheres.
Embodiment 2：
By 0.1g polystyrene microspheres (diameter 500nm), the molybdic acid hydrate sodium of 0.1g bis-, 0.14g thiocarbamides and 0.1g glucose
40mL deionized waters are dissolved in, obtaining mixed solution, (wherein, quality-volumetric concentration of polystyrene microsphere is 2.5mg/mL, two
The molar concentration of molybdic acid hydrate sodium, thiocarbamide and glucose is respectively 10.33mmol/L, 45.98mmol/L and 13.89mmol/L),
Mixed solution is inserted into 50mL reactors, reacted 12 hours at 200 DEG C, room temperature is naturally cooled to, reacted solution is carried out
Centrifuge washing, drying, obtains the powder of black.
Obtained black powder carries out heating sintering in a nitrogen atmosphere, and heating rate is 2 DEG C/min, is first warming up to 200
DEG C, 2 hours are incubated, then be warming up to 800 DEG C, insulation 2 hours；
Molybdenum disulfide prepared by embodiment 2/carbosphere lithium ion battery negative material carries out SEM, TEM, XRD and characterized,
And the CV of the lithium ion half-cell of molybdenum disulfide/carbosphere lithium ion battery negative material preparation is characterized, cycle performance test,
As a result see and show the negative material prepared in 1Ag in Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, figure-1Electric current under first electric discharge hold
Easily it is 743.4mAh/g, efficiency is 59.7% first, and the discharge capacity after 500 circulations is 689.7mAh/g.
Embodiment 3：
Embodiment 3 adjusts the addition of polystyrene microsphere as different from Example 2.Weigh 0.2g polystyrene microspheres
It is dissolved in 40mL deionized waters.Other steps are same as Example 2, and the negative material prepared is in 1Ag-1Electric current under first
Electric discharge is easily 705.2mAh/g, and efficiency is 55.6% first, and the discharge capacity after 500 circulations is 648.1mAh/g.
Embodiment 4：
Embodiment 4 adjusts the addition of glucose as different from Example 2.It is molten that 0.05g, 0.4g glucose are weighed respectively
Solution is in 2 parts of 40mL deionized waters.Other steps are same as Example 2, and the negative material prepared is in 1Ag-1Electric current under it is first
Secondary electric discharge is easily 695.2mAh/g, 629.5mAh/g respectively, and efficiency is 53.4%, 55.7% respectively first, and 500 circulate it
Discharge capacity afterwards is 630.4mAh/g, 587.9mAh/g respectively.
Embodiment 5：
Embodiment 5 adjusts the addition of two molybdic acid hydrate sodium as different from Example 2.It is molten that 0.05g, 0.3g are weighed respectively
Solution is in 2 parts of 40mL deionized waters.Other steps are same as Example 2, and the negative material prepared is in 1Ag-1Electric current under it is first
Secondary electric discharge is easily 655.2mAh/g, 599.8mAh/g respectively, and efficiency is 50.4%, 52.7% respectively first, and 500 circulate it
Discharge capacity afterwards is 598.4mAh/g, 534.9mAh/g respectively.
Embodiment 6：
Embodiment 6 adjusts the reaction time of mixed solution as different from Example 2.Take 2 the anti-of mixed solution is housed
Kettle is answered, is reacted 10 hours, 24 hours at 220 DEG C respectively.Other steps are same as Example 2, the negative material prepared
In 1Ag-1Electric current under to discharge first be easily 730.1mAh/g, efficiency is 58.6% first, and the electric discharge after 500 circulations is held
Amount is 675.8mAh/g.
Embodiment 7：
The preparation method of the present embodiment molybdenum disulfide/carbosphere lithium ion battery negative material, comprises the following steps：
S1, polystyrene microsphere, two molybdic acid hydrate sodium, thiocarbamide and glucose is dissolved in deionized water, obtains mixing molten
Quality-volumetric concentration that liquid, wherein polystyrene microsphere account for the mixed solution is 1mg/mL；Two molybdic acid hydrate sodium, thiocarbamide and
The molar concentration that glucose accounts for the mixed solution respectively is 5mmol/L, 200mmol/L and 100mmol/L；Polystyrene microsphere
A diameter of 200nm；
S2, mixed solution made from step S1 inserted into reactor, reacted 84 hours at 180 DEG C, naturally cool to room temperature,
Reacted mixed solution is subjected to centrifuge washing, drying obtains powder thing；
S3, by powder thing made from step S2 nitrogen, helium, argon gas mixed atmosphere be middle sintering, you can, wherein burning
The heating schedule of knot is：With 2 DEG C/min of heating rate, 100 DEG C are warming up to, soaking time 1 hour, then it is warming up to 700 DEG C, insulation
1 hour time.
Embodiment 8：
The preparation method of the present embodiment molybdenum disulfide/carbosphere lithium ion battery negative material, comprises the following steps：
S1, polystyrene microsphere, two molybdic acid hydrate sodium, thiocarbamide and glucose is dissolved in deionized water, obtains mixing molten
Quality-volumetric concentration that liquid, wherein polystyrene microsphere account for the mixed solution is 100mg/mL；Two molybdic acid hydrate sodium, thiocarbamide
The molar concentration for accounting for the mixed solution respectively with glucose is 100mmol/L, 20mmol/L and 5mmol/L；Polystyrene is micro-
A diameter of 1000nm of ball；
S2, mixed solution made from step S1 inserted into reactor, reacted 24 hours at 230 DEG C, naturally cool to room temperature,
Reacted mixed solution is subjected to centrifuge washing, drying obtains powder thing；
S3, powder thing made from step s2 sintered in a nitrogen atmosphere, you can, wherein the heating schedule sintered is：With
10 DEG C/min of heating rate, is warming up to 300 DEG C, soaking time 5 hours, then is warming up to 1000 DEG C, soaking time 10 hours.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
The present invention is described in detail, it will be understood by those within the art that：It still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic；And these modification or
Replace, the essence of appropriate technical solution is departed from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (6)
1. the preparation method of a kind of molybdenum disulfide/carbosphere lithium ion battery negative material, it is characterised in that including following step
Suddenly：
S1, polystyrene microsphere, two molybdic acid hydrate sodium, thiocarbamide and glucose is dissolved in deionized water, obtains mixed solution；
S2, mixed solution made from step S1 inserted into reactor, reacted 8-24 hours at 180-230 DEG C, naturally cool to room
Temperature, centrifuge washing is carried out by reacted mixed solution, and drying obtains powder thing；
S3, powder thing made from step S2 sintered under an inert atmosphere, you can.
2. preparation method according to claim 1, it is characterised in that：The polystyrene microsphere accounts for the mixed solution
Quality-volumetric concentration is 1-100mg/mL；The two molybdic acid hydrates sodium, thiocarbamide and glucose account for rubbing for the mixed solution respectively
Your concentration is 5-100mmol/L, 20-200mmol/L and 5-100mmol/L.
3. preparation method according to claim 1, it is characterised in that：A diameter of 200- of the polystyrene microsphere
1000nm。
4. preparation method according to claim 1, it is characterised in that：Mixed solution is inserted reactor by the step S2,
Reacted 10-24 hours at 200-220 DEG C.
5. preparation method according to claim 1, it is characterised in that：The heating schedule sintered described in step S3 is：To rise
Warm 2-10 DEG C of speed/min, is warming up to 100-300 DEG C, soaking time 1-5 hours, then is warming up to 700-1000 DEG C, soaking time
1-10 hours.
6. preparation method according to claim 1, it is characterised in that：The inert atmosphere is in nitrogen, helium, argon gas
It is at least one.
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| CN108133827A (en) * | 2017-12-14 | 2018-06-08 | 三峡大学 | A kind of preparation method of molybdenum disulfide and sulfur doping carbon ball combination electrode |
| CN108417789A (en) * | 2018-01-30 | 2018-08-17 | 合肥国轩高科动力能源有限公司 | A kind of MoS for negative electrode of lithium ion battery2/ C microballoon composite material and preparation methods |
| CN110844939A (en) * | 2019-11-12 | 2020-02-28 | 杭州电子科技大学 | Molybdenum sulfide carbon nanosphere carbon nanofiber composite electrode material and preparation method thereof |
| 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 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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Application publication date: 20170818 |