CN107342405A - A kind of MoS2‑xOx/ carbon negative pole material and preparation method thereof - Google Patents
A kind of MoS2‑xOx/ carbon negative pole material and preparation method thereof Download PDFInfo
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- CN107342405A CN107342405A CN201710448676.0A CN201710448676A CN107342405A CN 107342405 A CN107342405 A CN 107342405A CN 201710448676 A CN201710448676 A CN 201710448676A CN 107342405 A CN107342405 A CN 107342405A
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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
- H01M4/364—Composites as mixtures
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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
- H01M4/36—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
- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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 invention discloses a kind of MoS2‑xOx/ carbon negative pole material and preparation method thereof, belong to electrochemistry and new energy materialses field.Treated hygenic towelette is immersed in graphene oxide solution by the present invention, and MoS is formed with sodium molybdate, thiocarbamide mixed solution hydro-thermal, sodium molybdate and thiocarbamide after drying2, graphene oxide reduction.Resulting materials are calcined under high temperature inert atmosphere after hydro-thermal, improve MoS2Crystallinity, carbonizing degree and further redox graphene, obtain MoS2/ carbon composite.MoS2/ carbon composite is subsequently placed at low temperature calcination in oxygen, forms MoS2‑xOx/ carbon negative pole material, oxygen atom part substitution sulphur atom, causes MoS2Lattice defect, carrier concentration is improved, improve material electric conductivity.Carbon forms three-dimensional conductive network in material internal, and graphene graphene has very high electronic conductivity energy, bigger serface, physical and chemical stability, while improves material cyclical stability during removal lithium embedded.The MoS2‑xOx/ carbon negative pole material is as lithium ion battery negative material, hence it is evident that improves the reversible specific capacity of material.
Description
Technical field
The invention discloses a kind of MoS2-xOx/ carbon negative pole material and preparation method thereof, belongs to electrochemistry and new energy materialses
Field.
Background technology
It is well known that along with the consumption of fuel and the demand of mass energy, the material of pollution-free and low expense will be to future
Society there is very big value.Lithium ion battery has the features such as big energy density, long cycle life, is widely used in
Portable electric appts and electric automobile, therefore reduce the consumption to chemical dye to a certain extent.
In transition compounds of group, especially molybdenum sulfide has obtained the concern of people, because it is unique chemically and physically
Property, not only it is used only for doing lubricant, is also applied to various devices, energy reserves equipment, electronic sensor, biomedicine
Instrument, lithium ion battery and electrochemical catalyst hydrogen manufacturing etc..Molybdenum sulfide is connected by Van der Waals force between layers, has class
Graphene-structured, the specific area of layer structure is big, and interlamellar spacing is big, there is provided more avtive spots, is also beneficial to ion infiltration.Mesh
The research level of preceding pure molybdenum sulfide is ripe, however, this also the preparation to molybdenum sulfide nano material, application field propose
Higher requirement so that pure molybdenum sulfide can not be satisfied with demand now, therefore seek new carrier material or modification
The material sense of active component is great, and graphene has the features such as larger specific surface area, high electrical conductance and heat endurance, can
Significantly to improve the chemical property of material.
Foreign atom can such as change the band structure of material inside nitrogen phosphate and sulfur, boron incorporation carbon material, this explanation is adopted
With the method for low temperature calcination, oxygen atom part is substituted sulphur atom, change the band structure of material, reduce lithium ion diffusion speed
Rate, while the fault of construction of material is caused, improve the storage lithium performance of carbon material.Graphene have very high electronic conductivity energy,
Bigger serface, physical and chemical stability, the MoS that this explanation eventually forms2-xOx/ carbon negative pole material significantly improves material
Specific capacity and stable circulation performance.
The content of the invention
It is an object of the invention to provide a kind of MoS2-xOx/ carbon negative pole material and preparation method thereof.This method is by hygenic towelette
In 1 mol L-1Watery hydrochloric acid in soak 12h, be then transferred into absolute ethyl alcohol/acetone with volume ratio 1:Soaked in 1 mixed solution
6h is steeped, then cleans obtained hygenic towelette 3-5 times with absolute ethyl alcohol, deionized water, is then placed in 60 DEG C of drying boxes and dries
12h, the hygenic towelette handled well.One layer of 10ml 12mg ml are uniformly coated on the hygenic towelette surface that 0.1g is treated-1's
Graphene oxide, the hydro-thermal 24h at a temperature of 200 DEG C is placed in water heating kettle with 0.24g sodium molybdates and 0.76 thiocarbamide.Placed after drying
In tube furnace, calcine 4h for 800 DEG C under nitrogen atmosphere protection, the crystallinity and carbonizing degree of molybdenum sulfide are improved, finally in oxygen
The lower 500 DEG C of low temperature calcination 1h of atmosphere form a kind of MoS2-xOx/ carbon negative pole material, the material is with binding agent and conductive agent with 8:1:1
Ratio electrode slice is made.
The object of the present invention is achieved like this：MoS2-xOx/ carbon negative pole material and preparation method thereof, its processing step：
Moisture paper tissue papers soak 12h in 1mol/L watery hydrochloric acid, and moisture paper tissue papers then are transferred into absolute ethyl alcohol/acetone with volume ratio 1：
6h is soaked in 1 mixed solution, then obtained moisture paper tissue papers are cleaned 3-5 times with absolute ethyl alcohol, deionized water, are then placed in 60
12h, the moisture paper tissue papers handled well are dried in DEG C drying box.
Pretreated hygenic towelette is mixed with graphene oxide, dries, makes one layer of graphite oxide of hygenic towelette applied atop
Alkene, the hygenic towelette and sodium molybdate and thiocarbamide hydro-thermal reaction 1-24h, Ran Hou at 90-240 DEG C of graphene oxide will be loaded with
1-10h is calcined under nitrogen atmosphere at 500-1200 DEG C, obtains MoS2/ carbon negative pole material, it is subsequently placed in oxygen 100-600 DEG C and forges
1-5h is burnt, obtains MoS2-xOx/ carbon negative pole material.Hygenic towelette of the present invention is Victor board hygenic towelette.
A kind of MoS provided by the invention2-xOx/ carbon negative pole material, possesses following beneficial effect：
（1）Prepared MoS2-xOx/ carbon negative pole material electrode improve molybdenum sulfide in charge and discharge process Volume Changes lack
Point, so as to be favorably improved the energy of electrode material and cycle performance.
（2）MoS prepared by the method2-xOx/ carbon negative pole material can effectively improve molybdenum sulfide electric conductivity and increase vulcanization molybdenum materials
Fault of construction inside material, further improve the specific capacity of composite.
The present invention prepares MoS using a kind of straightforward procedure2-xOx/ carbon negative pole material.In water-heat process, sodium molybdate and thiocarbamide
Form MoS2, graphene oxide reduction.The finally low temperature calcination in oxygen is placed in, oxygen atom substitution part sulphur atom, is obtained
MoS2-xOx/ carbon negative pole material, modified electrode material can change the internal structure of molybdenum sulfide, improve its electric conductivity, and
Cyclical stability, excellent specific capacity and stable circulation performance are shown as lithium ion battery negative material.
Brief description of the drawings
Fig. 1 is MoS prepared by the embodiment of the present invention 11.9O0.1The X-ray diffraction of/carbon negative pole material（XRD）Collection of illustrative plates.
Fig. 2 is MoS prepared by the embodiment of the present invention 11.9O0.1The different amplification stereoscan photograph of/carbon negative pole material
(SEM)。
Fig. 3（a）（b）The MoS that respectively prepared by the embodiment of the present invention 11.9O0.1/ carbon and MoS2The 3 times charge and discharge of/carbon material
Electric curve.
Fig. 4 is MoS prepared by the embodiment of the present invention 11.9O0.1/ carbon material and MoS2/ carbon and as negative electrode of lithium ion battery
The cycle performance contrast of material.
Embodiment
With reference to instantiation, the present invention is further described.
Embodiment 1：A kind of MoS1.9O0.1/ carbon negative pole material and preparation method thereof
By hygenic towelette in 1 mol L-1Watery hydrochloric acid in soak 12h, hygenic towelette is then transferred to absolute ethyl alcohol/acetone with body
Product ratio 1:6h is soaked in 1 mixed solution, obtained hygenic towelette is then cleaned 3-5 times with absolute ethyl alcohol, deionized water, then
It is put into 60 DEG C of drying boxes and dries 12h, the hygenic towelette handled well.Take the mg mL of concentration 12-1Graphene oxide 10mL it is equal
Even is coated in 0.1g hygenic towelettes surface, dries, then itself and 0.24 g sodium molybdates and 0.76 g thiocarbamides are put into water heating kettle
200 DEG C of h of hydro-thermal 24.In water-heat process, sodium molybdate and thiocarbamide form MoS2, graphene oxide reduction.By the material in tube furnace
Middle 800 DEG C, 4h of calcining, while calcining, improve the crystallinity and carbonizing degree of material.Then by the material in oxygen
400 DEG C of low temperature calcination 1h, ultimately form MoS1.9O0.1/ carbon negative pole material.Fig. 1 is MoS1.9O0.1The XRD spectrum of/carbon.Fig. 2 is should
The SEM photograph of the different amplification of material.The MoS of lamellar structure1.9O0.1Flock together to form colored spherical structure, flower-shaped knot
Structure has relatively low impedance, largely improves its electrochemical reaction dynamics.By the material and binding agent
PVDF and conductive agent acetylene black are with 8:1:Electrode slice is made in 1 ratio, and lithium piece is that electrolyte is general lithium-ion electric to electrode
The M LiPF of pond electrolyte 16/DMC: EC=1:1,2025 type button cells are prepared, with 100 mA g-1Current density charge and discharge
Electricity.Shown in 3 times charging and discharging curve such as Fig. 3 (a) of the electrode, it can be seen that the discharge capacity first of the material is 898 mAh
g-1, reversible charging capacity is 734.6 mAh g first-1.Without the MoS by calcining in atmosphere2/ carbon discharge capacity first
For 726 mAh g-1, reversible capacity is 605 mAh g first-1.Fig. 4 is MoS1.9O0.1/ carbon and MoS2/ carbon cycle performance comparison
Figure.As can be seen from the figure MoS after 22 circulations1.9O0.1The reversible capacity of/carbon is 815 mAh g-1, and MoS2/ carbon material
Reversible capacity be 635 mAh g-1。
Embodiment 2 is a kind of MoS1.8O0.2/ carbon negative pole material and preparation method thereof II
By hygenic towelette in 1 mol L-1Watery hydrochloric acid in soak 12h, hygenic towelette is then transferred to absolute ethyl alcohol/acetone with body
Product ratio 1:6h is soaked in 1 mixed solution, obtained hygenic towelette is then cleaned 3-5 times with absolute ethyl alcohol, deionized water, then
It is put into 60 DEG C of drying boxes and dries 12h, the hygenic towelette handled well.Take the mg mL of concentration 12-1The mL of graphene oxide 10 it is equal
Even is coated in 0.1g hygenic towelettes surface, dries, then itself and 0.24g sodium molybdates and 0.76g thiocarbamides are put into 200 in water heating kettle
DEG C hydro-thermal 24h.In water-heat process, sodium molybdate and thiocarbamide form MoS2, graphene oxide reduction.The material is forged in tube furnace
800 DEG C, 4h, while calcining are burnt, the crystallinity and carbonizing degree of material are improved, then by the material 500 DEG C in oxygen
Low temperature calcination 1h, ultimately forms MoS1.8O0.2/ carbon negative pole material.The electrode material test condition as described in example 1 above, as
Lithium ion battery negative material is with 100 mA g-1Current density carries out discharge and recharge, and reversible capacity is 660 mAh g first-1, 22
Reversible capacity after secondary circulation is 750 mAh g-1。
A kind of 3 MoS of embodiment1.7O0.3/ carbon negative pole material and preparation method thereof III
By hygenic towelette in 1 mol L-1Watery hydrochloric acid in soak 12h, hygenic towelette is then transferred to absolute ethyl alcohol/acetone with body
Product ratio 1:6h is soaked in 1 mixed solution, obtained hygenic towelette is then cleaned 3-5 times with absolute ethyl alcohol, deionized water, then
It is put into 60 DEG C of drying boxes and dries 12h, the hygenic towelette handled well.Take the mg ml of concentration 12-1Graphene oxide 10ml it is equal
Even is coated in 0.1g hygenic towelettes surface, dries, then itself and 0.24g sodium molybdates and 0.76g thiocarbamides are put into 200 in water heating kettle
DEG C hydro-thermal 24h.In water-heat process, sodium molybdate and thiocarbamide form MoS2, graphene oxide reduction.The material is forged in tube furnace
800 DEG C, 4h, while calcining are burnt, the crystallinity and carbonizing degree of material are improved, then by the material 500 DEG C in oxygen
Low temperature calcination 2h, ultimately forms MoS1.7O0.3/ carbon negative pole material.The electrode material test condition as described in example 1 above, as
Lithium ion battery negative material is with 100mA g-1Current density carries out discharge and recharge, and reversible capacity is 680 mAh g first-1, 20 times
Reversible capacity after circulation is 770 mAh g-1。
Claims (5)
- A kind of 1. MoS2-xOxThe preparation method of/carbon negative pole material, it is characterised in that by pretreated hygenic towelette and graphite oxide Alkene mixes, and drying, makes one layer of graphene oxide of hygenic towelette applied atop, will be loaded with the hygenic towelette and sodium molybdate of graphene oxide With thiocarbamide at 90-240 DEG C hydro-thermal reaction 1-24h, then calcine 1-10h under nitrogen atmosphere at 500-1200 DEG C, obtain MoS2/ carbon negative pole material, 100-600 DEG C of calcining 1-5h in oxygen is subsequently placed in, obtains MoS2-xOx/ carbon negative pole material.
- 2. MoS as claimed in claim 12-xOxThe preparation method of/carbon negative pole material, it is characterised in that：Oxygen atom part substitutes Sulphur atom, x=0.1-0.4.
- 3. MoS as claimed in claim 12-xOxThe preparation method of/carbon negative pole material, it is characterised in that：Moisture paper tissue papers are in 1mol/L Watery hydrochloric acid in soak 12h, moisture paper tissue papers are then transferred to absolute ethyl alcohol/acetone with volume ratio 1：Soaked in 1 mixed solution 6h, then obtained moisture paper tissue papers are cleaned 3-5 times with absolute ethyl alcohol, deionized water, be then placed in 60 DEG C of drying boxes and dry 12h, the moisture paper tissue papers handled well.
- 4. MoS as claimed in claim 12-xOxThe preparation method of/carbon negative pole material, it is characterised in that：Graphite oxide is uniform It is supported on moisture paper tissue papers, the mass ratio of graphite oxide and moisture paper tissue papers is 1:1~5.
- 5. MoS as claimed in claim 12-xOxThe preparation method of/carbon negative pole material, it is characterised in that：Sodium molybdate and thiocarbamide Mol ratio is 1:5-20.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108538611A (en) * | 2018-02-23 | 2018-09-14 | 中国石油大学(北京) | A kind of nano-chip arrays cobalt acid nickel-carbon composite and its preparation method and application |
| CN108682834A (en) * | 2018-06-12 | 2018-10-19 | 郑州新世纪材料基因组工程研究院有限公司 | A kind of Magnesium ion battery material and preparation method thereof, Magnesium ion battery composite material and preparation method |
| CN109686954A (en) * | 2018-12-27 | 2019-04-26 | 陕西科技大学 | A kind of C-O-Mo key bridge joint monolithic taper MoS2/ NG sodium ion negative electrode material and preparation method thereof |
| CN110120507A (en) * | 2019-05-16 | 2019-08-13 | 常熟理工学院 | A kind of heterogeneous material compound and its preparation method and application that graphene is modified |
| CN110280232A (en) * | 2019-05-17 | 2019-09-27 | 华北电力大学 | A kind of preparation method of richness defect metal oxygen (sulphur) compound/graphene oxide composite material |
| CN110783542A (en) * | 2019-10-22 | 2020-02-11 | 济南大学 | Paper towel derived carbon fiber loaded MoS 2Preparation method of micro-flower composite material and application of micro-flower composite material in lithium-sulfur battery |
| CN112978800A (en) * | 2019-12-17 | 2021-06-18 | 山东海科创新研究院有限公司 | High-conductivity molybdenum disulfide material and preparation method and application thereof |
| CN113713833A (en) * | 2021-09-15 | 2021-11-30 | 北京师范大学 | Molybdenum oxysulfide/nickel sulfide/foamed nickel complex and preparation method and application thereof |
| CN114380326A (en) * | 2022-01-11 | 2022-04-22 | 辽宁石油化工大学 | Oxygen-containing defect lithium titanate zinc negative electrode material and preparation method thereof |
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| CN108538611B (en) * | 2018-02-23 | 2019-09-06 | 中国石油大学(北京) | A kind of nano-chip arrays cobalt acid nickel-carbon composite and its preparation method and application |
| CN108538611A (en) * | 2018-02-23 | 2018-09-14 | 中国石油大学(北京) | A kind of nano-chip arrays cobalt acid nickel-carbon composite and its preparation method and application |
| CN108682834B (en) * | 2018-06-12 | 2020-10-13 | 郑州新世纪材料基因组工程研究院有限公司 | Magnesium ion battery material and preparation method thereof, and magnesium ion battery composite material and preparation method thereof |
| CN108682834A (en) * | 2018-06-12 | 2018-10-19 | 郑州新世纪材料基因组工程研究院有限公司 | A kind of Magnesium ion battery material and preparation method thereof, Magnesium ion battery composite material and preparation method |
| CN109686954A (en) * | 2018-12-27 | 2019-04-26 | 陕西科技大学 | A kind of C-O-Mo key bridge joint monolithic taper MoS2/ NG sodium ion negative electrode material and preparation method thereof |
| CN110120507A (en) * | 2019-05-16 | 2019-08-13 | 常熟理工学院 | A kind of heterogeneous material compound and its preparation method and application that graphene is modified |
| CN110280232A (en) * | 2019-05-17 | 2019-09-27 | 华北电力大学 | A kind of preparation method of richness defect metal oxygen (sulphur) compound/graphene oxide composite material |
| CN110783542A (en) * | 2019-10-22 | 2020-02-11 | 济南大学 | Paper towel derived carbon fiber loaded MoS 2Preparation method of micro-flower composite material and application of micro-flower composite material in lithium-sulfur battery |
| CN112978800A (en) * | 2019-12-17 | 2021-06-18 | 山东海科创新研究院有限公司 | High-conductivity molybdenum disulfide material and preparation method and application thereof |
| CN112978800B (en) * | 2019-12-17 | 2022-12-20 | 山东海科创新研究院有限公司 | High-conductivity molybdenum disulfide material and preparation method and application thereof |
| CN113713833A (en) * | 2021-09-15 | 2021-11-30 | 北京师范大学 | Molybdenum oxysulfide/nickel sulfide/foamed nickel complex and preparation method and application thereof |
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