CN105047914A - Lithium-ion battery anode material molybdenum disulfide/carbon and preparation method thereof - Google Patents
Lithium-ion battery anode material molybdenum disulfide/carbon and preparation method thereof Download PDFInfo
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- CN105047914A CN105047914A CN201510284228.2A CN201510284228A CN105047914A CN 105047914 A CN105047914 A CN 105047914A CN 201510284228 A CN201510284228 A CN 201510284228A CN 105047914 A CN105047914 A CN 105047914A
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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
- H01M4/36—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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- 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 lithium-ion battery anode material molybdenum disulfide/carbon and a preparation method thereof. A dry tremella-like MoS2/C composite material is prepared by a thermal reduction method; a half-battery is prepared; the electrochemical property of the half-battery is tested; and the result shows that the half-battery is high in specific capacity and stable in cycle performance. The method is simple, reliable, good in process repeatability and high in operability, and can be widely popularized. The preparation method comprises the following steps: (1), taking a proper amount of ammonium tetrathiomolybdate, hexadecyl trimethyl ammonium bromide and silica nanospheres as raw materials; (2), preparing a sample by the thermal reduction method; and (3), removing silicon dioxide with hydrofluoric acid to obtain the required product.
Description
Technical field
The present invention relates to a kind of lithium ion battery cathode material and its preparation method, particularly a kind of lithium ion battery negative material molybdenum bisuphide/carbon (MoS
2/ C) and preparation method thereof.
Background technology
The progress of the present stage mankind and the achievement acquired by development of society depend on the traditional fossil energy such as oil, coal largely.Along with continuous consumption and the not exclusively use of these non-regeneration energies, the whole world is faced with energy crisis and serious problem of environmental pollution.The words such as Global Greenhouse Effect, disruption of ecological balance, haze become in recent years that what's frequently heard can be repeated in detail, how to address these problems, become the huge challenge of scientific technological advance.Therefore, the renewable new forms of energy that exploitation is clean become study hotspot.Wherein the regenerative resource such as solar energy, wind energy and biological energy source has had universal in some places, but high to geographical factors dictate due to it, realize that the whole world is universal exists certain difficulty, so its development process is slow.
With lithium ion battery be that the secondary cell energy system of representative has that operating voltage is high, specific capacity is high, self discharge effect is little, lightweight, volume is little, memory-less effect and the excellent properties such as environmental friendliness not only become current most popular portable electric appts power supply, cause great concern in electric automobile field simultaneously.Therefore, countries in the world using various lithium ion battery used for electric vehicle as giving priority to industry, also will open wide development space for China's electrokinetic cell industry simultaneously from now on.But, current lithium ion battery also cannot meet Large-scale Mobile equipment high-energy-density, can the requirement of fast charging and discharging.This is centered around raising battery energy density with regard to making the study hotspot of lithium ion battery, strengthen the cyclical stability of battery and solve fast charging and discharging problem, thus enable lithium ion battery meet the demand of Large-scale Mobile equipment, and then it is fast-developing to promote lithium ion battery industry.
Research wherein for negative material mainly concentrates on the following aspects: lower electrode potential, higher specific capacity and good cyclical stability, environment friendly with good compatibility, lower production cost and the safety non-pollution of the battery such as electrolyte and adhesive part.Current graphite is due to good cycling stability, and operating voltage is higher, and material source is wide, low production cost and by extensively with being lithium ion battery negative material, and commercialization.But the specific capacity of graphite electrode relatively low (~ 372mAh/g), which also limits further developing of lithium ion battery.Therefore, how to prepare the better negative material of performance and become the focus of Study on Li-ion batteries in recent years.
There is the molybdenum bisuphide (MoS of typical layered structure
2) have and structure like graphite-phase: in layer between S-Mo-S atom by stronger covalent bonds, then combined by more weak Van der Waals force between layers.Just because of MoS
2the bonding that interlayer is more weak, makes it can introduce external molecule, atom or ion by the method for intercalation at its interlayer and the structure that do not change in its layer, forms composite material.As lithium ion battery negative material, MoS
2have very high initial capacity (~ 670mAh/g), its special layer structure is beneficial to Li
+embedding with deviate from.But, the electrons/ions conductivity low due to itself and in removal lithium embedded process serious volumetric expansion make its cyclical stability extremely low.In addition, in cell reaction process, MoS
2with Li
+react and generate the Li of indissoluble
2s, Li
2s again catalytic electrolysis liquid decomposition thus form thick polymeric layer and cause irreversible capacitance loss, this is also the reason of its cyclical stability difference.Therefore how MoS is improved
2cyclical stability, become MoS
2as the key of lithium ion battery negative material research.
If by MoS
2combine formation composite material with material with carbon element, the electrode material of high power capacity and good circulation stability may be obtained.Softex kw (CTAB) is a kind of common cationic surfactant, be usually used in the controlled synthesis of material, can change the microscopic appearance of material, it contains a lot of carbon simultaneously, can carbon source be served as, obtain carbon after heat treatment.Silica nanosphere, through being often used as Template preparation porous material, can increase the surface area of material.In ion cathode material lithium, the increase of material surface area can increase the contact area of lithium ion in electrode and electrolyte and activated adoption, desorption center, thus is conducive to doff lithium reaction, increases the lithium storage content of material.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the invention provides a kind of lithium ion battery negative material molybdenum bisuphide/carbon (MoS
2/ C) and preparation method thereof, the method is simple and reliable, good process repeatability, workable.
Technical scheme: for achieving the above object, the technical solution used in the present invention is:
A kind of lithium ion battery negative material molybdenum bisuphide/carbon, raw material is made up of four thio ammonium molybdate, softex kw, silica nanosphere and absolute ethyl alcohol.
Further, in the present invention, the ratio of the amount of substance of described four thio ammonium molybdate, softex kw and silica nanosphere three is 1:0.14 ~ 0.43:1.7 ~ 1.75; Described absolute ethyl alcohol is 30ml.
Further, in the present invention, described silica nanosphere diameter is 20nm, and content is >99wt%.
Prepare the method for described lithium ion battery negative material molybdenum bisuphide/carbon, comprise the following steps:
1) described raw material is mixed, be stirred to absolute ethanol volatilizes, residual powder is carried out drying at 50 ~ 65 DEG C;
2) by step 1) described dried powder is incubated 4h at tube furnace under being placed in atmosphere, then is cooled to room temperature, obtains black powder;
3) by step 2) described black powder hydrofluoric acid treatment, filtration drying, obtains product MoS
2/ C composite.
Further, in the present invention, step 2) described in atmosphere be the mixed atmosphere of argon gas and hydrogen, the volume ratio of described argon gas and hydrogen is 9.5:0.5.
Further, in the present invention, step 2) described in the temperature stabilization of insulating process be 700 ~ 800 DEG C.
Further, in the present invention, step 3) described in the mass concentration of hydrofluoric acid be 5 ~ 6%.
Beneficial effect: lithium ion battery negative material molybdenum bisuphide/carbon (MoS provided by the invention
2/ C) and preparation method thereof, compared with prior art, there is following advantage:
1. the present invention adopts thermal reduction to prepare product, and the method is simple and reliable, good process repeatability, workable;
2. products obtained therefrom of the present invention carries out electrochemical property test after being assembled into half-cell, and test result shows this material and has high specific capacity and excellent cyclical stability.
Accompanying drawing explanation
Fig. 1 is the MoS prepared
2the thermogravimetric curve schematic diagram of/C composite;
Fig. 2 is the MoS prepared
2the scanning electron microscope image schematic diagram of/C composite;
Fig. 3 is the MoS prepared
2the images of transmissive electron microscope schematic diagram of/C composite, wherein illustration is high power images of transmissive electron microscope;
Fig. 4 is the MoS prepared
2the MoS that/C composite prepares
2the charging and discharging curve schematic diagram of the cycle characteristics curve of/C composite;
Fig. 5 is the MoS prepared
2the CV curve synoptic diagram of/C composite;
Fig. 6 is the MoS prepared
2/ C composite at 100mAg
-1current density under cycle characteristics curve synoptic diagram;
Fig. 7 is the MoS prepared
2the cycle characteristics curve synoptic diagram of/C composite under different multiplying.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described.
A kind of lithium ion battery negative material molybdenum bisuphide/carbon (MoS
2/ C), reaction raw materials is made up of four thio ammonium molybdate, softex kw, silica nanosphere and absolute ethyl alcohol.Wherein, the ratio of the amount of substance of four thio ammonium molybdate, softex kw and silica nanosphere three is 1:0.14 ~ 0.43:1.7 ~ 1.75; Absolute ethyl alcohol is 30ml.Silica nanosphere diameter is 20nm, and content is >99wt%.
Medicine is as follows:
Four thio ammonium molybdate, analyzes pure, Chemical Reagent Co., Ltd., Sinopharm Group, Shanghai;
Softex kw, analyzes pure, Shanghai Ling Feng chemical reagent Co., Ltd, Shanghai;
Silica nanosphere, diameter 20nm, content: >99wt%, Nanjing Xian Feng Nono-material Science & Technology Ltd., Nanjing;
Absolute ethyl alcohol, analyzes pure, Chemical Reagent Co., Ltd., Sinopharm Group, Shanghai.
Prepare the method for lithium ion battery negative material molybdenum bisuphide/carbon, prepare the MoS of dry auricularia auriculajudae shape with thermal reduction
2/ C composite, testing its chemical property after being prepared into half-cell, to show its specific capacity high, stable cycle performance.Specifically comprise the following steps:
1) all reaction raw materials are mixed, be at room temperature stirred to solvent absolute ethyl alcohol and volatilize completely, residual powder is carried out drying at 50 ~ 65 DEG C;
2) by step 1) dried powder to be placed under the mixed atmosphere of argon gas and hydrogen at tube furnace with 700 ~ 800 DEG C of insulation 4h, then to naturally cool to room temperature, obtains black powder;
3) by step 2) the black powder mass concentration that obtains is the hydrofluoric acid treatment of 5 ~ 6%, removing SiO
2, filtration drying, obtains end product MoS
2/ C composite.
Embodiment 1
A kind of lithium ion battery negative material molybdenum bisuphide/carbon (MoS
2/ C), reaction raw materials prepares MoS by four thio ammonium molybdate 0.250g, softex kw 0.050g, silica nanosphere 0.100g (ratio of three's amount of substance is 1:0.143:1.733) and absolute ethyl alcohol 30ml
2the reaction raw materials of/C;
1) by described MoS
2the reaction raw materials of/C composite at room temperature stirs until solvent volatilizees completely, and residual powder is carried out drying at 50 ~ 65 DEG C;
2) by step 1) the described dried powder volume ratio that is placed in argon gas and hydrogen is under the mixed atmosphere of 9.5:0.5, with 700 ~ 800 DEG C of insulation 4h in tube furnace, naturally cools to room temperature and obtains black powder;
3) be the hydrofluoric acid treatment of 5 ~ 6% by the black powder concentration described in step 3, removing SiO
2, after filtration drying, obtain end product MoS
2/ C composite.
Be illustrated in figure 1 the MoS that embodiment 1 prepares
2the thermogravimetric curve of/C composite.Can see from thermogravimetric curve has an obvious Weight lose at about 50 DEG C, and this is the evaporation of moisture in sample.270 DEG C to 500 DEG C be second time Weight lose, this is by MoS
2cause with carbon aerial oxidation.And have third time weightless at 650 DEG C to 1000 DEG C, corresponding to MoO
3distillation.According to this part MoO
3the weightlessness that causes of distillation be 42.9%, the carbon content calculated in material is 33.4%.
Fig. 2 is the MoS that embodiment 1 prepares
2the scanning electron microscope image of/C composite.From scan image, find out that material surface presents the plate like structure of a kind of class, overall pattern is similar to dry auricularia auriculajudae.This pattern being similar to dry auricularia auriculajudae of material adds the surface area of material, is conducive to more lithium ion and inserts, thus improve the lithium storage content of material.
Fig. 3 is the MoS that embodiment 1 prepares
2the images of transmissive electron microscope of/C composite, wherein illustration is high power images of transmissive electron microscope.Obviously can see the lamellar structure of material from high power figure, carrying out measurement discovery layer spacing to it is 1.03nm, compares MoS
2original 0.62nm increases to some extent.Lamella is unordered in a jumble simultaneously, and piling up the number of plies seldom, be individual layer or 2 ~ 3 layers, and lamella size is less.
Fig. 4 is the MoS that embodiment 1 prepares
2the MoS that/C composite prepares
2the charging and discharging curve of the cycle characteristics curve of/C composite.In discharge process first, the discharge curve of material is continually varying curve, does not have obvious potential plateau, this is because the existence of carbon is on the impact of material charge and discharge process.And in second time and third time discharge curve, occurred an obvious potential plateau at ~ 1.9V place, this platform corresponds to sulphur and is first reduced into polysulfide, and then becomes Li
2the reaction of S.Both have two potential plateau, corresponding to Li in ~ 2.2 and 1.75V place in three charging curves
2s has been oxidized to the reaction of sulphur.
Fig. 5 is the MoS that embodiment 1 prepares
2the CV curve of/C composite.In first time circulation, there is a unconspicuous wide reduction peak at ~ 0.8V place, ~ there is a reduction peak at 0.45V place, corresponds respectively to Li
+insert MoS
2interlayer, formed Li
xmoS
2and Li
xmoS
2convert Mo and Li to further
2the reaction of S.In second time and third time circulation, the position of oxidation peak does not change, and the reduction peak at ~ 0.45V and ~ 0.8V place disappears, and generates Li corresponding to multistep reaction
2s.
Fig. 6 is the MoS that embodiment 1 prepares
2/ C composite at 100mAg
-1current density under cycle characteristics curve; Be increased between 100 times in cycle-index by 0, the specific capacity that chemical property experiment records this product is approximately stabilized in 800 ~ 1000mAhg
-1between, illustrate that product of the present invention is through electrochemical property test, proves that it has specific capacity high, the characteristic of stable cycle performance.
Fig. 7 is the MoS that embodiment 1 prepares
2the cycle characteristics curve of/C composite under different multiplying.As can be seen from the figure respectively through 200mAg
-1, 400mAg
-1, 600mAg
-1, 800mAg
-1and 1000mAg
-1be circulated to after 150 times under the current density increased gradually, material still can keep 560mAhg
-1specific capacity, and from 1000mAg
-1return to 100mAg
-1time, its reversible capacity almost can return to rapidly initial 100mAg
-1the capability value of circulation time, and the decay not having capacity in follow-up circulation.
Embodiment 2
The present embodiment as different from Example 1, reaction raw materials is: four thio ammonium molybdate 0.250g, softex kw 0.100g, silica nanosphere 0.100g (ratio of three's amount of substance is 1:0.286:1.733) and absolute ethyl alcohol 30ml, other are identical with embodiment 1.
Embodiment 3
The present embodiment as different from Example 1, four thio ammonium molybdate 0.250g, softex kw 0.150g, silica nanosphere 0.100g (ratio of three's amount of substance is 1:0.429:1.733) and absolute ethyl alcohol 30ml in step 1, other are identical with embodiment 1.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. lithium ion battery negative material molybdenum bisuphide/carbon, is characterized in that: raw material is made up of four thio ammonium molybdate, softex kw, silica nanosphere and absolute ethyl alcohol.
2. lithium ion battery negative material molybdenum bisuphide/carbon according to claim 1, is characterized in that: the ratio of the amount of substance of described four thio ammonium molybdate, softex kw and silica nanosphere three is 1:0.14 ~ 0.43:1.7 ~ 1.75; Described absolute ethyl alcohol is 30ml.
3. lithium ion battery negative material molybdenum bisuphide/carbon according to claim 1, it is characterized in that: described silica nanosphere diameter is 20nm, content is >99wt%.
4. prepare the method for lithium ion battery negative material molybdenum bisuphide/carbon as claimed in claim 1, it is characterized in that: comprise the following steps:
1) described raw material is mixed, be stirred to absolute ethanol volatilizes, residual powder is carried out drying at 50 ~ 65 DEG C;
2) by step 1) described dried powder is incubated 4h at tube furnace under being placed in atmosphere, then is cooled to room temperature, obtains black powder;
3) by step 2) described black powder hydrofluoric acid treatment, filtration drying, obtains product MoS
2/ C composite.
5. the preparation method of lithium ion battery negative material molybdenum bisuphide/carbon according to claim 4, is characterized in that: step 2) described in atmosphere be the mixed atmosphere of argon gas and hydrogen, the volume ratio of described argon gas and hydrogen is 9.5:0.5.
6. the preparation method of lithium ion battery negative material molybdenum bisuphide/carbon according to claim 4, is characterized in that: step 2) described in the temperature stabilization of insulating process be 700 ~ 800 DEG C.
7. the preparation method of lithium ion battery negative material molybdenum bisuphide/carbon according to claim 4, is characterized in that: step 3) described in the mass concentration of hydrofluoric acid be 5 ~ 6%.
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| CN107248573A (en) * | 2017-06-26 | 2017-10-13 | 浙江工业大学 | Polyphosphazene is combined the preparation method of carbon composite electrode material for the molybdenum disulfide of carbon source |
| CN109830670A (en) * | 2019-03-04 | 2019-05-31 | 郑州大学 | A kind of hollow sandwich type SiO of lithium ion battery negative material2/C/MoS2Hybrid microspheres |
| CN111864209A (en) * | 2020-05-14 | 2020-10-30 | 清华大学 | Preparation method and application of lithium-sulfur battery positive electrode material |
| CN113173601A (en) * | 2021-04-25 | 2021-07-27 | 黑龙江大学 | Thin-layer MXene/hexagonal phase molybdenum disulfide composite material and preparation method and application thereof |
| CN114520327A (en) * | 2020-11-20 | 2022-05-20 | 中国科学院大连化学物理研究所 | Preparation method and application of mesoporous molybdenum disulfide/carbon composite material |
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| CN113173601A (en) * | 2021-04-25 | 2021-07-27 | 黑龙江大学 | Thin-layer MXene/hexagonal phase molybdenum disulfide composite material and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN105047914B (en) | 2017-11-17 |
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