CN110048095A - A method of preparing the molybdenum disulfide molybdenum dioxide composite material for sodium ion negative electrode material - Google Patents
A method of preparing the molybdenum disulfide molybdenum dioxide composite material for sodium ion negative electrode material Download PDFInfo
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- CN110048095A CN110048095A CN201910225159.6A CN201910225159A CN110048095A CN 110048095 A CN110048095 A CN 110048095A CN 201910225159 A CN201910225159 A CN 201910225159A CN 110048095 A CN110048095 A CN 110048095A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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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- 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 methods for preparing the molybdenum disulfide molybdenum dioxide composite material for sodium ion negative electrode material, and two molybdic acid hydrate sodium are add to deionized water, sodium molybdate solution is stirred to get；Thiocarbamide, CTAB are sequentially added into sodium molybdate solution and is sufficiently stirred, and are transferred in hydrothermal reaction kettle；Sediment separate out, washing are dried to obtain molybdenum disulfide/molybdenum dioxide dissimilar materials of nanometer sheet assembling flower.The material is assembled by molybdenum disulfide/molybdenum dioxide nanometer sheet of heterojunction structure, wherein the thickness of nanometer sheet is in 10-20nm, length is in 0.8-1.0um, the nanometer sheet of heterojunction structure substantially increases the stability of structure, and agglomeration does not occur for the nanometer sheet of heterojunction structure, nanometer sheet is by being overlapped to form flower, great increasing specific surface area, to improve molybdenum disulfide/molybdenum dioxide anode material of lithium-ion battery cyclical stability.
Description
Technical field
The invention belongs to inorganic nano materials to synthesize field.It is related to preparing the molybdenum disulfide two of heterogeneous combination with hydro-thermal method
Aoxidize molybdenum composite material.More particularly to a kind of molybdenum disulfide molybdenum dioxide composite material prepared for sodium ion negative electrode material
Method.
Background technique
Today's society, a large amount of portable equipments enter in people's lives, mobile phone, laptop, motion bracelet, wrist-watch etc.
Deng bringing great convenience to people's lives.People place hope on these electronic equipments, and can quickly to supplement power supply right
It uses for a long time afterwards, therefore more stringent requirements are proposed for energy storage device.Presently mainly lithium ion battery is assembled in this
In a little portable equipments, a large amount of lithium ion batteries cause the shortage of lithium resource while application by manufacture, it was reported that lithium mineral products money
The price in source increases year by year, and also when the river rises the boat goes up therewith for manufacturing cost.Therefore finding suitable replacer becomes the weight researched and developed at present
Point content.
Sodium ion and lithium ion have similar physicochemical properties, and sodium resource rich reserves in the earth's crust, former material
Expect it is low in cost, be increasingly becoming people research object.Composition similar with lithium ion battery, sodium-ion battery is mainly by bearing
Pole material, diaphragm, electrolyte, positive electrode composition.It is highly-safe, the service life is long, the sodium-ion battery of high capacity is ground as people
The Main way studied carefully.The capacity contribution of battery is concentrated mainly on negative electrode material, therefore finds appropriate negative electrode material as acquisition
The key of high-capacity battery.Negative electrode material by the type of material can be divided into carbon material, oxide, sulfide, phosphide and
Material can be divided into insertion deintercalation formula and alloying reaction by selenides etc. in the way of storing up sodium.Compared to insertion and deintercalation
Formula, alloying reaction will cause the serious volume expansion of material, and then material structure is caused to crush.Currently, research work
Person mainly by carbon or with the compound of other materials and change the structure of material and improve the electric conductivity of material and the stabilization of structure
Property.Heterogeneous combination be there are two types of or two different Material claddings form, between different materials have certain synergistic effect,
Structural stability of the material in cyclic process can be improved.Sodium is used for for the composite material of molybdenum disulfide molybdenum dioxide at present
The research of ion battery is less, Zhanwei Xu (Zhanwei Xu, Tian Wang, Luo Kong, Kai Yao, Hao Fu,
Kang Li,Liyun Cao,Jianfeng Huang,and Qinglin Zhang.Part.Syst.Charact.2017,34,
1600223) composite material for devising molybdenum disulfide molybdenum dioxide vulcanizes molybdenum dioxide surface layer, improves material knot
The stability of structure.But in this method, first synthesize molybdenum dioxide carry out again synthesis of carbon/molybdenum disulfide in the presence of both be unevenly distributed
The phenomenon that, it is difficult to give full play to the effect of hetero-junctions.Therefore, it is steady for the circulation of material to design equally distributed heterojunction structure
It is qualitative to play an important role.
Summary of the invention
It is different the purpose of the present invention is preparing the equally distributed original position of molybdenum disulfide/molybdenum dioxide by using hydrothermal carbonization method
Structural material material.The material is assembled by molybdenum disulfide/molybdenum dioxide nanometer sheet, and molybdenum disulfide/molybdenum dioxide in situ is heterogeneous
In conjunction with the uniformity for substantially increasing the two, heterojunction structure improves the cyclical stability of material.
The present invention provide it is a kind of using hydrothermal synthesis of carbon/molybdenum disulfide/molybdenum dioxide heterojunction structure material, at carbonization
Reason can be used for molybdenum disulfide/molybdenum dioxide composite material preparation method of sodium-ion battery cathode.
Technical scheme is as follows:
For molybdenum disulfide/molybdenum dioxide composite material preparation method of sodium-ion battery cathode, steps are as follows:
1) two molybdic acid hydrate sodium are dissolved stirring in deionized water by, and being prepared into concentration is 0.02-0.10mol/L molybdic acid
Sodium water solution；
2) thiocarbamide is added in the solution that step 1) is configured by, and thiourea solution concentration is 0.02-0.10mol/L, is stirred
It mixes, surfactant cetyl trimethylammonium bromide is added, the concentration of cetyl trimethylammonium bromide is 0.01-
0.05mol/L continues to stir；
3) step 2) acquired solution is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner by, and uses stainless steel reaction
After kettle sealing, hydro-thermal reaction is carried out；After reaction, it cools to room temperature with the furnace, reactant is taken out, with dehydrated alcohol and deionization
Water centrifuge washing, vacuum drying obtain molybdenum disulfide/molybdenum dioxide material of nanometer sheet assembling flower-like structure；
4) the resulting material of step 3) is placed in quartz boat by, then quartz boat is placed on to the tube furnace for being connected with Ar gas
Middle carbonization treatment, furnace cooling obtain molybdenum disulfide/titanium dioxide molybdenum materials of the good nanometer sheet assembling flower-like structure of crystallinity
Material.
Optimum condition is speed of agitator 200-400r/min, mixing time 0.5-1.5h in the step 1), step 2).
The middle step 3) hydrothermal reaction condition: being heated to 180-220 DEG C, keeps the temperature 12-36h.
The middle dehydrated alcohol of the middle step 3) and deionized water centrifuge washing 6-8 times, are dried in vacuo 10-12h.
Carbonization treatment condition is in the middle step 4): heating rate is 2-5 DEG C/min, keeps the temperature 2- at 700-900 DEG C
5h。
Method of the invention is prepared into molybdenum disulfide/molybdenum dioxide material of nanometer sheet assemble nanometer flower-like structure, uniformly
Distribution, and nanometer sheet mutually overlaps and forms three-dimensional space, and wherein molybdenum disulfide/molybdenum dioxide nanometer sheet is with a thickness of 10-20nm,
Length is in 0.8-1um.
Method of the invention is prepared into molybdenum disulfide/molybdenum dioxide material of nanometer sheet assembling flower-like structure for sodium ion
Battery.
Effect of the invention is that fabricated in situ molybdenum disulfide/molybdenum dioxide heterojunction structure material is negative for sodium-ion battery
Pole.Since system is not in acidic environment, molybdenum source does not cure sufficiently and forms molybdenum oxide, and the material is by molybdenum disulfide/bis-
Molybdenum oxide nanometer sheet assembles, and the heterogeneous combination of molybdenum disulfide/molybdenum dioxide, nanometer sheet mutually overlaps and forms three-dimensional space,
Middle molybdenum disulfide/molybdenum dioxide nanometer sheet is used in sodium-ion battery with a thickness of 10-20nm, length in 0.8-1um,
100mA g-1Current density under test its performance, its specific capacity is up to 400mAh g after circulation 50 times-1More than, hetero-junctions
Structure substantially increases the cyclical stability of material.
Detailed description of the invention
Fig. 1 is that molybdenum disulfide/molybdenum dioxide heterojunction structure composite material X of the assembling of nanometer sheet prepared by embodiment 1 is penetrated
Ray diffraction diagram, show in figure diffraction maximum at 14.2 ° of angle of diffraction, 32.9 °, 39.5 °, 58.7 ° with (002) of molybdenum disulfide,
(100), (103), (110) crystal face match；And diffraction maximum is at 27 °, and 38 °, 54 ° of (011) with molybdenum oxide, (- 112) (- 311)
Crystal face matches, and illustrates that prepared product is made of molybdenum disulfide/molybdenum dioxide, wherein molybdenum disulfide/molybdenum dioxide tool
There is excellent crystallinity.
Fig. 2 is molybdenum disulfide/molybdenum dioxide heterojunction structure composite material scanning of the assembling of nanometer sheet prepared by embodiment 2
Electron microscopic picture, it can be seen from the figure that the material is assembled by the structure composite of nanometer sheet.
Fig. 3 is molybdenum disulfide/molybdenum dioxide material scanning electron microscopic picture of the assembling of nanometer sheet prepared by embodiment 3, from
As can be seen that molybdenum disulfide/molybdenum dioxide material scanning electron microscopic picture of nanometer sheet assembling, the thickness of nanometer sheet exist in figure
10-20nm, length is in 0.8-1.0um.
Specific embodiment
Embodiment 1:
1) dissolves two molybdic acid hydrate sodium in deionized water, stirs 0.5h with 200r/min revolving speed, being prepared into concentration is
0.02mol/L sodium molybdate aqueous solution；
2) thiocarbamide is added in the solution that step 1) is configured by, thiourea solution concentration be 0.02mol/L, continue with
After 200r/min revolving speed stirs 0.5h, surfactant cetyl trimethylammonium bromide, cetyl trimethyl bromination is added
The concentration of ammonium is 0.01mol/L, continues to stir 0.5h with 200r/min revolving speed；
3) step 2) acquired solution is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner by, and uses stainless steel reaction
After kettle sealing, hydrothermal condition: being heated to 180 DEG C, keeps the temperature 18h.After reaction, it cools to room temperature with the furnace, takes out reactant, use
Dehydrated alcohol and deionized water centrifuge washing 6 times, 60 DEG C of vacuum drying 10h obtain the curing of nanometer sheet assembling flower-like structure
Molybdenum/molybdenum dioxide material；
4) the resulting material of step 4) is placed in quartz boat by, then quartz boat is placed on to the tube furnace for being connected with Ar gas
Middle carbonization treatment, Carbonization Conditions are: heating rate is 2 DEG C/min, 2h is kept the temperature at 700 DEG C, it is good to obtain crystallinity for furnace cooling
Molybdenum disulfide/molybdenum dioxide material of good nanometer sheet assembling flower-like structure.
As shown in Figure 1, the product of preparation is molybdenum disulfide/molybdenum dioxide composite material, there is excellent crystallinity.It is used in
In sodium-ion battery, in 100mAg-1Current density under test its performance, its specific capacity is up to 400mAh after circulation 50 times
g-1More than.
Embodiment 2:
1) dissolves two molybdic acid hydrate sodium in deionized water, stirs 1.0h with 300r/min revolving speed, being prepared into concentration is
0.060mol/L sodium molybdate aqueous solution；
2) thiocarbamide is added in the solution that step 1) is configured by, thiourea solution concentration be 0.06mol/L, continue with
After 300r/min revolving speed stirs 1.0h, surfactant cetyl trimethylammonium bromide, cetyl trimethyl bromination is added
The concentration of ammonium is 0.025mol/L, continues to stir 1.0h with 300r/min revolving speed；
3) step 2) acquired solution is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner by, and uses stainless steel reaction
After kettle sealing, hydrothermal condition: 200 DEG C are heated to, heat preservation is for 24 hours.After reaction, it cools to room temperature with the furnace, takes out reactant, use
Dehydrated alcohol and deionized water centrifuge washing 7 times, 70 DEG C of vacuum drying 11h obtain the curing of nanometer sheet assembling flower-like structure
Molybdenum/molybdenum dioxide material；
4) the resulting material of step 4) is placed in quartz boat by, then quartz boat is placed on to the tube furnace for being connected with Ar gas
Middle carbonization treatment, Carbonization Conditions are: heating rate is 3 DEG C/min, 3h is kept the temperature at 800 DEG C, it is good to obtain crystallinity for furnace cooling
Molybdenum disulfide/molybdenum dioxide material of good nanometer sheet assembling flower-like structure.
As shown in Fig. 2, the flower-like structure that product is assembled by the nanometer sheet of small size, wherein the thickness of nanometer sheet exists
10-20nm, length is in 0.8-1um.In sodium-ion battery, in 100mA g-1Current density under test its performance, recycle
Its specific capacity is up to 380mA h g after 100 times-1More than, coulombic efficiency is close to 100%.
Embodiment 3:
1) dissolves two molybdic acid hydrate sodium in deionized water, stirs 1.5h with 400r/min revolving speed, being prepared into concentration is
0.10mol/L sodium molybdate aqueous solution；
2) thiocarbamide is added in the solution that step 1) is configured by, thiourea solution concentration be 0.1mol/L, continue with
After 400r/min revolving speed stirs 1.5h, surfactant cetyl trimethylammonium bromide, cetyl trimethyl bromination is added
The concentration of ammonium is 0.05mol/L, continues to stir 1.5h with 400r/min revolving speed；
3) step 2) acquired solution is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner by, and uses stainless steel reaction
After kettle sealing, hydrothermal condition: being heated to 220 DEG C, keeps the temperature 36h.After reaction, it cools to room temperature with the furnace, takes out reactant, use
Dehydrated alcohol and deionized water centrifuge washing 8 times, 80 DEG C of vacuum drying 12h obtain the curing of nanometer sheet assembling flower-like structure
Molybdenum/molybdenum dioxide material；
4) the resulting material of step 4) is placed in quartz boat by, then quartz boat is placed on to the tube furnace for being connected with Ar gas
Middle carbonization treatment, Carbonization Conditions are: heating rate is 5 DEG C/min, 5h is kept the temperature at 900 DEG C, it is good to obtain crystallinity for furnace cooling
Molybdenum disulfide/molybdenum dioxide material of good nanometer sheet assembling flower-like structure.
As shown in figure 3, what product was assembled by the nanometer sheet of small size, wherein the thickness of nanometer sheet is in 10-20nm, length
Degree is in 0.8-1um.In sodium-ion battery, in 100mA g-1Current density under test its chemical property, recycle 300 times
Its specific capacity is up to 320mA h g later-1More than, coulombic efficiency is close to 100%.
To sum up the attached drawing of embodiment can also clearly be found out, product prepared by the present invention is the assembling of small size nanometer sheet
Molybdenum disulfide/molybdenum dioxide composite material.
Claims (7)
1. a kind of method for preparing the molybdenum disulfide molybdenum dioxide composite material for sodium ion negative electrode material, it is characterized in that including
Steps are as follows:
1) two molybdic acid hydrate sodium are dissolved stirring in deionized water by, and being prepared into concentration is 0.02-0.10mol/L sodium molybdate water
Solution；
2) thiocarbamide is added in the solution that step 1) is configured by, and thiourea solution concentration is 0.02-0.10mol/L, is stirred,
Surfactant cetyl trimethylammonium bromide is added, the concentration of cetyl trimethylammonium bromide is 0.01-0.05mol/
L continues to stir；
3) step 2) acquired solution is transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle liner by, and close using stainless steel cauldron
It is honored as a queen, carries out hydro-thermal reaction；After reaction, cool to room temperature with the furnace, take out reactant, with dehydrated alcohol and deionized water from
Heart washing, vacuum drying obtain molybdenum disulfide/molybdenum dioxide material of nanometer sheet assembling flower-like structure；
4) the resulting material of step 3) is placed in quartz boat by, then quartz boat is placed on to carbon in the tube furnace for being connected with Ar gas
Change processing, furnace cooling obtain molybdenum disulfide/molybdenum dioxide material of the good nanometer sheet assembling flower-like structure of crystallinity.
2. the method as described in claim 1, it is characterized in that speed of agitator 200-400r/min in the step 1), step 2),
Mixing time 0.5-1.5h.
3. the method as described in claim 1, it is characterized in that the middle step 3) hydrothermal reaction condition: it is heated to 180-220 DEG C,
Keep the temperature 12-36h.
4. the method as described in claim 1, it is characterized in that being washed in the middle step 3) with dehydrated alcohol and deionized water centrifugation
It washs 6-8 times, is dried in vacuo 10-12h.
5. the method as described in claim 1, it is characterized in that carbonization treatment condition is in the middle step 4): heating rate 2-
5 DEG C/min, 2-5h is kept the temperature at 700-900 DEG C.
6. method of claim 1 is prepared into molybdenum disulfide/molybdenum dioxide material of nanometer sheet assemble nanometer flower-like structure, uniformly
Distribution, and nanometer sheet mutually overlaps and forms three-dimensional space, and wherein molybdenum disulfide/molybdenum dioxide nanometer sheet is with a thickness of 10-20nm,
Length is in 0.8-1um.
7. molybdenum disulfide/molybdenum dioxide the material for being prepared into nanometer sheet assembling flower-like structure of claim 1 is for sodium ion electricity
Pond.
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| CN113823788A (en) * | 2021-09-17 | 2021-12-21 | 陕西科技大学 | MnO (MnO)2/MoS2Heterojunction composite material and preparation method and application thereof |
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| CN113617371A (en) * | 2021-08-23 | 2021-11-09 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of sandwich structure hollow nano reactor photocatalytic material, product and application |
| CN113823788A (en) * | 2021-09-17 | 2021-12-21 | 陕西科技大学 | MnO (MnO)2/MoS2Heterojunction composite material and preparation method and application thereof |
| CN113823788B (en) * | 2021-09-17 | 2024-03-15 | 深圳市鸿途科技服务有限公司 | MnO (MnO) 2 /MoS 2 Heterojunction composite material and preparation method and application thereof |
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