CN108630916A - A kind of bacteria cellulose supported titanium niobium O compoiste material and its preparation method and application - Google Patents
A kind of bacteria cellulose supported titanium niobium O compoiste material and its preparation method and application Download PDFInfo
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- CN108630916A CN108630916A CN201810263493.6A CN201810263493A CN108630916A CN 108630916 A CN108630916 A CN 108630916A CN 201810263493 A CN201810263493 A CN 201810263493A CN 108630916 A CN108630916 A CN 108630916A
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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
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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
- H01M4/48—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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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Abstract
The invention discloses a kind of bacteria cellulose supported titanium niobium O compoiste material and preparation method thereof and as the application of lithium ion battery negative material, which has larger specific surface area, and Ti is loaded on bacteria cellulose2Nb10O29Nano particle can increase the contact area of electrolyte and motor, provide bigger more effective active reaction area, meanwhile, electronics conduction velocity is accelerated, chemical property is improved.The present invention generates bacterial cellulose stent carbon, bacteria cellulose/Ti is prepared by hydro-thermal method and high temperature sintering methods as carrier by high-temperature sintering process, sintering2Nb10O29Electrode material.Bacteria cellulose/Ti of the present invention2Nb10O29Material has the characteristics that high circulation service life, high-energy and power density, has broad application prospects in fields such as mobile communication, electric vehicle, solar power generation and aerospaces.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative, and in particular to a kind of bacteria cellulose supported titanium niobium oxygen
(Ti2Nb10O29) composite material and preparation method and the application as lithium ion battery negative material.
Background technology
Electronic product consumption market expands rapidly so that increasing for the demand of high-performance, high stable battery material
Add.The storage lithium structure that titanium niobate lithium storage materials have had, to determine its chemical property possessed.It is currently mainly used
Negative material include graphite and lithium titanate etc., but all there is a problem that serious, graphite is easy due to its low voltage platform
It forms SEI films (solid electrolyte interface, solid electrolyte interface film) and causes Li dendrite, may cause quick-fried
It is fried, though and lithium titanate is higher without generating SEI films, its low theoretical capacity (175mAh g because of voltage platform-1) so that energy storage
It shows not ideal enough.Compared with the negative material that these are common, niobic acid titanium compound has the theoretical capacity of bigger and opposite
Security and stability.But niobic acid titanium compound equally exists some disadvantages, for example its electronic conductivity is low, lithium ion diffusion coefficient
It is smaller etc..
Using bacterial cellulose stent carbon as substrate, load on it grows titanium niobium oxygen (Ti2Nb10O29), it can be effective
Electronics conduction velocity is improved, the specific surface area of titanium niobium oxygen particle is improved, to improve its chemical property.Bacteria cellulose/
Ti2Nb10O29It can be used as the lithium ion battery negative material with high-energy density, high power density and high safety stability.
Invention content
It is an object of the invention to for the not high graphite of current security performance and the lower lithium titanate lithium of theoretical capacity from
Sub- cell negative electrode material provides a kind of bacteria cellulose supported titanium niobium oxygen (Ti2Nb10O29) composite material and preparation method and
As the application of lithium ion battery negative material, the bacteria cellulose/Ti2Nb10O29Electrode material is high with high power density
Energy density and high safety stability.
A kind of bacteria cellulose supported titanium niobium oxygen (Ti2Nb10O29) composite material preparation method, include the following steps：
(1) bacteria cellulose is lyophilized with freeze drier, is sintered, obtains bacterial cellulose stent carbon；
(2) columbium pentachloride and isopropyl titanate are dissolved in ethanol solution, are uniformly mixed to form mixed solution, added
Enter into reaction kettle, and bacterial cellulose stent carbon made from step (1) is added and seals and heats as growth substrate, it is cooling
Afterwards, product is washed into drying, obtains target predecessor, target predecessor is sintered, obtain bacteria cellulose supported titanium niobium oxygen
(Ti2Nb10O29) composite material.
It is used as the preferred technical solution of the present invention below：
In step (1), the sintering specifically includes：It is put into tube furnace, it is small that 1-2 is sintered under the conditions of 600-800 DEG C
When.Further preferably, the sintering specifically includes：It is put into tube furnace, is sintered 1-2 hours under the conditions of 700-800 DEG C.
In step (2), in molar ratio the 5 of the columbium pentachloride and isopropyl titanate：0.8~1.2, described is phosphoric
In molar ratio the 5 of niobium and isopropyl titanate：1,
The reaction kettle is polytetrafluoroethylene (PTFE) autoclave；
It is 150 DEG C -200 DEG C that the heating, which uses hydro-thermal method, hydrothermal temperature, and the hydro-thermal time is 6-24 hours, further
It is preferred that hydrothermal temperature is 160 DEG C -200 DEG C, the hydro-thermal time is 10-24 hours.
The condition of the described target predecessor sintering is：It is sintered 1-2 hours under the conditions of 600-900 DEG C in tube furnace.
Bacteria cellulose supported titanium niobium O compoiste material (i.e. bacteria cellulose/Ti prepared by the present invention2Nb10O29Material) it gathers around
There are high theoretical capacity (396mAh g-1), preferable electronic conductivity and higher security and stability, Ti2Nb10O29Nanometer
Average diameter of particles is about 10-40nm.Bacteria cellulose/the Ti2Nb10O29Material is compound as a kind of new titanium niobium oxygen
Material.Particularly as lithium ion battery negative material.
Compared with prior art, the invention has the advantages that：
The method of the present invention prepares bacterial cellulose stent carbon substrate by high-temperature sintering process, then with the simple hydro-thermal of a step
Method prepares bacteria cellulose/Ti2Nb10O29Predecessor.Bacteria cellulose/Ti is obtained finally by high temperature sintering2Nb10O29Mesh
Mark product.The preparation method is simple and convenient, easily controllable.
Bacteria cellulose/Ti prepared by the present invention2Nb10O29Electrode material has larger specific surface area, bacteria cellulose
Upper load Ti2Nb10O29Nano particle can increase the contact area of electrolyte and motor, provide bigger more effective active reaction
Area, meanwhile, electronics conduction velocity is accelerated, chemical property is improved.In the present invention, formation, the reaction for overcoming SEI films are dynamic
Mechanics disadvantage keeps high-energy density to realize while high power discharge performance, close with high power, high-energy to be formed
The novel cathode material for lithium ion battery of degree, high safety stability.
Bacteria cellulose supported titanium niobium O compoiste material of the present invention has larger specific surface area, is loaded on bacteria cellulose
Ti2Nb10O29Nano particle can increase the contact area of electrolyte and motor, provide bigger more effective active reaction area, together
When, electronics conduction velocity is accelerated, chemical property is improved.By high-temperature sintering process, it is sintered 1-2 hours and generates bacterial fibers
Plain holder carbon prepares bacteria cellulose/Ti as carrier by hydro-thermal method and high temperature sintering methods2Nb10O29Electrode material.
Bacteria cellulose/Ti of the present invention2Nb10O29Material has the characteristics that high circulation service life, high-energy and power density, mobile communication,
The fields such as electric vehicle, solar power generation and aerospace have broad application prospects.
Description of the drawings
Fig. 1 is bacteria cellulose/Ti obtained in embodiment 12Nb10O29The XRD diagram of target product.
Fig. 2 is bacteria cellulose/Ti obtained in embodiment 22Nb10O29The scanning electron microscope (SEM) photograph of target product.
Fig. 3 is bacteria cellulose/Ti obtained in embodiment 32Nb10O29The transmission electron microscope picture of target product.
Specific implementation mode
With reference to embodiment, the present invention will be described in detail, but the present invention is not limited to this.
Embodiment 1
The bacteria cellulose (purchase is in Guilin Qi Hong Science and Technology Ltd.s) of freezing is lyophilized with freeze drier, and
It is put into tube furnace, is sintered 2 hours under conditions of 800 DEG C, obtains bacterial cellulose stent carbon；It weighs
0.2849gC12H28O460mL absolute ethyl alcohols are added in Ti, stir 10 minutes, add 1.35g columbium pentachloride powder (NbCl5), it stirs
It mixes 15 minutes, until being completely dissolved.Solution is moved into polytetrafluoroethylene (PTFE) autoclave after mixing, and is put into bacterial fibers
The holder carbon that biscuit firing obtains seals autoclave as growth substrate, the hydro-thermal reaction 24 hours under conditions of 200 DEG C.Instead
It answers postcooling to 25 DEG C of room temperature, solution is outwelled into taking-up sample, and after drying is washed with deionized, cooled to room temperature,
Obtain bacteria cellulose/Ti2Nb10O29Predecessor.Finally by it in tube furnace under argon gas atmosphere 800 DEG C be sintered 2 hours, obtain
Bacteria cellulose/Ti2Nb10O29Target product (i.e. bacteria cellulose supported titanium niobium O compoiste material).
Bacteria cellulose/Ti obtained in embodiment 12Nb10O29Target product (writes a Chinese character in simplified form BC/Ti2Nb10O29) XRD diagram such as
Shown in Fig. 1.
Embodiment 2
The bacteria cellulose (purchase is in Guilin Qi Hong Science and Technology Ltd.s) of freezing is lyophilized with freeze drier, and
It is put into tube furnace, is sintered 1 hour under conditions of 700 DEG C, obtains bacterial cellulose stent carbon；It weighs
0.2849gC12H28O460mL absolute ethyl alcohols are added in Ti, stir 10 minutes, add 1.35g columbium pentachloride powder (NbCl5), it stirs
It mixes 15 minutes, until being completely dissolved.Solution is moved into polytetrafluoroethylene (PTFE) autoclave after mixing, and is put into bacterial fibers
The holder carbon that biscuit firing obtains seals autoclave as growth substrate, the hydro-thermal reaction 10 hours under conditions of 160 DEG C.Instead
It answers postcooling to room temperature, solution is outwelled into taking-up sample, and after drying is washed with deionized, cooled to room temperature obtains
Bacteria cellulose/Ti2Nb10O29Predecessor.Finally by it in tube furnace under argon gas atmosphere 750 DEG C be sintered 2 hours, obtain bacterium
Cellulose/Ti2Nb10O29Target product (i.e. bacteria cellulose supported titanium niobium O compoiste material).
Bacteria cellulose/Ti obtained in embodiment 22Nb10O29The scanning electron microscope (SEM) photograph of target product is as shown in Fig. 2, have
Larger specific surface area loads Ti on bacteria cellulose2Nb10O29Nano particle, Ti2Nb10O29Nano particle average diameter is about
For 10-40nm.
Embodiment 3
The bacteria cellulose (purchase is in Guilin Qi Hong Science and Technology Ltd.s) of freezing is lyophilized with freeze drier, and
It is put into tube furnace, is sintered 1 hour under conditions of 700 DEG C, obtains bacterial cellulose stent carbon；It weighs
0.2849gC12H28O460mL absolute ethyl alcohols are added in Ti, stir 10 minutes, add 1.35g columbium pentachloride powder (NbCl5), it stirs
It mixes 15 minutes, until being completely dissolved.Solution is moved into polytetrafluoroethylene (PTFE) autoclave after mixing, and is put into bacterial fibers
The holder carbon that biscuit firing obtains seals autoclave as growth substrate, the hydro-thermal reaction 15 hours under conditions of 180 DEG C.Instead
It answers postcooling to room temperature, solution is outwelled into taking-up sample, and after drying is washed with deionized, cooled to room temperature obtains
Bacteria cellulose/Ti2Nb10O29Predecessor.Finally by it in tube furnace under argon gas atmosphere 850 DEG C be sintered 1 hour, obtain bacterium
Cellulose/Ti2Nb10O29Target product (i.e. bacteria cellulose supported titanium niobium O compoiste material).
Bacteria cellulose/Ti obtained in embodiment 32Nb10O29The transmission electron microscope picture of target product is as shown in Figure 3.
Performance test
By bacteria cellulose/Ti made of above-described embodiment 1~32Nb10O29Material is assembled into button cell.By 75:15:
Bacteria cellulose/Ti that 10 mass ratio prepares experiment2Nb10O29Material activity substance and binder Kynoar
(PVDF1300) it is uniformly mixed with conductive agent acetylene black, is diluted to suitable viscosity with N-Methyl pyrrolidone (NMP) and is coated in
On the copper foil of LITHIUM BATTERY, it is subsequently placed in vacuum drying chamber and is dried in vacuo 12 hours at 120 DEG C.Metal lithium sheet is made to electrode,
Electrolyte selects LiPF6, it is 1 to be dissolved in mass ratio:1:1 ethylene carbonate (DC) and dimethyl carbonate (DMC) and
In the mixture of ethylene carbonate (EC), a concentration of 1molL-1.Button cell is assembled into glove box.In blue electric tester
Battery performance is tested respectively.Charging/discharging voltage be 1.0~2.5V, in 25 ± 1 DEG C of environment cycle measure bacteria cellulose/
Ti2Nb10O29Reversible charging and discharging capacity, charge-discharge performance and the high-rate characteristics of material.
The performance test results are as follows：
Bacteria cellulose/Ti of embodiment 1, embodiment 2 and embodiment 32Nb10O29Material is in 5C (1C=396mAh g-1)
Specific capacitance of discharging under current density is respectively 308mAh g-1、285mAh g-1With 297mAh g-1, and the ratio that discharges after 500 cycles
Capacity retention is up to 90% or more.As it can be seen that bacteria cellulose/Ti obtained above2Nb10O29Material charge/discharge capacity is high, cycle
Stability is good.
This is bacteria cellulose/Ti prepared by the present invention2Nb10O29Electrode material has larger specific surface area, bacterium fine
Ti is loaded on dimension element2Nb10O29Nano particle can increase the contact area of electrolyte and motor, it is more effectively active to provide bigger
Response area, meanwhile, electronics conduction velocity is accelerated, chemical property is improved.Therefore, bacteria cellulose of the present invention/
Ti2Nb10O29Material has the characteristics that high circulation service life, high-energy and power density, in mobile communication, electric vehicle, solar energy hair
The fields such as electricity and aerospace have broad application prospects.
Claims (8)
1. a kind of preparation method of bacteria cellulose supported titanium niobium O compoiste material, which is characterized in that include the following steps：
(1) bacteria cellulose is lyophilized with freeze drier, is sintered, obtains bacterial cellulose stent carbon；
(2) columbium pentachloride and isopropyl titanate are dissolved in ethanol solution, are uniformly mixed to form mixed solution, be added to
In reaction kettle, and bacterial cellulose stent carbon made from step (1) is added and seals and heats as growth substrate, it, will after cooling
Product washs drying, obtains target predecessor, target predecessor is sintered, obtain bacteria cellulose supported titanium niobium oxygen composite wood
Material.
2. the preparation method of bacteria cellulose supported titanium niobium O compoiste material according to claim 1, which is characterized in that step
Suddenly in (1), the sintering specifically includes：It is put into tube furnace, is sintered 1-2 hours under the conditions of 600-800 DEG C.
3. the preparation method of bacteria cellulose supported titanium niobium O compoiste material according to claim 1, which is characterized in that step
Suddenly in (2), in molar ratio the 5 of the columbium pentachloride and isopropyl titanate：0.8~1.2.
4. the preparation method of bacteria cellulose supported titanium niobium O compoiste material according to claim 1, which is characterized in that step
Suddenly in (2), it is 150 DEG C -200 DEG C that the heating, which uses hydro-thermal method, hydrothermal temperature, and the hydro-thermal time is 6-24 hours.
5. the preparation method of bacteria cellulose supported titanium niobium O compoiste material according to claim 4, which is characterized in that water
Hot temperature is 160 DEG C -200 DEG C, and the hydro-thermal time is 10-24 hours.
6. the preparation method of bacteria cellulose supported titanium niobium O compoiste material according to claim 1, which is characterized in that step
Suddenly in (2), the condition of target predecessor sintering is：It is sintered 1-2 hours under the conditions of 600-900 DEG C in tube furnace.
7. the bacteria cellulose supported titanium niobium O compoiste material prepared according to claim 1~6 any one of them preparation method.
8. bacteria cellulose supported titanium niobium O compoiste material according to claim 7 is as lithium ion battery negative material
Using.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109888245A (en) * | 2019-03-21 | 2019-06-14 | 浙江大学 | Titanium niobium oxygen/carbon composite and its preparation method and application that Lacking oxygen and carbon coating are adjusted |
| CN109950489A (en) * | 2019-03-21 | 2019-06-28 | 浙江大学 | Carbon cloth/carbon fiber array supported titanium niobium O compoiste material and its preparation method and application |
| CN114203952A (en) * | 2021-11-24 | 2022-03-18 | 江苏大学 | Sodium ion battery cathode, preparation method and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109888245A (en) * | 2019-03-21 | 2019-06-14 | 浙江大学 | Titanium niobium oxygen/carbon composite and its preparation method and application that Lacking oxygen and carbon coating are adjusted |
| CN109950489A (en) * | 2019-03-21 | 2019-06-28 | 浙江大学 | Carbon cloth/carbon fiber array supported titanium niobium O compoiste material and its preparation method and application |
| CN109888245B (en) * | 2019-03-21 | 2021-01-15 | 浙江大学 | Titanium niobium oxygen/carbon composite material with oxygen vacancy and carbon coating adjustment and preparation method and application thereof |
| CN114203952A (en) * | 2021-11-24 | 2022-03-18 | 江苏大学 | Sodium ion battery cathode, preparation method and application |
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