CN108630916B - Bacterial cellulose-loaded titanium niobium oxygen composite material and preparation method and application thereof - Google Patents
Bacterial cellulose-loaded titanium niobium oxygen composite material and preparation method and application thereof Download PDFInfo
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- CN108630916B CN108630916B CN201810263493.6A CN201810263493A CN108630916B CN 108630916 B CN108630916 B CN 108630916B CN 201810263493 A CN201810263493 A CN 201810263493A CN 108630916 B CN108630916 B CN 108630916B
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- H01M4/00—Electrodes
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- 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
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- 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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- 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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Abstract
The invention discloses a bacterial cellulose-loaded titanium niobium oxygen composite material, a preparation method thereof and application of the composite material as a lithium ion battery cathode material2Nb10O29The nano particles can increase the contact area of the electrolyte and the motor, provide a larger and more effective active reaction area, accelerate the electron conduction rate and improve the electrochemical performance. The invention prepares bacterial cellulose/Ti by sintering through a high-temperature sintering method to generate bacterial cellulose bracket carbon, taking the bacterial cellulose bracket carbon as a carrier and preparing the bacterial cellulose/Ti through a hydrothermal method and the high-temperature sintering method2Nb10O29An electrode material. The bacterial cellulose/Ti of the invention2Nb10O29The material has the characteristics of long cycle life, high energy and power density, and has wide application prospects in the fields of mobile communication, electric automobiles, solar power generation, aerospace and the like.
Description
Technical Field
The invention relates to the technical field of lithium ion battery cathode materials, in particular to a bacterial cellulose loaded titanium niobium oxygen (Ti)2Nb10O29) A composite material, a preparation method thereof and application of the composite material as a lithium ion battery cathode material.
Background
The rapid expansion of the consumer market for electronic products has greatly increased the demand for high performance, highly stable battery materials. The lithium-storage material of titanium niobate has a good lithium-storage structure, thereby determining that the material has good electrochemical performance. The negative electrode materials mainly used at present comprise graphite, lithium titanate and the like, but the graphite has a serious problem that the graphite is easy to form a Solid Electrolyte Interface (SEI) film due to a low voltage platform to cause lithium dendrites and possibly cause explosion, and the lithium titanate cannot generate the SEI film due to a high voltage platform but has a low theoretical capacity (175mAh g)-1) So that the energy storage performance is not ideal. Common to theseCompared with the negative electrode material, the titanium niobate compound has larger theoretical capacity and relative safety stability. However, the titanium niobate compound also has some disadvantages, such as low electronic conductivity, small lithium ion diffusion coefficient, and the like.
The bacterial cellulose bracket carbon is used as a substrate, and titanium niobium oxygen (Ti) is loaded and grown on the substrate2Nb10O29) The method can effectively improve the electron conduction rate and the specific surface area of the titanium niobium oxygen particles, thereby improving the electrochemical performance of the titanium niobium oxygen particles. Bacterial cellulose/Ti2Nb10O29Can be used as the cathode material of the lithium ion battery with high energy density, high power density and high safety and stability.
Disclosure of Invention
The invention aims to provide a bacterial cellulose loaded titanium niobium oxide (Ti) for the negative electrode material of a lithium titanate lithium ion battery with low safety performance and low theoretical capacity2Nb10O29) Composite material, preparation method thereof and application of composite material as lithium ion battery cathode material, and bacterial cellulose/Ti2Nb10O29The electrode material has high power density, high energy density and high safety and stability.
Bacterial cellulose loaded titanium niobium oxygen (Ti)2Nb10O29) The preparation method of the composite material comprises the following steps:
(1) freeze-drying the bacterial cellulose by using a freeze dryer, and sintering to obtain bacterial cellulose scaffold carbon;
(2) dissolving niobium pentachloride and isopropyl titanate in an absolute ethyl alcohol solution, stirring and mixing uniformly to form a mixed solution, adding the mixed solution into a reaction kettle, adding the bacterial cellulose scaffold carbon prepared in the step (1) as a growth substrate, sealing and heating, cooling, washing and drying a product to obtain a target precursor, and sintering the target precursor to obtain the bacterial cellulose loaded titanium niobium oxide (Ti)2Nb10O29) A composite material.
The following are preferred technical schemes of the invention:
in the step (1), the sintering specifically comprises: placing the mixture into a tube furnace, and sintering the mixture for 1 to 2 hours at the temperature of 600 ℃ and 800 ℃. Further preferably, the sintering specifically comprises: placing the mixture into a tube furnace, and sintering the mixture for 1 to 2 hours at the temperature of 700 ℃ and 800 ℃.
In the step (2), the molar ratio of the niobium pentachloride to the isopropyl titanate is 5: 0.8-1.2, wherein the molar ratio of the niobium pentachloride to the isopropyl titanate is 5:1,
the reaction kettle is a polytetrafluoroethylene high-pressure kettle;
the heating adopts a hydrothermal method, the hydrothermal temperature is 150-200 ℃, the hydrothermal time is 6-24 hours, and further optimization is carried out, the hydrothermal temperature is 160-200 ℃, and the hydrothermal time is 10-24 hours.
The sintering conditions of the target precursor are as follows: sintering for 1-2 hours in a tube furnace at the temperature of 600-900 ℃.
The bacterial cellulose load titanium niobium oxygen composite material (namely bacterial cellulose/Ti) prepared by the invention2Nb10O29Material) has a high theoretical capacity (396mAh g)-1) Better electron conductivity and higher safety stability, Ti2Nb10O29The average diameter of the nanoparticles is about 10-40 nm. The bacterial cellulose/Ti2Nb10O29The material is used as a new titanium niobium oxygen composite material. In particular as a negative electrode material of a lithium ion battery.
Compared with the prior art, the invention has the following advantages:
the method prepares the bacterial cellulose bracket carbon substrate by a high-temperature sintering method, and then prepares the bacterial cellulose/Ti by a simple hydrothermal method2Nb10O29A precursor. Finally, obtaining bacterial cellulose/Ti through high-temperature sintering2Nb10O29And (4) obtaining a target product. The preparation method is simple and convenient, and is easy to control.
Bacterial cellulose/Ti prepared by the invention2Nb10O29The electrode material has larger specific surface area, and Ti is loaded on the bacterial cellulose2Nb10O29Nanoparticles capable of increasing contact surface between electrolyte and motorThe product provides a larger and more effective active reaction area, and simultaneously, the electron conduction rate is accelerated, and the electrochemical performance is improved. The invention overcomes the defects of SEI film formation and reaction kinetics, thereby realizing high power discharge performance and simultaneously keeping high energy density, and forming the novel lithium ion battery cathode material with high power, high energy density and high safety and stability.
The bacterial cellulose loaded titanium niobium oxygen composite material has larger specific surface area, and Ti is loaded on the bacterial cellulose2Nb10O29The nano particles can increase the contact area of the electrolyte and the motor, provide a larger and more effective active reaction area, accelerate the electron conduction rate and improve the electrochemical performance. Sintering for 1-2 hours by a high-temperature sintering method to generate bacterial cellulose scaffold carbon, and preparing bacterial cellulose/Ti by a hydrothermal method and a high-temperature sintering method by using the bacterial cellulose scaffold carbon as a carrier2Nb10O29An electrode material. The bacterial cellulose/Ti of the invention2Nb10O29The material has the characteristics of long cycle life, high energy and power density, and has wide application prospects in the fields of mobile communication, electric automobiles, solar power generation, aerospace and the like.
Drawings
FIG. 1 shows the bacterial cellulose/Ti prepared in example 12Nb10O29XRD pattern of the target product.
FIG. 2 shows the bacterial cellulose/Ti prepared in example 22Nb10O29Scanning electron microscope images of the target product.
FIG. 3 shows the bacterial cellulose/Ti prepared in example 32Nb10O29Transmission electron microscopy images of the target product.
Detailed Description
The present invention will be described in detail with reference to examples, but the present invention is not limited thereto.
Example 1
Freeze drying frozen bacterial cellulose (purchased from Guilin Qihong science and technology Co., Ltd.) with a freeze dryer, and placing into a tube furnace, and drying at 800 deg.CSintering for 2 hours under the condition of a workpiece to obtain bacterial cellulose bracket carbon; weighing 0.2849gC12H28O4Ti, 60mL of absolute ethanol was added, the mixture was stirred for 10 minutes, and 1.35g of niobium pentachloride powder (NbCl)5) And stirred for 15 minutes until completely dissolved. After being mixed evenly, the solution is transferred into a polytetrafluoroethylene high-pressure reaction kettle, and bracket carbon obtained by sintering bacterial cellulose is put into the kettle to be used as a growth substrate, the high-pressure kettle is sealed, and the hydrothermal reaction is carried out for 24 hours at the temperature of 200 ℃. Cooling to room temperature of 25 ℃ after reaction, pouring the solution, taking out a sample, washing with deionized water, drying, and naturally cooling to room temperature to obtain bacterial cellulose/Ti2Nb10O29A precursor. Finally, sintering the mixture for 2 hours at 800 ℃ in a tube furnace under the argon atmosphere to obtain the bacterial cellulose/Ti2Nb10O29And (3) a target product (namely the bacterial cellulose-loaded titanium niobium oxygen composite material).
Bacterial cellulose/Ti prepared in example 12Nb10O29Target product (abbreviated as BC/Ti)2Nb10O29) The XRD pattern of (A) is shown in FIG. 1.
Example 2
Freeze-drying frozen bacterial cellulose (purchased from Guilin Qihong science and technology Co., Ltd.) by using a freeze dryer, putting the freeze-dried bacterial cellulose into a tube furnace, and sintering the freeze-dried bacterial cellulose at 700 ℃ for 1 hour to obtain bacterial cellulose scaffold carbon; weighing 0.2849gC12H28O4Ti, 60mL of absolute ethanol was added, the mixture was stirred for 10 minutes, and 1.35g of niobium pentachloride powder (NbCl)5) And stirred for 15 minutes until completely dissolved. After being mixed evenly, the solution is transferred into a polytetrafluoroethylene high-pressure reaction kettle, bracket carbon obtained by sintering bacterial cellulose is put into the kettle to be used as a growth substrate, the high-pressure kettle is sealed, and the hydrothermal reaction is carried out for 10 hours at the temperature of 160 ℃. Cooling to room temperature after reaction, pouring the solution, taking out a sample, washing with deionized water, drying, and naturally cooling to room temperature to obtain bacterial cellulose/Ti2Nb10O29A precursor. Finally, sintering the mixture for 2 hours at 750 ℃ in a tube furnace under the argon atmosphere to obtain the bacterial cellulose/Ti2Nb10O29Target product (i.e. fines)The bacterial cellulose loads titanium niobium oxygen composite material).
Bacterial cellulose/Ti prepared in example 22Nb10O29The scanning electron microscope image of the target product is shown in FIG. 2, and the target product has a large specific surface area and Ti is loaded on the bacterial cellulose2Nb10O29Nanoparticles of Ti2Nb10O29The average diameter of the nanoparticles is about 10-40 nm.
Example 3
Freeze-drying frozen bacterial cellulose (purchased from Guilin Qihong science and technology Co., Ltd.) by using a freeze dryer, putting the freeze-dried bacterial cellulose into a tube furnace, and sintering the freeze-dried bacterial cellulose at 700 ℃ for 1 hour to obtain bacterial cellulose scaffold carbon; weighing 0.2849gC12H28O4Ti, 60mL of absolute ethanol was added, the mixture was stirred for 10 minutes, and 1.35g of niobium pentachloride powder (NbCl)5) And stirred for 15 minutes until completely dissolved. After uniform mixing, the solution is transferred into a polytetrafluoroethylene high-pressure reaction kettle, and bracket carbon obtained by sintering bacterial cellulose is put into the kettle to be used as a growth substrate, the high-pressure kettle is sealed, and hydrothermal reaction is carried out for 15 hours at the temperature of 180 ℃. Cooling to room temperature after reaction, pouring the solution, taking out a sample, washing with deionized water, drying, and naturally cooling to room temperature to obtain bacterial cellulose/Ti2Nb10O29A precursor. Finally, sintering the mixture for 1 hour at 850 ℃ in a tube furnace under the argon atmosphere to obtain the bacterial cellulose/Ti2Nb10O29And (3) a target product (namely the bacterial cellulose-loaded titanium niobium oxygen composite material).
Bacterial cellulose/Ti prepared in example 32Nb10O29The transmission electron micrograph of the target product is shown in FIG. 3.
Performance testing
The bacterial cellulose/Ti prepared in the above examples 1 to 32Nb10O29The materials are assembled into a button cell. The bacterial cellulose/Ti prepared by the experiment is mixed according to the mass ratio of 75:15:102Nb10O29The active substance of the material is uniformly mixed with a binder polyvinylidene fluoride (PVDF1300) and a conductive agent acetylene black, and is diluted by N-methyl pyrrolidone (NMP)Coated on a battery grade copper foil to a suitable viscosity, and then vacuum-dried in a vacuum drying oven at 120 ℃ for 12 hours. The metal lithium sheet is used as a counter electrode, and the electrolyte is selected from LiPF6The mixture was dissolved in a 1:1:1 mass ratio mixture of ethylene carbonate (DC), dimethyl carbonate (DMC) and Ethylene Carbonate (EC) at a concentration of 1mol L-1. And assembling the button cell in the glove box. The performance of the cells was tested separately in a blue tester. The charging and discharging voltage is 1.0-2.5V, and the bacterial cellulose/Ti is measured in a circulating manner in the environment of 25 +/-1 DEG C2Nb10O29The material has reversible charge-discharge specific capacity, charge-discharge cycle performance and high rate characteristic.
The performance test results are as follows:
bacterial cellulose/Ti of examples 1, 2 and 32Nb10O29The material is 5C (1C 396mAh g)-1) The discharge specific capacitance under the current density is 308mAh g respectively-1、285mAh g-1And 297mAh g-1And the discharge specific capacitance retention rate after 500 cycles reaches more than 90%. Thus, the bacterial cellulose/Ti prepared by the method2Nb10O29The material has high charge and discharge capacity and good cycle stability.
It is the bacterial cellulose/Ti prepared by the invention2Nb10O29The electrode material has larger specific surface area, and Ti is loaded on the bacterial cellulose2Nb10O29The nano particles can increase the contact area of the electrolyte and the motor, provide a larger and more effective active reaction area, accelerate the electron conduction rate and improve the electrochemical performance. Thus, the bacterial cellulose/Ti of the present invention2Nb10O29The material has the characteristics of long cycle life, high energy and power density, and has wide application prospects in the fields of mobile communication, electric automobiles, solar power generation, aerospace and the like.
Claims (4)
1. The preparation method of the bacterial cellulose-loaded titanium niobium oxygen composite material is characterized by comprising the following steps of:
(1) freeze-drying the bacterial cellulose by using a freeze dryer, and sintering to obtain bacterial cellulose scaffold carbon;
the sintering specifically comprises: placing the mixture into a tube furnace, and sintering the mixture for 1 to 2 hours at the temperature of 600-;
(2) dissolving niobium pentachloride and isopropyl titanate in an absolute ethanol solution, stirring and mixing uniformly to form a mixed solution, adding the mixed solution into a reaction kettle, adding the bacterial cellulose scaffold carbon prepared in the step (1) as a growth substrate, sealing and heating, cooling, washing and drying a product to obtain a target precursor, and sintering the target precursor to obtain the bacterial cellulose loaded titanium niobium oxide composite material;
the mol ratio of the niobium pentachloride to the isopropyl titanate is 5: 0.8 to 1.2;
the heating adopts a hydrothermal method, the hydrothermal temperature is 150-200 ℃, and the hydrothermal time is 6-24 hours;
the sintering conditions of the target precursor are as follows: sintering for 1-2 hours in a tube furnace at the temperature of 600-900 ℃.
2. The preparation method of the bacterial cellulose-supported titanium niobium oxygen composite material as claimed in claim 1, wherein in the step (2), the hydrothermal temperature is 160-200 ℃ and the hydrothermal time is 10-24 hours.
3. The bacterial cellulose-supported titanium niobium oxide composite material prepared by the preparation method according to claim 1 or 2.
4. The application of the bacterial cellulose-loaded titanium niobium oxygen composite material as a negative electrode material of a lithium ion battery according to claim 3.
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| 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 |
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| CN104538207A (en) * | 2014-12-16 | 2015-04-22 | 南京航空航天大学 | Method for preparing titanium niobate and carbon nanotube composite material and lithium ion capacitor with material as negative electrode |
| CN104993111A (en) * | 2015-06-12 | 2015-10-21 | 中南大学 | Manganese dioxide/nitrating carbon fiber cathode composite material for sodium-ion battery and preparing method thereof |
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