CN104752707A - Titanium dioxide (B) negative electrode material and preparation method thereof - Google Patents
Titanium dioxide (B) negative electrode material and preparation method thereof Download PDFInfo
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- CN104752707A CN104752707A CN201510095116.2A CN201510095116A CN104752707A CN 104752707 A CN104752707 A CN 104752707A CN 201510095116 A CN201510095116 A CN 201510095116A CN 104752707 A CN104752707 A CN 104752707A
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
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- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The invention discloses a titanium dioxide (B) negative electrode material. The titanium dioxide (B) negative electrode material is prepared from the following raw materials in parts by weight: 200 to 350 parts of titanium dioxide, 150 to 200 parts of graphite, 155 to 175 parts of lithium source, 15 to 25 parts of doping agent, 40 to 45 parts of carbon source and 50 to 65 parts of ion liquid. The titanium dioxide (B) negative electrode material is prepared in steps of dispersing, grinding, drying, wrapping and sintering. By adopting the formula and the preparation method, the conducting property and mechanical property of the prepared negative electrode material can be greatly improved; due to the improved conducting property and the improved mechanical property, when the titanium dioxide (B) negative electrode material is used as a lithium ion battery negative electrode material, the cycling property, the rate capability charging-discharging property and the primary charging-discharging efficiency can be greatly improved; moreover, the preparation method is simple in process, the production cost is relatively low, and the preparation process is simple and easy.
Description
Technical field
The present invention relates to negative material art, refer in particular to a kind of titanium dioxide (B) negative material and preparation method thereof.
Background technology
Titanium dioxide has broad application prospects in fields such as photocatalysis, photocatalytic water, transducer, DSSC and lithium ion batteries due to it, has become the focus of Material Field research.Common titanium dioxide mainly comprises four kinds of crystalline phases: sharp titanium phase, Rutile Type, brookite and TiO2 (B) phase.In all crystalline phases, TiO2 (B) type titanium dioxide belongs to monoclinic system, and structure is the most loose, has larger interlamellar spacing and less density, be conducive to the embedding of lithium ion and remove, the application thus in lithium ion battery has potential superior function.
To a great extent, the direction of growth of the size of TiO2 (B), pattern and crystal all can affect its application in lithium ion battery.Such as, nano-scale and crossover network can shorten the transmission range of lithium ion and electronics, and undersized TiO2 (B) can expand the contact area of electrode and electrolyte, reduce current density, reduce the internal resistance of cell, improve battery performance.
But, the problems such as current titanium dioxide (B) negative material ubiquity complex process, cycle performance and rate charge-discharge performance are bad, therefore, develop that a kind of technique is simple, technical barrier that cycle performance and rate charge-discharge performance is good, first charge-discharge efficiency is high, preparation cost is cheap titanium dioxide (B) cathode material preparation method are affiliated field.
Summary of the invention
In view of this, the present invention is directed to the disappearance of prior art existence, its main purpose is to provide a kind of titanium dioxide (B) negative material and preparation method thereof, and it effectively can solve the problems such as existing titanium dioxide (B) complex process, cycle performance and rate charge-discharge performance be bad.
For achieving the above object, the present invention adopts following technical scheme:
A kind of titanium dioxide (B) negative material, is made up of the raw material of following weight portion: titanium dioxide 200 ~ 350, graphite 150 ~ 200, lithium source 155 ~ 175, dopant 15 ~ 25, carbon source 40 ~ 45, ionic liquid 50 ~ 65.
As a kind of preferred version, described graphite is at least one in native graphite, Delanium.
As a kind of preferred version, described ionic liquid is at least one in the two fluoroform sulfimide salt of N-methyl butyl pyrrolidines, the two fluoroform sulfimide salt of N-methyl butyl piperidines, the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole, 1-ethyl-3-methylimidazole tetrafluoroborate, the two fluoroform sulfimide salt of trimethyl third ammonium and the two fluoroform sulfimide salt of 1-hexyl-3-methylimidazole.
A kind of preparation method of titanium dioxide (B) negative material: include following steps:
(1) disperse: titanium dioxide, graphite, lithium source, dopant, carbon source are scattered in solvent, and ultrasonic 2 ~ 3h, obtains mixed slurry, and solvent is ethanol;
(2) grind: used by mixed slurry sand mill to grind 2 ~ 3 h, grinding rate is 1500 ~ 2500 r/min;
(3) dry: use spray dryer to be dried to powder ground mixed slurry, spraying dry inlet temperature is 150 ~ 300 DEG C, and leaving air temp is 100 ~ 150 DEG C, constant flow pump degree of turning 50 ~ 100 r/min;
(4) wrap up: by the material of ionic liquid and step (3) gained, join in homogenizer, use rotating speed 500 ~ 5000 r/min to carry out dispersion 2 ~ 4h;
(5) sinter: the material of step (4) gained is placed in atmosphere protection stove and sinters, rise to 600 ~ 1000 DEG C with the heating rate of 12 ~ 25 DEG C/min and be incubated 10 ~ 18 hours.
As a kind of preferred version, the protective atmosphere used in described atmosphere protection stove is selected from least one in helium, nitrogen, argon gas, carbon dioxide.
The present invention compared with prior art has obvious advantage and beneficial effect, specifically, as shown from the above technical solution:
By adopting formula of the present invention and preparation method, the electric conductivity of the negative material prepared and mechanical performance are greatly improved, due to the lifting of electric conductivity and mechanical performance, during as lithium ion battery negative material, cycle performance and rate charge-discharge performance, first charge-discharge efficiency are all greatly improved; Further, preparation method's technique of the present invention is simple, and production cost is lower, and preparation process is simple.
For more clearly setting forth architectural feature of the present invention and effect, below in conjunction with accompanying drawing and specific embodiment, the present invention is described in detail.
Accompanying drawing explanation
Fig. 1 is preparation flow schematic diagram of the present invention.
Embodiment
Please refer to shown in Fig. 1, that show a kind of titanium dioxide (B) the negative material machine preparation method of the present invention:
A kind of titanium dioxide (B) negative material, is made up of the raw material of following weight portion: titanium dioxide 200 ~ 350, graphite 150 ~ 200, lithium source 155 ~ 175, dopant 15 ~ 25, carbon source 40 ~ 45, ionic liquid 50 ~ 65.Described graphite is at least one in native graphite, Delanium.Described ionic liquid is at least one in the two fluoroform sulfimide salt of N-methyl butyl pyrrolidines, the two fluoroform sulfimide salt of N-methyl butyl piperidines, the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole, 1-ethyl-3-methylimidazole tetrafluoroborate, the two fluoroform sulfimide salt of trimethyl third ammonium and the two fluoroform sulfimide salt of 1-hexyl-3-methylimidazole.
A kind of preparation method of titanium dioxide (B) negative material, includes following steps:
(1) disperse: titanium dioxide, graphite, lithium source, dopant, carbon source are scattered in solvent, and ultrasonic 2 ~ 3h, obtains mixed slurry, and solvent is ethanol;
(2) grind: used by mixed slurry sand mill to grind 2 ~ 3 h, grinding rate is 1500 ~ 2500 r/min;
(3) dry: use spray dryer to be dried to powder ground mixed slurry, spraying dry inlet temperature is 150 ~ 300 DEG C, and leaving air temp is 100 ~ 150 DEG C, constant flow pump degree of turning 50 ~ 100 r/min;
(4) wrap up: by the material of ionic liquid and step (3) gained, join in homogenizer, use rotating speed 500 ~ 5000 r/min to carry out dispersion 2 ~ 4h;
(5) sinter: the material of step (4) gained is placed in atmosphere protection stove and sinters, rise to 600 ~ 1000 DEG C with the heating rate of 12 ~ 25 DEG C/min and be incubated 10 ~ 18 hours.The protective atmosphere used in described atmosphere protection stove is selected from least one in helium, nitrogen, argon gas, carbon dioxide.
The present invention will be described to use specific embodiment and comparative example below.
Embodiment 1
A kind of titanium dioxide (B) negative material, is made up of the raw material of following weight portion: titanium dioxide 200, graphite 150, lithium source 155, dopant 15, carbon source 40, ionic liquid 50.Described graphite is native graphite.Described ionic liquid is the two fluoroform sulfimide salt of N-methyl butyl pyrrolidines.
A kind of preparation method of titanium dioxide (B) negative material, includes following steps:
(1) disperse: titanium dioxide, graphite, lithium source, dopant, carbon source are scattered in solvent, and ultrasonic 2h, obtains mixed slurry, and solvent is ethanol;
(2) grind: used by mixed slurry sand mill to grind 2 h, grinding rate is 1500r/min;
(3) dry: use spray dryer to be dried to powder ground mixed slurry, spraying dry inlet temperature is 150 DEG C, and leaving air temp is 100 DEG C, constant flow pump degree of turning 50r/min;
(4) wrap up: by the material of ionic liquid and step (3) gained, join in homogenizer, use rotating speed 500 r/min to carry out dispersion 2h;
(5) sinter: the material of step (4) gained is placed in atmosphere protection stove and sinters, rise to 600 DEG C with the heating rate of 12 DEG C/min and be incubated 10 hours.The protective atmosphere used in described atmosphere protection stove is selected from helium.
Embodiment 2
A kind of titanium dioxide (B) negative material, is made up of the raw material of following weight portion: titanium dioxide 350, graphite 200, lithium source 175, dopant 25, carbon source 45, ionic liquid 65.Described graphite is Delanium.Described ionic liquid is the two fluoroform sulfimide salt of N-methyl butyl piperidines.
A kind of preparation method of titanium dioxide (B) negative material, includes following steps:
(1) disperse: titanium dioxide, graphite, lithium source, dopant, carbon source are scattered in solvent, and ultrasonic 3h, obtains mixed slurry, and solvent is ethanol;
(2) grind: used by mixed slurry sand mill to grind 3 h, grinding rate is 2500 r/min;
(3) dry: use spray dryer to be dried to powder ground mixed slurry, spraying dry inlet temperature is 300 DEG C, and leaving air temp is 150 DEG C, constant flow pump degree of turning 100 r/min;
(4) wrap up: by the material of ionic liquid and step (3) gained, join in homogenizer, use rotating speed 5000 r/min to carry out dispersion 4h;
(5) sinter: the material of step (4) gained is placed in atmosphere protection stove and sinters, rise to 1000 DEG C with the heating rate of 25 DEG C/min and be incubated 18 hours.The protective atmosphere used in described atmosphere protection stove is selected from nitrogen.
Embodiment 3
A kind of titanium dioxide (B) negative material, is made up of the raw material of following weight portion: titanium dioxide 275, graphite 175, lithium source 165, dopant 20, carbon source 43, ionic liquid 57.Described graphite is native graphite and Delanium.Described ionic liquid is the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole.
A kind of preparation method of titanium dioxide (B) negative material, includes following steps:
(1) disperse: titanium dioxide, graphite, lithium source, dopant, carbon source are scattered in solvent, and ultrasonic 2.5h, obtains mixed slurry, and solvent is ethanol;
(2) grind: used by mixed slurry sand mill to grind 2.5 h, grinding rate is 2000 r/min;
(3) dry: use spray dryer to be dried to powder ground mixed slurry, spraying dry inlet temperature is 225 DEG C, and leaving air temp is 125 DEG C, constant flow pump degree of turning 75 r/min;
(4) wrap up: by the material of ionic liquid and step (3) gained, join in homogenizer, use rotating speed 2750 r/min to carry out dispersion 3.5h;
(5) sinter: the material of step (4) gained is placed in atmosphere protection stove and sinters, rise to 800 DEG C with the heating rate of 19 DEG C/min and be incubated 14 hours.The protective atmosphere used in described atmosphere protection stove is selected from argon gas.
Embodiment 4
A kind of titanium dioxide (B) negative material, is made up of the raw material of following weight portion: titanium dioxide 210, graphite 155, lithium source 168, dopant 17, carbon source 42, ionic liquid 53.Described graphite is native graphite.Described ionic liquid is 1-ethyl-3-methylimidazole tetrafluoroborate.
A kind of preparation method of titanium dioxide (B) negative material, includes following steps:
(1) disperse: titanium dioxide, graphite, lithium source, dopant, carbon source are scattered in solvent, and ultrasonic 2.2h, obtains mixed slurry, and solvent is ethanol;
(2) grind: used by mixed slurry sand mill to grind 2h, grinding rate is 1600 r/min;
(3) dry: use spray dryer to be dried to powder ground mixed slurry, spraying dry inlet temperature is 155 DEG C, and leaving air temp is 110 DEG C, constant flow pump degree of turning 60 r/min;
(4) wrap up: by the material of ionic liquid and step (3) gained, join in homogenizer, use rotating speed 600 r/min to carry out dispersion 2.4h;
(5) sinter: the material of step (4) gained is placed in atmosphere protection stove and sinters, rise to 700 DEG C with the heating rate of 13 DEG C/min and be incubated 11 hours.The protective atmosphere used in described atmosphere protection stove is selected from carbon dioxide.
Embodiment 5
A kind of titanium dioxide (B) negative material, is made up of the raw material of following weight portion: titanium dioxide 240, graphite 165, lithium source 160, dopant 18, carbon source 43, ionic liquid 52.Described graphite is Delanium.Described ionic liquid is the two fluoroform sulfimide salt of trimethyl third ammonium.
A kind of preparation method of titanium dioxide (B) negative material, includes following steps:
(1) disperse: titanium dioxide, graphite, lithium source, dopant, carbon source are scattered in solvent, and ultrasonic 2.3h, obtains mixed slurry, and solvent is ethanol;
(2) grind: used by mixed slurry sand mill to grind 2.5 h, grinding rate is 1900 r/min;
(3) dry: use spray dryer to be dried to powder ground mixed slurry, spraying dry inlet temperature is 210 DEG C, and leaving air temp is 130 DEG C, constant flow pump degree of turning 60 r/min;
(4) wrap up: by the material of ionic liquid and step (3) gained, join in homogenizer, use rotating speed 2000 r/min to carry out dispersion 3h;
(5) sinter: the material of step (4) gained is placed in atmosphere protection stove and sinters, rise to 800 DEG C with the heating rate of 18 DEG C/min and be incubated 14 hours.The protective atmosphere used in described atmosphere protection stove is selected from helium and nitrogen.
Embodiment 6
A kind of titanium dioxide (B) negative material, is made up of the raw material of following weight portion: titanium dioxide 300, graphite 180, lithium source 168, dopant 19, carbon source 43, ionic liquid 59.Described graphite is Delanium.Described ionic liquid is the two fluoroform sulfimide salt of 1-hexyl-3-methylimidazole.
A kind of preparation method of titanium dioxide (B) negative material, includes following steps:
(1) disperse: titanium dioxide, graphite, lithium source, dopant, carbon source are scattered in solvent, and ultrasonic 2.6h, obtains mixed slurry, and solvent is ethanol;
(2) grind: used by mixed slurry sand mill to grind 2.4h, grinding rate is 2100 r/min;
(3) dry: use spray dryer to be dried to powder ground mixed slurry, spraying dry inlet temperature is 240 DEG C, and leaving air temp is 140 DEG C, constant flow pump degree of turning 90 r/min;
(4) wrap up: by the material of ionic liquid and step (3) gained, join in homogenizer, use rotating speed 3000 r/min to carry out dispersion 3.5h;
(5) sinter: the material of step (4) gained is placed in atmosphere protection stove and sinters, rise to 900 DEG C with the heating rate of 22 DEG C/min and be incubated 13 hours.The protective atmosphere used in described atmosphere protection stove is selected from helium, nitrogen and argon gas.
Embodiment 7
A kind of titanium dioxide (B) negative material, is made up of the raw material of following weight portion: titanium dioxide 320, graphite 180, lithium source 170, dopant 22, carbon source 44, ionic liquid 63.Described graphite is native graphite and Delanium.Described ionic liquid is the two fluoroform sulfimide salt of N-methyl butyl pyrrolidines and the two fluoroform sulfimide salt of N-methyl butyl piperidines.
A kind of preparation method of titanium dioxide (B) negative material, includes following steps:
(1) disperse: titanium dioxide, graphite, lithium source, dopant, carbon source are scattered in solvent, and ultrasonic 2.8h, obtains mixed slurry, and solvent is ethanol;
(2) grind: used by mixed slurry sand mill to grind 2.9 h, grinding rate is 2400 r/min;
(3) dry: use spray dryer to be dried to powder ground mixed slurry, spraying dry inlet temperature is 280 DEG C, and leaving air temp is 140 DEG C, constant flow pump degree of turning 90 r/min;
(4) wrap up: by the material of ionic liquid and step (3) gained, join in homogenizer, use rotating speed 4500 r/min to carry out dispersion 3.5h;
(5) sinter: the material of step (4) gained is placed in atmosphere protection stove and sinters, rise to 1000 DEG C with the heating rate of 24 DEG C/min and be incubated 16 hours.The protective atmosphere used in described atmosphere protection stove is selected from helium, nitrogen, argon gas and carbon dioxide.
Embodiment 8
A kind of titanium dioxide (B) negative material, is made up of the raw material of following weight portion: titanium dioxide 345, graphite 195, lithium source 172, dopant 24, carbon source 44, ionic liquid 64.Described graphite is native graphite and Delanium.Described ionic liquid is the two fluoroform sulfimide salt of N-methyl butyl pyrrolidines, the two fluoroform sulfimide salt of N-methyl butyl piperidines, the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole, 1-ethyl-3-methylimidazole tetrafluoroborate, the two fluoroform sulfimide salt of trimethyl third ammonium and the two fluoroform sulfimide salt of 1-hexyl-3-methylimidazole.
A kind of preparation method of titanium dioxide (B) negative material, includes following steps:
(1) disperse: titanium dioxide, graphite, lithium source, dopant, carbon source are scattered in solvent, and ultrasonic 2.9h, obtains mixed slurry, and solvent is ethanol;
(2) grind: used by mixed slurry sand mill to grind 2.8 h, grinding rate is 2450 r/min;
(3) dry: use spray dryer to be dried to powder ground mixed slurry, spraying dry inlet temperature is 290 DEG C, and leaving air temp is 145 DEG C, constant flow pump degree of turning 95 r/min;
(4) wrap up: by the material of ionic liquid and step (3) gained, join in homogenizer, use rotating speed 4900 r/min to carry out dispersion 3.8h;
(5) sinter: the material of step (4) gained is placed in atmosphere protection stove and sinters, rise to 950 DEG C with the heating rate of 24 DEG C/min and be incubated 17 hours.The protective atmosphere used in described atmosphere protection stove is selected from helium, nitrogen, argon gas and carbon dioxide.
Comparative example 1
Use the common graphite that pitch obtains as clad material.
Comparative example 2
Use the common graphite that phenolic resins obtains as clad material.
Electrochemical property test is carried out to foregoing individual embodiments and comparative example below:
For detecting the performance of the lithium ion battery negative material of ionic liquid cladding titanium dioxide (B) negative material of the present invention, test by half-cell method of testing, negative material by above embodiment and comparative example: SBR (solid content 50%): CMC: Super-p=95.5: 2: 1.5: 1 (weight ratio), add appropriate amount of deionized water and reconcile into pulpous state, to coat on Copper Foil and within 12 hours, to make negative plate in vacuum drying chamber inner drying, electrolyte is 1M LiPF6/EC+DEC+DMC=1: 1: 1, microporous polypropylene membrane is barrier film, be lithium sheet to electrode, be assembled into battery.Carry out constant current charge-discharge experiment at LAND battery test system, charging/discharging voltage is limited in 0.01 ~ 3.0 V, and the discharge and recharge cabinet computerizedd control carries out collection and the control of data, and the data obtained are as shown in table 1 below.
Table 1 lists the negative material Performance comparision of different embodiment and comparative example.
As can be seen from Table 1, prepared titanium dioxide (B) negative material, has excellent volumetric properties, cycle performance and rate charge-discharge performance, first charge-discharge efficiency.
Below know-why of the present invention is described in conjunction with specific embodiments.These describe just in order to explain principle of the present invention, and can not be interpreted as limiting the scope of the invention by any way.Based on explanation herein, those skilled in the art does not need to pay performing creative labour can associate other embodiment of the present invention, and these modes all will fall within protection scope of the present invention.
Claims (5)
1. titanium dioxide (B) negative material, is characterized in that: be made up of the raw material of following weight portion: titanium dioxide 200 ~ 350, graphite 150 ~ 200, lithium source 155 ~ 175, dopant 15 ~ 25, carbon source 40 ~ 45, ionic liquid 50 ~ 65.
2. a kind of titanium dioxide (B) negative material according to claim 1, is characterized in that: described graphite is at least one in native graphite, Delanium.
3. a kind of titanium dioxide (B) negative material according to claim 1, is characterized in that: described ionic liquid is at least one in the two fluoroform sulfimide salt of N-methyl butyl pyrrolidines, the two fluoroform sulfimide salt of N-methyl butyl piperidines, the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole, 1-ethyl-3-methylimidazole tetrafluoroborate, the two fluoroform sulfimide salt of trimethyl third ammonium and the two fluoroform sulfimide salt of 1-hexyl-3-methylimidazole.
4. a preparation method for titanium dioxide (B) negative material, is characterized in that: include following steps:
(1) disperse: titanium dioxide, graphite, lithium source, dopant, carbon source are scattered in solvent, and ultrasonic 2 ~ 3h, obtains mixed slurry, and solvent is ethanol;
(2) grind: used by mixed slurry sand mill to grind 2 ~ 3 h, grinding rate is 1500 ~ 2500 r/min;
(3) dry: use spray dryer to be dried to powder ground mixed slurry, spraying dry inlet temperature is 150 ~ 300 DEG C, and leaving air temp is 100 ~ 150 DEG C, constant flow pump degree of turning 50 ~ 100 r/min;
(4) wrap up: by the material of ionic liquid and step (3) gained, join in homogenizer, use rotating speed 500 ~ 5000 r/min to carry out dispersion 2 ~ 4h;
(5) sinter: the material of step (4) gained is placed in atmosphere protection stove and sinters, rise to 600 ~ 1000 DEG C with the heating rate of 12 ~ 25 DEG C/min and be incubated 10 ~ 18 hours.
5. the preparation method of a kind of titanium dioxide (B) negative material according to claim 4, is characterized in that: the protective atmosphere used in described atmosphere protection stove is selected from least one in helium, nitrogen, argon gas, carbon dioxide.
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| CN113130884A (en) * | 2021-04-07 | 2021-07-16 | 福建大成新能源科技有限公司 | F-doped TiO2Preparation method and application of (E) -B |
| CN113130884B (en) * | 2021-04-07 | 2024-02-13 | 福建大成新能源科技有限公司 | F-doped TiO 2 Preparation method and application of-B |
| CN114039032A (en) * | 2021-11-08 | 2022-02-11 | 深圳市翔丰华科技股份有限公司 | Titanium dioxide (B) negative electrode material with improved performance and preparation method thereof |
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