CN113130884B - F-doped TiO 2 Preparation method and application of-B - Google Patents
F-doped TiO 2 Preparation method and application of-B Download PDFInfo
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- CN113130884B CN113130884B CN202110372579.4A CN202110372579A CN113130884B CN 113130884 B CN113130884 B CN 113130884B CN 202110372579 A CN202110372579 A CN 202110372579A CN 113130884 B CN113130884 B CN 113130884B
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- 229910010413 TiO 2 Inorganic materials 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- -1 tetrabutylammonium tetrafluoroborate Chemical compound 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000002033 PVDF binder Substances 0.000 claims description 5
- 239000006230 acetylene black Substances 0.000 claims description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 5
- 229910013870 LiPF 6 Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 239000011889 copper foil Substances 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 239000000463 material Substances 0.000 description 3
- 239000007773 negative electrode material Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
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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
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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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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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to F-doped TiO 2 -B process for the preparation thereof and use thereof in lithium ion batteries. Dissolving glycollic acid in water, adding tetrabutyl titanate, concentrated sulfuric acid and tetrabutylammonium tetrafluoroborate, stirring, washing, drying and calcining after the reaction of the high-pressure kettle is finished to obtain F-doped TiO 2 -B, the F-doped TiO 2 The negative electrode of the lithium battery has high specific capacity and cycle stability, and the specific capacity is stabilized at 184.5 mAh/g when the battery is charged and discharged for 250 circles at a larger current density of 1.675A/g.
Description
Technical Field
The invention relates to a lithium ion battery technology, in particular to an F-doped TiO 2 -B process for the preparation thereof and use thereof in lithium ion batteries.
Background
Since the last nineties of development of lithium ion batteries, lithium ion batteries have been widely used, but to obtain lithium ion battery negative electrode materials with good cycle performance, high specific capacity and good high-current charge and discharge performance have been the focus of research by scientists.
TiO 2 The material has been a hot spot for research in the field of materials because of wide application prospects in the fields of photocatalysis, lithium ion batteries, dye sensitized solar cells, photolytic water, sensors and the like. Wherein TiO is 2 The phase B is used as an embedded material, and has the advantages of safety, innocuity, abundant sources, good circulation stability and the like, and is paid attention to scientific researchers. TiO (titanium dioxide) 2 The phase B belongs to metastable phase, and the structure of the phase B has more open space channels, so that the phase B is favorable for the intercalation and deintercalation of lithium ions and becomes a hot spot for research in recent years. However, tiO 2 -B is used as a negative electrode material of a lithium ion battery, has low conductivity and is pure-phase TiO 2 And (3) the problem of poor cycle performance and the like often exists in the B, so that the lithium storage performance is seriously influenced.
Disclosure of Invention
Therefore, in view of the above problems, the present invention provides an F-doped TiO 2 -B process for the preparation thereof and use thereof in lithium ion batteries.
In order to achieve the above object, the technical scheme of the invention is to provide an F-doped TiO 2 -B, comprising the steps of:
step (1), 1-5 g of glycolic acid is selected to be fully dissolved in 30-40 ml of water;
sequentially adding tetrabutyl titanate, concentrated sulfuric acid and an F reagent into the aqueous solution of the glycollic acid prepared in the step (1), and fully stirring to obtain a solution containing F ions;
step (3), transferring the stirred solution into a 50 milliliter reaction kettle, and placing the reaction kettle in an oven for hydrothermal reaction;
washing the product obtained after the reaction with water for a plurality of times, and then putting the product into a vacuum oven for drying to obtain a sample;
calcining the dried sample at 400 ℃ for 1-3 hours in an air atmosphere to finally obtain F-doped TiO 2 -B。
The further improvement is that: and (2) weighing 0.5-2 ml of tetrabutyl titanate, 0.1-1 ml of concentrated sulfuric acid and 1-5 g of F reagent in the step (2), and sequentially adding the tetrabutyl titanate, the concentrated sulfuric acid and the F reagent into the aqueous solution of the glycollic acid prepared in the step (1).
The further improvement is that: and (3) the reagent F in the step (2) is tetrabutylammonium tetrafluoroborate.
The further improvement is that: and (3) transferring the stirred solution into a 50 ml reaction kettle, and placing the reaction kettle in an oven at 100-220 ℃ for hydrothermal reaction for 2-24 hours.
F-doped TiO 2 Application of preparation method of-B in lithium ion battery, F-doped TiO prepared by preparation method 2 Mixing and grinding B, polyvinylidene fluoride and acetylene black, uniformly coating on copper foil after grinding to serve as a negative electrode in a lithium ion battery, and comparingThe electrode and the counter electrode are both lithium metal, and the electrolyte is a 1M LiPF6 EC+DMC+EMC solution.
The further improvement is that: f-doped TiO (titanium dioxide) in mass ratio 2 -B: polyvinylidene fluoride: acetylene black=70: 20:10.
the further improvement is that: the 1M LiPF 6 Ec+dmc+emc solution in volume ratio, wherein EC: DMC: emc=1: 1:1.
the invention relates to F-doped TiO 2 The preparation method of the-B and the application of the-B in the lithium ion battery have the following beneficial effects:
the invention provides F-doped TiO 2 Preparation method of-B and application of-B in lithium ion battery, solving the problem of traditional TiO 2 The problem of lower conductivity when B is used as a negative electrode material of the lithium ion battery ensures the lithium storage performance, and the method has the advantages of simple process, low cost, low energy consumption, good reproducibility and excellent performance.
Drawings
FIG. 1 is an F-doped TiO 2 -X-ray diffraction pattern of B;
FIG. 2 is an F-doped TiO 2 -X-ray photoelectron spectroscopy of B;
FIG. 3 is an F-doped TiO 2 -B scanning electron microscopy images;
FIG. 4 is an F-doped TiO 2 Electrochemical performance diagram of B (current density 1.675A/g).
Detailed Description
The following describes the embodiments of the present invention further with reference to the drawings and examples. The following examples are only for more clearly illustrating the technical aspects of the present invention, and are not intended to limit the scope of the present invention.
Referring to FIGS. 1 to 4, an F-doped TiO 2 The preparation method of the-B is as follows: dissolving 1-5 g of glycolic acid in 30-40 ml of water, adding 0.5-2 ml of tetrabutyl titanate, 0.1-1 ml of concentrated sulfuric acid and 1-5 g of tetrabutyl ammonium tetrafluoroborate, stirring, transferring into a 50 ml reaction kettle, placing into a 100-200 ℃ oven for hydrothermal reaction, reacting for 2-24 hours, and washing the product obtained after the reaction with waterWashing for several times, drying, calcining the dried sample at 400 deg.C under air atmosphere for 1-3 hr to obtain F-doped TiO 2 -B。
F-doped TiO 2 Use of B in lithium ion batteries, i.e. F-doped TiO in mass ratio during the assembly of lithium ion batteries 2 -B: polyvinylidene fluoride: acetylene black=70: 20:10 are uniformly coated on copper foil to be used as a negative electrode after being mixed and ground, the reference electrode and the counter electrode are both made of metal lithium, and the electrolyte is 1M LiPF 6 Ec+dmc+emc (EC/DMC/emc=1/1/1 v/v).
The method adopts a one-step hydrothermal method and a subsequent calcination process to rapidly prepare the F-doped TiO 2 -B, applied in lithium ion battery anode material, the F doped TiO 2 The negative electrode of the lithium battery has high specific capacity and cycle stability, and the capacity is stable at 184.5 mAh/g when the battery is charged and discharged for 250 circles at a larger current density of 1.675A/g.
FIG. 1 is an F-doped TiO 2 X-ray diffraction pattern of B, from which it can be seen that all diffraction peaks can be attributed to TiO of monoclinic phase 2 B (JCPDS card number: 74-1940). In addition, no impurity peak was found from the diffraction pattern. This illustrates F-doped TiO prepared by the method of the present invention 2 -B is a pure phase TiO 2 -B。
FIG. 2 is an F-doped TiO 2 X-ray photoelectron spectrum of F1s of-B, a more obvious spectrum peak can be seen from the graph, the corresponding spectrum peak is F1s, the binding energy is 684.5 eV, and F is successfully doped into TiO 2 -in the B lattice.
FIG. 3 is F-doped TiO 2 -B scanning electron microscopy. From the figure it can be seen that F-doped TiO 2 B is in a particle shape, the size of the B is about tens of nanometers, and the B has good dispersibility.
FIG. 4 is an F-doped TiO 2 -cycling performance of B over a voltage range of 1-3V (vs. Li/li+). The charge and discharge are carried out for 250 circles at a larger current density of 1.675A/g, the capacity is stabilized at 184.5 mAh/g, and the high specific capacity and stable cycle performance are shown.
While the basic principles and main features of the present invention and advantages thereof have been shown and described, it will be understood by those skilled in the art that the present invention is not limited by the foregoing embodiments, which are described merely by way of illustration of the principles of the present invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined in the appended claims and their equivalents.
Claims (6)
1. F-doped TiO 2 -B, characterized in that: the method comprises the following steps:
step (1), 1-5 g of glycolic acid is selected to be fully dissolved in 30-40 ml of water;
sequentially adding tetrabutyl titanate, concentrated sulfuric acid and an F reagent into the aqueous solution of the glycollic acid prepared in the step (1), and fully stirring to obtain a solution containing F ions;
step (3), transferring the stirred solution into a 50 milliliter reaction kettle, and placing the reaction kettle in an oven for hydrothermal reaction;
washing the product obtained after the reaction with water for a plurality of times, and then putting the product into a vacuum oven for drying to obtain a sample;
calcining the dried sample at 400 ℃ for 1-3 hours in an air atmosphere to finally obtain F-doped TiO 2 -B;
The reagent F is tetrabutylammonium tetrafluoroborate.
2. An F-doped TiO according to claim 1 2 -B, characterized in that: and (2) weighing 0.5-2 ml of tetrabutyl titanate, 0.1-1 ml of concentrated sulfuric acid and 1-5 g of F reagent in the step (2), and sequentially adding the tetrabutyl titanate, the concentrated sulfuric acid and the F reagent into the aqueous solution of the glycollic acid prepared in the step (1).
3. An F-doped TiO according to claim 1 2 -B, characterized in that: in the step (3), the stirred solution is transferred into a 50 milliliter reaction kettle and is placed into a baking oven with the temperature of 100-220 ℃ for hydrothermal reaction, and the hydrothermal reaction is carried outThe reaction time is 2-24 hours.
4. An F-doped TiO according to any one of claims 1 to 3 2 F-doped TiO prepared by preparation method of-B 2 -B use in a lithium ion battery, characterized in that: f-doped TiO to be prepared 2 Mixing and grinding the B, polyvinylidene fluoride and acetylene black, uniformly coating the ground mixture on a copper foil to serve as a negative electrode in a lithium ion battery, wherein a reference electrode and a counter electrode are both metal lithium, and an electrolyte is 1M LiPF 6 Ec+dmc+emc solution of (b).
5. The use according to claim 4, characterized in that: f-doped TiO (titanium dioxide) in mass ratio 2 -B: polyvinylidene fluoride: acetylene black=70: 20:10.
6. the use according to claim 4, characterized in that: the 1M LiPF 6 Ec+dmc+emc solution in volume ratio, wherein EC: DMC: emc=1: 1:1.
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| CN115548311A (en) * | 2022-10-20 | 2022-12-30 | 福州大学 | Fluorine doped TiO 2 (B) /rGO composite material and preparation method and application thereof |
| CN115626659B (en) * | 2022-10-25 | 2023-10-24 | 福州大学 | Preparation of three-dimensional reticular tin disulfide composite sulfur-nitrogen doped graphene and application of three-dimensional reticular tin disulfide composite sulfur-nitrogen doped graphene in lithium ion battery |
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