CN113130884A - F-doped TiO2Preparation method and application of (E) -B - Google Patents
F-doped TiO2Preparation method and application of (E) -B Download PDFInfo
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- CN113130884A CN113130884A CN202110372579.4A CN202110372579A CN113130884A CN 113130884 A CN113130884 A CN 113130884A CN 202110372579 A CN202110372579 A CN 202110372579A CN 113130884 A CN113130884 A CN 113130884A
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- 238000000034 method Methods 0.000 title claims description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 23
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 7
- 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 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-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
- -1 tetrabutyl ammonium 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
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 229910003075 TiO2-B Inorganic materials 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 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
- 239000007864 aqueous solution Substances 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910001290 LiPF6 Inorganic materials 0.000 claims description 3
- 239000011889 copper foil Substances 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910013870 LiPF 6 Inorganic materials 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000001351 cycling effect Effects 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract description 2
- 239000010406 cathode material Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 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
- 125000005842 heteroatom Chemical group 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
- 231100000956 nontoxicity Toxicity 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
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
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- 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
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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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- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to F-doped TiO2A preparation method of the (E) -B and application thereof in a lithium ion battery. Dissolving glycollic acid in water, adding tetrabutyl titanate, concentrated sulfuric acid and tetrabutyl ammonium tetrafluoroborate, stirring, washing and drying after the reaction of an autoclave is finished, and calcining to obtain F-doped TiO2B, the F being doped with TiO2the-B serving as the negative electrode of the lithium battery has high specific capacity and cycling stabilityThe specific capacity is stabilized at 184.5 mAh/g after the charge and the discharge of 250 circles when the large current density is 1.675A/g.
Description
Technical Field
The invention relates to a lithium ion battery technology, in particular to F-doped TiO2A preparation method of the (E) -B and application thereof in a lithium ion battery.
Background
Since the successful development of the lithium ion battery in the nineties of the last century, the lithium ion battery has been widely used, but it has been the research focus of scientists to obtain a lithium ion battery cathode material with good cycle performance, high specific capacity and good large-current charge and discharge performance.
TiO2The material has wide application prospect in the fields of photocatalysis, lithium ion batteries, dye-sensitized solar cells, photolysis water, sensors and the like, and has become a hotspot of research in the field of materials. Wherein the TiO is2the-B phase is taken as an embedded material, and is concerned by researchers due to the advantages of safety, no toxicity, abundant sources, good circulation stability and the like. TiO 22The phase-B belongs to a metastable phase, and has a structure with more open space channels, which is beneficial to the intercalation and deintercalation of lithium ions, and becomes a hot spot of research in recent years. However, TiO2the-B is used as the lithium ion battery cathode material with lower conductivity and pure-phase TiO2the-B often has the problems of poor cycle performance and the like, and the lithium storage performance of the-B is seriously influenced.
Disclosure of Invention
Therefore, in view of the above problems, the present invention provides a F-doped TiO2A preparation method of the (E) -B and application thereof in a lithium ion battery.
In order to achieve the purpose, the invention provides the technical scheme that F-doped TiO2-B, comprising the steps of:
step (1), selecting 1-5 g of glycolic acid to be fully dissolved in 30-40 ml of water;
step (2), tetrabutyl titanate, concentrated sulfuric acid and an F reagent are sequentially added into the glycolic acid aqueous solution prepared in the step (1), and are fully stirred to obtain a solution containing F ions;
step (3), transferring the stirred solution into a 50 ml reaction kettle, and placing the reaction kettle into an oven for hydrothermal reaction;
washing a product obtained after the reaction for several times by using water, and then putting the product into a vacuum oven for drying to obtain a sample;
calcining the dried sample for 1-3 hours at 400 ℃ in the air atmosphere to finally obtain F-doped TiO2-B。
The further improvement is that: and (3) in the step (2), 0.5-2 ml of tetrabutyl titanate, 0.1-1 ml of concentrated sulfuric acid and 1-5 g of F reagent are measured and added into the glycolic acid aqueous solution prepared in the step (1) in sequence.
The further improvement is that: and (3) in the step (2), the reagent F is tetrabutylammonium tetrafluoroborate.
The further improvement is that: in the step (3), the stirred solution is transferred into a 50 ml reaction kettle and placed in an oven at the temperature of 100-220 ℃ for hydrothermal reaction, and the hydrothermal reaction time is 2-24 hours.
F-doped TiO2The preparation method of the-B is applied to the lithium ion battery, and the prepared F is doped with TiO2And (3) mixing and grinding the-B, polyvinylidene fluoride and acetylene black, uniformly coating the ground mixture on copper foil to be used as a negative electrode in the lithium ion battery, wherein the reference electrode and the counter electrode are both made of metal lithium, and the electrolyte is EC + DMC + EMC solution of 1M LiPF 6.
The further improvement is that: f is doped with TiO according to the mass ratio2-B: polyvinylidene fluoride: acetylene black 70: 20: 10.
the further improvement is that: the 1M LiPF6In volume ratios, wherein EC: DMC: EMC = 1: 1: 1.
the invention relates to F-doped TiO2The preparation method of the-B and the application thereof in the lithium ion battery have the following beneficial effects:
the invention provides F-doped TiO2The preparation method of the-B is applied to the lithium ion battery, and the traditional TiO problem is solved2The problem of low conductivity when the-B is used as a lithium ion battery cathode material is solved, the lithium storage performance of the-B is ensured, and the method has the advantages of simple process, low cost, low energy consumption, good reproducibility and excellent performance.
Drawings
FIG. 1 shows F-doped TiO2-X-ray diffraction pattern of B;
FIG. 2 shows F-doped TiO2-X-ray photoelectron spectroscopy of B;
FIG. 3 shows F-doped TiO2-scanning electron micrographs of B;
FIG. 4 shows F-doped TiO2Electrochemical performance diagram of-B (current density of 1.675A/g).
Detailed Description
The following description of the embodiments of the present invention will be made with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Referring to FIGS. 1 to 4, an F-doped TiO2The preparation method of (E) -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 tetrabutylammonium tetrafluoroborate, stirring, transferring into a 50 ml reaction kettle, placing in an oven at the temperature of 100 ℃ and 200 ℃ for hydrothermal reaction for 2-24 hours, washing the product obtained after the reaction for a plurality of times with water, drying, calcining the dried sample for 1-3 hours at the temperature of 400 ℃ in the air atmosphere to obtain the F-doped TiO2-B。
F-doped TiO2The application of B in the lithium ion battery is that F is doped with TiO according to the mass ratio when the lithium ion battery is assembled2-B: polyvinylidene fluoride: acetylene black 70: 20: 10 is evenly coated on a copper foil after being mixed and ground to be used as a negative electrode, a reference electrode and a counter electrode are both made of metal lithium, and electrolyte is 1M LiPF6EC + DMC + EMC (EC/DMC/EMC =1/1/1 v/v) solution.
The invention adopts a one-step hydrothermal method and a subsequent calcination process to rapidly prepare F-doped TiO2B, applying the F-doped TiO negative electrode material into a lithium ion battery negative electrode material2the-B serving as the negative electrode of the lithium battery has high specific capacity and cycling stability, is charged and discharged for 250 circles at a larger current density of 1.675A/g, and has stable capacity of 184.5 mAh/g.
FIG. 1 is F-doped TiO2X-ray diffraction pattern of-B, from which it can be seen that all diffraction peaks can be attributed to monoclinic TiO2B (JCPDS card number: 74-1940). Further, no hetero peak was found from the diffraction pattern. This illustrates the F-doped TiO prepared by the process of the invention2TiO with B as pure phase2-B。
FIG. 2 shows F-doped TiO2The X-ray photoelectron spectrum of F1s of B shows a more distinct peak corresponding to F1s with a binding energy of 684.5 eV, indicating that F was successfully doped into TiO2-B lattice.
FIG. 3 is F-doped TiO2-scanning electron micrographs of B. From the figure, it can be seen that F-doped TiO2the-B is in a particle shape, the size is about dozens of nanometers, and the dispersibility is good.
FIG. 4 shows F-doped TiO2Cycling behavior of B in the voltage range 1-3V (vs. Li/Li +). The lithium ion battery is charged and discharged for 250 circles at a larger current density of 1.675A/g, the capacity is stabilized at 184.5 mAh/g, and the lithium ion battery shows higher specific capacity and stable cycle performance.
While there have been shown and described what are at present considered to be the fundamental principles of the invention and its essential features and advantages, it will be understood by those skilled in the art that the invention is not limited by the embodiments described above, which are included to illustrate the principles of the invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (7)
1. F-doped TiO2-B, characterized in that: the method comprises the following steps:
step (1), selecting 1-5 g of glycolic acid to be fully dissolved in 30-40 ml of water;
step (2), tetrabutyl titanate, concentrated sulfuric acid and an F reagent are sequentially added into the glycolic acid aqueous solution prepared in the step (1), and are fully stirred to obtain a solution containing F ions;
step (3), transferring the stirred solution into a 50 ml reaction kettle, and placing the reaction kettle into an oven for hydrothermal reaction;
washing a product obtained after the reaction for several times by using water, and then putting the product into a vacuum oven for drying to obtain a sample;
calcining the dried sample for 1-3 hours at 400 ℃ in the air atmosphere to finally obtain F-doped TiO2-B。
2. An F-doped TiO according to claim 12A process for the preparation of (A) B, characterized in thatThe method comprises the following steps: and (3) in the step (2), 0.5-2 ml of tetrabutyl titanate, 0.1-1 ml of concentrated sulfuric acid and 1-5 g of F reagent are measured and added into the glycolic acid aqueous solution prepared in the step (1) in sequence.
3. An F-doped TiO according to claim 12-B, characterized in that: and (3) in the step (2), the reagent F is tetrabutylammonium tetrafluoroborate.
4. An F-doped TiO according to claim 12-B, characterized in that: in the step (3), the stirred solution is transferred into a 50 ml reaction kettle and placed in an oven at the temperature of 100-220 ℃ for hydrothermal reaction, and the hydrothermal reaction time is 2-24 hours.
5. F-doped TiO according to any one of claims 1 to 42The application of the preparation method of the-B in the lithium ion battery is characterized in that: doping the prepared F with TiO2And (3) mixing and grinding the-B, polyvinylidene fluoride and acetylene black, uniformly coating the ground mixture on copper foil to be used as a negative electrode in the lithium ion battery, wherein the reference electrode and the counter electrode are both made of metal lithium, and the electrolyte is EC + DMC + EMC solution of 1M LiPF 6.
6. Use according to claim 2, characterized in that: f is doped with TiO according to the mass ratio2-B: polyvinylidene fluoride: acetylene black 70: 20: 10.
7. use according to claim 2, characterized in that: the 1M LiPF6In volume ratios, wherein EC: DMC: EMC = 1: 1: 1.
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Cited By (2)
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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 |
CN115626659A (en) * | 2022-10-25 | 2023-01-20 | 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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