CN114639817A - Super ion conductor KTi2(PO4)3With TiO2Preparation and use of composite materials - Google Patents
Super ion conductor KTi2(PO4)3With TiO2Preparation and use of composite materials Download PDFInfo
- Publication number
- CN114639817A CN114639817A CN202210389821.3A CN202210389821A CN114639817A CN 114639817 A CN114639817 A CN 114639817A CN 202210389821 A CN202210389821 A CN 202210389821A CN 114639817 A CN114639817 A CN 114639817A
- Authority
- CN
- China
- Prior art keywords
- tio
- kti
- ion conductor
- composite material
- heating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 239000010416 ion conductor Substances 0.000 title claims abstract description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910001415 sodium ion Inorganic materials 0.000 claims abstract description 24
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007773 negative electrode material Substances 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 229910010062 TiCl3 Inorganic materials 0.000 claims description 5
- 241000628997 Flos Species 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 9
- 239000002028 Biomass Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 3
- 230000001351 cycling effect Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 8
- 240000002853 Nelumbo nucifera Species 0.000 description 7
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 7
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 238000013329 compounding Methods 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 4
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 4
- 239000002033 PVDF binder Substances 0.000 description 4
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000005486 organic electrolyte Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229910001488 sodium perchlorate Inorganic materials 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 210000002969 egg yolk Anatomy 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000001757 thermogravimetry curve Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- 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
- H01M4/364—Composites as mixtures
-
- 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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- 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
-
- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
Abstract
The invention discloses a super ion conductor KTi2(PO4)3With TiO2Preparation and application of the composite material. The method takes the natural thermal biomass as a template to realize the super ion conductor KTi under the condition of only providing a Ti source2(PO4)3With TiO2The performance of the sodium-ion battery is improved by improving the material structure. The synthesis method is simple and easy to regulate, and TiO can be effectively improved by using the material as a sodium ion negative electrode material2Rate capability and cycling stability of sodium ion batteries. Is a super ion conductor KTi2(PO4)3With TiO2In the nanometer rangeThe particle battery provides a brand new thought and has a good application prospect.
Description
Technical Field
The invention belongs to a super ion conductor KTi2(PO4)3With TiO2Of (2), in particular KTi2(PO4)3/TiO2A synthetic method of a composite material and application of the composite material in a sodium ion battery belong to the technical field of energy and environmental protection.
Background
Sodium Ion Batteries (SIBs) inherit the similar "rocking chair" charging and discharging mechanism of Lithium Ion Batteries (LIBs) and avoid the shortage of lithium resources, and are considered as a new system which is most promising to become the next generation of energy storage batteries. The radius of sodium ions is far larger than that of lithium ions, so that the insertion and extraction resistance of sodium ions in the electrode material is large, and therefore, the exploration of a proper electrode material is one of the keys of the realization of large-scale application of the SIB. At present, the research of the anode material has become an important factor for restricting the development of the SIB compared with the research of the mature anode material. Among the many negative electrode materials, titanium dioxide (TiO)2) Stable structure, low price, abundant reserves, easy preparation, higher safety, proper sodium storage voltage platform and higher theoretical electrochemical performance index (the theoretical capacity can reach 335 mAh g)-1) Etc., but still has low conductivity and Na+The problem of slow diffusion. At present, the research is mainly to improve the conductivity of the surface and the inside of the material and improve Na by adding a conductive agent, doping bulk phases, controlling the particle size, improving the appearance characteristics and the like+The migration rate is less, and the research on improving the battery performance by adding additional materials and compounding the additional materials is less. In addition, the implementation of the above scheme often requires the addition of additional chemical reagents, which undoubtedly increases the preparation cost and causes environmental problems, and the Na is realized by the strategies of doping, changing the size and shape of the material and the like+The improvement of the migration rate has a larger limit. Super ion conductor KTi2(PO4)3The embedded negative electrode material has high ionic conductivity and high K+The ion radius and the space along the c-axis are larger, and can be embedded with Na+Providing a larger ion diffusion path. In the aspect of synthetic materials, nature provides a good reference for us, biomass with various appearances and different element compositions exists in nature, and the biomass is taken as a template, so that various biomasses can be realized in an environment-friendly and efficient mannerAnd (4) obtaining the functional material. The natural biomass is taken as a template, and the super ion conductor KTi is realized under the condition of only providing a Ti source2(PO4)3With TiO2The performance of the sodium ion battery is improved.
Disclosure of Invention
The purpose of the invention is: aiming at TiO which is currently used as the cathode material of the sodium-ion battery2Low electrical conductivity and Na+The problem of slow diffusion is that the super ion conductor KTi is realized by using rich miscellaneous elements (K, P and C) and a pore structure in the biomass under the condition of only providing a Ti source2(PO4)3With TiO2By constructing a porous structure and embedding KTi with large ion diffusion channels2(PO4)3Realize Na+The migration rate is improved by in-situ doping C and compounding KTi2(PO4)3The conductivity is improved, and the performance of the SIB battery is improved.
To achieve the above object, the present invention KTi2(PO4)3/TiO2The technical scheme of the composite material is as follows:
super ion conductor KTi2(PO4)3With TiO2The preparation method of the composite material is characterized by comprising the following steps:
measuring a certain amount of TiCl3The hydrochloric acid solution is evenly dispersed in 100 mL of absolute ethyl alcohol, and then weighed and mixed with TiCl3Adding pretreated flos Nelumbinis pollen (LP-Et) at a mass ratio of 1:1 into the above solution, stirring in dark for not less than 12 hr, centrifuging with anhydrous ethanol for several times, and washing 60 timesoDrying C overnight, calcining, and calcining in muffle furnace at a temperature rise rate of 5oC/min heating from room temperature to 300oC, and is at 300oKeeping the temperature for 6 hours at the temperature of C; then at a heating rate of 10oC/min is 300oC heating to 700 deg.CoC, and is at 700oKeeping the temperature for 3 hours under C; the white powdery solid obtained after twice calcination is KTi2(PO4)3/TiO2A composite material.
Will be described in the specificationPrepared KTi2(PO4)3/TiO2And commercial TiO2And after the electrode plates are manufactured, assembling the sodium ion battery to test the electrochemical performance of the sodium ion battery.
Compared with the prior art, the implementation mode has the following characteristics:
the invention adopts lotus pollen as a biological template, and realizes the super ion conductor KTi under the condition of only providing a Ti source2(PO4)3With TiO2And (4) compounding. The result of X-ray powder diffraction combined with the X-ray photoelectron spectrum and transmission electron microscope shows that KTi in the invention2(PO4)3With TiO2Compounded with an approximate mass.
Drawings
The following description of the main parameter features of the present invention is illustrated by the figures
FIG. 1 shows the pre-treated lotus pollen and KTi obtained in example 12(PO4)3/TiO2SEM image of (d). The results show that KTi produced2(PO4)3/TiO2The lotus powder and surface gully are kept, the lotus powder is in a yolk shell structure, the shell is in a net-shaped porous structure, the inner core is in a surface-folded spherical structure, and the shell has a layer of porous structure inside except net-shaped holes on the surface; in the figure: a and B are SEM images of lotus pollen after pretreatment, C and D are KTi2(PO4)3/TiO2SEM image of (d).
FIG. 2 shows KTi obtained in example 12(PO4)3/TiO2EDS line scan of (a). The results show that, whether core or shell, KTi2(PO4)3/TiO2All distributed with K, Ti, P, C, O and N elements.
FIG. 3 shows KTi obtained in example 12(PO4)3/TiO2The transmission electron microscope and its high resolution image. As a result, it was confirmed that the sample was KTi formed by stacking small particles2(PO4)3/TiO2A composite material. In the figure: a is KTi2(PO4)3/TiO2B is KTi2(PO4)3/TiO2High resolution transmission electron microscopy images of (a).
FIG. 4.1 shows KTi obtained in example 12(PO4)3/TiO2Fine fit XRD pattern. The results show KTi2(PO4)3With TiO2Is close to 56.53: 43.47.
FIG. 4.2 shows KTi obtained in example 12(PO4)3/TiO2Thermogram of (a). The results show KTi2(PO4)3/TiO2The carbon content of (A) was 0.35%.
FIG. 5 shows KTi obtained in example 12(PO4)3/TiO2Fine spectrum of C, P, N. The result shows that the use of the lotus pollen template realizes N, P to C and TiO2Is doped with, but not with, KTi2(PO4)3Has effects, and needs further research. In the figure: a is a C1 s spectrum, B is an N1 s spectrum, and C is a P2P spectrum.
FIG. 6 shows KTi obtained in example 12(PO4)3/TiO2And commercial TiO2As a rate capability graph for sodium ion negative electrode materials. The results show that2(PO4)3Compounding can improve TiO2Rate capability in sodium ion batteries.
FIG. 7 shows KTi obtained in example 12(PO4)3/TiO2And commercial TiO2As a cycle performance diagram for the sodium ion negative electrode material. The results show that KTi2(PO4)3/TiO2The better cycling stability is shown.
FIG. 8.1 shows KTi obtained in example 12(PO4)3/TiO2And commercial TiO2Impedance graph of (a). The results show that KTi is compounded2(PO4)3After that, the conductivity of the material is enhanced.
FIG. 8.2 shows KTi obtained in example 12(PO4)3/TiO2And commercial TiO2Z' and ω of-1/2A graph of the relationship (c).The results show that KTi is compounded2(PO4)3Na of the latter material+The diffusion rate increases.
FIG. 9.1 shows KTi obtained in example 12(PO4)3/TiO2CV of (1). The results show that Na+At KTi2(PO4)3，TiO2And KTi2(PO4)3/TiO2The interface is embedded and separated, and the embedding and the separation are more and more stable along with the scanning.
FIG. 9.2 is commercial TiO2CV of (1). The results show that Na+In TiO2Neutralizing KTi obtained in example 12(PO4)3/TiO2There is a great difference between the insertion and the extraction.
Detailed Description
In the invention, the KTi is realized by only providing a Ti source by utilizing the advantages of the structure and the composition of lotus pollen2(PO4)3With TiO2And (4) compounding. A series of tests show that the composite material can improve the performance of the sodium-ion battery.
Example 1
Measuring 20 mL of TiCl3Dispersing hydrochloric acid solution (15% -20%) in 100 mL anhydrous ethanol, weighing 4 g flos Nelumbinis pollen (LP-Et) which is ultrasonically cleaned with ethanol for three times and dried, adding into the above solution, stirring for 12 hr in dark place, centrifuging with anhydrous ethanol for 3 times, and washing 60 timesoDrying and roasting the mixture after the mixture is dried overnight, and placing the obtained product at 300 DEG CoCalcining in a C muffle furnace at a heating rate of 5oC/min (here means that the product produced is from room temperature to 300 ℃ in a muffle furnace)oC at a rate of temperature rise of 5oC/min heating) and then 300 deg.C/minoKeeping the temperature for 6 hours under C; then the temperature is raised to 700 DEGoC, the rate of temperature rise is 10oC/min (from 300 in muffle furnace here)oCTo 700oC at a heating rate of 10oC/min heating), and then 700 deg.C/min heatingoKeeping the temperature for 3 hours under C; the white powdery solid obtained after twice calcination is KTi2(PO4)3/TiO2A composite material.
Example 2
KTi obtained in example 12(PO4)3/TiO2The performance of the sodium ion battery of the composite material is as follows: the working electrode is KTi2(PO4)3/TiO2The conductive carbon (Super P) and polyvinylidene fluoride (PVDF) adhesive in a weight ratio of 8:1:1, and the current collector is copper foil. The active material has a mass loading of about-1.5 mg/cm2. Na metal is used as a positive electrode, a working electrode is used as a negative electrode, glass fiber (Whatman GF/D) is used as a diaphragm, and 1M NaClO4Type 2430 coin cells were assembled in a glove box filled with pure Ar using Ethylene Carbonate (EC)/dimethyl carbonate (DMC) (1: 1 wol%) and 5.0 wt% fluoroethylene carbonate (FEC) solutions as the organic electrolyte. Constant current charge and discharge measurements over a voltage range of 0.01-3.0V were performed using a multi-channel battery test system (LAND CT 2001A).
Example 3
Commercial TiO2The performance of the sodium ion battery of (2): the working electrode is made of TiO2The conductive carbon (Super P) and polyvinylidene fluoride (PVDF) adhesive in a weight ratio of 8:1:1, and the current collector is copper foil. The active material has a mass loading of about-1.5 mg/cm2. Na metal is used as a positive electrode, a working electrode is used as a negative electrode, glass fiber (Whatman GF/D) is used as a diaphragm, and 1M NaClO4Type 2430 coin cells were assembled in a glove box filled with pure Ar using Ethylene Carbonate (EC)/dimethyl carbonate (DMC) (1: 1 wol%) and 5.0 wt% fluoroethylene carbonate (FEC) solution as the organic electrolyte. Constant current charge and discharge measurements over a voltage range of 0.01-3.0V were performed using a multi-channel battery test system (LAND CT 2001A).
Example 4
LP-Ti prepared in example 12(PO4)3/TiO2Electrochemical properties of the composite material: cyclic voltammetry tests (CV) were performed using an electrochemical workstation (CHI 760E) at a scan rate of 0.1 mV/s and Electrochemical Impedance Spectroscopy (EIS) tests were performed at 0.01 Hz to 10 kHz.
Example 5
Commercial TiO2Electrochemical performance of (2): cyclic voltammetry tests (CV) were performed using an electrochemical workstation (CHI 760E) at a scan rate of 0.1 mV/s and Electrochemical Impedance Spectroscopy (EIS) tests were performed at 0.01 Hz to 10 kHz.
Claims (2)
1. Super ion conductor KTi2(PO4)3With TiO2The preparation method of the composite material is characterized by comprising the following steps:
measuring a certain amount of TiCl3The hydrochloric acid solution is evenly dispersed in 100 mL of absolute ethyl alcohol, and then weighed and mixed with TiCl3Adding pretreated flos Nelumbinis pollen (LP-Et) at a mass ratio of 1:1 into the above solution, stirring in dark for at least 12 hr, centrifuging with anhydrous ethanol, and washing for 60 timesoC, drying overnight, then roasting, placing the prepared product in a muffle furnace for roasting, and heating in the muffle furnace at a heating rate of 5oC/min heating from room temperature to 300oC, and is at 300oKeeping the temperature for 6 hours at the temperature of C; then at a heating rate of 10oC/min is 300oC heating to 700 deg.CoC, and is at 700oKeeping the temperature for 3 hours under C; the white powdery solid obtained after twice calcination is KTi2(PO4)3/TiO2A composite material.
2. KTi prepared in claim 12(PO4)3/TiO2The composite material is applied to the aspect of negative electrode materials of sodium-ion batteries.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210389821.3A CN114639817B (en) | 2022-04-13 | 2022-04-13 | Super-ion conductor KTi 2 (PO 4 ) 3 With TiO 2 Preparation and application of composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210389821.3A CN114639817B (en) | 2022-04-13 | 2022-04-13 | Super-ion conductor KTi 2 (PO 4 ) 3 With TiO 2 Preparation and application of composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114639817A true CN114639817A (en) | 2022-06-17 |
| CN114639817B CN114639817B (en) | 2023-12-26 |
Family
ID=81952299
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210389821.3A Active CN114639817B (en) | 2022-04-13 | 2022-04-13 | Super-ion conductor KTi 2 (PO 4 ) 3 With TiO 2 Preparation and application of composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114639817B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104787799A (en) * | 2015-05-13 | 2015-07-22 | 武汉理工大学 | Web-type three-dimensional perforated macroporous-mesoporous-structure titanium dioxide material, and preparation method and application thereof |
| CN105826521A (en) * | 2016-05-11 | 2016-08-03 | 西南大学 | Polyanion compound KTi2(PO4)3, preparation of carbon coating thereof and application of product of polyanion compound KYi(PO4)3 |
| CN106450226A (en) * | 2016-11-22 | 2017-02-22 | 华南师范大学 | Preparation method of natural pollen-based metal sulfide-carbon composite material and application thereof |
| CN108878876A (en) * | 2018-06-28 | 2018-11-23 | 中国科学院福建物质结构研究所 | Potassium titanyl phosphate negative electrode material for potassium ion secondary cell |
| US20190067692A1 (en) * | 2015-12-07 | 2019-02-28 | National Institute Of Advanced Industrial Science And Technology | Positive electrode active material for potassium ion secondary cell |
-
2022
- 2022-04-13 CN CN202210389821.3A patent/CN114639817B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104787799A (en) * | 2015-05-13 | 2015-07-22 | 武汉理工大学 | Web-type three-dimensional perforated macroporous-mesoporous-structure titanium dioxide material, and preparation method and application thereof |
| US20190067692A1 (en) * | 2015-12-07 | 2019-02-28 | National Institute Of Advanced Industrial Science And Technology | Positive electrode active material for potassium ion secondary cell |
| CN105826521A (en) * | 2016-05-11 | 2016-08-03 | 西南大学 | Polyanion compound KTi2(PO4)3, preparation of carbon coating thereof and application of product of polyanion compound KYi(PO4)3 |
| CN106450226A (en) * | 2016-11-22 | 2017-02-22 | 华南师范大学 | Preparation method of natural pollen-based metal sulfide-carbon composite material and application thereof |
| CN108878876A (en) * | 2018-06-28 | 2018-11-23 | 中国科学院福建物质结构研究所 | Potassium titanyl phosphate negative electrode material for potassium ion secondary cell |
Non-Patent Citations (2)
| Title |
|---|
| RU, Q ET AL: "Biological carbon skeleton of lotus-pollen surrounded by rod-like Sb2S3 as anode material in lithium ion battery", MATERIALS LETTERS, vol. 198, pages 57 - 60 * |
| XU HOU ET AL: "TiO2@LiTi2(PO4)3 enabling fast and stable lithium storage for high voltage aqueous lithium-ion batteries", JOURNAL OF POWER SOURCES, vol. 484, pages 229255 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114639817B (en) | 2023-12-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Hou et al. | An aqueous rechargeable sodium ion battery based on a NaMnO 2–NaTi 2 (PO 4) 3 hybrid system for stationary energy storage | |
| JP6165345B2 (en) | Layered copper-containing oxide material, its preparation process and its use | |
| AU2014336895B2 (en) | Tungsten-based material super battery and supercapacitor | |
| CN103999266B (en) | active material for battery pack | |
| AU2014336895A1 (en) | Tungsten-based material super battery and supercapacitor | |
| CN108878826B (en) | Sodium manganate/graphene composite electrode material and preparation method and application thereof | |
| CN110034283A (en) | Phosphorization tin composite material and preparation method and application | |
| Liu et al. | An aqueous rechargeable sodium− magnesium mixed ion battery based on NaTi2 (PO4) 3–MnO2 system | |
| CN108922788A (en) | A kind of PEDOT@Na3(VOPO4)2F composite material, preparation method and its application | |
| CN109301209A (en) | A kind of preparation method of titania modified phosphorus/carbon compound cathode materials | |
| CN110518295A (en) | One kind can fill zinc-base battery | |
| CN110467170B (en) | High-potential positive electrode material of potassium ion battery and preparation method thereof | |
| CN109286002A (en) | Thousand layers of Bark Biomass carbon load red phosphorus anode material of lithium-ion battery of one kind and preparation method thereof | |
| CN105680016B (en) | One kind contains addition of C o3O4Lithium sulfur battery anode material and preparation method | |
| Li et al. | Carbon coated heterojunction CoSe 2/Sb 2 Se 3 nanospheres for high-efficiency sodium storage | |
| Ba et al. | Synergistically enhancing cycleability and rate performance of sodium titanate nanowire anode via hydrogenation and carbon coating for advanced sodium ion batteries | |
| Fan et al. | Zn/Ti/F synergetic-doped Na 0.67 Ni 0.33 Mn 0.67 O 2 for sodium-ion batteries with high energy density | |
| CN109980200A (en) | A kind of noncrystal phosphorus base negative electrode material of domain Dispersed precipitate and preparation method thereof | |
| CN109950640B (en) | Metal graphite medium-temperature energy storage battery and preparation method thereof | |
| Xu et al. | Exploration of Na 2.65 Ti 3.35 Fe 0.65 O 9 as anode materials for Na-ion batteries | |
| CN114551891B (en) | Tin disulfide/titanium dioxide/carbon composite material and preparation method and application thereof | |
| CN113809302B (en) | Magnesium-calcium modified layered P2-phase nickel-manganese-based positive electrode material and preparation method and application thereof | |
| Yang et al. | A novel approach to LiVO3 synthesis enables its outstanding lithium storage performance | |
| CN105591091B (en) | A kind of sodium ion secondary battery negative electrode active material and its preparation method and application | |
| CN114639817A (en) | Super ion conductor KTi2(PO4)3With TiO2Preparation and use of composite materials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |