CN113772728A - Mixed-phase niobium-titanium oxide, and preparation method and energy storage application thereof - Google Patents

Mixed-phase niobium-titanium oxide, and preparation method and energy storage application thereof Download PDF

Info

Publication number
CN113772728A
CN113772728A CN202111198879.1A CN202111198879A CN113772728A CN 113772728 A CN113772728 A CN 113772728A CN 202111198879 A CN202111198879 A CN 202111198879A CN 113772728 A CN113772728 A CN 113772728A
Authority
CN
China
Prior art keywords
niobium
titanium oxide
mixed
phase
titanium
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.)
Pending
Application number
CN202111198879.1A
Other languages
Chinese (zh)
Inventor
余翠平
王岩
吴玉程
张剑芳
崔接武
秦永强
舒霞
张勇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hefei University of Technology
Original Assignee
Hefei University of Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Hefei University of Technology filed Critical Hefei University of Technology
Priority to CN202111198879.1A priority Critical patent/CN113772728A/en
Publication of CN113772728A publication Critical patent/CN113772728A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G33/00Compounds of niobium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/46Metal oxides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/50Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/20Particle morphology extending in two dimensions, e.g. plate-like
    • C01P2004/24Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/80Particles consisting of a mixture of two or more inorganic phases
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/40Electric properties
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention discloses a mixed-phase niobium-titanium oxide, a preparation method and an energy storage application thereof. The mixed-phase niobium-titanium oxide can be applied to preparing electrode materials of electrochemical energy storage devices such as lithium ion capacitors and the like, wherein the electrochemical performance of the materials can be further improved through the synergistic energy storage effect of all phases; the preparation method is simple, low in cost, easy to control in process and capable of realizing batch production.

Description

Mixed-phase niobium-titanium oxide, and preparation method and energy storage application thereof
Technical Field
The invention belongs to the field of preparation of nano functional materials, and particularly relates to a mixed-phase niobium titanium oxide, and a preparation method and an energy storage application thereof.
Background
In recent years, niobium-titanium oxide has attracted much attention in the fields of electrochemical energy storage, environmental catalysis, gas sensing and the like by virtue of its advantages of excellent physicochemical properties, abundant structural compositions, nontoxicity, abundant sources and the like. Especially when applied to electrochemical energy storage, the deintercalation type niobium titanium oxide with high working potential and theoretical capacity is an ideal negative electrode material: firstly, the rapid ion intercalation/deintercalation process of niobium-titanium oxide can effectively make up the difference of the internal electrochemical reaction kinetics of the energy storage device; secondly, the niobium-titanium oxide with relatively high working potential can simultaneously avoid the formation of SEI film and lithium dendrite, thereby ensuring the safety of the electrode; moreover, the niobium-titanium oxide can provide a wider ion diffusion channel, so that the structure of the niobium-titanium oxide is not changed before and after ion implantation, and the structural stability and the cycling stability of the niobium-titanium oxide are enhanced. However, the low intrinsic ion mobility and conductivity of niobium-titanium oxide seriously affect the rate capability thereof, thereby restricting the wide application thereof in the field of electrochemical energy storage.
On the basis of abundant niobium-titanium oxide structure composition, further construction of mixed-phase niobium-titanium oxide is one of effective means for improving electrochemical performance of niobium-titanium oxide. Compared with a single phase, the mixture phase can provide more redox couples and active centers, the energy storage characteristics of the components of each phase are fully utilized, and the electrochemical performance of the active material can be further improved through synergistic effect. However, similar niobium-titanium oxides reported at present generally involve a relatively complex preparation process, so that exploring a simple preparation method of the niobium-titanium oxide and realizing systematic regulation and control of the morphology, phase and performance of the niobium-titanium oxide have important effects on further improving the electrochemical performance of the niobium-titanium oxide and expanding the application field of the niobium-titanium oxide.
Disclosure of Invention
Based on the problems in the prior art, the invention discloses a mixed-phase niobium titanium oxide, a preparation method and an energy storage application thereof, and aims to obtain a high-performance electrochemical energy storage material with adjustable and controllable morphology, phase and performance by a simple method.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses a preparation method of mixed-phase niobium-titanium oxide, which is characterized by comprising the following steps: firstly, preparing a mixed solution containing metal niobium salt and metal titanium salt, preparing a precursor by a solvothermal method, and then calcining at high temperature to obtain the mixed-phase niobium-titanium oxide with high crystallinity and adjustable morphology and phase. The method specifically comprises the following steps:
(1) preparing a precursor by a solvothermal method: weighing 0-5.0 mmol of metal niobium salt and 0-1.2 mmol of metal titanium salt, and dissolving in 5-50 mL of organic solvent to obtain a solution A; weighing 0.3-10 mmol of hexamethylenetetramine and dissolving in 50-150 mL of deionized water to obtain a solution B; adding the solution B into the solution A, uniformly mixing, carrying out a solvothermal reaction at a solvothermal temperature of 100-200 ℃ for 5-60 h, centrifuging, washing with water, drying, and collecting a powder product to obtain a precursor;
(2) preparing mixed-phase niobium-titanium oxide by high-temperature calcination: placing the precursor in a tube furnace, and calcining at high temperature under the protection of argon, wherein the calcining temperature is 500-900 ℃, the heat preservation time is 30-600 min, and the heating rate is 0.5-10 ℃ for min-1And naturally cooling to room temperature after the calcination is finished, thus obtaining the mixed-phase niobium-titanium oxide.
Further, the metal niobium salt is at least one of niobium chloride, niobium oxalate and ammonium niobium oxalate, and the metal titanium salt is at least one of titanium isopropoxide, titanyl sulfate, titanium tetrachloride, tetrabutyl titanate and n-butyl titanate.
Further, the organic solvent in the step (1) is one or a mixture of any more of ethanol, methanol, ethylene glycol, N-dimethylformamide and N-methylpyrrolidone.
According to the method, the morphology and the phase composition of the obtained mixed-phase niobium-titanium oxide can be regulated and controlled by regulating the molar ratio of the metal niobium salt to the metal titanium salt, so that the electrochemical energy storage characteristic of the obtained mixed-phase niobium-titanium oxide can be regulated and controlled.
The mixed-phase niobium-titanium oxide can be used as an electrode material of electrochemical energy storage materials such as lithium ion capacitors, lithium ion batteries and sodium ion batteries, and the mixed-phase niobium-titanium oxide can show higher specific capacity and excellent rate capability when used as an electrode material of a lithium ion capacitor. In addition, the mixed-phase niobium-titanium oxide has great application potential in the fields of catalysis, sensing and the like.
The invention has the beneficial effects that:
1. the preparation method is simple, low in cost, easy to control in process and capable of realizing batch production; the mixed-phase niobium-titanium oxide prepared by the method has higher specific capacity and excellent rate capability, and has better application prospect in the fields of electrochemical energy storage materials and the like.
2. The preparation method can realize synchronous optimization of the morphology, phase composition and electrochemical performance of the mixed-phase niobium-titanium oxide by regulating and controlling the molar ratio of the metal niobium salt to the metal titanium salt, for example, when the molar ratio of niobium chloride to titanium isopropoxide is 2:1 (1.8mmol of niobium pentachloride and 0.9mmol of titanium isopropoxide), the obtained product has a nano-sheet structure, and the phase composition is TiO2/TiNb2O7And the electrochemical performance is optimal.
Drawings
FIG. 1 is a FESEM photograph of mixed phase niobium titanium oxide obtained in example 1;
FIG. 2 is a FESEM photograph of mixed phase niobium titanium oxide obtained in example 2;
FIG. 3 is a FESEM photograph of mixed phase niobium titanium oxide obtained in example 3;
FIG. 4 is a FESEM photograph of mixed phase niobium titanium oxide obtained in example 4;
FIG. 5 is a FESEM photograph of mixed phase niobium titanium oxide obtained in example 5;
FIG. 6 is a FESEM photograph of mixed phase niobium titanium oxide obtained in example 6;
FIG. 7 is an XRD spectrum of mixed phase niobium titanium oxide obtained in examples 1 to 6;
FIG. 8 is a graph showing rate capability of mixed phase niobium titanium oxide obtained in examples 1 to 6;
FIG. 9 is a graph of the power density versus energy density for a lithium ion capacitor assembled with the mixed phase niobium titanium oxide prepared in example 4 as the negative electrode.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
A preparation method of mixed-phase niobium-titanium oxide specifically comprises the following steps:
(1) preparing a precursor by a solvothermal method: weighing 1.8mmol niobium pentachloride and dissolving in 22.5mL N-methyl pyrrolidone to obtain a solution A; 7.2mmol of hexamethylenetetramine was weighed and dissolved in 67.5mL of deionized water to obtain solution B. And adding the solution B into the solution A, uniformly mixing, carrying out a solvothermal reaction, wherein the solvothermal temperature is 200 ℃, the heat preservation time is 24 hours, then centrifuging, washing with water, drying, and collecting a powder product to obtain a precursor.
(2) Preparing mixed-phase niobium-titanium oxide by high-temperature calcination: placing the precursor in a tube furnace, and calcining at high temperature under the protection of argonCalcining at 750 deg.C for 300min at 2 deg.C for 2 min-1And naturally cooling to room temperature after the calcination is finished to obtain the mixed-phase niobium titanium oxide, wherein the FESEM photograph of the mixed-phase niobium titanium oxide is shown in figure 1.
Example 2
A preparation method of mixed-phase niobium-titanium oxide specifically comprises the following steps:
(1) preparing a precursor by a solvothermal method: weighing 1.8mmol of niobium pentachloride and 0.3mmol of titanium isopropoxide, and dissolving in 22.5mL of N-methylpyrrolidone to obtain a solution A; 7.2mmol of hexamethylenetetramine was weighed and dissolved in 67.5mL of deionized water to obtain solution B. And adding the solution B into the solution A, uniformly mixing, carrying out a solvothermal reaction, wherein the solvothermal temperature is 200 ℃, the heat preservation time is 24 hours, then centrifuging, washing with water, drying, and collecting a powder product to obtain a precursor.
(2) Preparing mixed-phase niobium-titanium oxide by high-temperature calcination: placing the precursor in a tube furnace, and calcining at high temperature under the protection of argon, wherein the calcining temperature is 750 ℃, the heat preservation time is 300min, and the heating rate is 2 ℃ for min-1And naturally cooling to room temperature after the calcination is finished to obtain the mixed-phase niobium titanium oxide, wherein the FESEM photograph of the mixed-phase niobium titanium oxide is shown in figure 2.
Example 3
A preparation method of mixed-phase niobium-titanium oxide specifically comprises the following steps:
(1) preparing a precursor by a solvothermal method: weighing 1.8mmol of niobium pentachloride and 0.6mmol of titanium isopropoxide, and dissolving in 22.5mL of N-methylpyrrolidone to obtain a solution A; 7.2mmol of hexamethylenetetramine was weighed and dissolved in 67.5mL of deionized water to obtain solution B. And adding the solution B into the solution A, uniformly mixing, carrying out a solvothermal reaction, wherein the solvothermal temperature is 200 ℃, the heat preservation time is 24 hours, then centrifuging, washing with water, drying, and collecting a powder product to obtain a precursor.
(2) Preparing mixed-phase niobium-titanium oxide by high-temperature calcination: placing the precursor in a tube furnace, and calcining at high temperature under the protection of argon, wherein the calcining temperature is 750 ℃, the heat preservation time is 300min, and the heating rate is 2 ℃ for min-1Naturally cooling to the temperature after calcinationAt room temperature, mixed-phase niobium titanium oxide is obtained, and the FESEM photograph is shown in figure 3.
Example 4
A preparation method of mixed-phase niobium-titanium oxide specifically comprises the following steps:
(1) preparing a precursor by a solvothermal method: weighing 1.8mmol of niobium pentachloride and 0.9mmol of titanium isopropoxide, and dissolving in 22.5mL of N-methylpyrrolidone to obtain a solution A; 7.2mmol of hexamethylenetetramine was weighed and dissolved in 67.5mL of deionized water to obtain solution B. And adding the solution B into the solution A, uniformly mixing, carrying out a solvothermal reaction, wherein the solvothermal temperature is 200 ℃, the heat preservation time is 24 hours, then centrifuging, washing with water, drying, and collecting a powder product to obtain a precursor.
(2) Preparing mixed-phase niobium-titanium oxide by high-temperature calcination: placing the precursor in a tube furnace, and calcining at high temperature under the protection of argon, wherein the calcining temperature is 750 ℃, the heat preservation time is 300min, and the heating rate is 2 ℃ for min-1And naturally cooling to room temperature after the calcination is finished to obtain the mixed-phase niobium titanium oxide, wherein the FESEM photograph of the mixed-phase niobium titanium oxide is shown in figure 4.
Example 5
A preparation method of mixed-phase niobium-titanium oxide specifically comprises the following steps:
(1) preparing a precursor by a solvothermal method: weighing 1.8mmol of niobium pentachloride and 1.8mmol of titanium isopropoxide, and dissolving in 22.5mL of N-methylpyrrolidone to obtain a solution A; 7.2mmol of hexamethylenetetramine was weighed and dissolved in 67.5mL of deionized water to obtain solution B. And adding the solution B into the solution A, uniformly mixing, carrying out a solvothermal reaction, wherein the solvothermal temperature is 200 ℃, the heat preservation time is 24 hours, then centrifuging, washing with water, drying, and collecting a powder product to obtain a precursor.
(2) Preparing mixed-phase niobium-titanium oxide by high-temperature calcination: placing the precursor in a tube furnace, and calcining at high temperature under the protection of argon, wherein the calcining temperature is 750 ℃, the heat preservation time is 300min, and the heating rate is 2 ℃ for min-1And naturally cooling to room temperature after the calcination is finished to obtain the mixed-phase niobium titanium oxide, wherein the FESEM photograph of the mixed-phase niobium titanium oxide is shown in figure 5.
Example 6
A preparation method of mixed-phase niobium-titanium oxide specifically comprises the following steps:
(1) preparing a precursor by a solvothermal method: weighing 1.8mmol of titanium isopropoxide, and dissolving the titanium isopropoxide in 22.5mL of N-methylpyrrolidone to obtain a solution A; 7.2mmol of hexamethylenetetramine was weighed and dissolved in 67.5mL of deionized water to obtain solution B. And adding the solution B into the solution A, uniformly mixing, carrying out a solvothermal reaction, wherein the solvothermal temperature is 200 ℃, the heat preservation time is 24 hours, then centrifuging, washing with water, drying, and collecting a powder product to obtain a precursor.
(2) Preparing mixed-phase niobium-titanium oxide by high-temperature calcination: placing the precursor in a tube furnace, and calcining at high temperature under the protection of argon, wherein the calcining temperature is 750 ℃, the heat preservation time is 300min, and the heating rate is 2 ℃ for min-1And naturally cooling to room temperature after the calcination is finished to obtain the mixed-phase niobium titanium oxide, wherein the FESEM photograph of the mixed-phase niobium titanium oxide is shown in figure 6.
Referring to the above examples, the present inventors investigated the effect of different ratios of niobium pentachloride and titanium isopropoxide on the morphology and phase of mixed phase niobium titanium oxide. As can be seen from FIGS. 1 to 6, the samples of the other examples all have a nano-sheet structure, except that the sample of example 6 is in a granular form. The phase characterization of XRD in FIG. 7 shows that the phase compositions of the materials obtained in examples 1-6 are Nb2O5、TiNb2O7/Nb2O5、TiNb2O7/Nb2O5、TiO2/TiNb2O7、TiO2/TiNb2O7And TiO2
In order to test the performance of the mixed-phase niobium titanium oxide obtained in the above examples as an electrochemical energy storage material, the mixed-phase niobium titanium oxide was prepared as an electrode material of a lithium ion capacitor and subjected to electrochemical test as follows:
assembling the half cell: dispersing the material synthesized in the embodiment 1-6, conductive agent carbon black and adhesive polyvinylidene fluoride in N-methyl pyrrolidone according to the mass ratio of 8:1:1, uniformly mixing to obtain slurry, and coating the slurry on a copper foil to prepare an electrode plate; to dissolve in Ethylene Carbonate (EC) and carbonic acid1.0mol L of dimethyl ester (DMC) (volume ratio 1:1)-1LiPF6And a 2320 type polypropylene microporous membrane is taken as a diaphragm, and the diaphragm is assembled into a 2032 type button battery in an argon glove box. Constant current charge and discharge test is carried out through an LAND CT-2001A test system, wherein the selected voltage range is 1.0-3.0V (V vs. Li/Li)+) Current density of 0.1A g-1、0.2A g-1、0.5A g-1、1.0A g-1、2.0A g-1、5.0A g-1、10.0A g-1
Assembling a lithium ion capacitor: using the mixed-phase niobium titanium oxide obtained in example 4 as a negative electrode and activated carbon as a positive electrode, 1.0mol L of the mixed-phase niobium titanium oxide dissolved in Ethylene Carbonate (EC) and dimethyl carbonate (DMC) (volume ratio 1:1) was added-1LiPF6Assembling a lithium ion capacitor by using a 2320 type polypropylene microporous membrane as a diaphragm as an electrolyte, and performing constant current charge and discharge test by using a CHI 760E electrochemical workstation, wherein the selected voltage range is 0-4.0V, and the current density is 0.1A g-1、0.2A g-1、0.5A g-1、1.0A g-1、2.0A g-1
FIG. 8 is a graph showing the rate capability of six mixed-phase niobium titanium oxides prepared in examples 1 to 6, wherein the phase composition obtained in example 4 is TiO2/TiNb2O7The mixed-phase niobium-titanium oxide has the highest specific capacity and the optimal rate capability, and the specific capacity is 0.1A g-1The specific capacity under the current density is as high as 300.3mAh g-1And at 10A g-1Can still maintain 205.1mAh g under the high current density-1. FIG. 9 is a graph showing the relationship between power density and energy density of a lithium ion capacitor assembled by using mixed-phase niobium titanium oxide prepared in example 4 as a negative electrode, and it can be seen that the assembled lithium ion capacitor is 200W kg-1The energy density at the power density is up to 149.6Wh kg-1And the excellent energy storage characteristics are proved again.
The present invention is not limited to the above exemplary embodiments, and any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. A preparation method of mixed-phase niobium-titanium oxide is characterized by comprising the following steps: firstly, preparing a mixed solution containing metal niobium salt and metal titanium salt, preparing a precursor by a solvothermal method, and then calcining at high temperature to obtain the mixed-phase niobium-titanium oxide.
2. The method of claim 1, comprising the steps of:
(1) preparing a precursor by a solvothermal method: weighing 0-5.0 mmol of metal niobium salt and 0-1.2 mmol of metal titanium salt, and dissolving in 5-50 mL of organic solvent to obtain a solution A; weighing 0.3-10 mmol of hexamethylenetetramine and dissolving in 50-150 mL of deionized water to obtain a solution B; adding the solution B into the solution A, uniformly mixing, carrying out a solvothermal reaction at a solvothermal temperature of 100-200 ℃ for 5-60 h, centrifuging, washing with water, drying, and collecting a powder product to obtain a precursor;
(2) preparing mixed-phase niobium-titanium oxide by high-temperature calcination: placing the precursor in a tube furnace, and calcining at high temperature under the protection of argon, wherein the calcining temperature is 500-900 ℃, the heat preservation time is 30-600 min, and the heating rate is 0.5-10 ℃ for min-1And naturally cooling to room temperature after the calcination is finished, thus obtaining the mixed-phase niobium-titanium oxide.
3. The method for producing mixed-phase niobium titanium oxide according to claim 1 or 2, characterized in that: the metal niobium salt is at least one of niobium chloride, niobium oxalate and ammonium niobium oxalate, and the metal titanium salt is at least one of titanium isopropoxide, titanyl sulfate, titanium tetrachloride, tetrabutyl titanate and n-butyl titanate.
4. The method of preparing mixed phase niobium titanium oxide as claimed in claim 2, wherein: in the step (1), the organic solvent is one or a mixture of any more of ethanol, methanol, ethylene glycol, N-dimethylformamide and N-methylpyrrolidone.
5. The method for producing mixed-phase niobium titanium oxide according to claim 1 or 2, characterized in that: the morphology and phase composition of the obtained mixed-phase niobium-titanium oxide can be regulated and controlled by regulating the molar ratio of the metal niobium salt to the metal titanium salt, so that the electrochemical energy storage characteristic of the obtained mixed-phase niobium-titanium oxide can be regulated and controlled.
6. A mixed-phase niobium titanium oxide obtained by the production method according to any one of claims 1 to 5.
7. An energy storage application of the mixed phase niobium titanium oxide of claim 6, wherein: the material is used as an electrode material of an electrochemical energy storage device or as a catalytic material or a sensing material.
CN202111198879.1A 2021-10-14 2021-10-14 Mixed-phase niobium-titanium oxide, and preparation method and energy storage application thereof Pending CN113772728A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111198879.1A CN113772728A (en) 2021-10-14 2021-10-14 Mixed-phase niobium-titanium oxide, and preparation method and energy storage application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111198879.1A CN113772728A (en) 2021-10-14 2021-10-14 Mixed-phase niobium-titanium oxide, and preparation method and energy storage application thereof

Publications (1)

Publication Number Publication Date
CN113772728A true CN113772728A (en) 2021-12-10

Family

ID=78871310

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111198879.1A Pending CN113772728A (en) 2021-10-14 2021-10-14 Mixed-phase niobium-titanium oxide, and preparation method and energy storage application thereof

Country Status (1)

Country Link
CN (1) CN113772728A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114789050A (en) * 2022-04-29 2022-07-26 浙江大学 Bimetal titanium niobium oxide, preparation method thereof and application of bimetal titanium niobium oxide as catalyst of hydrogen storage material

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150129797A1 (en) * 2013-11-08 2015-05-14 Kabushiki Kaisha Toshiba Production method of battery active material, battery active material, nonaqueous electrolyte battery and battery pack
US20150270541A1 (en) * 2014-03-18 2015-09-24 Kabushiki Kaisha Toshiba Active material, nonaqueous electrolyte battery, and battery pack
CN105575675A (en) * 2015-12-30 2016-05-11 哈尔滨工业大学 Method for preparing titanium-niobium composite oxide by water/solvothermal method and application of method in lithium-ion supercapacitor
CN109616628A (en) * 2018-11-26 2019-04-12 天津普兰能源科技有限公司 A kind of titanium niobium zirconium composite oxide electrode material, preparation method and application
CN110156081A (en) * 2019-05-22 2019-08-23 合肥学院 A kind of porous flake TiNb of negative electrode of lithium ion battery2O7Nanocrystalline preparation method
CN111646510A (en) * 2020-05-27 2020-09-11 武汉工程大学 High-rate titanium niobium oxide microsphere and preparation method and application thereof
CN112103493A (en) * 2020-08-13 2020-12-18 华北电力大学 Preparation method of lithium battery negative electrode material titanium-niobium composite oxide

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150129797A1 (en) * 2013-11-08 2015-05-14 Kabushiki Kaisha Toshiba Production method of battery active material, battery active material, nonaqueous electrolyte battery and battery pack
US20150270541A1 (en) * 2014-03-18 2015-09-24 Kabushiki Kaisha Toshiba Active material, nonaqueous electrolyte battery, and battery pack
CN105575675A (en) * 2015-12-30 2016-05-11 哈尔滨工业大学 Method for preparing titanium-niobium composite oxide by water/solvothermal method and application of method in lithium-ion supercapacitor
CN109616628A (en) * 2018-11-26 2019-04-12 天津普兰能源科技有限公司 A kind of titanium niobium zirconium composite oxide electrode material, preparation method and application
CN110156081A (en) * 2019-05-22 2019-08-23 合肥学院 A kind of porous flake TiNb of negative electrode of lithium ion battery2O7Nanocrystalline preparation method
CN111646510A (en) * 2020-05-27 2020-09-11 武汉工程大学 High-rate titanium niobium oxide microsphere and preparation method and application thereof
CN112103493A (en) * 2020-08-13 2020-12-18 华北电力大学 Preparation method of lithium battery negative electrode material titanium-niobium composite oxide

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SUNG-YUN LEE ET AL.: "Copper, zinc, and manganese niobates (CuNb2O6,ZnNb2O6, and MnNb2O6): structural characteristics, Li+ storage properties, and working mechanisms", 《INORG. CHEM. FRONT.》, 31 July 2020 (2020-07-31), pages 3176 - 3183 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114789050A (en) * 2022-04-29 2022-07-26 浙江大学 Bimetal titanium niobium oxide, preparation method thereof and application of bimetal titanium niobium oxide as catalyst of hydrogen storage material

Similar Documents

Publication Publication Date Title
CN102738458B (en) Surface modification method of lithium-rich cathode material
CN111244422A (en) Organic ion doped vanadium oxide positive electrode material for water-based zinc ion battery and preparation method and application thereof
CN102324511B (en) Preparation method for lithium ion battery composite cathode material
CN111244448B (en) In-situ carbon-coated high-rate large-size Prussian blue type sodium ion positive electrode material and preparation method thereof
Zhao et al. Titanium niobium oxides (TiNb2O7): Design, fabrication and application in energy storage devices
Wan et al. Pillow-shaped porous CuO as anode material for lithium-ion batteries
CN104900861B (en) A kind of lithium hydrogentitanate Li H Ti O material and preparation method thereof
CN112103493A (en) Preparation method of lithium battery negative electrode material titanium-niobium composite oxide
CN113851633B (en) Niobium-doped high-nickel ternary cathode material coated with niobium phosphate and preparation method thereof
CN103956475A (en) Method for preparing lithium titanate of lithium ion battery cathode material
CN103050679A (en) Spherical hollow porous MnO/C composite material and application thereof
CN113683120B (en) Mixed-phase niobium-based oxide and preparation method and energy storage application thereof
CN101704681B (en) Method for preparing lithium titanate with spinel structure
CN111943259B (en) Carbon-coated mesoporous dual-phase titanium dioxide and preparation method and energy storage application thereof
CN108511735A (en) A kind of modified lithium titanate composite material and preparation method and lithium ion battery
CN104810515A (en) Preparation method of doped Li4Ti5O12 anode material
TWI651272B (en) Process for producing lr-lnmo composite materials and use the same
CN108598458B (en) Nitrogen-doped lithium titanate composite material, preparation method thereof and lithium ion battery
CN104934577B (en) Mesoporous Li3VO4/C nano ellipsoid composite material embedded into graphene network, and preparation method and application of composite material
CN108281620B (en) Preparation method of negative electrode material titanium dioxide of sodium-ion battery
CN113772728A (en) Mixed-phase niobium-titanium oxide, and preparation method and energy storage application thereof
CN107994220A (en) LiMn2O4 composite material, its preparation method and the lithium ion battery that a kind of molybdenum doping is modified
CN110190277A (en) A kind of anode material for lithium-ion batteries LiMnO2@C and preparation method thereof
CN114792606A (en) Carbon-loaded manganese-doped sodium titanate energy storage material, preparation method and application thereof, and negative electrode plate
CN114906880A (en) Preparation method of positive electrode material of sodium-ion battery and sodium-ion battery

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
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20211210