CN105428633A - Method for preparing titanium niobate mesoporous microspheres - Google Patents
Method for preparing titanium niobate mesoporous microspheres Download PDFInfo
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- CN105428633A CN105428633A CN201510908762.6A CN201510908762A CN105428633A CN 105428633 A CN105428633 A CN 105428633A CN 201510908762 A CN201510908762 A CN 201510908762A CN 105428633 A CN105428633 A CN 105428633A
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- titanium
- niobate
- niobium
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- mesoporous
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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
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a method for preparing titanium niobate mesoporous microspheres. The method comprises the steps of mixing isopropyl alcohol with glycerin according to a certain proportion; adding a niobium source and a titanium source to the obtained solution; placing the obtained mixed liquid in a high pressure reactor to perform heating reaction; after cooling, obtaining the titanium niobate mesoporous microspheres through washing, drying and calcinating. The method has the advantages that the method is simple, convenient to implement and practical, and the product shape and size are easy to control. The prepared titanium niobate mesoporous microspheres have large specific surface area and pore volume, the electrochemical performance of titanium niobate is greatly improved, and particularly the large-multiplying-power charging and discharging cycle performance is greatly improved.
Description
Technical field
The application belongs to new energy materials field, specifically, relates to a kind of preparation method of titanium niobate mesoporous microsphere.
Background technology
Along with the enhancing of people's environmental consciousness, electric automobile more and more receives the concern of people.Although lithium ion battery is considered to the ideal power source of electric automobile, its fail safe, power density and specific capacity need further raising.Current business-like lithium ion battery generally with graphite-like material with carbon element for negative pole, carbon negative pole material easily causes the generation of Li dendrite, cause safety issue, carbon negative pole material can not carry out fast charging and discharging in addition.Though lithium titanate has high fail safe and excellent cyclical stability compared with material with carbon element, but its theoretical specific capacity lower (175mAh/g), be about 1/2nd of material with carbon element.
Titanium niobate (TiNb
2o
7) similar with lithium titanate, there is high electrode potential (1.65Vvs.Li
+/ Li), not easily cause the generation of Li dendrite, there is excellent fail safe; In charge and discharge process, change in volume is little, has excellent cyclical stability; And the theoretical specific capacity of this material (387mAh/g) is higher than the theoretical specific capacity of material with carbon element.Therefore, titanium niobate is considered to the power battery cathode material of very with prospects, gets more and more people's extensive concerning.But because the conductivity of this material is lower, make its high rate performance undesirable, constrain its commercial applications.
Current titanium niobate mainly adopts high temperature solid-state method to prepare, although the method technique is simple, easy large-scale production, its energy consumption is large, and the particle size of product is larger.Large particle size is unfavorable for the transmission of lithium ion and electronics, makes its chemical property poor.Mesoporous material has large specific area and pore volume, is conducive to the contact area increasing electrolyte and electrode material, can shortens the diffusion length of lithium ion and battery, reduce electrode polarization etc.The people such as Li take ethanol as solvent, utilize solvent structure to go out and assemble by nano particle the mesoporous microsphere formed, and show excellent chemical property (LiH, ShenL, PangG, FangS, LuoH, YangKandZhangX.TiNb
2o
7nanoparticlesassembledintohierarchicalmicrospheresashigh-ratecapabilityandlongcycle-lifeanodematerialsforlithiumi onbatteries.Nanoscale, 2015,7:619-624.).
Summary of the invention
In view of this, technical problems to be solved in this application there is provided a kind of preparation method of titanium niobate mesoporous microsphere, and the method can regulate and control sample topography and size by regulating the ratio of isopropyl alcohol and glycerol, reactant concentration, hydrothermal condition; The titanium niobate mesoporous microsphere of preparation has excellent chemical property as lithium ion battery negative material.
In order to solve the problems of the technologies described above, this application discloses a kind of preparation method of titanium niobate mesoporous microsphere, specifically comprising the following steps:
1) isopropyl alcohol and glycerol are mixed by a certain percentage, stir 0.1-20 hour;
2) titanium source and niobium source being joined step 1 respectively by atomic ratio titanium/niobium=0.4-0.9) in the mixed liquor for preparing, stir to clarify, wherein the concentration of titanium ion is 0.001-32mol/L;
3) by step 2) gained mixed liquor load inner liner polytetrafluoroethylene stainless steel cauldron in, be placed in thermostatic drying chamber, at 100-260 DEG C, heat 2-60 hour;
4) be cooled to room temperature after reaction, by gained precipitation respectively with deionized water and ethanol washing several, then at 60-130 DEG C, vacuumize obtains white powder;
5) by step 4) gained white powder roasting 1-65 hour at 350-1200 DEG C, obtain titanium niobate mesoporous material.
Further, step 1) in the volume ratio of isopropyl alcohol and glycerol be 1:10-8:1.
Further, step 2) in titanium source be one or more in titanyl sulfate, titanium tetrafluoride, titanium tetraisopropylate, titanium sulfate, titanium potassium oxalate, titanium tetrachloride, titanium trichloride, butyl titanate.
Further, step 2) in niobium source be one or more in niobium oxalate, ethanol niobium, columbium pentachloride, ammonium niobium oxalate.
Further, step 3) in heating-up temperature be 110-240 DEG C.
Further, step 5) in sintering temperature be 400-1000 DEG C.
Compared with prior art, the application can obtain and comprise following technique effect:
1) the titanium niobate mesoporous microsphere that prepared by the present invention has larger specific area and pore volume, adds the contact area of electrode material and electrolyte, significantly improves the chemical property of material.
2) the titanium niobate mesoporous microsphere prepared of the present invention, had both had the advantage that nano-electrode material the evolving path is short, had had again the advantage of micro materials good stability.
3) the present invention can regulate and control sample topography and size by regulating the ratio of propyl alcohol and glycerol, reactant concentration and hydrothermal condition.
4) to have technique simple in the present invention, and product pattern and size are easy to the features such as control, can the preparation of other inorganic functional material of extensive use.
Certainly, the arbitrary product implementing the application must not necessarily need to reach above-described all technique effects simultaneously.
Accompanying drawing explanation
Accompanying drawing described herein is used to provide further understanding of the present application, and form a application's part, the schematic description and description of the application, for explaining the application, does not form the improper restriction to the application.In the accompanying drawings:
Fig. 1 is the XRD figure that the embodiment of the present application 1 prepares titanium niobate mesoporous microsphere;
Fig. 2 is the stereoscan photograph that the embodiment of the present application 1 prepares titanium niobate mesoporous microsphere;
Fig. 3 is the chemical property curve chart that the embodiment of the present application 1 prepares titanium niobate mesoporous microsphere.
Embodiment
Drawings and Examples will be coordinated below to describe the execution mode of the application in detail, by this to the application how application technology means solve technical problem and the implementation procedure reaching technology effect can fully understand and implement according to this.
Embodiment 1
A isopropyl alcohol and glycerol mix in the ratio of 1:3 by (), stir 6 hours;
B titanium tetrachloride and columbium pentachloride join in above-mentioned mixed liquor by atomic ratio titanium/niobium=0.48 by () respectively, stir to clarify, and wherein the concentration of titanium ion is 0.17mol/L;
C step (b) gained mixed liquor loads in the stainless steel cauldron of inner liner polytetrafluoroethylene by (), be placed in thermostatic drying chamber, heats 32 hours at 130 DEG C;
D be cooled to room temperature after () reaction, by gained precipitation respectively with deionized water and ethanol washing several, then at 65 DEG C, vacuumize obtains white powder.
E (), by the roasting 35 hours at 600 DEG C of step (d) gained white powder, obtains titanium niobate mesoporous material.
As shown in Figure 1, the diffraction maximum of sample and the standard diffraction peak of titanium niobate fit like a glove the XRD figure of the titanium niobate mesoporous microsphere prepared by embodiment 1, and do not find impurity peaks, interpret sample is purer; And diffraction maximum is wider, the particle size of interpret sample is less.As shown in Figure 2, sample topography is uniform microballoon to the stereoscan photograph of the titanium niobate mesoporous microsphere prepared by embodiment 1, and can observe obvious hole on the surface of microballoon; In addition as can be seen from super loose microballoon, microballoon is assembled by nano particle and is formed.As shown in Figure 3, sample shows good high rate performance to the chemical property curve chart of the titanium niobate mesoporous microsphere prepared by embodiment 1, and the capacity under 20C multiplying power is about 220mAh/g; Capacity under 50C multiplying power still can remain on about 170mAh/g.
Embodiment 2
A isopropyl alcohol and glycerol mix in 1:5 ratio by (), stir 6 hours;
B butyl titanate and ethanol niobium join in above-mentioned mixed liquor by atomic ratio titanium/niobium=0.7 by () respectively, stir to clarify, and wherein the concentration of titanium ion is 3.2mol/L;
C step (b) gained mixed liquor loads in the stainless steel cauldron of inner liner polytetrafluoroethylene by (), be placed in thermostatic drying chamber, heats 20 hours at 160 DEG C;
D be cooled to room temperature after () reaction, by gained precipitation respectively with deionized water and ethanol washing several, then at 80 DEG C, vacuumize obtains white powder.
E (), by the roasting 13 hours at 980 DEG C of step (d) gained white powder, obtains titanium niobate mesoporous material.
Embodiment 3
A) be 1:10 mixing by volume by isopropyl alcohol and glycerol, stir 0.1 hour;
B) titanium tetraisopropylate and ethanol niobium joined respectively in the mixed liquor that step a) prepares by atomic ratio titanium/niobium=0.4, stir to clarify, wherein the concentration of titanium ion is 0.001mol/L;
C) by step b) gained mixed liquor load inner liner polytetrafluoroethylene stainless steel cauldron in, be placed in thermostatic drying chamber, at 100 DEG C heat 60 hours;
D) be cooled to room temperature after reaction, by gained precipitation respectively with deionized water and ethanol washing several, then at 60 DEG C, vacuumize obtains white powder;
E) by steps d) roasting 65 hours at 450 DEG C of gained white powder, obtain titanium niobate mesoporous material.
Embodiment 4
A) be 8:1 mixing by volume by isopropyl alcohol and glycerol, stir 20 hours;
B) titanium sulfate and columbium pentachloride joined respectively in the mixed liquor that step a) prepares by atomic ratio titanium/niobium=0.9, stir to clarify, wherein the concentration of titanium ion is 12mol/L;
C) by step b) gained mixed liquor load inner liner polytetrafluoroethylene stainless steel cauldron in, be placed in thermostatic drying chamber, at 260 DEG C heat 2 hours;
D) be cooled to room temperature after reaction, by gained precipitation respectively with deionized water and ethanol washing several, then at 130 DEG C, vacuumize obtains white powder;
E) by steps d) roasting 1 hour at 1100 DEG C of gained white powder, obtain titanium niobate mesoporous material.
Embodiment 5
A) be 2:1 mixing by volume by isopropyl alcohol and glycerol, stir 12 hours;
B) titanium potassium oxalate and ammonium niobium oxalate joined respectively in the mixed liquor that step a) prepares by atomic ratio titanium/niobium=0.6, stir to clarify, wherein the concentration of titanium ion is 10mol/L;
C) by step b) gained mixed liquor load inner liner polytetrafluoroethylene stainless steel cauldron in, be placed in thermostatic drying chamber, at 110 DEG C heat 24 hours;
D) be cooled to room temperature after reaction, by gained precipitation respectively with deionized water and ethanol washing several, then at 75 DEG C, vacuumize obtains white powder;
E) by steps d) roasting 45 hours at 400 DEG C of gained white powder, obtain titanium niobate mesoporous material.
Embodiment 6
A) be 1:1 mixing by volume by isopropyl alcohol and glycerol, stir 4 hours;
B) butyl titanate and niobium oxalate joined respectively in the mixed liquor that step a) prepares by atomic ratio titanium/niobium=0.75, stir to clarify, wherein the concentration of titanium ion is 4mol/L;
C) by step b) gained mixed liquor load inner liner polytetrafluoroethylene stainless steel cauldron in, be placed in thermostatic drying chamber, at 240 DEG C heat 12 hours;
D) be cooled to room temperature after reaction, by gained precipitation respectively with deionized water and ethanol washing several, then at 60-130 DEG C, vacuumize obtains white powder;
E) by steps d) roasting 55 hours at 1000 DEG C of gained white powder, obtain titanium niobate mesoporous material.
In the preparation process in accordance with the present invention, the ratio of isopropyl alcohol and glycerol is most important to formation spherical morphology: can not get spherical morphology when solvent is only isopropyl alcohol, in addition because glycerol viscosity is larger, not easily stir when being all glycerol, follow-up centrifugal, drying all comparatively difficulty, and its price is higher.In the selection of reaction temperature: the heat resisting temperature of general polytetrafluoroethylene reactor is less than 260 DEG C, and temperature crosses higher position needs special substance, expensive, and dangerous large; May can not react when temperature is too low, can not get product.Sintering temperature can affect degree of crystallinity and the size of product, and temperature is too high to waste energy, and the particle size of material can be made to grow up; The too low meeting of temperature makes the crystallization of material bad or can not get titanium niobate material.
Above-mentioned explanation illustrate and describes some preferred embodiments of the present invention, but as previously mentioned, be to be understood that the present invention is not limited to the form disclosed by this paper, should not regard the eliminating to other embodiments as, and can be used for other combinations various, amendment and environment, and can in invention contemplated scope described herein, changed by the technology of above-mentioned instruction or association area or knowledge.And the change that those skilled in the art carry out and change do not depart from the spirit and scope of the present invention, then all should in the protection range of claims of the present invention.
Claims (6)
1. a preparation method for titanium niobate mesoporous microsphere, is characterized in that, specifically comprises the following steps:
1) isopropyl alcohol and glycerol are mixed by a certain percentage, stir 0.1-20 hour;
2) titanium source and niobium source being joined step 1 respectively by atomic ratio titanium/niobium=0.4-0.9) in the mixed liquor for preparing, stir to clarify, wherein the concentration of titanium ion is 0.001-32mol/L;
3) by step 2) gained mixed liquor load inner liner polytetrafluoroethylene stainless steel cauldron in, be placed in thermostatic drying chamber, at 100-260 DEG C, heat 2-60 hour;
4) be cooled to room temperature after reaction, by gained precipitation respectively with deionized water and ethanol washing several, then at 60-130 DEG C, vacuumize obtains white powder;
5) by step 4) gained white powder roasting 1-65 hour at 350-1200 DEG C, obtain titanium niobate mesoporous material.
2. the preparation method of titanium niobate mesoporous microsphere as claimed in claim 1, is characterized in that, described step 1) in the volume ratio of isopropyl alcohol and glycerol be 1:10-8:1.
3. the preparation method of titanium niobate mesoporous microsphere as claimed in claim 1, it is characterized in that, described step 2) in titanium source be one or more in titanyl sulfate, titanium tetrafluoride, titanium tetraisopropylate, titanium sulfate, titanium potassium oxalate, titanium tetrachloride, titanium trichloride, butyl titanate.
4. the preparation method of titanium niobate mesoporous microsphere as claimed in claim 1, is characterized in that, described step 2) in niobium source be one or more in niobium oxalate, ethanol niobium, columbium pentachloride, ammonium niobium oxalate.
5. the preparation method of titanium niobate mesoporous microsphere as claimed in claim 1, is characterized in that, described step 3) in heating-up temperature be 110-240 DEG C.
6. the preparation method of titanium niobate mesoporous microsphere as claimed in claim 1, is characterized in that, described step 5) in sintering temperature be 400-1000 DEG C.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105633456A (en) * | 2016-04-07 | 2016-06-01 | 南阳师范学院 | Preparation method of lithium ion battery negative material titanium niobate |
| CN105776334A (en) * | 2016-04-07 | 2016-07-20 | 南阳师范学院 | Spherical Ti2Nb10O29 material and preparation method thereof |
| CN105958049A (en) * | 2016-06-23 | 2016-09-21 | 南阳师范学院 | TiNb<6>O<17> negative electrode material, preparation method thereof and lithium ion battery |
| CN105958113A (en) * | 2016-06-23 | 2016-09-21 | 南阳师范学院 | Niobium pentoxide mesoporous microsphere electrode material and preparation method therefor |
| CN106025255A (en) * | 2016-06-23 | 2016-10-12 | 南阳师范学院 | Spherical Nb2O5 electrode material and preparation method thereof |
| CN106025285A (en) * | 2016-06-23 | 2016-10-12 | 南阳师范学院 | Spherical titanium niobate electrode material and preparation method thereof |
| CN106129402A (en) * | 2016-06-23 | 2016-11-16 | 南阳师范学院 | A kind of Ti2nb10o29mesoporous microsphere and preparation method thereof |
| CN106519660A (en) * | 2016-11-10 | 2017-03-22 | 佛山慧创正元新材料科技有限公司 | Anti-mildewing nylon cable material and preparation method thereof |
| CN107601564A (en) * | 2017-09-04 | 2018-01-19 | 北京工业大学 | A kind of method of alcoholic solvent hot preparation niobic acid tin nanosphere |
| CN109888245A (en) * | 2019-03-21 | 2019-06-14 | 浙江大学 | Titanium niobium oxygen/carbon composite and its preparation method and application that Lacking oxygen and carbon coating are adjusted |
| 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 |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105633456A (en) * | 2016-04-07 | 2016-06-01 | 南阳师范学院 | Preparation method of lithium ion battery negative material titanium niobate |
| CN105776334A (en) * | 2016-04-07 | 2016-07-20 | 南阳师范学院 | Spherical Ti2Nb10O29 material and preparation method thereof |
| CN105776334B (en) * | 2016-04-07 | 2017-12-15 | 南阳师范学院 | A kind of spherical Ti2Nb10O29Material and preparation method thereof |
| CN106025255A (en) * | 2016-06-23 | 2016-10-12 | 南阳师范学院 | Spherical Nb2O5 electrode material and preparation method thereof |
| CN105958113A (en) * | 2016-06-23 | 2016-09-21 | 南阳师范学院 | Niobium pentoxide mesoporous microsphere electrode material and preparation method therefor |
| CN106025285A (en) * | 2016-06-23 | 2016-10-12 | 南阳师范学院 | Spherical titanium niobate electrode material and preparation method thereof |
| CN106129402A (en) * | 2016-06-23 | 2016-11-16 | 南阳师范学院 | A kind of Ti2nb10o29mesoporous microsphere and preparation method thereof |
| CN105958049A (en) * | 2016-06-23 | 2016-09-21 | 南阳师范学院 | TiNb<6>O<17> negative electrode material, preparation method thereof and lithium ion battery |
| CN106519660A (en) * | 2016-11-10 | 2017-03-22 | 佛山慧创正元新材料科技有限公司 | Anti-mildewing nylon cable material and preparation method thereof |
| CN106519660B (en) * | 2016-11-10 | 2018-12-21 | 盐城庆达新材料有限公司 | A kind of mould proof nylon cable material and preparation method thereof |
| CN107601564A (en) * | 2017-09-04 | 2018-01-19 | 北京工业大学 | A kind of method of alcoholic solvent hot preparation niobic acid tin nanosphere |
| CN107601564B (en) * | 2017-09-04 | 2019-06-07 | 北京工业大学 | A kind of method of alcoholic solvent hot preparation niobic acid tin nanosphere |
| CN109888245A (en) * | 2019-03-21 | 2019-06-14 | 浙江大学 | Titanium niobium oxygen/carbon composite and its preparation method and application that Lacking oxygen and carbon coating are adjusted |
| CN109888245B (en) * | 2019-03-21 | 2021-01-15 | 浙江大学 | Titanium niobium oxygen/carbon composite material with oxygen vacancy and carbon coating adjustment 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 |
| 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 |
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Inventor after: Qiao Zhanping Inventor after: Hu Min Inventor after: Liu Miao Inventor after: Hu Yingtao Inventor after: Duan Xinying Inventor after: Liu Guangyin Inventor before: Liu Guangyin Inventor before: Bao Keyan Inventor before: Guo Jiali Inventor before: Zhang Ruixue Inventor before: Sun Ruixue Inventor before: Xie Haiquan Inventor before: Liu Wenmin Inventor before: Yang Hao Inventor before: Ji Xiaoguang |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180511 Termination date: 20181209 |