CN102531050B - Method for preparing TiO2 (B) nano wires and application of prepared TiO2 (B) nano wires - Google Patents
Method for preparing TiO2 (B) nano wires and application of prepared TiO2 (B) nano wires Download PDFInfo
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- CN102531050B CN102531050B CN 201010614211 CN201010614211A CN102531050B CN 102531050 B CN102531050 B CN 102531050B CN 201010614211 CN201010614211 CN 201010614211 CN 201010614211 A CN201010614211 A CN 201010614211A CN 102531050 B CN102531050 B CN 102531050B
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Abstract
The invention discloses a method for preparing TiO2 (B) nano wires with high specific surface area. The method comprises the following steps of: preparing potassium titanate nano wires in a concentrated potassium hydroxide solution by using titanium oxide powder and adopting a hydrothermal or heating method, washing, performing acid exchange and secondary hydrothermal conversion, controlling the acid concentration and the reaction temperature of the hydrothermal reaction, and thus obtaining a large quantity of TiO2 (B) nano wires with the high specific surface. The prepared TiO2 (B) nano wires with the high specific surface have a good application prospect in the fields of lithium ion batteries, water treatment, sensors, sensitized solar cells and the like. Particularly, the TiO2 (B) nano wires applied to a cathode material for the lithium ion batteries have large capacity and can still keep large capacity at a high charge/discharge rate.
Description
Technical field
The present invention relates to a kind of high-specific surface area TiO for preparing
2(B) method of nano wire and TiO
2(B) nano wire is in the purposes of lithium ion battery, water treatment, sensing, field of dye-sensitized solar cells.
Background technology
Titanium dioxide, because it has broad application prospects in photochemical catalysis, lithium ion battery, dye sensitization solar battery, photodissociation water and sensor field, has become the focus of Material Field research.
Common titanium dioxide mainly comprises sharp titanium (I4
1/ amd), rutile (P4
2/ mnm), plate state (Pbca) and TiO
2(B) (C2/m) four kinds of crystalline phases.Different crystalline phases has different physicochemical property, thereby shows different functions.In all crystalline phases, form TiO
2(B) titanyl octahedral body crosslinking method is the most loose, makes it have larger interlamellar spacing and less density, thereby has superior performance aspect lithium ion battery.
Up to the present, the TiO reported
2(B) make peace greatly document (Armstrong, A.R. of the synthetic method of nano wire; Armstrong, G.; Canales, J.; Bruce, P.G.Angew.Chem.Int.Ed.2004,43,2286.) consistent.Synthesis mode is as follows: at first from the titanyl powder, adopt hydrothermal method to obtain the sodium titanate nano wire under dense sodium hydroxide condition; After exchanging by hydrogen ion, the sodium titanate nano wire is converted into to the metatitanic acid nano wire; Finally metatitanic acid is annealed, controlled temperature at 400-500 ℃, metatitanic acid is converted into to TiO
2(B) nano wire.The TiO that this mode prepares
2(B) nanowire size is larger, has less specific surface area and (usually is less than 50m
2/ g).
TiO
2(B) direction of growth of size, pattern and crystal can affect its application in lithium ion battery to a large extent.As little size can shorten the transmission range of lithium ion and electronics, enlarge the contact area of electrode and electrolytic solution, the minimizing current density.One dimension TiO
2(B) nanostructure is conducive to electronics along motion along the long axis, and short-axis direction is conducive to quick insertion and the de-embedding of lithium ion.Equally, lithium ion is at TiO
2(B) disalignment in show different rate of migration, the order of its rate of migration be b>c>>the a-axle.Therefore, regulation and control TiO
2(B) size, pattern and the direction of growth are extremely important, especially in the directions such as charge-discharge performance that improve lithium ion battery.
Summary of the invention
The invention provides a kind of high-specific surface area TiO for preparing
2(B) method of nano wire reaches the TiO made thus
2(B) purposes of nano wire.The method is from the titanyl powder, at first adopt the method for hydro-thermal or heating to prepare Nano lines of potassium titanate in dense potassium hydroxide solution, after washing, acid exchange, carry out again the intermediate water thermal transition, by controlling acid concentration and the temperature of reaction of hydro-thermal reaction, obtained a large amount of TiO with high-specific surface area
2(B) nano wire.
In order to make the TiO obtained
2(B) nanowire properties further improves, TiO also prepared hydro-thermal by the present invention
2(B) nano wire carries out aftertreatment, comprises Annealing Crystallization processing and finishing.
The TiO that the present invention prepares
2(B) nano thread structure has one-dimentional structure, less particle diameter, high specific surface area, and short b-axle and c-axle (Fig. 3 and Fig. 4).
According to this high-specific surface area TiO
2(B) unique distinction of nano wire, can be applied to the negative material of lithium ion battery, or be applied to the fields such as water treatment, sensing, dye sensitization solar battery.
Preparation method's flow process of the present invention as shown in Figure 1.Wherein 1 is the titanyl powder, and 2 is potassium hydroxide aqueous solution, and 3 is Nano lines of potassium titanate, and 4 is acid solution, and 5 is the Nano lines of potassium titanate after the acid exchange, and 6 is acid solution, and 7 is TiO
2(B) nano wire.Titanyl powder 1 and potassium hydroxide aqueous solution 2 mix by after hydro-thermal or reacting by heating a, obtaining Nano lines of potassium titanate 3; Through filtering, carry out the acid exchange after washing and obtain Nano lines of potassium titanate 5 in acid solution 4; Carry out hydro-thermal reaction b after washing in acid solution 6 after filtration again, dry and make TiO after filtration washing
2(B) nano wire 7.
Various processing condition in preparation process of the present invention are as follows:
1. titanyl powder: can be TiO
2powder, metatitanic acid, positive metatitanic acid, potassium titanate, titanyl sulfate, titanium tetrachloride or their combination.
2. the selection of acid concentration: the concentration of acid solution 4 is at 0.001-1mol/L, and the concentration of acid solution 6 is between 0.01-0.4mol/L.
3. the concentration of potassium hydroxide: 5-20mol/L.
4. the temperature of hydrothermal temperature and time: hydro-thermal reaction a is 100-250 ℃, and the temperature of reacting by heating a is 80-120 ℃.Time is 5-120 hour, concrete relevant with temperature of reaction with the selection of titanyl powder; The temperature of hydro-thermal reaction b is 100-250 ℃, and the time is 1-72 hour.
5. washing: must be through multiple times of filtration and washing after hydro-thermal reaction a.
6. dry: dry purpose is in order to remove the moisture of precipitation absorption, can or adopt 30-60 ℃ of vacuum-drying 60-100 ℃ of drying.
TiO prepared by the present invention
2(B) when nano wire is as lithium ion battery negative material, because it has one-dimentional structure, less particle diameter, high specific surface area, and the characteristics (Fig. 3 and Fig. 4) such as short b-axle and c-axle, showed good cycle performance.Especially still can keep higher capacity under fast charging and discharging speed.In order better to embody this TiO
2(B) performance of lithium ion battery of nano wire, can carry out aftertreatment to it, comprises Annealing Crystallization processing and finishing.Wherein, the temperature that Annealing Crystallization is processed is between 200-600 ℃, and the purpose of annealing is to improve TiO
2(B) degree of crystallinity of nano wire; Finishing comprises load carbon, ruthenium oxide, metal platinum, Jin Heyin, for improving TiO
2(B) electroconductibility of nano wire.
TiO prepared by the method
2(B) nano wire has high-specific surface area, low cost, monocrystalline, the easily separated and characteristics such as can be recycled, aspect Adsorption of Organic and degraded, the field such as water treatment, sensing, dye sensitization solar battery has wide practical use.
The invention has the advantages that:
1. the TiO that the method obtains
2(B) there is one-dimentional structure and short b-axle and c-axle (Fig. 4).
2. the TiO that the method obtains
2(B) nano wire has less particle diameter and bigger serface very, is (Fig. 3) that other method can't realize.
3. preparation technology is simple, and processing parameter is easy to control, is easy to large-scale industrial production.
4. raw material is easy to get, and production cost is lower.
5. by controlling processing parameter, can obtain TiO under given conditions
2(B) monocrystal nanowire, the purity of product high (being greater than 95%).
TiO of the present invention
2(B) nano wire is for the advantage of lithium ion battery negative material:
1. capacity is high, and capacity reaches 388mAh g first
-1, i.e. Li
1.15tiO
2.In all titanium-oxygen system of having reported at present, for lithium ion battery negative, the effect best material.
2. cycle efficiency is high.Repeatedly discharge and recharge, capacity descends hardly.
3. fast charging and discharging performance is good.Under fast charging and discharging speed, still keep large capacity, surmounted all results of in the past reporting based on titanium-oxygen system.
4. it is carried out to aftertreatment, can further improve effect.
TiO of the present invention
2(B) nano wire is for the advantage of other field:
1. larger specific surface area, can adsorb more organism or heavy metal ion, plays the effect of fractionation by adsorption.
2. have photocatalytic activity, the product of photocatalysis to degrade organic matter is carbonic acid gas and water, does not produce secondary pollution.
3. larger specific surface area, can adsorb more dyestuff, and one-dimentional structure is conducive to the transmission of electronics simultaneously, aspect dye sensitization solar battery, has superiority.
4. larger specific surface area, be conducive to gas sensing, as be applied to the sensing of the gases such as hydrogen, oxygen, steam.
The accompanying drawing explanation
Fig. 1 is preparation method's flow process of the present invention;
Fig. 2 is Nano lines of potassium titanate (a) and the TiO of the acid exchange of embodiment 1 preparation
2(B) the x x ray diffration pattern x of nano wire (b);
Fig. 3 is Nano lines of potassium titanate (a) and the TiO of the acid exchange of embodiment 1 preparation
2(B) scintigram of nano wire (b), the TiO prepared
2(B) particle diameter of nano wire is 2-30nm, and very large length-to-diameter ratio is arranged, and has high specific surface area;
Fig. 4 is TiO prepared by method that the embodiment of the present invention 1 provides
2(B) transmission electron microscope photo of nano wire (a) and high resolution transmission photo (b), a schemes visible TiO
2(B) nano wire has very little particle diameter, and b figure has disclosed TiO
2(B) direction of growth of nano wire is<110>direction.Can find out this TiO by simulation picture c, d
2(B) nano wire has short b-axle and c-axle, i.e. TiO
2(B) diameter of nano wire;
Fig. 5 is the high TiO of crystallization degree of embodiment 3 preparations
2(B) the x x ray diffration pattern x of nano wire;
Fig. 6 is the TiO of embodiment 1 preparation
2(B) nano wire is applied to the first charge-discharge capacity plan of lithium ion battery;
Fig. 7 is the TiO of embodiment 1 preparation
2(B) nano wire is applied to the capacity circulating figure of lithium ion battery;
Fig. 8 is the TiO of embodiment 1 preparation
2(B) when nano wire is applied to lithium ion battery, the capacity circulating figure under different charge-discharge velocities.
Embodiment
Further illustrate technical scheme of the present invention by the following examples and Comparative Examples, but the application's protection atmosphere is not subject to the restriction of the actual conditions of these embodiment.
2g titanium oxide (Deguass P25) is dispersed in the potassium hydroxide solution of 80mL 10mol/L, solution is transferred in water heating kettle, be heated to 200 ℃, constant temperature 24 hours, after temperature of reaction kettle is down to room temperature, water heating kettle is taken out, and to falling supernatant liquid, the bottom white solid is transferred in beaker, ultrasonic dispersion, with deionized water, repeatedly wash, centrifugation, until washings pH value reaches 9-11.Add the 0.1mol/L salpeter solution to the solution souring, ultrasonic and standing more than 6 hours, make H
+ion can be by the K in nano wire
+the ion major part exchanges.With deionized water, repeatedly wash, centrifugation, until washings pH approaches neutrality, 80 ℃ of dryings.0.1-1.0g metatitanic acid nano wire is distributed in the salpeter solution of 40mL 0.1mol/L, solution is shifted in water heating kettle, be warming up to 150 ℃, constant temperature 24 hours, be down to room temperature when reactor, repeatedly wash with deionized water, centrifugation, until washings pH value reaches neutral, 80 ℃ of dryings, obtain TiO
2(B) nano wire.
The 2g metatitanic acid is dispersed in the potassium hydroxide solution of 80mL 6mol/L, solution is transferred in water heating kettle, be heated to 240 ℃, constant temperature 48 hours, after temperature of reaction kettle is down to room temperature, water heating kettle is taken out, and to falling supernatant liquid, the bottom white solid is transferred in beaker, ultrasonic dispersion, with deionized water, repeatedly wash, centrifugation, until washings pH value reaches 9-11.Add the 0.001-1mol/L hydrochloric acid soln to the solution souring, ultrasonic and standing more than 12 hours, make H
+ion can be by the K in nano wire
+the ion major part exchanges.With deionized water, repeatedly wash, centrifugation, until washings pH approaches neutrality, 80 ℃ of dryings.0.1-1.0g metatitanic acid nano wire is distributed in the hydrochloric acid soln of 40mL 0.3mol/L, solution is shifted in water heating kettle, be warming up to 180 ℃, constant temperature 12 hours, be down to room temperature when reactor, with deionized water, repeatedly washs, centrifugation, until washings pH value reaches neutral, 60 ℃ of vacuum-dryings, obtain TiO
2(B) nano wire.
Embodiment 3
The 2g potassium titanate is dispersed in the potassium hydroxide solution of 80mL 15mol/L, solution is transferred in water heating kettle, be heated to 220 ℃, constant temperature 8 hours, after temperature of reaction kettle is down to room temperature, water heating kettle is taken out, and to falling supernatant liquid, the bottom white solid is transferred in beaker, ultrasonic dispersion, with deionized water, repeatedly wash, centrifugation, until washings pH value reaches 9-11.Add the 0.001-1mol/L salpeter solution to the solution souring, ultrasonic and standing 12 hours, make H
+ion can be by the K in nano wire
+the ion major part exchanges.With deionized water, repeatedly wash, centrifugation, until washings pH approaches neutrality, 80 ℃ of dryings.0.1-1.0g metatitanic acid nano wire is distributed in the salpeter solution of 40mL 0.8mol/L, solution is shifted in water heating kettle, be warming up to 220 ℃, constant temperature 5 hours, be down to room temperature when reactor, repeatedly wash with deionized water, centrifugation, until washings pH value reaches neutral, 80 ℃ of dryings, obtain TiO
2(B) nano wire.
Embodiment 4
The 2g titanium oxide is dispersed in the potassium hydroxide solution of 80mL 20mol/L, solution is transferred in plastic flask, stirring heating, reaction is 72 hours under 105 ℃, after temperature of reaction is down to room temperature, to falling supernatant liquid, the bottom white solid is transferred in beaker, and ultrasonic dispersion, repeatedly wash with deionized water, centrifugation, until washings pH value reaches 9-11.Add the 0.1M hydrochloric acid soln to the solution souring, ultrasonic and standing more than 6 hours, make H
+ion can be by the K in nano wire
+the ion major part exchanges.With deionized water, repeatedly wash, centrifugation, until washings pH approaches neutrality, 60 ℃ of vacuum-dryings.0.1-1g metatitanic acid nano wire is distributed in the hydrochloric acid soln of 80mL 0.01-1mol/L, solution is shifted in water heating kettle, be warming up to 100 ℃, constant temperature 72 hours, be down to room temperature when reactor, with deionized water, repeatedly washs, centrifugation, until washings pH value reaches neutral, 60 ℃ of vacuum-dryings, obtain TiO
2(B) nano wire.
Embodiment 5
TiO
2(B) Annealing Crystallization of nano wire is processed, and improves its degree of crystallinity.
By TiO
2(B) nano wire is put into retort furnace, and under air atmosphere, the temperature rise rate of 5 °/min, rise to 400 ℃, and 2h anneals under 400 ℃.
Embodiment 6
TiO
2(B) finishing of nano wire, improve its electroconductibility.
Get 1g TiO
2(B) nano wire is placed in beaker, adds a small amount of deionized water fully to infiltrate, then adds 0.05g sucrose, fully stirs and makes sucrose can evenly spread to carrier surface, then beaker is put into to 80 degree water-baths and is heated, until evaporate to dryness takes out.The sample of absorption sucrose is put into to U-shaped silica tube, and 400 ℃ of roasting 2h under inert atmosphere, can make the TiO of carbon load
2(B) nano wire.
Embodiment 7
TiO
2(B) nano wire is for the negative material of lithium ion battery
Get TiO
2(B) nano wire, carbon black, polyvinylidene difluoride (PVDF) binding agent mix according to a certain percentage, and its compression is made to working electrode.Lithium hexafluoro phosphate, as electrolytic solution, is tested the charge-discharge performance of its lithium ion battery under the system of anhydrous and oxygen-free.Capacity reaches 388mA h g first
-1, i.e. Li
1.15tiO
2.At charge-discharge velocity, be 2000mA g
-1the time, still can keep 140mA h g
-1capacity.
TiO
2(B) nano wire is for water treatment absorption degradation organic dye
20mg TiO
2(B) nano wire joins in the aqueous solution of methylene blue of 100mL 10mg/L and carries out dye adsorption degraded, under obstructed oxygen condition, irradiates and is degraded with 8 watts of ultraviolet lamps (254nm), this TiO
2(B) nano wire has certain dye adsorption ability and rate of photocatalytic oxidation.
Finally it should be noted that publicizing and implementing routine purpose is to help further to understand the present invention, but it will be appreciated by those skilled in the art that: without departing from the spirit and scope of the invention and the appended claims, various substitutions and modifications are all possible.Therefore, the present invention should not be limited to the disclosed content of embodiment, and the scope that the scope of protection of present invention defines with claims is as the criterion.
Claims (7)
1. a TiO
2(B) preparation method of nano wire, its step comprises:
1) titanyl powder and potassium hydroxide aqueous solution mix by after hydro-thermal or reacting by heating, obtaining Nano lines of potassium titanate;
2) through filtering, carry out ion-exchange after washing in acidic aqueous solution;
3) carry out hydro-thermal reaction after washing in acidic aqueous solution after filtration again, the concentration of acidic aqueous solution is between 0.01-0.4mol/L, and the temperature of hydro-thermal reaction is 100-250 ℃, and the time is 1-72 hour, dry and make TiO after filtration washing
2(B) nano wire.
2. the method for claim 1, is characterized in that step 1) in, described titanyl powder is selected from TiO
2a kind of in powder, metatitanic acid, positive metatitanic acid, potassium titanate, titanyl sulfate, titanium tetrachloride or their combination.
3. the method for claim 1, is characterized in that step 1) in, the concentration of described potassium hydroxide aqueous solution is 5-20mol/L.
4. the method for claim 1, is characterized in that step 1) in, if adopt hydro-thermal reaction, temperature is 100-250 ℃, if adopt the reflux stirring reaction, temperature is 80-120 ℃, and the time is 5-120 hour.
5. the method for claim 1, is characterized in that step 2) in, the concentration of described acidic aqueous solution is between 0.001-1mol/L.
6. the arbitrary described method of claim 1-5, is characterized in that, to the TiO made
2(B) nano wire carries out the Annealing Crystallization processing, and wherein annealing temperature is between 200-600 ℃.
7. the arbitrary described method of claim 1-5, is characterized in that, to the TiO made
2(B) nano wire carries out finishing, and this finishing comprises load carbon, ruthenium oxide, metal platinum, Jin Heyin.
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| CN103427076B (en) * | 2013-07-12 | 2016-08-10 | 新疆大学 | A kind of solid state reaction prepares TiO2the method of-B nano material |
| CN104098134A (en) * | 2014-07-07 | 2014-10-15 | 北京大学 | Preparation method and application of TiO2 nanotube coated with amorphous layer |
| CN104649319B (en) * | 2015-03-02 | 2016-02-10 | 北华大学 | A kind of TiO 2(B) preparation method of nanosponges |
| CN105217679A (en) * | 2015-11-04 | 2016-01-06 | 上海电机学院 | A kind of mesoporous TiO 2-B nano wire and preparation method thereof |
| CN105826546B (en) * | 2016-03-28 | 2018-07-20 | 福建师范大学 | A kind of TiO2Thin nano wire of B ultrasound and the preparation method and application thereof |
| CN107952423A (en) * | 2016-10-18 | 2018-04-24 | 天津大学 | A kind of titanium dioxide high-efficiency photocatalysis material of 2D and preparation method thereof |
| CN107227510B (en) * | 2017-05-17 | 2019-10-18 | 华南农业大学 | A kind of preparation method of modifying titanium dioxide fiber |
| CN108899549A (en) * | 2018-07-14 | 2018-11-27 | 西南大学 | Carbon coating TiO in situ2(B) preparation method and application of negative electrode material |
| CN109052464B (en) * | 2018-08-09 | 2020-10-16 | 陕西师范大学 | High-temperature phase TiO2(B) Method for producing a material |
| CN109264774A (en) * | 2018-08-30 | 2019-01-25 | 中国石油天然气股份有限公司 | A kind of preparation method of the titanate with hierarchical structure of size tunable, metatitanic acid and titanium dioxide |
| CN109179492B (en) * | 2018-08-30 | 2021-01-29 | 中国石油天然气股份有限公司 | Lithium titanate nano-particles and preparation method and application thereof |
| CN109279649B (en) | 2018-08-30 | 2021-01-29 | 中国石油天然气股份有限公司 | Preparation method of lithium titanate with nanotube hierarchical structure, application of lithium titanate and product |
| CN109133166B (en) * | 2018-08-30 | 2021-01-29 | 中国石油天然气股份有限公司 | Titanium dioxide porous nanowire and preparation method thereof |
| CN108946798B (en) * | 2018-09-06 | 2021-04-30 | 中国石油天然气股份有限公司 | Linear hierarchical structure lithium titanate material and preparation and application thereof |
| CN108975390B (en) * | 2018-09-06 | 2021-01-29 | 中国石油天然气股份有限公司 | Linear hierarchical structure lithium titanate and preparation method and application thereof |
| CN110518216B (en) * | 2019-09-03 | 2024-03-15 | 银隆新能源股份有限公司 | Negative electrode composite material of sodium ion battery and preparation method thereof |
| CN110627117A (en) * | 2019-09-23 | 2019-12-31 | 聊城大学 | Porous anatase type TiO2Preparation method and application of nanowire bundle |
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Granted publication date: 20131225 Termination date: 20191230 |