CN102826600A - Method for preparing titanium dioxide nanowire - Google Patents
Method for preparing titanium dioxide nanowire Download PDFInfo
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- CN102826600A CN102826600A CN201210351453XA CN201210351453A CN102826600A CN 102826600 A CN102826600 A CN 102826600A CN 201210351453X A CN201210351453X A CN 201210351453XA CN 201210351453 A CN201210351453 A CN 201210351453A CN 102826600 A CN102826600 A CN 102826600A
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Abstract
The invention relates to a method for preparing titanium dioxide nanowire, which belongs to the technical field of production of inorganic materials. The method for preparing titanium dioxide comprises the following steps of: firstly putting titanium foils as the titanium source into a NaOH solution added with water soluble chlorate to carry out hydro-thermal reaction to produce sodium titanate nanometer, then carrying out acid replacement treatment to obtain meta-titanic acid nanowire, and finally calcining the meta-titanic acid nanowire to obtain titanium dioxide nanowire. The titanium dioxide nanowire obtained by using the method has the diameter of 3-15nm and the length of 1-15 nu m, is pure and regular in size arrangement, and has good crystallinity and large specific surface area; the diameter of the titanium dioxide nanowire can be adjusted through adjusting the concentration of water soluble chlorate; the titanium dioxide nanowire produced by using the method can be used in the aspects of solar batteries, photocatalysis, water splitting, sensors, nano-electronics, optoelectronic nano-devices and the like.
Description
Technical field
The invention belongs to the preparing technical field of inorganic materials, be specifically related to the preparation method of titanium dioxide nano thread.
Background technology
Titanium oxide has wide application at aspects such as solar cell, photochemical catalysis, photodissociation water, transmitter, coating, function ceramics, high-grade paint.Because photo-generated carrier can axially be grown the migration of distance at the titanium oxide of 1-dimention nano line structure; And move to the surface more easily internally; Reduced the probability of hole and electron recombination, the efficient in the time of can improving it and be applied to photochemical catalysis, photodissociation water and solar cell.The one-dimentional structure titanium dioxide nano thread is with its unique physicochemical property and at the huge potential application foreground aspect nanoelectronic and the photoelectron nano-device; The titanium dioxide nano thread diameter is very thin, and the quantization effect occurs, and the bandwidth of titanium oxide is strengthened; Has stronger redox ability; Have big specific surface area, stronger adsorptive power, these all help the titanium-dioxide photo electrical property to improve.
Reported the multiple method for preparing one-dimensional titanium dioxide nanostructure so far, comprised that the auxiliary self-assembly of template, tensio-active agent is sent out, electrostatic spinning is sent out, hydrothermal method under chemical Vapor deposition process, titanium plate anonizing, direct oxidation metallic titanium matrix method and the alkaline condition.Template is mainly adopted in the preparation of titanium oxide one-dimensional nano line, (being main with the anodic oxidation aluminium formwork method especially).This method can obtain the nano wire of tactical rule, and yardstick is even, and live width can be regulated and control from tens to hundreds of nanometers, but maximum shortcoming is that productive rate is very low.It also is a kind of important method that the hot alkaline solution hydro-thermal reaction prepares titanium dioxide nano thread, if any report the titanyl powder is added in the aqueous sodium hydroxide solution, obtains the sodium titanate nano wire through hydro-thermal reaction; IX is carried out in acid then, obtains the metatitanic acid nano wire; Last hydro-thermal reaction is converted into titanium dioxide nano thread with the metatitanic acid nano wire.Utilize titanium foil as titanium source and substrate in addition, utilize hot alkaline solution process for producing metatitanic acid nano wire, come out to change into titanium dioxide nano thread through IX and roasting then; [reference; B Liu etc., Oriented single crystalline titanium dioxide nanowires, Nanotechnology 19 (2008) 505604]; Concrete mode is for adopting titanium foil; 220 ℃ of following hydro-thermal reactions obtain the metatitanic acid nano-wire array in the NaOH of 1M solution, come out to change into titanium dioxide nanowire array through IX and roasting then.Diameter is that 105 ± 10nm length is 12.16 ± 0.56 μ m.Reported in addition and adopted in the 10M NaOH solution of titanium foil under 180 ℃ that hydro-thermal reaction obtains the metatitanic acid nano-wire array, come out to change into titanium dioxide nanowire array through IX and roasting then, diameter is 70～90nm.[reference, Wenli Wang etc., Formation of Titania Nanoarrays by Hydrothermal Reaction and Their Application in Photovoltaic Cells, J.Am.Ceram.Soc., 91 [2] 628 – 631 (2008)].Titanium foil prepares titanium dioxide nano thread does not need template and catalyzer, simple and easy to do, and cost titanium oxide diameter low, still preparation is bigger, generally greater than 70nm, is main with 100nm rice.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of titanium dioxide nano thread at first handles titanium foil and obtains the sodium titanate nano wire in being added with the alkaline solution of NaCl, change titanium dioxide nano thread into through IX and roasting then.The titanium dioxide nano thread diameter of preparation is carefully to 3～15nm, and length is 1～15 μ m, and pure, size is arranged regular, good crystallinity, and specific surface area is big.Can regulate the diameter of titanium dioxide nano thread through the concentration of simple adjusting NaCl.Prepared titanium dioxide nano thread can be used for aspects such as solar cell, photochemical catalysis, photodissociation water, transmitter.This one-dimensional titanium dioxide nano thread structure; Because photo-generated carrier can be in the migration of axially growing distance of one dimension Nano structure; And move to the surface more easily internally; Reduced the probability of hole and electron recombination, the efficient in the time of can improving it and be applied to photochemical catalysis, photodissociation water and solar cell.
Technical scheme of the present invention is following:
A kind of preparation method of titanium dioxide nano thread, as shown in Figure 1, may further comprise the steps:
Step 1: preparing reaction solution.
In deionized water, add NaOH and, stir, obtain reflecting solution until dissolving fully as the soluble chloride hydrochlorate of additive.Wherein the concentration of NaOH is 1M～10M, and the concentration of soluble chloride hydrochlorate is 0.1～1M.
Step 2: hydro-thermal reaction generates the sodium titanate nano wire.
The reaction soln that step 1 is prepared is transferred in the teflon-lined water heating kettle, added the titanium foil of cleaning, airtight then, 160～250 ℃ of following hydro-thermal reactions 6～48 hours; Then hydro-thermal reaction is scraped in the sodium titanate that the titanium foil surface generates, together with the filtration of sodium titanate that is scattered in the solution, deionized water wash, 105～130 ℃ of oven dry down obtain the sodium titanate nano wire.
Step 3: step 2 gained sodium titanate nano wire is obtained the metatitanic acid nano wire through the peracid replacement Treatment.
Step 2 gained sodium titanate nano wire was immersed in the HCl solution of 0.1～2M 0.5～10 hour, and filtered then, deionized water wash, 105～130 ℃ of oven dry down obtain metatitanic acid superfine nano line.
Step 4: roasting metatitanic acid nano wire obtains titanium dioxide nano thread.
Step 3 gained metatitanic acid nano wire 300～1000 ℃ of following roastings 0.5～5 hour, is promptly got titanium dioxide nano thread.
In the technique scheme, the hydrochlorate of soluble chloride described in the step 1 can adopt NaCl, SnCl2 or KCl etc.
The present invention compared with prior art has following advantage:
The present invention is the titanium source with the titanium foil; At first place the NaOH solution that is added with the soluble chloride hydrochlorate to carry out hydro-thermal reaction titanium foil and generate the sodium titanate nano wire; Obtain the metatitanic acid nano wire through the peracid replacement Treatment then, at last the metatitanic acid nano wire is carried out roasting and obtain titanium dioxide nano thread.The titanium dioxide nano thread that the present invention is prepared, diameter are carefully to 3～15nm, and length is 1～15 μ m, and pure, size is arranged regular, good crystallinity, and specific surface area is big.Through regulating the diameter of water-soluble perchlorate concentration's adjustable titanium dioxide nano thread.Prepared titanium dioxide nano thread can be used at aspects such as solar cell, photochemical catalysis, photodissociation water, transmitter, nanoelectronic and photoelectron nano-devices.
Description of drawings
Fig. 1 is a schematic flow sheet of the present invention.
Fig. 2 is the stereoscan photograph (some nano wires exist with pencil) of the titanium dioxide nano thread of the present invention's preparation.
Embodiment
Embodiment 1
In the 500ml deionized water, add 60g NaOH and 6.5g NaCl, stir until dissolving fully.Then above-mentioned solution is transferred in the teflon-lined water heating kettle, added the titanium foil of cleaning, airtight, 200 ℃ of following hydro-thermal reactions 48 hours.Hydro-thermal reaction generates the sodium titanate of one deck white on the titanium foil surface, a part is distributed in the solution.With the sodium titanate white mass on the titanium foil scrape off and solution in filtration of sodium titanate, deionized water wash, 110 ℃ of down oven dry obtain the sodium titanate nano wire.Metatitanic acid is received nano wire immersed in the HCl solution of 0.5M 10 hours, filter then, deionized water wash, 105～130 ℃ of oven dry down obtain the metatitanic acid nano wire.The metatitanic acid nano wire 400 ℃ of following roastings 1 hour, is promptly got titanium dioxide nano thread.Its diameter of electron microscope observation is thin, average out to 6nm, and evaluation length is 10 μ m, and is pure, good crystallinity, the XRD measuring result shows that chromic oxide has anatase crystal type.
Embodiment 2
In the 1000ml deionized water, add 120g NaOH and 3.0g NaCl, stir until dissolving fully.Then above-mentioned solution is transferred in the teflon-lined water heating kettle, added the titanium foil clean up, airtight, 180 ℃ of following hydro-thermal reactions 48 hours.Hydro-thermal reaction generates the sodium titanate of one deck white on the titanium foil surface, a part is distributed in the solution.With the sodium titanate white mass on the titanium foil scrape off and solution in filtration of sodium titanate, deionized water wash, 110 ℃ of down oven dry obtain the sodium titanate nano wire.Metatitanic acid is received nano wire immersed in the HCl solution of 0.5M 10 hours, filter then, deionized water wash, 105～130 ℃ of oven dry down obtain the metatitanic acid nano wire.The metatitanic acid nano wire 400 ℃ of following roastings 1 hour, is promptly got titanium dioxide nano thread.Its diameter of electron microscope observation is thin, average out to 15nm, and evaluation length is 3 μ m, and is pure, good crystallinity, the XRD measuring result shows that chromic oxide has anatase crystal type.
Claims (3)
1. the preparation method of a titanium dioxide nano thread may further comprise the steps:
Step 1: preparing reaction solution;
In deionized water, add NaOH and, stir, obtain reflecting solution until dissolving fully as the soluble chloride hydrochlorate of additive; Wherein the concentration of NaOH is 1M～10M, and the concentration of soluble chloride hydrochlorate is 0.1～1M;
Step 2: hydro-thermal reaction generates the sodium titanate nano wire;
The reaction soln that step 1 is prepared is transferred in the teflon-lined water heating kettle, added the titanium foil of cleaning, airtight then, 160～250 ℃ of following hydro-thermal reactions 6～48 hours; Then hydro-thermal reaction is scraped in the sodium titanate that the titanium foil surface generates, together with the filtration of sodium titanate that is scattered in the solution, deionized water wash, 105～130 ℃ of oven dry down obtain the sodium titanate nano wire;
Step 3: step 2 gained sodium titanate nano wire is obtained the metatitanic acid nano wire through the peracid replacement Treatment;
Step 2 gained sodium titanate nano wire was immersed in the HCl solution of 0.1～2M 0.5～10 hour, and filtered then, deionized water wash, 105～130 ℃ of oven dry down obtain metatitanic acid superfine nano line;
Step 4: roasting metatitanic acid nano wire obtains titanium dioxide nano thread;
Step 3 gained metatitanic acid nano wire 300～1000 ℃ of following roastings 0.5～5 hour, is promptly got titanium dioxide nano thread.
2. the preparation method of titanium dioxide nano thread according to claim 1 is characterized in that, the hydrochlorate of soluble chloride described in the step 1 is NaCl, SnCl
2Or KCl.
3. the preparation method of titanium dioxide nano thread according to claim 1 is characterized in that, through the diameter of water-soluble perchlorate concentration's adjustable titanium dioxide nano thread in the regulating step 1.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285861A (en) * | 2013-06-24 | 2013-09-11 | 大连民族学院 | An Ag3VO4/TiO2 compound nano-wire having visible light activity, a preparation method and applications thereof |
| CN104386741A (en) * | 2014-11-01 | 2015-03-04 | 吉林大学 | Preparation method of anatase crystal type nanometer strip-shaped titanium dioxide |
| CN106521465A (en) * | 2016-11-07 | 2017-03-22 | 南京航空航天大学 | Tertiary-structure super-hydrophobic surface for icing prevention and preparation method thereof |
| CN107572582A (en) * | 2017-06-14 | 2018-01-12 | 上海友兰科技有限公司 | A kind of preparation method of titanium dioxide nano thread |
| CN107961791A (en) * | 2016-10-19 | 2018-04-27 | 张家港市沙源检测技术有限公司 | The preparation method of titanium dioxide nano thread based on hydro-thermal method |
| CN107961805A (en) * | 2016-10-20 | 2018-04-27 | 张家港市沙源检测技术有限公司 | The TiO of N doping2The preparation method of nano-wire array |
| TWI631986B (en) * | 2017-01-12 | 2018-08-11 | 國立宜蘭大學 | Titanium dioxide nanotube adsorbent for water treatment and the preparation method thereof |
| CN112125333A (en) * | 2019-06-24 | 2020-12-25 | 中国石油化工股份有限公司 | Preparation method of titanium dioxide nanowire |
| CN112467081A (en) * | 2020-12-02 | 2021-03-09 | 四川大学 | High-load self-supporting lithium titanate electrode with multilayer hierarchical nanostructure and preparation method thereof |
| CN113539695A (en) * | 2020-10-13 | 2021-10-22 | 南通一品机械电子有限公司 | High specific volume solid aluminum electrolytic capacitor and preparation method thereof |
| CN114361387A (en) * | 2022-01-12 | 2022-04-15 | 四川大学 | Self-supporting B-type titanium dioxide nano long strip network electrode and preparation method thereof |
| CN114950398A (en) * | 2022-06-12 | 2022-08-30 | 桂林理工大学 | Preparation method of one-dimensional ordered titanium dioxide nanowire array film with high aspect ratio |
-
2012
- 2012-09-20 CN CN201210351453XA patent/CN102826600A/en active Pending
Non-Patent Citations (2)
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| TSUNG-YING KE, ET AL.: "{110}-exposed rutile titanium dioxide nanorods in photocatalytic performance", 《CRYSTENGCOMM》 * |
| WENLI WANG, ET AL.: "Formation of Titania Nanoarrays by Hydrothermal Reaction and Their Application in Photovoltaic Cells", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285861A (en) * | 2013-06-24 | 2013-09-11 | 大连民族学院 | An Ag3VO4/TiO2 compound nano-wire having visible light activity, a preparation method and applications thereof |
| CN104386741A (en) * | 2014-11-01 | 2015-03-04 | 吉林大学 | Preparation method of anatase crystal type nanometer strip-shaped titanium dioxide |
| CN107961791A (en) * | 2016-10-19 | 2018-04-27 | 张家港市沙源检测技术有限公司 | The preparation method of titanium dioxide nano thread based on hydro-thermal method |
| CN107961805A (en) * | 2016-10-20 | 2018-04-27 | 张家港市沙源检测技术有限公司 | The TiO of N doping2The preparation method of nano-wire array |
| CN106521465A (en) * | 2016-11-07 | 2017-03-22 | 南京航空航天大学 | Tertiary-structure super-hydrophobic surface for icing prevention and preparation method thereof |
| TWI631986B (en) * | 2017-01-12 | 2018-08-11 | 國立宜蘭大學 | Titanium dioxide nanotube adsorbent for water treatment and the preparation method thereof |
| CN107572582A (en) * | 2017-06-14 | 2018-01-12 | 上海友兰科技有限公司 | A kind of preparation method of titanium dioxide nano thread |
| CN107572582B (en) * | 2017-06-14 | 2019-08-06 | 上海友兰科技有限公司 | A kind of preparation method of titanium dioxide nano thread |
| CN112125333A (en) * | 2019-06-24 | 2020-12-25 | 中国石油化工股份有限公司 | Preparation method of titanium dioxide nanowire |
| CN113539695A (en) * | 2020-10-13 | 2021-10-22 | 南通一品机械电子有限公司 | High specific volume solid aluminum electrolytic capacitor and preparation method thereof |
| CN113539695B (en) * | 2020-10-13 | 2023-02-28 | 南通一品机械电子有限公司 | High specific volume solid aluminum electrolytic capacitor and preparation method thereof |
| CN112467081A (en) * | 2020-12-02 | 2021-03-09 | 四川大学 | High-load self-supporting lithium titanate electrode with multilayer hierarchical nanostructure and preparation method thereof |
| CN112467081B (en) * | 2020-12-02 | 2021-10-15 | 四川大学 | High-load self-supporting lithium titanate electrode with multilayer hierarchical nanostructure and preparation method thereof |
| CN114361387A (en) * | 2022-01-12 | 2022-04-15 | 四川大学 | Self-supporting B-type titanium dioxide nano long strip network electrode and preparation method thereof |
| CN114950398A (en) * | 2022-06-12 | 2022-08-30 | 桂林理工大学 | Preparation method of one-dimensional ordered titanium dioxide nanowire array film with high aspect ratio |
| CN114950398B (en) * | 2022-06-12 | 2023-06-23 | 桂林理工大学 | Preparation method of one-dimensional ordered titanium dioxide nanowire array film with high aspect ratio |
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Effective date of registration: 20130308 Address after: 611731 Chengdu province high tech Zone (West) West source Avenue, No. 2006 Applicant after: University of Electronic Science and Technology of China Applicant after: Laser Fusion Research Center, Chinese Academy of Engineering Physics Address before: 611731 Chengdu province high tech Zone (West) West source Avenue, No. 2006 Applicant before: University of Electronic Science and Technology of China |
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