CN104724755A - Preparation method of micron-sized lamellar titanium dioxide nano material - Google Patents

Preparation method of micron-sized lamellar titanium dioxide nano material Download PDF

Info

Publication number
CN104724755A
CN104724755A CN201510100430.5A CN201510100430A CN104724755A CN 104724755 A CN104724755 A CN 104724755A CN 201510100430 A CN201510100430 A CN 201510100430A CN 104724755 A CN104724755 A CN 104724755A
Authority
CN
China
Prior art keywords
titanium dioxide
nano material
dioxide nano
deionized water
micron
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
CN201510100430.5A
Other languages
Chinese (zh)
Inventor
李美成
陈杰威
贺延聪
贺月
王宇
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.)
SUZHOU RESEARCH INSTITUTE NORTH CHINA ELECTRIC POWER UNIVERSITY
North China Electric Power University
Original Assignee
SUZHOU RESEARCH INSTITUTE NORTH CHINA ELECTRIC POWER UNIVERSITY
North China Electric Power University
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 SUZHOU RESEARCH INSTITUTE NORTH CHINA ELECTRIC POWER UNIVERSITY, North China Electric Power University filed Critical SUZHOU RESEARCH INSTITUTE NORTH CHINA ELECTRIC POWER UNIVERSITY
Priority to CN201510100430.5A priority Critical patent/CN104724755A/en
Publication of CN104724755A publication Critical patent/CN104724755A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like

Abstract

The invention discloses a preparation method of a micron-sized lamellar titanium dioxide nano material and belongs to the technical field of nano materials. The method comprises the following steps: with tetra-n-butyl titanate as a precursor, adding a certain amount of HF as a modifier, and synthesizing lamellar titanium dioxide by employing a hydrothermal method, wherein the prepared lamellar titanium dioxide has a micron-sized lamellar structure. The structure is beneficial to improvement of the charge transmission performance, so that the photocatalytic performance, the photocatalysis performance and the like of the titanium dioxide are improved.

Description

A kind of preparation method of micron order sheet titanium dioxide nano material
Technical field
The invention belongs to technical field of nano material, particularly a kind of preparation method of micron order sheet titanium dioxide nano material.It is laminar structured that this material has micron order, contributes to improving charge transport properties, can improve the catalytic performance of catalyzer, also can be used as light anode material and be applied in dye-sensitized solar cells.
Background technology
TiO 2nano material is a kind of stable chemical nature, environmental friendliness, the semiconductor material of excellent performance.Due to the charge transport properties of its excellence, there is the very feature such as high catalytic activity under illumination condition, be widely used in fields such as photochemical catalysis, photodissociation hydrogen manufacturing and dye sensitization solar batterys (DSSC).By regulation and control TiO 2nanostructure, adjustment energy level band gap, adds different doping agents, can functional materials required for design and synthesis.At regulation and control TiO 2in the process of nanostructure, need the pH value etc. of strict controlled hydrolysis speed, reactant concn and solution.By the method for Hydrothermal Synthesis, utilize tetra-n-butyl titanate as presoma, hydrofluoric acid, as conditioning agent, obtains a kind of micron order sheet titanium dioxide.Synthesized titanium dioxide has micron-sized laminated structure, and have good conductivity, this laminated structure has certain application at catalytic field and electrochemical field.
Summary of the invention
The object of the invention is to propose one and prepare sheet TiO 2the method of nano material, method provided by the invention adopts tetra-n-butyl titanate as presoma, using hydrofluoric acid as conditioning agent, adopts a simple one-step hydro-thermal synthesis method to prepare micron order sheet TiO 2nanostructure.Concrete preparation method comprises the steps:
(1) 20 ~ 30mL deionized water and 1 ~ 3mL tetra-n-butyl titanate are added in a clean beaker respectively, and carry out the stirring of 0.5 ~ 1h;
(2) add the hydrofluoric acid of 0.6 ~ 0.7mL, continue stirring 0.5 ~ 1h;
(3) be transferred in autoclave by (2) gained solution, at 160 ~ 200 DEG C, hydro-thermal reaction naturally cooled to room temperature after 19 ~ 24 hours;
(4) be neutral by step (3) gained precipitate with deionized water and absolute ethanol washing to filtrate, then carry out drying treatment, sheet titanium dioxide nano material;
Deionized water in described step (1) is 20 ~ 3mL, and tetra-n-butyl titanate used is 1 ~ 3ml, and churning time is 0.5 ~ 1 hour;
The content of the hydrofluoric acid added in described step (2) is 0.6 ~ 0.7mL, and churning time is 0.5 ~ 1 hour;
In described step (3), the temperature of hydro-thermal reaction is 160 ~ 200 DEG C, and the reaction times is 19 ~ 24 hours;
The invention has the beneficial effects as follows and adopt tetra-n-butyl titanate as presoma, hydrofluoric acid, as conditioning agent, utilizes water heat transfer sheet TiO 2nanostructure.The advantage of Hydrothermal Synthesis is that reactant is heated evenly, and effectively can control temperature of reaction, and controllability is good, and carries out in airtight container, pollutes little.Due to sheet TiO 2nano material has larger crystal plane, and conductivity is better, therefore can be widely used in the fields such as optoelectronic device chemistry, dye sensitization solar battery.
Accompanying drawing explanation
Fig. 1 is the sheet TiO of synthesis in example 1 of the present invention 2the scanning electron microscope (SEM) photograph of nano material.
Embodiment
The one that the present invention proposes prepares sheet TiO 2the method of nano material is implemented by following method, and concrete preparation method comprises the steps:
Embodiment 1
(1) 25mL deionized water and 1.5mL tetra-n-butyl titanate are added in a clean beaker respectively, and carry out the stirring of 1h;
(2) add the hydrofluoric acid of 0.6mL, continue to stir 0.5h;
(3) be transferred in autoclave by (2) gained solution, at 180 DEG C, hydro-thermal reaction naturally cooled to room temperature after 23 hours;
(4) be neutral by step (3) gained precipitate with deionized water and absolute ethanol washing to filtrate, then carry out drying treatment, sheet titanium dioxide nano material.As shown in Figure 1.
Embodiment 2
1) 28mL deionized water and 1.7mL tetra-n-butyl titanate are added in a clean beaker respectively, and carry out the stirring of 1h;
(2) add the hydrofluoric acid of 0.65mL, continue to stir 1h;
(3) be transferred in autoclave by (2) gained solution, at 190 DEG C, hydro-thermal reaction naturally cooled to room temperature after 21 hours;
(4) be neutral by step (3) gained precipitate with deionized water and absolute ethanol washing to filtrate, then carry out drying treatment, sheet titanium dioxide nano material.

Claims (4)

1. a preparation method for micron order sheet titanium dioxide nano material, is characterized in that, comprises step as follows:
(1) 20 ~ 30mL deionized water and 1 ~ 3mL tetra-n-butyl titanate are added in a clean beaker respectively, and carry out the stirring of 0.5 ~ 1h;
(2) add the hydrofluoric acid of 0.6 ~ 0.7mL, continue stirring 0.5 ~ 1h;
(3) be transferred in autoclave by (2) gained solution, at 160 ~ 200 DEG C, hydro-thermal reaction naturally cooled to room temperature after 19 ~ 24 hours;
(4) be neutral by step (3) gained precipitate with deionized water and absolute ethanol washing to filtrate, then carry out drying treatment, sheet titanium dioxide nano material.
2. the method preparing micron order sheet titanium dioxide nano material according to claim 1, is characterized in that, in step (1), deionized water used is 20 ~ 30mL, and the volume of tetra-n-butyl titanate used is 1 ~ 3mL, and churning time is 0.5 ~ 1h.
3. the method preparing sheet titanium dioxide nano material according to claim 1, is characterized in that, the hydrofluoric acid volume added in step (2) is 0.6 ~ 0.7mL, and churning time is 0.5 ~ 1h.
4. according to claim 1ly prepare pinecone shape TiO 2the method of nano material, is characterized in that, in step (3), solution reaction conditions is in a kettle. react 19 ~ 24 hours at 160 ~ 200 DEG C.
CN201510100430.5A 2015-03-06 2015-03-06 Preparation method of micron-sized lamellar titanium dioxide nano material Pending CN104724755A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510100430.5A CN104724755A (en) 2015-03-06 2015-03-06 Preparation method of micron-sized lamellar titanium dioxide nano material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510100430.5A CN104724755A (en) 2015-03-06 2015-03-06 Preparation method of micron-sized lamellar titanium dioxide nano material

Publications (1)

Publication Number Publication Date
CN104724755A true CN104724755A (en) 2015-06-24

Family

ID=53449259

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510100430.5A Pending CN104724755A (en) 2015-03-06 2015-03-06 Preparation method of micron-sized lamellar titanium dioxide nano material

Country Status (1)

Country Link
CN (1) CN104724755A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105126796A (en) * 2015-07-13 2015-12-09 华北电力大学 Preparation method of fluorine-doped lamellar black titanium dioxide nano material
CN105510401A (en) * 2015-12-01 2016-04-20 中国科学院新疆理化技术研究所 Method for identifying explosives by using titanium dioxide nanosheet-based gas sensor array
CN105642262A (en) * 2016-02-04 2016-06-08 梁书齐 Two-dimensional-layered titanium-dioxide nanometer photocatalytic material and preparing method
CN106629837A (en) * 2016-09-13 2017-05-10 华北电力大学 Method for preparing titanium dioxide material rich in trivalent titanium defects
CN109759005A (en) * 2019-03-13 2019-05-17 郑州大学 A kind of quick response Pd-TiO2The preparation method of the quick material of nano particle hydrogen

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0908494A2 (en) * 1997-10-08 1999-04-14 E.I. Dupont De Nemours And Company Uniformly coated particulate metal oxide
CN101462769A (en) * 2009-01-09 2009-06-24 厦门大学 Titanium dioxide nanoplate and synthesizing method thereof
WO2009117770A1 (en) * 2008-03-25 2009-10-01 The University Of Queensland Crystalline inorganic species having optimised reactivity
CN102895964A (en) * 2012-10-18 2013-01-30 南京工业大学 Preparation method for blue sheet-like titanium dioxide nanomaterial
CN103232064A (en) * 2013-04-28 2013-08-07 奇瑞汽车股份有限公司 Nano titanium dioxide and preparation method thereof as well as dye-sensitized solar battery
CN103318955A (en) * 2013-06-24 2013-09-25 华北电力大学 String-shaped TiO2 micro-sphere material and preparation method thereof
CN103657619A (en) * 2013-10-16 2014-03-26 江苏大学 Preparation method of titanium dioxide nanosheet photocatalytic material with controllable size
CN103818954A (en) * 2014-02-19 2014-05-28 东华大学 Preparation method of anatase TiO2 hollow microspheres with exposed (001) surface
CN103831091A (en) * 2014-03-31 2014-06-04 中国科学院新疆理化技术研究所 Method for generating anatase titanium dioxide antarafacial junction through one-step hydrothermal method

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0908494A2 (en) * 1997-10-08 1999-04-14 E.I. Dupont De Nemours And Company Uniformly coated particulate metal oxide
WO2009117770A1 (en) * 2008-03-25 2009-10-01 The University Of Queensland Crystalline inorganic species having optimised reactivity
CN101462769A (en) * 2009-01-09 2009-06-24 厦门大学 Titanium dioxide nanoplate and synthesizing method thereof
CN102895964A (en) * 2012-10-18 2013-01-30 南京工业大学 Preparation method for blue sheet-like titanium dioxide nanomaterial
CN103232064A (en) * 2013-04-28 2013-08-07 奇瑞汽车股份有限公司 Nano titanium dioxide and preparation method thereof as well as dye-sensitized solar battery
CN103318955A (en) * 2013-06-24 2013-09-25 华北电力大学 String-shaped TiO2 micro-sphere material and preparation method thereof
CN103657619A (en) * 2013-10-16 2014-03-26 江苏大学 Preparation method of titanium dioxide nanosheet photocatalytic material with controllable size
CN103818954A (en) * 2014-02-19 2014-05-28 东华大学 Preparation method of anatase TiO2 hollow microspheres with exposed (001) surface
CN103831091A (en) * 2014-03-31 2014-06-04 中国科学院新疆理化技术研究所 Method for generating anatase titanium dioxide antarafacial junction through one-step hydrothermal method

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
HUA GUI YANG等: "Anatase TiO2single crystals with a large percentage of reactive facets", 《NATURE》 *
JIAGUO YU等: "Hydrogen Production by Photocatalytic Water Splitting over Pt/TiO2 Nanosheets with Exposed (001) Facets", 《J. PHYS. CHEM. C》 *
冯氏云等: "{001}面TiO2光催化降解罗丹明B的研究", 《水处理技术》 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105126796A (en) * 2015-07-13 2015-12-09 华北电力大学 Preparation method of fluorine-doped lamellar black titanium dioxide nano material
CN105126796B (en) * 2015-07-13 2017-12-22 华北电力大学 A kind of preparation method of Fluorin doped sheet black titanium dioxide nano material
CN105510401A (en) * 2015-12-01 2016-04-20 中国科学院新疆理化技术研究所 Method for identifying explosives by using titanium dioxide nanosheet-based gas sensor array
CN105510401B (en) * 2015-12-01 2017-12-01 中国科学院新疆理化技术研究所 Utilize the method for titanium dioxide nanoplate base gas sensor array identification explosive
CN105642262A (en) * 2016-02-04 2016-06-08 梁书齐 Two-dimensional-layered titanium-dioxide nanometer photocatalytic material and preparing method
CN106629837A (en) * 2016-09-13 2017-05-10 华北电力大学 Method for preparing titanium dioxide material rich in trivalent titanium defects
CN106629837B (en) * 2016-09-13 2019-02-15 华北电力大学 A kind of preparation method of the titanic oxide material rich in titanous defect
CN109759005A (en) * 2019-03-13 2019-05-17 郑州大学 A kind of quick response Pd-TiO2The preparation method of the quick material of nano particle hydrogen
CN109759005B (en) * 2019-03-13 2021-09-14 郑州大学 Quick response Pd-TiO2Preparation method of nano-particle hydrogen sensitive material

Similar Documents

Publication Publication Date Title
CN104724755A (en) Preparation method of micron-sized lamellar titanium dioxide nano material
CN105817253B (en) The preparation method of graphite phase carbon nitride nanometer sheet/Nano tube array of titanium dioxide catalysis material
CN102773110B (en) Method for preparing SnS2/SnO2 composite photocatalyst material of numismatics-shaped hollow structure
CN102701275B (en) Method for preparing TiO2 nano laces
CN101949054B (en) Method for preparing single-crystal anatase titanium dioxide film
CN103880072B (en) A kind of preparation method of pinecone shape titanium dioxide nano material
CN100534910C (en) Method of preparing TiO2 nano-tube array
CN104525168B (en) Method for synthesizing anatase/brookite nano composite material for photocatalytic decomposition of water into hydrogen through one-step hydrothermal method
CN105080579A (en) BiOBr/Bi2WO6 composite photocatalyst with heterostructure and preparation method thereof
CN106512985B (en) A kind of ZnO/WO3The synthetic method of heterojunction array
CN105126796A (en) Preparation method of fluorine-doped lamellar black titanium dioxide nano material
CN105664902A (en) Trivalent titanium ion self-doped titanium dioxide nanosheet catalyst
CN103657625B (en) A kind of exposure high energy crystal face { preparation method of 001} rutile-type boron doped titanic oxide microballoon
CN102553563A (en) Method for preparing high catalytic activity sodium tantalate photo-catalyst by hydro-thermal method
CN105645459A (en) Surface modified urchin-shaped ZnO/TiO2 composite material and preparation method thereof
CN105771958B (en) A kind of Bi4V2O11The preparation method of nano particle
CN106629830A (en) Zinc titanate nanowire material and application thereof to perovskite solar cell
CN104226320A (en) Preparation method of vanadium-boron co-doping titanium dioxide and nickel oxide composite photocatalyst
CN103611527A (en) Visible-light response Ce doped Bi2WO6 microcrystal, preparation method and application thereof
CN103240068B (en) Preparation method of self-doped titanium dioxide nanorod
CN102249299A (en) Method for preparing TiO2 overlong micro rod in NaCl molten salt system
CN103754929B (en) Preparation method for TiO2/InVO4 composite porous micro-sphere
CN103933979B (en) A kind of for control TiO 2the preparation method of nano tube supported metal state
CN104353444A (en) Method of synthesizing metatitanic acid/TiO2 nano composite material for hydrogen production from water by photodecomposition via one-step solvothermal method
CN103922385B (en) A kind of preparation method of cerium oxide hexagonal nanosheet shape structure

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20150624

WD01 Invention patent application deemed withdrawn after publication