CN107010660A - A kind of anatase TiO2The preparation method for the nanostructured that is connected - Google Patents

A kind of anatase TiO2The preparation method for the nanostructured that is connected Download PDF

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Publication number
CN107010660A
CN107010660A CN201710317038.5A CN201710317038A CN107010660A CN 107010660 A CN107010660 A CN 107010660A CN 201710317038 A CN201710317038 A CN 201710317038A CN 107010660 A CN107010660 A CN 107010660A
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China
Prior art keywords
nanostructured
annealing
oac
anatase tio
tio
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CN201710317038.5A
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Chinese (zh)
Inventor
楚亮
李兴鳌
刘维
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Nanjing Post and Telecommunication University
Nanjing University of Posts and Telecommunications
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Nanjing Post and Telecommunication University
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Priority to CN201710317038.5A priority Critical patent/CN107010660A/en
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    • 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
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/08—Drying; Calcining ; After treatment of titanium oxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • 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
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter
    • C01P2006/17—Pore diameter distribution

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a kind of anatase TiO2The preparation method for the nanostructured that is connected, relates generally to titaniferous nano wire, compound micron ball and micro-flowers Ti6(OAc)6(OiPr)6‑n(OH)nAnd generation anatase TiO after its annealing2Connected nanostructured.Isopropyl titanate thermal response in acetic acid solution then cleans the Ti of generation nano wire, compound micron ball and micron floral structure with deionized water and ethanol6(OAc)6(OiPr)6‑n(OH)n, anneal be cracked into anatase TiO in atmosphere2Be connected nanostructured.This method manufacture craft is simple, without toxic by-products, the low and suitable large-scale application of cost.

Description

A kind of anatase TiO2The preparation method for the nanostructured that is connected
Technical field
The invention belongs to a kind of high-specific surface area, possesses the TiO of long-range electric charge transmission channel2Research in nanotechnology field, mainly It is related to a kind of anatase TiO2The preparation method for the nanostructured that is connected.
Background technology
TiO2It is excellent with Stability Analysis of Structures, broad stopband, suitable band structure, nontoxic, excellent electrical and optical properties etc. Point, excellent performance is shown in fields such as solar cell, lithium ion battery, photocatalytic water, photodetections.How simply to synthesize TiO with high-specific surface area and long-range electric charge transmission channel2One challenge of nanostructured., Britain Henry in 2013 J.Snaith professors seminar exists《Nature》Reported on magazine and nanometer monocrystalline TiO is prepared using template2Many hollow structures, it is real TiO is showed2The characteristic of high-specific surface area and long-range electric charge transmission channel is provided simultaneously with, but the preparation technology engineering is cumbersome.
This patent synthesizes the micron or nanostructured of titaniferous using hydro-thermal method first, with after annealing formation anatase TiO2 Be connected nanostructured.
The content of the invention
The technical problems to be solved by the invention are：The micron or nanostructured of titaniferous are prepared, with after annealing formation rutile titania Ore deposit TiO2Be connected nanostructured.
The present invention solves its technical problem and uses following technical scheme, comprises the following steps：
(1) with isopropyl titanate, acetic acid is raw material, and heating response is then handled with deionized water, generates Ti6(OAc)6 (OiPr)6-n(OH)nNano/micron structure, such as nano wire, compound micron ball, micro-flowers.
(2)Ti6(OAc)6(OiPr)6-n(OH)nMaterial in atmosphere heat resolve into anatase TiO2Be connected nanostructured.
In the step (1), heat treatment temperature is 120~220 degree.
In the step (1), the volume ratio of isopropyl titanate and acetic acid is 1：5~100.
In step (2), annealing temperature is 400~550 degree.
In the step (2), annealing time is 30 minutes to 4 hours.
Beneficial effect
The present invention has the advantages that following main compared with prior art：Manufacture craft is simple, without toxic by-products, cost Low and suitable large-scale application etc..
Brief description of the drawings
Fig. 1 is the XRD piece that (a) different time thermal response of the invention generates powder；(b) the XRD piece after annealing；(c)3 The FTIR spectrum of hour generation sample；Scheme (a) and show that acid heat generation powder sample is amorphous, figure (b) is shown after amorphous annealing For anatase TiO2。
Fig. 2 is the SEM pictures that different time thermal response of the present invention generates powder sample, and figure (a) is 3 hours samples, product Microcosmic appearance is nano wire；It is 6 hours samples to scheme (b, c, d).
Fig. 3 is that different time acid heat of the present invention generates SEM picture of the powder sample after 500 degree of annealing in 2 hours.
Fig. 4 is to generate TiO after differential responses time sample of the present invention is stepped back2N2Adsorption/desorption isothermal curve, illustration is hole Footpath distribution curve.
Embodiment
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings.
A kind of anatase TiO2The preparation method of connected nano particle, relates generally to step in detail below：
(1) isopropyl titanate, the titanium compound of heating generation nanostructure-containing are added in acetic acid solution；
(2) titanium compound is first washed with deionized water, then with alcohol flushing, dries, product is Ti6(OAc)6(OiPr)6-n (OH)n.；
(3) annealing forms TiO2The structure for the nanometer that is connected, wherein annealing temperature is set between 400~550 degree.
Fig. 1 (a) different times thermal response generates the XRD piece of powder；(b) the XRD piece after annealing；(c) generate within 3 hours The FTIR spectrum of sample.Scheme (a) and show that acid heat generation powder sample is amorphous, it is anatase that figure (b), which is shown after amorphous annealing, TiO2, wherein peak value corresponds to anatase TiO respectively2(101), (004), (200), (105), (211), (204), (116) diffraction Crystal face (JCPDS No.21-1272).In FTIR spectrum, signal 2939cm-1Correspondence-OAc andiC-H vibration moulds between PrOH Formula.1753 and 1717cm-1In correspondence difference carboxyl, 1554cm-1With 1417,1453cm-1Asymmetric and symmetric is corresponded to respectively Carboxyl vibration mode.The interval of the two vibration modes about 100cm-1, 1554cm-1For double bond vibration mode.1348 and 1029cm-1C-C vibration modes between correspondence link acetate and Ti.Low energetic vibration signal 757 and 658cm-1Correspondence chemical bond Ti-O (Ti-Ac) and Ti-O (Ti-O-Pr) vibration mode.Thermal response generation powder sample is Ti6(OAc)6(OiPr)6-n (OH)n。
As shown in Figure 2：0.5ml isopropyl titanates are added in the 50ml autoclaves containing 30ml acetic acid, at 150 degree Lower reaction, different time thermal response generates the SEM pictures of powder sample, and figure (a) is 3 hours samples, and the microcosmic appearance of product is to receive Rice noodles；It is 6 hours samples to scheme (b, c, d), and the microcosmic appearance of product is micron ball, and micron ball is made up of nanobelt；It is 9 to scheme (e, f) Hour sample, the microcosmic appearance of product is micro-flowers, and micro-flowers are made up of big nanometer sheet.During the course of the reaction, first nucleation, then Nano wire is generated, further independently dress generates micron ball to nano wire, and your moral cures (Ostwald Ripening) due to Oswald Process, micron ball is converted for micro-flowers.
500 degree annealing two hours after with the TiO in Fig. 32Pattern correspondence.
Fig. 3 different times acid heat generates SEM picture of the powder sample after 500 degree of annealing in 2 hours, and figure (a) is 3 small When sample annealing after SEM pictures, it is shown that the nano thread structure that constitutes is connected by nano particle；It is 6 hours samples to scheme (b, c, d) SEM pictures after product annealing, it is shown that decomposed after the annealing of micro-flowers sample, micron spherical structure is broken off into nanometer plate Deng nanometer plate etc. is made up of nano particle；It is the SEM pictures after sample annealing in 9 hours to scheme (e, f), and micro-flowers are decomposed, microcosmic knot Structure is made up of nano particle.
Fig. 4 differential responses time samples generate TiO after stepping back2N2Adsorption/desorption isothermal curve, illustration is pore-size distribution Curve.3 hours, 6 hours, 9 hours samples step back generation TiO2BET specific surface area be respectively 54.55,43.52,52.96 ㎡/ g.6 hours small possible causes of specific surface area are that its granular size is maximum, and due to Oswald, your moral is cured 9 hours samples (Ostwald Ripening) process nanometer sheet is thinning while growing up, and the size that particle is formed after annealing diminishes.

Claims (5)

1. a kind of anatase TiO2The preparation method for the nanostructured that is connected, it is characterised in that comprise the following steps：
(1) titanium source is heat-treated in acetic acid solution, is then first handled with deionized water, is then cleaned with ethanol, is obtained after drying Ti6(OAc)6(OiPr)6-n(OH)nMicron or nanostructured；
(2)Ti6(OAc)6(OiPr)6-n(OH)nMicron or nano material anneal in atmosphere, form anatase TiO2It is connected and receives Rice structure.
2. according to the method described in claim 1, it is characterised in that titanium source is isopropyl titanate, heat treatment in the step (1) Temperature is 120~220 degree.
3. according to the method described in claim 1, it is characterised in that in described step (1), the body of isopropyl titanate and acetic acid Product is than being 1：5~100.
4. according to the method described in claim 1, it is characterised in that in described step (2), annealing temperature is 400~550 Degree.
5. according to the method described in claim 1, it is characterised in that in described step (2), annealing time is 30 minutes to 4 Hour.
CN201710317038.5A 2017-05-08 2017-05-08 A kind of anatase TiO2The preparation method for the nanostructured that is connected Pending CN107010660A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111675240A (en) * 2020-06-01 2020-09-18 南开大学 Black titanium dioxide and preparation method and application thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SAYEKTI WAHYUNINGSIH ET AL.: ""Visible light photoelectrocatalytic degradation of rhodamine B using a dye-sensitised TiO2 electrode"", 《CHEMICAL PAPERS》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111675240A (en) * 2020-06-01 2020-09-18 南开大学 Black titanium dioxide and preparation method and application thereof
CN111675240B (en) * 2020-06-01 2021-06-01 南开大学 Black titanium dioxide and preparation method and application thereof

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