CN103332725B - Multistage and ordered In2O3 structures growing along TiO2 nanofiber surfaces and preparation method - Google Patents
Multistage and ordered In2O3 structures growing along TiO2 nanofiber surfaces and preparation method Download PDFInfo
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- CN103332725B CN103332725B CN201310217883.7A CN201310217883A CN103332725B CN 103332725 B CN103332725 B CN 103332725B CN 201310217883 A CN201310217883 A CN 201310217883A CN 103332725 B CN103332725 B CN 103332725B
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Abstract
The invention discloses an In2O3 oriented growth structure, flower-like structure, dendritic structure, hollowed structure and tetrahedral structure along TiO2 nanofiber surfaces and a preparation method. The TiO2 nanofiber is prepared by the hydro-thermal synthesis method. The In2O3 is prepared by the magnetron sputtering technology. The In2O3 oriented growth, flower-like, dendritic, hollowed and tetrahedral structures are multistage and ordered, and are advantaged by high specific surface area, high permeability, good photocatalytic performance and conductivity.
Description
Technical field
The present invention relates to a kind of multilevel ordered In
2o
3structure, particularly relates to a kind of at TiO
2the oriented growth structure that nanofiber surface demonstrates, flower-like structure, dendritic structure, Openworks shape structure, tetrahedral structure and preparation method thereof.
Background technology
Three oxidation two (In
2o
3) indium belongs to the extension product of indium, it is the starting material often used in resistive touch screen, is mainly used in window of tube, glass, pottery, chemical reagent etc.In addition, tinted shade, pottery, alkaline Mn cell is widely used in for traditional field such as mercury inhibition Liu, chemical reagent.Be widely used in the high-technology fields such as photovoltaic industry and military field in recent years, be specially adapted to be processed as indium tin oxide (ITO) target, manufacture transparency electrode and transparent heat reflection body material, for the production of flat liquid crystal display and demist ice device.
Along with the development of science and technology, indium trioxide is more and more wider in the application of liquid-crystal display especially in ITO target.Liquid-crystal display has now become technology-intensive, fund-intensive new high-tech industry, and transparent conducting glass is then one of three large main raws of LCD.Why liquid-crystal display can show specific figure, utilize the nesa coating on conductive glass exactly, the electrode of specified shape is made through etching, after liquid crystal cell made by upper and lower conductive glass, these electrodes add appropriate voltage signal, make to have the liquid crystal molecule of moment of dipole specific under electric field action in arrangement, only demonstrate the figure corresponding with electrode wavelength.In oxide conductive film, to mix the In of Sn (tin)
2o
3(ITO) transmitance of film is the highest best with conductivity, and easily in acid solution, etches fine figure.Its transmitance to have reached in more than 90%, ITO its transmitance and resistance respectively by In
2o
3with Sn
2o
3ratio control, usual SnO
2: In
2o
3=1:9.ITO is a kind of N-type oxide semiconductor-tin indium oxide, ito thin film and indium tin oxide transparent conductive semiconductor film, usually has a two entirely different things main performance pointer: resistivity and light transmission rate.
The resistivity of current ito film layer is generally at 5*10
-4left and right, preferably can reach 5*10
-5, close to the resistivity of metal, when practical application, often characterize the conductivity of ITO with square resistance, its transmitance then can reach more than 90%, and the transmitance of ito film and resistance are respectively by In
2o
3with Sn
2o
3ratio control, increase the transmitance that Indium sesquioxide ratio then can improve ITO, usual Sn
2o
3: In
2o
3=1:9, because when the thickness of stannic oxide is more than 200nm, normally transparent degree is good not, although conductivity is fine.Therefore, prepare a kind of high-specific surface area, the In of high penetration rate
2o
3become the focus of people's research.
The method producing indium trioxide is a lot: have high frequency blow oxygen, nitrates decompose method, indium hydroxide decomposition method, carbonic acid decomposes method etc., but can not prepare desirable In
2o
3multilevel ordered nanostructure.In
2o
3nanostructure also waits for the exploitation of people, and this is just in the urgent need to In
2o
3technology of preparing carries out constantly bringing forth new ideas and development, prepares a kind of new multistage ordered nano In
2o
3structure remains a challenge so far.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of multilevel ordered In is provided
2o
3structure and preparation method thereof.
1. a multilevel ordered In
2o
3structure, is characterized in that: In
2o
3prolong TiO
2nanofiber surface demonstrates oriented growth structure, flower-like structure, dendritic structure, Openworks shape structure, tetrahedral structure:
Described In
2o
3oriented growth structure is by multiple In
2o
3nano-pillar oriented growth, to align at TiO
2nanofiber surface;
Described In
2o
3flower-like structure is by described In
2o
3oriented growth structure is tending towards the In that saturated its surface growth rear goes out
2o
3petal is formed;
Described In
2o
3dendritic structure is by described In
2o
3petal further raw;
Described In
2o
3openworks shape structure is by multiple described In
2o
3dendritic structure self-assembly;
Described In
2o
3tetrahedral structure is by described In
2o
3openworks shape structure is tending towards saturated.
Described In
2o
3oriented growth structure, flower-like structure, dendritic structure, Openworks shape structure, tetrahedral structure have good photocatalysis performance and conductivity.
2. In described in a claim 1
2o
3the preparation method of Openworks shape nanometer tetrahedron, is characterized in that: the method mainly comprises the following steps:
(1) hydrothermal method prepares TiO
2nanofiber substrate: put into after titanium sheet being put into acetone ultrasonic cleaning in loft drier and dry; Then titanium sheet is placed in reactor, and is the NaOH solution submergence of 2mol/L by concentration; Reactor is placed in resistance furnace with Temperature fall after the heating temperatures 2-10 of 220 DEG C-240 DEG C hour; Take out titanium sheet, with distilled water flushing, dry, obtaining required surface length has many walls toughness TiO
2nanofiber substrate.
(2) magnetron sputtering prepares multilevel ordered In
2o
3structure: by In
2o
3tiO prepared by target and step 1
2nanofiber substrate is placed in multi-target magnetic control sputtering instrument, and regulate target class interval to be 3cm-4cm, pass into argon gas, operating pressure is between 0.6Pa-2.0Pa, and power is 100W-150W; At TiO
2nanofiber surface, sputters 5-10 minute in the above conditions to prepare In
2o
3oriented growth structure; Sputter 10-15 minute to prepare In in the above conditions
2o
3flower-like structure; Sputter 15-20 minute to prepare In in the above conditions
2o
3dendritic structure; Sputter 20-30 minute to prepare In in the above conditions
2o
3openworks shape structure; Sputter 30-60 minute to prepare In in the above conditions
2o
3tetrahedral structure.
The invention has the beneficial effects as follows, compared with prior art, the In that the present invention prepares
2o
3the structure such as oriented growth, flower-shaped, dendroid, Openworks shape, tetrahedron aligns by multiple multilevel hierarchy, interweaves with being connected, therefore described In
2o
3multi-scale structure has high-specific surface area, high penetration rate, possesses good photocatalysis performance and conductivity.
Accompanying drawing explanation
Fig. 1 A-H is the multilevel ordered In of the different sputtering time of the present invention
2o
3the SEM image of structure: A, sputtering time 0min B, sputtering time 5min C, sputtering time 10min D, sputtering time 15min E, sputtering time 20min F, sputtering time 25min G, sputtering time 30min H, sputtering time 35min(target pole span are 3cm, sputtering power 100W);
Fig. 2 A-H is the multilevel ordered In of the different sputtering time of the present invention
2o
3the SEM enlarged image of structure: A, sputtering time 0min B, sputtering time 5min C, sputtering time 10min D, sputtering time 15min E, sputtering time 20min F, sputtering time 25min G, sputtering time 30min H, sputtering time 35min(target pole span are 3cm, sputtering power 100W);
Fig. 3 A-H is the multilevel ordered In of the different sputtering time of the present invention
2o
3the TEM image of structure: A, sputtering time 0min B, sputtering time 5min C, sputtering time 10min D, sputtering time 15min E, sputtering time 20min F, sputtering time 25min G, sputtering time 30min H, sputtering time 35min(target pole span are 3cm, sputtering power 100W);
Fig. 4 A-C is the multilevel ordered In of the present invention
2o
3the SEM of structure, TEM image, the multilevel ordered In of the present invention that corresponding A *-C* is underlayer temperature when being 400 °
2o
3the SEM of structure, TEM image (target pole span is 3cm, sputtering power 100W, sputtering time 5min);
Fig. 5 A is In of the present invention
2o
3the TEM pattern of oriented growth structure, 5 B are In of the present invention
2o
3oriented growth structure HRTEM image, the corresponding electron diffraction pattern (target pole span is 3cm, sputtering power 100W, sputtering time 5min) in the lower right corner;
Fig. 6 A-C is the multilevel ordered In of the present invention
2o
3the EDX image of the different sputtering time of structure: (target pole span is 3cm, sputtering power 100W);
Fig. 7 is the multilevel ordered In of the present invention
2o
3the XRD figure picture of the different sputtering time of structure: (target pole span is 3cm, sputtering power 100W).
Embodiment
In of the present invention
2o
3the preparation method of multi-scale structure, comprises the following steps:
(1) hydrothermal method prepares TiO
2nanofiber substrate: put into after titanium sheet being put into acetone ultrasonic cleaning in loft drier and dry; Then titanium sheet is placed in reactor, and is the NaOH solution submergence of 2mol/L by concentration; Reactor is placed in resistance furnace with Temperature fall after the heating temperatures 2-10 of 220 DEG C-240 DEG C hour; Take out titanium sheet, with distilled water flushing, dry, obtaining required surface length has many walls toughness TiO
2nanofiber substrate.
(2) magnetron sputtering prepares multilevel ordered In
2o
3structure: by In
2o
3tiO prepared by target and step 1
2nanofiber substrate is placed in multi-target magnetic control sputtering instrument, and regulate target class interval to be 3cm-4cm, pass into argon gas, operating pressure is between 0.6Pa-2.0Pa, and power is 100W-150W; At TiO
2nanofiber surface, sputters 5-10 minute in the above conditions to prepare In
2o
3oriented growth structure; Sputter 10-15 minute to prepare In in the above conditions
2o
3flower-like structure; Sputter 15-20 minute to prepare In in the above conditions
2o
3dendritic structure; Sputter 20-30 minute to prepare In in the above conditions
2o
3openworks shape structure; Sputter 30-60 minute to prepare In in the above conditions
2o
3tetrahedral structure.
To In
2o
3multi-scale structure characterizes:
Adopt JSM-5610LV type scanning electronic microscope multilevel ordered In to the different sputtering time of the present invention under 10kV high pressure
2o
3structure and morphology carries out observation analysis.The corresponding 2A-H of Figure 1A-H(enlarged view) give the In of different times
2o
3the SEM image of multi-scale structure, contrasts 3A-H simultaneously and also can find out, In
2o
3first TiO is prolonged
2nanofiber surface life is going out oriented growth structure.When sputtering time arrives 10 minutes, orientation life close to saturated, In
2o
3start to show flower-like structure and dendritic structure.When sputtering time arrives 20 minutes, In
2o
3openworks shape structure manifests gradually.After sputtering time arrives 30 minutes, In
2o
3tetrahedral structure just can manifest, and now this structure is the most stable.
Fig. 4 A-C and A*-C* contrast can be found out, underlayer temperature can affect In in early stage
2o
3the degree of roughness of oriented growth body structure surface, underlayer temperature is higher, and roughness is larger.
In of the present invention by Fig. 5 A-B
2o
3tEM and the HRTEM pattern of oriented growth structure.In can be seen
2o
3oriented growth structural lattice spacing is 0.292nm, corresponding In
2o
3(222) crystal face, this and TiO
2(102) crystal face 0.29nm is consistent, proves In
2o
3with TiO
2lattice match is the reason causing generating oriented growth.
By the elementary composition image analysis of EDX (Fig. 6), and draw in conjunction with electron diffraction analysis with standard comparison card comparing result (Fig. 7) in conjunction with in XRD figure picture, the present invention prepares oriented growth, flower-shaped, dendroid, Openworks shape, tetrahedral structure be all Cubic, la-3(206) high-purity In of crystalline form
2o
3.
The In that the present invention prepares
2o
3the structure such as oriented growth, flower-shaped, dendroid, Openworks shape, tetrahedron aligns by multiple multilevel hierarchy, interweaves with being connected, therefore described In
2o
3multi-scale structure has high-specific surface area, high penetration rate, possesses good photocatalysis performance and conductivity.
Claims (2)
1. a multilevel ordered In
2o
3structure, is characterized in that: In
2o
3prolong TiO
2nanofiber surface grows oriented growth structure, flower-like structure, dendritic structure, Openworks shape structure or tetrahedral structure:
Described In
2o
3oriented growth structure is by multiple In
2o
3nano-pillar oriented growth, to align at TiO
2nanofiber surface;
Described In
2o
3flower-like structure is by described In
2o
3oriented growth structure is tending towards the In that saturated its surface growth rear goes out
2o
3petal is formed;
Described In
2o
3dendritic structure is by described In
2o
3petal further growth;
Described In
2o
3openworks shape structure is by multiple described In
2o
3dendritic structure self-assembly;
Described In
2o
3tetrahedral structure is by described In
2o
3openworks shape structure is tending towards saturated.
2. a multilevel ordered according to claim 1
2o
3the preparation method of structure, is characterized in that: the method comprises the following steps:
(1) hydrothermal method prepares TiO
2nanofiber substrate: put into after titanium sheet being put into acetone ultrasonic cleaning in loft drier and dry; Then titanium sheet is placed in reactor, and is the NaOH solution submergence of 2mol/L by concentration; Reactor is placed in resistance furnace with Temperature fall after the heating temperatures 2-10 of 220 DEG C-240 DEG C hour; Take out titanium sheet, with distilled water flushing, dry, obtaining required surface length has many walls toughness TiO
2nanofiber substrate;
(2) magnetron sputtering prepares multilevel ordered In
2o
3structure: by In
2o
3tiO prepared by target and step (1)
2nanofiber substrate is placed in multi-target magnetic control sputtering instrument, and regulate target class interval to be 3cm-4cm, pass into argon gas, operating pressure is between 0.6Pa-2.0Pa, and power is 100W-150W; At TiO
2nanofiber surface, sputters 5-10 minute in the above conditions to prepare In
2o
3oriented growth structure; Sputter 10-15 minute to prepare In in the above conditions
2o
3flower-like structure; Sputter 15-20 minute to prepare In in the above conditions
2o
3dendritic structure; Sputter 20-30 minute to prepare In in the above conditions
2o
3openworks shape structure; Sputter 30-60 minute to prepare In in the above conditions
2o
3tetrahedral structure.
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| CN201310217883.7A CN103332725B (en) | 2013-06-02 | 2013-06-02 | Multistage and ordered In2O3 structures growing along TiO2 nanofiber surfaces and preparation method |
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| CN103332725B true CN103332725B (en) | 2015-05-20 |
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| CN104867532B (en) * | 2015-04-08 | 2017-01-11 | 浙江理工大学 | Preparation method of compact In2O3 conductive thin film |
| CN104925750B (en) * | 2015-05-07 | 2017-01-04 | 南京文钧医疗科技有限公司 | A kind of TiO with Yolk-Shell structure2nano wire-Ag/AgCl-Fe3o4the preparation method of composite |
| CN105424673B (en) * | 2015-11-03 | 2018-03-20 | 宁波大学 | The SERS substrates and preparation method of carried noble metal nano-cluster with 3D reticulated structures |
| CN113750983A (en) * | 2021-08-27 | 2021-12-07 | 宁波工程学院 | TiO 22/In2O3Heterogeneous mesoporous nanofiber photocatalytic material and preparation method and application thereof |
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| JP4175071B2 (en) * | 2002-10-04 | 2008-11-05 | 住友金属鉱山株式会社 | Oxide sintered body and sputtering target |
| CN102219552A (en) * | 2010-04-19 | 2011-10-19 | 华东师范大学 | Semiconductor material for compounding In2O3 arrow-shaped nano structure on silicon chip and preparation method thereof |
| CN102557114A (en) * | 2011-12-29 | 2012-07-11 | 中国科学院上海光学精密机械研究所 | Preparation method of indium oxide-based gas-sensitive material with three-dimensional hollow multi-stage structure and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4175071B2 (en) * | 2002-10-04 | 2008-11-05 | 住友金属鉱山株式会社 | Oxide sintered body and sputtering target |
| CN102219552A (en) * | 2010-04-19 | 2011-10-19 | 华东师范大学 | Semiconductor material for compounding In2O3 arrow-shaped nano structure on silicon chip and preparation method thereof |
| CN102557114A (en) * | 2011-12-29 | 2012-07-11 | 中国科学院上海光学精密机械研究所 | Preparation method of indium oxide-based gas-sensitive material with three-dimensional hollow multi-stage structure and application thereof |
Non-Patent Citations (1)
| Title |
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| The structure of titanate nanobelts used as seeds for the nucleation of hydroxyapatite at the surface of titanium implants;E. Conforto. et, al.;《Acta Biomaterialia》;20080513;第4卷;第1935页第2栏第7-14行和第1936页第1栏第23-26行 * |
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