CN103628106B - A kind of method preparing indium/tellurium porous nano linear array - Google Patents
A kind of method preparing indium/tellurium porous nano linear array Download PDFInfo
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Abstract
Prepare a method for indium/tellurium porous nano linear array, belong to porous material, technical field of nanometer material preparation.It is characterized in that the method adopts two-step electrochemical anodizing method, self-control porous anodic alumina template (PAA); Prepare the electric depositing solution be made up of the salt of the salt of high-purity In or compound, Te or compound, pH adjusting agent, additive and deionized water; Adopt coating by pulse electrochemical deposition technology, under certain deposition parameter and condition, using the PAA template of metal spraying as anode, graphite is as negative electrode, use the electric depositing solution containing In and Te element, the electrochemical deposition of In and Te element is carried out, the one dimension finally obtained orderly In/Te porous nano linear array in alumina formwork duct.Effect of the present invention and benefit are that preparation is simple, and with low cost, component and structure easy-regulating, exist huge potential application foreground, particularly in sensor application, have important value in the energy, catalysis, absorption, thermoelectricity, optics and electricity etc.
Description
Technical field
The invention belongs to porous material, technical field of nanometer material preparation, relate to the method that one prepares indium/tellurium (In/Te) porous nano linear array.
Background technology
Develop the key areas that nano material novel method for synthesizing controlled on formed shape and size is nanotechnology research.The intrinsic properties of nano-sized materials depends primarily on the factors such as its composition, scantlings of the structure and pattern, and the inorganic nano material thus with special appearance always is the focus that material supply section scholars study.Nano-porous materials refers to have a large amount of certain nano-scale pore textures and the material of high specific surface area.Compare body material and general nano material, nano-porous materials generally has that relative density is low, specific surface area is high, heat insulation, good penetrability and the feature such as absorption property is excellent, thus nano-porous materials has been widely used in the fields such as molecular sieve, filtration, purification, templated synthesis, catalysis, sensing, electricity, optics, energy storage and drug release, plays an important role in science and technology and the development of the national economy.Research proves, compared with zero dimension material, monodimension nanometer material has higher potential using value because having anisotropic growth characteristic in electron optics field of magnetic material.
At present, porous silicon, porous silica, poriferous titanium dioxide, porous carbon are successfully prepared.Along with the development of nanosecond science and technology, one dimension porous nano line (combining the feature of porous material and one-dimensional material) is successfully synthesized out, such as Zhang etc. the porous C o that utilized hydrothermal method to prepare
3o
4nano wire [Y.G.Zhang, Y.C.Chenetal, SolidStateCommun.149 (2009) 585 – 588], the porous Au nano wire [S.Samanman that utilized electrochemical deposition method to prepare such as SalumaSamanman, C.Thammakhetetal, ElectrochimicaActa102 (2013) 342-350.], the metal Assisted Chemical Etching Process method such as Lin has prepared porous Si nano wire [L.H.Lin, S.P.Guoetal, NanoscaleResLett5 (2010) 1822 – 1828] etc.Indium (In) is III A race element, for having the low melting point metal of tetragonal structure, can be used for manufacturing low melting alloy, bearing metal, semi-conductor, electric light source etc.The indium nano wire that utilized porous alumina formwork to prepare such as Chen, and have studied its application in electroluminescent device [F.Chen, A.H.Kitai, JournalofLuminescence128 (2008) 1856 – 1862]; Li etc. utilize plating substitution method to prepare indium nano wire and have studied its optical property [H.H.Li, C.L.Liangetal, NanoscaleResLett4 (2009) 47 – 53].Tellurium (Te), be a kind of narrow-band semiconductor material, there is excellent optics, photoelectricity and thermoelectric property, be described as " VITAMIN of modern industry, national defence and sophisticated technology; the bridge created a miracle of the world ", " being the propping material of contemporary high-tech art novel material ".Along with the development of science and technology, tellurium has become the propping material of novel material needed for robot calculator, communication and aerospace exploitation, the energy, medical and health.Simultaneously due to anisotropic growth tendency and the potential application of its uniqueness, the nano wire of synthesis tellurium causes scientific circles and more and more payes attention to.Zhao etc. utilize electrochemistry and electrophoretic deposition method to prepare tellurium nano-wire array [A.W.Zhaoetal, J.Mater.Res., 18 (2003) 10]; The one dimension tellurium nano-wire of the high-sequential that utilized physical vaporous deposition to prepare such as MuhammadSafdar also have studied its application [M.Safdaretal as field emission device; Nanotechnology24 (2013) 185705].Applicant used the preparation of coating by pulse electrochemical deposition method by Bi/Sb superlattice nano line nano-wire array in 2005.JohnL.Stickney uses electrochemistry Atomic layer deposition method (EC-ALD) on GaAs matrix, by alternately electrochemical deposition synthesis InTe film in independently Te solution and In solution.Porous nano line has larger specific surface area compared with nano thin-film or superlattice nano line.But still do not use pulse electrochemical method in a kind of solution, prepare the report of the indium/tellurium nano-wire with three-dimensional space gap structure so far.Here prepare In/Te nano-wire array by alumina formwork mainly to be deposited by pulsed current or DC electrodeposition mode.Its cost is low, technique is simple and convenient, component and structure easy-regulating.Due to structure and the own physical chemical property of its vesicular nano wire, in the energy, catalysis, absorption, thermoelectricity, optics and electricity etc., there is huge potential application foreground, particularly there is in sensor application important value.
Summary of the invention
The object of the present invention is to provide a kind of method preparing indium/tellurium porous nano linear array, to obtain the porous indium/tellurium nano-wire with novel texture, its step is simple, and controllability is strong, and cost is low.
The present invention uses coating by pulse electrochemical deposition technology, carries out coating by pulse electrochemical deposition to the electrolytic solution containing indium and tellurium element, obtains indium/tellurium porous nano line.The method comprises following concrete steps:
(1) porous alumina formwork is prepared: high-purity aluminum foil is cut into the disk that diameter is 22mm, adopt two-step electrochemical anodizing method, porous anodic alumina template (PAA) is prepared in the electrolytic solution Anodic galvanic corrosion of the oxalic acid containing 0.3M or sulfuric acid or phosphoric acid, and at the golden film of its back spatter evaporation 100nm ~ 200nm as electrode.
(2) preparation is containing the electric depositing solution of In and Te element, and this solution is that pH adjusting agent, additive and deionized water form by the salt of the salt of In or compound, Te or compound.
(3) coating by pulse electrochemical deposition method is used, under certain deposition parameter and condition, using the PAA template of metal spraying as negative electrode, graphite is as anode, use the above-mentioned electric depositing solution containing In and Te element, in alumina formwork duct, carry out the electrochemical deposition of In and Te element.
(4) after galvanic deposit terminates, sample is taken out, place in deionized water and clean, after etching away alumina formwork, obtain In/Te porous nano linear array.
Homogeneous in step (1) described pore size, under the electrolytic solution of oxalic acid or sulfuric acid or phosphoric acid, prepare alumina formwork, bore dia is 10 ~ 200nm, and thickness is 10-150 μm.
Nanowire diameter in the In/Te porous nano linear array prepared in step (4) is 10 ~ 200nm, and nano wire is three-dimensional porous shape structure, and the size of nano wire mesopore is 5 ~ 20nm; The filling ratio of nano wire in template duct is 50% ~ 95%, and in array, nanowire length is 10-150 μm.
Salt or the compound of the In described in step (2) are InCl
3, InF
3, In (NO
3)
3, In (SO
4)
3or In
2o
3in one or more, the salt of Te or compound are TeCl
4, TeO
2, H
6teO
6or H
2teO
3in one or more.Additive is tartrate, or citric acid one or both, content is 0.05M ~ 5M.The pH adjusting agent of solution is nitric acid or sulfuric acid or hydrochloric acid, and in electrolytic solution, pH value is adjusted to 0.1 ~ 3.0.
Coating by pulse electrochemical deposition method in step (3) be apply bias voltage electrodeposition method, its high level sedimentation potential V
1=-2 ~-0.7V, lower level sedimentation potential is V
2=-0.7 ~ 0V; Corresponding depositing time is respectively T
1=5s ~ 100s, T
2=1 ~ 50s; Total electrodeposition time is 60-420min.
Effect of the present invention and benefit are that preparation is simple, and with low cost, component and structure easy-regulating, exist huge potential application foreground, particularly in sensor application, have important value in the energy, catalysis, absorption, thermoelectricity, optics and electricity etc.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of embodiment 1 gained PAA template.
Fig. 2 is the transmission electron microscope high power number form looks photo figure of In/Te porous nano linear array in embodiment 1.
Fig. 3 is the X-ray diffraction collection of illustrative plates of In/Te nano-wire array in embodiment 1.
Fig. 4 is the transmission electron microscope low power number form looks photo figure of In/Te porous nano linear array in embodiment 2.
Embodiment
The specific embodiment of the present invention is described in detail below in conjunction with technical scheme and accompanying drawing.
Embodiment 1:
Two-step electrochemical anodizing method is used to prepare PAA template, and at its back side and at the golden film of its back spatter evaporation 100nm ~ 200nm as electrode.Then prepare electric depositing solution, this solution is by TeO
2, InCl
34H
2o, tartrate, HNO
3solution composition.First by 5mMTeO
2be dissolved in a small amount of deionized water, in 60 DEG C of constant temperature, under magnetic agitation condition, drip dense HNO with dropper
3after making solution become clarification, the solution obtained is poured into and is dissolved with 2.5mMInCl
34H
2in the middle of the tartaric solution of O and 0.133M, obtain required electrolytic solution, gained electrolyte PH value is 1.Use coating by pulse electrochemical deposition method, using the PAA template of metal spraying as anode, graphite is negative electrode, switches on power, and regulates sedimentation potential to be respectively V
1=-0.7V, V
2=-0.23V, corresponding depositing time is respectively T
1=20s, T
2=7s.After galvanic deposit terminates, sample is taken out, place in deionized water and clean, after etching away alumina formwork, obtain In/Te porous nano linear array.
Embodiment 1 gained PAA template as shown in Figure 1.
Embodiment 1 gained In/Te porous nano line TEM image as shown in Figure 2, is shown as vesicular.
Embodiment 1 gained In/Te porous nano line XRD figure spectrum as shown in Figure 3, is shown as heterogeneous indium and tellurium
Embodiment 2:
Two-step electrochemical anodizing method is used to prepare PAA template, and at its back side and at the golden film of its back spatter evaporation 100nm ~ 200nm as electrode.Then prepare electric depositing solution, this solution is by TeO
2, InCl
34H
2o, citric acid, HNO
3solution composition.First by 5mMTeO
2be dissolved in a small amount of deionized water, in 60 DEG C of constant temperature, under magnetic agitation condition, drip dense HNO with dropper
3after making solution become clarification, the solution obtained is poured into and is dissolved with 2.5mMInCl
34H
2in the middle of the solution of O and 0.133M citric acid, obtain required electrolytic solution, gained electrolyte PH value is 1.Use coating by pulse electrochemical deposition method, using the PAA template of metal spraying as anode, graphite is negative electrode, switches on power, and regulates sedimentation potential to be respectively V
1=-0.7V, V
2=-0.23V, corresponding depositing time is respectively T
1=20s, T
2=7s.After galvanic deposit terminates, sample is taken out, place in deionized water and clean, after etching away alumina formwork, obtain In/Te porous nano linear array.
Embodiment 2 gained In/Te porous nano line TEM image as shown in Figure 4.
Claims (7)
1. prepare a method for indium/tellurium porous nano linear array, be utilize porous alumina formwork PAA to assist, use the preparation of coating by pulse electrochemical deposition method, it is characterized in that, indium/tellurium nano-wire has three dimensional pore structures, and its preparation process comprises the following steps:
(1) porous alumina formwork is prepared: high-purity aluminum foil is cut into the disk that diameter is 22mm, adopt two-step electrochemical anodizing method, porous anodic alumina template PAA is prepared in the electrolytic solution Anodic galvanic corrosion of the oxalic acid containing 0.3M or sulfuric acid or phosphoric acid, and at the golden film of its back spatter evaporation 100nm ~ 200nm as electrode;
(2) preparation is containing the electric depositing solution of In and Te element, and this solution is the compound of compound by In, Te, and pH adjusting agent, additive and deionized water form;
(3) coating by pulse electrochemical deposition method is used, under deposition parameter and condition, using the PAA template of metal spraying as negative electrode, graphite is as anode, use the above-mentioned electric depositing solution containing In and Te element, in alumina formwork duct, carry out the electrochemical deposition of In and Te element;
(4) after galvanic deposit terminates, sample is taken out, place in deionized water and clean, after etching away alumina formwork, obtain In/Te porous nano linear array.
2. a kind of method preparing indium/tellurium porous nano linear array according to claim 1, it is characterized in that: step (1) described pore size is homogeneous, alumina formwork is prepared under the electrolytic solution of oxalic acid or sulfuric acid or phosphoric acid, bore dia is 10 ~ 200nm, and thickness is 10-150 μm.
3. a kind of method preparing indium/tellurium porous nano linear array according to claim 1 and 2, it is characterized in that: the nanowire diameter in the In/Te porous nano linear array prepared in step (4) is 10 ~ 200nm, the size of nano wire mesopore is 5 ~ 20nm; The filling ratio of nano wire in template duct is 50% ~ 95%, and in array, nanowire length is 10-150 μm.
4. a kind of method preparing indium/tellurium porous nano linear array according to claim 1, is characterized in that: the compound of step (2) described In is InCl
3, InF
3, In (NO
3)
3, In (SO
4)
3or In
2o
3in one or more, the compound of Te is TeCl
4, TeO
2, H
6teO
6or H
2teO
3in one or more.
5. a kind of method preparing indium/tellurium porous nano linear array according to claim 1, is characterized in that: the additive described in step (2) is one or both in tartrate or citric acid, and content is 0.05M ~ 5M.
6. a kind of method preparing indium/tellurium porous nano linear array according to claim 1, is characterized in that: the pH adjusting agent of step (2) described solution is nitric acid or sulfuric acid or hydrochloric acid, and in electrolytic solution, pH value is adjusted to 0.1 ~ 3.0.
7. a kind of method preparing indium/tellurium porous nano linear array according to claim 1, is characterized in that: the coating by pulse electrochemical deposition method in step (3) be apply bias voltage electrodeposition method, its high level sedimentation potential V
1=-2 ~-0.7V, lower level sedimentation potential is V
2=-0.7 ~ 0V; Corresponding depositing time is respectively T
1=5s ~ 100s, T
2=1 ~ 50s; Total electrodeposition time is 60-420min.
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| CN105112913B (en) * | 2015-09-28 | 2017-10-10 | 西南大学 | A kind of transferable Fe2O3/ Au nano-pore array thin films and preparation method thereof |
| CN105668526B (en) * | 2016-03-24 | 2017-11-10 | 武汉纺织大学 | A kind of preparation method of nanoporous tellurium |
| CN109298027A (en) * | 2017-07-25 | 2019-02-01 | 天津大学 | Gas sensor and preparation method thereof based on the nano-particle modified tungsten oxide nanometer stick of tellurium oxide |
| CN108597710B (en) * | 2018-04-13 | 2019-08-30 | 中国计量大学 | A kind of preparation method of samarium iron nitrogen magnetic nano-array |
| US10443147B1 (en) | 2018-06-06 | 2019-10-15 | King Fahd University Of Petroleum And Minerals | Anodization method for the production of one-dimensional (1D) nanoarrays of indium oxide |
| CN109331820A (en) * | 2018-10-29 | 2019-02-15 | 大连理工大学 | A kind of method that pulse electrodeposition prepares Pt base catalyst under ultrasound condition |
| CN111912881B (en) * | 2019-05-09 | 2024-01-09 | 林宗宏 | Thermoelectric nanosensor and method of making and using same |
| CN110364429B (en) * | 2019-06-12 | 2022-01-07 | 北海惠科光电技术有限公司 | Metal nanowire film, preparation method thereof and thin film transistor array |
| CN112467145B (en) * | 2020-11-25 | 2021-05-28 | 诺正集团股份有限公司 | Aluminum foil with graphene for lithium battery and preparation method thereof |
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