CN103628106A - Method for preparing indium/tellurium porous nanowire array - Google Patents
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- CN103628106A CN103628106A CN201310538989.7A CN201310538989A CN103628106A CN 103628106 A CN103628106 A CN 103628106A CN 201310538989 A CN201310538989 A CN 201310538989A CN 103628106 A CN103628106 A CN 103628106A
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Abstract
The invention discloses a method for preparing an indium/tellurium porous nanowire array, and belongs to the technical field of preparation of porous materials and nano materials. The method is characterized by comprising the following steps: preparing a porous anode alumina template (PAA) by using a two-step anodization method, preparing an electrolytic deposition solution consisting of a high-purity In salt or compound, a salt or compound of Te, a pH conditioning agent, an additive and deionized water, and performing electrochemical deposition on In and Te elements in pore canals of the alumina template by adopting a pulse electrochemical deposition technology, using the electrolytic deposition solution containing the In and Te elements and taking metal-sprayed PAA template as an anode and graphite as a cathode under certain deposition parameters and conditions, so as to finally obtain a one-dimensional ordered In/Te porous nanowire array. The method has the effects and benefits that the preparation is simple, the cost is low, and components and structures are easy to regulate and control; the array has a significant potential application prospect in fields of energy, catalysis, adsorption, thermoelectricity, optics, electrics and the like, and particularly has great values in application of sensors.
Description
Technical field
The invention belongs to porous material, nano material preparing technical field, relate to a kind of method of preparing indium/tellurium (In/Te) porous nano linear array.
Background technology
Exploitation nano material controlled novel method for synthesizing in formed shape and size is a key areas of nanotechnology research.The intrinsic properties of nano-sized materials depends primarily on its factors such as composition, scantlings of the structure and pattern, thereby the inorganic nano material 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, the features such as nano-porous materials generally has that relative density is low, specific surface area is high, heat insulation, good penetrability and absorption property excellence, thereby the field such as nano-porous materials has been widely used in that molecular sieve, filtration, purification, template are synthetic, catalysis, sensing, electricity, optics, energy storage and drug release, in science and technology and the development of the national economy, play an important role.Studies have shown that, compare 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, successfully preparation of porous silicon, porous silica, poriferous titanium dioxide, porous carbon.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. utilizes hydrothermal method to prepare porous C o
3o
4nano wire [Y.G.Zhang, Y.C.Chen et al, Solid State Commun.149 (2009) 585 – 588], Saluma Samanman etc. utilizes electrochemical deposition method to prepare porous Au nano wire [S.Samanman, C.Thammakhet et al, Electrochimica Acta102 (2013) 342-350.], the use metal Assisted Chemical Etching Process methods such as Lin have been prepared porous Si nano wire [L.H.Lin, S.P.Guo et al, Nanoscale Res Lett5 (2010) 1822 – 1828] etc.Indium (In) ShiⅢ A family 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.Chen etc. utilize porous alumina formwork to prepare indium nano wire, and have studied its application [F.Chen, A.H.Kitai, Journal of Luminescence128 (2008) 1856 – 1862] in electroluminescent device; The utilizations such as Li are electroplated substitution method and have been prepared indium nano wire and studied its optical property [H.H.Li, C.L.Liang et al, Nanoscale Res Lett4 (2009) 47 – 53].Tellurium (Te), be a kind of narrow-band semiconductor material, there is good optics, photoelectricity and thermoelectric property, be described as " VITAMIN of modern industry, national defence and sophisticated technology; the bridge creating a miracle of the world ", " being the propping material of contemporary high-tech art novel material ".Along with scientific and technological development, tellurium has become the propping material of robot calculator, communication and aerospace exploitation, the energy, the required novel material of medical and health.Due to anisotropic growth tendency and the potential application of its uniqueness, the nano wire of synthetic tellurium has caused that scientific circles more and more pay attention to simultaneously.Zhao etc. utilize electrochemistry and electrophoretic deposition method to prepare tellurium nano-wire array [A.W.Zhao et al, J.Mater.Res., 18(2003) 10]; Muhammad Safdar etc. utilizes physical vaporous deposition to prepare the one dimension tellurium nano-wire of high-sequential and has studied its application as field emission device [M.Safdar et al; Nanotechnology 24 (2013) 185705].Yet still do not combine so far the report of preparing porous nano line of indium and tellurium.Here by alumina formwork, preparing In/Te nano-wire array is mainly to deposit or DC electrodeposition mode by pulsed current.Its cost is low, technique is simple and convenient, component and structure easy-regulating., there is huge potential application foreground at aspects such as the energy, catalysis, absorption, thermoelectricity, optics and electricity in structure and self physicochemical property due to its vesicular nano wire, particularly in sensor application, has important value.
Summary of the invention
The object of the present invention is to provide a kind of method of 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, and the electrolytic solution that contains indium and tellurium element is carried out to coating by pulse electrochemical deposition, obtains indium/tellurium porous nano line.The method comprises following concrete steps:
(1) prepare porous alumina formwork: high-purity aluminum foil is cut into the disk that diameter is 22mm, adopt two-step anodization method, porous anodic alumina template (PAA) is prepared in electrolytic solution Anodic galvanic corrosion at the oxalic acid that contains 0.3M or sulfuric acid or phosphoric acid, and at the golden film of its back spatter evaporation 100nm～200nm as electrode.
(2) electric depositing solution that preparation contains In and Te element, this solution is salt or the compound by the salt of In or compound, Te, pH adjusting agent, additive and deionized water form.
(3) use coating by pulse electrochemical deposition method, 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 that contains In and Te element, in alumina formwork duct, carry out the electrochemical deposition of In and Te element.
(4) after galvanic deposit finishes, sample is taken out, place in deionized water and clean, etch away after alumina formwork, obtain In/Te porous nano linear array.
Nanowire diameter in the In/Te porous nano linear array preparing in step (4) is 10～200nm, 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 10-150um.
At the described pore size homogeneous of step (1), under the electrolytic solution of oxalic acid or sulfuric acid or phosphoric acid, prepare alumina formwork, bore dia is 10～200nm, thickness is 10-150um.
Salt or compound at 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 pulse 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 at aspects such as the energy, catalysis, absorption, thermoelectricity, optics and electricity, particularly in sensor application, has important value.
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
Below in conjunction with technical scheme and accompanying drawing, describe the specific embodiment of the present invention in detail.
Embodiment 1:
Use two-step anodization legal system for 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 5mM TeO
2be dissolved in a small amount of deionized water, in 60 ℃ of constant temperature, under magnetic agitation condition, with dropper, drip dense HNO
3solution is become after clarification, the solution obtaining is poured into and is dissolved with 2.5mM InCl
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 finishes, sample is taken out, place in deionized water and clean, etch away after 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:
Use two-step anodization legal system for 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 5mM TeO
2be dissolved in a small amount of deionized water, in 60 ℃ of constant temperature, under magnetic agitation condition, with dropper, drip dense HNO
3solution is become after clarification, the solution obtaining is poured into and is dissolved with 2.5mM InCl
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 finishes, sample is taken out, place in deionized water and clean, etch away after alumina formwork, obtain In/Te porous nano linear array.
Embodiment 2 gained In/Te porous nano line TEM images as shown in Figure 4.
Claims (7)
1. a method of preparing indium/tellurium porous nano linear array, is to utilize porous alumina formwork (PAA) auxiliary, uses the preparation of coating by pulse electrochemical deposition method, and its feature comprises the following steps:
(1) prepare porous alumina formwork: high-purity aluminum foil is cut into the disk that diameter is 22mm, adopt two-step anodization method, porous anodic alumina template (PAA) is prepared in electrolytic solution Anodic galvanic corrosion at the oxalic acid that contains 0.3M or sulfuric acid or phosphoric acid, and at the golden film of its back spatter evaporation 100nm～200nm as electrode;
(2) electric depositing solution that preparation contains In and Te element, this solution is salt or the compound by the salt of In or compound, Te, pH adjusting agent, additive and deionized water form;
(3) use coating by pulse electrochemical deposition method, 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 that contains In and Te element, in alumina formwork duct, carry out the electrochemical deposition of In and Te element;
(4) after galvanic deposit finishes, sample is taken out, place in deionized water and clean, etch away after alumina formwork, obtain In/Te porous nano linear array.
2. a kind of method of preparing indium/tellurium porous nano linear array according to claim 1, it is characterized in that: the described pore size homogeneous of step (1), under the electrolytic solution of oxalic acid or sulfuric acid or phosphoric acid, prepare alumina formwork, bore dia is 10～200nm, and thickness is 10-150um.
3. a kind of method of preparing indium/tellurium porous nano linear array according to claim 1, is characterized in that: salt or the compound of the described In of 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.
4. a kind of method of preparing indium/tellurium porous nano linear array according to claim 1, is characterized in that: the described additive of step (2) is tartrate, or citric acid one or both, content is 0.05M～5M.
5. a kind of method of preparing indium/tellurium porous nano linear array according to claim 1, is characterized in that: the pH adjusting agent of the described solution of step (2) is nitric acid or sulfuric acid or hydrochloric acid, and in electrolytic solution, pH value is adjusted to 0.1～3.0.
6. a kind of method of 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 pulse 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.
7. a kind of method of preparing indium/tellurium porous nano linear array according to claim 1, it is characterized in that: the nanowire diameter in the In/Te porous nano linear array preparing in step (4) is 10～200nm, 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 10-150um.
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| CN105112913A (en) * | 2015-09-28 | 2015-12-02 | 西南大学 | Transferable Fe<2>O<3>/Au nano-pore array film and method for preparing same |
| CN105668526A (en) * | 2016-03-24 | 2016-06-15 | 武汉纺织大学 | Preparation method of nano porous tellurium |
| CN108597710A (en) * | 2018-04-13 | 2018-09-28 | 徐靖才 | A kind of preparation method of samarium iron nitrogen magnetic nano-array |
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| 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 |
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| CN105668526A (en) * | 2016-03-24 | 2016-06-15 | 武汉纺织大学 | Preparation method of nano porous tellurium |
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