CN112499599A - Macroscopic preparation method of ultra-long Se nanowire - Google Patents

Macroscopic preparation method of ultra-long Se nanowire Download PDF

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Publication number
CN112499599A
CN112499599A CN202011375033.6A CN202011375033A CN112499599A CN 112499599 A CN112499599 A CN 112499599A CN 202011375033 A CN202011375033 A CN 202011375033A CN 112499599 A CN112499599 A CN 112499599A
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nanowire
solution
long
ultra
reducing agent
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CN202011375033.6A
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兰金叻
冯李楠
杨小平
陈晓娜
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/02—Elemental selenium or tellurium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Abstract

The invention relates to a macroscopic preparation method of an ultralong Se nanowire, which solves the technical problems of nonuniform diameter or length, nonuniform appearance, low length-diameter ratio, toxic reducing agent, environmental pollution and the like existing in the synthesis of the conventional Se nanowire, and comprises the following steps: (1) placing the Se precursor in deionized water to prepare a solution; (2) putting a reducing agent and a surfactant into deionized water to prepare a solution; (3) and (3) dripping the solution prepared in the step (2) into the solution obtained in the step (1), stirring at normal temperature, and standing at room temperature to obtain the ultra-long Se nanowire. The method can be used in the field of preparation of the ultra-long Se nanowire.

Description

Macroscopic preparation method of ultra-long Se nanowire
Technical Field
The invention relates to a preparation method of a material, in particular to a macroscopic preparation method of an ultralong Se nanowire.
Background
Over the past few decades, there has been a great potential application of one-dimensional nanomaterials in the fabrication of nanoelectronic, optical, optoelectronic and high-energy storage and conversion devices, and efforts have been made to develop one-dimensional (1D) nanomaterials. Selenium is a useful group VI element semiconductor, a Se nanomaterial has attracted much attention due to its unique optical, electrical and magnetic properties and its potential as a fundamental component in nanoelectronic device fabrication, and is anisotropic, including amorphous selenium (a-Se), monoclinic selenium (m-Se) and trigonal selenium (t-Se), where t-Se is the most stable azeotropic form and has a unique atomic chain that facilitates anisotropic growth, readily growing into one-dimensional nanostructures.
At present, there are many reports on solution phase synthesis of Se one-dimensional nanomaterial structures, such as nanoparticles, nanorods and nanowires, and the synthesis methods mainly include a hydrothermal method, a sonochemical method, a solvothermal method, a microwave-assisted hydrothermal method, an oil bath method, and the like. However, the synthesis of the Se nanowires at present has the problems of non-uniform diameter or length, non-uniform morphology, low length-diameter ratio and the like, and even if Se nanowires with uniform synthesis morphology exist, the precursors and reducing agents adopted by the Se nanowires have the problems of toxicity, environmental pollution and the like, and the adopted synthesis methods mostly have dangerous operations such as high temperature and the like, so that the macro-synthesis of the Se nanowires and the subsequent conversion of the Se nanowires serving as templates into other functional materials are greatly hindered.
Disclosure of Invention
The invention provides a macroscopic preparation method of an ultralong Se nanowire which is uniform in diameter or length, uniform in appearance, higher in length-diameter ratio and free of pollution, aiming at the technical problems that the diameter or length of the existing Se nanowire is not uniform enough, the appearance is not uniform, the length-diameter ratio is not high enough, or a reducing agent is toxic and pollutes the environment.
Therefore, the invention provides a macroscopic preparation method of an ultralong Se nanowire, which comprises the following steps: (1) placing the Se precursor in deionized water to prepare a solution with the mass volume concentration of 0.02-0.04 g/ml; (2) putting a reducing agent and a surfactant into deionized water, wherein the mass volume concentration of the reducing agent is 0.04g/ml-0.08 g/ml; the mass volume concentration of the surfactant is 0.004g/ml-0.008 g/ml; (3) and (3) dripping the solution prepared in the step (2) into the solution obtained in the step (1) at 1-3ml/min, stirring at normal temperature, standing at room temperature, and spontaneously growing for 2-96h to obtain the ultra-long Se nanowire.
Preferably, the Se precursor in the step (1) is one or more of sodium selenite, selenious acid, selenium dioxide, selenic acid, sodium selenosulfate and selenium powder.
Preferably, the reducing agent is one or more of ascorbic acid, ethylene glycol, D-sorbitol and glucose.
Preferably, the surfactant is one or more of sodium dodecyl sulfonate, polyvinylpyrrolidone, cetyl trimethyl ammonium bromide and sodium dodecyl benzene sulfonate.
The invention has the following beneficial effects:
(1) the preparation process is simple and easy to implement, has good controllability, and can prepare the Se nanowire with high length-diameter ratio in one step;
(2) the preparation process of the invention directly uses commercial micromolecules as precursors, has high product purity and good uniformity, greatly reduces the cost, and is environment-friendly and pollution-free.
Drawings
Fig. 1 is an XRD pattern of Se nanowires prepared in examples 1-3 of the present invention;
fig. 2a, 2b, and 2c are SEM images of Se nanowires prepared in example 2 of the present invention, respectively.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
(1) Weighing 10g of Na2SeO3Putting the precursor solution into a beaker filled with 500ml of deionized water to prepare a precursor solution with the mass concentration of 0.02 g/ml;
(2) 20g of ascorbic acid and 2g of sodium dodecyl sulfate are weighed and placed in a beaker filled with 500ml of deionized water, the mass concentration of the reducing agent is 0.04g/ml, and the mass concentration of the surfactant is 0.004 g/ml.
(3) Stirring the solution in the (1) and the (2) until the solution is clear, then dripping the solution in the (2) into the solution in the (1) by a peristaltic pump at 1ml/min, stirring for 6h at normal temperature, and then standing at room temperature for spontaneous growth for 2 h.
(4) The XRD of the product Se nanowire obtained by the method is shown as a curve 1 in figure 1, the diffraction peak of the product is completely matched with the Se peak, and no impurity peak exists, so that the pure product Se is obtained, the SEM picture of the product Se is shown as a figure 2a, the length and the diameter of the nanowire all show uniformity, the length can reach 9-13 mu m, the diameter is 30-50nm, and the length-diameter ratio can reach 260-300.
Example 2
(1) Weighing 16gNa2SeO3Putting the precursor solution into a beaker filled with 500ml of deionized water to prepare a precursor solution with the mass concentration of 0.032 g/ml;
(2) 32g of ascorbic acid and 3.2g of sodium dodecyl sulfate are weighed and placed in a beaker filled with 500ml of deionized water, the mass concentration of the reducing agent is 0.064g/ml, and the mass concentration of the surfactant is 0.0064 g/ml.
(3) Stirring the solution in the (1) and the (2) until the solution is clear, then dripping the solution in the (2) into the solution in the (1) by a peristaltic pump at 1ml/min, stirring for 6h at normal temperature, and then standing at room temperature for spontaneous growth for 48 h.
(4) The XRD of the product Se nanowire obtained by the method is shown as a curve 2 in figure 1, the diffraction peak of the product is completely matched with the Se peak, and no impurity peak exists, so that the pure product Se is obtained, the SEM picture of the product Se is shown as a figure 2b, the length and the diameter of the nanowire all show uniformity, the length can reach 9-13 mu m, the diameter is 30-50nm, and the length-diameter ratio can reach 260-300.
Example 3
(1) Weighing 20g of Na2SeO3Putting the precursor solution into a beaker filled with 500ml of deionized water to prepare a precursor solution with the mass concentration of 0.04 g/ml;
(2) 40g of ascorbic acid and 4g of sodium dodecyl sulfate are weighed and placed in a beaker filled with 500ml of deionized water, the mass concentration of the reducing agent is 0.08g/ml, and the mass concentration of the surfactant is 0.008 g/ml.
(3) Stirring the solution in the (1) and the (2) until the solution is clear, then dripping the solution in the (2) into the solution in the (1) by a peristaltic pump at 1ml/min, stirring for 6h at normal temperature, and standing at room temperature for spontaneous growth for 96 h.
(4) The XRD of the product Se nanowire obtained by the method is shown as a curve 3 in figure 1, the diffraction peak of the product is completely matched with the Se peak, and no impurity peak exists, so that the pure product Se is obtained, the SEM picture of the product Se is shown as a figure 2c, the length and the diameter of the nanowire all show uniformity, the length can reach 9-13 mu m, the diameter is 30-50nm, and the length-diameter ratio can reach 260-300.
Example 4
(1) Weighing 10g of Na2SeO3Putting the precursor solution into a beaker filled with 500ml of deionized water to prepare a precursor solution with the mass concentration of 0.02 g/ml;
(2) 20g of glucose and 2g of polyvinylpyrrolidone are weighed and placed in a beaker filled with 500ml of deionized water, the mass concentration of the reducing agent is 0.04g/ml, and the mass concentration of the surfactant is 0.004 g/ml.
(3) Stirring the solution in the (1) and the (2) until the solution is clear, then dripping the solution in the (2) into the solution in the (1) by a peristaltic pump at 1ml/min, stirring for 6h at normal temperature, and standing at room temperature for spontaneous growth for 48 h.
Example 5
(1) Weighing 12gH2SeO3Placing the mixture into a beaker filled with 500ml of deionized water to prepare a precursor solution with the mass concentration of 0.024 g/ml;
(2) 24g of ascorbic acid and 2.4g of sodium dodecyl sulfate are weighed into a beaker filled with 500ml of deionized water, the mass concentration of the reducing agent is 0.048.048 g/ml, and the mass concentration of the surfactant is 0.0048 g/ml.
(3) Stirring the solution in the (1) and the (2) until the solution is clear, then dripping the solution in the (2) into the solution in the (1) by a peristaltic pump at 1ml/min, stirring for 6h at normal temperature, and standing for spontaneous growth for 2h at room temperature.
However, the above description is only exemplary of the present invention, and the scope of the present invention should not be limited thereby, and the replacement of the equivalent components or the equivalent changes and modifications made according to the protection scope of the present invention should be covered by the claims of the present invention.

Claims (4)

1. A macro preparation method of an ultra-long Se nanowire is characterized by comprising the following steps:
(1) placing the Se precursor in deionized water to prepare a solution with the mass volume concentration of 0.02-0.04 g/ml;
(2) putting a reducing agent and a surfactant into deionized water to prepare a solution; the mass concentration of the reducing agent is 0.04-0.08 g/ml; the mass concentration of the surfactant is 0.004-0.008 g/ml;
(3) and (3) dripping the solution prepared in the step (2) into the solution obtained in the step (1) at a rate of 1-3ml/min, stirring at normal temperature, standing at room temperature, and spontaneously growing for 2-96h to obtain the ultra-long Se nanowire.
2. The method for preparing ultra-long Se nanowires of claim 1, wherein the Se precursor in step (1) is one or more of sodium selenite, selenious acid, selenium dioxide, selenic acid, sodium selenosulfate and selenium powder.
3. The method for preparing the ultra-long Se nanowire according to claim 1, wherein the reducing agent is one or more of ascorbic acid, ethylene glycol, D-sorbitol and glucose.
4. The method for preparing super-long Se nanowire according to claim 1, wherein the surfactant is one or more of sodium dodecyl sulfate, polyvinylpyrrolidone, cetyltrimethylammonium bromide and sodium dodecyl benzene sulfonate.
CN202011375033.6A 2020-11-30 2020-11-30 Macroscopic preparation method of ultra-long Se nanowire Pending CN112499599A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN113307234A (en) * 2021-06-08 2021-08-27 南阳师范学院 Tellurium nanowire and synthesis method and application thereof

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US20170365729A1 (en) * 2016-06-20 2017-12-21 National Tsing Hua University Nanowire composite structure and methods of forming the same, sensing device and methods of forming the same and protective structures of a nanowire
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CN101885475A (en) * 2010-07-26 2010-11-17 南京理工大学 Method for synthesizing elemental selenium nano-belt
US20170365729A1 (en) * 2016-06-20 2017-12-21 National Tsing Hua University Nanowire composite structure and methods of forming the same, sensing device and methods of forming the same and protective structures of a nanowire
CN108128760A (en) * 2018-01-03 2018-06-08 韩金玲 A kind of method that simple and fast prepares high length-diameter ratio tellurium nano-wire
CN110492068A (en) * 2019-08-05 2019-11-22 中南大学 Redox graphene-selenium nanowires hydrogel composite material and the preparation method and application thereof

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113307234A (en) * 2021-06-08 2021-08-27 南阳师范学院 Tellurium nanowire and synthesis method and application thereof
CN113307234B (en) * 2021-06-08 2022-03-04 南阳师范学院 Tellurium nanowire and synthesis method and application thereof

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