CN103332658A - Preparation method of high-purity selenium nanometer powder - Google Patents
Preparation method of high-purity selenium nanometer powder Download PDFInfo
- Publication number
- CN103332658A CN103332658A CN2013102536767A CN201310253676A CN103332658A CN 103332658 A CN103332658 A CN 103332658A CN 2013102536767 A CN2013102536767 A CN 2013102536767A CN 201310253676 A CN201310253676 A CN 201310253676A CN 103332658 A CN103332658 A CN 103332658A
- Authority
- CN
- China
- Prior art keywords
- selenium
- preparation
- purity
- powder
- anode
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention relates to a preparation method of high-purity selenium nanometer powder and belongs to the field of nanometer material preparation. The preparation process is characterized by comprising the following steps of adopting direct current arc evaporation condensation equipment, taking an elemental nonmetal high-purity selenium block as an anode, taking metal tungsten as a cathode and preparing the high-purity selenium nanometer powder with the grain size of 20-100nm in the atmosphere that the argon pressure is 0.1-0.5MPa and under the conditions that the reaction current is 40-80A, the voltage between the anode and the cathode is 40-60V and the evaporation time is 20-40min. The method disclosed by the invention is simple in process and has the advantages that the purity of the prepared selenium nanometer powder is high and the grain size is controllable.
Description
Technical field
The invention belongs to the nano material preparation technology, be specifically related to a kind of preparation method of high-purity selenium nanometer powder.
Background technology
Simple substance selenium is a kind of important elemental semiconductors, and has important physical function and pharmacological action.Have excellent characteristics such as optical property, electric property and mechanical property, can be used for solar cell, rectifier, photosensor, optoelectronic areas such as toner cartridge, the catalyzer of electrolytic manganese industry also is simultaneously the preferred material of synthetic other selenide.And selenium still is a kind of good antioxidants and immunomodulator.
Along with development of science and technology, the critical role that high-purity nano selenium and compound-material thereof occupy in present high-technology industry, national defence and sophisticated technology field more and more is subject to people's attention.Synthetic other functional materialss such as CdSe, Ag
2The first-selected material of Se, PbSe etc. is that assemble nanometer functional device, optoelectronic device structure Se nano wire have important meaning at aspects such as functional device exploitation and ultra-large integrated researchs.The quantum confined effect of selenium and unique anisotropy characteristics attract much attention gradually, become the construction unit of the nano photoelectronic devices of a new generation, in the electricity that makes up nanoscale, photoelectric device, there is good prospects for application nonlinear optical material and photocatalyst material aspect, these nano materials have unique light,, magnetic property, at precision instrument, field such as space flight and electronics is widely used in sensor, opticinstrument such as micro laser and atom-probe and photometer, the physics that it is superior, chemical property and in the potential application of field of nanometer devices has become the focus of nano materials research and concern.
Research mainly concentrates on nano wire, nano belt, nanotube, nanometer rod, field such as nanocrystalline utilizes liquid phase synthetic technology, vapour deposition (CVD) and microemulsion method.The ultrasonic method chemical method, etc., the nanocrystalline preparation of Se can also be adopted other method, as utilizes laser ablation method and electrochemical process.L. Qi etc. makes one-dimensional nano line in the micellar solution of ionic surface active agent; Y. N. Xia group utilizes glucose reduction Na
2SeO
3The preparation elemental selenium nanotube; Employing gas phase deposition technologies such as Y.Xie make selenium nano-belt at 300 ℃; C. N. R. Rao etc. passes through NaBH respectively
4Reduction selenium powder and [(CH
3) N]
4Ge
4Se
10Pyrolytic technique obtains the selenium nanometer rod of simple substance.But these methods still exist equipment requirements height, complex process, use tensio-active agent guiding or complicated problems and deficiencies such as selenium presoma, and the material system instability is easily reunited, and demands developing safety urgently, simple selenium nanometer synthetic technology.
Traditional selenium nano powder preparation method is difficult to prepare high-purity selenium nanometer powder controlled than crystal particle scale in the big scale scope below 100nm.And using vaporization condensation process prepares nano material and sends out that environmental pollution is few, cost is lower, be easy to suitability for industrialized production, and nano-powder purity height, the crystal formation of comparing the using vaporization condensation process preparation with other preparation method be good, single to be disperseed, the reunion degree is low and particle diameter is controlled.
Summary of the invention
The objective of the invention is to solve prior art problems, and a kind of preparation method of high-purity selenium nanometer powder is provided.Method provided by the present invention has realized the control of grain diameter, and technology is simple.
The present invention adopts noble gas protection-direct current arc evaporative condenser to prepare selenium nano powder material, and concrete steps are as follows:
Adopt the direct current arc evaporation condensing plant, be anode with the nonmetal high-purity selenium piece of simple substance (purity is 99.999%), tungsten is negative electrode, be in the atmosphere of 0.1-0.5MPa at ar pressure, reaction current 40～80A, voltage is 40～60V between anode and negative electrode, and the reaction times is 20～40min, the preparation selenium nano powder;
Wherein, the particle diameter of described selenium nano powder is 20～100nm;
Compared with prior art, the present invention has following beneficial effect:
Detecting through X-ray diffraction, X-ray fluorescence spectra etc. is single selenium (Te) thing phase, and chemical purity reaches 99.999%.
Description of drawings
The powder X-ray ray spectrogram of the selenium of Fig. 1, embodiment 1 preparation.
The TEM photo of the nanometer selenium powder of Fig. 2, embodiment 1 preparation.
The TEM photo of the nanometer selenium powder of Fig. 3, embodiment 2 preparations
The TEM photo of the nanometer selenium powder of Fig. 4, embodiment 3 preparations
The invention will be further described below in conjunction with the drawings and specific embodiments, but protection scope of the present invention is not limited to following embodiment.
Embodiment
Embodiment 1
1) adopts the direct current arc evaporation condensing plant, be anode with the nonmetal selenium piece of simple substance (purity is 99.999%), tungsten is negative electrode, be in the atmosphere of 0.1MPa at ar pressure, reaction current 40A, voltage is 40V between anode and negative electrode, and the reaction times is 40min, the selenium nano powder of preparation 20～50nm;
The X-ray spectrogram of selenium nano powder as shown in Figure 1, as we know from the figure, sample is the Te pure phase, diffraction peak intensity height, well-crystallized.Through the X-ray fluorescence spectra test shows, the chemical purity of this powder reaches 99.999%.The tem analysis result (Fig. 2) of powder shows that the particle diameter of selenium nano powder is 20～50nm.
Embodiment 2
1) adopts the direct current arc evaporation condensing plant, be anode with the nonmetal selenium piece of simple substance (purity is 99.999%), tungsten is negative electrode, be in the atmosphere of 0.3MPa at ar pressure, reaction current 60A, voltage is 50V between anode and negative electrode, and the reaction times is 30min, the selenium nano powder of preparation 40～80nm;
The X-ray spectrogram of selenium nano powder as shown in Figure 1, as we know from the figure, sample is the Te pure phase, diffraction peak intensity height, well-crystallized.Through the X-ray fluorescence spectra test shows, the chemical purity of this sintering block sample reaches 99.999%.(Fig. 3) shows through tem analysis, and the size of microcrystal of selenium nano powder is 40～80nm.
Embodiment 3
1) adopts the direct current arc evaporation condensing plant, be anode with the nonmetal selenium piece of simple substance (purity is 99.999%), tungsten is negative electrode, be in the atmosphere of 0.5MPa at ar pressure, reaction current 80A, voltage is 60V between anode and negative electrode, and the reaction times is 20min, the selenium nano powder of preparation 60～100nm.
The X-ray spectrogram of selenium nano powder as shown in Figure 1, as we know from the figure, sample is the Te pure phase, diffraction peak intensity height, well-crystallized.Through the X-ray fluorescence spectra test shows, the chemical purity of this powder reaches 99.999%.The tem analysis result (Fig. 4) of powder shows that the particle diameter of selenium nano powder is 60～100nm.
Claims (1)
1. the preparation method of a high-purity selenium nano-powder material is characterized in that, may further comprise the steps:
Adopting the direct current arc evaporation condensing plant, is anode with the nonmetal selenium piece of simple substance, and tungsten is negative electrode, is in the atmosphere of 0.1～0.5MPa at ar pressure, reaction current 40～80A, and voltage is 40～60V between anode and negative electrode, the reaction times is 20～40min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013102536767A CN103332658A (en) | 2013-06-24 | 2013-06-24 | Preparation method of high-purity selenium nanometer powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013102536767A CN103332658A (en) | 2013-06-24 | 2013-06-24 | Preparation method of high-purity selenium nanometer powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103332658A true CN103332658A (en) | 2013-10-02 |
Family
ID=49240887
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013102536767A Pending CN103332658A (en) | 2013-06-24 | 2013-06-24 | Preparation method of high-purity selenium nanometer powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103332658A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105720249A (en) * | 2016-02-22 | 2016-06-29 | 北京工业大学 | Preparation method of Sn-Si alloy-type nano-composite powder |
| CN105967152A (en) * | 2016-05-17 | 2016-09-28 | 广东省稀有金属研究所 | Method and device for preparing high-purity oxygen-free selenium granules |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776524A (en) * | 2011-05-09 | 2012-11-14 | 河北天寅生物技术股份有限公司 | Preparation method for nanometer selenium |
-
2013
- 2013-06-24 CN CN2013102536767A patent/CN103332658A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776524A (en) * | 2011-05-09 | 2012-11-14 | 河北天寅生物技术股份有限公司 | Preparation method for nanometer selenium |
Non-Patent Citations (1)
| Title |
|---|
| 周飞鹏等: "电弧法制备纳米粉体实验装置的设计", 《中国科技论文在线》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105720249A (en) * | 2016-02-22 | 2016-06-29 | 北京工业大学 | Preparation method of Sn-Si alloy-type nano-composite powder |
| CN105720249B (en) * | 2016-02-22 | 2018-03-13 | 北京工业大学 | A kind of preparation method of Sn Si alloy-type nano composite powders |
| CN105967152A (en) * | 2016-05-17 | 2016-09-28 | 广东省稀有金属研究所 | Method and device for preparing high-purity oxygen-free selenium granules |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Jian et al. | Arrays of ZnO/MoS2 nanocables and MoS2 nanotubes with phase engineering for bifunctional photoelectrochemical and electrochemical water splitting | |
| Wang et al. | Zr-doped β-In2S3 ultrathin nanoflakes as photoanodes: enhanced visible-light-driven photoelectrochemical water splitting | |
| Wu et al. | In situ growth of matchlike ZnO/Au plasmonic heterostructure for enhanced photoelectrochemical water splitting | |
| He et al. | One-step solvothermal synthesis of petalous carbon-coated Cu+-doped CdS nanocomposites with enhanced photocatalytic hydrogen production | |
| Zhang et al. | 3D branched ZnO nanowire arrays decorated with plasmonic Au nanoparticles for high-performance photoelectrochemical water splitting | |
| Hou et al. | Visible light-driven α-Fe2O3 nanorod/graphene/BiV1–x Mo x O4 core/shell heterojunction array for efficient photoelectrochemical water splitting | |
| Chen et al. | Fabrication of TiO2− Pt coaxial nanotube array Schottky structures for enhanced photocatalytic degradation of phenol in aqueous solution | |
| Pan et al. | Facile fabrication of hierarchical TiO2 nanobelt/ZnO nanorod heterogeneous nanostructure: an efficient photoanode for water splitting | |
| Yu et al. | ZnS/ZnO heteronanostructure as photoanode to enhance the conversion efficiency of dye-sensitized solar cells | |
| Shen et al. | Surface tuning for promoted charge transfer in hematite nanorod arrays as water-splitting photoanodes | |
| Hussain et al. | Spray pyrolysis deposition of ZnFe2O4/Fe2O3 composite thin films on hierarchical 3-D nanospikes for efficient photoelectrochemical oxidation of water | |
| Lin et al. | Electrodeposition preparation of ZnO nanobelt array films and application to dye-sensitized solar cells | |
| Meng et al. | Facet cutting and hydrogenation of In2O3 nanowires for enhanced photoelectrochemical water splitting | |
| Xia et al. | Visible-light self-powered photodetector and recoverable photocatalyst fabricated from vertically aligned Sn3O4 nanoflakes on carbon paper | |
| Liu et al. | Electrodeposition of ZnO nanoflake-based photoanode sensitized by carbon quantum dots for photoelectrochemical water oxidation | |
| Xue et al. | Photosensitization of TiO2 nanotube arrays with CdSe nanoparticles and their photoelectrochemical performance under visible light | |
| Kadhim et al. | Photocatalytic activity and photoelectrochemical properties of Ag/ZnO core/shell nanorods under low-intensity white light irradiation | |
| Joshna et al. | Fast response of UV photodetector based on Ag nanoparticles embedded uniform TiO2 nanotubes array | |
| Liao et al. | Enhancing the efficiency of CdS quantum dot-sensitized solar cells via electrolyte engineering | |
| Li et al. | CdS/CdSe co-sensitized 3D SnO 2/TiO 2 sea urchin-like nanotube arrays as an efficient photoanode for photoelectrochemical hydrogen generation | |
| Lin et al. | Pt-doped α-Fe2O3 photoanodes prepared by a magnetron sputtering method for photoelectrochemical water splitting | |
| Li et al. | InP nanopore arrays for photoelectrochemical hydrogen generation | |
| Zhang et al. | In situ growth of single-crystal TiO 2 nanorod arrays on Ti substrate: Controllable synthesis and photoelectro-chemical water splitting | |
| Nasori et al. | Realizing super-long Cu2O nanowires arrays for high-efficient water splitting applications with a convenient approach | |
| Shin et al. | Highly transparent dual-sensitized titanium dioxide nanotube arrays for spontaneous solar water splitting tandem configuration |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131002 |