CN101885475B - Method for synthesizing elemental selenium nano-belt - Google Patents
Method for synthesizing elemental selenium nano-belt Download PDFInfo
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- CN101885475B CN101885475B CN2010102358446A CN201010235844A CN101885475B CN 101885475 B CN101885475 B CN 101885475B CN 2010102358446 A CN2010102358446 A CN 2010102358446A CN 201010235844 A CN201010235844 A CN 201010235844A CN 101885475 B CN101885475 B CN 101885475B
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Abstract
The invention discloses a method for preparing an elemental selenium nano-belt through liquid phase reduction. The method comprises the following steps of: using sodium selenite as a selenium source; using oligosaccharide beta-cyclodextrin as a reducing agent; and preparing a one-dimensional elemental selenium nano-belt by one step through a hydro-thermal reaction. In the reaction process, a surfactant and any other template is not added, the hydro-thermal reaction is performed for 6 to 18 hours at the temperature of between 140 and 180 DEG C to prepare an elemental selenium mono-crystal nano-belt of which the width is 50 to 80 nanometers, the thickness is 10 to 30 nanometers and the length is more than tens of microns, and the materials are crystallized in good condition. The reducing capacity of the beta-cyclodextrin and a hydro-thermal reaction system provide a suitable environment for the full growth of elemental selenium in a one-dimensional direction. The method has the characteristics of simple process route, convenient operation, environment-friendly reducing agent and the like.
Description
Technical field
The invention belongs to field of nanometer material technology, particularly a kind of preparation method of elemental selenium nano-belt.
Background technology
Simple substance selenium is a kind of important elemental semiconductors, have lower melting point (～490K), high optical conductivity (～8 * 10
4S cm
-1), character such as high chemically reactive and nonlinear optical response, can be used for photoelectronics fields such as solar cell, RF, toner cartridge, also be simultaneously the preferred material of synthetic other selenide.In recent years, monodimension nanometer material (like nano wire, nanometer rod, nano belt and nanotube) is because its superior physics, chemical property and in the potential application of field of nanometer devices have become the focus of nano materials research and concern.
The method of synthetic simple substance selenium monodimension nanometer material generally includes liquid phase synthetic technology, vapour deposition (CVD) and microemulsion method etc.For example, C.N.R.Rao etc. passes through NaBH respectively
4Reduction selenium powder and [(CH
3) N]
4Ge
4Se
10Pyrolytic technique obtains the nanometer rod and the nano wire (U.K.Gautam, M.Nath and C.N.R.Rao, J.Mater.Chem., 2003,13,2845.) of simple substance selenium.L.Qi etc. make the monodimension nanometer material (Y.Ma, L.Qi, J.Ma and H.Cheng, Adv.Mater., 2004,16,1023.) of selenium in the micellar solution of nonionogenic tenside.Especially Y.N.Xia group is utilizing Hydrazine Hydrate 80 to prepare work (B.Gates, Y.Yin and Y.Xia, J.Am.Chem.Soc., 2000,122,12582 of having done a series of brilliances in the research of one dimension selenium nano material as reductive agent; B.T.Mayers, K.Liu, D.Sunderland and Y.Xia, Chem.Mater., 2003,15,3852).Other reductive agent also is used to prepare one dimension selenium nano material, as utilizes glucose reduction Na
2SeO
3Preparation elemental selenium nanotube (high Lian, Chen Minghai, Chinese patent: ZL200510024071.6); Utilize vitamins C reduction H
2SeO
3Make elemental selenium nano line (Q.Li and V.W.Yam, Chem.Commun., 2006,1006.).Above research work relates generally to the synthetic of one dimension elemental selenium nano materials such as nano wire, nanotube, but rarely has report for the Study on Preparation Technology of high quality selenium nano-belt.The direct gas phase deposition technology of employings such as Y.Xie makes selenium nano-belt (X.Cao, Y.Xie, S.Zhang and F.Li, Adv.Mater., 2004,16,649.) at 300 ℃; Y.Qian etc. are with SeO
2For Se source, glucose are that reductive agent, Vinylpyrrolidone polymer (PVP) are tensio-active agent, under 160 ℃ of mixed solvent heat conditions, obtain Se nano belt (Q.Xie, Z.Dai, W.Huang; W.Zhang, D.Ma, X.Hu, Y.Qian; Cryst.Growth Design, 2006,6 (6), 1514.).But problems and deficiencies such as these methods still exist, and equipment requirements is higher, complex process, use tensio-active agent guiding are demanded exploitation safety, use, simple selenium nano-belt synthetic technology urgently.
Summary of the invention
The object of the present invention is to provide a kind of new nano material compound method, it is a kind ofly prepare the method for elemental selenium nano-belt through the reduction of oligose one step, have technology simply, the reductive agent environmental friendliness, need not advantages such as other tensio-active agent and template.
The technical solution that realizes the object of the invention is: a kind of compound method of elemental selenium nano-belt, and step is following:
The first step: with the Sodium Selenite is selenium source, is reductive agent with the beta-cyclodextrin, mixes to stir and be dissolved in zero(ppm) water to obtain transparent mixed solution;
Second step: under agitation, the first step gained transparent mixed solution transferred to carry out hydro-thermal reaction in the reaction kettle;
The 3rd step: products therefrom in second step is washed respectively with zero(ppm) water and absolute ethyl alcohol, after the vacuum-drying, make banded elemental selenium nano material.
The present invention compared with prior art, its remarkable advantage: (1) with the oligose beta-cyclodextrin as reductive agent, environmental protection, reducing property is gentle, is easy to control, avoids the use of severe toxicity, dangerous big reductive agent, like NaBH
4Or Hydrazine Hydrate 80 etc.; (2) reaction process need not to add tensio-active agent or other any templates, and gentle reaction system is that the growth of monodimension nanometer material provides suitable environment; (3) the experimental technique route is simple, operation is convenient; (4) the synthetic elemental selenium nano-belt productive rate of institute is high, nano belt width 50～80nm, and thick 5～30nm, length reaches more than tens of microns, and length-to-diameter ratio is big, is the monocrystalline of complete crystallization.
Description of drawings
Fig. 1 is the prepared elemental selenium nano powder of the present invention XRD figure spectrum.
Fig. 2 is the TEM and the FESEM photo of the prepared elemental selenium nano-belt of the present invention, and wherein (a) is the TEM photo, (b) is the FESEM photo.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
The present invention is a kind of method for preparing elemental selenium nano-belt through oligose one step reduction.Have that technology is simple, the reductive agent environmental friendliness, need not advantages such as other tensio-active agent and template.
The compound method of a kind of elemental selenium nano-belt of the present invention is a selenium source with the Sodium Selenite, is reductive agent with the beta-cyclodextrin, makes the nano belt of simple substance selenium through one step of hydro-thermal reaction at water solution system.Concrete steps are following:
The first step: with mol ratio is that 1: 0.5～1: 5 commercially available analyzes Sodium Selenite and beta-cyclodextrin is dissolved in zero(ppm) water, forms colourless transparent solution; This solution is transferred to has in the teflon-lined stainless steel cauldron, the 50-80% of adding distil water to TV, airtight, tighten.
Second step: reaction kettle is put into constant temperature oven, and it is 140～180 ℃ that temperature of reaction is set, and the reaction times is 6～18 hours.
The 3rd step:, wash respectively 3～5 times with zero(ppm) water and absolute ethyl alcohol with products therefrom spinning in second step.50～80 ℃ of vacuum-dryings in vacuum drying oven at last.
Below in conjunction with specific embodiment the present invention is further specified.
Embodiment 1
The preparation mol ratio is 1: 2 Sodium Selenite and a beta-cyclodextrin mixing solutions; Take by weighing 0.005mol analytical pure Sodium Selenite respectively and the 0.01mol beta-cyclodextrin is dissolved in zero(ppm) water; The gained settled solution is transferred in the teflon-lined stainless steel autoclave 80% of adding distil water to cubic capacity.After fully stirring, autoclave is tightened, put into 160 ℃ of constant temperature ovens and react 12h.After reaction finishes, take out reaction kettle, make its naturally cooling.Subsequently throw out in the still is filtered,, use twice of absolute ethanol washing again with distilled water wash three times.With sample 60 ℃ of dry 4h in vacuum drying oven, make elemental selenium nano-belt at last.Fig. 1 is the X ray diffracting spectrum of the prepared elemental selenium nano-belt of present embodiment; All diffraction peaks can index be that the standard powder diffraction data of tripartite phase simple substance selenium is [referring to Joint Committee on Powder Diffraction Standards (JCPDS) among the figure; File No.06-0362], do not find the diffraction peak of any impurity.Fig. 2 is the transmission electron microscope photo and the field emission scanning electron microscope photo of institute's synthetic sample, can find that simple substance selenium presents the banded pattern of one dimension, nanometer bandwidth 60～90nm, and thick 10～20nm, length reaches more than tens of microns, has all exceeded the field range in the photo.
Embodiment 2
The preparation mol ratio is that 1: 0.5 Sodium Selenite and beta-cyclodextrin is dissolved in zero(ppm) water, the gained settled solution is transferred in the teflon-lined stainless steel autoclave 80% of adding distil water to cubic capacity.After fully stirring, autoclave is tightened, put into 140 ℃ of constant temperature ovens and react 18h.After reaction finishes, take out reaction kettle, make its naturally cooling.Subsequently throw out in the still is filtered,, use twice of absolute ethanol washing again with distilled water wash three times.With sample 50 ℃ of dry 6h in vacuum drying oven, make elemental selenium nano-belt at last.Elemental selenium nano bandwidth 60～80nm, thick 10～20nm, length reaches more than tens of microns.
Embodiment 3
The preparation mol ratio is that 1: 3 Sodium Selenite and beta-cyclodextrin is dissolved in zero(ppm) water, the gained settled solution is transferred in the teflon-lined stainless steel autoclave 50% of adding distil water to cubic capacity.After fully stirring, autoclave is tightened, put into 180 ℃ of constant temperature ovens and react 6h.After reaction finishes, take out reaction kettle, make its naturally cooling.Subsequently throw out in the still is filtered,, use twice of absolute ethanol washing again with distilled water wash three times.With sample 70 ℃ of dry 4h in vacuum drying oven, make elemental selenium nano-belt at last.Elemental selenium nano bandwidth 60～90nm, thick 10～30nm, length reaches more than tens of microns.
Embodiment 4
The preparation mol ratio is that 1: 5 Sodium Selenite and beta-cyclodextrin is dissolved in zero(ppm) water, the gained settled solution is transferred in the teflon-lined stainless steel autoclave 70% of adding distil water to cubic capacity.After fully stirring, autoclave is tightened, put into 150 ℃ of constant temperature ovens and react 16h.After reaction finishes, take out reaction kettle, make its naturally cooling.Subsequently throw out in the still is filtered,, use twice of absolute ethanol washing again with distilled water wash three times.With sample 60 ℃ of dry 4h in vacuum drying oven, make elemental selenium nano-belt at last.Elemental selenium nano bandwidth 60～70nm, thick 10～20nm, length reaches more than tens of microns.
Embodiment 5
The preparation mol ratio is that 1: 4 Sodium Selenite and beta-cyclodextrin is dissolved in zero(ppm) water, the gained settled solution is transferred in the teflon-lined stainless steel autoclave 60% of adding distil water to cubic capacity.After fully stirring, autoclave is tightened, put into 160 ℃ of constant temperature ovens and react 8h.After reaction finishes, take out reaction kettle, make its naturally cooling.Subsequently throw out in the still is filtered,, use twice of absolute ethanol washing again with distilled water wash three times.With sample 50 ℃ of dry 6h in vacuum drying oven, make elemental selenium nano-belt at last.Elemental selenium nano bandwidth 60～70nm, thick 5～10nm, length reaches more than tens of microns.
Claims (3)
1. the compound method of an elemental selenium nano-belt is characterized in that step is following:
The first step: with the Sodium Selenite is selenium source, is reductive agent with the beta-cyclodextrin, mixes to stir and be dissolved in zero(ppm) water to obtain transparent mixed solution, and the mol ratio of reactant Sodium Selenite and beta-cyclodextrin is 1: 0.5～1: 5;
Second step: under agitation, the first step gained transparent mixed solution transferred to carry out hydro-thermal reaction in the reaction kettle, hydro-thermal reaction is carried out under 140～180 ℃ temperature condition, and the hydro-thermal reaction time is 6～18 hours;
The 3rd step: products therefrom in second step is washed respectively with zero(ppm) water and absolute ethyl alcohol, after the vacuum-drying, make banded elemental selenium nano material.
2. the compound method of elemental selenium nano-belt according to claim 1 is characterized in that: the transparent mixed solution in second step is transferred in the reaction kettle, to the 50-80% of reaction kettle cubic capacity.
3. the compound method of elemental selenium nano-belt according to claim 1 is characterized in that: the reaction kettle in second step is the teflon-lined stainless steel cauldron.
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| CN102530890B (en) * | 2011-12-15 | 2014-03-26 | 温州大学 | Tellurium semiconductor micro-nanometer crystal and preparation method |
| CN102730651A (en) * | 2012-07-08 | 2012-10-17 | 桂林理工大学 | Solvothermal method for regulating morphology of elemental nano-selenium |
| CN106495105B (en) * | 2016-10-17 | 2018-07-20 | 扬州大学 | A method of synthesis nanometer selenium material |
| CN112499599A (en) * | 2020-11-30 | 2021-03-16 | 北京化工大学 | Macroscopic preparation method of ultra-long Se nanowire |
| CN114988373B (en) * | 2022-06-28 | 2024-03-01 | 安徽大学 | Quasi two-dimensional selenium nano-sheet and preparation method thereof |
| CN115084290B (en) * | 2022-07-06 | 2023-07-25 | 中国科学院化学研究所 | Polycrystalline selenium film, preparation method thereof and solar cell |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1669913A (en) * | 2005-02-25 | 2005-09-21 | 中国科学院上海硅酸盐研究所 | Non-template liquid phase reduction method for preparing elemental selenium nanotube |
| CN101759159A (en) * | 2009-12-24 | 2010-06-30 | 暨南大学 | Method for manufacturing nano-selenium in liquid phase and obtained nano-selenium thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1669913A (en) * | 2005-02-25 | 2005-09-21 | 中国科学院上海硅酸盐研究所 | Non-template liquid phase reduction method for preparing elemental selenium nanotube |
| CN101759159A (en) * | 2009-12-24 | 2010-06-30 | 暨南大学 | Method for manufacturing nano-selenium in liquid phase and obtained nano-selenium thereof |
Non-Patent Citations (2)
| Title |
|---|
| Byron Gates et al..A solution-phase approach to the synthesis of uniform nanowires of crystalline selenium with lateral dimensions in the range of 10-30nm.《J.Am.Chem.Soc》.2000,第122卷(第50期),12582-12583. * |
| Qing Li et al..High-yield synthesis of selenium nanowires in water at room temperature.《Chem.Commun.》.2006,1006-1008. * |
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