CN101049917A - Method for preparing Nano nickelous diselenide in hexagon - Google Patents
Method for preparing Nano nickelous diselenide in hexagon Download PDFInfo
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- CN101049917A CN101049917A CN 200710038608 CN200710038608A CN101049917A CN 101049917 A CN101049917 A CN 101049917A CN 200710038608 CN200710038608 CN 200710038608 CN 200710038608 A CN200710038608 A CN 200710038608A CN 101049917 A CN101049917 A CN 101049917A
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Abstract
This invention relates to a method for preparing hexagonal NiSe2 nanostars. The method utilizes oleic acid as the surfactant, Se powder as the Se source and organic solvent as the reaction medium, and adopts chemical solution method to prepare ordered hexagonal NiSe2 nanostars. The method comprises: dissolving nickel salt, Se source and surfactant in an organic solvent to prepare the reaction solution, performing solvent thermal treatment on the reaction solution, and controlling the reaction temperature and time to obtain ordered hexagonal NiSe2 nanostars. The method is simple, and the morphology of the obtained NiSe2 nanostars is controllabled. Each angle of the hexagonal NiSe2 nanostars is 85 nm, and the central core is 90 nm. The distance between ends of two symmetric angles is 260 nm.
Description
Technical field
The present invention relates to a kind of preparation method of two nickelous selenides, especially relate to a kind of preparation method, adopt the hot legal system of chemical solvents to be equipped with Nano nickelous diselenide with Nano nickelous diselenide of hexagonal configuration.Belong to the nano material preparation technical field.
Background technology
In the past few decades, metal selenide is owing to its excellent physicochemical property have been subjected to paying close attention to widely, and nano material's structure and pattern have very big influence for the performance of nano material with using, so the control of metal selenide serial nano material is synthetic has been subjected to increasing attention.Wherein, two nickelous selenides are a kind of important semiconductor materials, and this material has special electricity and magnetic property.As a kind of good electric conductor and Pauli paramagnetic material, two nickelous selenides belong to weak paramagnetic material and its susceptibility varies with temperature less.In two present nickelous selenide synthetic methods, relatively Chang Yong method have that hydro-thermal is synthetic, solvent thermal synthesis method etc., but it generally can only obtain erose agglomerated particles or larger-size micron order material.As: Hydrothermal Preparation two nickelous selenides, all obtain having erose product or serious nanoparticle of reuniting, be unfavorable for the product morphology control; In addition, with quadrol, pyridine or N, N-dicarboximide etc. also can only synthesize the irregular agglomerated particles of pattern, micron order two nickelous selenides that have or even larger-size for the solvent thermal synthesis method of reaction medium.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of Nano nickelous diselenide in hexagon is provided, technology is simple, and product two nickelous selenides of preparation are the nanometer star with hexagonal configuration of rule, and pattern is controlled.
For realizing such purpose, in the technical scheme of the present invention, be tensio-active agent with oleic acid, with the selenium powder selenium source, be reaction medium with the organic solvent methyl-phenoxide, adopt the chemical solution method preparation to have the Nano nickelous diselenide of the hexagonal configuration of rule.At first nickel salt, selenium source and tensio-active agent are mixed in the organic solvent, preparation feedback liquid carries out solvent heat treatment with the reaction solution for preparing then, controlled temperature and reaction times, can obtain the Nano nickelous diselenide in hexagon of pattern rule.Nano nickelous diselenide is center radiation, highly symmetric hexagonal configuration, and each angular length is 85 ± 2nm, and centronucleus is 90 ± 3nm, and two symmetric angle summit spacings are 260 ± 6nm.
Preparation method of the present invention comprises following concrete steps:
1. the preparation of chemical reaction liquid: nickel salt, tensio-active agent, selenium source are mixed in the reaction solvent, preparation feedback liquid, wherein the concentration of nickel salt remains 0.01～0.05moll
-1, the mol ratio of tensio-active agent and nickel salt is 5: 1～50: 1, the mol ratio of selenium source and nickel salt is 2: 1.
The said nickel salt of the present invention is a nickel acetylacetonate, and described tensio-active agent is an oleic acid, and selenium source is the simple substance selenium powder; Reaction solvent is a methyl-phenoxide.
2. Nano nickelous diselenide in hexagon is synthetic: reaction solution is moved into the autoclave that has polytetrafluoroethylliner liner, in 160 ℃～200 ℃ after solvent heat treatment 8-24 hour, naturally cool to room temperature, product is filtered, with absolute ethanol washing for several times, vacuum is drained sample, promptly can obtain to have the Nano nickelous diselenide of hexagonal configuration.
Excellent results of the present invention is:
1. be tensio-active agent owing to having adopted oleic acid; make the nanocrystal of two nickelous selenides in the process of growth, reach the better controlled growth; this anisotropic growth for Nano nickelous diselenide in hexagon provides good guide effect; and Nano nickelous diselenide in hexagon played the better protecting effect, make it to have homogeneity preferably.
2. because the present invention has adopted the chemical solution method reaction, simple to operate, pattern is controlled, efficient is high, two nickelous selenides of preparation are the hexagonal nano star, the nanometer star is center radiation, highly symmetric hexagonal configuration, each angular length is 85 ± 2nm, centronucleus is 90 ± 3nm, and two symmetric angle summit spacings are 260 ± 6nm.
Description of drawings
Fig. 1 is the collection of illustrative plates of the Nano nickelous diselenide in hexagon of the embodiment of the invention 1 gained, wherein, (a) is X-ray diffracting spectrum, (b) is energy dispersive X-ray spectra.
Fig. 2 is the photo of the Nano nickelous diselenide in hexagon of the embodiment of the invention 1 gained, wherein, (a) is the field emission scanning electron microscope photo, (b) is transmission electron microscope photo, and (b) middle illustration is the electron-diffraction diagram at any angle.
Fig. 3 is the transmission electron microscope photo of the Nano nickelous diselenide in hexagon of the embodiment of the invention 2 gained.
Fig. 4 is the field emission scanning electron microscope photo of the Nano nickelous diselenide in hexagon of the embodiment of the invention 3 gained.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described.The following examples are to further specify of the present invention, and do not limit the scope of the invention.
Embodiment 1
1. in the beaker of a 100ml, the nickel acetylacetonate of 0.4mmol, the oleic acid of 1ml are joined in the methyl-phenoxide of 39ml, magnetic agitation adds the 0.8mmol selenium powder after 30 minutes,, be prepared into the reaction solution of two nickelous selenides.
2. will move into according to the reaction solution that 1. step prepares and have in the autoclave of 50ml polytetrafluoroethylliner liner, in 180 ℃ of solvent thermal after 24 hours, reactor naturally cools to room temperature, centrifugation, with absolute ethanol washing for several times, vacuum is drained sample, promptly can obtain to have the Nano nickelous diselenide of hexagonal configuration.
The x-ray diffraction pattern of the Nano nickelous diselenide of resulting hexagonal configuration such as Fig. 1 a.By the visible prepared material of Fig. 1 a is two nickelous selenides of cubic.Fig. 1 b is the energy dispersive x-ray analysis collection of illustrative plates that obtains the Nano nickelous diselenide of hexagonal configuration, and the contained element of prepared as seen from the figure material is nickel and selenium, and the two atom content ratio is 1: 2.2, meets the stoichiometric ratio of two nickelous selenides.Fig. 2 is field emission scanning electron microscope photo and the transmission electron microscope photo that obtains the Nano nickelous diselenide of hexagonal configuration.By Fig. 2 a as seen, Nano nickelous diselenide is center radiation, highly symmetric hexagonal configuration, and each angular length is 85nm, and centronucleus is 90nm, and two symmetric angle summit spacings are 260nm.The size of Nano nickelous diselenide is identical with Fig. 2 a among Fig. 2 b, and proves that further the Nano nickelous diselenide of gained is a single crystal structure.
Embodiment 2
1. in the beaker of a 100ml, the nickel acetylacetonate of 1mmol, the oleic acid of 5ml are joined in the methyl-phenoxide of 35ml, magnetic agitation adds the 2mmol selenium powder after 30 minutes, be prepared into the reaction solution of two nickelous selenides.
2. will have in the autoclave of 50ml polytetrafluoroethylliner liner according to the reaction solution immigration that 1. step prepares, after 12 hours, reactor naturally cools to room temperature in 200 ℃ of solvent thermal, centrifugation, and with absolute ethanol washing for several times, vacuum is drained sample.Promptly can obtain the big slightly hexagonal Nano nickelous diselenide of size.
Fig. 3 is the transmission electron microscope photo of resulting hexagonal Nano nickelous diselenide under 12 hours condition of 200 ℃ of solvent heat treatment, and two of the hexagonal Nano nickelous diselenide symmetric angle summit spacings increase to and are 300nm as seen from the figure.
Embodiment 3
1. in the beaker of a 100ml, the nickel acetylacetonate of 0.4mmol, the oleic acid of 2ml are joined in the methyl-phenoxide of 38ml, magnetic agitation adds the 0.8mmol selenium powder after 30 minutes,, be prepared into the reaction solution of two nickelous selenides.
2. will have in the autoclave of 50ml polytetrafluoroethylliner liner according to the reaction solution immigration that 1. step prepares, after 8 hours, reactor naturally cools to room temperature in 160 ℃ of solvent thermal, centrifugation, and with absolute ethanol washing for several times, vacuum is drained sample.Promptly can obtain to have the Nano nickelous diselenide of hexagonal configuration.Fig. 4 is the field emission scanning electron microscope photo of the Nano nickelous diselenide of the hexagonal configuration that obtains of embodiment 3.
Claims (2)
1, a kind of preparation method of Nano nickelous diselenide in hexagon is characterized in that may further comprise the steps:
1) preparation of chemical reaction liquid: nickel salt, tensio-active agent, selenium source are mixed in the reaction solvent, preparation feedback liquid, wherein the concentration of nickel salt is 0.01～0.05moll
-1, the mol ratio of tensio-active agent and nickel salt is 5: 1～50: 1, the mol ratio of selenium source and nickel salt is 2: 1; Wherein said nickel salt is a nickel acetylacetonate, and tensio-active agent is an oleic acid, and selenium source is the simple substance selenium powder, and reaction solvent is a methyl-phenoxide;
2) Nano nickelous diselenide in hexagon is synthetic: reaction solution is moved into the autoclave that has polytetrafluoroethylliner liner, in 160 ℃～200 ℃ after solvent heat treatment 8-24 hour, naturally cooling, product is filtered, use absolute ethanol washing, vacuum is drained, and promptly obtains to have the Nano nickelous diselenide of hexagonal configuration.
2, a kind of Nano nickelous diselenide in hexagon that adopts the method preparation of claim 1, it is characterized in that this nanometer star is center radiation, highly symmetric hexagonal configuration, each angular length is 85 ± 2nm, and centronucleus is 90 ± 3nm, and two symmetric angle summit spacings are 260 ± 6nm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079513A (en) * | 2011-02-25 | 2011-06-01 | 安徽大学 | Preparation method of non-integer ratio graphene selenium cobalt nano sheet |
| CN102225340A (en) * | 2011-04-08 | 2011-10-26 | 安徽大学 | Method for synthesizing catalyst capable of efficiently decomposing hydrazine at room temperature |
| CN102583273A (en) * | 2012-02-13 | 2012-07-18 | 安徽大学 | Method for preparing nano nickel selenide with octahedral structure |
| CN102874773A (en) * | 2012-09-10 | 2013-01-16 | 江苏大学 | Preparation method of porous nickel selenide hollow nanospheres |
| CN103043630A (en) * | 2013-01-11 | 2013-04-17 | 长沙理工大学 | Preparation method of spherical nickel diselenide powder |
| CN103466563A (en) * | 2013-08-30 | 2013-12-25 | 天津大学 | Method for synthesizing nickel diselenide nanocrystal in polyalcohol-base solution |
| CN105947995A (en) * | 2016-04-22 | 2016-09-21 | 国家纳米科学中心 | NiSe2 nanosheet with selenium enriched on surface, preparation method thereof, and application thereof |
| CN107161959A (en) * | 2017-04-27 | 2017-09-15 | 中国科学院兰州化学物理研究所 | A kind of preparation method of nickelous selenide micron tube |
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2007
- 2007-03-29 CN CNB2007100386083A patent/CN100526216C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079513A (en) * | 2011-02-25 | 2011-06-01 | 安徽大学 | Preparation method of non-integer ratio graphene selenium cobalt nano sheet |
| CN102079513B (en) * | 2011-02-25 | 2013-05-29 | 安徽大学 | Preparation method of non-integer ratio graphene selenium cobalt nano sheet |
| CN102225340A (en) * | 2011-04-08 | 2011-10-26 | 安徽大学 | Method for synthesizing catalyst capable of efficiently decomposing hydrazine at room temperature |
| CN102225340B (en) * | 2011-04-08 | 2013-11-13 | 安徽大学 | Method for synthesizing catalyst capable of efficiently decomposing hydrazine at room temperature |
| CN102583273A (en) * | 2012-02-13 | 2012-07-18 | 安徽大学 | Method for preparing nano nickel selenide with octahedral structure |
| CN102874773A (en) * | 2012-09-10 | 2013-01-16 | 江苏大学 | Preparation method of porous nickel selenide hollow nanospheres |
| CN102874773B (en) * | 2012-09-10 | 2014-06-25 | 江苏大学 | Preparation method of porous nickel selenide hollow nanospheres |
| CN103043630A (en) * | 2013-01-11 | 2013-04-17 | 长沙理工大学 | Preparation method of spherical nickel diselenide powder |
| CN103466563A (en) * | 2013-08-30 | 2013-12-25 | 天津大学 | Method for synthesizing nickel diselenide nanocrystal in polyalcohol-base solution |
| CN105947995A (en) * | 2016-04-22 | 2016-09-21 | 国家纳米科学中心 | NiSe2 nanosheet with selenium enriched on surface, preparation method thereof, and application thereof |
| CN107161959A (en) * | 2017-04-27 | 2017-09-15 | 中国科学院兰州化学物理研究所 | A kind of preparation method of nickelous selenide micron tube |
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| CN100526216C (en) | 2009-08-12 |
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