CN101025416B - Luminescent zinc selenide nano rod synthesizing method and its use - Google Patents
Luminescent zinc selenide nano rod synthesizing method and its use Download PDFInfo
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- CN101025416B CN101025416B CN2007100130077A CN200710013007A CN101025416B CN 101025416 B CN101025416 B CN 101025416B CN 2007100130077 A CN2007100130077 A CN 2007100130077A CN 200710013007 A CN200710013007 A CN 200710013007A CN 101025416 B CN101025416 B CN 101025416B
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Abstract
The present invention supplies a synthetic method of luminescence zinc selenide Nanorods, the method proceed with the following steps: a. first putting sodium borohydride and selenium powder with reaction ratio dissolved in water, and then, under the protection of inert gases they react to get the solution of sodium borohydride with the 1.5-2% weight concentration ; b. zinc ions are dissolved in accordance with the soluble salt: L-mercapto alanine: water = 100:22-37:140000-240000 weight ratio of blending, then mixing to join the thioglycolic acid or mercaptopropionic acid, adjusting pH = 9-11, and then remove the dissolved oxygen from solution by filling inert gas; c. putting the sodium borohydride solution of a procedure into the solution of b procedure, and then heating reversing, obtain a luminescent zinc selenide Nanorods Solution.
Description
Technical field
The invention belongs to technical field of inorganic chemical industry, relate to the production method of nano material, refer more particularly to synthetic method water-soluble, luminescence zinc selenide Nanorods; In addition, the purposes that also relates to this luminescence zinc selenide Nanorods.
Background technology
Since carbon nano-tube is found, one-dimensional nano structure material receives much attention because of its peculiar electricity, optics, magnetic and mechanical property and the potential application in nano-device structure thereof, thereby to explore preparation low-dimension nano material structurally ordered, function admirable be the focus of research always.As a rule, the preparation of one dimension semiconductor nano material mainly is to make by decomposing metal organic compound under the high temperature.But resulting product is not water-soluble and bio-compatibility, and this just limits its application in bioanalysis.Meanwhile, the preparation semiconductor nano material has also obtained certain development in aqueous solution, but resulting product substantially all is granular.
In II-VI compound semiconductor nano material, have only one dimension water soluble cadmium telluride nano material to appear in the newspapers, other one dimension II-VI compound semiconductor nano materials research also is in the elementary stage.Zinc selenide is a kind of important broadband (2.8eV) II-VI compound semiconductor nano material, is to make bluish-green semiconductor laser device, the important materials of nonlinear optical thermal device and infrared device.The exploitation of zinc selenide base semiconductor laser and light emitting diode becomes one of focus of semiconductor light sources exploitation.Because it is little to have leakage current, be difficult for the character of many uniquenesses such as deliquescence, can make nuclear radiation detector and some base materials under the room temperature with it.Simultaneously, from the angle of energy gap, having bigger energy gap (Eg=117eV), also is solar cell material preferably.As be widely used in various light-emitting devices, laser and infrared detector, infrared window and fields such as nonlinear optical material photochemical catalyst and light sensor.Along with reducing of particle size, because quantum size effect, II-VI family semiconductor nano material presents a series of and the distinct specific physique of body phase material, as light absorption and remarkable enhancing of fluorescent emission and generation blue shift, optics third-order non-linear response speed significantly improves etc., is expected to become the material of making solid-state electronic optoelectronic device of new generation.So far the report of water breakthrough dissolubility, luminescence zinc selenide Nanorods not as yet.
Summary of the invention
One of purpose of the present invention provides a kind of simple, with low cost, and stability is the synthetic method of luminescence zinc selenide Nanorods preferably; Two of purpose provides the purposes of this luminescence zinc selenide Nanorods.
One of purpose of the present invention can realize by following technical measures:
This method is carried out according to the following steps:
A, elder generation are dissolved in sodium borohydride and selenium powder in the water according to reaction ratio, react under inert gas shielding then, and getting weight concentration is the sodium hydrogen selenide solution of 1.5-2%;
B, according to the soluble-salt that is dissolved with zinc ion: L-cysteine: water=100:22-37:140000-240000 weight portion proportioning mixing, add mercaptoacetic acid or mercaptopropionic acid down in stirring again, transfer pH=9-11, filling with inert gas is removed the dissolved oxygen DO in the solution then;
C, according to sodium hydrogen selenide solution and the b operation solution mixing of reaction ratio with a operation, reflux then, the luminescence zinc selenide Nanorods aqueous solution.
One of purpose of the present invention also can realize by following technical measures:
The described soluble-salt that is dissolved with zinc ion is selected from zinc acetate, zinc chloride or zinc nitrate; The described reflux time is 4-6 hour.
Two of purpose of the present invention can realize by following technical measures:
The luminescence zinc selenide Nanorods that the present invention synthesizes is used for the industry of biomarker, cell imaging, bioanalysis and solid-state electronic optoelectronic device and implements.
The present invention at first is dissolved in sodium borohydride and selenium powder in the water according to the chemical reaction proportioning, makes mixed solution, is prepared into sodium hydrogen selenide solution again under inert gas shielding; Be raw material with this water miscible salt solusion that contains zinc ion then, with L cysteine and mercaptoacetic acid is part, regulating the pH value is 9-11, the dissolved oxygen DO that filling with inert gas is removed in the solution adds the sodium hydrogen selenide solution for preparing previously afterwards again, through reflux, obtain the aqueous solution of zinc selenide nanometer rods.This method is that solvent has prepared luminous zinc selenide nanometer rods with water, and course of reaction is simple, and is with low cost, and the pattern of working condition and product is easy to control, and is free from environmental pollution.Prepared luminous zinc selenide nanometer rods product can be stablized half a year at least, owing to its water-soluble and stability of photoluminescence, can be widely used in bioanalysis, mark and the imaging in addition.
Description of drawings:
Fig. 1 is luminescence zinc selenide Nanorods transmission photo (TEM) and the high-resolution photo (HRTEM) that the present invention prepares;
Fig. 2 is the luminescence zinc selenide Nanorods X-ray powder diffraction figure that the present invention prepares;
Fig. 3 is the time dependent absorption spectrum of luminescence zinc selenide Nanorods that the present invention prepares;
Fig. 4 is that the luminescence zinc selenide Nanorods for preparing of the present invention is with changing fluorescence spectrum standing time;
Fig. 5 is that the luminescence zinc selenide Nanorods that the present invention prepares changes fluorescence spectrum with return time;
Fig. 6 is the fluorescence spectrum that the luminescence zinc selenide Nanorods for preparing of the present invention changes with pH.
Embodiment:
Embodiment 1:
A, 0.2056g sodium borohydride and 0.195g selenium powder are dissolved in the 10mL ultrapure water, under argon shield, react then, make weight concentration and be 1.5% sodium hydrogen selenide solution;
B, take by weighing the 0.0686g zinc acetate and 0.0152g L-cysteine is dissolved in the 16mL ultrapure water, add mercaptoacetic acid under magnetic agitation, regulator solution pH value equals 9, and applying argon gas is removed the dissolved oxygen DO in the solution;
C, the sodium hydrogen selenide solution 0.4mL of a operation is added in the b operation solution, reflux 6 hours, the aqueous solution of luminescence zinc selenide Nanorods.Product is accredited as a cube phase zinc selenide through X-ray powder diffraction; TEM, HRTEM Electronic Speculum testing product pattern are nanometer rods.
This luminous zinc selenide nanometer rods is expected to be used for bioanalysis, can detect chemical system, the metallic ion in living things system and the cell.
Embodiment 2:
A, 0.2056g sodium borohydride and 0.195g selenium powder are dissolved in the 10mL ultrapure water, under argon shield, react then, make weight concentration and be 2% sodium hydrogen selenide solution;
B, take by weighing the 0.0686g zinc acetate and 0.0252g L-cysteine is dissolved in the 10mL ultrapure water, add mercaptoacetic acid under magnetic agitation, regulator solution pH value equals 11, and applying argon gas is removed the dissolved oxygen DO in the solution;
C, the sodium hydrogen selenide solution 0.4mL of a operation is added in the b operation solution, reflux 4 hours, the aqueous solution of luminescence zinc selenide Nanorods.Product is accredited as a cube phase zinc selenide through X-ray powder diffraction; TEM, HRTEM Electronic Speculum testing product pattern are nanometer rods.
This luminous zinc selenide nanometer rods is used for biomarker, can mark specific tissue and the specific position in organ or the cell.
Embodiment 3:
A, 0.2056g sodium borohydride and 0.195g selenium powder are dissolved in the 10mL ultrapure water, under argon shield, react then, make weight concentration and be 1.5% sodium hydrogen selenide solution;
B, take by weighing the 0.0686g zinc acetate and 0.0200g L-cysteine is dissolved in the 130mL ultrapure water, add mercaptoacetic acid under magnetic agitation, regulator solution pH value equals 10, and applying argon gas is removed the dissolved oxygen DO in the solution;
C, the sodium hydrogen selenide solution 0.4mL of a operation is added in the b operation solution, reflux 5 hours, the aqueous solution of luminescence zinc selenide Nanorods.Product is accredited as a cube phase zinc selenide through X-ray powder diffraction; TEM, HRTEM Electronic Speculum testing product pattern are nanometer rods.
This luminous zinc selenide nanometer rods is used for cell imaging, can detect the specific ion in the cell and do respective imaging.
Embodiment 4:
With embodiment 1～3, different is to substitute mercaptoacetic acid with mercaptopropionic acid respectively.
Embodiment 5:
With embodiment 1～4, different is to substitute zinc acetate with zinc chloride, zinc nitrate respectively.
Claims (2)
1. the synthetic method of luminescence zinc selenide Nanorods is characterized in that this method carries out according to the following steps:
A, 0.2056g sodium borohydride and 0.195g selenium powder are dissolved in the 10mL ultrapure water, under argon shield, react then, make weight concentration and be 1.5% sodium hydrogen selenide solution;
B, take by weighing the 0.0686g zinc acetate and 0.0152g L-cysteine is dissolved in the 16mL ultrapure water, add mercaptoacetic acid under magnetic agitation, regulator solution pH value equals 9, and applying argon gas is removed the dissolved oxygen DO in the solution;
C, the sodium hydrogen selenide solution 0.4mL of a operation is added in the b operation solution, reflux 6 hours, the aqueous solution of luminescence zinc selenide Nanorods.
2. the purposes of the synthetic luminescence zinc selenide Nanorods of the method for claim 1 is characterized in that described luminescence zinc selenide Nanorods is used for bioanalysis detects metallic ion in the cell.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9719926B2 (en) | 2015-11-16 | 2017-08-01 | International Business Machines Corporation | Nanopillar microfluidic devices and methods of use thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424248A (en) * | 2003-01-10 | 2003-06-18 | 清华大学 | Synthesis of nano hollow balls of zinc selenide |
| CN1483665A (en) * | 2003-07-23 | 2004-03-24 | 西安交通大学 | Process for preparing zinc selenide (zn se) powder material |
| CN1687303A (en) * | 2005-04-07 | 2005-10-26 | 上海交通大学 | Microwave assistant method for quickly synthesizing quanta point of zinc selenide fluorescence |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424248A (en) * | 2003-01-10 | 2003-06-18 | 清华大学 | Synthesis of nano hollow balls of zinc selenide |
| CN1483665A (en) * | 2003-07-23 | 2004-03-24 | 西安交通大学 | Process for preparing zinc selenide (zn se) powder material |
| CN1687303A (en) * | 2005-04-07 | 2005-10-26 | 上海交通大学 | Microwave assistant method for quickly synthesizing quanta point of zinc selenide fluorescence |
Non-Patent Citations (1)
| Title |
|---|
| 张叶.Ⅱ-Ⅵ族硒化物薄膜的研究进展.《太原师范学院学报(自然科学版)》.2006,第5卷(第3期),77-79. * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9719926B2 (en) | 2015-11-16 | 2017-08-01 | International Business Machines Corporation | Nanopillar microfluidic devices and methods of use thereof |
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