CN101012054A - Method of synthesizing cadmium selenide nano stick and use thereof - Google Patents
Method of synthesizing cadmium selenide nano stick and use thereof Download PDFInfo
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- CN101012054A CN101012054A CN 200710013006 CN200710013006A CN101012054A CN 101012054 A CN101012054 A CN 101012054A CN 200710013006 CN200710013006 CN 200710013006 CN 200710013006 A CN200710013006 A CN 200710013006A CN 101012054 A CN101012054 A CN 101012054A
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Abstract
The invention discloses a synthesizing method of cadmium selenite nanometer bar, which comprises the following steps: a. dissolving sodium borohydride and selenium powder in the water according to certain rate; obtaining 1.5-2% sodium selehydride solution under inert gas; b. blending soluble salt, L-cysteine and water with rate at 100:23-44:150000-300000 evenly; adding mercaptoacetic acid or mercaptopropionic acid to stir; adjusting pH value to 10-12; removing dissolved oxygen in the solution after aerating inert gas; c. blending the sodium selehydride solution and solution in the step b; heating to reflux; obtaining the product.
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, cadmium selenide nanorod; In addition, the purposes that also relates to this cadmium selenide nanorod.
Background technology:
Since carbon nanotube 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, excellent property 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 the aqueous solution, but resulting product substantially all is granular.Recently, in the II-VI compound semiconductor nano material, have only one dimension water soluble cadmium telluride nano material to appear in the newspapers.Li Jun etc. are that part has synthesized cadmium telluride nanometer rod (J.Li, X.Hong, D.Li, K.Zhao, L.Wang in the aqueous solution with Thiovanic acid and L-halfcystine, H.Z.Wang, Z.L.Du, J.H.Li, Y.B.Bai and T.J.Li, Chem.Commun., 2004,15,1740.).Wang Dayang etc. are that part has synthesized cadmium telluride nanometer rod (H.Zhang, D.Y.Wang and H.Mohwald, Angew.Chem.Int.Ed., 2006,45,748 with various similar in the organism of the band sulfydryl of Thiovanic acid; H.Zhang, D.Y.Wang, B.Yang and H.Mohwald, J.Am.Chem.Soc., 2006,128,10171.).The present inventor has synthesized the cadmium telluride nano wire in the aqueous solution, and with it as probe in detecting cupric ion (B.Tang, J.Y.Niu, C.G.Yu, L.H Zhuo and J.C.Ge, Chem Commun., 2005,33,4184.) but the preparation research of the water-soluble semiconductor nano material of other one dimensions yet there are no report, cadmium selenide for example.
Cadmium selenide has good photoconductive property as the semi-conductor of direct band gap, is a kind of fabulous indoor temperature nucleus radiation detecting material.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 photosensor.Along with reducing of size of particles, because quantum size effect, II-VI family semiconductor nano material presents a series of and the distinct specific physique of body phase material, as photoabsorption 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 opto-electronic device of new generation.So far the report of water breakthrough dissolubility, cadmium selenide nanorod not as yet.
Summary of the invention:
One of purpose of the present invention provides a kind of simple, with low cost, the synthetic method of stable better water solubility, cadmium selenide nanorod; Two of purpose provides the purposes of this cadmium selenide nanorod.
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 protection of inert gas 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 cadmium ion: L-thioserine: water=100: 23-44: 150000-300000 weight part proportioning mixing, add Thiovanic acid or thiohydracrylic acid down in stirring again, transfer pH=10-12, filling with inert gas is removed the dissolved oxygen 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 cadmium selenide nanorod aqueous solution.
One of purpose of the present invention also can realize by following technical measures:
The described soluble salt that is dissolved with cadmium ion is selected from cadmium perchlorate, Cadmium chloride fine powder or cadmium acetate: the described reflux time is 2-4 hour.
Two of purpose of the present invention can realize by following technical measures:
The industry that described luminous cadmium selenide nanorod is used for biomarker, cell imaging, bioanalysis and solid-state electronic opto-electronic device is implemented.
The present invention at first is dissolved in sodium borohydride and selenium powder in the water according to the chemical reaction proportioning, makes mixing solutions, is prepared into sodium hydrogen selenide solution again under protection of inert gas; Be raw material with this water miscible salts solution that contains cadmium ion then, with L-thioserine and Thiovanic acid is part, regulating the pH value is 10-12, the dissolved oxygen 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 cadmium selenide nanorod.This method is that solvent has prepared luminous cadmium selenide nanorod with water, and reaction process 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 cadmium selenide nanorod 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, imaging and the solid-state electronic opto-electronic device in addition.
Description of drawings:
Fig. 1 is cadmium selenide nanorod transmission photo (TEM) and the high resolution photo (HRTEM) that the present invention prepares;
Fig. 2 is the cadmium selenide nanorod X-ray powder diffraction figure that the present invention prepares;
Fig. 3 is the time dependent absorption spectrum of cadmium selenide nanorod that the present invention prepares;
Fig. 4 is the fluorescence spectrum that the cadmium selenide nanorod 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 cadmium acetate and 0.0152g L-thioserine is dissolved in the 20mL ultrapure water, add Thiovanic acid under magnetic agitation, regulator solution pH value equals 12, and applying argon gas is removed the dissolved oxygen 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 luminous cadmium selenide nanorod.Product is accredited as a cube phase cadmium selenide through X-ray powder diffraction; TEM, HRTEM Electronic Speculum testing product pattern are nanometer rod.
This luminous cadmium selenide nanorod is used for bioanalysis, can detect chemical system, the metal 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 cadmium acetate and 0.0225g L-thioserine is dissolved in the 10mL ultrapure water, add Thiovanic acid under magnetic agitation, regulator solution pH value equals 10, and applying argon gas is removed the dissolved oxygen in the solution;
C, the sodium hydrogen selenide solution 0.4mL of a operation is added in the b operation solution, reflux 2 hours, the aqueous solution of luminous cadmium selenide nanorod.Product is accredited as a cube phase cadmium selenide through X-ray powder diffraction; TEM, HRTEM Electronic Speculum testing product pattern are nanometer rod.
This luminous cadmium selenide nanorod is used for biomarker, specific position in can mark specific tissue and 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 1.7% sodium hydrogen selenide solution;
B, take by weighing the 0.0686g cadmium acetate and 0.0195g L-thioserine is dissolved in the 15mL ultrapure water, add Thiovanic acid under magnetic agitation, regulator solution pH value equals 11, and applying argon gas is removed the dissolved oxygen in the solution;
C, the sodium hydrogen selenide solution 0.4mL of a operation is added in the b operation solution, reflux 3 hours, the aqueous solution of luminous cadmium selenide nanorod.Product is accredited as a cube phase cadmium selenide through X-ray powder diffraction; TEM, HRTEM Electronic Speculum testing product pattern are nanometer rod.
This luminous cadmium selenide nanorod is used for cell imaging, can detect the specific ion in the cell and do respective imaging.
Embodiment 4:
Substitute Thiovanic acid with thiohydracrylic acid, other are respectively with embodiment 1,2,3.
Embodiment 5:
Substitute cadmium acetate with cadmium perchlorate, Cadmium chloride fine powder respectively, other are respectively with embodiment 1,2,3,4.
Claims (4)
1, the synthetic method of cadmium selenide nanorod is characterized in that this method carries 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 protection of inert gas 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 cadmium ion: L-thioserine: water=100: 23-44: 150000-300000 weight part proportioning mixing, add Thiovanic acid or thiohydracrylic acid down in stirring again, transfer pH=10-12, filling with inert gas is removed the dissolved oxygen 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 cadmium selenide nanorod aqueous solution.
2,, it is characterized in that the described soluble salt that is dissolved with cadmium ion is selected from cadmium perchlorate, Cadmium chloride fine powder or cadmium acetate according to the synthetic method of the described cadmium selenide nanorod of claim 1.
3, the synthetic method of cadmium selenide nanorod according to claim 1 is characterized in that the described reflux time is 2-4 hour.
4, the purposes of the method synthetic cadmium selenide nanorod of claim 1 is characterized in that described luminous cadmium selenide nanorod is used for the industry enforcement of biomarker, cell imaging, bioanalysis and solid-state electronic opto-electronic device.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071453A (en) * | 2010-12-14 | 2011-05-25 | 吉林大学 | Method for preparing high-quality aqueous phase semiconductor nanocrystals by one pot method at room temperature |
| CN102689881A (en) * | 2011-03-22 | 2012-09-26 | 国家纳米科学中心 | Inorganic semiconductor super nanoparticle and its preparation method |
| CN102795605A (en) * | 2012-08-06 | 2012-11-28 | 西北工业大学 | Method for preparing nanometer material lead selenide by aqueous phase method |
| CN105218994A (en) * | 2015-08-31 | 2016-01-06 | 江汉大学 | A kind of preparation method of quanta polymer display material |
| CN105618086A (en) * | 2015-12-17 | 2016-06-01 | 江苏大学 | Preparation and application of vesicular CdSe nano-semiconductor photocatalyst |
| CN106976847A (en) * | 2017-04-13 | 2017-07-25 | 中国石油大学(华东) | A kind of two selenizing ferrum nano materials and its synthetic method and application |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1208238C (en) * | 2003-09-17 | 2005-06-29 | 中国科学院长春应用化学研究所 | Manufacturing method of cadmium selenide and cadmium telluride nanometer rod |
| CN1234601C (en) * | 2004-04-29 | 2006-01-04 | 上海交通大学 | Aqueous phase synthesis for high quality cadmium selenide quantum dots in temperature controlled microwave reactor |
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2007
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071453A (en) * | 2010-12-14 | 2011-05-25 | 吉林大学 | Method for preparing high-quality aqueous phase semiconductor nanocrystals by one pot method at room temperature |
| CN102071453B (en) * | 2010-12-14 | 2012-05-02 | 吉林大学 | Method for preparing high-quality aqueous phase semiconductor nanocrystals by one pot method at room temperature |
| CN102689881A (en) * | 2011-03-22 | 2012-09-26 | 国家纳米科学中心 | Inorganic semiconductor super nanoparticle and its preparation method |
| CN102689881B (en) * | 2011-03-22 | 2016-03-02 | 国家纳米科学中心 | Super nanoparticle of a kind of inorganic semiconductor and preparation method thereof |
| CN102795605A (en) * | 2012-08-06 | 2012-11-28 | 西北工业大学 | Method for preparing nanometer material lead selenide by aqueous phase method |
| CN105218994A (en) * | 2015-08-31 | 2016-01-06 | 江汉大学 | A kind of preparation method of quanta polymer display material |
| CN105618086A (en) * | 2015-12-17 | 2016-06-01 | 江苏大学 | Preparation and application of vesicular CdSe nano-semiconductor photocatalyst |
| CN105618086B (en) * | 2015-12-17 | 2018-06-26 | 江苏大学 | A kind of preparation and its application of vesica shape CdSe Nano semiconductor photochemical catalysts |
| CN106976847A (en) * | 2017-04-13 | 2017-07-25 | 中国石油大学(华东) | A kind of two selenizing ferrum nano materials and its synthetic method and application |
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| CN100509617C (en) | 2009-07-08 |
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