CN100509635C - Method for synthesizing water-soluble Nano CdllgTe stick, and usage of Nano stick - Google Patents
Method for synthesizing water-soluble Nano CdllgTe stick, and usage of Nano stick Download PDFInfo
- Publication number
- CN100509635C CN100509635C CNB2007100132123A CN200710013212A CN100509635C CN 100509635 C CN100509635 C CN 100509635C CN B2007100132123 A CNB2007100132123 A CN B2007100132123A CN 200710013212 A CN200710013212 A CN 200710013212A CN 100509635 C CN100509635 C CN 100509635C
- Authority
- CN
- China
- Prior art keywords
- solution
- cadmium
- cys
- soluble
- tga
- 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.)
- Expired - Fee Related
Links
Images
Abstract
This invention provides a method for synthesizing water-soluble CdHgTe nanorods, and their applications. The method comprises: (1) preparing sodium hydrotelluride solution from sodium borohydride and tellurium powder at stoichiometric ratio under the protection of inert gas; (2) adding thioglycolic acid into a solution containing soluble cadmium salt and L-cysteine under magnetically stirring to obtain Cd-Cys-TGA solution; (3) adjusting the Ph value of to 10-11 with alkali solution, and introducing inert gas to remove dissolved oxygen; (4) mixing sodium hydrotelluride solution obtained in step 1 and Cd-Cys-TGA solution obtained in step 3 at stoichiometric ratio, and heating for refluxing to obtain aqueous solution of cadmium telluride nanorods; (5) adjusting the pH value to 10-11 with alkali solution, adding soluble bivalent mercury salt solution at a mercury/cadmium telluride wt. ratio of 1:(1.5-6) into the aqueous solution of cadmium telluride nanorods, mixing uniformly, and reacting at room temperature to obtain the product.
Description
Technical field:
The present invention relates to field of inorganic chemical engineering, relate in particular to that one dimension is water-soluble, the synthetic method of the CdHgTe nano composite material of emission wavelength tunable; The invention still further relates to the purposes of this water-soluble Nano CdllgTe stick.
Background technology:
One dimension semiconductor nano material (nano wire, nanometer rod and nanotube) is owing to it has very high application potential to become the focus of nanosecond science and technology research in technical field.So far, various 1-dimention nano semiconductor materials synthetic mainly is to be limited in the organic phase or to utilize solvent thermal process.Water is synthetic, and to have method easy, low consumption, and advantages such as the controlled and biocompatibility of surface properties become current semiconductor nano material synthetic focus, but have zero-dimension structural usually at aqueous phase synthetic semiconductor nano material at present.Recently, people such as Nicholas A.Kotov at first utilizes dipole-dipolar interaction to synthesize water-soluble CdTe nano wire [Tang, Z. at aqueous phase; Kotov, N.A.; Giersig, M.Science 2002,297, and 237]; People such as Li Jun and Dayang Wang utilize the coordination of part to synthesize one dimension CdTe nano material [Li, J.; Li, J.H.; Bai, Y.B.; Li, T.J.Chem.Commun.2004,1740; Zhang, H.; Wang, D.Y.;
H.Angew.Chem.Int.Ed.2006,45,748].The red shift with the increase of mercury content near infrared region and wavelength of CdHgTe composite nano materials emission wavelength, its this character make it that widespread use [Rogal ski, A.Opt.Eng.1994,33,1395 arranged aspect optical electron device and the biomarker; Tsay, J.M.; Pflughoefft, M.; Bentolila, L.A.; Weiss, S.J.Am.Chem.Soc.2004,126,1926].People such as Harrison have synthesized zero dimension CdHgTe nano material [Harrison, M.T. at aqueous phase; Kershaw, S.V.; Burt, M.G.; Eychmuller, A.; Weller, H.; Rogach, A.L.Mater.Sci.Eng., B 2000,69, and 355].Do not find at present the preparation method of one dimension water-soluble Nano CdllgTe stick as yet.
Summary of the invention:
It is simple that one of purpose of the present invention provides a kind of technology, the method in aqueous phase synthesizing water-solubility CdHgTe nanometer rod that cost is low; Two of purpose provides the purposes of this water-soluble Nano CdllgTe stick.
One of purpose of the present invention can realize by following technical measures:
A, get sodium borohydride and tellurium powder, under protection of inert gas, make sodium hydrogen telluride solution according to the solution of chemical reaction proportioning;
B, in the L-thioserine solution of the soluble salt that is dissolved with cadmium ion of 1 weight part and 0.2-0.5 weight part, under magnetic agitation, add the Thiovanic acid of 0.4-0.6 weight part, Cd-Cys-TGA solution;
C, regulate Cd-Cys-TGA solution to pH=10～11 with alkaline solution then, filling with inert gas is removed the dissolved oxygen in the Cd-Cys-TGA solution;
D, the sodium hydrogen telluride solution of a operation Cd-Cys-TGA solution with the preparation of c operation is mixed reflux, the aqueous solution that must the cadmium telluride nanometer rod according to the chemical reaction proportioning;
E, transfer the cadmium telluride nanometer rod with alkaline solution again the aqueous solution to pH=10～11, then under agitation, add the soluble salt solution that is dissolved with dimercurion according to divalence mercury: cadmium telluride=1:1.5～6 weight part proportionings, behind the mixing, react under the room temperature, product.
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, cadmium nitrate, cadmium acetate; Described alkaline solution is selected from the aqueous solution of sodium hydroxide, potassium hydroxide, ammonia; The soluble salt solution of described dimercurion is selected from the aqueous solution of mercuric acetate, mercuric perchlorate, Mercury pernitrate, mercury chloride; The described reaction times is 15～20 days; Described return time is 2-5 hour.
Two of purpose of the present invention can realize by following technical measures:
The water-soluble Nano CdllgTe stick that makes is used in the industry in optical electron device and bioanalysis field.
The present invention as template, by adding the mercury ion of different amounts, realizes emission wavelength tunable with the water miscible CdTe nanometer rod of synthetic, has prepared CdHgTe nanometer rod water-soluble, emission wavelength tunable.Owing to add the mercury ion of different amounts CdHgTe composite nano materials optical property is produced different influences, it is transmitted near infrared region, therefore, the CdHgTe nanometer rod of method preparation of the present invention is implemented and will be used widely in the industry in optical electron device and bioanalysis field.Preparation technology of the present invention is simple, and cost is low, and whole technological process is carried out at aqueous phase, and working condition is easy to control.
Description of drawings:
Fig. 1 is transmission electron microscope (TEM) figure of the bar-shaped CdHgTe nano material for preparing of the present invention;
Fig. 2 is powdery diffractometry (XRD) figure of the bar-shaped CdHgTe nano material for preparing of the present invention;
Fig. 3 is electronic spectrum (EDS) figure of the bar-shaped CdHgTe nano material for preparing of the present invention;
Fig. 4 is high-resolution electron microscopy (HRTEM) figure of the bar-shaped CdHgTe nano material for preparing of the present invention;
Fig. 5 is the fluorescence spectrum and the abosrption spectrogram of the bar-shaped CdHgTe nano material for preparing of the present invention.
Embodiment:
Embodiment 1:
A, according to the chemical reaction proportioning, get the sodium borohydride of 0.2056 weight part and the tellurium powder of 0.195 weight part and join in the ultrapure water of 5 weight parts, the dissolving, under argon shield, make sodium hydrogen telluride solution;
B, in containing the L-thioserine solution of 1 weight part cadmium perchlorate and 0.2 weight part, under magnetic agitation, add the Thiovanic acid of 0.6 weight part, Cd-Cys-TGA solution;
C, regulate Cd-Cys-TGA solution to pH=10 with aqueous sodium hydroxide solution then, applying argon gas is removed the dissolved oxygen in the Cd-Cys-TGA solution;
D, the sodium hydrogen telluride solution of a operation Cd-Cys-TGA solution with the preparation of c operation is mixed according to the chemical reaction proportioning, reflux 5 hours, the aqueous solution that must the cadmium telluride nanometer rod, product is accredited as cadmium telluride through X-ray powder diffraction; TEM Electronic Speculum testing product pattern is a nanometer rod;
E, transfer the aqueous solution of cadmium telluride nanometer rod to pH=11 with aqueous sodium hydroxide solution again, then under vigorous stirring, according to divalence mercury: cadmium telluride=1:1.5 weight part proportioning adds the aqueous solution that is dissolved with mercuric acetate, behind the mixing, reaction is 20 days under the room temperature, gets product, and solution colour is by the orange red scarlet that becomes, be defined as CdHgTe through X-ray powder diffraction and power spectrum, TEM testing product pattern is bar-shaped.
Embodiment 2:
A, according to the chemical reaction proportioning, get the sodium borohydride of 0.2056 weight part and the tellurium powder of 0.195 weight part and join in the ultrapure water of 5 weight parts, the dissolving, under argon shield, make sodium hydrogen telluride solution;
B, in the L-that contains 1 weight part cadmium perchlorate and 0.5 weight part dredges basic L-Ala solution, under magnetic agitation, add the Thiovanic acid of 0.4 weight part, Cd-Cys-TGA solution;
C, regulate Cd-Cys-TGA solution to pH=11 with aqueous sodium hydroxide solution then, applying argon gas is removed the dissolved oxygen in the Cd-Cys-TGA solution;
D, the sodium hydrogen telluride solution of a operation Cd-Cys-TGA solution with the preparation of c operation is mixed according to the chemical reaction proportioning, reflux 2 hours, the aqueous solution that must the cadmium telluride nanometer rod, product is accredited as cadmium telluride through X-ray powder diffraction; TEM Electronic Speculum testing product pattern is a nanometer rod;
E, transfer the aqueous solution of cadmium telluride nanometer rod to pH=10 with aqueous sodium hydroxide solution again, then under vigorous stirring, according to divalence mercury: cadmium telluride=1:6 weight part proportioning adds the aqueous solution that is dissolved with mercuric acetate, behind the mixing, reaction is 15 days under the room temperature, gets product, and solution colour is by the orange red grass green that becomes, be defined as CdHgTe through X-ray powder diffraction and power spectrum, TEM testing product pattern is bar-shaped.
Embodiment 3:
A, according to the chemical reaction proportioning, get the sodium borohydride of 0.2056 weight part and the tellurium powder of 0.195 weight part and join in the ultrapure water of 5 weight parts, the dissolving, under argon shield, make sodium hydrogen telluride solution;
B, in containing the L-thioserine solution of 1 weight part cadmium perchlorate and 0.3 weight part, under magnetic agitation, add the Thiovanic acid of 0.5 weight part, Cd-Cys-T6A solution;
C, regulate Cd-Cys-TGA solution to pH=10.5 with aqueous sodium hydroxide solution then, applying argon gas is removed the dissolved oxygen in the Cd-Cys-TGA solution;
D, the sodium hydrogen telluride solution of a operation Cd-Cys-TGA solution with the preparation of c operation is mixed according to the chemical reaction proportioning, reflux 3 hours, the aqueous solution that must the cadmium telluride nanometer rod, product is accredited as cadmium telluride through X-ray powder diffraction; TEM Electronic Speculum testing product pattern is a nanometer rod;
E, transfer the aqueous solution of cadmium telluride nanometer rod to pH=10.5 with aqueous sodium hydroxide solution again, then under vigorous stirring, according to divalence mercury: cadmium telluride=1:4 weight part proportioning adds the aqueous solution that is dissolved with mercuric acetate, behind the mixing, reaction is 17 days under the room temperature, gets product, and solution colour is by the orange red brown that becomes, be defined as CdHgTe through X-ray powder diffraction and power spectrum, TEM testing product pattern is bar-shaped.
Embodiment 4:
Replace cadmium perchlorate with Cadmium chloride fine powder, other are respectively with embodiment 1,2,3.
Embodiment 5:
Replace cadmium perchlorate with cadmium nitrate, other are respectively with embodiment 1,2,3.
Embodiment 6:
Replace cadmium perchlorate with cadmium acetate, other are respectively with embodiment 1,2,3.
Embodiment 7:
Replace aqueous sodium hydroxide solution with potassium hydroxide aqueous solution, other are respectively with embodiment 1,2,3,4,5,6.
Embodiment 8:
The aqueous solution with ammonia replaces aqueous sodium hydroxide solution, and other are respectively with embodiment 1,2,3,4,5,6.
Embodiment 9:
With the aqueous solution of the aqueous solution substituted acetic acid mercury of mercuric perchlorate, other are respectively with embodiment 1,2,3,4,5,6,7,8.
Embodiment 10:
With the aqueous solution of the aqueous solution substituted acetic acid mercury of Mercury pernitrate, other are respectively with embodiment 1,2,3,4,5,6,7,8.
Embodiment 11:
With the aqueous solution of the aqueous solution substituted acetic acid mercury of mercury chloride, other are respectively with embodiment 1,2,3,4,5,6,7,8.
Claims (4)
1, the synthetic method of water-soluble Nano CdllgTe stick is characterized in that:
A, get sodium borohydride and the tellurium powder is dissolved in the pure water according to the chemical reaction proportioning, wiring solution-forming makes sodium hydrogen telluride solution under protection of inert gas;
B, in containing the L-thioserine solution that 1 weight part is dissolved with the soluble salt of cadmium ion and 0.2-0.5 weight part, under magnetic agitation, add the Thiovanic acid of 0.4-0.6 weight part, Cd-Cys-TGA solution;
C, regulate Cd-Cys-TGA solution to pH=10～11 with alkaline solution then, filling with inert gas is removed the dissolved oxygen in the Cd-Cys-TGA solution;
D, the sodium hydrogen telluride solution of a operation Cd-Cys-TGA solution with the preparation of c operation is mixed according to the chemical reaction proportioning, reflux 2-5 hour, the aqueous solution that must the cadmium telluride nanometer rod;
E, transfer the aqueous solution of cadmium telluride nanometer rod to pH=10～11 with alkaline solution again, then under agitation, add the soluble salt solution that is dissolved with dimercurion according to divalence mercury: cadmium telluride=1:1.5～6 weight part proportionings, behind the mixing, reacted under the room temperature 15～20 days, and got product.
2, the synthetic method of water-soluble Nano CdllgTe stick according to claim 1 is characterized in that the described soluble salt that is dissolved with cadmium ion is selected from cadmium perchlorate, Cadmium chloride fine powder, cadmium nitrate or cadmium acetate.
3, the synthetic method of water-soluble Nano CdllgTe stick according to claim 1 is characterized in that described alkaline solution is selected from the aqueous solution of sodium hydroxide, potassium hydroxide or ammonia.
4, the synthetic method of water-soluble Nano CdllgTe stick according to claim 1 is characterized in that the soluble salt solution of described dimercurion is selected from the aqueous solution of mercuric acetate, mercuric perchlorate, Mercury pernitrate or mercury chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100132123A CN100509635C (en) | 2007-01-15 | 2007-01-15 | Method for synthesizing water-soluble Nano CdllgTe stick, and usage of Nano stick |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100132123A CN100509635C (en) | 2007-01-15 | 2007-01-15 | Method for synthesizing water-soluble Nano CdllgTe stick, and usage of Nano stick |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101003384A CN101003384A (en) | 2007-07-25 |
| CN100509635C true CN100509635C (en) | 2009-07-08 |
Family
ID=38702821
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100132123A Expired - Fee Related CN100509635C (en) | 2007-01-15 | 2007-01-15 | Method for synthesizing water-soluble Nano CdllgTe stick, and usage of Nano stick |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100509635C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311383B (en) * | 2008-03-11 | 2012-04-18 | 河南大学 | Semiconductor nanocrystalline and method for preparing same |
| CN105218994B (en) * | 2015-08-31 | 2017-11-14 | 江汉大学 | A kind of preparation method of quanta polymer display material |
| CN108204951A (en) * | 2016-12-19 | 2018-06-26 | 深圳大学 | A kind of photoacoustic imaging probe and its preparation method and application |
| CN111977617B (en) * | 2019-05-22 | 2022-05-17 | 北京理工大学 | Method for preparing cadmium-based alloy nano material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0040939A1 (en) * | 1980-05-27 | 1981-12-02 | The Secretary of State for Defence in Her Britannic Majesty's Government of the United Kingdom of Great Britain and | Manufacture of cadmium mercury telluride |
| US5602414A (en) * | 1993-06-18 | 1997-02-11 | Mitsubishi Denki Kabushiki Kaisha | Infrared detector having active regions and isolating regions formed of CdHgTe |
| RU2244366C1 (en) * | 2003-12-09 | 2005-01-10 | Федеральное государственное унитарное предприятие "Альфа" | PHOTORESISTOR BUILT AROUND HETEROEPITAXIAL STRUCTURE CdHgTe (ALTERNATIVES) |
-
2007
- 2007-01-15 CN CNB2007100132123A patent/CN100509635C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0040939A1 (en) * | 1980-05-27 | 1981-12-02 | The Secretary of State for Defence in Her Britannic Majesty's Government of the United Kingdom of Great Britain and | Manufacture of cadmium mercury telluride |
| US5602414A (en) * | 1993-06-18 | 1997-02-11 | Mitsubishi Denki Kabushiki Kaisha | Infrared detector having active regions and isolating regions formed of CdHgTe |
| RU2244366C1 (en) * | 2003-12-09 | 2005-01-10 | Федеральное государственное унитарное предприятие "Альфа" | PHOTORESISTOR BUILT AROUND HETEROEPITAXIAL STRUCTURE CdHgTe (ALTERNATIVES) |
Non-Patent Citations (2)
| Title |
|---|
| 无机镉化合物的开发与应用. 傅新华，林鸿权.湖南化工，第25卷第2期. 1995 |
| 无机镉化合物的开发与应用. 傅新华，林鸿权.湖南化工，第25卷第2期. 1995 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101003384A (en) | 2007-07-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Gong et al. | Highly efficient Sb3+ emitters in 0D cesium indium chloride nanocrystals with switchable photoluminescence through water-triggered structural transformation | |
| Sczancoski et al. | Morphology and blue photoluminescence emission of PbMoO4 processed in conventional hydrothermal | |
| Fang et al. | Rapid synthesis and mechanochemical reactions of cesium copper halides for convenient chromaticity tuning and efficient white light emission | |
| Ding et al. | Sodium doping controlled synthesis of monodisperse lanthanide oxysulfide ultrathin nanoplates guided by density functional calculations | |
| Ye et al. | Controllable emission bands and morphologies of high-quality CsPbX 3 perovskite nanocrystals prepared in octane | |
| Ding et al. | Chemoaffinity-mediated synthesis of NaRES2-based nanocrystals as versatile nano-building blocks and durable nano-pigments | |
| Taxak et al. | Tartaric acid-assisted sol–gel synthesis of Y2O3: Eu3+ nanoparticles | |
| Zhou et al. | Phase-selective synthesis and formation mechanism of CZTS nanocrystals | |
| CN100509635C (en) | Method for synthesizing water-soluble Nano CdllgTe stick, and usage of Nano stick | |
| Wang et al. | Morphology-controlled synthesis of CdWO4 nanorods and nanoparticles via a molten salt method | |
| Xing et al. | Confined growth of quantum dots in silica spheres by ion exchange of “Trapped NH4+” for white-light emission | |
| Yin et al. | Effect of calcinations temperature on the luminescence intensity and fluorescent lifetime of Tb3+-doped hydroxyapatite (Tb-HA) nanocrystallines | |
| Kamble et al. | Monodispersed wurtzite Cu 2 SnS 3 nanocrystals by phosphine and oleylamine free facile heat-up technique | |
| CN109093124A (en) | A kind of method that high-energy ball milling reduction method prepares metal nano material | |
| CN100509617C (en) | Method of synthesizing cadmium selenide nano stick | |
| Huang et al. | Crystalline nanowires of Ln2O2S, Ln2O2S2, LnS2 (Ln= La, Nd), and La2O2S: Eu3+. conversions via the boron-sulfur method that preserve shape | |
| Zhu et al. | Facile synthesis and photoluminescence of europium ion doped LaF3 nanodisks | |
| De Azevedo et al. | A new and straightforward synthesis route for preparing Cds quantum Dots | |
| Fu et al. | Photoluminescence of Dy3+ ions in yttrium-stabilized zirconium oxide with different phases | |
| Liu et al. | Recent research progress of luminescent materials with apatite structure: A review | |
| Xu et al. | Synthesis and optical properties of Eu3+ ion-doped La2O2S2 via a solid state reaction method using La2O2SO4 as a raw material | |
| Stephen et al. | Effect of Yb3+ substitution on the structural and optical properties of Ba1-xYbxWO4 nanoparticles-NIR luminescence emissions for optical communication and bioanalyses | |
| Zhang et al. | Synthesis by organic molten salt method and characterization of chalcopyrite AgInS2 nanorods | |
| CN110627125B (en) | Method for synthesizing manganese sulfide and lead sulfide nanorod with core-shell structure | |
| CN103145105B (en) | Preparation method of metal selenide nanocrystals |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090708 Termination date: 20100222 |