CN1524782A - Manufacturing method of cadmium selenide and cadmium telluride nanometer rod - Google Patents
Manufacturing method of cadmium selenide and cadmium telluride nanometer rod Download PDFInfo
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- CN1524782A CN1524782A CNA03127160XA CN03127160A CN1524782A CN 1524782 A CN1524782 A CN 1524782A CN A03127160X A CNA03127160X A CN A03127160XA CN 03127160 A CN03127160 A CN 03127160A CN 1524782 A CN1524782 A CN 1524782A
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Abstract
The invention relates to the process for preparing cadmium selenide and cadmium telluride nano sticks , wherein cadmium oxide is used as the monomer, and tetradecanoic acid is used as ligand, by controlling the nucleation and growth procedure of the nanocrystalline, and injecting selenium or tellurium precursor solution into the cadmium precursor solution at the temperature of 190 deg. C to 230 deg. C, the nano sticks can be prepared at the temperature of 160-180 deg. C. The advantages of the cadmium selenide and cadmium telluride nano sticks are high yield, narrow dimension distribution, uniform shapes and fine repeatability for experiment.
Description
Technical field
The invention belongs to the preparation method of cadmium selenide and cadmium telluride nanometer rod.
Background technology
The nano material particularly research of nano semiconductor material is acknowledged as 21st century one of the most promising subject.And will help understanding crystalline nucleation and growth on atom or molecular level to the preparation and the research of one dimension or accurate 1-dimention nano semiconductor material, help further to explore the relation between quantum size effect and the unique physicochemical property, to being implemented in the future design on the molecular level, making microelectronic device and have important directive significance.As the member in the semiconductor material, have character such as excellent optics, magnetics, electricity owing to II-VI family material (as cadmium selenide, cadmium telluride, Cadmium Sulfide etc.) and be widely used in the nano-device, therefore how to prepare effectively and the II-VI family nano material of control different shapes and size is the problem of a lot of in the last few years researchists' explorations.
The method for preparing II-VI family nano material has a variety of, as the organic method of metal, template, hydrothermal method, gas phase-liquid phase-solid phase method, reverse microemulsion process, solvent heating method etc., but wherein the most frequently used be the metal methodology of organic synthesis.In the early 1990s, it is monomer that people such as Murray have been developed with dimethyl cadmium and selenium powder, with trioctylphosphine oxide/trioctylphosphine phosphorus is the organic method of metal of tensio-active agent, has synthesized CdSe nano-particle and nanometer rod under anhydrous and oxygen-free and hot conditions (T=300 ℃).Subsequently, Peng laughs at the firm people of grade and has further improved this method, having adopted toxicity and dangerous little Cadmium oxide is reaction monomers, and part adopts n-hexyl phosphoric acid or tetradecyl phosphoric acid and trioctylphosphine oxide synergy, the cadmium selenide of different shapes and size and cadmium telluride nanocrystalline (1. Murray, C.B. have been synthesized; Norris, D.J.; Bawend, M.G.J Am Chem Soc 1993,115,8706; 2. Peng, X.G.; Manna, L.; Yang, W.D.; Wickham, J.; Scher, E.; Kadavanich, A.; Alivisatos, A.P.Nature2000,407,981; 3. Manna, L.; Scher, E.C.; Alivisatos, A.P.J Am ChemSoc 2000,122,12700; 4. Peng, Z.A.; Peng, X.G.J Am Chem Soc2001,123,1389).But the metal methodology of organic synthesis need react under the anhydrous condition of anaerobic, and the reaction conditions requirement is harsh, and is dangerous high, big and difficult acquisition of reaction monomers toxicity.Peng laughs at and just waits the people to improve on this basis, has adopted Cadmium oxide as monomer, has reduced the danger and the toxicity of reaction, but the phosphoric acid class part that adopts costs an arm and a leg, and reaction needs at high temperature that (T=300-360 ℃) carries out, and is unfavorable for suitability for industrialized production.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of cadmium selenide and cadmium telluride nanometer rod.
Because the boiling point of part TETRADECONIC ACID is 250 ℃, so nucleation temperature is controlled at 190-230 ℃, growth temperature is between 160-180.Adopt the mode of injection to carry out nucleation,, synthesized the cadmium selenide and the cadmium telluride nanometer rod of output height and distribution of sizes homogeneous by controlling nanocrystalline nucleation and process of growth.
The monomer that adopts among the present invention is: Cadmium oxide CdO and selenium powder Se or Cadmium oxide CdO and tellurium powder Te; Part is: TETRADECONIC ACID (MA); Tensio-active agent is: trioctylphosphine oxide (TOPO); Solvent is: tributyl phosphorus (TBP) or trioctylphosphine phosphorus (TOP).
Preparation process is as follows:
(2) preparation of cadmium selenide nanorod
The weight ratio of monomer Cadmium oxide and selenium powder is CdO: Se=2: 5～5: 1, selenium powder is dissolved in is mixed with the selenium precursor solution in the tributyl phosphorus, the weight ratio of selenium powder and solvent tributyl phosphorus is Se: TBP=6: 5～4: 1, the weight ratio of Cadmium oxide and TETRADECONIC ACID is CdO: MA=1: 5～3: 5, the weight ratio of part TETRADECONIC ACID and tensio-active agent trioctylphosphine oxide is MA: TOPO=1: 5～1: 2, earlier with load weighted Cadmium oxide, TETRADECONIC ACID and trioctylphosphine oxide place reaction flask, be heated to 190 ℃～230 ℃, begin to stir after the thing fusing to be mixed, inject the selenium precursor solution then, react cooling after 2～5 minutes, growth temperature is 160～180 ℃, react stopped reaction after 8～16 hours, treat to wash with toluene and methyl alcohol after the solution cooling, centrifugal, drying, the nanometer rod diameter that makes is 3～15nm, length-to-diameter ratio is 2～10;
(2) preparation of cadmium telluride nanometer rod
The weight ratio of monomer Cadmium oxide and tellurium powder is CdO: Te=1: 4～3: 1, the tellurium powder is dissolved in is mixed with the tellurium precursor solution in the trioctylphosphine phosphorus, the weight ratio of tellurium powder and trioctylphosphine phosphorus is Te: TOP=1: 30～1: 10, the weight ratio of Cadmium oxide and TETRADECONIC ACID is CdO: MA=1: 10～3: 10, the weight ratio of part TETRADECONIC ACID and tensio-active agent trioctylphosphine oxide is MA: TOPO=1: 20～1: 5, earlier with load weighted Cadmium oxide, TETRADECONIC ACID and trioctylphosphine oxide place reaction flask, be heated to 190 ℃～230 ℃, begin to stir after the thing fusing to be mixed, inject the tellurium precursor solution for preparing then, react cooling after 2～5 minutes, growth temperature is 160～180 ℃, stopped reaction after reacting 8～16 hours under this temperature, treat to wash with toluene and methyl alcohol after the solution cooling, centrifugal, drying, the cadmium telluride nanometer rod diameter that makes is 3～10nm, length-to-diameter ratio is 2～8.
Synthetic cadmium selenide of the present invention and cadmium telluride nanometer rod productive rate height, narrow size distribution, shape is regular and repeatability experiment is strong.Experiment condition gentleness of the present invention, preparation cost is cheap, and synthetic route is simple, and environmental pollution is little, more helps following large-scale industrial production and theoretic research.Synthetic cadmium selenide and cadmium telluride nanometer rod can be used as substrate material and are prepared into nano-device, at optoelectronic areas and biosensor etc. extraordinary application prospect are arranged all.
Embodiment
Embodiment 1:
The preparation of cadmium selenide nanorod
Take by weighing the 1.60g selenium powder earlier, dissolve in the 0.4g tributyl phosphorus and make the selenium precursor solution.Take by weighing the 0.625g Cadmium oxide then, 3.13g TETRADECONIC ACID and 6.2g trioctylphosphine oxide place reaction flask, are heated to 230 ℃ under continuously stirring, treat the transparent back injection of solution selenium precursor solution, after 2 minutes, cool the temperature to 180 ℃, stopped reaction after 8 hours treats that solution cooling back adds toluene and methyl alcohol, wash, centrifugal, drying gets the cadmium selenide nanorod diameter range at 3～7nm, and length-to-diameter ratio is 2～4.
Embodiment 2:
The preparation of cadmium selenide nanorod
Take by weighing the 0.16g selenium powder earlier, dissolve in the 0.06g tributyl phosphorus and make the selenium precursor solution.Take by weighing the 0.82g Cadmium oxide then, 2.1g TETRADECONIC ACID and 10.0g trioctylphosphine oxide place reaction flask, are heated to 210 ℃ under continuously stirring, treat the selenium precursor solution that solution transparent back injection prepares in advance, after 3 minutes, cool the temperature to 170 ℃, stopped reaction after 16 hours treats that solution cooling back adds toluene and methyl alcohol, wash, centrifugal, drying, getting the cadmium selenide nanorod diameter is 6～12nm, length-to-diameter ratio is 4～7.
Embodiment 3:
The preparation of cadmium selenide nanorod
Take by weighing the 0.25g selenium powder earlier, dissolve in the 0.20g tributyl phosphorus and make the selenium precursor solution.Take by weighing the 0.64g Cadmium oxide then, 1.10g TETRADECONIC ACID and 3.20g trioctylphosphine oxide place reaction flask, are heated to 190 ℃ under continuously stirring, treat the selenium precursor solution that solution transparent back injection prepares, after 5 minutes, cool the temperature to 160 ℃, stopped reaction after 12 hours treats that solution cooling back adds toluene and methyl alcohol, wash, centrifugal, drying, getting the cadmium selenide nanorod diameter is 8～15nm, length-to-diameter ratio is 6～10.
Embodiment 4:
The preparation of cadmium selenide nanorod
Take by weighing the 0.20g selenium powder earlier, dissolve in the 0.50g tributyl phosphorus and make the selenium precursor solution.Take by weighing the 1.02g Cadmium oxide then, 1.60g TETRADECONIC ACID and 3.30g trioctylphosphine oxide place reaction flask, are heated to 210 ℃ under continuously stirring, treat the selenium precursor solution that solution transparent back injection prepares, after 5 minutes, cool the temperature to 160 ℃, stopped reaction after 12 hours treats that solution cooling back adds toluene and methyl alcohol, wash, centrifugal, drying, getting the cadmium selenide nanorod diameter is 3～7nm, length-to-diameter ratio is 4～6.
Embodiment 5:
The preparation of cadmium telluride nanometer rod
Take by weighing 2.20g tellurium powder earlier, dissolve in the 22.1g trioctylphosphine phosphorus and make the tellurium precursor solution.Take by weighing the 0.54g Cadmium oxide then, 2.75g TETRADECONIC ACID and 13.0g trioctylphosphine oxide place reaction flask, are heated to 230 ℃ under continuously stirring, treat the tellurium precursor solution that solution transparent back injection prepares, after 2 minutes, cool the temperature to 180 ℃, stopped reaction after 8 hours treats that solution cooling back adds toluene and methyl alcohol, wash, centrifugal, drying, getting cadmium telluride nanometer rod diameter is 3～6nm, length-to-diameter ratio is 2～4.
Embodiment 6:
The preparation of cadmium telluride nanometer rod
Take by weighing 0.25g tellurium powder earlier, dissolve in the 7.50g trioctylphosphine phosphorus and make the tellurium precursor solution.Take by weighing the 0.76g Cadmium oxide then, 3.8g TETRADECONIC ACID and 29.0g trioctylphosphine oxide place reaction flask, are heated to 190 ℃ under continuously stirring, treat the tellurium precursor solution that solution transparent back injection prepares, after 5 minutes, cool the temperature to 160 ℃, stopped reaction after 16 hours treats that solution cooling back adds toluene and methyl alcohol, wash, centrifugal, drying, getting cadmium telluride nanometer rod diameter is 4～10nm, length-to-diameter ratio is 4～8.
Embodiment 7:
The preparation of cadmium telluride nanometer rod
Take by weighing 0.55g tellurium powder earlier, dissolve in the 10.1g trioctylphosphine phosphorus and make the tellurium precursor solution.Take by weighing the 0.64g Cadmium oxide then, 6.4g TETRADECONIC ACID and 30.0g trioctylphosphine oxide place reaction flask, are heated to 210 ℃ under continuously stirring, treat the tellurium precursor solution that solution transparent back injection prepares, after 3 minutes, cool the temperature to 170 ℃, stopped reaction after 12 hours, the worker treats that solution cooling back adds toluene and methyl alcohol, wash, centrifugal, drying, getting cadmium telluride nanometer rod diameter is 3～7nm, length-to-diameter ratio is 2～6.
Embodiment 8:
The preparation of cadmium telluride nanometer rod
Take by weighing 0.75g tellurium powder earlier, dissolve in the 7.60g trioctylphosphine phosphorus and make the tellurium precursor solution.Take by weighing the 0.25g Cadmium oxide then, 0.82g TETRADECONIC ACID and 16.0g trioctylphosphine oxide place reaction flask, are heated to 210 ℃ under continuously stirring, treat the tellurium precursor solution that solution transparent back injection prepares, after 5 minutes, cool the temperature to 160 ℃, stopped reaction after 8 hours treats that solution cooling back adds toluene and methyl alcohol, wash, centrifugal, drying, getting cadmium telluride nanometer rod diameter is 4～9nm, length-to-diameter ratio is 2～7.
Claims (1)
1. the preparation method of cadmium selenide and cadmium telluride nanometer rod, the monomer of employing is: Cadmium oxide CdO and selenium powder Se or Cadmium oxide CdO and tellurium powder Te; Part is: TETRADECONIC ACID; Tensio-active agent is: trioctylphosphine oxide; Solvent is: tributyl phosphorus or trioctylphosphine phosphorus; Preparation process is as follows:
(1) preparation of cadmium selenide nanorod
The weight ratio of monomer Cadmium oxide and selenium powder is CdO: Se=2: 5～5: 1, selenium powder is dissolved in is mixed with the selenium precursor solution in the tributyl phosphorus, the weight ratio of selenium powder and solvent tributyl phosphorus is Se: TBP=6: 5～4: 1, the weight ratio of Cadmium oxide and TETRADECONIC ACID is CdO: MA=1: 5～3: 5, the weight ratio of part TETRADECONIC ACID and tensio-active agent trioctylphosphine oxide is MA: TOPO=1: 5～1: 2, earlier with load weighted Cadmium oxide, TETRADECONIC ACID and trioctylphosphine oxide place reaction flask, be heated to 190 ℃～230 ℃, begin to stir after the thing fusing to be mixed, inject the selenium precursor solution then, react cooling after 2～5 minutes, growth temperature is 160～180 ℃, react stopped reaction after 8～16 hours, treat to wash with toluene and methyl alcohol after the solution cooling, centrifugal, drying, the nanometer rod diameter that makes is 3～15nm, length-to-diameter ratio is 2～10;
(2) preparation of cadmium telluride nanometer rod
The weight ratio of monomer Cadmium oxide and tellurium powder is CdO: Te=1: 4～3: 1, the tellurium powder is dissolved in is mixed with the tellurium precursor solution in the trioctylphosphine phosphorus, the weight ratio of tellurium powder and trioctylphosphine phosphorus is Te: TOP=1: 30～1: 10, the weight ratio of Cadmium oxide and TETRADECONIC ACID is CdO: MA=1: 10～3: 10, the weight ratio of part TETRADECONIC ACID and tensio-active agent trioctylphosphine oxide is MA: TOPO=1: 20～1: 5, earlier with load weighted Cadmium oxide, TETRADECONIC ACID and trioctylphosphine oxide place reaction flask, be heated to 190 ℃～230 ℃, begin to stir after the thing fusing to be mixed, inject the tellurium precursor solution for preparing then, react cooling after 2～5 minutes, growth temperature is 160～180 ℃, stopped reaction after reacting 8～16 hours under this temperature, treat to wash with toluene and methyl alcohol after the solution cooling, centrifugal, drying, the cadmium telluride nanometer rod diameter that makes is 3～10nm, length-to-diameter ratio is 2～8.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1299998C (en) * | 2004-11-05 | 2007-02-14 | 中国科学院长春应用化学研究所 | Synthesis method for cadmium selenide and cadmium telluride quantum dot |
| CN1317737C (en) * | 2004-12-03 | 2007-05-23 | 中国科学院长春应用化学研究所 | Method for synthesizing cadmium selenide and quantum point with cadmium selenide cadmium sulfide nucleocapsid structure |
| CN1320051C (en) * | 2005-03-26 | 2007-06-06 | 吉林大学 | Method for preparing transparent optical material of polymer in high nano phase |
| CN100336729C (en) * | 2006-07-03 | 2007-09-12 | 天津大学 | Raw materials components for preparation sulfide of cadmium nano crystal and process for preparing same |
| CN100379902C (en) * | 2006-08-16 | 2008-04-09 | 中国科学技术大学 | Low-temperature solvent heat growth method of cadmium telluride single-crystal |
| CN100509617C (en) * | 2007-01-04 | 2009-07-08 | 山东师范大学 | Method of synthesizing cadmium selenide nano stick |
| CN100557091C (en) * | 2007-11-07 | 2009-11-04 | 华东理工大学 | A kind of micro-reaction device and method of utilizing the thermograde synthesizing cadmium selenide nano-crystal |
| CN101328615B (en) * | 2008-04-28 | 2010-10-13 | 新疆大学 | Growth method of CdTe nanorod by catalyst assistant vacuum heat evaporation |
| CN101871127A (en) * | 2010-05-31 | 2010-10-27 | 武汉大学 | Size-controllable synthesis method for MSe (M equal to Cd, Pb) nanocrystals |
| CN101074493B (en) * | 2007-04-09 | 2011-05-11 | 吉林大学 | Method for synthesizing supefine CdSe and CdTe nano-crystal |
| CN104386656A (en) * | 2014-10-30 | 2015-03-04 | 浙江医药高等专科学校 | Method for synthesizing CdTe nano-rods in organic phase |
| TWI623945B (en) * | 2016-06-20 | 2018-05-11 | 國立清華大學 | Sensing device and methods of forming the same |
| CN110182768A (en) * | 2019-05-21 | 2019-08-30 | 南京工业大学 | A method of CdSe nanometer rods are formed by templating self-assembly of grafting block polymer |
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2003
- 2003-09-17 CN CN 03127160 patent/CN1208238C/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1299998C (en) * | 2004-11-05 | 2007-02-14 | 中国科学院长春应用化学研究所 | Synthesis method for cadmium selenide and cadmium telluride quantum dot |
| CN1317737C (en) * | 2004-12-03 | 2007-05-23 | 中国科学院长春应用化学研究所 | Method for synthesizing cadmium selenide and quantum point with cadmium selenide cadmium sulfide nucleocapsid structure |
| CN1320051C (en) * | 2005-03-26 | 2007-06-06 | 吉林大学 | Method for preparing transparent optical material of polymer in high nano phase |
| CN100336729C (en) * | 2006-07-03 | 2007-09-12 | 天津大学 | Raw materials components for preparation sulfide of cadmium nano crystal and process for preparing same |
| CN100379902C (en) * | 2006-08-16 | 2008-04-09 | 中国科学技术大学 | Low-temperature solvent heat growth method of cadmium telluride single-crystal |
| CN100509617C (en) * | 2007-01-04 | 2009-07-08 | 山东师范大学 | Method of synthesizing cadmium selenide nano stick |
| CN101074493B (en) * | 2007-04-09 | 2011-05-11 | 吉林大学 | Method for synthesizing supefine CdSe and CdTe nano-crystal |
| CN100557091C (en) * | 2007-11-07 | 2009-11-04 | 华东理工大学 | A kind of micro-reaction device and method of utilizing the thermograde synthesizing cadmium selenide nano-crystal |
| CN101328615B (en) * | 2008-04-28 | 2010-10-13 | 新疆大学 | Growth method of CdTe nanorod by catalyst assistant vacuum heat evaporation |
| CN101871127A (en) * | 2010-05-31 | 2010-10-27 | 武汉大学 | Size-controllable synthesis method for MSe (M equal to Cd, Pb) nanocrystals |
| CN101871127B (en) * | 2010-05-31 | 2012-03-21 | 武汉大学 | Size-controllable synthesis method for MSe (M equal to Cd, Pb) nanocrystals |
| CN104386656A (en) * | 2014-10-30 | 2015-03-04 | 浙江医药高等专科学校 | Method for synthesizing CdTe nano-rods in organic phase |
| TWI623945B (en) * | 2016-06-20 | 2018-05-11 | 國立清華大學 | Sensing device and methods of forming the same |
| CN110182768A (en) * | 2019-05-21 | 2019-08-30 | 南京工业大学 | A method of CdSe nanometer rods are formed by templating self-assembly of grafting block polymer |
| CN110182768B (en) * | 2019-05-21 | 2022-12-16 | 南京工业大学 | Method for forming CdSe nanorod by self-assembly by taking grafted block polymer as template |
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