CN104386656A - Method for synthesizing CdTe nano-rods in organic phase - Google Patents
Method for synthesizing CdTe nano-rods in organic phase Download PDFInfo
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- CN104386656A CN104386656A CN201410596992.9A CN201410596992A CN104386656A CN 104386656 A CN104386656 A CN 104386656A CN 201410596992 A CN201410596992 A CN 201410596992A CN 104386656 A CN104386656 A CN 104386656A
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- C01B19/00—Selenium; Tellurium; Compounds thereof
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses a method for synthesizing CdTe nano-rods in an organic phase. The method comprises the following steps: (1) putting Te in a single-neck round-bottomed flask; adding trioctylphosphine to prepare a Te-TOP solution under nitrogen protection; mixing the Te-TOP solution with oleylamine to prepare a precursor solution; (2) adding oleic acid and oleylamine which are in a volume ratio of 1:(5-100) into a three-necked round-bottomed flask, adding CdO; and heating to 280-310 DEG C under nitrogen protection, injecting in the precursor solution, and cooling to 230-260 DEG C. The method can be used for effectively synthesizing CdTe nano-rods which have the length of 50-200nm and high crystal degree.
Description
Technical field
The present invention relates to a kind of method of synthesizing CdTe nanometer rod in organic phase.
Background technology
Inorganic semiconductor nanometer rod, because special shape, electronic energy is directional transmissions in nanometer rod, therefore has more superiority than nano spherical particle, especially there is in nano electron device very high expectation, such as improve the electricity conversion etc. of organic inorganic hybridization solar cell.Therefore the inorganic semiconductor nanometer rod that synthesis has length (being greater than 50nm) is developed, significant.
The synthetic method of current CdTe nano material, is mainly divided into Aqueous phase and organic phase method, and CdTe nano material prepared by Aqueous phase is mainly used in the middle of life science, mainly synthesizes in organic phase for the CdTe nano material in photoelectric device.Use organic phase method to prepare CdTe nano material, be mainly high temperature organometallic compound decomposition method, catalyst method and micro emulsion method.
High temperature organometallic compound decomposition method is a kind of very outstanding method preparing high-quality semiconductor nanometer rod, and this method has started the epoch of semi-conductor nano particles morphology control.But make the length of the CdTe nanometer rod prepared in this way substantially at about 20nm, length is shorter, cannot provide direct transmission path in hybrid solar cell to electronics.
Catalyst method also can carry out morphology control to CdTe nano material, this method mainly uses Bi compound as catalyzer, synthesizing one-dimensional CdTe nano wire, successfully can synthesize high-quality CdTe nano wire now, there is good degree of crystallinity and homogeneity, the prepared CdTe nanowire length obtained can reach several micron, but can prepare high-quality CdTe nano wire in this way, uncontrollable synthesis CdTe nanometer rod.In addition, the preparation synthesis of Bi compound is very crucial in this approach, and the synthesis ratio of high quality Bi compound (catalyzer) is more difficult, is difficult to control.
Micro emulsion method can prepare CdTe nanoparticle, but preparation-obtained nanoparticle is mainly spherical, and homogeneity is not as high temperature organometallic compound decomposition method.But rarely have report for the CdTe nanometer rod of particle length between 50-200 nanometer, concerning organic inorganic hybridization solar cell, the nanometer rod of this length is the most suitable, most possibly provides direct transmission path to electron hole.The raising of CdTe nanometer rod to hybrid solar cell energy conversion efficiency of the Gao Jingdu that the synthetic method that therefore researchdevelopment is new is prepared within the scope of this has great importance.
Summary of the invention
Technical problem to be solved by this invention is, overcomes the shortcoming of above prior art: provide a kind of nanorod length between 50-200 nm, Gao Jingdu, in organic phase, synthesize the method for CdTe nanometer rod.
Technical solution of the present invention is as follows: a kind of method of synthesizing CdTe nanometer rod in organic phase, comprises the following steps:
1) preparation of precursor solution: Te is placed in single neck round-bottomed flask, adds tri octyl phosphine (TOP), at N
2be heated to 240 DEG C of-300 DEG C of successive reaction 8-10 hour under protection, treat the Te solid completely dissolve in solution, obtained Te-TOP solution; Under the protection of nitrogen, Te-TOP solution is mixed obtained Te-TOP-OLAM precursor solution with oleyl amine (OLAM);
2) in three neck round-bottomed flasks, add the oleic acid that volume ratio is 1 ︰ 5-100 and oleyl amine, then add CdO; Under the protection of nitrogen; be heated to 280-310 DEG C; solution becomes clarification; when 280-310 DEG C; be injected into the precursor solution prepared in step 1), solution becomes brown at once, cools between 230 DEG C-260 DEG C; allow semiconductor crystal grow up, the CdTe nanometer rod of length range between 50-200 nm after 20 s-15 min, can be obtained.
In step 1), the volume ratio of Te-TOP solution and oleyl amine is: 1 ︰ 7-50.
In described Te-TOP solution, the concentration of Te is 0.2-1.5 mol/L.
Preferably, in described Te-TOP solution, the concentration of Te is 0.7 mol/L in effect.
In step 2) in, the add-on of CdO is every milliliter of oleyl amine 0.0013 mmol-0.02 mmol.
As preferably, in step 2) in, the add-on of CdO is every milliliter of oleyl amine 0.01 mmol.
In step 2) in, the volume ratio of precursor solution and oleyl amine is 1 ︰ 2.5-20.
The invention has the beneficial effects as follows: existing CdTe nanometer rod of synthesizing in organic phase is maximum under normal circumstances can only reach 20-30 about nm, too short concerning length a lot of photoelectric nano device, do not utilize the special efficent electronic transmission performance playing nanometer rod, such as in organic inorganic hybridization solar cell, the thickness of battery-active layer is far longer than 20-30 nm, therefore, the CdTe nanometer rod of preparation length between 50-200 nm can provide better electronic transmission performance for Novel Optoelectronic Device, method of the present invention can in organic phase efficient synthesis of nano rod length between 50-200 nm, the CdTe nanometer rod of Gao Jingdu, be applicable to promoting.
Accompanying drawing explanation
Fig. 1 is the CdTe nanometer rod Electronic Speculum figure that the embodiment of the present invention 1 obtains.
Fig. 2 is the CdTe nanometer rod Electronic Speculum figure that the embodiment of the present invention 2 obtains.
Fig. 3 is the CdTe nanometer rod Electronic Speculum figure that the embodiment of the present invention 3 obtains.
Fig. 4 is the CdTe nanometer rod Electronic Speculum figure that the embodiment of the present invention 5 obtains.
Embodiment
With specific embodiment, the present invention is described in further details below, but the present invention is not only confined to following specific embodiment.
Embodiment one
1) preparation of precursor solution: by 0.8932g Te(tellurium) be placed in the mono-neck round-bottomed flask of 25ml, add 10 ml tri octyl phosphines (TOP), at N
2be heated to 250 DEG C of successive reaction 8-10 hour under protection, treat the Te solid completely dissolve in solution, obtain the Te-TOP solution that Te concentration is 0.7 mol/L; Under the protection of nitrogen, get 0.071 ml Te-TOP solution and be dissolved in obtained precursor solution in 2 ml oleyl amines;
2) in 50 ml tri-neck round-bottomed flasks, 0.013 mmol CdO, 10 ml oleyl amines, 2000 μ l oleic acid are added; under nitrogen protection; be heated to 300 DEG C; solution becomes clarification, is injected into ready precursor solution 2 ml, wherein containing 0.05 mmolTe; solution becomes brown at once; cool between 230 DEG C-260 DEG C, allow semiconductor crystal grow up, the CdTe nanometer rod of length between 50-100 nm after 5 min, can be obtained.
Embodiment two
1) preparation of precursor solution: by 0.8932g Te(tellurium) be placed in the mono-neck round-bottomed flask of 25 ml, add 10 ml tri octyl phosphines (TOP), at N
2be heated to 250 DEG C of successive reaction 8-10 hour under protection, treat the Te solid completely dissolve in solution, obtain the Te-TOP solution that Te concentration is 0.7 mol/L; Under the protection of nitrogen, get 0.071 ml Te-TOP solution and be dissolved in obtained precursor solution in 2 ml oleyl amines;
2) in 50ml tri-neck round-bottomed flask, add 0.10 mmol CdO(Cadmium oxide), 10 ml oleyl amines, 200 μ l oleic acid; under nitrogen protection; be heated to 300 DEG C; solution becomes clarification, is injected into ready precursor solution 2 ml, wherein containing 0.05 mmolTe; solution becomes brown at once; cool between 230 DEG C-260 DEG C, allow semiconductor crystal grow up, the CdTe nanometer rod of length between 100-200 nm after 5 min, can be obtained.
Embodiment three
1) preparation of precursor solution: by 0.8932g Te(tellurium) be placed in the mono-neck round-bottomed flask of 25 ml, add 10ml tri octyl phosphine (TOP), at N
2be heated to 250 DEG C of successive reaction 8-10 hour under protection, treat the Te solid completely dissolve in solution, obtain the Te-TOP solution that Te concentration is 0.7 mol/L; Under the protection of nitrogen, get 0.071 ml Te-TOP solution and be dissolved in obtained precursor solution in 2 ml oleyl amines;
2) in 50ml tri-neck round-bottomed flask, add 0.013 mmol CdO(Cadmium oxide), 10ml oleyl amine, 800 μ l oleic acid; under nitrogen protection; be heated to 300 DEG C; solution becomes clarification, is injected into ready precursor solution 2 ml, wherein containing 0.05 mmolTe; solution becomes brown at once; cool between 230 DEG C-260 DEG C, allow semiconductor crystal grow up, can obtain length after 120 s is 50-100 nmCdTe nanometer rod.
Embodiment four
1) preparation of precursor solution: by 0.8932g Te(tellurium) be placed in the mono-neck round-bottomed flask of 25 ml, add 10 ml tri octyl phosphines (TOP), at N
2be heated to 250 DEG C of successive reaction 8-10 hour under protection, treat the Te solid completely dissolve in solution, obtain the Te-TOP solution that Te concentration is 0.7 mol/L; Under the protection of nitrogen, get 0.29 mlTe-TOP solution and be dissolved in obtained precursor solution in 2ml oleyl amine;
2) in 50 ml tri-neck round-bottomed flasks, add 0.05 mmol CdO(Cadmium oxide), 10 ml oleyl amines, 200 μ l oleic acid; under nitrogen protection; be heated to 300 DEG C; solution becomes clarification, is injected into ready precursor solution 2 ml, wherein containing 0.20 mmolTe; solution becomes brown at once; cool between 230 DEG C-260 DEG C, allow semiconductor crystal grow up, the CdTe nanometer rod of length between 50-100 nanometer after 5 min, can be obtained.
Embodiment five
1) preparation of precursor solution: by 0.8932g Te(tellurium) be placed in the mono-neck round-bottomed flask of 25 ml, add 10 ml tri octyl phosphines (TOP), at N
2be heated to 250 DEG C of successive reaction 8-10 hour under protection, treat the Te solid completely dissolve in solution, obtain the Te-TOP solution that Te concentration is 0.7 mol/L; Under the protection of nitrogen, get 0.14 ml Te-TOP solution and be dissolved in obtained precursor solution in 2 ml oleyl amines;
2) in 50ml tri-neck round-bottomed flask, add 0.05 mmol CdO(Cadmium oxide), 10 ml oleyl amines, 100 μ l oleic acid; under nitrogen protection; be heated to 300 DEG C; solution becomes clarification, is injected into ready precursor solution 2 ml, wherein containing 0.10 mmolTe; solution becomes brown at once; cool between 230 DEG C-260 DEG C, allow semiconductor crystal grow up, the CdTe nanometer rod of length between 50-200 nm after 20 s, can be obtained.
Below be only that feature of the present invention implements example, scope is not constituted any limitation.The technical scheme that all employings exchange on an equal basis or equivalence is replaced and formed, all drops within rights protection scope of the present invention.
Claims (7)
1. synthesize a method for CdTe nanometer rod in organic phase, it is characterized in that: comprise the following steps:
1) preparation of precursor solution: Te is placed in single neck round-bottomed flask, adds tri octyl phosphine, at N
2be heated to 240 DEG C of-300 DEG C of successive reaction 8-10 hour under protection, treat the Te solid completely dissolve in solution, obtained Te-TOP solution; Under the protection of nitrogen, Te-TOP solution is mixed obtained precursor solution with oleyl amine;
2) in three neck round-bottomed flasks, add the oleic acid that volume ratio is 1 ︰ 5-100 and oleyl amine, then add CdO; Under the protection of nitrogen; be heated to 280 DEG C-310 DEG C; solution becomes clarification; 280 DEG C-310 DEG C time; be injected into the precursor solution prepared in step 1), solution becomes brown at once, cools between 230 DEG C-260 DEG C; allow semiconductor crystal grow up, the CdTe nanometer rod of length range between 50nm-200nm after 20s-15min, can be obtained.
2. synthesize the method for CdTe nanometer rod in organic phase according to claim 1, it is characterized in that: in step 1), the volume ratio of Te-TOP solution and oleyl amine is: 1 ︰ 7-50.
3. synthesize the method for CdTe nanometer rod in organic phase according to claim 1, it is characterized in that: in described Te-TOP solution, the concentration of Te is 0.2-1.5mol/L.
4. synthesize the method for CdTe nanometer rod in organic phase according to claim 3, it is characterized in that: in described Te-TOP solution, the concentration of Te is 0.7mol/L.
5. synthesize the method for CdTe nanometer rod in organic phase according to claim 1, it is characterized in that: in step 2) in, the add-on of CdO is every milliliter of oleyl amine 0.0013mmol-0.02mmol.
6. synthesize the method for CdTe nanometer rod in organic phase according to claim 5, it is characterized in that: in step 2) in, the add-on of CdO is every milliliter of oleyl amine 0.01mmol.
7. synthesize the method for CdTe nanometer rod in organic phase according to claim 1, it is characterized in that: in step 2) in, the volume ratio of precursor solution and oleyl amine is 1 ︰ 2.5-20.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110342475A (en) * | 2019-06-24 | 2019-10-18 | 吉林大学 | A kind of preparation method of the adjustable two telluride ferrum nano material of appearance and size |
Citations (3)
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| CN1524782A (en) * | 2003-09-17 | 2004-09-01 | 中国科学院长春应用化学研究所 | Manufacturing method of cadmium selenide and cadmium telluride nanometer rod |
| CN1884093A (en) * | 2006-07-03 | 2006-12-27 | 天津大学 | Raw materials components for preparation sulfide of cadmium nano crystal and process for preparing same |
| CN102530891A (en) * | 2011-03-02 | 2012-07-04 | 北京师范大学 | Method for preparing Cd Te nano-wire and Cd Te-based core-shell type nano-wire by liquid-phase non-catalysis |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1524782A (en) * | 2003-09-17 | 2004-09-01 | 中国科学院长春应用化学研究所 | Manufacturing method of cadmium selenide and cadmium telluride nanometer rod |
| CN1884093A (en) * | 2006-07-03 | 2006-12-27 | 天津大学 | Raw materials components for preparation sulfide of cadmium nano crystal and process for preparing same |
| CN102530891A (en) * | 2011-03-02 | 2012-07-04 | 北京师范大学 | Method for preparing Cd Te nano-wire and Cd Te-based core-shell type nano-wire by liquid-phase non-catalysis |
Non-Patent Citations (1)
| Title |
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| XIAOPING JIN ET AL.: ""Catalyst-Free Synthesis and Shape Control of CdTe Nanowires"", 《NANO RESEARCH》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110342475A (en) * | 2019-06-24 | 2019-10-18 | 吉林大学 | A kind of preparation method of the adjustable two telluride ferrum nano material of appearance and size |
| CN110342475B (en) * | 2019-06-24 | 2022-07-19 | 吉林大学 | Preparation method of iron ditelluride nano material with adjustable shape and size |
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