CN101962177B - Method for solvent thermal growth of cubic phase CdTe nano belt - Google Patents
Method for solvent thermal growth of cubic phase CdTe nano belt Download PDFInfo
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- CN101962177B CN101962177B CN 201010508431 CN201010508431A CN101962177B CN 101962177 B CN101962177 B CN 101962177B CN 201010508431 CN201010508431 CN 201010508431 CN 201010508431 A CN201010508431 A CN 201010508431A CN 101962177 B CN101962177 B CN 101962177B
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Abstract
The invention discloses a method for solvent thermal growth of a cubic phase CdTe nano belt, which is implemented through the following technical processes: reducing tellurium powder (Te) into solution of Te2- by using potassium borohydride; and adding a Cd source and aqueous solution of ethylene diamine in turn, sealing and keeping at high temperature for one day, cleaning samples after reaction so as to prepare black solid, namely a cubic-phase cadmium telluride nano belt. The method has the characteristics of simpleness, high yield, high uniformity of the prepared CdTe nano belt, low environmental damage, easy popularization and suitability for large-scale industrial production.
Description
Technical field
The present invention is a kind of method about the growth of the solvent thermal under water, quadrol binary mixed solvent system CdTe nano belt.
Background technology
CdTe is the photovaltaic material that a kind of direct energy gap is about 1.5eV, at the solar spectrum wave band very high uptake factor is arranged, and can be electric energy with conversion of solar energy effectively, is a kind of outstanding photovoltaic energy material.Nano materials research report in recent years shows that the material of nanoscale might have more excellent performance, can prepare the better device of performance.In at present numerous methods for preparing nano material, the hydro-thermal solvent thermal process has numerous advantages, and is very fast in development in recent years, and it is simple to operate, temperature is low, and environmental pollution is less, and product is dispersed, homogeneity is good.Because it is the preparation process is carried out in totally sealed environment, has effectively reduced the effusion and the release of toxic gas in the preparation process, especially practical to nano material with toxic compound.
In September, 1998, Li Yadong was with CdCl
2For cadmium source and simple substance Te are solvent at quadrol, having grown long 100-300nm diameter under 120-190 ℃ is the nanometer stub about 10nm, and proposes the small molecules coordination theory.Consult 2301 pages of Chem.Mater.1998 the 9th phase the 10th volumes.
In 1999 the safe group of escaping utilizes Cd (NO
3)
2With 3: 1 mixed of Te powder, in several kinds of different solvents, the nanometer rod that is uneven in length has been made in 160 degree reactions respectively.Consult 1509 pages of the 35th phases of Materials Research Bulletin2000.
Li Yadong group primary study in 2002 quadrol as molecular tempiate, can form organic-inorganic composite body with CdTe, guiding monodimension nanometer material synthetic.Consult 2331 pages of Inorganic Chemistry 2003 the 7th phases the 42nd volumes.
The Wang Qiang of Changchun university in 2004 etc. are the forerunner with the product that obtains of polyvalent alcohol circumfluence method, have synthesized nano particle, the stub about 50nm and triangular shape about 10nm under the hydro-thermal.Consult 83 pages of Journal of CrystalGrowth 2006 84 phases the 286th volumes.
Kotov group in 2006 finds that the nano particle of CdTe can reconstitute the crystalline nano wire under the protection that loses the organism stablizer.Consult 518 pages of the 18th phases of Adv.Mater.2006.
People such as Zheng Rong ripple were with Te and NaBH in 2007
4Reaction generates NaHTe, stirs down at 30 ℃, makes Te
2-Generated the nano wire of Te by airborne dioxygen oxidation.Nano wire with the Te that generates is the Te source then, and MSA (sulfenyl Succinic Acid) is a coverture, has generated the CdTe nano wire, and has made subminiature red fluorescence valve with it.Consult the 6920th page of the 46th phase of Inorg.Chem.2007
Escape doctor Xi Guangcheng of safe group of in 2008 makes the Te/C nano-cable under the condition of hydro-thermal, and lets they and metal-salt under the condition of hydro-thermal, permutoid reaction take place, and obtains MTe/C (M=Cd, Pb, Ag) nano-cable.Consult 965 pages of J.Phys.Chem.2008 the 4th phase the 112nd volumes.
2008, people such as the Gong of Shandong University hypo joined the Te powder the dense HNO of heat
3In, add NaOH again and form NaTeO
3Basic soln, be the Te source with this solution, with Cd (NO
3)
2At CTAB is dispersion agent, is that solvent has obtained the CdTe nanometer rod with the deionized water.Consult the 445603rd page of Nanotechnology 2008 the 19th phase.
Can see, use simple solvent-thermal method to prepare the CdTe nano belt and do not report.
The present invention proposes a kind of simple water, quadrol binary mixed solution system, with KBH
4Be reductive agent, under 120-160 ℃, generate thick 100-200, wide 0.2-1mm, long several microns nano belt.Infer that from growth mechanism this method can be applicable to the preparation of the metallic compound nano material of other selenium (Se), tellurium (Te).
Summary of the invention
The present invention is achieved in that tellurium powder (Te), POTASSIUM BOROHYDRIDE 97MIN (KBH
4) dissolve in a spot of water, secluding air leaves standstill, and treats that solution is red by the black pulverize, promptly obtains Te
2-Solution; Source cadmium (comprising cadmium nitrate, Cadmium Sulphate, Cadmium chloride fine powder, cadmium acetate) is dissolved in a spot of water, obtain Cd after the dissolving fully
2+Solution.Two kinds of solution are mixed, strong reaction takes place, produce a large amount of gases, solution colour becomes black rapidly.When question response slows down gradually, add quadrol, the TV of water and the volume ratio of quadrol are about 1: 4 before and after making.Transfer in the tetrafluoroethylene hydrothermal reaction kettle after stirring for some time, make liquor capacity account for about 80% of container TV.Seal in the high temperature oven that is kept at 100-180 ℃, left standstill 12-48 hour.Reaction cleans up after accomplishing, and the black solid that obtains is the CdTe nano belt.
Description of drawings
The XRD figure spectrum of Fig. 1 embodiment one product, ★ representes the diffraction peak of impurity Te.
The ESEM picture of Fig. 2 embodiment one product.
The ESEM picture of Fig. 3 embodiment two products.
The ESEM picture of Fig. 4 embodiment three products.
The ESEM picture of Fig. 5 embodiment four-product.
The ESEM picture of Fig. 6 embodiment five products.
The ESEM picture of Fig. 7 embodiment six products.
The ESEM picture of Fig. 8 embodiment seven products.
The ESEM picture of Fig. 9 embodiment eight products.
Specific embodiment
Embodiment one
With 3mmol tellurium powder (0.3828gTe), 0.35gKBH
4Dissolve in a spot of water, secluding air leaves standstill, and treats that solution is red by the black pulverize, promptly obtains Te
2-Solution; With 3mmol Cadmium chloride fine powder (0.6851gCdCl
22.5H
2O) dissolve in a spot of water, obtain Cd after the dissolving fully
2+Solution.Two kinds of solution are mixed, strong reaction takes place, produce a large amount of gases, solution colour becomes black rapidly.When question response slows down gradually, add quadrol, the TV of water and the volume ratio of quadrol are about 1: 4 before and after making.Transfer in the tetrafluoroethylene hydrothermal reaction kettle after stirring for some time, make liquor capacity account for about 80% of container TV.Seal in the high temperature oven that is kept at 160 ℃, left standstill 48 hours.Reaction cleans up after accomplishing, and the black solid that obtains is the CdTe nano belt.The XRD analysis result shows that the principal phase of product is cube CdTe, like Fig. 1; ESEM (SEM) analytical results shows that product is banded nano material, like Fig. 2.
Embodiment two
With 3mmol tellurium powder (0.3828gTe), 0.35gKBH
4Dissolve in a spot of water, secluding air leaves standstill, and treats that solution is red by the black pulverize, promptly obtains Te
2-Solution; With 3mmol cadmium acetate (0.7996gCd (CH
3COO)
22H
2O) dissolve in a spot of water, obtain Cd after the dissolving fully
2+Solution.Two kinds of solution are mixed, strong reaction takes place, produce a large amount of gases, solution colour becomes black rapidly.When question response slows down gradually, add quadrol, the TV of water and the volume ratio of quadrol are about 1: 4 before and after making.Transfer in the tetrafluoroethylene hydrothermal reaction kettle after stirring for some time, make liquor capacity account for about 80% of container TV.Seal in the high temperature oven that is kept at 160 ℃, left standstill 48 hours.Reaction cleans up after accomplishing, and the black solid that obtains is the CdTe nano belt.ESEM (SEM) analytical results shows that product is banded nano material, like Fig. 3.
Embodiment three
With 3mmol tellurium powder (0.3828gTe), 0.35gKBH
4Dissolve in a spot of water, secluding air leaves standstill, and treats that solution is red by the black pulverize, promptly obtains Te
2-Solution; With 3mmol cadmium nitrate (0.9254gCd (NO
3)
24H
2O) dissolve in a spot of water, obtain Cd after the dissolving fully
2+Solution.Two kinds of solution are mixed, strong reaction takes place, produce a large amount of gases, solution colour becomes black rapidly.When question response slows down gradually, add quadrol, the TV of water and the volume ratio of quadrol are about 1: 4 before and after making.Transfer in the tetrafluoroethylene hydrothermal reaction kettle after stirring for some time, make liquor capacity account for about 80% of container TV.Seal in the high temperature oven that is kept at 160 ℃, left standstill 48 hours.Reaction cleans up after accomplishing, and the black solid that obtains is the CdTe nano belt.ESEM (SEM) analytical results shows that product is banded nano material, like Fig. 4.
Embodiment four
With 3mmol tellurium powder (0.3828gTe), 0.35gKBH
4Dissolve in a spot of water, secluding air leaves standstill, and treats that solution is red by the black pulverize, promptly obtains Te
2-Solution; With 3mmol cadmium nitrate (0.9254gCd (NO
3)
24H
2O) dissolve in a spot of water, obtain Cd after the dissolving fully
2+Solution.Two kinds of solution are mixed, strong reaction takes place, produce a large amount of gases, solution colour becomes black rapidly.When question response slows down gradually, add quadrol, the TV of water and the volume ratio of quadrol are about 1: 4 before and after making.Transfer in the tetrafluoroethylene hydrothermal reaction kettle after stirring for some time, make liquor capacity account for about 80% of container TV.Seal in the high temperature oven that is kept at 160 ℃, left standstill 24 hours.Reaction cleans up after accomplishing, and the black solid that obtains is the CdTe nano belt.ESEM (SEM) analytical results shows that product is banded nano material, like Fig. 5.
Embodiment five
With 3mmol tellurium powder (0.3828gTe), 0.35gKBH
4Dissolve in a spot of water, secluding air leaves standstill, and treats that solution is red by the black pulverize, promptly obtains Te
2-Solution; With 3mmol Cadmium chloride fine powder (0.9254gCd (NO
3)
24H
2O) dissolve in a spot of water, obtain Cd after the dissolving fully
2+Solution.Two kinds of solution are mixed, strong reaction takes place, produce a large amount of gases, solution colour becomes black rapidly.When question response slows down gradually, add quadrol, the TV of water and the volume ratio of quadrol are about 1: 4 before and after making.Transfer in the tetrafluoroethylene hydrothermal reaction kettle after stirring for some time, make liquor capacity account for about 80% of container TV.Seal in the high temperature oven that is kept at 160 ℃, left standstill 36 hours.Reaction cleans up after accomplishing, and the black solid that obtains is the CdTe nano belt.ESEM (SEM) analytical results shows that product is banded nano material, like Fig. 6.
Embodiment six
With 3mmol tellurium powder (0.3828gTe), 0.35gKBH
4Dissolve in a spot of water, secluding air leaves standstill, and treats that solution is red by the black pulverize, promptly obtains Te
2-Solution; With 3mmol Cadmium chloride fine powder (0.6851g CdCl
2) dissolve in a spot of water, obtain Cd after the dissolving fully
2+Solution.Two kinds of solution are mixed, strong reaction takes place, produce a large amount of gases, solution colour becomes black rapidly.When question response slows down gradually, add quadrol, the TV of water and the volume ratio of quadrol are about 1: 4 before and after making.Transfer in the tetrafluoroethylene hydrothermal reaction kettle after stirring for some time, make liquor capacity account for about 80% of container TV.Seal in the high temperature oven that is kept at 160 ℃, left standstill 24 hours.Reaction cleans up after accomplishing, and the black solid that obtains is the CdTe nano belt.ESEM (SEM) analytical results shows that product is banded nano material, like Fig. 7.
Embodiment seven
With 3mmol tellurium powder (0.3828gTe), 0.35gKBH
4Dissolve in a spot of water, secluding air leaves standstill, and treats that solution is red by the black pulverize, promptly obtains Te
2-Solution; With 3mmol Cadmium chloride fine powder (0.6851gCdCl
22.5H
2O) dissolve in a spot of water, obtain Cd after the dissolving fully
2+Solution.Two kinds of solution are mixed, strong reaction takes place, produce a large amount of gases, solution colour becomes black rapidly.When question response slows down gradually, add quadrol, the TV of water and the volume ratio of quadrol are about 1: 4 before and after making.Transfer in the tetrafluoroethylene hydrothermal reaction kettle after stirring for some time, make liquor capacity account for about 80% of container TV.Seal in the high temperature oven that is kept at 140 ℃, left standstill 24 hours.Reaction cleans up after accomplishing, and the black solid that obtains is the CdTe nano belt.ESEM (SEM) analytical results shows that product is banded nano material, like Fig. 8.
Embodiment eight
With 3mmol tellurium powder (0.3828gTe), 0.35gKBH
4Dissolve in a spot of water, secluding air leaves standstill, and treats that solution is red by the black pulverize, promptly obtains Te
2-Solution; With 3mmol Cadmium chloride fine powder (0.6851gCdCl
22.5H
2O) dissolve in a spot of water, obtain Cd after the dissolving fully
2+Solution.Two kinds of solution are mixed, strong reaction takes place, produce a large amount of gases, solution colour becomes black rapidly.When question response slows down gradually, add quadrol, the TV of water and the volume ratio of quadrol are about 1: 4 before and after making.Transfer in the tetrafluoroethylene hydrothermal reaction kettle after stirring for some time, make liquor capacity account for about 80% of container TV.Seal in the high temperature oven that is kept at 100 ℃, left standstill 24 hours.Reaction cleans up after accomplishing, and the black solid that obtains is the CdTe nano belt.ESEM (SEM) analytical results shows that product is the near banded nano material of bluring, like Fig. 9.
Claims (1)
1. the method for solvent thermal growth cube phase CdTe nano belt: 0.3828g tellurium powder, 0.35g POTASSIUM BOROHYDRIDE 97MIN are dissolved in a spot of water, and secluding air leaves standstill, and treats that solution is red by the black pulverize, promptly obtains Te
2-Solution; The 3.0mmol Cadmium chloride fine powder is dissolved in a spot of water, obtain Cd after the dissolving fully
2+Solution; With above-mentioned Te
2-Solution and Cd
2+Solution mix, strong reaction takes place, produce a large amount of gases, solution colour becomes black rapidly; When question response slows down gradually, add quadrol, making the TV of water and the volume ratio of quadrol is 1: 4; Transfer in the tetrafluoroethylene hydrothermal reaction kettle after stirring for some time, make liquor capacity account for 80% of container TV, seal in the high temperature oven that is kept at 100-180 ℃; Left standstill 12-48 hour, reaction cleans up after accomplishing, and the black solid that obtains is a cube phase CdTe nano belt.
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| CN112573490A (en) * | 2020-11-09 | 2021-03-30 | 青海大学 | Method for macro-preparation of uniform single crystal cadmium telluride nanorods |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1159211C (en) * | 2002-06-07 | 2004-07-28 | 清华大学 | Synthesis of several metal selenides and tellurides as semiconductor material |
| CN100545307C (en) * | 2007-06-29 | 2009-09-30 | 陕西师范大学 | The KBH of ZnSe nano belt 4-Zn-Se-NH 2C 2H 4NH 2Solvothermal preparation method |
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2010
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1159211C (en) * | 2002-06-07 | 2004-07-28 | 清华大学 | Synthesis of several metal selenides and tellurides as semiconductor material |
| CN100545307C (en) * | 2007-06-29 | 2009-09-30 | 陕西师范大学 | The KBH of ZnSe nano belt 4-Zn-Se-NH 2C 2H 4NH 2Solvothermal preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 张刚等.水热法制备稳定的发光CdTe材料.《高等学校化学学报》.2003,第24卷(第4期),第662-663. |
| 水热法制备稳定的发光CdTe材料;张刚等;《高等学校化学学报》;20030430;第24卷(第4期);第662-663 * |
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