CN1278941C - Bi2Te3 nanometer capsule and preparation thereof - Google Patents
Bi2Te3 nanometer capsule and preparation thereof Download PDFInfo
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- CN1278941C CN1278941C CN 200410073387 CN200410073387A CN1278941C CN 1278941 C CN1278941 C CN 1278941C CN 200410073387 CN200410073387 CN 200410073387 CN 200410073387 A CN200410073387 A CN 200410073387A CN 1278941 C CN1278941 C CN 1278941C
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- nanocapsule
- bi2te3
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- 239000002775 capsule Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims description 9
- 229910002899 Bi2Te3 Inorganic materials 0.000 title abstract 6
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000002088 nanocapsule Substances 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 230000002829 reductive effect Effects 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 abstract description 5
- 238000004377 microelectronic Methods 0.000 abstract description 2
- 238000007704 wet chemistry method Methods 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000002041 carbon nanotube Substances 0.000 description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 239000002071 nanotube Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 206010065042 Immune reconstitution inflammatory syndrome Diseases 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- QCAWEPFNJXQPAN-UHFFFAOYSA-N methoxyfenozide Chemical compound COC1=CC=CC(C(=O)NN(C(=O)C=2C=C(C)C=C(C)C=2)C(C)(C)C)=C1C QCAWEPFNJXQPAN-UHFFFAOYSA-N 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000001239 high-resolution electron microscopy Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
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Abstract
The present invention discloses an Bi2Te3 nanometer capsule which is a seamless hollow capsule whose ratio of length to diameter is from 2 to 5. The Bi2Te3 nanometer capsule comprises the constituents of the atom percentage content: 39.8 to 40.3% of Bi and 59.7 to 60.2% of Te. The Bi2Te3 nanometer capsule is prepared by adopting a wet chemistry method. The Bi2Te3 nanometer capsule with hollow tube type structural is possible to improve the thermoelectric properties of semiconductors, and the Bi2Te3 nanometer capsule can be used for preparing thermoelectric material with high performance and is widely used in the fields of material, physics, chemistry, microelectronics, etc.
Description
Technical field
The present invention relates to semi-conductor Bi
2Te
3Nanocapsule and preparation method thereof.
Background technology
From Japanese carbonization scholar Iijima in 1991 since (S.Lijima) find carbon nanotube (CNTs) first, people have carried out extensive and deep research to synthetic, structure, performance and the application etc. of carbon nanotube.Carbon nanotube has the seamless tubular shaped structure that unique one dimension hollow graphite sheet is curled into because of it, and have a series of peculiar properties, as the height chemical stability, (Theoretical Calculation shows high physical strength, its tensile strength is 100 times of steel, and density have only steel 1/6), special electric property (different according to caliber and helicity, can be the conductor not worse than copper, also can be semi-conductor).Carbon nanotube is the material that a class has the applications well prospect, nowadays has been widely used in a plurality of high-tech areas such as physics, chemistry, material, electronic technology.
Since carbon nanotube, other various one dimension tubular nanometer materials are because its special structure and application prospects also receive much concern BN, BC
3, BC
2N, WS
2, MoS
2Emerge in succession Deng nanotube, but still do not satisfy the demand of a plurality of researchs and Application Areas, the nanotube of more materials and type still awaits R and D.
Bi
2Te
3It is one of binary mineral compound of present known nucleidic mass maximum.Bi
2Te
3The base alloy also is the best room temperature type thermoelectric material of present performance, is used to make semiconductor cooling device or thermoelectric power generation device.There are some researches prove that the nanometer of material (as: superlattice, nano wire etc.) can further improve Bi
2Te
3The thermoelectricity capability of sill.Existing solvent thermal or the synthetic Bi of hydrothermal method of adopting
2Te
3Nanotube, and be used to prepare the research report of high performance thermoelectric material.
Summary of the invention
The objective of the invention is Application Areas, and a kind of Bi is provided for the expansion nano material
2Te
3Nanocapsule and preparation method thereof.
Bi of the present invention
2Te
3Nanocapsule is that L/D ratio is 2～5 seamless hollow capsules, and its component and atomic percentage conc are:
Bi 39.8～40.3％，
Te 59.7～60.2％。
Bi
2Te
3The diameter of nanocapsule is 50～200 nanometers, wall thickness 5～20 nanometers, length 200～1000 nanometers.
Bi of the present invention
2Te
3The preparation method of nanocapsule adopts wet chemistry method, and its step is as follows:
1) compound of Bi element and the pure Te powder ratio according to Bi and Te atomic percentage conc is placed in the reaction vessel, add the deionized water of 80～850 times of Te weight, and mix;
2) in above-mentioned mixed solution, add 0.25～2.5 times the complexing agent that is equivalent to Te weight, add alkaline conditioner and make the pH value of solution value be in 12～14, add 0.5～3 times the reductive agent that is equivalent to Te weight;
3) be heated to the interior setting temperature of reaction of 55～85 ℃ of scopes, react after 6～100 hours, cool to room temperature stops to stir;
4) collect the interior solid reaction product of reaction vessel, behind cleaning-drying, obtain material of the present invention.
The compound of above-mentioned Bi element can be muriate, nitrate, vitriol or carbonate; Said alkaline conditioner can be NaOH or KOH; Complexing agent can adopt disodium ethylene diamine tetraacetate (hereinafter to be referred as EDTA); Said reductive agent can adopt NaBH
4Or KBH
4
In above-mentioned preparation process, the stirring of mixed solution from step 1), is lasted till that always reaction finishes.Used reaction vessel can be Glass Containers or acidproof, alkaline-resisting, heat-stable plastic containers.
The present invention has developed novel Bi
2Te
3Nanocapsule, length-to-diameter ratio is significantly less than nanotube, and its particular structure is expected to improve Bi
2Te
3The semiconductor heat electrical property of nano material, and can be widely used in fields such as physics, chemistry, material, microelectronics.
Description of drawings
Fig. 1 is at 85 ℃ of following synthetic Bi
2Te
3The field emission scanning electron microscope of nanocapsule and transmission electron microscope photo;
Fig. 2 is at 55 ℃ of following synthetic Bi
2Te
3The transmission electron microscope of nanocapsule and high-resolution electron microscopy photo.
Embodiment
Below in conjunction with embodiment the present invention is done further to state in detail.
Embodiment 1
1) in the glass beaker of a 800ml capacity, adds the 200ml deionized water successively, 3.83g Te powder (about 30 mmoles, 99.99% purity are crossed 30 μ m sieve), 6.31g BiCl
3(about 20 mmoles, analytical pure), and mix liquid with the 120rpm rotating speed with magnetic stirrer.
2) interpolation 1g EDTA in beaker, and interpolation NaOH makes the pH value of solution value reach 12, and then adds 2g NaBH
4
3) be heated to solution temperature with the speed of 5 ℃/min and reach 85 ℃ and maintain this temperature.
4) during 85 ℃ of isothermal reactions, keep the 120rpm stirring velocity, and prevent that with plastics film covering beaker solvent from excessively volatilizing.
5) reaction stops heating after 6 hours, naturally cools to room temperature.Collect the Powdered reaction product in the beaker, clean repeatedly for several times with deionized water, dehydrated alcohol and acetone successively, get Bi after the room temperature vacuum-drying
2Te
3Nanocapsule.
Adopt IRIS Intrepid II type XSP plasma emission spectrometry, the result shows that the atomic percentage conc of institute's synthetic nanocapsule is: 40.2%Bi and 59.8%Te.Adopt SIRION-FEI type field emission scanning electron microscope and JEM-2010 type transmission electron microscope observation nanocapsule form, as shown in Figure 1, nanocapsule length is between 200～800nm, and diameter is between 50～160nm, and thickness of pipe is 8～10nm.Adopt Rigaku-D/MAX-2550PC type X ray polycrystalline diffractometer to analyze the nanocapsule crystalline structure, the result is single-phase Bi
2Te
3Structure.
Get 0.6g and adopt above-mentioned route synthetic Bi
2Te
3Nanocapsule, by 250 ℃, 50MPa, 30min vacuum hotpressing, the acquisition diameter is 10mm, the disk shape sample of the about 1.2mm of thickness.At room temperature measure electric property after the cutting, the thermoelectric coefficient absolute value is 2.1 * 10
-4V/K, resistivity is 2.5 * 10
-5Ω m has typical pyroelectric material performance feature.
Embodiment 2
1) in the glass beaker of a 800ml capacity, adds the 450ml deionized water successively, 0.765g Te powder (about 6 mmoles, 99.99% purity are crossed 30 μ m sieve), 1.58g Bi (NO
3)
3(about 4 mmoles, analytical pure), and mix liquid with the 100rpm rotating speed with magnetic stirrer.
2) be heated to solution temperature with the speed of 5 ℃/min and reach 55 ℃ and maintain this temperature.
3) interpolation 1.9g EDTA in beaker, and interpolation KOH makes the pH value of solution value reach 14, and then adds 2.3g KBH
4
4) during 55 ℃ of isothermal reactions, keep the 100rpm stirring velocity, and prevent that with plastics film covering beaker solvent from excessively volatilizing.
5) reaction stops heating after 100 hours, naturally cools to room temperature.Collect the Powdered reaction product in the beaker, clean repeatedly for several times with deionized water, dehydrated alcohol and acetone successively, get Bi after the room temperature vacuum-drying
2Te
3Nanocapsule.
Adopt IRIS Intrepid II type XSP plasma emission spectrometry, the result shows that the atomic percentage conc of institute's synthetic nanocapsule is: 39.9%Bi and 60.1%Te.Adopt JEM-2010 type transmission electron microscope and JEOL-4000EX type high resolution transmission electron microscopy to observe the nanocapsule form, as shown in Figure 2, nanocapsule length is between 300～1000nm, and diameter is between 80～200nm, and thickness of pipe is 5～8nm.Adopt Rigaku-D/MAX-2550PC type X ray polycrystalline diffractometer to analyze the nanocapsule crystalline structure, the result is single-phase Bi
2Te
3Structure.
Get 0.6g and adopt above-mentioned route synthetic Bi
2Te
3Nanocapsule, by 250 ℃, 50MPa, 30min vacuum hotpressing, the acquisition diameter is 10mm, the disk shape sample of the about 1.2mm of thickness.At room temperature measure electric property after the cutting, the thermoelectric coefficient absolute value is 1.4 * 10
-4V/K, resistivity is 9.2 * 10
-6Ω m has typical pyroelectric material performance feature.
Claims (5)
1. Bi
2Te
3Nanocapsule is characterized in that it is that L/D ratio is 2～5 seamless hollow capsules, and its component and atomic percentage conc are:
Bi 39.8～40.3％，Te 59.7～60.2％。
2. Bi according to claim 1
2Te
3Nanocapsule is characterized in that capsular diameter in 50～200 nanometers, wall thickness 5～20 nanometers, and length is in 200～1000 nanometers.
3. the described Bi of claim 1
2Te
3The preparation method of nanocapsule, its step is as follows:
1) compound of Bi element and the pure Te powder ratio according to Bi and Te atomic percentage conc is placed in the reaction vessel, add the deionized water of 80～850 times of Te weight, and mix;
2) in above-mentioned mixed solution, add 0.25～2.5 times the complexing agent that is equivalent to Te weight, add alkaline conditioner and make the pH value of solution value be in 12～14, add 0.5～3 times the reductive agent that is equivalent to Te weight;
3) be heated to the interior setting temperature of reaction of 55～85 ℃ of scopes, react after 6～100 hours, cool to room temperature stops to stir;
4) collect the interior solid reaction product of reaction vessel, behind cleaning-drying, obtain Bi
2Te
3The nanocapsule material.
4. Bi according to claim 3
2Te
3The preparation method of nanocapsule, the compound that it is characterized in that said Bi element is muriate, nitrate, vitriol or carbonate.
5. Bi according to claim 3
2Te
3The preparation method of nanocapsule is characterized in that said reductive agent is NaBH
4Or KBH
4
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410073387 CN1278941C (en) | 2004-12-08 | 2004-12-08 | Bi2Te3 nanometer capsule and preparation thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410073387 CN1278941C (en) | 2004-12-08 | 2004-12-08 | Bi2Te3 nanometer capsule and preparation thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1644509A CN1644509A (en) | 2005-07-27 |
| CN1278941C true CN1278941C (en) | 2006-10-11 |
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|---|---|---|---|
| CN 200410073387 Expired - Fee Related CN1278941C (en) | 2004-12-08 | 2004-12-08 | Bi2Te3 nanometer capsule and preparation thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2319082B1 (en) * | 2008-08-29 | 2017-11-15 | LG Chem, Ltd. | New compound semiconductor and producing method thereof, and solar cell and thermoelectric conversion element using the same |
| CN103738929A (en) * | 2013-09-03 | 2014-04-23 | 吉林化工学院 | Preparation of graded bismuth telluride micrometer structure with simple solvothermal method |
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Granted publication date: 20061011 Termination date: 20100108 |