CN1234599C - Bi2Te3 base compound nano line and its preparing method - Google Patents
Bi2Te3 base compound nano line and its preparing method Download PDFInfo
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- CN1234599C CN1234599C CN 200310122821 CN200310122821A CN1234599C CN 1234599 C CN1234599 C CN 1234599C CN 200310122821 CN200310122821 CN 200310122821 CN 200310122821 A CN200310122821 A CN 200310122821A CN 1234599 C CN1234599 C CN 1234599C
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 7
- 229910002899 Bi2Te3 Inorganic materials 0.000 title abstract 4
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 239000002070 nanowire Substances 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- 230000002829 reductive effect Effects 0.000 claims description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 claims description 4
- 229910052711 selenium Inorganic materials 0.000 claims description 4
- 229910052714 tellurium Inorganic materials 0.000 claims description 4
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 3
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 3
- 229960004756 ethanol Drugs 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 3
- 229940038773 trisodium citrate Drugs 0.000 claims description 3
- 238000010792 warming Methods 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
- 229910052728 basic metal Inorganic materials 0.000 claims description 2
- 150000003818 basic metals Chemical class 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910052794 bromium Inorganic materials 0.000 abstract description 2
- 229910052740 iodine Inorganic materials 0.000 abstract description 2
- 229910052745 lead Inorganic materials 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000011669 selenium Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 230000005260 alpha ray Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000005492 condensed matter physics Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a Bi2Te3 base compound nanometer line which comprises the following constituents by the atomic percentage of 95 to 100% of p-shaped or n-shaped Bi2Te3 group compounds formed from Sb and/ or Bi elements, and Te elements according to the atomic ratio of 1.9 to 2.1: 2.9 to 3.1, and 0 to 5% of one or multiple kinds of doping atomic elements Sn, Pb, I, Br, Al or Li. The preparation adopts a hydrothermal method or a solvent heating method. The Bi2Te3 base compound nanometer line has the advantages of simple and convenient technical equipment, low cost, low synthesis temperature, short period, high product purity, good maneuverability, etc.
Description
Technical field
The present invention relates to one dimension semiconductor thermoelectric material and preparation method thereof.Specifically, be about Bi
2Te
3Based compound nano wire and preparation method thereof.
Background technology
Along with rapid development of science and technology, as one of member of nano material family, nano wire has important application prospects because of it at aspects such as Jie's sight field, nano-device development, magneticsubstance, electronic material, optical material and functional composite materials, cause Condensed Matter Physics circle, chemical boundary and the scientist's of material supply section educational circles extensive interest, become a focus of investigation of materials in recent years.
Bi
2Te
3It is the semiconductor material of a kind of narrow band gap (energy gap is 0.13ev).Bi
2Te
3Based compound has high conductivity simultaneously owing to it and lower thermal conductivity becomes the best room temperature type thermoelectric material of present performance, but its thermoelectricity capability still awaits further raising.Bi
2Te
3Be the compound that is made of V, VI family element, preferably in the material, it is the stable binary compound of molecular weight maximum in chemical stability.Bi
2Te
3Have the accurate laminate structure of hexahedron, on same one deck of this structure, have identical atomic species.Arranging by " Te-Bi-Te-Bi-Te-" mode between atomic shell, is the Van der Waals force combination between adjacent two Te layers.Theoretical investigation shows, the unique microstructures of this kind nano wire may produce unique physics, chemical property, thereby makes this kind material possess special transport property and can be used for preparing high performance thermoelectric material; In addition, Bi
2Te
3The based compound nano wire also might obtain other application in fields such as material, physics, chemistry, electronics.
Bi
2Te
3Electrochemical process is adopted in the preparation of based compound nano wire usually, and the equipment of required usefulness and technology are all comparatively complicated, and usually need make preparation cost improve greatly by growth templates.
Summary of the invention
The purpose of this invention is to provide a kind of Bi
2Te
3Based compound nano wire and preparation method thereof.
Bi of the present invention
2Te
3The based compound nano wire, its component and content are as follows: by Sb or/and Bi element and Se or/and the Te element is p type or the n type Bi that 1.9～2.1: 2.9～3.1 ratio forms in atomic ratio
2Te
3Based compound accounts for 95～100% of material total atom per-cent;
Among doped element atom Sn, Pb, I, Br, Al or the Li etc. one or more account for 0～5% of material total atom per-cent.
Bi
2Te
3The geometric properties of based compound nano wire is: diameter 5～150nm, length 50nm～50 μ m.
Bi of the present invention
2Te
3The preparation method of based compound nano wire is to adopt hydro-thermal or solvent thermal process, may further comprise the steps:
1) with Sb or/and Bi element and Se or/and the simple substance of the simple substance of Te element or compound and/or doped element or compound, according to the determined mixed of final product chemical ingredients in water or organic solvent;
2) above-mentioned mixed solution is placed in the reaction vessel of autoclave, add the reductive agent of q.s, then sealing immediately;
3) certain temperature and 6～50 hours postcooling of insulation reaction that reaction vessel is warming up in 100～300 ℃ of scopes arrives room temperature;
4) collect the interior solid reaction product of reaction vessel, repeatedly clean after drying, obtain material of the present invention through deionized water, organic solvent and/or dilute acid soln.
For controls reaction speed with generate the particle diameter of product, in step 2) in can add an amount of alkaline conditioner and complexing agent.Said alkaline conditioner can be NaOH, KOH etc., and said complexing agent can be EDTA disodium salt, citric acid, Trisodium Citrate or ethylenediamine tetraacetic acid (EDTA) etc.
Above-mentioned steps 1) said Sb in or/and Bi element and Se or/and the compound of the compound of Te element and doped element can be muriate, oxide compound, nitrate, vitriol or carbonate etc.Wherein Sb and Bi are the relations that mutually replaces, and Se and Te are the relations that replaces mutually, its substitute proportion separately be any than.
Above-mentioned steps 1) said organic solvent can be ethanol, acetone, pyridine, quadrol, benzene or toluene etc. in.
Above-mentioned steps 2) said reductive agent can adopt NaBH in
4, KBH
4Etc. alkali-metal hydroborates or basic metal such as Na, K.Said organic solvent can be ethanol, acetone, tetracol phenixin etc. in the step 4).
Bi of the present invention
2Te
3The based compound nano wire, hydro-thermal or solvent thermal process are adopted in its preparation, have advantages such as processing unit is easy, cost is low, synthesis temperature is low, the cycle is short, product purity is high, controllability is good.The Bi that makes by present method
2Te
3The based compound nanowire diameter is at 5～150nm, and length 50nm～50 μ m can be used for preparing high performance thermoelectric material.
Embodiment
Below in conjunction with embodiment the present invention is done further to state in detail.
Embodiment 1
1) with analytical pure BiCl
3, the tellurium powder (＞99.5wt%), in Bi: be mixed in the deionized water after 2: 3 ratio of the Te atomic ratio batching, and add alkaline conditioner NaOH.
2) mixed solution for preparing is placed the reaction vessel (the filling degree is 80%) of autoclave (WDF-0.25 type), and in solution, add reductive agent NaBH
4, sealing immediately then;
3) with reaction vessel heat temperature raising to 180 ℃ and be incubated 12 hours.
4) reaction naturally cools to room temperature after finishing, and collects the Powdered reaction product at the bottom of the still, clean for several times repeatedly with deionized water, dehydrated alcohol and acetone successively after, with powder at 100 ℃ of following vacuum-drying 6h, must Bi
2Te
3Nano wire.
Embodiment 2
1) raw material: with analytical pure BiNO
3With analytical pure TeO
2In Bi: the Te atomic ratio is 2: 3 a ratio batching, and is that 3% ratio is added analytical pure SnCl in Sn atom content per-cent
22H
2O.
2) with the above-mentioned raw materials mixed dissolution in dehydrated alcohol, and add a small amount of complexing agent EDTA disodium salt and a certain amount of KOH.
3) above-mentioned mixed solution is placed in the reaction vessel of autoclave, add the reductive agent KBH of capacity
4, sealing immediately then;
4) reaction vessel is warming up to 150 ℃, and is incubated 24 hours and reacts, then cool to room temperature;
5, collect the interior solid reaction product of reactor, behind the repetitive scrubbing of deionized water, dehydrated alcohol, acetone and other organic solvent,, obtain Bi in 100 ℃ of following vacuum-dryings 6 hours
2Te
3Base nano-wire.
Embodiment 3
1) with analytical pure BiCO
3, the tellurium powder, selenium powder is in Bi: Se: be mixed in the quadrol after 2: 0.5: 2.5 ratio of the Te atomic percent batching, and add capacity KOH and a small amount of Trisodium Citrate.
2) mixed solution for preparing is placed the reaction vessel (the filling degree is 80%) of autoclave (WDF-0.25 type), and in solution, add the reductive agent metal Na, sealing immediately then;
3) with reaction vessel heat temperature raising to 120 ℃ and be incubated 48 hours.
4) reaction naturally cools to room temperature after finishing, and collects the Powdered reaction product at the bottom of the still, clean several repeatedly with deionized water, dehydrated alcohol and acetone successively after, powder at 100 ℃ of following vacuum-drying 6h, is obtained Bi
2Se
0.5Te
2.5Nano wire.
Adopt Rigaku-D/MAX-2550PC type X ray polycrystalline diffractometer (CuK
αRay, wavelength X=0.154056nm) carry out composition and structural analysis to the product of above-mentioned 3 embodiment respectively, show that the product of gained is respectively Bi
2Te
3, Bi
2Te
3And Bi
2Se
0.5Te
2.5Adopt JEM-2010 (HR) type transmission electron microscope to observe the granular size and the microscopic appearance of above-mentioned product respectively, acceleration voltage is 200KV.The result shows that 3 products all contain length at 1 μ m～50 μ m, and diameter is at the nano wire of 20～100nm.
Claims (5)
1. Bi
2Te
3The based compound nano wire is characterized in that its component and content are as follows:
Be 1.9～2.1: 2.9～3.1 in atomic ratio or be p type or the n type Bi that 2: 0.5: 2.5 ratio forms in atomic ratio by Bi element and Te element by Bi element and Se and Te element
2Te
3Based compound accounts for 95～100% of material total atom per-cent; Doped element atom Sn accounts for 0～5% of material total atom per-cent; The length of nano wire is 1 μ m～50 μ m, and diameter is 20～100nm.
2. the described Bi of claim 1
2Te
3The preparation method of based compound nano wire is characterized in that adopting hydro-thermal or solvent thermal process, may further comprise the steps:
1) with the simple substance or the compound of Bi element and Te element, the perhaps simple substance or the compound of Bi element and Se and Te element, add or do not add simple substance or the compound of doped element Sn, according to the described mixed of claim 1 in solvent, solvent is water or is selected from dehydrated alcohol or the organic solvent of quadrol, when solvent is organic solvent, add complexing agent EDTA disodium salt, citric acid, Trisodium Citrate or ethylenediamine tetraacetic acid (EDTA);
2) above-mentioned mixed solution is placed in the reaction vessel of autoclave, add alkaline conditioner and reductive agent, then sealing immediately;
3) reaction vessel is warming up to certain temperature in 100～300 ℃ of scopes, and 6～50 hours postcooling of insulation reaction are to room temperature;
4) collect the interior solid reaction product of reaction vessel, repeatedly clean after drying, obtain Bi through deionized water, ethanol and acetone
2Te
3The based compound nano wire.
3. Bi according to claim 2
2Te
3The preparation method of based compound nano wire is characterized in that said alkaline conditioner is NaOH, KOH.
4. Bi according to claim 2
2Te
3The preparation method of based compound nano wire is characterized in that said Bi element and the compound of Se and Te element and the compound of doped element in the step 1), is muriate, oxide compound, nitrate, vitriol or carbonate.
5. Bi according to claim 2
2Te
3The preparation method of based compound nano wire is characterized in that step 2) in said reductive agent be NaBH
4, KBH
4Or metal Na, K basic metal.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310122821 CN1234599C (en) | 2003-12-21 | 2003-12-21 | Bi2Te3 base compound nano line and its preparing method |
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|---|---|---|---|
| CN 200310122821 CN1234599C (en) | 2003-12-21 | 2003-12-21 | Bi2Te3 base compound nano line and its preparing method |
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| Publication Number | Publication Date |
|---|---|
| CN1554574A CN1554574A (en) | 2004-12-15 |
| CN1234599C true CN1234599C (en) | 2006-01-04 |
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|---|---|---|---|
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857971B (en) * | 2009-04-07 | 2013-04-03 | 中国科学院合肥物质科学研究院 | Bismuth/bismuth-antimony extensional superlattice nanowire and preparation method thereof |
| CN107611247A (en) * | 2016-07-11 | 2018-01-19 | 林宗宏 | Growth tellurium and tellurides nano-wire array are in the method on conductive base and tellurium and tellurides nano wire thermoelectric device |
| CN108163820B (en) * | 2018-03-09 | 2021-10-26 | 太原理工大学 | Method for preparing tin diselenide nanowire at low temperature |
| CN113697780B (en) * | 2021-10-20 | 2022-12-16 | 哈尔滨工业大学 | Preparation method of pH-regulated bismuth telluride nanowire |
| CN115490212B (en) * | 2022-10-13 | 2023-07-14 | 中国科学技术大学 | Near-infrared active periodic plasma heterojunction photo-anode material and preparation method thereof |
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