CN100585032C - Method for preparing lead telluride nano-wire - Google Patents
Method for preparing lead telluride nano-wire Download PDFInfo
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- CN100585032C CN100585032C CN200710134454A CN200710134454A CN100585032C CN 100585032 C CN100585032 C CN 100585032C CN 200710134454 A CN200710134454 A CN 200710134454A CN 200710134454 A CN200710134454 A CN 200710134454A CN 100585032 C CN100585032 C CN 100585032C
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- 239000002070 nanowire Substances 0.000 title claims abstract description 40
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 11
- 229910002665 PbTe Inorganic materials 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000005352 clarification Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 5
- 230000003252 repetitive effect Effects 0.000 claims description 5
- 238000005201 scrubbing Methods 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 2
- 238000007667 floating Methods 0.000 claims description 2
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- VOADVZVYWFSHSM-UHFFFAOYSA-L sodium tellurite Chemical compound [Na+].[Na+].[O-][Te]([O-])=O VOADVZVYWFSHSM-UHFFFAOYSA-L 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000013459 approach Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000005057 refrigeration Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 3
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 230000005619 thermoelectricity Effects 0.000 description 3
- -1 PbTe compound Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- UPLPHRJJTCUQAY-WIRWPRASSA-N 2,3-thioepoxy madol Chemical compound C([C@@H]1CC2)[C@@H]3S[C@@H]3C[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@](C)(O)[C@@]2(C)CC1 UPLPHRJJTCUQAY-WIRWPRASSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000009415 formwork Methods 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- JEHCHYAKAXDFKV-UHFFFAOYSA-J lead tetraacetate Chemical compound CC(=O)O[Pb](OC(C)=O)(OC(C)=O)OC(C)=O JEHCHYAKAXDFKV-UHFFFAOYSA-J 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 230000005676 thermoelectric effect Effects 0.000 description 1
- 230000004304 visual acuity Effects 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method of a lead telluride nano-wire, belonging to the technical field of thermoelectric semiconductor materials, which comprises the following steps: first, prepare a Te nano-wire with the diameter of 3-20 nanometers; second, add Pb (NO3)2 with the same molar ratio with Na2TeO3 to the solution of Te nano-wire, seal in an autoclave at 90-100 DEG C to react for 9-12 hours, and get PbTe nano-wire with uniform diameter and the length of 1 micron to 100 microns. The preparation method of a lead telluride nano-wire has the advantages that: PbTe nano-wire with uniform diameter and average length smaller than the exciton Bohr radius can be produced through controlling the growth temperature, the lead salt concentration and the reaction time; the PbTe nano-wire prepared with the method can be used as an ideal scientific research material, laying good basis for preparing and realizing thermoelectric nanometer devices in the future.
Description
Technical field
The present invention relates to the semiconductor thermoelectric preparation method of nano material.Specifically, be preparation method about the thermoelectric lead telluride nano-wire of one dimension.
Background technology
1823, Thomas Seebeck found thermoelectric effect first, thus the human application that has begun thermoelectric material.Thermoelectric material is a kind of functional materials that heat energy and electric energy can be changed mutually.It is pollution-free for making, the motion of noiselessness, nothing machinery, do not have wearing and tearing, high efficiency generating and refrigeration equipment wide prospect is provided.It is being widely used aspect remote navigation system, thermoelectric refrigerator, pyroelectric infrared detector, the superelectron instrument, and has the potential significant application value aspect the industrial exhaust heat waste-heat power generation.Especially in recent years, along with environment and energy problem become increasingly conspicuous, and human extensive concern to sustainable development, development of new energy substitution fossil oil material has caused the great attention of countries in the world scientific circles and engineering circle.Because freonll-11 generally is familiar with by people to the havoc effect of ozonosphere, make the target that pollution-free muting refrigerator has become Refrigeration Technique to pursue.Simultaneously, along with the development of computer technology, spationautics and superconductor technology and microelectronics, press for small-sized, static refrigeration and the hard-wired long-life refrigeration plant of energy.Therefore, the thermoelectric material that is suitable for making this device causes people's keen interest again.But the conversion efficiency of thermoelectric of more sophisticated a few class thermoelectric materials is lower, except that as being unsuitable for general application the special purpose.In recent years, because thermoelectric theoretical development and to the deepening continuously of thermoelectric material experimental study, the research of thermoelectric material had had bigger progress and had demonstrated application prospects.
PbTe has a cube phase crystalline structure, has metallic bond of half and the covalent linkage feature of half.Its fusing point higher (1095K), energy gap is big (about 0.3eV during 300K), it is chemical stability macromolecule compound preferably, pyroelecthc properties has isotropy completely, be often used as the thermoelectric material that uses in the 300-900K scope, advanced body phase thermoelectric material has maximum value ZT-0.7 when 700K.Theoretical prediction in recent years and experimental observation have confirmed that all nanometer can greatly improve the thermoelectricity capability of material, and especially one-dimensional nano line more can improve the thermoelectricity capability of material than the quantum well of two dimension.
The existing method for preparing thermoelectric nano-wire mainly is the alumina formwork method, although make can access in this way size evenly, the nano-material of length controlled, can not be suitable for suitability for industrialized production but output is too low, and at every turn when template removes nano wire owing to use strong acid that nano wire is damaged.And the nano wire that usually generates is polycrystalline, and this has seriously influenced the thermoelectricity capability of material.
Summary of the invention
The purpose of this invention is to provide simple, the preparation method that can mass production PbTe nano wire of a kind of low cost, less energy-consumption, technology.
The inventive method wants lead telluride as follows hereinafter referred to as the component concentration of (PbTe) compound nano line:
The mol ratio of final nano wire two component Pb that generate and Te was near 1: 1, and tellurium is excessive a little, and therefore the nano wire that generates is the p N-type semiconductorN.
The geometric properties of PbTe nano wire is: diameter is the 20-40 nanometer, and length is several microns and arrives above 100 microns.
The preparation method of PbTe nano wire of the present invention is to adopt two one-step hydrothermals, may further comprise the steps:
1) synthetic Te nano wire: with 98% sodium tellurite Na of the polyvinylpyrrolidone PVP k30 of 0.18-0.6 gram and 0.1085-0.3616 gram
2TeO
3Put into the autoclave of volume 30-100 milliliter, add 15-50 milliliter redistilled water more therein, at room temperature stir and make its formation homogeneous solution.25% the ammoniacal liquor that in autoclave, adds 85% hydrazine hydrate of 0.9-3 milliliter and 1.8-6 milliliter then.After final solution becomes clarification, add redistilled water and liquor capacity is reached behind the autoclave volumetrical 80% its sealing placed 180 ℃ baking oven 6-24 hour.At last autoclave is naturally cooled to room temperature and obtain the Te nano wire;
2) synthetic PbTe nano wire: with the lead nitrate Pb (NO of 0.161-0.536 gram 99%
3)
2Join in the solution of the Te nano wire that generates by the first step, make Pb (NO
3)
2With initial Na
2TeO
3Mol ratio be 1: 1, after stirring 9-12 hour under 5-10 ℃, the autoclave sealing was put into baking oven at 90-100 ℃ of following 9-12 hour, question response finishes, floating matter is used redistilled water and ethanol repetitive scrubbing with the acetone deposition after 12 hours, under 40-80 ℃ vacuum dry 6-12 hour then, obtain the PbTe nano-material.
It is the reactor of liner that above-mentioned autoclave generally adopts with the tetrafluoroethylene.
Above-mentioned steps 2) said Pb (NO in
3)
2Also can be plumbic acetate Pb (CH
3COO)
2
Advantages such as two step hydrothermal synthesis methods of PbTe compound nano line of the present invention have that technology is easy, cost is low, synthesis temperature is low, and product purity height, size are even.The PbTe compound nano linear diameter that is obtained by present method is in the 20-40 nanometer, length be several micron to 100 micron dimensions, and size is even, and is smooth, having the diameter less than its exciton Bohr radius, is the good material of the thermoelectric transport property of the single thermoelectric PbTe nano wire of research.
Description of drawings
Fig. 1 is the FESEM photo (including the high FESEM photo of resolving power) of PbTe nano wire.
Fig. 2 is TEM figure and high resolution TEM figure (lower left corner) and electron-diffraction diagram (upper right corner), (c) diameter Distribution figure and (d) composition analysis of the low TEM of the resolution figure of PbTe nano wire (a), (b) single nano-wire.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
1. raw material: analytically pure Pb (NO
3)
2, Na
2TeO
3
2. with 0.1808 gram Na
2TeO
3(K30, MW=40000) placing volume is 50 milliliters of autoclaves, adds the stirring of 25ml redistilled water and makes it to become clarification with 0.3 gram PVP.
3. will drip 1.5 milliliters hydrazine hydrate and 3 milliliters ammoniacal liquor in the above-mentioned solution, and continue stirring and make it to become clarification.
4. add the 10.5ml redistilled water, place 180 ℃ in baking oven to take out after following 24 hours the autoclave sealing and make it naturally cool to room temperature.
5. Pb (the NO that in above-mentioned reaction soln, adds 0.268 gram
3)
2, stirred down in the baking oven that was placed on 100 ℃ in 12 hours 12 hours in 5 ℃.Use redistilled water and ethanol repetitive scrubbing with adding in the reacted system after acetone deposits the black suspension thing, drying is 12 hours under 80 ℃, obtains target product.
The FESEM photo of the PbTe nano wire of preparation can see that by the SEM figure lower left corner enlarged view PbTe wire diameter distribution is very even as shown in Figure 1.The TEM of PbTe nano wire, high resolution TEM photo, electron diffraction and size distribution plot and composition analysis are as shown in Figure 2.Fig. 2 (b) upper right corner is its image K-M, finds out that from this figure the PbTe nano wire is a cube phase monocrystal structure.By Fig. 2 (b) lower left corner high resolution TEM photo as can be seen the PbTe nano wire along (100) oriented growth.By diameter Distribution figure (Fig. 2 (c)) mean diameter 30 nanometers of reaction product as can be seen.By composition analysis figure (Fig. 2 (d)) mol ratio Te: Pb=51.15 as can be seen: 48.85, the mole metering that approaches PbTe in the experimental error allowed band was than 1: 1.
Embodiment 2
1. raw material: analytically pure Pb (NO
3)
2, Na
2TeO
3
2. with 0.3616 gram Na
2TeO
3(K30, MW=40000) placing volume is 100 milliliters of autoclaves, adds 50 milliliters of redistilled waters stirrings and makes it to become clarification with 0.6 gram PVP.
3. will drip 3 milliliters hydrazine hydrate and 6 milliliters ammoniacal liquor in the above-mentioned solution, and continue stirring and make it to become clarification.
4. add the 21ml redistilled water, place 180 ℃ in baking oven to take out after following 24 hours the autoclave sealing and make it naturally cool to room temperature.
5. Pb (the NO that in above-mentioned reaction soln, adds 0.536 gram
3)
2, stirred down in the baking oven that was placed on 100 ℃ in 12 hours 12 hours in 5 ℃.Use redistilled water and ethanol repetitive scrubbing with adding in the reacted system after acetone deposits the black suspension thing, drying is 12 hours under 60 ℃, obtains target product.
The gained result approaches example 1 gained result.
Embodiment 3
1. raw material: analytically pure Pb (NO
3)
2, Na
2TeO
3
2. with 0.1085 gram Na
2TeO
3(K30, MW=40000) placing volume is 30 milliliters autoclave, adds 15 milliliters of redistilled waters stirrings and makes it to become clarification with 0.18 gram PVP.
3. will drip 0.9 milliliter hydrazine hydrate and 1.8 milliliters ammoniacal liquor in the above-mentioned solution, and continue stirring and make it to become clarification.
4. add the 6.3ml redistilled water, place 180 ℃ in baking oven to take out after following 24 hours the autoclave sealing and make it naturally cool to room temperature.
5. Pb (the NO that in above-mentioned reaction soln, adds 0.161 gram
3)
2, stirred down in the baking oven that was placed on 100 ℃ in 12 hours 12 hours in 5 ℃.Use redistilled water and ethanol repetitive scrubbing with adding in the reacted system after acetone deposits the black suspension thing, drying is 12 hours under 60 ℃, obtains target product.
The gained result approaches example 1 gained result.
Embodiment 4
Step is with example 1, and difference is that the 4th step was to place 180 ℃ in baking oven to take out after following 18 hours the autoclave sealing to make it naturally cool to room temperature.The gained result approaches example 1 gained result.
Embodiment 5
Step is with example 1, and difference is that the step 1) raw material is Pb (CH
3COO)
2, the mol ratio of reaction does not become, and temperature of reaction also is 100 ℃, and the PbTe nanowire size of preparation distributes and approaches example 1 gained result.
Claims (2)
1. method for preparing lead telluride nano-wire is characterized in that:
1) synthetic Te nano wire: with 98% sodium tellurite Na of the polyvinylpyrrolidone PVP k30 of 0.18-0.6 gram and 0.1085-0.3616 gram
2TeO
3Put into the autoclave of volume 30-100 milliliter, add 15-50 milliliter redistilled water more therein, at room temperature stirring makes it form uniform solution, 25% the ammoniacal liquor that in autoclave, adds 85% hydrazine hydrate of 0.9-3 milliliter and 1.8-6 milliliter then, after final solution becomes clarification, add redistilled water and liquor capacity is reached behind the autoclave volumetrical 80% its sealing placed 180 ℃ baking oven 6-24 hour, at last autoclave is naturally cooled to room temperature and can obtain the Te nano wire;
2) synthetic PbTe nano wire: with the lead nitrate Pb (NO of 0.161-0.536 gram 99%
3)
2Join in the solution of the Te nano wire that generates by the first step, make Pb (NO
3)
2With initial Na
2TeO
3Mol ratio kept 1: 1, after stirring 9-12 hour under 5-10 ℃, the autoclave sealing was put into baking oven at 90-100 ℃ of following 9-12 hour, question response finishes, floating matter is used redistilled water and ethanol repetitive scrubbing with the acetone deposition after 12 hours, under 40-80 ℃ vacuum dry 6-12 hour then, obtain the lead telluride nano-wire material.
2. method for preparing lead telluride nano-wire as claimed in claim 1 is characterized in that, described lead telluride nano-wire diameter is the 20-40 nanometer, and length is that several microns are to 100 microns.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602496B (en) * | 2009-07-07 | 2011-05-25 | 同济大学 | Synchronic preparation method of lead telluride thin film and nano powder |
| CN104993042A (en) * | 2015-05-27 | 2015-10-21 | 哈尔滨工业大学 | Preparation method of PbTe-SrTe microcrystal thermoelectric materials |
| CN105819412A (en) * | 2016-03-16 | 2016-08-03 | 浙江理工大学 | Preparation method of bud shape nano tellurium oxide |
| CN108217611B (en) * | 2017-12-29 | 2019-03-29 | 北京航空航天大学 | A kind of preparation method of high natrium doping lead telluride |
| CN108190847B (en) * | 2018-02-14 | 2019-11-22 | 中国科学技术大学 | A kind of preparation method of telluride indium nano wire |
| CN109166958B (en) * | 2018-09-05 | 2021-11-12 | 河南工程学院 | P-n type lead telluride/polypyrrole double-layer thermoelectric thin film material and preparation method thereof |
| CN109148904A (en) * | 2018-09-20 | 2019-01-04 | 宁波高新区诠宝绶新材料科技有限公司 | A kind of preparation method of proton exchange membrane direct methanoic acid fuel cell catalyst |
| CN115058766B (en) * | 2022-06-08 | 2023-06-06 | 中国科学院重庆绿色智能技术研究院 | Lead telluride nanowire film and preparation method and application thereof |
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| CN1136092A (en) * | 1996-04-11 | 1996-11-20 | 中国科学院上海技术物理研究所 | Manufacture of lead telluride with high tellurium content |
| CN1384047A (en) * | 2002-06-07 | 2002-12-11 | 清华大学 | Synthesis of several metal selenides and tellurides as semiconductor material |
| CN1384048A (en) * | 2002-06-21 | 2002-12-11 | 清华大学 | Nano level metal telluride preparing process |
-
2007
- 2007-10-23 CN CN200710134454A patent/CN100585032C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1136092A (en) * | 1996-04-11 | 1996-11-20 | 中国科学院上海技术物理研究所 | Manufacture of lead telluride with high tellurium content |
| CN1384047A (en) * | 2002-06-07 | 2002-12-11 | 清华大学 | Synthesis of several metal selenides and tellurides as semiconductor material |
| CN1384048A (en) * | 2002-06-21 | 2002-12-11 | 清华大学 | Nano level metal telluride preparing process |
Non-Patent Citations (2)
| Title |
|---|
| 富碲碲化铅薄膜的晶体结构、表面形貌、元素深度分布和中红外光学常数. 李斌，张素英.红外与毫米波学报，第24卷第1期. 2005 |
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