CN101434455B - Method for preparing bismuth telluride nano-wire array by physical vapour deposition - Google Patents
Method for preparing bismuth telluride nano-wire array by physical vapour deposition Download PDFInfo
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- CN101434455B CN101434455B CN2008102269746A CN200810226974A CN101434455B CN 101434455 B CN101434455 B CN 101434455B CN 2008102269746 A CN2008102269746 A CN 2008102269746A CN 200810226974 A CN200810226974 A CN 200810226974A CN 101434455 B CN101434455 B CN 101434455B
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- bismuth telluride
- wire array
- telluride nano
- vacuum chamber
- glass substrate
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Abstract
The invention discloses a preparation method of a bismuth telluride nano-wire array by adopting a physical vapor deposition method. The method comprises the following steps: in a vacuum chamber, raw bismuth telluride is thermally evaporated and a membrane with bismuth telluride nano-wire array structure is deposited on the glass substrate by regulating the output electric current of the mains supply and the distance between the glass substrate and a tungsten boat. The whole deposition process is simple, the cost is low, and mass production is easy to be achieved; the obtained bismuth telluride nano-wire arrays are uniform in structure and the even distribution of nanophases is effectively ensured.
Description
Technical field
The present invention relates to a kind of preparation Tellurobismuthite (Bi
2Te
3) method of nano-wire array, more particularly say, be meant a kind of method that adopts physical vaporous deposition on glass substrate, to prepare bismuth telluride nano-wire array.
Background technology
Rowe is described in detail thermoelectric material in its " CRC Handbook of Thermoelectrics " that writes (being published by CRC Press1995) book.In present all thermoelectric materials, Bi
2Te
3The based semiconductor material is respectively to generally acknowledge best room temperature, middle warm area thermoelectric material at present, and they have been the industrial standards of current commercial thermo-electric device.At present the highest level in the world is the Bi of report such as R.Venkatasubramanian
2Te
3/ Sb
2Te
3Superstructure (ZT=2.4), but to make thermoelectric material can reach the refrigerating efficiency of traditional refrigeration (compressor) system, and the ZT value will reach more than 3 at least.The Theoretical Calculation of Hicks etc. proves that because the comparable quantum well of quantum wire further improves density of states(DOS), nano wire may have better thermoelectricity capability than superlattice.Though utilize vapor condensation, electrochemistry, technology such as high pressure injection can obtain the nano thread structure of certain thermoelectric material, and nano-material will obtain using, and just must prepare linear density up to 5 * 10
10/ cm
2And structure homogeneous nano-wire array.
At present the success of the report M.Stacy etc. of having only for preparing the bismuth telluride nano-wire array structure utilizes bismuth telluride nano-wire array about alumina formwork method synthetic minimum grain size 40nm in the world, be subjected to its pattern hole to fill complete the influence, its linear density can not reach the density requirements (5 * 10 that is applied to little refrigeration device fully
10/ cm
2), and the specification of quality of used template is very high, and the existing alumina formwork of commercially producing can not satisfy its production standard.
Summary of the invention
In order to solve Tellurobismuthite (Bi
2Te
3) problems that the nano-wire array thermoelectric material exists aspect synthetic, the present invention adopts physical vaporous deposition, the size by regulating the AC power outward current and the distance of glass substrate and tungsten boat, and in vacuum chamber, thermal evaporation Tellurobismuthite (Bi
2Te
3) raw material, directly on glass substrate, deposit film with bismuth telluride nano-wire array structure.Whole deposition process is simple, and is with low cost, is easy to large-scale production, and resulting bismuth telluride nano-wire array structure homogeneous has effectively guaranteed the uniform distribution of nanophase.
The technical scheme that Applied Physics vapour deposition process of the present invention prepares bismuth telluride nano-wire array is: the tungsten boat 2 of the Tellurobismuthite powder of particle diameter 5～20 μ m being put into the vacuum chamber 1 of vacuum plating unit, glass substrate 3 is positioned on the sample table 4, regulate glass substrate 3 and tungsten boat 2 apart from d=6～10cm;
Sealed vacuum chamber 1 stops to charge into 2～5min nitrogen in vacuum chamber 1 after, subsequently vacuum chamber 1 is vacuumized, and makes that vacuum tightness reaches 2.0 * 10 in the vacuum chamber 1
-3Pa～5.0 * 10
-5Pa;
On vacuum plating unit, set sedimentation rate 0.5～10nm/min, depositing time 5～12h;
Open AC power, regulate outward current 165A～175A; Beginning deposits preparation bismuth telluride nano-wire array film on glass substrate 3.
Bismuth telluride nano-wire diameter in the bismuth telluride nano-wire array film that makes is 18～100nm.
Description of drawings
Fig. 1 is the schematic diagram of vacuum coater of the present invention.
Fig. 2 is the XRD figure that adopts four embodiment product-bismuth telluride nano-wire arrays that the inventive method makes.
Fig. 3 is the stereoscan photograph of embodiment 1.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
The technical scheme that Applied Physics vapour deposition process of the present invention prepares bismuth telluride nano-wire array is: the tungsten boat 2 of the Tellurobismuthite powder of particle diameter 5～20 μ m being put into the vacuum chamber 1 of vacuum plating unit, glass substrate 3 is positioned on the sample table 4, regulate glass substrate 3 and tungsten boat 2 apart from d=6～10cm;
Sealed vacuum chamber 1 stops to charge into 2～5min nitrogen in vacuum chamber 1 after, subsequently vacuum chamber 1 is vacuumized, and makes that vacuum tightness reaches 2.0 * 10 in the vacuum chamber 1
-3Pa～5.0 * 10
-5Pa;
On vacuum plating unit, set sedimentation rate 0.5～10nm/min, depositing time 5～12h;
Open AC power, regulate outward current 165A～175A; Beginning deposits preparation bismuth telluride nano-wire array film on glass substrate 3.
Preparation finishes, and closes AC power, naturally cool to room temperature (22～28 ℃) after, take out the glass substrate 3 be shaped on the bismuth telluride nano-wire array film.
In preparation method of the present invention, the size, glass substrate 3 that will regulate the AC power outward current earlier and tungsten boat 2 apart from d, regulate the sedimentation rate of thermal evaporation sources (Tellurobismuthite raw material) in the vacuum chamber then, can control the linear density that is deposited on the bismuth telluride nano-wire array on the glass substrate 3, make the bismuth telluride nano-wire array structure homogeneous that physical vapor deposition makes, effectively guaranteed the uniform distribution of nanophase.
Embodiment 1:
The Tellurobismuthite simple substance powder of particle diameter 5～10 μ m is put into the tungsten boat 2 of the vacuum chamber 1 of vacuum plating unit, glass substrate 3 is positioned on the sample table 4, regulate glass substrate 3 and tungsten boat 2 apart from d=10cm;
Sealed vacuum chamber 1 stops (inflated with nitrogen can fill 2 times repeatedly) charge into 3min nitrogen in vacuum chamber 1 after, subsequently vacuum chamber 1 is vacuumized, and makes that vacuum tightness reaches 2.0 * 10 in the vacuum chamber 1
-4Pa;
On vacuum plating unit, set sedimentation rate 0.7nm/min, depositing time 8h;
Open AC power, regulate outward current 165A; Beginning physical vapor deposition on glass substrate 3 goes out the bismuth telluride nano-wire array film.
Preparation finishes, and closes AC power, naturally cool to room temperature after, take out the glass substrate 3 be shaped on the bismuth telluride nano-wire array film.
Adopt X-ray diffractometer that the bismuth telluride nano-wire array film that embodiment 1 makes is carried out material phase analysis, in " a " illustrates that the bismuth telluride nano-wire array film that makes is a Tellurobismuthite simple substance as shown in Figure 2.
The bismuth telluride nano-wire array film that above-mentioned physical vapor deposition makes is observed under scanning electronic microscope, and the nanowire diameter in the bismuth telluride nano-wire array film is 18nm, and stereoscan photograph as shown in Figure 3.
Embodiment 2:
The Tellurobismuthite powder of particle diameter 5～20 μ m is put into the tungsten boat 2 of the vacuum chamber 1 of vacuum plating unit, glass substrate 3 is positioned on the sample table 4, regulate glass substrate 3 and tungsten boat 2 apart from d=6cm;
Sealed vacuum chamber 1 stops to charge into 5min nitrogen in vacuum chamber 1 after, subsequently vacuum chamber 1 is vacuumized, and makes that vacuum tightness reaches 3.0 * 10 in the vacuum chamber 1
-4Pa;
On vacuum plating unit, set sedimentation rate 1.8nm/min, depositing time 5h;
Open AC power, regulate outward current 175A; Beginning deposits preparation bismuth telluride nano-wire array film on glass substrate 3.
Preparation finishes, and closes AC power, naturally cool to 28 ℃ after, take out the glass substrate 3 be shaped on the bismuth telluride nano-wire array film.
Adopt X-ray diffractometer that the bismuth telluride nano-wire array film that embodiment 2 makes is carried out material phase analysis, in " b " illustrates that the bismuth telluride nano-wire array film that makes is a Tellurobismuthite simple substance as shown in Figure 2.
The bismuth telluride nano-wire array film that embodiment 2 makes is observed under scanning electronic microscope, and the nanowire diameter in the bismuth telluride nano-wire array film is 30nm.
Embodiment 3:
The Tellurobismuthite powder of particle diameter 10～20 μ m is put into the tungsten boat 2 of the vacuum chamber 1 of vacuum plating unit, glass substrate 3 is positioned on the sample table 4, regulate glass substrate 3 and tungsten boat 2 apart from d=9cm;
Sealed vacuum chamber 1 stops to charge into 3min nitrogen in vacuum chamber 1 after, subsequently vacuum chamber 1 is vacuumized, and makes that vacuum tightness reaches 5.0 * 10 in the vacuum chamber 1
-5Pa;
On vacuum plating unit, set sedimentation rate 4nm/min, depositing time 6h;
Open AC power, regulate outward current 170A; Beginning deposits preparation bismuth telluride nano-wire array film on glass substrate 3.
Preparation finishes, and closes AC power, naturally cool to 22 ℃ after, take out the glass substrate 3 be shaped on the bismuth telluride nano-wire array film.
Adopt X-ray diffractometer that the bismuth telluride nano-wire array film that embodiment 3 makes is carried out material phase analysis, in " c " illustrates that the bismuth telluride nano-wire array film that makes is a Tellurobismuthite simple substance as shown in Figure 2.
The bismuth telluride nano-wire array film that embodiment 3 makes is observed under scanning electronic microscope, and the nanowire diameter in the bismuth telluride nano-wire array film is 50nm.
Embodiment 4:
The Tellurobismuthite powder of particle diameter 5～20 μ m is put into the tungsten boat 2 of the vacuum chamber 1 of vacuum plating unit, glass substrate 3 is positioned on the sample table 4, regulate glass substrate 3 and tungsten boat 2 apart from d=10cm;
Sealed vacuum chamber 1 stops to charge into 2min nitrogen in vacuum chamber 1 after, subsequently vacuum chamber 1 is vacuumized, and makes that vacuum tightness reaches 4.0 * 10 in the vacuum chamber 1
-4Pa;
On vacuum plating unit, set sedimentation rate 10nm/min, depositing time 12h;
Open AC power, regulate outward current 165A; Beginning deposits preparation bismuth telluride nano-wire array film on glass substrate 3.
Preparation finishes, and closes AC power, naturally cool to 25 ℃ after, take out the glass substrate 3 be shaped on the bismuth telluride nano-wire array film.
Adopt X-ray diffractometer that the bismuth telluride nano-wire array film that embodiment 4 makes is carried out material phase analysis, in " d " illustrates that the bismuth telluride nano-wire array film that makes is a Tellurobismuthite simple substance as shown in Figure 2.
The bismuth telluride nano-wire array film that embodiment 4 makes is observed under scanning electronic microscope, and the nanowire diameter in the bismuth telluride nano-wire array film is 100nm.
Claims (2)
1. method that adopts physical vaporous deposition to prepare bismuth telluride nano-wire array, it is characterized in that: the tungsten boat (2) of the Tellurobismuthite powder of particle diameter 5～20 μ m being put into the vacuum chamber (1) of vacuum plating unit, glass substrate (3) is positioned on the sample table (4), regulate glass substrate (3) and tungsten boat (2) apart from d=6～10cm; Sealed vacuum chamber (1) stops to charge into 2～5min nitrogen in vacuum chamber (1) after, subsequently vacuum chamber (1) is vacuumized, and makes the interior vacuum tightness of vacuum chamber (1) reach 2.0 * 10
-3Pa～5.0 * 10
-5Pa;
On vacuum plating unit, set sedimentation rate 0.5～10nm/min, depositing time 5～12h;
Open AC power, regulate outward current 165A～175A; Beginning is gone up deposition preparation bismuth telluride nano-wire array film at glass substrate (3);
Preparation finishes, and closes AC power, naturally cool to room temperature after, take out the glass substrate (3) be shaped on the bismuth telluride nano-wire array film.
2. employing physical vaporous deposition according to claim 1 prepares the method for bismuth telluride nano-wire array, it is characterized in that: the bismuth telluride nano-wire diameter in the bismuth telluride nano-wire array film that makes is 18～100nm.
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| CN101434455B true CN101434455B (en) | 2011-01-12 |
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| CN102330058B (en) * | 2011-09-20 | 2013-07-03 | 北京航空航天大学 | Method for preparing multi-grade antimonytelluride nano wire harness array by adopting physical vapor deposition |
| CN104841939B (en) * | 2015-04-27 | 2017-08-25 | 中国人民解放军装甲兵工程学院 | A kind of preparation method of highly exothermic self-propagating combustion composite nano-powder |
| CN109950138B (en) * | 2019-04-11 | 2020-11-13 | 广东工业大学 | Nano-pillar array heterojunction and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4036665A (en) * | 1974-07-16 | 1977-07-19 | Nuclear Battery Corporation | Thermopile for microwatt thermoelectric generator |
| CN1948545A (en) * | 2006-09-15 | 2007-04-18 | 华东理工大学 | Single target sputter method for preparing bismuth telluride thin film using powder target material |
| CN101168836A (en) * | 2006-10-25 | 2008-04-30 | 国家纳米技术与工程研究院 | Method for preparing bismuth telluride alloy thin film by employing cosputtering sedimentation method |
-
2008
- 2008-12-01 CN CN2008102269746A patent/CN101434455B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4036665A (en) * | 1974-07-16 | 1977-07-19 | Nuclear Battery Corporation | Thermopile for microwatt thermoelectric generator |
| CN1948545A (en) * | 2006-09-15 | 2007-04-18 | 华东理工大学 | Single target sputter method for preparing bismuth telluride thin film using powder target material |
| CN101168836A (en) * | 2006-10-25 | 2008-04-30 | 国家纳米技术与工程研究院 | Method for preparing bismuth telluride alloy thin film by employing cosputtering sedimentation method |
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