CN101435067A - Preparation of tellurium nano-wire array based on physical vapour deposition - Google Patents
Preparation of tellurium nano-wire array based on physical vapour deposition Download PDFInfo
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- CN101435067A CN101435067A CNA2008102269750A CN200810226975A CN101435067A CN 101435067 A CN101435067 A CN 101435067A CN A2008102269750 A CNA2008102269750 A CN A2008102269750A CN 200810226975 A CN200810226975 A CN 200810226975A CN 101435067 A CN101435067 A CN 101435067A
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- wire array
- tellurium nano
- glass substrate
- vacuum chamber
- tellurium
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Abstract
The invention discloses a preparation method of tellurium nano wire array based on physical vapor deposition. By adjusting the magnitude of current output by alternative power supply and the distance of glass substrate and tungsten boat, a thin film with tellurium nano wire array structure is directly deposited on the glass substrate by thermal evaporation of tellurium material in a vacuum chamber; the whole deposition technique has simple process, low cost and easy scale production; and the obtained tellurium nano wire array has uniform structure, thus effectively guaranteeing uniform distribution of nanophase.
Description
Technical field
The present invention relates to a kind of method for preparing tellurium nano-wire array, more particularly say, be meant a kind of method that adopts physical vaporous deposition on glass substrate, to prepare tellurium nano-wire array.
Background technology
By the certain way forming array system of lining up, is the forward position and the focus of current nano material and nanostructure research with the semi-conductor monodimension nanometer material, and it is the material foundation of nano structure device design of future generation.Tellurium (Te) is a low energy gap width semi-conductor; produce many functional materialss such as thermoelectric material especially; piezoelectric; the presoma of light-guide material etc., thus its oldered array system construct for the mass-producing functional device for example the development tool of scan-probe, field emission device, transmitter etc. with the meaning of particularly important.
At present the tellurium array structure that utilizes vapor phase process to prepare of report is the nanometer rod of the tellurium prepared in the nanotube of preparation tellurium of people such as Shashwati Sen and Paritosh Mohanty in the world, the diameter of rod is more than 100nm, and its linear density is being far smaller than 5 * 10
10/ cm
2, and also there is very big shortcoming in the regularity of nanometer rod, and big area realizes that the nano wire high standardization still faces huge challenge.
Summary of the invention
In order to solve the tellurium nano-wire array thermoelectric material in the problems that exist aspect synthesizing, the present invention adopts physical vaporous deposition, by the size of adjusting AC power outward current and the distance of glass substrate and tungsten boat, in vacuum chamber, by thermal evaporation tellurium raw material, directly on glass substrate, deposit film with tellurium nano-wire array structure.Whole deposition process is simple, and is with low cost, is easy to large-scale production, and resulting tellurium 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 tellurium nano-wire array is: the tungsten boat 2 of the telloy 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 4～16nm/min, depositing time 5～12h;
Open AC power, regulate outward current 165A～175A; Beginning deposits preparation tellurium nano-wire array film on glass substrate 3.
Tellurium nano-wire diameter in the tellurium nano-wire array film that makes is 20～115nm.
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-tellurium 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 tellurium nano-wire array is: the tungsten boat 2 of the telloy 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 4～16nm/min, depositing time 5～12h;
Open AC power, regulate outward current 165A～175A; Beginning deposits preparation tellurium 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 tellurium 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 (tellurium raw material) in the vacuum chamber then, can control the linear density that is deposited on the tellurium nano-wire array on the glass substrate 3, make the tellurium nano-wire array structure homogeneous that physical vapor deposition makes, effectively guaranteed the uniform distribution of nanophase.
Embodiment 1:
The tellurium Te 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 4nm/min, depositing time 8h;
Open AC power, regulate outward current 165A; Beginning physical vapor deposition on glass substrate 3 goes out the tellurium 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 tellurium nano-wire array film.
Adopt X-ray diffractometer that the tellurium nano-wire array film that embodiment 1 makes is carried out material phase analysis, in " a " illustrates that the tellurium nano-wire array film that makes is a tellurium Te simple substance as shown in Figure 2.
The tellurium nano-wire array film that above-mentioned physical vapor deposition makes is observed under scanning electronic microscope, and the nanowire diameter in the tellurium nano-wire array film is 20nm, and stereoscan photograph as shown in Figure 3.
Embodiment 2:
The telloy 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 8nm/min, depositing time 5h;
Open AC power, regulate outward current 175A; Beginning deposits preparation tellurium 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 tellurium nano-wire array film.
Adopt X-ray diffractometer that the tellurium nano-wire array film that embodiment 2 makes is carried out material phase analysis, in " b " illustrates that the tellurium nano-wire array film that makes is a tellurium Te simple substance as shown in Figure 2.
The tellurium nano-wire array film that embodiment 2 makes is observed under scanning electronic microscope, and the nanowire diameter in the tellurium nano-wire array film is 30nm.
Embodiment 3:
The telloy 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 12nm/min, depositing time 6h;
Open AC power, regulate outward current 170A; Beginning deposits preparation tellurium 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 tellurium nano-wire array film.
Adopt X-ray diffractometer that the tellurium nano-wire array film that embodiment 3 makes is carried out material phase analysis, in " c " illustrates that the tellurium nano-wire array film that makes is a tellurium Te simple substance as shown in Figure 2.
The tellurium nano-wire array film that embodiment 3 makes is observed under scanning electronic microscope, and the nanowire diameter in the tellurium nano-wire array film is 50nm.
Embodiment 4:
The telloy 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 5nm/min, depositing time 12h;
Open AC power, regulate outward current 165A; Beginning deposits preparation tellurium 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 tellurium nano-wire array film.
Adopt X-ray diffractometer that the tellurium nano-wire array film that embodiment 4 makes is carried out material phase analysis, in " d " illustrates that the tellurium nano-wire array film that makes is a tellurium Te simple substance as shown in Figure 2.
The tellurium nano-wire array film that embodiment 4 makes is observed under scanning electronic microscope, and the nanowire diameter in the tellurium nano-wire array film is 115nm.
Claims (2)
1, a kind of preparation method of the tellurium nano-wire array based on physical vapor deposition, it is characterized in that: be the tungsten boat (2) of the telloy 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 4～16nm/min, depositing time 5～12h; Open AC power, regulate outward current 165A～175A; Beginning is gone up deposition preparation tellurium 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 tellurium nano-wire array film.
2, the preparation method of the tellurium nano-wire array based on physical vapor deposition according to claim 1, it is characterized in that: the tellurium nano-wire diameter in the tellurium nano-wire array film that makes is 20～115nm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496675A (en) * | 2013-09-23 | 2014-01-08 | 国家纳米科学中心 | Tellurium nanowire array with field emission characteristic and preparation method as well as application thereof |
| CN104419894A (en) * | 2013-08-30 | 2015-03-18 | 国家纳米科学中心 | Infiltration-performance-controllable one-dimensional tellurium micro-nano structure membrane and preparation method thereof |
| CN109065662A (en) * | 2018-06-29 | 2018-12-21 | 国家纳米科学中心 | A kind of Te/MoS2Van der Waals heterojunction structure and its preparation method and application |
| CN109368605A (en) * | 2018-11-01 | 2019-02-22 | 西北大学 | A kind of preparation method of tellurium nano-wire material, tellurium nano-wire material and device |
| CN114032510A (en) * | 2021-11-17 | 2022-02-11 | 中国科学院半导体研究所 | Growth method of tellurium nanowire vertical array |
-
2008
- 2008-12-01 CN CN2008102269750A patent/CN101435067B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104419894A (en) * | 2013-08-30 | 2015-03-18 | 国家纳米科学中心 | Infiltration-performance-controllable one-dimensional tellurium micro-nano structure membrane and preparation method thereof |
| CN103496675A (en) * | 2013-09-23 | 2014-01-08 | 国家纳米科学中心 | Tellurium nanowire array with field emission characteristic and preparation method as well as application thereof |
| CN109065662A (en) * | 2018-06-29 | 2018-12-21 | 国家纳米科学中心 | A kind of Te/MoS2Van der Waals heterojunction structure and its preparation method and application |
| CN109368605A (en) * | 2018-11-01 | 2019-02-22 | 西北大学 | A kind of preparation method of tellurium nano-wire material, tellurium nano-wire material and device |
| CN109368605B (en) * | 2018-11-01 | 2021-10-19 | 西北大学 | Preparation method of tellurium nanowire material, tellurium nanowire material and device |
| CN114032510A (en) * | 2021-11-17 | 2022-02-11 | 中国科学院半导体研究所 | Growth method of tellurium nanowire vertical array |
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|---|---|
| CN101435067B (en) | 2010-09-08 |
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