CN106711030A - Method using stannic oxide for catalytic growth of Si nanowire - Google Patents
Method using stannic oxide for catalytic growth of Si nanowire Download PDFInfo
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- CN106711030A CN106711030A CN201611140652.0A CN201611140652A CN106711030A CN 106711030 A CN106711030 A CN 106711030A CN 201611140652 A CN201611140652 A CN 201611140652A CN 106711030 A CN106711030 A CN 106711030A
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- tin oxide
- fluorine doped
- doped tin
- catalytic growth
- conductive glass
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy
- H01L21/205—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy using reduction or decomposition of a gaseous compound yielding a solid condensate, i.e. chemical deposition
- H01L21/2053—Expitaxial deposition of elements of Group IV of the Periodic System, e.g. Si, Ge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention provides a method using stannic oxide for the catalytic growth of a Si nanowire. Fluorine doped tin oxide coating conductive glass is used as a substrate, is heated, is filled with Ar gas, and is ionized into a plasma body, and at the same time flowing Ar gas is used to adjust pressure intensity in a vacuum cavity, and the pressure intensity is maintained at 10 to 100Pa. SiH4 and H2 are filled. A fluorine doped tin oxide coating on the fluorine doped tin oxide coating conductive glass is melt into a liquid phase SnO2 sphere with the diameter of 0.2 to 0.5 micro. Under vacuum, deposition is carried out to acquire the Si nanowire. According to the invention, the fluorine doped tin oxide layer on the fluorine doped tin oxide coating conductive glass is used to provide SnO2; SnO2 is used as a catalyst to grow the silicon nanowire to realize an in-situ growth effect; and the method has the advantages of simple process, low cost and mass production.
Description
Technical field
The present invention relates to a kind of preparation method of silicon nanowires, and in particular to one kind is received using tin ash catalytic growth Si
The method of rice noodles.
Background technology
Nano wire refers to as one of various nanometer semiconductor structure things, the cable architecture body with nano-grade size.According to
Different growth mechanisms, prepare silicon nanowires method be broadly divided into it is following several：(1) metal catalytic gas-liquid-solid (VLS) is raw
Silicon nanowires long adds the metallic catalysts such as Fe, Ni, Au, Ag in silicon source, and laser ablation, heat are used according to VLS growing principles
Evaporation, chemical vapour deposition technique prepare a large amount of silicon nanowires.(2) Silicon Nanowires Fabricated by Oxide-assisted Growth Mechanism, but with gold
During category or metal oxide are catalyst preparation silicon nanowires, discovery is not that the top of each silicon nanowires has
Catalyst pellet.Research finds that it is by two outside silicon wafer not use metallic catalyst to obtain internal under certain condition
The silicon nanowires of silicon oxide layer cladding.(3) template, the template for being usually used in preparing silicon nanowires at present has anodic oxidation aluminum dipping form
Plate, zeolite template etc..Template can be used for preparing including nanometers such as the metal including silicon nanowires, semiconductor, carbon, polymer
Line.
But there is energy consumption greatly in the above method, the problem of high cost.
The content of the invention
The present invention is in order to overcome the problems of the prior art, it is therefore intended that provide a kind of using tin ash catalytic growth Si
The method of nano wire, used as catalyst, catalytic growth silicon nanowires make use of plasma to breakthrough use metal oxide
Strengthen chemical gaseous phase depositing process depositing temperature is low, deposition of elements controllability the advantages of, broken traditional noble metal and urged
The method of metaplasia silicon nanowires long, effectively reduces the cost of growth silicon nanowires, is that the production in enormous quantities of silicon nanowires is carried
Effective technical support is supplied.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of method of utilization tin ash catalytic growth Si nano wires, comprises the following steps：
1) the metal oxide SnO of catalytic growth silicon nanowires2Preparation：
Using fluorine doped tin oxide coated conductive glass as substrate, plasma enhanced chemical vapor deposition unit is placed in
On lower pole target sample platform in vacuum chamber；Vacuum is evacuated to, while heating substrate；Ar gas is passed through again and plasma is ionized into, together
Pressure in the Ar controlled atmosphere section vacuum chambers of Shi Caiyong flowings maintains 10-100Pa；Then pass to SiH4And H2, fluorine doped tin oxide painting
The overcoat fusing liquid phase SnO into a diameter of 0.2-0.5 μm of fluorine doped tin oxide on layer electro-conductive glass2Spheroid；
2) according to solid-liquid-gas growing principle catalytic growth silicon nanowires：
Under vacuo, be heated to 450-750 DEG C of depositing temperature, and with deposition power as 10-75W, deposition pressure is as 80-
140Pa, sedimentation time are that distance, for 2.5-3cm is deposited, obtains Si nano wires between 50-90min, target.
Further improvement of the invention is that the thickness of fluorine doped tin oxide coating is on fluorine doped tin oxide coated conductive glass
0.15-0.4μm。
Further improvement of the invention is that heating substrate temperature is 200-350 DEG C, and the time of heating is 3-8 minutes.
The present invention is further improved, SiH4Flow be 2-20Sccm, H2Flow be 10-100Sccm.
Of the invention further improvement be, step 1) and step 2) in vacuum be 1 × 10-4Pa。
Further improvement of the invention is to carry out step 1) before, fluorine doped tin oxide electro-conductive glass is placed at room temperature
Ultrasonic oscillation removes the spot of fluorine doped tin oxide conductive glass surface in absolute ethyl alcohol.
Compared with prior art, this hair has the advantage that：
First by fluorine doped tin oxide coated conductive glass in plasma enhanced chemical vapor deposition unit in the present invention, enter
After row heating, then it is passed through SiH4And H2Under conditions of, substantial amounts of SiH3·、SiH2, SiH, H isoreactivity particle be adsorbed
In fluorine doped tin oxide coating surface, wherein the SnO on the particle containing Si elements for adsorbing and electro-conductive glass2Film forms Sn-
Si-O eutectic solid solution, so that film gradually forms liquid phase SnO in the presence of temperature2.Liquid phase SnO2Can be with spherical
Minimum energy state is present, liquid phase SnO2It is spherical to be deposited as catalyst, with adsorbing and be solid-solubilized in Sn-Si-O low common
The increase of the Si atomic quantities in blow solution progressivelyes reach its solid solution saturation value, and Si atoms are just gradually separated out and form Si nanometers
Line.Step 1 in the present invention) in heating-up temperature and step 2) although in depositing temperature be far below SnO2Normal melting point, but
Because of the relative out-of-flatness on fluorine doped tin oxide top layer, it may appear that rough phenomenon, recess is more prone to receive lower pole target conduction
Heat.Other plasma release substantial amounts of heat during the shock to fluorine doped tin oxide film and bonding so that
, in the case where heating-up temperature is far below fusing point, fluorine doped tin oxide coating can partly be fused into liquid phase for it.The SnO of liquid phase2Absorption
Around Si elements diffusions to bottom separate out, in above-mentioned sedimentation time, nano wire can length gradually, so as to collapse, formation is not
Regularly arranged nano wire.
The present invention is heated using fluorine doped tin oxide coated conductive glass as substrate, prepares the SnO of liquid phase2, novelty
Provide SnO using the fluorine doped tin oxide layer on fluorine doped tin oxide layer electro-conductive glass2, and SnO2As catalyst growth silicon
Nano wire, reaches growth in situ effect.SnO2Silicon nanowires can be during deposition in the preparation of catalytic growth silicon nanowires
Out, overcome is needed again through too high true direct growth using Fe, Ni as catalyst preparation silicon carbide nanometer line in the prior art
High-temperature process under reciprocal of duty cycle, because the fusing point of Fe, Ni alloy is high, according to the temperature of vapor-liquid-solid growth principle catalytic growth
Problem higher.Present invention process is simple, low cost, and can realize batch production.Therefore, the present invention is obtained Si nanometers
Line, can be applied to the various industries such as the luminous energy such as electronic component and solar energy industry, biology sensor.
Further, the thickness of fluorine doped tin oxide coating is 0.15-0.4 μm on fluorine doped tin oxide coated conductive glass, is melted
It is melted into a diameter of 0.2-0.5 μm of liquid phase SnO2Spheroid, reason is that the spherical Sn-Si-O eutectic formed in the present invention is consolidated
The size of solution will produce influence, SnO to the stand density of nano wire, thickness form2The diameter of spheroid is determined from it
Bottom separate out thin silicon nanowires quantity number.SnO2The diameter of catalyst pellet is bigger, and the radical of thin silicon nanowires is more,
The diameter of the silicon nanowires that spiral tangles is also bigger.
Brief description of the drawings
Fig. 1 is the electromicroscopic photograph of the silicon nanowires of embodiments of the invention 1.
Fig. 2 is the electromicroscopic photograph of the silicon nanowires of embodiments of the invention 2.
Specific embodiment
Describe in detail by the following examples, but the present invention is not limited to following examples.
Embodiment 1
The first step：The treatment of substrate
Step one, by fluorine doped tin oxide electro-conductive glass (specification 150mm × 200mm, transmitance>80%, thickness 2.2mm, electricity
13 ohm of resistance, mist degree<1%.Japanese NSG companies imported product.) as substrate, ultrasonic wave in absolute ethyl alcohol is placed at room temperature
Concussion cleaning 10min, to remove the spot of substrate surface；
Step 2, cleaned with deionized water and ultrasonic oscillation 10min；
Step 3, substrate is dried after encased with clean lens paper, with the secondary pollution during avoiding contact with；
Second step：Metal oxide SnO2The preparation of catalytic growth silicon nanowires
Step one, the lower pole that the substrate that the first step is prepared is placed in plasma enhanced chemical vapor deposition vacuum chamber
On target sample platform.It is 1 × 10 to be evacuated to vacuum-4Pa, while heating substrate to 200 DEG C, and is incubated 8 minutes；Ar gas is passed through again simultaneously
Plasma is ionized into, while maintaining 10Pa using the pressure in the Ar controlled atmosphere section vacuum chambers of flowing；Then pass to SiH4With
H2, SiH4Flow be 2Sccm, H2Flow be 10Sccm；Fluorine doped tin oxide coating on fluorine doped tin oxide coated conductive glass
It is melted into a diameter of 0.3 μm or so of liquid phase SnO2Spheroid；
Wherein, the thickness of fluorine doped tin oxide coating is 0.15-0.4 μm on fluorine doped tin oxide coated conductive glass.
Step 2, according to solid-liquid-gas growing principle catalytic growth silicon nanowires
In a higher vacuum (1 × 10-4Pa 490 DEG C of depositing temperature is heated under), SiH is passed through4And H2, SiH4Stream
Measure is 3Sccm, H2Flow is 20Sccm, and with distance between deposition power 10W, deposition pressure 80Pa, deposition 50min, target
2.5cm, grows Si nano wires, and silicon nanowires scanning electron microscope (SEM) photograph is as shown in Figure 1.It will be seen from figure 1 that nanowire growth is uniform,
Simultaneously it can be seen that nano wire is grown from the bottom of white globules, nano wire is growing into the generation of certain length rear upper part
Bending.
Embodiment 2
The first step：The treatment of substrate
Step one, using fluorine doped tin oxide electro-conductive glass as substrate, absolute ethyl alcohol ultrasonic oscillation is placed at room temperature clear
20min is washed, to remove the spot of substrate surface；
Step 2, cleaned with deionized water and ultrasonic oscillation 20min；
Step 3, substrate is dried after encased with clean lens paper, with the secondary pollution during avoiding contact with；
Second step：Metal oxide SnO2The preparation of catalytic growth silicon nanowires
Step one, the lower pole target that the above-mentioned substrate for preparing is placed in plasma enhanced chemical vapor deposition vacuum chamber
On sample stage.It is 1 × 10 to be evacuated to vacuum-4Pa, while heating substrate to 350 DEG C, and is incubated 3 minutes；Ar gas and electricity are passed through again
From into plasma, while maintaining 100Pa using the pressure in the Ar controlled atmosphere section vacuum chambers of flowing；Then pass to SiH4And H2,
SiH4Flow be 20Sccm, H2Flow be 70Sccm；Fluorine doped tin oxide coating on fluorine doped tin oxide coated conductive glass melts
It is melted into a diameter of 0.4 μm or so of liquid phase SnO2Spheroid；
Wherein, the thickness of fluorine doped tin oxide coating is 0.15-0.4 μm on fluorine doped tin oxide coated conductive glass.
Step 2, according to solid-liquid-gas growing principle catalytic growth silicon nanowires
In a higher vacuum (1 × 10-4Pa 750 DEG C of depositing temperature is heated under), SiH is passed through4And H2, SiH4Stream
It is 15Sccm to measure, H2Flow is 30Sccm, and with distance between deposition power 75W, deposition pressure 140Pa, deposition 15min, target
3cm, grows Si nano wires, and silicon nanowires scanning electron microscope (SEM) photograph is as shown in Figure 2.Figure it is seen that nanowire growth is uniform.
Nano wire is reached after certain length, and due to the difference of growth rate, nano wire can occur a certain degree of bending.
Embodiment 3
The first step：The treatment of substrate
Step one, by fluorine doped tin oxide electro-conductive glass (specification 150mm × 200mm, transmitance>80%, thickness 2.2mm, electricity
13 ohm of resistance, mist degree<1%.Japanese NSG companies imported product.) as substrate, ultrasonic wave in absolute ethyl alcohol is placed at room temperature
Concussion cleaning 10min, to remove the spot of substrate surface；
Step 2, cleaned with deionized water and ultrasonic oscillation 10min；
Step 3, substrate is dried after encased with clean lens paper, with the secondary pollution during avoiding contact with；
Second step：The metal oxide SnO of catalytic growth silicon nanowires2Preparation：
Using fluorine doped tin oxide coated conductive glass as substrate, plasma enhanced chemical vapor deposition unit is placed in
On lower pole target sample platform in vacuum chamber；Vacuum is evacuated to, while heating substrate to 250 DEG C, and 5 minutes is incubated；Ar gas is passed through again
And plasma is ionized into, while maintaining 50Pa using the pressure in the Ar controlled atmosphere section vacuum chambers of flowing；Then pass to SiH4
And H2, SiH4Flow be 10Sccm, H2Flow be 100Sccm；Fluorine doped tin oxide on fluorine doped tin oxide coated conductive glass
The overcoat fusing liquid phase SnO into a diameter of 0.2 μm2Spheroid；
Wherein, the thickness of fluorine doped tin oxide coating is 0.15-0.4 μm on fluorine doped tin oxide coated conductive glass.
3rd step：According to solid-liquid-gas growing principle catalytic growth silicon nanowires：
It is 1 × 10 in vacuum-4Under Pa, be heated to 600 DEG C of depositing temperature, and with deposition power as 50W, deposition pressure be
100Pa, sedimentation time are that distance, for 3cm is deposited, obtains Si nano wires between 60min, target.
Embodiment 4
The first step：The treatment of substrate
Step one, by fluorine doped tin oxide electro-conductive glass (specification 150mm × 200mm, transmitance>80%, thickness 2.2mm, electricity
13 ohm of resistance, mist degree<1%.Japanese NSG companies imported product.) as substrate, ultrasonic wave in absolute ethyl alcohol is placed at room temperature
Concussion cleaning 10min, to remove the spot of substrate surface；
Step 2, cleaned with deionized water and ultrasonic oscillation 10min；
Step 3, substrate is dried after encased with clean lens paper, with the secondary pollution during avoiding contact with；
Second step：The metal oxide SnO of catalytic growth silicon nanowires2Preparation：
Using fluorine doped tin oxide coated conductive glass as substrate, plasma enhanced chemical vapor deposition unit is placed in
On lower pole target sample platform in vacuum chamber；Vacuum is evacuated to, while heating substrate to 300 DEG C, and 6 minutes is incubated；Ar gas is passed through again
And plasma is ionized into, while maintaining 70Pa using the pressure in the Ar controlled atmosphere section vacuum chambers of flowing；Then pass to SiH4
And H2, SiH4Flow be 15Sccm, H2Flow be 40Sccm；Fluorine doped tin oxide on fluorine doped tin oxide coated conductive glass
The overcoat fusing liquid phase SnO into a diameter of 0.5 μm2Spheroid；
Wherein, the thickness of fluorine doped tin oxide coating is 0.15-0.4 μm on fluorine doped tin oxide coated conductive glass.
3rd step：According to solid-liquid-gas growing principle catalytic growth silicon nanowires：
It is 1 × 10 in vacuum-4Under Pa, be heated to 450 DEG C of depositing temperature, and with deposition power as 50W, deposition pressure be
120Pa, sedimentation time are that distance, for 2.5cm is deposited, obtains Si nano wires between 70min, target.
It is of the invention that a kind of method of utilization tin ash catalytic growth Si nano wires is provided, comprise the following steps：Substrate
Cleaning with treatment；SnO is prepared on substrate using plasma reinforced chemical vapour deposition2Sample；By controlling liquid phase SnO2Directly
Footpath scope, using plasma reinforced chemical vapour deposition, quickly prepares silicon nanowires at 2-10 μm.
Claims (6)
1. a kind of method of utilization tin ash catalytic growth Si nano wires, it is characterised in that comprise the following steps：
1) the metal oxide SnO of catalytic growth silicon nanowires2Preparation：
Using fluorine doped tin oxide coated conductive glass as substrate, the vacuum of plasma enhanced chemical vapor deposition unit is placed in
On lower pole target sample platform in chamber；Vacuum is evacuated to, while heating substrate；Ar gas is passed through again and plasma is ionized into, while adopting
10-100Pa is maintained with the pressure in the Ar controlled atmosphere section vacuum chambers of flowing；Then pass to SiH4And H2, fluorine doped tin oxide coating leads
The overcoat fusing liquid phase SnO into a diameter of 0.2-0.5 μm of fluorine doped tin oxide on electric glass2Spheroid；
2) according to solid-liquid-gas growing principle catalytic growth silicon nanowires：
Under vacuo, be heated to 450-750 DEG C of depositing temperature, and with deposition power as 10-75W, deposition pressure as 80-140Pa,
Sedimentation time is that distance, for 2.5-3cm is deposited, obtains Si nano wires between 50-90min, target.
2. the method for a kind of utilization tin ash catalytic growth Si nano wires according to claim 1, it is characterised in that mix
The thickness of fluorine doped tin oxide coating is 0.15-0.4 μm on fluorine tin oxide coated conductive glass.
3. the method for a kind of utilization tin ash catalytic growth Si nano wires according to claim 1, it is characterised in that plus
Hot substrate temperature is 200-350 DEG C, and the time of heating is 3-8 minutes.
4. the method for a kind of utilization tin ash catalytic growth Si nano wires according to claim 1, it is characterised in that
SiH4Flow be 2-20Sccm, H2Flow be 10-100Sccm.
5. a kind of method of utilization tin ash catalytic growth Si nano wires according to claim 1, it is characterised in that step
It is rapid 1) and step 2) in vacuum be 1 × 10-4Pa。
6. the method for a kind of utilization tin ash catalytic growth Si nano wires according to claim 1, it is characterised in that enter
Row step 1) before, fluorine doped tin oxide electro-conductive glass is placed in ultrasonic oscillation removal fluorine doped tin oxide in absolute ethyl alcohol at room temperature
The spot of conductive glass surface.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109850843A (en) * | 2019-03-14 | 2019-06-07 | 南京大学 | A kind of hanging nano wire manipulator batch preparation |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2334848B1 (en) * | 2008-10-09 | 2012-12-26 | Ecole Polytechnique | Method for making side growth semiconductor nanowires and transistors obtained by said method |
| CN104103817A (en) * | 2014-05-19 | 2014-10-15 | 南京大学 | Nano heterostructure material for anode material of lithium battery, and preparation |
-
2016
- 2016-12-12 CN CN201611140652.0A patent/CN106711030A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2334848B1 (en) * | 2008-10-09 | 2012-12-26 | Ecole Polytechnique | Method for making side growth semiconductor nanowires and transistors obtained by said method |
| CN104103817A (en) * | 2014-05-19 | 2014-10-15 | 南京大学 | Nano heterostructure material for anode material of lithium battery, and preparation |
Non-Patent Citations (1)
| Title |
|---|
| LINWEI YU ET AL.: ""Synthesis，morphology and compositional evolution of silicon nanowires directly grown on SnO2 substrates"", 《NANOTECHNOLOGY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109850843A (en) * | 2019-03-14 | 2019-06-07 | 南京大学 | A kind of hanging nano wire manipulator batch preparation |
| CN109850843B (en) * | 2019-03-14 | 2021-01-15 | 南京大学 | Batch preparation method of suspended nanowire manipulator |
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