CN101993050A - Method for preparing AlN nanowire macro ordered array by using secondary template method - Google Patents
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Abstract
The invention relates to a method for preparing an AlN nanowire macro ordered array by using a secondary template method, which comprises the following steps of: hydrophilically treating a Si substrate; depositing a single-layer order PS (Polystyrene) sphere array on the Si substrate; preparing a metal particle template; and preparing an AlN nanowire macro array. The invention aims at overcoming the defects of the conventional technology for preparing the aluminium nitride nanowire macro ordered array and provides a method for preparing the AlN nanowire macro ordered array by using the secondary template method. The size and the morphology of the nanowire macro array and the uniformity and the length of nanowires are effectively controlled by adjusting the working parameters of each process.
Description
Technical field
The present invention relates to a kind of method that is equipped with AlN nano wire macroscopic view oldered array with the secondary template legal system.
Background technology
AlN is as a kind of important semiconductor material, and its excellent heat conductivility, good thermal expansivity, high physical strength, very high specific inductivity make it in fields such as high temperature and high-power electronic devices very big application prospect be arranged.The preparation method of one dimension AlN nano-wire array has caused people's attention, and various preparation methods constantly occur, and obtains remarkable progress.Its preparation mainly contains chemical vapour deposition, molecular beam epitaxy, gas-liquid solid (VLS) method, carbon nanotube confinement method, porous alumina formwork method and thermal evaporation.That but present most of method has can't prepare in a large number because apparatus expensive or temperature of reaction are too high, have then purity is not high because the existence of impurity is arranged, therefore, explores new low cost and on a large scale the synthetic method be necessary.
Summary of the invention
The objective of the invention is to prepare the deficiency of aluminum nitride nanowire macroscopic view array technique at routine, provide a kind of and be equipped with the method for AlN nano wire macroscopic view oldered array with the secondary template legal system, by regulate each process working parameter effectively control nano wire macroscopic view array the uniformity coefficient and the length of size, pattern and nano wire.
Technical scheme of the present invention is:
A kind ofly be equipped with the method for AlN nano wire macroscopic view oldered array, it is characterized in that: said method comprising the steps of with the secondary template legal system:
(1) the Si substrate is carried out wetting ability and handle, promptly the Si substrate is put into the vitriol oil and H
2O
2Soaked in the 1:2-1:3 blended solution 2-4 hour by volume, use absolute ethanol washing, immerse again in the aqueous isopropanol of concentration 99.7%, take out afterwards air-dryly, obtain the Si substrate after the hydrophilic treatment with ultrasonication 30-50 minute;
Is size that 300-500nm, concentration are that 0.1% PS ball solution with water and alcohol furnishing concentration are 0.05% PS solution, the ratio of water and alcohol volume is 7:3, inject little flask, handled the Si substrate and put into flask carrying out wetting ability with vertically becoming 5 ° of angles, under temperature 30-60 ℃, humidity 50-75 condition, evaporate, take out in the evaporative process and use ultra-sonic oscillation 5-15min, behind the evaporation 24-48h, will on the Si substrate, deposit the orderly PS array of one deck individual layer;
(2) utilize the high temperature resistance evaporation equipment to prepare the metallic particles template, high-purity aluminium block is placed on the tungsten boat that has fixed, the Si basic mode plate that will deposit the orderly PS ball of one deck individual layer then is fixed on the baffle plate directly over the corresponding aluminium block, opens mechanical pump successively and molecular pump is evacuated to 3 * 10
-3The vacuum tightness of Pa, closure molecule pump and mechanical pump charge into 50-200torr Ar working gas;
Regulate secondary current intensity and rise to set(ting)value 150-250A, make the metallic aluminium evaporation, when rising cigarette and stablize, baffle plate is removed, metal nano powder is evaporated on the Si substrate, and 6-15s retracts baffle plate again, puts into micro-air and carries out the 1-2h passivation;
The material that cooling is good is put into high temperature sintering furnace, is evacuated down to 0.1Pa, sintering oven slowly is warming up to 500-800 ℃, and keeps 1-5h, treats that it naturally cools to room temperature, makes the metallic particles template;
(3) utilize chemical Vapor deposition process (CVD) preparation AlN nano wire macroscopic view array, at first the tubular type sintering oven is cleared up and wiping; Central inner sleeve is placed on the center of heating tube continuously, the corundum porcelain boat that high-purity aluminum strip is housed is placed on the central inner sleeve, the metallic particles template that has prepared is being placed on wherein apart from central 15-20cm place; Opening mechanical pump heating tube inside is evacuated to 0.1Pa, is under the Ar gas shiled of 100-200sccm at flow velocity, with the temperature rise rate of 40 ℃/min heating tube is warmed up to 500-600 ℃, and charging into air pressure again is the N of 50sccm for the 300-500torr flow velocity
2Gas is heated to 1100-1300 ℃ with the temperature rise rate of 20 ℃/min, behind this temperature constant temperature 120 min, is the mobile N of 50sccm at flow velocity
2Under the gas condition, horizontal electric furnace naturally cools to room temperature, makes AlN nano wire macroscopic view array.
The metallic particles template is evenly distributed, median size 40-80nm.
The AlN nano wire macroscopic view array of preparing is a hexagonal structure.
The AlN nano wire macroscopic view array area of preparing is 0.3 * 0.2mm
2
The nano wire mean diameter is 41nm in the AlN nano wire macroscopic view array of preparing.
The AlN nano wire macroscopic view array mean length of preparing is 1.8 μ m.
Advantage of the present invention is, for mechanism research provides good sample preparation methods, difficult problems such as ordinary method funds costliness have been solved, and can effectively control the size and the pattern of AlN nano wire macroscopic view array by the diameter of regulating electric current, voltage, work atmosphere and time, PS ball, so this method is the macroscopical array approach of a kind of AlN nano wire simple, that controllability is strong.
Description of drawings:
Fig. 1 is the PS ball array of diameter 500nm;
Fig. 2 contains the metal array of PS ball and the metal array of no PS ball for half;
Fig. 3 is an AlN nano wire macroscopic view array;
Fig. 4 is nano wire and the corresponding power spectrum of preparing;
Fig. 5 is the high resolution photograph of square frame portion in the corresponding diagram 4.
Embodiment:
Describe the present invention below in conjunction with specific embodiment.
Embodiment 1:
Be equipped with the method for AlN nano wire macroscopic view oldered array with the secondary template legal system, may further comprise the steps:
(1) the Si substrate is carried out wetting ability and handle, promptly the Si substrate is put into the vitriol oil and H
2O
2By volume soaked in the 1:2 blended solution 2 hours, use absolute ethanol washing, immerse again in the aqueous isopropanol (concentration 99.7%) with ultrasonication 30-minute, air-dry after taking out, obtain the Si substrate after the hydrophilic treatment;
Is 300nm, concentration that 0.1% PS ball solution with water and alcohol furnishing concentration are 0.05% PS solution, the ratio of water and alcohol volume is 7:3, inject little flask, handled the Si substrate and put into flask carrying out wetting ability with vertically becoming 5 ° of angles, under 30 ℃ of temperature, humidity 50 conditions, evaporate, use ultra-sonic oscillation 5min in the evaporative process, behind the evaporation 24h, will on the Si substrate, deposit the orderly PS array of one deck individual layer;
(2) utilize the high temperature resistance evaporation equipment to prepare the metallic particles template, with purity is that high-purity aluminium block of 99.99% is placed on the tungsten boat that has fixed, the Si basic mode plate that will deposit the orderly PS ball of one deck individual layer then is fixed on the baffle plate directly over the corresponding aluminium block, opens mechanical pump successively and molecular pump is evacuated to 3 * 10
-3The vacuum tightness of Pa, closure molecule pump and mechanical pump charge into 50torr Ar working gas;
Regulate secondary current intensity and rise to set(ting)value 150A, 24V, the metallic aluminium evaporation when rising cigarette and stablize, is removed baffle plate, and nano metal powder is evaporated on the Si substrate, baffle plate is retracted behind the 6s again, puts into micro-air and carries out the 1h passivation;
The material that cooling is good is put into high temperature sintering furnace, is evacuated down to 0.1Pa, and sintering oven slowly is warming up to 500 ℃, and keeps 1h, treats that it naturally cools to room temperature, make be evenly distributed, median size 40-80nm metallic particles template;
(3) utilize chemical Vapor deposition process (CVD) preparation AlN nano wire macroscopic view array, at first the tubular type sintering oven is cleared up and wiping; Central inner sleeve is placed on the center of heating tube continuously, the corundum porcelain boat that high-purity aluminum strip is housed is placed on the central inner sleeve, the metallic particles template that has prepared is being placed on wherein apart from central 15cm place; Opening mechanical pump heating tube inside is evacuated to 0.1Pa, is under the mobile Ar gas shiled of 100sccm at flow velocity, with the temperature rise rate of 40 ℃/min heating tube is warmed up to 500 ℃, and charging into air pressure 300torr flow velocity again is the N of 50sccm
2Gas is heated to 1100 ℃ with the temperature rise rate of 20 ℃/min, behind this temperature constant temperature 120 min, is the mobile N of 50sccm at flow velocity
2Under the gas condition, horizontal electric furnace naturally cools to room temperature, makes AlN nano wire macroscopic view array.
Embodiment 2:
A kind ofly be equipped with the method for AlN nano wire macroscopic view oldered array, may further comprise the steps with the secondary template legal system:
(1) the Si substrate is carried out wetting ability and handle, promptly the Si substrate is put into the vitriol oil and H
2O
2By volume soaked in the 1:3 blended solution 4 hours, use absolute ethanol washing, immerse again in the aqueous isopropanol (concentration 99.7%) with ultrasonication 50 minutes, air-dry after taking out, obtain the Si substrate after the hydrophilic treatment;
Is 500nm, concentration that 0.1% PS ball solution with water and alcohol furnishing concentration are 0.05% PS solution, the ratio of water and alcohol volume is 7:3, inject little flask, handled the Si substrate and put into flask carrying out wetting ability with vertically becoming 5 ° of angles, under 60 ℃ of temperature, humidity 75 conditions, evaporate, use ultra-sonic oscillation 15min in the evaporative process, behind the evaporation 48h, will on the Si substrate, deposit the orderly PS array of one deck individual layer;
(2) utilize the high temperature resistance evaporation equipment to prepare the metallic particles template, with purity is that high-purity aluminium block of 99.99% is placed on the tungsten boat that has fixed, the Si basic mode plate that will deposit the orderly PS ball of one deck individual layer then is fixed on the baffle plate directly over the corresponding aluminium block, opens mechanical pump successively and molecular pump is evacuated to 3 * 10
-3The vacuum tightness of Pa, closure molecule pump and mechanical pump charge into 200torr Ar working gas;
Regulate secondary current intensity and rise to set(ting)value 250A, 35V, the metallic aluminium evaporation when rising cigarette and stablize, is removed baffle plate, and nano metal powder is evaporated on the Si substrate, and 15s retracts baffle plate again, puts into micro-air and carries out the 2h passivation;
The material that cooling is good is put into high temperature sintering furnace, is evacuated down to 0.1Pa, and sintering oven slowly is warming up to 800 ℃, and keeps 5h, treats that it naturally cools to room temperature, make be evenly distributed, median size 40-80nm metallic particles template;
(3) utilize chemical Vapor deposition process (CVD) preparation AlN nano wire macroscopic view array, at first the tubular type sintering oven is cleared up and wiping; Central inner sleeve is placed on the center of heating tube continuously, the corundum porcelain boat that high-purity aluminum strip is housed is placed on the central inner sleeve, the metallic particles template that has prepared is being placed on wherein apart from central 20cm place; Opening mechanical pump heating tube inside is evacuated to 0.1Pa, is under the mobile Ar gas shiled of 200sccm at flow velocity, with the temperature rise rate of 40 ℃/min heating tube is warmed up to 600 ℃, and charging into air pressure 500torr flow velocity again is the N of 50sccm
2Gas is heated to 1300 ℃ with the temperature rise rate of 20 ℃/min, behind this temperature constant temperature 120 min, is the mobile N of 50sccm at flow velocity
2Under the gas condition, horizontal electric furnace naturally cools to room temperature, makes AlN nano wire macroscopic view array.
Embodiment 3:
A kind ofly be equipped with the method for AlN nano wire macroscopic view oldered array, it is characterized in that: said method comprising the steps of with the secondary template legal system:
(1) the Si substrate is carried out wetting ability and handle, promptly the Si substrate is put into the vitriol oil and H
2O
2By volume soaked in the 1:2.5 blended solution 3 hours, use absolute ethanol washing, immerse again in the aqueous isopropanol (concentration 99.7%) with ultrasonication 40 minutes, air-dry after taking out, obtain the Si substrate after the hydrophilic treatment;
Is 400nm, concentration that 0.1% PS ball solution with water and alcohol furnishing concentration are 0.05% PS solution, the ratio of water and alcohol volume is 7:3, inject little flask, handled the Si substrate and put into flask carrying out wetting ability with vertically becoming 5 ° of angles, under 50 ℃ of temperature, humidity 60 conditions, evaporate, use ultra-sonic oscillation 10min in the evaporative process, behind the evaporation 30h, will on the Si substrate, deposit the orderly PS array of one deck individual layer;
(2) utilize the high temperature resistance evaporation equipment to prepare the metallic particles template, with purity is that high-purity aluminium block of 99.99% is placed on the tungsten boat that has fixed, the Si basic mode plate that will deposit the orderly PS ball of one deck individual layer then is fixed on the baffle plate directly over the corresponding aluminium block, opens mechanical pump successively and molecular pump is evacuated to 3 * 10
-3The vacuum tightness of Pa, closure molecule pump and mechanical pump charge into 150torr Ar working gas;
Regulate secondary current intensity and rise to set(ting)value 200A, 30V, the metallic aluminium evaporation when rising cigarette and stablize, is removed baffle plate, and nano metal powder is evaporated on the Si substrate, and 10s retracts baffle plate again, puts into micro-air and carries out the 1.5h passivation;
The material that cooling is good is put into high temperature sintering furnace, is evacuated down to 0.1Pa, and sintering oven slowly is warming up to 600 ℃, and keeps 3h, treats that it naturally cools to room temperature, make be evenly distributed, median size 40-80nm metallic particles template;
(3) utilize chemical Vapor deposition process (CVD) preparation AlN nano wire macroscopic view array, at first the tubular type sintering oven is cleared up and wiping; Central inner sleeve is placed on the center of heating tube continuously, the corundum porcelain boat that high-purity aluminum strip is housed is placed on the central inner sleeve, the metallic particles template that has prepared is being placed on wherein apart from central 17cm place; Opening mechanical pump heating tube inside is evacuated to 0.1Pa, is under the mobile Ar gas shiled of 150sccm at flow velocity, with the temperature rise rate of 40 ℃/min heating tube is warmed up to 550 ℃, and charging into air pressure 400torr flow velocity again is the N of 50sccm
2Gas is heated to 1200 ℃ with the temperature rise rate of 20 ℃/min, behind this temperature constant temperature 120 min, is the mobile N of 50sccm at flow velocity
2Under the gas condition, horizontal electric furnace naturally cools to room temperature, makes AlN nano wire macroscopic view array.
Embodiment 4:
A kind ofly be equipped with the method for AlN nano wire macroscopic view oldered array, it is characterized in that: said method comprising the steps of with the secondary template legal system:
(1) the Si substrate is carried out wetting ability and handle, promptly the Si substrate is put into the vitriol oil and H
2O
2By volume soaked in the 1:2.7 blended solution 2.5 hours, use absolute ethanol washing, immerse again in the aqueous isopropanol (concentration 99.7%) with ultrasonication 35 minutes, air-dry after taking out, obtain the Si substrate after the hydrophilic treatment;
Is 450nm, concentration that 0.1% PS ball solution with water and alcohol furnishing concentration are 0.05% PS solution, the ratio of water and alcohol volume is 7:3, inject little flask, handled the Si substrate and put into flask carrying out wetting ability with vertically becoming 5 ° of angles, under 35 ℃ of temperature, humidity 70 conditions, evaporate, use ultra-sonic oscillation 8min in the evaporative process, behind the evaporation 40h, will on the Si substrate, deposit the orderly PS array of one deck individual layer;
(2) utilize the high temperature resistance evaporation equipment to prepare the metallic particles template, high-purity aluminium block is placed on the tungsten boat that has fixed, the Si basic mode plate that will deposit the orderly PS ball of one deck individual layer then is fixed on the baffle plate directly over the corresponding aluminium block, opens mechanical pump successively and molecular pump is evacuated to 3 * 10
-3The vacuum tightness of Pa, closure molecule pump and mechanical pump charge into 80torr Ar working gas;
Regulate secondary current intensity and rise to set(ting)value 190A, 28V, the metallic aluminium evaporation when rising cigarette and stablize, is removed baffle plate, and metal nano powder is evaporated on the Si substrate, and 13s retracts baffle plate again, puts into micro-air and carries out the 1h passivation;
The material that cooling is good is put into high temperature sintering furnace, is evacuated down to 0.1Pa, and sintering oven slowly is warming up to 700 ℃, and keeps 4h, treats that it naturally cools to room temperature, make be evenly distributed, median size 40-80nm metallic particles template;
(3) utilize chemical Vapor deposition process (CVD) preparation AlN nano wire macroscopic view array, at first the tubular type sintering oven is cleared up and wiping; Central inner sleeve is placed on the center of heating tube continuously, the corundum porcelain boat that high-purity aluminum strip is housed is placed on the central inner sleeve, the metallic particles template that has prepared is being placed on wherein apart from central 19cm place; Opening mechanical pump heating tube inside is evacuated to 0.1Pa, is under the mobile Ar gas shiled of 110sccm at flow velocity, with the temperature rise rate of 40 ℃/min heating tube is warmed up to 590 ℃, and charging into air pressure 350torr flow velocity again is the N of 50sccm
2Gas is heated to 1150 ℃ with the temperature rise rate of 20 ℃/min, behind this temperature constant temperature 120 min, is the mobile N of 50sccm at flow velocity
2Under the gas condition, horizontal electric furnace naturally cools to room temperature, makes AlN nano wire macroscopic view array.
Embodiment 5:
A kind ofly be equipped with the method for AlN nano wire macroscopic view oldered array, it is characterized in that: said method comprising the steps of with the secondary template legal system:
(1) the Si substrate is carried out wetting ability and handle, promptly the Si substrate is put into the vitriol oil and H
2O
2By volume soaked in the 1:2.3 blended solution 3.5 hours, use absolute ethanol washing, immerse again in the aqueous isopropanol (concentration 99.7%) with ultrasonication 45 minutes, air-dry after taking out, obtain the Si substrate after the hydrophilic treatment;
Is 350nm, concentration that 0.1% PS ball solution with water and alcohol furnishing concentration are 0.05% PS solution, the ratio of water and alcohol volume is 7:3, inject little flask, handled the Si substrate and put into flask carrying out wetting ability with vertically becoming 5 ° of angles, under 55 ℃ of temperature, humidity 55 conditions, evaporate, use ultra-sonic oscillation 13min in the evaporative process, behind the evaporation 28h, will on the Si substrate, deposit the orderly PS array of one deck individual layer;
(2) utilize the high temperature resistance evaporation equipment to prepare the metallic particles template, high-purity aluminium block is placed on the tungsten boat that has fixed, the Si basic mode plate that will deposit the orderly PS ball of one deck individual layer then is fixed on the baffle plate directly over the corresponding aluminium block, opens mechanical pump successively and molecular pump is evacuated to 3 * 10
-3The vacuum tightness of Pa, closure molecule pump and mechanical pump charge into 170torr Ar working gas;
Regulate secondary current intensity and rise to set(ting)value 230A, 31V, the metallic aluminium evaporation when rising cigarette and stablize, is removed baffle plate, and metal nano powder is evaporated on the Si substrate, and 8s retracts baffle plate again, puts into micro-air and carries out the 2h passivation;
The material that cooling is good is put into high temperature sintering furnace, is evacuated down to 0.1Pa, and sintering oven slowly is warming up to 550 ℃, and keeps 2h, treats that it naturally cools to room temperature, make be evenly distributed, median size 40-80nm metallic particles template;
(3) utilize chemical Vapor deposition process (CVD) preparation AlN nano wire macroscopic view array, at first the tubular type sintering oven is cleared up and wiping; Central inner sleeve is placed on the center of heating tube continuously, the corundum porcelain boat that high-purity aluminum strip is housed is placed on the central inner sleeve, the metallic particles template that has prepared is being placed on wherein apart from central 16cm place; Opening mechanical pump heating tube inside is evacuated to 0.1Pa, is under the mobile Ar gas shiled of 180sccm at flow velocity, with the temperature rise rate of 40 ℃/min heating tube is warmed up to 520 ℃, and charging into air pressure 450torr flow velocity again is the N of 50sccm
2Gas is heated to 1100 ℃ with the temperature rise rate of 20 ℃/min, behind this temperature constant temperature 120 min, is the mobile N of 50sccm at flow velocity
2Under the gas condition, horizontal electric furnace naturally cools to room temperature, makes AlN nano wire macroscopic view array.
Embodiment 6:
A kind ofly be equipped with the method for AlN nano wire macroscopic view oldered array, may further comprise the steps with the secondary template legal system:
(1) the Si substrate is carried out wetting ability and handle, promptly the Si substrate is put into the vitriol oil and H
2O
2By volume soaked in the 1:2.1 blended solution 2 hours, use absolute ethanol washing, immerse again in the aqueous isopropanol (concentration 99.7%) with ultrasonication 48 minutes, air-dry after taking out, obtain the Si substrate after the hydrophilic treatment;
Is 380nm, concentration that 0.1% PS ball solution with water and alcohol furnishing concentration are 0.05% PS solution, the ratio of water and alcohol volume is 7:3, inject little flask, handled the Si substrate and put into flask carrying out wetting ability with vertically becoming 5 ° of angles, under 40 ℃ of temperature, humidity 65 conditions, evaporate, use ultra-sonic oscillation 11min in the evaporative process, behind the evaporation 45h, will on the Si substrate, deposit the orderly PS array of one deck individual layer;
(2) utilize the high temperature resistance evaporation equipment to prepare the metallic particles template, high-purity aluminium block is placed on the tungsten boat that has fixed, the Si basic mode plate that will deposit the orderly PS ball of one deck individual layer then is fixed on the baffle plate directly over the corresponding aluminium block, opens mechanical pump successively and molecular pump is evacuated to 3 * 10
-3The vacuum tightness of Pa charges into 100torr Ar working gas;
Regulate secondary current intensity and rise to set(ting)value 160A, 25V, the metallic aluminium evaporation when rising cigarette and stablize, is removed baffle plate, and metal nano powder is evaporated on the Si substrate, and 14s retracts baffle plate again, and closure molecule pump and mechanical pump are put into micro-air and are carried out the 1h passivation;
The material that cooling is good is put into high temperature sintering furnace, is evacuated down to 0.1Pa, and sintering oven slowly is warming up to 650 ℃, and keeps 3.5h, treats that it naturally cools to room temperature, make be evenly distributed, median size 40-80nm metallic particles template;
(3) utilize chemical Vapor deposition process (CVD) preparation AlN nano wire macroscopic view array, at first the tubular type sintering oven is cleared up and wiping; Central inner sleeve is placed on the center of heating tube continuously, the corundum porcelain boat that high-purity aluminum strip is housed is placed on the central inner sleeve, the metallic particles template that has prepared is being placed on wherein apart from central 18cm place; Opening mechanical pump heating tube inside is evacuated to 0.1Pa, is under the mobile Ar gas shiled of 130sccm at flow velocity, with the temperature rise rate of 40 ℃/min heating tube is warmed up to 530 ℃, and charging into air pressure 480torr flow velocity again is the N of 50sccm
2Gas is heated to 1300 ℃ with the temperature rise rate of 20 ℃/min, behind this temperature constant temperature 120 min, is the mobile N of 50sccm at flow velocity
2Under the gas condition, horizontal electric furnace naturally cools to room temperature, makes AlN nano wire macroscopic view array.
With the JSM-6301F field emission scanning electron microscope PS ball template, metal A l granular formwork and AlN nano wire macroscopic view array are carried out microscopic appearance respectively and observe, and utilize the Oxford energy spectrometer that AlN nano wire macroscopic view array is carried out the Chemical Composition analysis.Fig. 1 can see the PS ball array of diameter 500nm in the Figure of description; Fig. 2 is that half contains the metal array of PS ball and the metal array of no PS ball in the Figure of description; Fig. 3 is an AlN nano wire macroscopic view array in the Figure of description, and its area is about 0.3 * 0.2mm
2, mean diameter is 41nm, mean length is about 1.8 μ m; With the JEM-2010 high-resolution electron microscope nano wire in the array is tested and analyzed, Fig. 4 is nano wire and the corresponding power spectrum of preparing in the Figure of description, and nanometer the end of a thread has catalyzer, meets the VLS growth mechanism.Fig. 5 is the high resolution photograph of square frame portion in the corresponding diagram 4 in the Figure of description, is shown as the single crystal AlN of hexagonal structure, and is consistent with selected area electron diffraction.
Claims (6)
1. one kind is equipped with the method for AlN nano wire macroscopic view oldered array with the secondary template legal system, it is characterized in that: said method comprising the steps of:
(1) the Si substrate is carried out wetting ability and handle, promptly the Si substrate is put into the vitriol oil and H
2O
2Soaked in the 1:2-1:3 blended solution 2-4 hour by volume, use absolute ethanol washing, immerse again in the aqueous isopropanol of concentration 99.7%, take out afterwards air-dryly, obtain the Si substrate after the hydrophilic treatment with ultrasonication 30-50 minute;
Is size that 300-500nm, concentration are that 0.1% PS ball solution with water and alcohol furnishing concentration are 0.05% PS solution, the ratio of water and alcohol volume is 7:3, inject little flask, handled the Si substrate and put into flask carrying out wetting ability with vertically becoming 5 ° of angles, under temperature 30-60 ℃, humidity 50-75 condition, evaporate, take out in the evaporative process and use ultra-sonic oscillation 5-15min, behind the evaporation 24-48h, will on the Si substrate, deposit the orderly PS array of one deck individual layer;
(2) utilize the high temperature resistance evaporation equipment to prepare the metallic particles template, high-purity aluminium block is placed on the tungsten boat that has fixed, the Si basic mode plate that will deposit the orderly PS ball of one deck individual layer then is fixed on the baffle plate directly over the corresponding aluminium block, opens mechanical pump successively and molecular pump is evacuated to 3 * 10
-3The vacuum tightness of Pa, closure molecule pump and mechanical pump charge into 50-200torr Ar working gas;
Regulate secondary current intensity and rise to set(ting)value 150-250A, make the metallic aluminium evaporation, when rising cigarette and stablize, baffle plate is removed, metal nano powder is evaporated on the Si substrate, and 6-15s retracts baffle plate again, puts into micro-air and carries out the 1-2h passivation;
The material that cooling is good is put into high temperature sintering furnace, is evacuated down to 0.1Pa, sintering oven slowly is warming up to 500-800 ℃, and keeps 1-5h, treats that it naturally cools to room temperature, makes the metallic particles template;
(3) utilize chemical Vapor deposition process (CVD) preparation AlN nano wire macroscopic view array, at first the tubular type sintering oven is cleared up and wiping; Central inner sleeve is placed on the center of heating tube continuously, the corundum porcelain boat that high-purity aluminum strip is housed is placed on the central inner sleeve, the metallic particles template that has prepared is being placed on wherein apart from central 15-20cm place; Opening mechanical pump heating tube inside is evacuated to 0.1Pa, is under the Ar gas shiled of 100-200sccm at flow velocity, with the temperature rise rate of 40 ℃/min heating tube is warmed up to 500-600 ℃, and charging into air pressure again is the N of 50sccm for the 300-500torr flow velocity
2Gas is heated to 1100-1300 ℃ with the temperature rise rate of 20 ℃/min, behind this temperature constant temperature 120 min, is the mobile N of 50sccm at flow velocity
2Under the gas condition, horizontal electric furnace naturally cools to room temperature, makes AlN nano wire macroscopic view array.
2. be equipped with the method for AlN nano wire macroscopic view oldered array according to claim 1 is described with the secondary template legal system, it is characterized in that: the metallic particles template is evenly distributed, median size 40-80nm.
3. be equipped with the method for AlN nano wire macroscopic view oldered array according to claim 1 is described with the secondary template legal system, it is characterized in that: the AlN nano wire macroscopic view array of preparing is a hexagonal structure.
4. be equipped with the method for AlN nano wire macroscopic view oldered array according to claim 1 is described with the secondary template legal system, it is characterized in that: the AlN nano wire macroscopic view array area of preparing is 0.3 * 0.2mm
2
5. be equipped with the method for AlN nano wire macroscopic view oldered array according to claim 1 is described with the secondary template legal system, it is characterized in that: the nano wire mean diameter is 41nm in the AlN nano wire macroscopic view array of preparing.
6. be equipped with the method for AlN nano wire macroscopic view oldered array according to claim 1 is described with the secondary template legal system, it is characterized in that: the AlN nano wire macroscopic view array mean length of preparing is 1.8 μ m.
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| CN108970612A (en) * | 2018-06-26 | 2018-12-11 | 西安理工大学 | A method of preparing Ag loading ZnO nanometer stick array |
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| CN1544315A (en) * | 2003-11-10 | 2004-11-10 | �Ϻ���ͨ��ѧ | Unidimensional aluminium nitride nanometer structure array and its preparation method |
| CN101041905A (en) * | 2007-03-13 | 2007-09-26 | 南京大学 | Aluminum oxide porous one-dimensional nano material and method for making same and usage |
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| CN1544315A (en) * | 2003-11-10 | 2004-11-10 | �Ϻ���ͨ��ѧ | Unidimensional aluminium nitride nanometer structure array and its preparation method |
| CN101041905A (en) * | 2007-03-13 | 2007-09-26 | 南京大学 | Aluminum oxide porous one-dimensional nano material and method for making same and usage |
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| 《纳米科技》 20090228 吕惠民等 硅衬底上有序氮化铝纳米线阵列的生长 23-25，71 1-6 第6卷, 第1期 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108970612A (en) * | 2018-06-26 | 2018-12-11 | 西安理工大学 | A method of preparing Ag loading ZnO nanometer stick array |
| CN108970612B (en) * | 2018-06-26 | 2021-01-15 | 西安理工大学 | Method for preparing Ag-loaded ZnO nanorod array |
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