CN104947043A - Preparation method of Si-ITO composite nanowire ordered array - Google Patents
Preparation method of Si-ITO composite nanowire ordered array Download PDFInfo
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Abstract
The invention discloses a preparation method of a Si-ITO composite nanowire ordered array. The method comprises the following steps: etching a structured and ordered Si nanowire array on a clean monocrystalline silicon chip by using a dry-wet etching combination process, and growing ITO nanowires in an ITO electron beam vapor plating mode according to an autocatalysis principle to realize seamless combination of Si nanowires and the ITO nanowires in order to obtain the Si-ITO composite nanowire ordered array. The obtained Si-ITO nanowires have the advantages of uniform diameter, adjustable proportion, and coverage of the surface and the front of the Si-ITO nanowires by ITO grains. The method has the characteristics of simple operation, concise preparation process, good repeatability, stable performance and strong compounding property. The composite nanowires have good application prospects in the fields of nanocrystalline solar batteries, nanometer sensors and field emission display.
Description
[technical field]
The invention belongs to technical field of semiconductor, particularly the preparation method of a kind of Si-ITO (silicon-tin indium oxide) composite nano-line oldered array.
[background technology]
One-dimensional nano line has the characteristics such as large specific surface area, good assembling property and microcosmic one-dimentional structure, has wide practical use in the fields such as bio-sensing, solar cell, biological medicine carrying, and progressively plays fresh combatants' effect.Composite nano-line is owing to itself having the physics-chem characteristic of two kinds or two or more monodimension nanometer material, and there is controllable one-dimensional, be widely used in fields such as optics, catalysis, absorption, detections, therefore synthesize the study hotspot that composite nano-line is Material Field in recent years.
The Si nano-material with one-dimentional structure has important practical application in the opto-electronic devices such as feds, Monoelectron memory device, high efficiency laser, nano-sensor and solar cell.ITO material is a kind of semiconductor material with wide forbidden band (band gap is between 3.5-4.3eV), and have important application at optoelectronic areas, its one dimension form has enhanced field emission characteristic and the highly sensitive in gas sensor.Si-ITO structure realizes except the advantage of optoelectronic intagration except having, and also has the features such as easy to prepare, ratio controllable.The seamless combination of silicon materials and ITO nano material forms heterojunction structure, in nano-device is practical, have extremely important effect.What prior art grew on Si nano wire mostly is ZnO (zinc oxide) nanostructure, and the ITO material of growth is membrane structure, there is no the report about the synthesis of Si-ITO composite nano-line oldered array at present.
[summary of the invention]
The object of the present invention is to provide a kind of preparation method of Si-ITO composite nano-line oldered array, directly on Si nano wire, grow ITO nano wire, realize the seamless combination of two kinds of nano wires.The present invention makees mask by utilizing PS (polystyrene) bead, and dry-wet etch process combines and etches Si nano wire, and the mode of recycling electron beam evaporation plating, directly grows ITO nano wire on Si nano wire.By the size of control PS bead mask, the regulation and control of the diameter of etching Si nano wire can be realized, and then regulate and control the diameter of whole composite nano-line; Utilize time and the evaporation time of different etchings, the ratio of Si and ITO in composite nano-line can be regulated and controled.This composite nano-line has application prospect in nano-crystalline solar battery, nano-sensor and Field Emission Display.
To achieve these goals, the present invention adopts following technical scheme:
A kind of preparation method of Si-ITO composite nano-line oldered array, comprise the following steps: on clean monocrystalline silicon piece, first utilize dry-wet etching to combine and etch regular orderly Si nano-wire array, then the mode of electron beam evaporation plating ITO is utilized, according to autocatalysis principle, growth ITO nano wire, realize the seamless combination of Si nano wire and ITO nano wire, obtain Si-ITO composite nano-line oldered array.
The present invention further improves and is: on clean monocrystalline silicon piece, utilize dry-wet etching step etching regular orderly Si nano-wire array that combines to be specially: carry out PS bead at clean monocrystalline silicon sheet surface and be self-assembled into unitary film, as etching mask; Carry out etching 150-200s by ICP etching machine oxygen to PS bead, afterwards on PS bead mask, the argent of evaporation a layer thickness 20-40nm, is then soaked in chloroform and gets rid of PS bead mask under ultrasound condition; Carry out silver induction etching to silicon substrate again, then be immersed in concentrated nitric acid and remove argent, put into deionized water for ultrasonic cleaning afterwards, nitrogen dries up, and completes the preparation of Si nano-wire array.
The present invention further improves and is: the step of growth ITO nano wire specifically comprises: the monocrystalline silicon piece of the Si nano-wire array prepared is put into electron beam evaporation plating chamber, has one of Si nano-wire array facing to ITO target; Carry out vacuumizing in cavity, carry out cavity heating simultaneously; Then ITO is deposited, the preparation of complete Si-ITO composite nano-line oldered array.
The present invention further improves and is: the clean of monocrystalline silicon piece comprises the following steps: monocrystalline silicon piece is soaked in ultrasonic cleaning in chloroformic solution, and then puts into deionized water for ultrasonic cleaning, and nitrogen dries up afterwards; Then be soak in the hydrofluoric acid of 10% in concentration, using deionized water ultrasonic cleaning afterwards, nitrogen dries up, and completes the cleaning of monocrystalline silicon piece.
The present invention further improves and is: the diameter of PS bead is 200-800nm.
The present invention further improves and is: the etching liquid adopting hydrofluoric acid and hydrogen peroxide to configure by 10:1 carries out silver induction etching to silicon substrate, and etching time is 3-5 minute.
The present invention further improves and is: pressure <5 × 10 after vacuumizing in cavity
-4pa, chamber temp is stabilized in 300 DEG C.
The present invention further improves and is: ITO sedimentation rate is 0.08-0.1nm/s, and depositing time is 15-50 minute.
The present invention further improves and is: the evaporation electric current of argent is 115A, and vaporator rate is
evaporation cavity pressure is 7 × 10
-4pa.
The present invention further improves and is: Si nano wire and ITO nanowire surface are attached with ITO particle.
Relative to prior art, the present invention has following beneficial effect:
In the present invention, adopt the regular orderly Si nano wire of etching, make it as the substrate of ITO nanowire growth, utilize the mode of autocatalysis, grow consistent with Si nanowire size, regular orderly ITO nano wire.Realize the seamless spliced of Si nano wire and ITO nano wire, be prepared into a kind of Si-ITO composite nano-line of oldered array.
In the present invention, the Si-ITO nanowire diameter obtained is even, and ratio can regulate and control, and it is granular that surface and front end are covered with ITO.
In the present invention, the PS bead mask of different size can be adopted, etch, the Si nano wire of different diameter can be obtained;
In the present invention, different etching times can be adopted, the Si nano wire of different lengths can be obtained;
In the present invention, the regulation and control to nano-wire array can be realized by PS bead mask, there is uniform diameter, feature that length is consistent;
In the present invention, the etching time of regulation and control Si nano wire can be passed through, and the time of evaporation ITO, obtain the composite nano-line of Si-ITO different ratios;
In the present invention, the Si-ITO nanowire diameter of acquisition is even, and ratio can regulate and control, and the composite nano-line of this pattern has significant field emission performance, and this characteristic has good application prospect in Field Emission Display.
In the present invention, it is granular that the Si-ITO nanowire surface of preparation and front end are covered with ITO, granular size can be regulated by ITO evaporation rate, it can as a kind of functional material, realize sensitive detection (detection as to alcohol gas), in nanometer detection device, there is widespread use.
A kind of method preparing Si-ITO composite nano-line oldered array that the present invention proposes, have simple to operate, preparation technology is succinct, favorable repeatability, stable performance, the features such as plyability is strong, have potential using value in fields such as bio-sensing, solar cell, biological medicine carryings.
[accompanying drawing explanation]
Fig. 1 is the principle schematic that the inventive method prepares Si-ITO composite nano-line oldered array;
Mark implication in figure to be respectively: 1-nano wire substrate (monocrystalline silicon piece), 2-Si nano-wire array, 3-ITO nano-wire array, 4-ITO particle;
Fig. 2 is Si nano-wire array scanning electronic microscope (SEM) figure that in the present invention, embodiment 1 prepares gained;
Fig. 3 is Si-ITO nano-wire array scanning electronic microscope (SEM) figure that in the present invention, embodiment 1 prepares gained; Wherein Fig. 3 (a) is Local map, and Fig. 3 (b) is overall diagram;
Fig. 4 is Si nano-wire array scanning electronic microscope (SEM) figure that in the present invention, embodiment 2 prepares gained;
Fig. 5 is Si-ITO nano-wire array scanning electronic microscope (SEM) figure that in the present invention, embodiment 2 prepares gained.
[embodiment]
The preparation method of a kind of Si-ITO composite nano-line of the present invention oldered array, comprises the following steps:
The first step: the clean of nano wire substrate.
1.1), by nano wire substrate 1 (monocrystalline silicon piece) put into chloroform ultrasonic cleaning 10 minutes, remove the organic residue of silicon face;
1.2), by nano wire substrate 1 put into deionized water for ultrasonic about 5 minutes again, remove residual chloroform, then dry up with nitrogen;
1.3), by nano wire substrate 1 put into hydrofluoric acid (HF) the immersion 30s that concentration is 10%, silicon-dioxide oxidized for nano wire substrate 1 surface is removed;
1.4), by nano wire substrate 1 to put on deionized water ultrasonic cleaning again 5 minutes, in order to remove residual HF, then dry up with nitrogen.
Second step: the preparation of Si nano wire.
The mode adopting dry etching to combine with wet etching, carries out the preparation of Si nano wire.
2.1) nano wire substrate 1 surface, after the first step process is carried out diameter 200-800nm PS bead and is self-assembled into unitary film, as etching mask;
2.2), by ICP etching machine oxygen etching 150-200s is carried out to PS bead, thus obtain regular PS bead mask;
2.3), on PS bead mask, the argent of evaporation a layer thickness 20-40nm;
2.4) the PS bead mask on nano wire substrate 1 surface after the complete argent of evaporation, is got rid of with chloroform; Now nano wire substrate 1 surface has formed one deck silver reticulated film;
2.5) hydrofluoric acid (HF) and hydrogen peroxide (H, is utilized
2o
2) become etching solution by the proportions of 10:1, by wet-etching technology, silver induction etching 3-5 minute is carried out to nano wire substrate 1, obtain the Si nano-wire array 2 of orientation perpendicular to nano wire substrate 1;
2.6), with salpeter solution remove the argent on nano wire substrate 1 surface, then carry out silicon substrate cleaning.
3rd step: the preparation of evaporation ITO, Si-ITO composite nano-line.
3.1), by the nano wire substrate 1 prepared put into electron beam evaporation plating chamber, have one of Si nano-wire array facing to ITO target, carry out vacuumizing (<5 × 10 in cavity
-4pa), carry out cavity heating simultaneously, make chamber temp be stabilized in 300 DEG C;
3.2), to arrange sedimentation rate be 0.08-0.1nm/s, carries out the deposition (15-50 minute) of certain hour, then stop evaporation, takes out, obtain Si-ITO composite nano-line oldered array after sample cooling.
Embodiment 1
On monocrystalline p-type (100) the Si sheet surface self-organization cleaned up, individual layer diameter is the PS bead of 670nm, after utilizing inductively coupled plasma (ICP) etching machine oxygen to carry out etching 200s to PS bead, PS the small ball's diameter becomes ~ 500nm, then carries out the evaporation of argent.Arranging evaporation current is 115A, and vaporator rate is
evaporation cavity pressure is 7 × 10
-4pa, the thickness of evaporation silverskin is 40nm, then silicon chip is put into chloroformic solution, soak 15 minutes under ultrasound condition, in order to remove PS bead, then sample silicon chip is put into deionized water for ultrasonic clean 5 minutes, in order to go out residual chloroformic solution, naturally dry under nitrogen environment.Now sample silicon chip surface has formed one deck silver reticulated film.
Configuration hydrofluoric acid (HF): the etching solution of hydrogen peroxide (H2O2)=10:1, silver induction etch silicon is carried out by wet-etching technology, etch 5 minutes, the Si nano-wire array 2 of orientation perpendicular to silicon chip can be obtained, the diameter etching Si nano wire in the Si nano-wire array 2 obtained is ~ about 350nm, length is 1500-2000nm, then 2 minutes are immersed in concentrated nitric acid (analytical pure), remove argent, put it into deionized water for ultrasonic afterwards and clean 5 minutes, take out nitrogen and dry up.The scanning electron microscope diagram sheet of finally prepd Si nano wire as shown in Figure 2.
Then be positioned in electron beam evaporation plating chamber, had one of Si nano wire facing to ITO target (In
2o
3: SnO
2=9:1), arranging pressure in chamber is 5 × 10
-4pa, temperature-stable is at 300 DEG C, and evaporation rate is 0.08nm/s, and evaporation is after 35 minutes, and take out after sample cooling, scanning electron microscope diagram sheet as shown in Figure 3.The Si-ITO composite Nano linear array of final preparation can be found out, nanowire length ~ about 5um, Si-ITO ratio is 25%:75%, and due to ITO evaporation rate less, so surperficial ITO particle is less.
Embodiment 2
On the Si sheet surface self-organization cleaned up, individual layer diameter is the PS bead of 500nm, after utilizing inductively coupled plasma (ICP) etching machine oxygen to carry out etching 150s to PS bead, PS the small ball's diameter becomes ~ 350nm, then carries out the evaporation of argent.Arranging evaporation current is 115A, and vaporator rate is
evaporation cavity pressure is 7 × 10
-4pa, the thickness of evaporation silverskin is 35nm, then silicon chip is put into chloroformic solution, soak 15 minutes under ultrasound condition, in order to remove PS bead, then sample silicon chip is put into deionized water for ultrasonic clean 5 minutes, in order to go out residual chloroformic solution, naturally dry under nitrogen environment.Now sample silicon chip surface has formed one deck silver reticulated film.
Configuration hydrofluoric acid (HF): the etching solution of hydrogen peroxide (H2O2)=10:1, silver induction etch silicon is carried out by wet-etching technology, etch 3 minutes, the Si nano-wire array of orientation perpendicular to silicon chip can be obtained, the diameter etching Si nano wire in the Si nano-wire array obtained is ~ about 200nm, length is ~ 500nm, then 100s in concentrated nitric acid (analytical pure) is immersed in, remove argent, put it into deionized water for ultrasonic afterwards and clean 5 minutes, take out nitrogen and dry up.The scanning electron microscope diagram sheet of finally prepd Si nano wire as shown in Figure 4.
Then be positioned in electron beam evaporation plating chamber, had one of Si nano wire facing to ITO target (In
2o
3: SnO
2=9:1), arranging pressure in chamber is 5 × 10
-4pa, temperature-stable is at 300 DEG C, and evaporation rate is 0.1nm/s, and evaporation is after 15 minutes, and take out after sample cooling, scanning electron microscope diagram sheet as shown in Figure 5.The Si-ITO composite Nano linear array of final preparation can be found out, nanowire length ~ about 1um, Si-ITO ratio is 50%:50%, and owing to increasing ITO evaporation rate, the ITO Particle Phase on final composite nano-line surface is to becoming large in embodiment 1.
Embodiment 3
On the Si sheet surface self-organization cleaned up, individual layer diameter is the PS bead of 200nm, and after utilizing inductively coupled plasma (ICP) etching machine oxygen to carry out etching 150s to PS bead, PS the small ball's diameter diminishes, and then carries out the evaporation of argent.Arranging evaporation current is 115A, and vaporator rate is
evaporation cavity pressure is 7 × 10
-4pa, the thickness of evaporation silverskin is 20nm, then silicon chip is put into chloroformic solution, soak 15 minutes under ultrasound condition, in order to remove PS bead, then sample silicon chip is put into deionized water for ultrasonic clean 5 minutes, in order to go out residual chloroformic solution, naturally dry under nitrogen environment.Now sample silicon chip surface has formed one deck silver reticulated film.
Configuration hydrofluoric acid (HF): the etching solution of hydrogen peroxide (H2O2)=10:1, silver induction etch silicon is carried out by wet-etching technology, etch 3 minutes, the Si nano-wire array of orientation perpendicular to silicon chip can be obtained, the diameter etching Si nano wire in the Si nano-wire array obtained is ~ about 100nm, length is ~ 500nm, then 80s in concentrated nitric acid (analytical pure) is immersed in, remove argent, put it into deionized water for ultrasonic afterwards and clean 5 minutes, take out nitrogen and dry up.
Then be positioned in electron beam evaporation plating chamber, had one of Si nano wire facing to ITO target (In
2o
3: SnO
2=9:1), arranging pressure in chamber is 5 × 10
-4pa, temperature-stable is at 300 DEG C, and evaporation rate is 0.1nm/s, and evaporation, after 30 minutes, takes out, obtains Si-ITO composite nano-line oldered array after sample cooling.
Embodiment 4
On the Si sheet surface self-organization cleaned up, individual layer diameter is the PS bead of 800nm, and after utilizing inductively coupled plasma (ICP) etching machine oxygen to carry out etching 200s to PS bead, PS the small ball's diameter diminishes, and then carries out the evaporation of argent.Arranging evaporation current is 115A, and vaporator rate is
evaporation cavity pressure is 7 × 10
-4pa, the thickness of evaporation silverskin is 40nm, then silicon chip is put into chloroformic solution, soak 15 minutes under ultrasound condition, in order to remove PS bead, then sample silicon chip is put into deionized water for ultrasonic clean 5 minutes, in order to go out residual chloroformic solution, naturally dry under nitrogen environment.Now sample silicon chip surface has formed one deck silver reticulated film.
Configuration hydrofluoric acid (HF): the etching solution of hydrogen peroxide (H2O2)=10:1, silver induction etch silicon is carried out by wet-etching technology, etch 5 minutes, the Si nano-wire array of orientation perpendicular to silicon chip can be obtained, then 120s in concentrated nitric acid (analytical pure) is immersed in, remove argent, put it into deionized water for ultrasonic afterwards and clean 5 minutes, take out nitrogen and dry up.
Then be positioned in electron beam evaporation plating chamber, had one of Si nano wire facing to ITO target (In
2o
3: SnO
2=9:1), arranging pressure in chamber is 5 × 10
-4pa, temperature-stable is at 300 DEG C, and evaporation rate is 0.08nm/s, and evaporation, after 50 minutes, takes out, obtains Si-ITO composite nano-line oldered array after sample cooling.
Claims (10)
1. a preparation method for Si-ITO composite nano-line oldered array, is characterized in that, comprises the following steps:
First on clean monocrystalline silicon piece, utilize dry-wet etching to combine and etch regular orderly Si nano-wire array, then the mode of electron beam evaporation plating ITO is utilized, according to autocatalysis principle, growth ITO nano wire, realize the seamless combination of Si nano wire and ITO nano wire, obtain Si-ITO composite nano-line oldered array.
2. the preparation method of Si-ITO composite nano-line oldered array as claimed in claim 1, is characterized in that, clean monocrystalline silicon piece utilizes dry-wet etching step etching regular orderly Si nano-wire array that combines be specially:
Carry out PS bead at clean monocrystalline silicon sheet surface and be self-assembled into unitary film, as etching mask; Carry out etching 150-200s by ICP etching machine oxygen to PS bead, afterwards on PS bead mask, the argent of evaporation a layer thickness 20-40nm, is then soaked in chloroform and gets rid of PS bead mask under ultrasound condition; Carry out silver induction etching to silicon substrate again, then be immersed in concentrated nitric acid and remove argent, put into deionized water for ultrasonic cleaning afterwards, nitrogen dries up, and completes the preparation of Si nano-wire array.
3. the preparation method of Si-ITO composite nano-line oldered array as claimed in claim 1, is characterized in that, the step of growth ITO nano wire specifically comprises:
The monocrystalline silicon piece of the Si nano-wire array prepared is put into electron beam evaporation plating chamber, has one of Si nano-wire array facing to ITO target; Carry out vacuumizing in cavity, carry out cavity heating simultaneously; Then ITO is deposited, the preparation of complete Si-ITO composite nano-line oldered array.
4. the preparation method of Si-ITO composite nano-line oldered array as claimed in claim 1, it is characterized in that, the clean of monocrystalline silicon piece comprises the following steps: monocrystalline silicon piece is soaked in ultrasonic cleaning in chloroformic solution, and then puts into deionized water for ultrasonic cleaning, and nitrogen dries up afterwards; Then be soak in the hydrofluoric acid of 10% in concentration, use deionized water ultrasonic cleaning more afterwards, nitrogen dries up, and completes the cleaning of monocrystalline silicon piece.
5. the preparation method of Si-ITO composite nano-line oldered array as claimed in claim 2, it is characterized in that, the diameter of PS bead is 200-800nm.
6. the preparation method of Si-ITO composite nano-line oldered array as claimed in claim 2, is characterized in that, the etching liquid adopting hydrofluoric acid and hydrogen peroxide to configure by 10:1 carries out silver induction etching to silicon substrate, and etching time is 3-5 minute.
7. the preparation method of Si-ITO composite nano-line oldered array as claimed in claim 3, is characterized in that, pressure <5 × 10 after vacuumizing in cavity
-4pa, chamber temp is stabilized in 300 DEG C.
8. the preparation method of Si-ITO composite nano-line oldered array as claimed in claim 3, it is characterized in that, ITO sedimentation rate is 0.08-0.1nm/s, and depositing time is 15-50 minute.
9. the preparation method of Si-ITO composite nano-line oldered array as claimed in claim 2, it is characterized in that, the evaporation electric current of argent is 115A, and vaporator rate is
evaporation cavity pressure is 7 × 10
-4pa.
10. the preparation method of Si-ITO composite nano-line oldered array as claimed in claim 1, it is characterized in that, Si nano wire and ITO nanowire surface are attached with ITO particle.
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| CN107046228A (en) * | 2017-04-07 | 2017-08-15 | 华南师范大学 | A kind of Electroabsorption Modulated Laser and preparation method thereof |
| CN107393977A (en) * | 2017-08-09 | 2017-11-24 | 西安交通大学 | A kind of ultra wide band antireflective film and preparation method thereof |
| CN109580650A (en) * | 2018-12-14 | 2019-04-05 | 清华大学 | A kind of detection method of graphene surface cleannes |
| CN109908464A (en) * | 2019-04-16 | 2019-06-21 | 北京师范大学 | A kind of biodegradable silicon nanometer needle injection and its application |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107046228A (en) * | 2017-04-07 | 2017-08-15 | 华南师范大学 | A kind of Electroabsorption Modulated Laser and preparation method thereof |
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| CN107393977A (en) * | 2017-08-09 | 2017-11-24 | 西安交通大学 | A kind of ultra wide band antireflective film and preparation method thereof |
| CN109580650A (en) * | 2018-12-14 | 2019-04-05 | 清华大学 | A kind of detection method of graphene surface cleannes |
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