CN103757693A - Growth method of GaN nanowire - Google Patents
Growth method of GaN nanowire Download PDFInfo
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- CN103757693A CN103757693A CN201410011149.XA CN201410011149A CN103757693A CN 103757693 A CN103757693 A CN 103757693A CN 201410011149 A CN201410011149 A CN 201410011149A CN 103757693 A CN103757693 A CN 103757693A
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Abstract
The invention discloses a growth method of a GaN nanowire. The method comprises the following steps: leading trimethylindium to a quartz substrate or a substrate coated with a layer of silica film on the surface in advance, forming a liquid-phase indium drop on the bottom surface of the substrate, and then leading trimethyl gallium and an ammonia gas simultaneously, so as to form an alloy liquid drop; finally, simultaneously leading the trimethyl gallium, the ammonia gas and silicane; growing the GaN nanowire on the alloy liquid drop. By adopting the method, the trimethylindium is adopted as a tin catalyst source, a high-quality GaN nanowire grows on the cheap and available quartz or the substrate coated with the silica film on the surface, the method belongs to in-situ introduction, and is free of fussy processes of transferring and cleaning between different equipments, staining of a product in the transferring process is effectively avoided, a complicated buffer layer design is not needed, and the growth method is simple and convenient, and feasible to operate, and beneficial to industrial production.
Description
Technical field
The invention belongs to semiconductor material growing technical field, relate to a kind of growth method of GaN nano wire, be specifically related to a kind of in quartz substrate or be coated with the method for the Grown GaN nano wire of silica membrane.
Background technology
GaN base semiconductor material has wider direct band gap, with its excellent physics, chemical stability, high saturated electron drift velocity, the performances such as high breaking down field strength, be widely used at present the fields such as high frequency, high temperature, high power electronic device and opto-electronic device, become the third generation semiconductor material after first-generation germanium (Ge), silicon (Si) semiconductor material and s-generation gallium arsenide (GaAs), indium phosphide (InP) compound semiconductor materials.
MOCVD(organometallics chemical gaseous phase deposition) and MBE(molecular beam epitaxy) be two kinds of major techniques of growing high-quality semiconductor material, be that other technology is incomparable.Especially MOCVD technology, in industry member widespread use.If only need to utilize MOCVD equipment can grow high-quality GaN nano wire, that will be ideal.
The preparation method of semiconductor nanowires, can be divided into method and from bottom to top method from top to bottom generally, and wherein method is to utilize existing etching technics synthesis of nano line structure from top to bottom.Yet the size of the accuracy limitations nanowire diameter of existing etching technics further reduces.And the method for grow nanowire from bottom to top at material selecting party mask, have very large popularity, and the size of nano wire can be controlled in less scope.
Growth method can be divided into again two large classes from bottom to top: the one, utilize template direction growth, and the 2nd, without template self-organizing growth.Template direction growth needs mask openings, is subject to photoetching process, the restriction of resolving power.And can be divided into without template self-organizing growth, there is catalyzer growth, and catalyst-free growth.
The external metal catalysts such as gold, nickel are mainly quoted in catalyzer growth, and this need to shift sample between distinct device, easily cause the pollution of impurity when increasing the loaded down with trivial details degree of technique.Catalyst-free growth method can be avoided the pollution of impurity, but the quality of the GaN nano wire of this method growth and pattern need to promote.
Current GaN material is mainly grown in sapphire, silicon and silicon carbide substrates.For sapphire, its price is more expensive, is also difficult to prepare large-sized Sapphire Substrate simultaneously.And silicon substrate price is cheap, mature preparation process, can make large-sized silicon substrate, but on silicon substrate growing GaN, because the Siliciumatom of Ga and substrate surface easily forms melt back, and lattice and coefficient of thermal expansion mismatch are large, need to carry out complicated layer buffer design.For silicon carbide, price is too expensive, is not too applicable to large-scale application.
Summary of the invention
In order to address the above problem, the present invention has set up in quartz substrate cheap and easy to get or has been coated with the method for the Grown GaN nano wire of silica membrane, and the inventive method is easy and simple to handle, quick.
The object of the present invention is to provide a kind of method of growing GaN nano wire.
The technical solution used in the present invention is:
A growth method for GaN nano wire, the quartzy or surperficial material that is coated with silica membrane of take is substrate, the trimethyl indium of usining forms liquid phase indium as source and drips as catalyzer, at substrate surface catalytic growth, goes out GaN nano wire.
Further, the material that above-mentioned surface is coated with silica membrane is selected from Si, the Al that is coated with silica membrane on surface
2o
3, a kind of in SiC or GaAs.
A growth method for GaN nano wire, comprises the following steps:
1) substrate is put into MOCVD reaction chamber, 1000～1100 ℃ of thermal treatment substrate 10～20min under atmosphere of hydrogen;
2) then at 600～700 ℃, pass into trimethyl indium 30～300s, on substrate, forming density is 8 * 10
6～5 * 10
8individual/cm
2liquid phase indium drip, as catalyzer;
3) then pass into trimethyl-gallium and ammonia simultaneously, make to generate GaN and be dissolved in indium and drip, form alloy liquid droplet;
4) finally pass into trimethyl-gallium, ammonia and silane simultaneously, on alloy liquid droplet, controllably grow GaN nano wire.
Further, step 2) pass into trimethyl indium time bias voltage be 350～450mbar.
Further, the diameter length of alloy liquid droplet described in step 3) is 100～600nm.
Further, the molar flow that passes into trimethyl-gallium described in step 3) and step 4) is 60～80 μ mol/min, and the molar flow of ammonia is 10～100 times of trimethyl-gallium.
Further, the logical silane flow rate described in step 4) is 30～40nmol/min.
Further, the diameter of the nano wire of GaN described in step 4) is 300～1000nm, is highly 1～10 μ m.
The invention has the beneficial effects as follows:
1. in cheap quartz substrate or be coated with the high-quality GaN nano wire of realizing controllable growth on silica membrane substrate.
2. utilize the conventional trimethyl indium of MOCVD epitaxy to originate as indium catalyzer, belonging to original position introduces, compare with other catalyzer such as introducing gold, nickel, do not need loaded down with trivial details flow process that substrate is shifted and cleaned between distinct device, and staining of effectively avoiding that sample causes in transfer process.
3. by control, form the density that density that liquid phase indium drips can be controlled GaN nanowire growth.
4. without carrying out complicated buffer layer, establish, directly and simply grow GaN nano wire.
Accompanying drawing explanation
Fig. 1 is the schema of the growth method of a kind of GaN nano wire of the present invention;
Fig. 2 is the structural representation of the present invention's growing GaN nano wire in quartz substrate, and 1 represents quartz substrate substrate, and 2 represent GaN nano wire;
Fig. 3 be the present invention at the structural representation that is coated with silica membrane Grown GaN nano wire, 1 represents non-quartz substrate, 2 represent GaN nano wires, 3 represent silica membranes;
Fig. 4 is the sectional view of alloy liquid droplet;
Fig. 5 is the vertical view of alloy liquid droplet;
Fig. 6 is the sectional view of GaN nano wire;
Fig. 7 is the vertical view of GaN nano wire.
Embodiment
The specific embodiment of the following stated, further describes object, technical scheme and the beneficial effect of invention, and the schema of GaN nanowire growth method of the present invention as shown in Figure 1; Institute's the following stated that it should be understood that, only for specific embodiments of the invention, is not limited to the present invention, within the spirit and principles in the present invention all, any modification of making, is equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
In quartz substrate, the sample mode chart of growing GaN nano wire as shown in Figure 2, is followed successively by from bottom to up, quartz substrate, GaN nano wire; Its preparation method is:
1) quartz substrate is put into MOCVD reaction chamber, the lower 1000 ℃ of thermal treatment substrates of atmosphere of hydrogen 15 minutes;
2) at 700 ℃, bias voltage is 400mbar condition, passes into trimethyl indium (TMIn) 30s, forms liquid phase indium and drip on substrate, and indium drips density and is about 8 * 10
6individual/cm
2;
3) then pass into ammonia and trimethyl-gallium (TMGa), the molar flow of trimethyl-gallium is 60 μ mol/min simultaneously, and the molar flow of ammonia is 50 times of trimethyl-gallium, generates GaN and be dissolved in indium to drip, and forms alloy liquid droplet, and droplet dia is 100～300nm;
4) finally pass into ammonia, trimethyl-gallium (TMGa) and silane simultaneously, the same step 3) of flow of ammonia and trimethyl-gallium, silane flow rate is 30nmol/min, makes to grow GaN nano wire on alloy liquid droplet, after testing, the GaN nanowire density obtaining is about 5 * 10
6bar/cm
2, diameter is 400～500nm, is highly 2～5 μ m.
In quartz substrate, the sample mode chart of growing GaN nano wire as shown in Figure 2, is followed successively by from bottom to up, quartz substrate, GaN nano wire; Its preparation method is:
1) quartz substrate is put into MOCVD reaction chamber, the lower 1000 ℃ of thermal treatment substrates of atmosphere of hydrogen 20 minutes;
2) at 600 ℃, bias voltage is 350mbar condition, passes in advance trimethyl indium (TMIn) 150s, forms liquid phase indium and drip on substrate, and indium drips density and is about 6 * 10
7individual/cm
2;
3) then pass into ammonia and trimethyl-gallium (TMGa), the molar flow of trimethyl-gallium is 60 μ mol/min simultaneously, and the molar flow of ammonia is 100 times of trimethyl-gallium, makes to generate GaN and be dissolved in indium to drip, and forms alloy liquid droplet, and diameter is 100～300nm;
4) finally pass into ammonia, trimethyl-gallium (TMGa) and silane simultaneously, the same step 3) of flow of ammonia and trimethyl-gallium, silane flow rate is 40nmol/min, makes to grow GaN nano wire on alloy liquid droplet, after testing, the GaN nanowire density obtaining is about 4 * 10
7bar/cm
2, diameter is 500～800nm, is highly 4～7 μ m.
In quartz substrate, the sample mode chart of growing GaN nano wire as shown in Figure 2, is followed successively by from bottom to up, quartz substrate, GaN nano wire.Its preparation method is:
1) quartz substrate is put into MOCVD reaction chamber, the lower 1100 ℃ of thermal treatment substrates of atmosphere of hydrogen 20 minutes;
2) at 600 ℃, bias voltage is 450mbar condition, first passes into trimethyl indium (TMIn) 300s, forms liquid phase indium and drip on substrate, and indium drips density and is about 5 * 10
8individual/cm
2;
3) then pass into ammonia and trimethyl-gallium (TMGa), the molar flow of trimethyl-gallium is 80 μ mol/min simultaneously, and the molar flow of ammonia is 10 times of trimethyl-gallium, makes to generate GaN and be dissolved in indium to drip, and forms alloy liquid droplet, and diameter is 400～500nm;
4) finally pass into ammonia, trimethyl-gallium (TMGa) and silane simultaneously, the same step 3) of flow of ammonia and trimethyl-gallium, silane flow rate is 40nmol/min, makes to grow GaN nano wire on alloy liquid droplet, after testing, obtain ground GaN nanowire density and be about 3 * 10
8bar/cm
2, diameter is 600～1000nm, is highly 5～10 μ m.
embodiment 4
On surface, be coated with silica membrane Si Grown GaN nano wire sample mode chart as shown in Figure 3, be followed successively by from bottom to up: Si substrate, silica membrane, GaN nano wire.Its preparation method is:
1) the Si substrate that surface is coated with to silica membrane is put into MOCVD reaction chamber, the lower 1000 ℃ of thermal treatment substrates of atmosphere of hydrogen 20 minutes;
2) at 700 ℃, bias voltage is 400mbar condition, passes in advance trimethyl indium (TMIn) 30s, forms liquid phase indium and drip on substrate, and indium drips density and is about 8 * 10
6individual/cm
2;
3) then pass into ammonia and trimethyl-gallium (TMGa), the molar flow of trimethyl-gallium is 70 μ mol/min simultaneously, and the molar flow of ammonia is 50 times of trimethyl-gallium, makes to generate GaN and be dissolved in indium to drip, and forms alloy liquid droplet, and diameter is 400～500nm;
4) finally pass into ammonia, trimethyl-gallium (TMGa) and silane simultaneously, the same step 3) of flow of ammonia and trimethyl-gallium, silane flow rate is 40nmol/min, makes to grow GaN nano wire on alloy liquid droplet, after testing, the GaN nanowire density obtaining is about 5 * 10
6bar/cm
2, diameter is 500～700nm, is highly 3～8 μ m.
embodiment 5
Be coated with silica membrane Si Grown GaN nano wire sample mode chart as shown in Figure 3, be followed successively by from bottom to up: Si substrate, silica membrane, GaN nano wire.Its preparation method is:
1) the Si substrate substrate that surface is coated with to silica membrane is put into MOCVD reaction chamber, the lower 1000 ℃ of thermal treatment substrates of atmosphere of hydrogen 15 minutes;
2) at 700 ℃, bias voltage is 400mbar condition, passes in advance trimethyl indium (TMIn) 150s, forms liquid phase indium and drip on substrate, and density is about 7.1 * 10
7individual/cm
2;
3) then pass into ammonia and trimethyl-gallium (TMGa) simultaneously, the molar flow of trimethyl-gallium is 70 μ mol/min, and the molar flow of ammonia is 50 times of trimethyl-gallium, makes to generate GaN and is dissolved in indium and drip, form alloy liquid droplet (as shown in Figure 4,5), diameter is 400～500nm;
4) finally pass into ammonia, trimethyl-gallium (TMGa) and silane simultaneously, the same step 3) of flow of ammonia and trimethyl-gallium, silane flow rate is 40nmol/min, makes to grow GaN nano wire on alloy liquid droplet, after testing, the GaN nanowire density obtaining is about 5.5 * 10
7bar/cm
2.The diameter of GaN nano wire is 500～900nm, be highly 4～5 μ m(as shown in Figure 6,7).
embodiment 6
Be coated with silica membrane Si Grown GaN nano wire sample mode chart as shown in Figure 3, be followed successively by from bottom to up: Si substrate, silica membrane, GaN nano wire.Its preparation method is:
1) the Si substrate substrate that surface is coated with to silica membrane is put into MOCVD reaction chamber, the lower 1100 ℃ of thermal treatment substrates of atmosphere of hydrogen 10 minutes;
2) at 700 ℃, bias voltage is 400mbar condition, passes in advance trimethyl indium (TMIn) 300s, forms liquid phase indium and drip on substrate, and indium drips density and is about 5 * 10
8individual/cm
2;
3) then pass into ammonia and trimethyl-gallium (TMGa), the molar flow of trimethyl-gallium is 70 μ mol/min simultaneously, and the molar flow of ammonia is 50 times of trimethyl-gallium, makes to generate GaN and be dissolved in indium to drip, and forms alloy liquid droplet, and diameter is 200～400nm;
4) finally pass into ammonia, trimethyl-gallium (TMGa) and silane simultaneously, the same step 3) of flow of ammonia and trimethyl-gallium, silane flow rate is 30nmol/min, makes to grow GaN nano wire on alloy liquid droplet, after testing, the GaN nanowire density obtaining is about 3 * 10
8bar/cm
2, the diameter of GaN nano wire is 300～700nm, is highly 4～6 μ m.
embodiment 7
To be coated with the Al of silica membrane
2o
3, SiC or GaAs substrate adopt as the method for embodiment 4,5,6, can grow similar GaN nano wire.
Below the GaN nano wire of preparing in embodiment is done further to detect.
Get embodiment 5 the is coated with silica membrane sample of Si Grown GaN nano wire on surface by SEM(scanning electron microscope) carry out pattern detection.
Fig. 4 forms the sectional view of alloy liquid droplet in embodiment 5, Fig. 5 is the vertical view of alloy liquid droplet, alloy liquid droplet globulate, and diameter is 400～500nm, density is about 7.1 * 10
7individual/cm
2;
Fig. 6 is the sectional view of the GaN nano wire of growth in embodiment 5, and Fig. 7 is the vertical view of the GaN nano wire of growth in embodiment 5, and diameter is 500～900nm, is highly 4～5 μ m, and density is about 5.5 * 10
7bar/cm
2.
Above-mentioned detected result explanation the inventive method can grow vertically high-quality GaN nano wire on silicon dioxide substrates or surface are coated with the substrate of silica membrane.
Claims (8)
1. a growth method for GaN nano wire, is characterized in that: the quartzy or surperficial material that is coated with silica membrane of take is substrate, and the trimethyl indium of usining is that the liquid phase indium that source forms drips as catalyzer, at substrate surface catalytic growth, goes out GaN nano wire.
2. the growth method of a kind of GaN nano wire according to claim 1, is characterized in that: the material that described surface is coated with silica membrane is selected from Si, the Al that is coated with silica membrane on surface
2o
3, a kind of in SiC, GaAs.
3. the growth method of a kind of GaN nano wire according to claim 1, is characterized in that: comprise the following steps:
1) substrate claimed in claim 1 is put into MOCVD reaction chamber, 1000～1100 ℃ of thermal treatment substrate 10～20min under atmosphere of hydrogen;
2) then at 600～700 ℃, pass into trimethyl indium 30～300s, on substrate, forming density is 8 * 10
6～5 * 10
8individual/cm
2liquid phase indium drip, as catalyzer;
3) then pass into trimethyl-gallium and ammonia simultaneously, make to generate GaN and be dissolved in indium and drip, form alloy liquid droplet;
4) finally pass into trimethyl-gallium, ammonia and silane simultaneously, on alloy liquid droplet, controllably grow GaN nano wire.
4. the growth method of a kind of GaN nano wire according to claim 2, is characterized in that: step 2) described in pass into trimethyl indium time bias voltage be 350～450mbar.
5. the growth method of a kind of GaN nano wire according to claim 2, is characterized in that: the diameter length of alloy liquid droplet described in step 3) is 100～600nm.
6. the growth method of a kind of GaN nano wire according to claim 2, is characterized in that: the molar flow that passes into trimethyl-gallium described in step 3) and step 4) is 60～80 μ mol/min, and the molar flow of ammonia is 10～100 times of trimethyl-gallium.
7. the growth method of a kind of GaN nano wire according to claim 2, is characterized in that: the logical silane flow rate described in step 4) is 30～40nmol/min.
8. the growth method of a kind of GaN nano wire according to claim 2, is characterized in that: the diameter of the nano wire of GaN described in step 4) is 300～1000nm, is highly 1～10 μ m.
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Cited By (3)
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| CN107046088A (en) * | 2017-02-06 | 2017-08-15 | 华南理工大学 | GaN nano-pillars being grown on Si (111) substrate and its preparation method and application |
| CN107881554A (en) * | 2017-10-18 | 2018-04-06 | 中国科学院半导体研究所 | In the method for Grown GaN plane nano lines |
| CN112038442A (en) * | 2020-09-10 | 2020-12-04 | 华南师范大学 | Photoelectric detector and preparation method thereof |
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| CN107046088B (en) * | 2017-02-06 | 2019-10-18 | 华南理工大学 | The GaN nano-pillar and its preparation method and application being grown on Si (111) substrate |
| CN107881554A (en) * | 2017-10-18 | 2018-04-06 | 中国科学院半导体研究所 | In the method for Grown GaN plane nano lines |
| CN112038442A (en) * | 2020-09-10 | 2020-12-04 | 华南师范大学 | Photoelectric detector and preparation method thereof |
| CN112038442B (en) * | 2020-09-10 | 2022-02-15 | 华南师范大学 | Photoelectric detector and preparation method thereof |
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