CN102828250A - Growing method for GaN nanowire - Google Patents

Growing method for GaN nanowire Download PDF

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Publication number
CN102828250A
CN102828250A CN2012103172284A CN201210317228A CN102828250A CN 102828250 A CN102828250 A CN 102828250A CN 2012103172284 A CN2012103172284 A CN 2012103172284A CN 201210317228 A CN201210317228 A CN 201210317228A CN 102828250 A CN102828250 A CN 102828250A
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purity
carrier gas
hcl
film
gan
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修向前
华雪梅
张士英
林增钦
谢自力
张�荣
韩平
陆海
顾书林
施毅
郑有炓
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Nanjing University
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Nanjing University
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Priority to CN2012103172284A priority Critical patent/CN102828250A/en
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Priority to PCT/CN2013/077974 priority patent/WO2014032465A1/en
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/005Growth of whiskers or needles
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/40AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C30B29/403AIII-nitrides
    • C30B29/406Gallium nitride
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape

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  • Crystallography & Structural Chemistry (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention relates to a method for preparing a GaN nanowire. The method comprises the following steps: evaporating a metal Ni film on a sapphire substrate after being cleaned; causing the thickness of the Ni film to be 5-50nm; placing the sapphire substrate coated with the Ni film into a HVPE (High Voltage Paper Electrophoresis) growing system and starting to grow the GaN nanowire, wherein the growing temperature is at 500-850 DEG C; taking high-purity N2 as a carrier gas, wherein the total N2 carrier gas flow is 1-5sccm; taking conventional high-purity metal gallium as a Ga source and reacting with high-purity HCl, thereby generating GaCl, wherein the HCl flow is 1-20sccm and the HCl carrier gas flow is 10-200sccm; taking high-purity ammonia as a nitrogen source, wherein NH3 flow is 50-500sccm; and growing for 1-10 minutes, thereby growing the GaN nanowire.

Description

A kind of GaN nanowire growth method
Technical field
The present invention relates to a kind of method with the hydride gaseous epitaxially groven GaN nano wire.
Background technology
With GaN and InGaN, AlGaN alloy material is that master's III-V group nitride material (claiming the GaN sill again) is the novel semiconductor material of extremely paying attention in the world in recent years.The GaN sill is the direct band gap semiconductor material with wide forbidden band, has the direct band gap of continuous variable between 1.9-6.2eV, excellent physics, chemicalstability; High saturated electron drift velocity; High-performances such as high breaking down field strength and high heat conductance have important use at aspects such as short wavelength's semiconductor photoelectronic device and high frequency, high pressure, the preparations of high temperature microelectronic device, are used for making such as indigo plant, purple, ultraviolet band luminescent device, sensitive detection parts; High temperature, high frequency, High-Field high power device; Feds, radioprotective device, piezoelectric device etc.
The nano material of one dimension system is the effective smallest dimension structure of transmission electronic and optics exciton, also is the basic structural unit of nano-machine device and nano electron device.The GaN material makes the One-Dimensional GaN nanostructure have potential application foreground widely in fields such as micro-nano photoelectric device, photoelectric detector, electron device, environment and medical science as the good characteristic of important semiconductor material; Therefore, processability excellence, high-quality One-Dimensional GaN nanostructure and characteristic research just become the advanced subject of the current world, domestic research.
The growth of GaN sill has a variety of methods, like gas phase epitaxy of metal organic compound (MOCVD), HTHP compound body GaN monocrystalline, molecular beam epitaxy (MBE), subliming method and hydride gas-phase epitaxy (HVPE) etc.The preparation of GaN nanostructure mainly contains anisotropy controllable growth method, VLS (Vapor – Liquid – Solid) and the machine-processed growth method of SLS (Solution – Liquid – Solid), template assisting growth method, surfactant method, nanoparticle self-assembly and physics or chemical process shearing etc.The growth of GaN nanostructure can be adopted multiple mode such as acquisitions such as MOCVD, MBE, but this type of equipment price cost is high, the source material expensive.
The present invention has provided a kind of employing metallic nickel (Ni) and has made catalyzer, with the method and the technology of hydride gas-phase epitaxy (HVPE) equipment growing GaN nano wire.
Summary of the invention
The present invention seeks to: propose a kind of with metallic nickel as catalyzer, growing GaN nano wire in hydride gas phase epitaxial growth equipment.Can prepare excellent performance, high-quality One-Dimensional GaN nanostructure product.
Technical scheme of the present invention is, prepares the method for GaN nano wire, utilizes hydride gas-phase epitaxy (HVPE) equipment growing GaN nano wire.Make catalyzer with metallic nickel, after the cleaning of Sapphire Substrate, first evaporation metal Ni film; The setting of Ni film deposition rate is about 1-2 dust/second, Ni film thickness 5-50nm; The Sapphire Substrate that is covered with metal nickel film is put into the HVPE growing system, beginning low-temperature epitaxy GaN nano wire; Growth temperature: 850 ℃ of 500 –; High-purity N 2As carrier gas, total N 2Carrier gas flux 1-5slm; The Ga source adopts conventional high purity metal gallium and high-purity HCl reaction to generate GaCl, HCl flow: 1-20sccm, HCl carrier gas flux 10-200sccm.High-purity ammonia is as nitrogenous source, NH 3Flow: 50 – 500sccm; Growth time 1-10 minute.
Growth temperature is especially: 650 ℃ of 500-.
Metallic nickel is during as catalyzer, and the HVPE of GaN nano wire is a VLS mechanism.Because HVPE growth velocity fast (hundreds of micron/hour) is usually used in growing fast thick film.In the present invention, need the control growing condition, make HVPE GaN growth velocity reduce, to obtain the GaN nano wire.Technical scheme of the present invention is: the method evaporation metal Ni on Sapphire Substrate with physical vapor deposition, put into the HVPE growing system, low-temperature epitaxy GaN nano wire then.
Beneficial effect of the present invention is: the present invention has provided a kind of technology GaN nanowire growth method and technology simple, with low cost.Diameter reaches tens nanometer, and length can reach several microns.
Description of drawings
Fig. 1 is the product photo of the embodiment of the invention.Under the situation of other parameter constant, NH 3Fluctuations in discharge prepare the GaN nano wire pattern (Fig. 1 in the left, center, right three photos respectively corresponding NH 3The difference of flow: promptly be respectively 50,100 and 200sccm.Growth temperature: 550,600 and 650 ℃ are removed nano wire and directly are outside one's consideration, and outward appearance does not have remarkable difference.
Fig. 2 is the product photo of the embodiment of the invention.The electron scanning micrograph of HVPE growing GaN nano wire, wherein inserting figure is high multiple photo.
Embodiment
The inventive method and technology comprise several sections: the physical vapor deposition of metal Ni film on Sapphire Substrate; The HVPE low-temperature epitaxy of GaN nano wire.
One of technology implementation mode of the present invention, HVPE technology preparation GaN nano wire comprises following a few step:
1, the cleaning of Sapphire Substrate and processing.Sample is carried out ultrasonic cleaning successively in deionized water, ethanol and deionized water, remove the pollutent of remained on surface, dry up with nitrogen.
2, Sapphire Substrate is put into the physical vapor deposition device reaction chamber, under certain reaction cavity pressure and source metal temperature, can begin the vapor deposition of metal Ni film.The setting of Ni film deposition rate is about 1-2 dust/second, Ni nano film thickness 5-50nm.Present embodiment is selected 20-30nm.
The Sapphire Substrate that 3, will be covered with metal nickel film is put into the HVPE growing system, beginning low-temperature epitaxy GaN nano wire.Growth temperature: 550,600 and 650 ℃ of three temperature condition; High-purity N 2As carrier gas, total N 2Carrier gas flux 1-5slm; High purity metal gallium and high-purity HCl reaction generate GaCl as the gallium source, HCl flow: 1-20sccm, HCl carrier gas flux 10-200sccm.High-purity ammonia is as nitrogenous source, NH 3Flow (corresponding three kinds of flows): 50,100 and 200sccm; Growth time 5 minutes.
4, take out sample according to cooling after the step 3 growth completion, promptly obtain the GaN nano wire.
5, the parameter among the controlled step 2-4 can realize that metal Ni film is annealed into orderly particle when nanowire growth temperature, thereby obtains the GaN nano wire of ordered arrangement.

Claims (2)

1. method for preparing the GaN nano wire, it is characterized in that the cleaning of Sapphire Substrate after, first evaporation metal Ni film; Ni film thickness 5-50nm; The Sapphire Substrate that is covered with the nickel film is put into the HVPE growing system, beginning low-temperature epitaxy GaN nano wire; Growth temperature: 850 ℃ of 500 –; High-purity N 2As carrier gas, total N 2Carrier gas flux 1-5slm; The Ga source adopts conventional high purity metal gallium and high-purity HCl reaction to generate GaCl, HCl flow: 1-20sccm, HCl carrier gas flux 10-200sccm; With high-purity ammonia as nitrogenous source, NH 3Flow: 50 – 500sccm; Growth time 1-10 minute.
2. according to claim 1 with HVPE growing GaN nano wire, it is characterized in that growth temperature is: 650 ℃ of 500-.
CN2012103172284A 2012-08-31 2012-08-31 Growing method for GaN nanowire Pending CN102828250A (en)

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PCT/CN2013/077974 WO2014032465A1 (en) 2012-08-31 2013-06-26 METHOD FOR GROWING GaN NANOWIRE

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103456602A (en) * 2013-03-18 2013-12-18 深圳信息职业技术学院 Method for preparing non-polar surface gallium nitride nanometer cone material
WO2014032465A1 (en) * 2012-08-31 2014-03-06 南京大学 METHOD FOR GROWING GaN NANOWIRE
CN107910243A (en) * 2017-10-18 2018-04-13 中国科学院半导体研究所 The method for preparing GaN nano wire on substrate
WO2021012496A1 (en) * 2019-07-22 2021-01-28 南京大学 Molecular beam epitaxial growth method for controlling structure and morphology of gan nanowire

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080010707A1 (en) * 2004-10-21 2008-01-10 Sharp Laboratories Of America, Inc. Ambient environment nanowire sensor
JP2008108757A (en) * 2006-10-23 2008-05-08 Matsushita Electric Works Ltd Compound semiconductor light-emitting element, illumination apparatus employing the same and manufacturing method of compound semiconductor element
CN101229912A (en) * 2007-12-26 2008-07-30 中国科学院上海微系统与信息技术研究所 Method for preparing gallium nitride nano-wire array by using dry etching
CN101728248A (en) * 2008-10-15 2010-06-09 中国科学院半导体研究所 Growing method of gallium nitride
CN101510504B (en) * 2009-03-13 2010-09-08 苏州纳晶光电有限公司 Transversal epitaxial growth method for nano area of semiconductor film
JP2011073894A (en) * 2009-09-29 2011-04-14 Toyoda Gosei Co Ltd Method for producing group iii nitride compound semiconductor
CN101689484B (en) * 2007-07-10 2012-02-15 Nxp股份有限公司 Single crystal growth on a mis-matched substrate

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101898751B (en) * 2009-05-27 2012-08-08 中国科学院半导体研究所 Method for growing group III nitride nanometer material
CN102828250A (en) * 2012-08-31 2012-12-19 南京大学 Growing method for GaN nanowire

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080010707A1 (en) * 2004-10-21 2008-01-10 Sharp Laboratories Of America, Inc. Ambient environment nanowire sensor
JP2008108757A (en) * 2006-10-23 2008-05-08 Matsushita Electric Works Ltd Compound semiconductor light-emitting element, illumination apparatus employing the same and manufacturing method of compound semiconductor element
CN101689484B (en) * 2007-07-10 2012-02-15 Nxp股份有限公司 Single crystal growth on a mis-matched substrate
CN101229912A (en) * 2007-12-26 2008-07-30 中国科学院上海微系统与信息技术研究所 Method for preparing gallium nitride nano-wire array by using dry etching
CN101728248A (en) * 2008-10-15 2010-06-09 中国科学院半导体研究所 Growing method of gallium nitride
CN101510504B (en) * 2009-03-13 2010-09-08 苏州纳晶光电有限公司 Transversal epitaxial growth method for nano area of semiconductor film
JP2011073894A (en) * 2009-09-29 2011-04-14 Toyoda Gosei Co Ltd Method for producing group iii nitride compound semiconductor

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LIU ZHAN HUI ET AL: "Gallium Nitride Nanowires Grown by", 《CHINESE PHYSIES LETTERS》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014032465A1 (en) * 2012-08-31 2014-03-06 南京大学 METHOD FOR GROWING GaN NANOWIRE
CN103456602A (en) * 2013-03-18 2013-12-18 深圳信息职业技术学院 Method for preparing non-polar surface gallium nitride nanometer cone material
CN103456602B (en) * 2013-03-18 2016-12-07 深圳信息职业技术学院 The preparation method of non-polar surface gallium nitride nanometer cone material
CN107910243A (en) * 2017-10-18 2018-04-13 中国科学院半导体研究所 The method for preparing GaN nano wire on substrate
WO2021012496A1 (en) * 2019-07-22 2021-01-28 南京大学 Molecular beam epitaxial growth method for controlling structure and morphology of gan nanowire

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Application publication date: 20121219