CN102828250A - 一种GaN纳米线生长方法 - Google Patents
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- 239000002070 nanowire Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000012159 carrier gas Substances 0.000 claims abstract description 12
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 11
- 239000010980 sapphire Substances 0.000 claims abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 10
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 5
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 4
- XOYLJNJLGBYDTH-UHFFFAOYSA-M chlorogallium Chemical compound [Ga]Cl XOYLJNJLGBYDTH-UHFFFAOYSA-M 0.000 claims abstract description 4
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 22
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 claims description 14
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- 238000004140 cleaning Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
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- 238000000151 deposition Methods 0.000 description 2
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- 238000001451 molecular beam epitaxy Methods 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910002704 AlGaN Inorganic materials 0.000 description 1
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- C30B—SINGLE-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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/005—Growth of whiskers or needles
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
- C30B29/406—Gallium nitride
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Abstract
一种制备GaN纳米线的方法,蓝宝石衬底的清洗后,先蒸镀金属Ni薄膜;Ni薄膜厚度5-50nm;将覆有镍薄膜的蓝宝石衬底放入HVPE生长***中,开始低温生长GaN纳米线;生长温度:500–850℃;高纯N2作为载气,总N2载气流量1-5slm;Ga源采用常规的高纯金属镓和高纯HCl反应生成GaCl,HCl流量:1-20sccm,HCl载气流量10-200sccm;以高纯氨气作为氮源,NH3流量:50–500sccm;生长时间1-10分钟。生长出GaN纳米线。
Description
技术领域
本发明涉及一种用氢化物气相外延生长GaN纳米线的方法。
背景技术
以GaN及InGaN、AlGaN合金材料为主的III-V族氮化物材料(又称GaN基材料)是近几年来国际上倍受重视的新型半导体材料。GaN基材料是直接带隙宽禁带半导体材料,具有1.9—6.2eV之间连续可变的直接带隙,优异的物理、化学稳定性,高饱和电子漂移速度,高击穿场强和高热导率等优越性能,在短波长半导体光电子器件和高频、高压、高温微电子器件制备等方面具有重要的应用,用于制造比如蓝、紫、紫外波段发光器件、探测器件,高温、高频、高场大功率器件,场发射器件,抗辐射器件,压电器件等。
一维体系的纳米材料是可以有效传输电子和光学激子的最小维度结构,也是纳米机械器件和纳米电子器件的最基本结构单元。GaN材料作为重要半导体材料的优良特性使得一维GaN纳米结构在微纳光电器件、光电探测器件、电子器件、环境和医学等领域具有更广泛的的潜在应用前景,因此,制备性能优异、高质量的一维GaN纳米结构及特性研究就成为当前国际、国内研究的前沿课题。
GaN基材料的生长有很多种方法,如金属有机物气相外延(MOCVD)、高温高压合成体GaN单晶、分子束外延(MBE)、升华法以及氢化物气相外延(HVPE)等。GaN纳米结构的制备主要有各向异性可控生长法、VLS (Vapor– Liquid–Solid)和SLS(Solution–Liquid–Solid)机制生长法、模板辅助生长法、表面活性剂法、纳米粒子自组装及物理或化学方法剪切等。GaN纳米结构的生长可以采用多种方式如MOCVD、MBE等获得,但是此类设备价格成本高,源材料价格高昂。
本发明给出了一种采用金属镍(Ni)做催化剂,用氢化物气相外延(HVPE)设备生长GaN纳米线的方法及工艺。
发明内容
本发明目的是:提出一种用金属镍作为催化剂,在氢化物气相外延生长设备中生长GaN纳米线。能制备出性能优异、高质量的一维GaN纳米结构产品。
本发明的技术方案是,制备GaN纳米线的方法,利用氢化物气相外延(HVPE)设备生长GaN纳米线。以金属镍作催化剂,蓝宝石衬底的清洗后,先蒸镀金属Ni薄膜的;Ni薄膜沉积速率设置约为1-2埃/秒,Ni薄膜厚度5-50nm;将覆有金属镍薄膜的蓝宝石衬底放入HVPE生长***中,开始低温生长GaN纳米线;生长温度:500–850℃;高纯N2作为载气,总N2载气流量1-5slm;Ga源采用常规的高纯金属镓和高纯HCl反应生成GaCl,HCl流量:1-20sccm,HCl载气流量10-200sccm。高纯氨气作为氮源,NH3流量:50–500sccm;生长时间1-10分钟。
生长温度尤其是:500- 650℃。
金属镍作为催化剂时, GaN纳米线的HVPE为VLS机制。由于HVPE生长速率快(几百微米/小时),常用于快速生长厚膜。在本发明中, 需要控制生长条件,使得HVPE GaN生长速率降低,以获得GaN纳米线。本发明的技术方案为:用物理气相沉积的方法在蓝宝石衬底上蒸镀金属Ni,然后放入HVPE生长***中,低温生长 GaN纳米线。
本发明有益效果是:本发明给出了一种工艺简单、成本低廉的GaN纳米线生长方法和工艺。直径达到数十纳米,且长度可以达到数微米。
附图说明
图1为本发明实施例的产物照片。在其它参数不变的情况下, NH3流量变化制备GaN纳米线的形貌(图1在左中右三幅照片分别对应着 NH3流量的不同:即分别为50,100和200sccm。生长温度:550、600和650℃除纳米线径度外,外观无显著区别。
图2 为本发明实施例的产物照片。HVPE生长GaN纳米线的扫描电子显微镜照片,其中***图为高倍数照片。
具体实施方式
本发明方法和工艺包括几个部分:金属Ni薄膜在蓝宝石衬底上的物理气相沉积;GaN纳米线的HVPE低温生长。
本发明技术实施方式之一,HVPE技术制备GaN纳米线,包括下面几步:
1、 蓝宝石衬底的清洗和处理。将样品依次在去离子水、乙醇和去离子水中进行超声清洗,除去表面残留的污染物,用氮气吹干。
2、 蓝宝石衬底放入物理气相沉积装置反应腔内,在一定反应腔体压力和金属源温度下,即可开始金属Ni薄膜的蒸镀。Ni薄膜沉积速率设置约为1-2埃/秒,Ni纳米薄膜厚度5-50nm。 本实施例选择20-30nm。
3、 将覆有金属镍薄膜的蓝宝石衬底放入HVPE生长***中,开始低温生长GaN纳米线。生长温度:550、600和650℃三个温度条件;高纯N2作为载气,总N2载气流量1-5slm;高纯金属镓和高纯HCl反应生成GaCl作为镓源,HCl流量:1-20sccm,HCl载气流量10-200sccm。高纯氨气作为氮源,NH3流量(对应三种流量):50,100和200sccm;生长时间5分钟。
4、 按照步骤3生长完成后降温取出样品,即获得GaN纳米线。
5、 控制步骤2-4中的参数,可以实现金属Ni薄膜在纳米线生长温度时退火成有序颗粒,从而获得有序排列的GaN纳米线。
Claims (2)
1.一种制备GaN纳米线的方法,其特征是蓝宝石衬底的清洗后,先蒸镀金属Ni薄膜;Ni薄膜厚度5-50nm;将覆有镍薄膜的蓝宝石衬底放入HVPE生长***中,开始低温生长GaN纳米线;生长温度:500–850℃;高纯N2作为载气,总N2载气流量1-5slm;Ga源采用常规的高纯金属镓和高纯HCl反应生成GaCl,HCl流量:1-20sccm,HCl载气流量10-200sccm;以高纯氨气作为氮源,NH3流量:50–500sccm;生长时间1-10分钟。
2.根据权利要求1所述的用HVPE生长GaN纳米线,其特征是,生长温度是:500- 650℃。
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Cited By (4)
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CN103456602A (zh) * | 2013-03-18 | 2013-12-18 | 深圳信息职业技术学院 | 非极性面氮化镓纳米锥材料的制备方法 |
WO2014032465A1 (zh) * | 2012-08-31 | 2014-03-06 | 南京大学 | 一种GaN纳米线生长方法 |
CN107910243A (zh) * | 2017-10-18 | 2018-04-13 | 中国科学院半导体研究所 | 在衬底上制备GaN纳米线的方法 |
WO2021012496A1 (zh) * | 2019-07-22 | 2021-01-28 | 南京大学 | 一种控制GaN纳米线结构与形貌的分子束外延生长方法 |
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WO2021012496A1 (zh) * | 2019-07-22 | 2021-01-28 | 南京大学 | 一种控制GaN纳米线结构与形貌的分子束外延生长方法 |
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