CN106783948B - 生长在Si衬底上的InN纳米柱外延片及其制备方法 - Google Patents
生长在Si衬底上的InN纳米柱外延片及其制备方法 Download PDFInfo
- Publication number
- CN106783948B CN106783948B CN201611166965.3A CN201611166965A CN106783948B CN 106783948 B CN106783948 B CN 106783948B CN 201611166965 A CN201611166965 A CN 201611166965A CN 106783948 B CN106783948 B CN 106783948B
- Authority
- CN
- China
- Prior art keywords
- substrate
- inn
- nano
- pillar
- epitaxial wafer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000758 substrate Substances 0.000 title claims abstract description 80
- 239000002061 nanopillar Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 31
- 229910052751 metal Inorganic materials 0.000 claims abstract description 31
- 239000004005 microsphere Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 abstract description 14
- 239000004065 semiconductor Substances 0.000 abstract description 12
- 230000007547 defect Effects 0.000 abstract description 5
- 230000005855 radiation Effects 0.000 abstract description 4
- 239000000969 carrier Substances 0.000 abstract description 3
- 230000006798 recombination Effects 0.000 abstract description 3
- 238000005215 recombination Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- NWAIGJYBQQYSPW-UHFFFAOYSA-N azanylidyneindigane Chemical compound [In]#N NWAIGJYBQQYSPW-UHFFFAOYSA-N 0.000 description 54
- 229910052594 sapphire Inorganic materials 0.000 description 4
- 239000010980 sapphire Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 239000011807 nanoball Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/06—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions
- H01L29/0657—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by the shape of the body
- H01L29/0665—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by the shape of the body the shape of the body defining a nanostructure
- H01L29/0669—Nanowires or nanotubes
- H01L29/0676—Nanowires or nanotubes oriented perpendicular or at an angle to a substrate
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/02373—Group 14 semiconducting materials
- H01L21/02381—Silicon, silicon germanium, germanium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02439—Materials
- H01L21/02491—Conductive materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02494—Structure
- H01L21/02513—Microstructure
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02538—Group 13/15 materials
- H01L21/0254—Nitrides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/20—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only AIIIBV compounds
- H01L29/2003—Nitride compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Computer Hardware Design (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
本发明公开了生长在Si衬底上的InN纳米柱外延片，由下至上依次包括Si衬底、In金属纳米微球层和InN纳米柱层。所述In金属纳米微球层中的In金属纳米微球的直径为20‑70nm。所述InN纳米柱层中InN纳米柱直径为40‑80nm。本发明还公开了生长在Si衬底上的InN纳米柱外延片的制备方法。本发明的纳米柱直径均一，同时解决了InN因与Si之间存在较大晶格失配而在其中产生大量位错的技术难题，大大减少了InN纳米柱外延层的缺陷密度，有利提高了载流子的辐射复合效率，可大幅度提高氮化物器件如半导体激光器、发光二极管的发光效率。
Description
技术领域
本发明涉及InN纳米柱外延片及制备方法，特别涉及生长在Si衬底上的InN纳米柱外延片及其制备方法。
背景技术
III-V族氮化物由于稳定的物理化学性质、高的热导率和高的电子饱和速度等优点，广泛应用于发光二极管(LED)、激光器和光电子器件等方面。在III-V族氮化物中，氮化铟(InN)由于其自身独特的优势而越来越受到研究者的关注。在III族氮化物半导体中，InN具有最小的有效电子质量、最高的载流子迁移率和最高饱和渡越速度，对于发展高速电子器件极为有利。不仅如此，InN具有最小的直接带隙，其禁带宽度约为0.7eV，这就使得氮化物基发光二极管的发光范围从紫外(6.2eV)拓宽至近红外区域(0.7eV)，在红外激光器、全光谱显示及高转换效率太阳电池等方面展示了极大的应用前景。与其他III-V族氮化物半导体材料相比，InN材料除具有上述优点外，其纳米级的材料在量子效应、界面效应、体积效应、尺寸效应等方面还表现出更多新颖的特性。
目前，III-V族氮化物半导体器件主要是基于蓝宝石衬底上外延生长和制备。然而，蓝宝石由于热导率低，以蓝宝石为衬底的大功率氮化物半导体器件产生的热量无法有效释放，导致热量不断累计使温度上升，加速氮化物半导体器件的劣化，存在器件性能差、寿命短等缺点。相比之下，Si的热导率比蓝宝石高，且成本较低。在Si衬底上制备高性能、低成本的氮化物半导体器件是必然的发展趋势。然而，在Si衬底上生长直径均一、有序性高的InN纳米柱是制备高性能氮化物半导体光电器件的先提条件。由于Si与InN之间的晶格失配和热失配大；同时，在生长初期，衬底表面的In和N原子分布比例的差异，导致生长的InN纳米柱会有高度、径长不均匀、有序性差等情况。
目前多数采用在Si衬底上直接生长InN纳米柱，这种生长方法所获得的纳米柱直径不均一，也就是顶部和底部的直径不一致，呈倒金字塔、垒球棒等形貌的纳米柱。若采用In、Ni、Au等作为催化剂进行InN纳米柱的生长，作为催化剂的In、Ni和Au等金属在生长后存在于InN的顶端，在后续进行器件制作时，需要把顶端的金属催化剂去除，增加了器件工艺的复杂性。
发明内容
为了克服现有技术的上述缺点与不足，本发明的目的在于提供一种生长在Si衬底上的InN纳米柱外延片，通过Si衬底上的In金属纳米微球，首先，In金属纳米微球作为在InN纳米柱生长过程中的In补充源，有利于高有序性、直径均一InN纳米柱的形核与生长；其次，解决了InN因与Si之间存在较大晶格失配而在其中产生大量位错的技术难题，大大减少了InN纳米柱外延层的缺陷密度，有利提高了载流子的辐射复合效率，可大幅度提高氮化物器件如半导体激光器、发光二极管的发光效率。
本发明的另一目的在于提供上述生长在Si衬底上的InN纳米柱外延片的制备方法，具有生长工艺简单，纳米柱形貌可控、制备成本低廉的优点。
本发明的目的通过以下技术方案实现：
生长在Si衬底上的InN纳米柱外延片，由下至上依次包括Si衬底、In金属纳米微球层和InN纳米柱层。
所述In金属纳米微球层中的In金属纳米微球的直径为20-70nm。
所述InN纳米柱层中InN纳米柱直径为40-80nm。
所述的生长在Si衬底上的InN纳米柱外延片的制备方法，包括以下步骤：
(1)Si衬底清洗；
(2)沉积In金属纳米微球层：采用分子束外延生长工艺，衬底温度控制在400-550℃，在反应室的压力为5.0～6.0×10-10Torr条件下，在Si衬底上沉积In薄膜，并退火，得到In金属纳米微球；
(3)InN纳米柱层的生长：采用分子束外延生长工艺，衬底温度控制在500～700℃，在反应室的压力为4.0～10.0×10-5Torr，束流比V/III值为30～40条件下，在步骤(2)得到的In金属纳米微球上生长直径均一的InN纳米柱。
步骤(2)中退火的温度为400-550℃，退火时间为50-300秒。
步骤(1)所述衬底清洗，具体为：
将Si衬底放入体积比为1:20的HF和去离子水混合溶液中超声1～2分钟，去除硅衬底表面氧化物和粘污颗粒，再放入去离子水中超声1～2分钟，去除表面杂质，用高纯干燥氮气吹干。
所述In金属纳米微球层中的In金属纳米微球的直径为20-70nm。
所述InN纳米柱层中InN纳米柱直径为40-80nm。
与现有技术相比，本发明具有以下优点和有益效果：
(1)本发明的生长在Si衬底上的InN纳米柱外延片，通过Si衬底上的In金属纳米微球，解决了InN因与Si之间存在较大晶格失配而在其中产生大量位错的技术难题，大大减少了InN纳米柱外延层的缺陷密度，有利提高了载流子的辐射复合效率，可大幅度提高氮化物器件如半导体激光器、发光二极管的发光效率。
(2)本发明的生长在Si衬底上的InN纳米柱外延片，采用Si衬底，Si衬底具有容易去除的优点，在去除Si衬底后的InN纳米柱半导体外延片上制作电极，有利于制备垂直结构的氮化物半导体器件。同时Si衬底有抗辐射、热导率高、耐高温、化学性质较稳定、强度较高等优点，具有很高的可靠性，基于Si衬底的InN纳米柱外延片可广泛应用于高温器件。
(3)本发明使用Si作为衬底，采用分子束外延技术先在Si衬底上沉积In并退火形成In金属纳米微球，预沉积在Si衬底上的In金属纳米微球作为在InN纳米柱生长过程中的In补充源，避免InN纳米柱在生长过程中由于In源不足导致出现顶部直径大于底部直径，直径不均一的纳米柱，有利于高有序性、直径均一InN纳米柱的形核与生长，解决了在Si衬底上难以直接生长直径均一InN纳米柱的技术难题。
(4)本发明的生长工艺独特而简单易行，具有可重复性。
附图说明
图1为本发明的生长在Si衬底上的InN纳米柱外延片的结构示意图。
图2为本发明的实施例1在Si衬底上沉积In金属纳米微球的扫描电子显微镜照片。
图3为本发明的实施例1在Si衬底上的In金属纳米微球层上沉积得到的InN纳米柱的扫描电子显微镜照片。
图4为在Si衬底上直接生长InN纳米柱的截面扫描电子显微镜照片。
具体实施方式
下面结合实施例，对本发明作进一步地详细说明，但本发明的实施方式不限于此。
实施例1
图1为本实施例的生长在硅衬底上的InN纳米柱外延片的结构示意图，由下至上依次包括Si衬底1、In金属纳米微球层2和InN纳米柱层3。
本实施例的生长在硅衬底上的InN纳米柱外延片的制备方法，包括以下步骤：
(1)衬底以及其晶向的选取：采用普通Si衬底；
(2)衬底清洗：将Si衬底放入体积比为1:20的HF和去离子水混合溶液中超声2分钟，去除Si衬底表面氧化物和粘污颗粒，再放入去离子水中超声2分钟，去除表面杂质，用高纯干燥氮气吹干；
(3)沉积In金属纳米微球：采用分子束外延生长工艺，衬底温度控制在400℃，在反应室的压力为6.0×10-10Torr条件下，在Si衬底上沉积In薄膜，并在原位退火50秒，形成直径为30-50nm的In金属纳米微球。
(4)直径均一InN纳米柱的生长：采用分子束外延生长工艺，衬底温度控制在600℃，在反应室的压力为6.0×10-5Torr，束流比V/III值为30条件下，在步骤(3)得到的In金属纳米微球的Si衬底上生长顶部和底部直径均一、直径分布为30-80nm的InN纳米柱。
如图2所示，本实施例在Si衬底上预沉积In金属纳米微，其直径为30-50nm的In金属纳米微球扫描电子显微镜照片。
图3是实施例1在Si衬底上生长高有序性、直径均一、顶部无金属In残留的InN纳米柱扫描电子显微镜照片，显示出了本发明制备的InN纳米柱外延片性能优异。而在Si衬底上直接生长InN纳米柱的截面扫描电子显微镜照片如图4所示，可知，采用在Si衬底上直接生长InN纳米柱的生长方法所获得的纳米柱直径不均一，也就是顶部和底部的直径不一致，呈倒金字塔、垒球棒等形貌的纳米柱。
实施例2
本实施例的生长在硅衬底上的InN纳米柱外延片由下至上依次包括Si衬底、In金属纳米微球层和InN纳米柱层。
本实施例的生长在Si衬底上的GaN纳米柱LED外延片的制备方法，包括以下步骤：
(1)衬底以及其晶向的选取：采用普通Si衬底；
(2)衬底清洗：将Si衬底放入体积比为1:20的HF和去离子水混合溶液中超声2分钟，去除硅衬底表面氧化物和粘污颗粒，再放入去离子水中超声1分钟，去除表面杂质，用高纯干燥氮气吹干；
(3)沉积In金属纳米微球：采用分子束外延生长工艺，衬底温度控制在550℃，在反应室的压力为6.0×10-10Torr条件下，在Si衬底上沉积In薄膜，并在原位退火300秒，形成直径为50-70nm的In金属纳米微球。
(4)直径均一InN纳米柱的生长：采用分子束外延生长工艺，衬底温度控制在700℃，在反应室的压力为6.0×10-5Torr，束流比V/III值为40条件下，在步骤(3)得到的In金属纳米微球的Si衬底上生长顶部和底部直径均一、直径分布为30-80nm的InN纳米柱。
本实施例制备的Si衬底上的InN纳米柱外延片无论是在电学性质、光学性质上，还是在缺陷密度、结晶质量都具有非常好的性能，测试数据与实施例1相近，在此不再赘述。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受所述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (3)
1.生长在Si衬底上的InN纳米柱外延片的制备方法，其特征在于，包括以下步骤：
(1)Si衬底清洗；
(2)沉积In金属纳米微球层：采用分子束外延生长工艺，衬底温度控制在400°C，在反应室的压力为6.0×10-10Torr条件下，在Si衬底上沉积In薄膜，并原位退火，得到直径为30-50nm 的In金属纳米微球；所述退火的温度为400°C，退火时间为50秒；
(3)InN纳米柱层的生长：采用分子束外延生长工艺，衬底温度控制在500～700°C，在反应室的压力为4.0～10.0×10-5Torr，束流比V/III值为30～40条件下，在步骤(2)得到的In金属纳米微球上生长直径均一的InN纳米柱。
2.根据权利要求1所述的生长在Si衬底上的InN纳米柱外延片的制备方法，其特征在于，步骤(1)所述Si衬底清洗，具体为：
将Si衬底放入体积比为1:20的HF和去离子水混合溶液中超声1～2分钟，去除硅衬底表面氧化物和粘污颗粒，再放入去离子水中超声1～2分钟，去除表面杂质，用高纯干燥氮气吹干。
3.根据权利要求1所述的生长在Si衬底上的InN纳米柱外延片的制备方法，其特征在于，所述InN纳米柱层中InN纳米柱直径为40-80nm。
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611166965.3A CN106783948B (zh) | 2016-12-16 | 2016-12-16 | 生长在Si衬底上的InN纳米柱外延片及其制备方法 |
| PCT/CN2017/090006 WO2018107713A1 (zh) | 2016-12-16 | 2017-06-26 | 生长在Si衬底上的InN纳米柱外延片及其制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611166965.3A CN106783948B (zh) | 2016-12-16 | 2016-12-16 | 生长在Si衬底上的InN纳米柱外延片及其制备方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106783948A CN106783948A (zh) | 2017-05-31 |
| CN106783948B true CN106783948B (zh) | 2023-08-22 |
Family
ID=58891924
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611166965.3A Active CN106783948B (zh) | 2016-12-16 | 2016-12-16 | 生长在Si衬底上的InN纳米柱外延片及其制备方法 |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN106783948B (zh) |
| WO (1) | WO2018107713A1 (zh) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106783948B (zh) * | 2016-12-16 | 2023-08-22 | 华南理工大学 | 生长在Si衬底上的InN纳米柱外延片及其制备方法 |
| CN107731975B (zh) * | 2017-10-24 | 2023-10-31 | 江门市奥伦德光电有限公司 | 一种纳米管led及其制作方法 |
| CN108206130B (zh) * | 2018-01-11 | 2023-10-10 | 华南理工大学 | 生长在铝箔衬底上的氮化铟纳米柱外延片及其制备方法 |
| CN108231545B (zh) * | 2018-01-11 | 2020-09-22 | 华南理工大学 | 生长在铜箔衬底上的InN纳米柱外延片及其制备方法 |
| CN108735866A (zh) * | 2018-07-20 | 2018-11-02 | 华南理工大学 | 生长在Si/石墨烯复合衬底上InN纳米柱外延片及其制备方法 |
| CN110747506A (zh) * | 2019-10-22 | 2020-02-04 | 华南理工大学 | 一种过渡金属掺杂的InxGa1-xN纳米柱及其制备方法与应用 |
| CN114657534B (zh) * | 2022-02-18 | 2023-06-16 | 华南理工大学 | 一种基于MoS2上的InN纳米柱及其制备方法与应用 |
| CN114657641A (zh) * | 2022-02-22 | 2022-06-24 | 华南理工大学 | 一种退火处理的Si基InN纳米柱异质结及其制备方法与应用 |
| CN114921804B (zh) * | 2022-04-26 | 2023-06-20 | 华南理工大学 | 一种基于InN/有机异质结构光电极材料及其制备方法与应用 |
| CN114875493B (zh) * | 2022-04-29 | 2023-08-18 | 华南理工大学 | 一种Si衬底上的InN-ⅥA族异质结及其制备方法与应用 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7745315B1 (en) * | 2007-10-03 | 2010-06-29 | Sandia Corporation | Highly aligned vertical GaN nanowires using submonolayer metal catalysts |
| CN102201332A (zh) * | 2011-05-08 | 2011-09-28 | 北京燕园中镓半导体工程研发中心有限公司 | 一种GaN衬底的制备方法 |
| CN102842490A (zh) * | 2012-08-17 | 2012-12-26 | 马鞍山圆融光电科技有限公司 | 一种化合物半导体薄膜的自组装生长方法 |
| CN206271710U (zh) * | 2016-12-16 | 2017-06-20 | 华南理工大学 | 生长在Si衬底上的InN纳米柱外延片 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103050350A (zh) * | 2012-12-28 | 2013-04-17 | 青岛润鑫伟业科贸有限公司 | 一种场发射阴极的制备方法 |
| CN106783948B (zh) * | 2016-12-16 | 2023-08-22 | 华南理工大学 | 生长在Si衬底上的InN纳米柱外延片及其制备方法 |
-
2016
- 2016-12-16 CN CN201611166965.3A patent/CN106783948B/zh active Active
-
2017
- 2017-06-26 WO PCT/CN2017/090006 patent/WO2018107713A1/zh active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7745315B1 (en) * | 2007-10-03 | 2010-06-29 | Sandia Corporation | Highly aligned vertical GaN nanowires using submonolayer metal catalysts |
| CN102201332A (zh) * | 2011-05-08 | 2011-09-28 | 北京燕园中镓半导体工程研发中心有限公司 | 一种GaN衬底的制备方法 |
| CN102842490A (zh) * | 2012-08-17 | 2012-12-26 | 马鞍山圆融光电科技有限公司 | 一种化合物半导体薄膜的自组装生长方法 |
| CN206271710U (zh) * | 2016-12-16 | 2017-06-20 | 华南理工大学 | 生长在Si衬底上的InN纳米柱外延片 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106783948A (zh) | 2017-05-31 |
| WO2018107713A1 (zh) | 2018-06-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106783948B (zh) | 生长在Si衬底上的InN纳米柱外延片及其制备方法 | |
| CN108206130B (zh) | 生长在铝箔衬底上的氮化铟纳米柱外延片及其制备方法 | |
| US10177275B2 (en) | Epitaxial structure and method for making the same | |
| US9070794B2 (en) | Method for making light emitting diode | |
| CN106981549B (zh) | 生长在硅衬底上的氮化镓纳米柱led外延片及其制备方法 | |
| US20140306256A1 (en) | Light emitting diode | |
| CN107046088B (zh) | 生长在Si(111)衬底上的GaN纳米柱及其制备方法和应用 | |
| CN108231545B (zh) | 生长在铜箔衬底上的InN纳米柱外延片及其制备方法 | |
| CN206271710U (zh) | 生长在Si衬底上的InN纳米柱外延片 | |
| CN105088181A (zh) | 一种硅基量子点激光器材料的mocvd制备方法 | |
| CN101807648B (zh) | 引入式粗化氮极性面氮化镓基发光二极管及其制作方法 | |
| CN104952987B (zh) | 发光二极管 | |
| CN208157359U (zh) | 生长在铝箔衬底上的氮化铟纳米柱外延片 | |
| CN109003888A (zh) | 硅/石墨烯复合衬底上外延生长GaN纳米柱及制备方法 | |
| CN108735866A (zh) | 生长在Si/石墨烯复合衬底上InN纳米柱外延片及其制备方法 | |
| CN201956386U (zh) | 一种发光二极管结构 | |
| CN207834252U (zh) | 生长在铜箔衬底上的InN纳米柱外延片 | |
| CN106601887B (zh) | 生长在玻璃衬底上的GaN薄膜及其制备方法 | |
| CN117374183A (zh) | 一种基于高温难熔金属衬底外延生长GaN进而制备LED的方法 | |
| CN104733580A (zh) | 一种以硅烯作为缓冲层外延GaN的结构及其制备方法 | |
| CN115020556A (zh) | 制备高发光效率AlGaN纳米柱LED结构的方法 | |
| CN111146299A (zh) | 一种p型AlN薄膜及其制备方法与应用 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |