WO2014032467A1 - 一种制备低应力GaN薄膜的方法 - Google Patents

一种制备低应力GaN薄膜的方法 Download PDF

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WO2014032467A1
WO2014032467A1 PCT/CN2013/077986 CN2013077986W WO2014032467A1 WO 2014032467 A1 WO2014032467 A1 WO 2014032467A1 CN 2013077986 W CN2013077986 W CN 2013077986W WO 2014032467 A1 WO2014032467 A1 WO 2014032467A1
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stress
composite substrate
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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
Nanjing Tech University
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Nanjing Tech University
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P50/00—Etching of wafers, substrates or parts of devices
    • H10P50/60—Wet etching
    • H10P50/64—Wet etching of semiconductor materials
    • H10P50/642—Chemical etching
    • H10P50/646—Chemical etching of Group III-V materials
    • H10P50/648—Anisotropic liquid etching

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  • the present invention relates to a method for etching and obtaining nanostructures of an electrodeless photo-assisted GaN material for reducing stress in a GaN film material grown by a hydride vapor phase epitaxy (HVPE) and a method and a process for obtaining a self-supporting GaN substrate.
  • HVPE hydride vapor phase epitaxy
  • III-V nitride materials (also known as GaN-based materials) mainly composed of GaN, InGaN, and AlGaN alloy materials are new semiconductor materials that have received international attention in recent years.
  • the GaN-based material is a direct bandgap wide bandgap semiconductor material with a continuously variable direct bandgap between 1.9 and 6.2 eV, excellent physical and chemical stability, high saturation electron drift velocity, high breakdown field strength and high thermal conductivity. Excellent performance such as high-frequency, high-frequency, high-frequency High field high power devices, field emission devices, radiation resistant devices, piezoelectric devices, etc.
  • GaN-based materials there are many methods for growing GaN-based materials, such as metal organic vapor phase epitaxy (MOCVD), high temperature and high pressure composite GaN single crystal, molecular beam epitaxy (MBE), sublimation, and hydride vapor phase epitaxy (HVPE). Due to the physical properties of the GaN-based material itself, the growth of the GaN bulk single crystal has great difficulty and has not yet been put into practical use. Hydride vapor phase epitaxy can be used for homoepitaxial growth of self-supporting GaN substrates due to its high growth rate and lateral-longitudinal epitaxy, which has attracted extensive attention and research.
  • MOCVD metal organic vapor phase epitaxy
  • MBE molecular beam epitaxy
  • HVPE hydride vapor phase epitaxy
  • the main method is to use a method of lateral epitaxy, suspension epitaxy, etc., to grow a thick film by HVPE high-rate epitaxy, and finally remove the original substrate, thereby obtaining a self-supporting GaN substrate material with a low dislocation density.
  • the self-supporting GaN substrate grown by HVPE has a dislocation density of less than 10 6 cm - 2 and an area of 2 inches. But still far from meeting the needs of practical applications.
  • GaN can only grow on a heterogeneous substrate such as sapphire, silicon or the like, lattice mismatch and thermal mismatch cause large stress inside the GaN film, which makes it difficult to improve the performance of the GaN-based device.
  • the large stress causes the GaN thick film and the heterogeneous substrate to be fragmented and thus cannot be applied. Therefore, reducing or eliminating the stress in the GaN thick film is an important solution to effectively realize the potential of the GaN material.
  • the invention provides a method for etching and obtaining nanostructures of an electrodeless photo-assisted GaN material and a method and a process for reducing stress in a GaN thin film material of a hydride-vapor phase epitaxy (HVPE) growth semiconductor material and obtaining a self-supporting GaN substrate.
  • HVPE hydride-vapor phase epitaxy
  • the object of the present invention is: Since existing GaN thin films are grown on a foreign substrate such as sapphire or the like, lattice mismatch and thermal mismatch cause a large stress in the GaN thin film. The presence of stress causes a decrease in the performance of the GaN-based material.
  • the present invention provides a method of obtaining a high quality low stress GaN film.
  • the technical solution of the present invention is a method for preparing a low-stress GaN film, which is characterized by photo-assisted etching of a GaN/sapphire composite substrate to form a nanostructured GaN/sapphire composite substrate; on the nanostructure composite substrate Conductive vapor phase epitaxy (HVPE) lateral epitaxial growth of GaN to obtain low-stress high-quality GaN film; photo-assisted etching using UV-assisted, etching solvent using a mixture of strong alkali and oxidant, ie molar concentration range of 0.5-1.5M
  • HVPE vapor phase epitaxy
  • etching solvent using a mixture of strong alkali and oxidant, ie molar concentration range of 0.5-1.5M
  • the nanostructured GaN/sapphire composite substrate is laterally epitaxially grown in an HVPE growth system to obtain a low stress GaN film.
  • the GaN film is etched by photo-assisted etching and nanostructured GaN is obtained.
  • the sample is irradiated with ultraviolet light.
  • the photons of the ultraviolet light should be able to excite electrons in the GaN, so that electrons are excited from the valence band to the conduction band, leaving holes in the valence band. Therefore, the energy of the ultraviolet light should be greater than 3.4 eV (corresponding to the forbidden band width of GaN, the corresponding ultraviolet light length is less than 365 nm, generally the ultraviolet wavelength used in this patent is in the range of 260-350 nm), and the holes contribute to the oxidation reaction of the semiconductor surface. Excess electrons are consumed by the reduction of the oxidant. Increasing the incident illumination increases the voids on the surface, thereby increasing the corrosion rate. At the same time accompanied by the recombination of electron holes.
  • the photoassisted etching of the present invention is wet etching of semiconductors, including the oxidation of the surface of the semiconductor and the dissolution of the generated oxide, the holes contributing to the oxidation reaction of the semiconductor surface, and the oxidizing agent replacing the reduction reaction of the cathode to consume excess electrons.
  • Increasing the incident illumination increases the voids on the surface, thereby increasing the corrosion rate.
  • Oxidizer requirements Strong oxidizing power, stable in alkali, dissolved Ga203.
  • the invention uses a photo-assisted electrodeless method to etch a GaN thin film/sapphire composite substrate material with a strong oxidizing agent to form a nano GaN structure (nanocolumn or nanodots). Place a composite substrate forming a nano-GaN structure in an HVPE reaction
  • the lateral epitaxial growth in the cavity (refer to the patent: "Transverse epitaxial growth of high-quality gallium nitride film", patent number ZL021113084.1), can be obtained low-stress GaN film.
  • the beneficial effects of the present invention are:
  • the present invention provides a method for etching and obtaining nanostructures of an electrodeless photo-assisted GaN material and reducing stress in a GaN thin film material of a hydride vapor phase epitaxy (HVPE) grown semiconductor material and obtaining a self-supporting GaN lining Bottom method and process.
  • HVPE hydride vapor phase epitaxy
  • FIG. 2 is a photomicrograph of a GaN nanostructure formed by a photo-assisted electrodeless etch of a GaN/sapphire sample according to an electron micrograph of an embodiment of the present invention.
  • the method and process of the present invention comprises several parts: photo-assisted electrodeless etching of GaN/sapphire composite substrates (referred to as GaN grown on sapphire substrates) to obtain GaN nanostructures; HVPE regrowth of low stress GaN films.
  • the distribution and scale of the nanostructured GaN pillar can be controlled (the more intense the corrosion, the longer the etching time, the thinner the size distribution of the GaN pillar and the smaller the scale), in the subsequent In the lateral epitaxy of HVPE, self-separation between the GaN film and the sapphire can also be achieved, thereby obtaining a low-stress self-supporting GaN substrate material.
  • a low stress GaN film is prepared, including the following steps:
  • the GaN/sapphire composite substrate is placed in a prepared etching solvent.
  • the corrosive materials used were analytically pure and dissolved in deionized water.
  • a mixture of 1 M KOH and B + 0.1 MK 2 S 2 0 8 was used as the etching solvent.
  • the etching process is carried out at room temperature without stirring the solution.
  • the UV power is 10-300W, the wavelength of the main peak of UV is shorter than 350nm; the corrosion time is 5 or 10 hours, in this case, 5 hours.
  • step 4 Place the sample in step 4 into a hydride vapor phase epitaxy apparatus for HVPE lateral epitaxial growth of GaN.
  • the specific method of lateral epitaxy can be referred to the patent: "Transverse epitaxial growth of high quality gallium nitride thin film", patent number ZL021113084.1.
  • step 6 Remove the sample from step 5 to obtain a high quality low stress GaN film.
  • steps 2-6 the separation between the GaN film and the sapphire can be achieved, thereby obtaining a self-supporting low stress GaN substrate material.

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Abstract

一种制备低应力GaN薄膜的方法，通过光助法腐蚀溶剂腐蚀GaN/蓝宝石复合衬底，形成纳米结构的GaN/蓝宝石复合衬底；光助法腐蚀采用紫外光辅助腐蚀，腐蚀溶剂采用强碱和氧化剂混合溶液，即NaOH或KOH摩尔浓度范围为0.5-1.5M与K2S2O8的混和物摩尔浓度范围为0.05-0.15M，在室温或50°C以下的温度，反应时间为0.5-10小时；得到纳米结构GaN/蓝宝石复合衬底。本发明用于降低氢化物气相外延（HVPE）生长半导体材料GaN薄膜材料中应力。

Description

一种制备低应力 GaN薄膜的方法 技术领域
本发明涉及一种无电极光助 GaN材料腐蚀并获得纳米结构的方法， 用于降低氢化物 气相外延 （HVPE)生长半导体材料 GaN薄膜材料中应力和获得自支撑 GaN衬底的方法 以及工艺。 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 1.9一 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。
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。 由于 GaN基材料本身物理性质的限制， GaN体单晶的生长具有很大的困难， 尚未实用化。 氢化物气相外延由于具有高的生长率和横向-纵向外延比， 可用于同质外延生长自支撑 GaN 衬底， 引起广泛地重视和研究。 早期人们主要采用氢化物气相外延 （HVPE) 方法 在蓝宝石衬底上直接生长 GaN基材料， 再加以分离， 获得 GaN衬底材料。 此法的突出 缺点是 GaN外延层中位错密度很高， 一般达 101Qcm- 2左右。 目前的主要方法是采用横向 外延、 悬挂外延等方法， 辅以 HVPE高速率外延技术生长厚膜， 最后将原衬底去除， 从 而获得位错密度较低的自支撑 GaN衬底材料。 迄今为止， HVPE生长得到的自支撑 GaN 衬底， 位错密度低于 106cm- 2， 面积已经达到 2英寸。 但是仍然远远不能满足实际应用的 需求。
由于 GaN只能生长在异质衬底如蓝宝石、硅等衬底上， 晶格失配和热失配造成 GaN 薄膜内部具有大的应力， 造成 GaN基器件性能很难提高。 另外， 巨大的应力会造成 GaN 厚膜和异质衬底裂成碎片， 因而无法应用。 因此降低或者消除 GaN厚膜中的应力， 是有 效发挥 GaN材料潜能的重要解决方法。 本发明给出了一种无电极光助 GaN材料腐蚀并 获得纳米结构的方法以及降低氢化物气相外延 （HVPE) 生长半导体材料 GaN薄膜材料 中应力和获得自支撑 GaN衬底的方法以及工艺。 发明内容
本发明目的是： 由于现有的 GaN薄膜生长在异质衬底如蓝宝石等上面， 晶格失配和 热失配会引起 GaN薄膜中存在较大的应力。 应力的存在会造成 GaN基材料性能的降低。 本发明提出一种获得高质量低应力 GaN薄膜的方法。
本发明的技术方案是， 一种制备低应力 GaN薄膜的方法， 通过光助法腐蚀溶剂腐蚀 GaN/蓝宝石复合衬底， 形成纳米结构的 GaN/蓝宝石复合衬底； 在此纳米结构复合衬底上 进行 GaN的氢化物气相外延 （HVPE)横向外延生长得到低应力高质量的 GaN薄膜； 光 助法腐蚀采用紫外光辅助， 腐蚀溶剂采用强碱和氧化剂混合溶液， 即摩尔浓度范围为 0.5-1.5M的 aOH或 KOH与摩尔浓度范围为 0.05-0. 15M的 K2S208的混和物， 在室温或 50°C以下的温度， 反应时间为 0.5-10小时。。
所述的纳米结构 GaN/蓝宝石复合衬底放在 HVPE生长系统中进行横向外延生长，得 到低应力 GaN薄膜。
采用光助腐蚀的方法腐蚀 GaN薄膜并获得纳米结构的 GaN。在光助腐蚀中， 向样品 上照射紫外光。该紫外光的光子应能在 GaN中激发电子一空穴即需把电子从价带激发到 导带之上， 而在价带中留下空穴。 因此紫外光的能量应大于 3.4eV (对应 GaN的禁带宽 度， 相对应紫外光长小于 365nm， 一般本专利所用的紫外线波长在 260-350nm范围）， 空 穴有助于半导体表面的氧化反应， 通过氧化剂的还原来消耗过剩电子。 增加入射光照， 增加表面的空穴， 从而提高腐蚀速率。 同时伴随着电子空穴的复合。
本发明光助法腐蚀是半导体湿腐蚀， 包括对半导体表面的氧化和产生的氧化物的溶 解， 空穴有助于半导体表面的氧化反应， 氧化剂代替阴极的还原反应， 来消耗过剩电子。 增加入射光照， 增加表面的空穴， 从而提高腐蚀速率。 氧化剂的要求： 强氧化能力， 碱 液中稳定， 溶解 Ga203。
光助无电极化学腐蚀机理- -化学方程式
GaN + photon → GaN + e~ + h** (I )
GAN + 6h" + m -→ ( a203 + 3H20 + N2, {2}
( ( -f- (()H ― 2GaC)| + 3¾0， (3)
Figure imgf000004_0001
本发明用光助无电极方法，用强氧化剂腐蚀 GaN薄膜 /蓝宝石复合衬底材料，形成纳 米 GaN结构 （纳米柱或者纳米点）。 将形成纳米 GaN结构的复合衬底放置在 HVPE反应 腔中进行横向外延生长 （参考专利： 《横向外延技术生长高质量氮化镓薄膜》， 专利号 ZL021113084.1 ), 即可得到低应力 GaN薄膜。
本发明的有益效果是： 本发明给出了一种无电极光助 GaN材料腐蚀并获得纳米结构 的方法以及降低氢化物气相外延 （HVPE) 生长半导体材料 GaN薄膜材料中应力和获得 自支撑 GaN衬底的方法以及工艺。
附图说明
图 1 光助腐蚀的基本原理图
图 2 为本发明实施例的电镜照片， GaN/蓝宝石样品在光助无电极腐蚀后形成的 GaN 纳米结构形貌。
具体实施方式
本发明方法和工艺包括几个部分： GaN/蓝宝石复合衬底（指在蓝宝石衬底上生长的 GaN) 的光助无电极腐蚀得到 GaN纳米结构； 低应力 GaN薄膜的 HVPE再生长。
进一步的， 通过腐蚀时间和溶剂浓度等的选择， 可以控制纳米结构的 GaN柱的分布 和尺度 （腐蚀愈剧烈、 腐蚀时间愈长则 GaN柱的尺寸分布愈稀且尺度愈小）， 在随后的 HVPE横向外延中， 也可以实现 GaN薄膜和蓝宝石之间的自分离， 从而获得低应力自支 撑 GaN衬底材料。
本发明技术实施方式之一， 制备低应力 GaN薄膜， 包括下面几步：
1、 GaN/蓝宝石复合衬底的清洗和处理。 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、 GaN/蓝宝石复合衬底放入配制的腐蚀溶剂中。所采用的腐蚀材料是分析纯的， 溶于去离子水中。 实施例中采用的是 1 M的 KOH 禾 B+0.1 M K2S208的混合液 为腐蚀溶剂。
3、 调整紫外光照射样品的角度， 距离和紫外光功率， 进行蓝宝石衬底上 GaN腐 蚀， 腐蚀过程在室温下进行， 不搅拌溶液。 紫外光功率 10-300W, 紫外的主 峰的波长短于 350nm; 腐蚀时间 5或 10小时均可， 本例中取 5小时。
4、 将上述步骤 3 中的样品取出， 依次在去离子水、 乙醇和去离子水中进行超声 清洗， 用氮气吹干。
5、 将步骤 4 中的样品放入氢化物气相外延设备中， 进行 HVPE 横向外延生长 GaN。 横向外延的具体方法可参考专利： 《横向外延技术生长高质量氮化镓薄 膜》， 专利号 ZL021113084.1。
6、 将步骤 5中样品取出， 即获得高质量低应力 GaN薄膜。 控制步骤 2-6中的参数， 可以实现 GaN薄膜和蓝宝石之间的分离， 从而获 自支撑低应力 GaN衬底材料。

Claims

权利要求书
1、 一种制备低应力 GaN薄膜的方法， 其特征是通过光助法腐蚀溶剂腐蚀 GaN/蓝宝 石复合衬底， 形成纳米结构的 GaN/蓝宝石复合衬底； 光助法腐蚀采用紫外光辅助腐蚀， 腐蚀溶剂采用强碱和氧化剂混合溶液， 即摩尔浓度范围为 0.5-1.5M的 NaOH或 KOH与 摩尔浓度范围为 0.05-0. 15M K2S208混和物， 在室温或 50°C以下的温度， 反应时间为 0.5- 10小时； 得到纳米结构 GaN/蓝宝石复合衬底。
2、 根据权利要求 1 所述的制备低应力 GaN 薄膜的方法， 其特征是所述的纳米结构 GaN/蓝宝石复合衬底放在 HVPE生长系统中进行横向外延生长， 得到低应力 GaN薄膜。
3、 根据权利要求 1所述的制备低应力 GaN薄膜的方法， 其特征是紫外光的能量应大 于 3.4eV， 对应 GaN的禁带宽度， 相对应紫外光波长小于 365nm。
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