GaN纳米材料的CVD制备与研究
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摘要
氮化镓(GaN)是宽带隙Ⅲ-Ⅴ族化合物半导体材料的代表,其禁带宽度为Eg=3.4eV,具有高饱和电子漂移速度、高热导率、耐高温、抗辐射、耐酸碱、高硬度等特性,是制作高效率蓝绿光发光二极管、蓝光半导体激光器、高频大功率场效应晶体管和紫外光探测器等半导体器件的首选材料。在实际应用中通常使用的GaN材料为薄膜形式,研究人员尝试用不同方法来制备GaN薄膜,最早出现的是氢化物气相外延生长(HVPE),随后是金属有机气相沉积(MOCVD)和分子束外延生长(MBE)。近年来出现的一些新型方法有电泳沉积(EPD)、脉冲激光沉积(PLD)、磁控溅射(MS)、溶胶-凝胶(Sol-Gel)等。本文中实验均采用设备简单、成本低廉、操作容易的化学气相沉积法(APCVD)。通过HRXRD、FESEM、AFM、EDS、PL等测试手段对样品的结构、形貌及光学性能等特性进行了表征,通过对测试结果的分析,不断优化制备工艺,提高产物性能。
目前,除GaN衬底外,其他衬底与GaN纳米材料之间均存在晶格失配和热膨胀系数失配,因此,采用合适的衬底并借助缓冲层成了研究者关注的热点。本论文中实验采用常压化学气相沉积法在不同衬底、不同缓冲层上制备GaN薄膜,分析了合成产物的组分、结构和光学性质,探讨了所得产物的生长机理与影响因素。
除了GaN薄膜材料外,其他形貌的GaN微纳米材料也被应用于光电子器件。本文采用简单的CVD方法,以金膜和铟丝作辅助剂,在硅衬底上以双催化剂模式生长GaN微纳材料。在此过程中,出现了不同形貌的GaN微纳米材料,并研究了产物的结构、辅助剂的作用及其生长机理。
1、以金属镓和氨气为原料,分别在Si、Al2O3和GaAs三种衬底上生长GaN薄膜。由于GaAs衬底的热稳定性不好,而氨气的分解温度在850℃左右,因此实验选择在870℃下进行。分析结果表明产物均为六方纤锌矿多晶结构,其中Al2O3衬底上所得薄膜的结晶质量和发光性能最好,而GaAs衬底上所得薄膜出现脱层。
2、以金属镓和氨气为原料,金属Al和Au/Al为缓冲层,在1000℃下生长GaN薄膜。分析结果表明加入金属缓冲层后所得的GaN薄膜的致密度、结晶性能、发光强度都有所改善。
3、以金属镓和氨气为原料,金和铟为辅助剂,在双辅助剂的生长模式下合成GaN微纳材料,出现了各种不同形貌的GaN微纳米材料。考察了辅助剂、反应时间、反应温度、氨气流量对产物的影响。
Ⅲ-Ⅴcompound semiconductor materials with wide band gap is represented by gallium initride (GaN), whoes energy band gap is 3.4eV. Due to the high saturated electronic drift velocity, high thermal conductivity, resistance to high temperature, rad resistance, resistance to acid and alkali, high hardness features, etc.. It is used to make the semiconductor devices, such as efficient blue-green light emitting diodes, blue-ray semiconductor laser, high power-high frequency Field Effect Transistors, and ultraviolet detectors. The GaN film is mainly used in practice. The researchers tried to produce the GaN films by different methods. HVPE was the earliest, and then MOCVD and MBE were used.At present, some new methods appear, such as electrophoresis deposition (EPD), pulse laser deposition (PLD), magnetron sputtering (MS), sol-gel (Sol-Gel), etc.. In this paper, chemical vapor deposition (CVD) with simple equipment, low cost and easy operation was adopted. The crystalline phase, structure, composition, morphology, and optical property of each sample were analyzed using High-Resolution X-Ray Diffraction (HRXRD), Field Emission Scanning Electron Microscope (FESEM), Atomic Force Microscopy (AFM), Energy Dispersive X-Ray Spectroscopy (EDS), and Photoluminescence (PL). Through the test results, we constantly optimized the preparation process to improve performance of products.
Currently, except the GaN substrate, lattice mismatch and thermal expansion coefficient mismatch exist between other substrates and GaN nanomaterials. Therefore, the use of appropriate substract and buffer layer becomes the focus of attention of researchers. GaN films were deposited on different substrates and different GaN buffer layers by atmospheric pressure chemical vapor deposition (APCVD). The structure, composition and optical property of each sample were analyzed and the growth mechanism and influencing factors were discussed.
In addition to GaN films, micro-nano materials with other morphologies also are applied in light-electronic devices. In this study, GaN micro/nano materials were prepared on Si (100) substrate by CVD with double catalyst mode using Au film and indium silk as auxiliaries. In the process, GaN micro/nano materials with different morphologies was obtained and the structure, catalyst role and growth mechanisms of the products were analyzed.
1. The polycrystal GaN films were produced using gallium and ammonia as raw materials, Si, Al2O3 and GaAs as substrates. Due to the bad thermal stability of GaAs substrate and 850℃decomposition temperature of ammonia gas, the experiment was done under the temperature less than 870℃. The results showed that the product was polycrystal with six-party fine zinc mine structure. The crystallization property and optical property of GaN films on Al2O3 substrate were best; but GaN film on GaAs substrate was worst and delaminated.
2. The GaN films grew at 1000℃, using gallium and ammonia as raw materials, Al and Au/Al as buffer layers. The density, crystallization property and luminous intensity of GaN films were improved by the buffer layers.
3. GaN mico/nano materials were systhesized under the growth mode of double auxiliaries, using gold and indium as auxiliaries, gallium and ammonia gas as raw materials, by CVD method. GaN micro/nano materials with different morphologies were obtained. The influence of auxiliaries, reaction time, reaction temperature and ammonia flow on the product was studied.
目前,除GaN衬底外,其他衬底与GaN纳米材料之间均存在晶格失配和热膨胀系数失配,因此,采用合适的衬底并借助缓冲层成了研究者关注的热点。本论文中实验采用常压化学气相沉积法在不同衬底、不同缓冲层上制备GaN薄膜,分析了合成产物的组分、结构和光学性质,探讨了所得产物的生长机理与影响因素。
除了GaN薄膜材料外,其他形貌的GaN微纳米材料也被应用于光电子器件。本文采用简单的CVD方法,以金膜和铟丝作辅助剂,在硅衬底上以双催化剂模式生长GaN微纳材料。在此过程中,出现了不同形貌的GaN微纳米材料,并研究了产物的结构、辅助剂的作用及其生长机理。
1、以金属镓和氨气为原料,分别在Si、Al2O3和GaAs三种衬底上生长GaN薄膜。由于GaAs衬底的热稳定性不好,而氨气的分解温度在850℃左右,因此实验选择在870℃下进行。分析结果表明产物均为六方纤锌矿多晶结构,其中Al2O3衬底上所得薄膜的结晶质量和发光性能最好,而GaAs衬底上所得薄膜出现脱层。
2、以金属镓和氨气为原料,金属Al和Au/Al为缓冲层,在1000℃下生长GaN薄膜。分析结果表明加入金属缓冲层后所得的GaN薄膜的致密度、结晶性能、发光强度都有所改善。
3、以金属镓和氨气为原料,金和铟为辅助剂,在双辅助剂的生长模式下合成GaN微纳材料,出现了各种不同形貌的GaN微纳米材料。考察了辅助剂、反应时间、反应温度、氨气流量对产物的影响。
Ⅲ-Ⅴcompound semiconductor materials with wide band gap is represented by gallium initride (GaN), whoes energy band gap is 3.4eV. Due to the high saturated electronic drift velocity, high thermal conductivity, resistance to high temperature, rad resistance, resistance to acid and alkali, high hardness features, etc.. It is used to make the semiconductor devices, such as efficient blue-green light emitting diodes, blue-ray semiconductor laser, high power-high frequency Field Effect Transistors, and ultraviolet detectors. The GaN film is mainly used in practice. The researchers tried to produce the GaN films by different methods. HVPE was the earliest, and then MOCVD and MBE were used.At present, some new methods appear, such as electrophoresis deposition (EPD), pulse laser deposition (PLD), magnetron sputtering (MS), sol-gel (Sol-Gel), etc.. In this paper, chemical vapor deposition (CVD) with simple equipment, low cost and easy operation was adopted. The crystalline phase, structure, composition, morphology, and optical property of each sample were analyzed using High-Resolution X-Ray Diffraction (HRXRD), Field Emission Scanning Electron Microscope (FESEM), Atomic Force Microscopy (AFM), Energy Dispersive X-Ray Spectroscopy (EDS), and Photoluminescence (PL). Through the test results, we constantly optimized the preparation process to improve performance of products.
Currently, except the GaN substrate, lattice mismatch and thermal expansion coefficient mismatch exist between other substrates and GaN nanomaterials. Therefore, the use of appropriate substract and buffer layer becomes the focus of attention of researchers. GaN films were deposited on different substrates and different GaN buffer layers by atmospheric pressure chemical vapor deposition (APCVD). The structure, composition and optical property of each sample were analyzed and the growth mechanism and influencing factors were discussed.
In addition to GaN films, micro-nano materials with other morphologies also are applied in light-electronic devices. In this study, GaN micro/nano materials were prepared on Si (100) substrate by CVD with double catalyst mode using Au film and indium silk as auxiliaries. In the process, GaN micro/nano materials with different morphologies was obtained and the structure, catalyst role and growth mechanisms of the products were analyzed.
1. The polycrystal GaN films were produced using gallium and ammonia as raw materials, Si, Al2O3 and GaAs as substrates. Due to the bad thermal stability of GaAs substrate and 850℃decomposition temperature of ammonia gas, the experiment was done under the temperature less than 870℃. The results showed that the product was polycrystal with six-party fine zinc mine structure. The crystallization property and optical property of GaN films on Al2O3 substrate were best; but GaN film on GaAs substrate was worst and delaminated.
2. The GaN films grew at 1000℃, using gallium and ammonia as raw materials, Al and Au/Al as buffer layers. The density, crystallization property and luminous intensity of GaN films were improved by the buffer layers.
3. GaN mico/nano materials were systhesized under the growth mode of double auxiliaries, using gold and indium as auxiliaries, gallium and ammonia gas as raw materials, by CVD method. GaN micro/nano materials with different morphologies were obtained. The influence of auxiliaries, reaction time, reaction temperature and ammonia flow on the product was studied.
引文
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