MOCVD生长Si衬底上HT-AlN缓冲层低生长压力对GaN薄膜的影响

采用金属有机化学气相沉积（MOCVD）技术在Si（111）衬底上外延GaN薄膜,对高温AlN（HT-AlN）缓冲层在小范围内低生长压力（6.7~16.6 kPa）条件下对GaN薄膜特性的影响进行了研究。研究结果表明GaN外延层的表面形貌、结构和光学性质对HT-AlN缓冲层的生长压力有很强的的依赖关系。增加HT-AlN缓冲层的生长压力,GaN薄膜的光学和形貌特性均有明显改善,当HT-AlN缓冲层的生长压力为13.3 kPa时,得到无裂纹的GaN薄膜,其（002）和（102）面的X射线衍射峰值半高宽分别为735 arcsec和778 arcsec,由拉曼光谱计算得到的张应力为0.437 GPa,原子力显微镜（AFM）观测到表面粗糙度为1.57 nm。     

氢化物气相外延生长高质量GaN膜生长参数优化研究

系统研究了低温成核层生长时间、高温生长时的V/Ⅲ 比以及生长温度对氢化物气相外延生长GaN膜晶体质量的影响. 研究发现合适的低温成核层为后续高温生长提供成核中心, 并能有效降低外延膜与衬底间的界面自由能, 促进成核岛的横向生长; 优化的V/Ⅲ比和最佳生长温度有利于降低晶体缺陷密度, 促进横向生长, 增强外延膜的二维生长. 利用扫描电子显微镜、原子力显微镜、高分辨X射线衍射、 低温光致发光谱和室温拉曼光谱对优化条件下生长的GaN外延膜进行了结构和光电特性表征. 测试结果表明, 膜表面平整光滑, 呈现二维生长模式表面形貌; (002)和(102)面摇摆曲线半高宽分别为317和343 arcsec; 低温光致发光谱中近带边发射峰为3.478 eV附近的中性施主束缚激子发射峰, 存在11 meV的蓝移, 半高宽为10 meV, 并且黄带发光强度很弱;常温拉曼光谱中E₂ (high) 峰发生1.1 cm^-1蓝移.结果表明, 优化条件下生长的GaN外延膜具有良好的晶体质量和光电特性, 但GaN 膜中存在压应力. 关键词： 氮化镓 氢化物气相外延 低温成核层     

Synthesis of ZnAl2O4/α-Al2O3 complex substrates and growth of GaN films

With the solid phase reaction between pulsed-laser-deposited (PLD) ZnOfilm and α-Al2O3 substrate, ZnAl2O4/α-Al2O3 complex substrates were synthesized. X-ray diffraction (XRD) spectra show that as the reaction proceeds, ZnAl2O4 changes from the initial (111)-oriented single crystal to poly-crystal, and then to inadequate (111) orientation. Corresponding scanning electron microscope (SEM)images indicate that the surface morphology of ZnAl2O4 transforms from uniform islands to stick structures, and then to bulgy-line structures. In addition, XRDspectra present that ZnAl2O4 prepared at low temperature is unstable at the environment of higher temperature. On the as-obtained ZnAl2O4/α-Al2O3 substrates, GaN films were grown without any nitride buffer using light-radiation heating low-pressure MOCVD (LRH-LP-MOCVD). XRD spectra indicate that GaN film on this kind of complex substrate changes from c-axis single crystal to poly-crystal as ZnAl2O4 layer is thickened. For the single crystal GaN, its full width at half maximum (FWHM) of X-ray rocking curve is 0.4°. Results indicate that islands on thin ZnAl2O4 layer can promote nucleation at initial stage of GaN growth, which leadsto the (0001)-oriented GaN film.     

AlN/蓝宝石模板上生长的GaN研究

研究了在分子束外延制备的AlN/蓝宝石模板上采用金属有机物化学气相外延生长的非故意掺杂GaN的材料性质.采用X射线衍射(XRD)、透射电镜(TEM)和原子力显微镜研究了AlN模板的晶体质量和表面相貌对GaN的影响.结果表明,当AlN的表面粗糙度较小时,尽管AlN模板的位错密度较高((102)面XRD ω扫描半高全宽900—1500 arcsec),但生长得到的GaN依然具有和在蓝宝石衬底上采用"二步法"生长的GaN可比拟的晶体质量((002)面XRD ω扫描半高全宽200—30 关键词： 氮化镓 氮化铝 金属有机物化学气相外延     

国产SiC衬底上利用AIN缓冲层生长高质量GaN外延薄膜

采用高温AlN作为缓冲层在国产SiC衬底上利用金属有机物化学气相外延技术生长GaN外延薄膜.通过优化AlN缓冲层的生长参数得到了高质量的GaN外延薄膜,其对称(0002)面和非对称(1012)面X射线衍射摇摆曲线的半峰宽分别达到130 arcsec和252 arcsec,这是目前报道的在国产SiC衬底上生长GaN最好的...     

AlN缓冲层对Si基GaN外延薄膜性质的影响

采用金属有机化合物化学气相沉积（MOCVD）方法制备了不同AlN缓冲层厚度的GaN样品,研究了AlN缓冲层厚度对GaN外延层的应力、表面形貌和晶体质量的影响。研究结果表明：厚度为15 nm的AlN缓冲层不仅可以有效抑制Si扩散,而且还给GaN外延层提供了一个较大的压应力,避免GaN薄膜出现裂纹。在该厚度AlN缓冲层上制备的GaN薄膜表面光亮、无裂纹,受到的张应力为0.3 GPa,（0002）和（1012）面的高分辨X射线衍射摇摆曲线峰值半高宽分别为536 arcsec和594 arcsec,原子力显微镜测试得到表面粗糙度为0.2 nm。     

Characterization of GaN/AlGaN epitaxial layers grown by metalorganic chemical vapour deposition for high electron mobility transistor applications

GaN and AlGaN epitaxial layers are grown by a metalorganic chemical vapour deposition (MOCVD) system. The crystalline quality of these epitaxially grown layers is studied by different characterization techniques. PL measurements indicate band edge emission peak at 363.8 nm and 312 nm for GaN and AlGaN layers respectively. High resolution XRD (HRXRD) peaks show FWHM of 272 and 296 arcsec for the (0 0 0 2) plane of GaN and GaN in GaN/AlGaN respectively. For GaN buffer layer, the Hall mobility is 346 cm²/V-s and carrier concentration is 4.5 × 10¹⁶/cm³. AFM studies on GaN buffer layer show a dislocation density of 2 × 10⁸/cm² by wet etching in hot phosphoric acid. The refractive indices of GaN buffer layer on sapphire at 633 nm are 2.3544 and 2.1515 for TE and TM modes respectively.     

The influence of an SixNy interlayer on a GaN film grown on an Si（lll） substrate

<正>A method to drastically reduce dislocation density in a GaN film grown on an Si(111) substrate is newly developed. In this method,the Si_xN_y interlayer which is deposited on an A1N buffer layer in situ is introduced to grow the GaN film laterally.The crack-free GaN film with thickness over 1.7 micron is successfully grown on an Si(111) substrate. A synthesized GaN epilayer is characterized by X-ray diffraction(XRD),atomic force microscope(AFM),and Raman spectrum.The test results show that the GaN crystal reveals a wurtzite structure with the(0001) crystal orientation and the full width at half maximum of the X-ray diffraction curve in the(0002) plane is as low as 403 arcsec for the GaN film grown on the Si substrate with an Si_xN_y interlayer.In addition,Raman scattering is used to study the stress in the sample.The results indicate that the Si_xN_y interlayer can more effectively accommodate the strain energy.So the dislocation density can be reduced drastically,and the crystal quality of GaN film can be greatly improved by introducing an Si_xN_y interlayer.     

Optical and structural investigation of a-plane GaN layers on r-plane sapphire with nucleation layer optimization

Nonpolar a-plane GaN epilayers are grown on several r-plane sapphire substrates by metal organic chemical vapour deposition using different nucleation layers:(A) a GaN nucleation layer deposited at low temperature(LT);(B) an AlN nucleation layer deposited at high temperature;or(C) an LT thin AlN nucleation layer with an AlN layer and an AlN/AlGaN superlattice both subsequently deposited at high temperature.The samples have been characterized by Xray diffraction(XRD),atomic force microscopy and photoluminescence.The GaN layers grown using nucleation layers B and C show narrower XRD rocking curves than that using nucleation layer A,indicating a reduction in crystal defect density.Furthermore,the GaN layer grown using nucleation layer C exhibits a surface morphology with triangular defect pits eliminated completely.The improved optical property,corresponding to the enhanced crystal quality,is also confirmed by temperature-dependent and excitation power-dependent photoluminescence measurements.     

Influence of Al Preflow Time on Surface Morphology and Quality of AlN and GaN on Si(111) Grown by MOCVD

We investigate the influence of Al preflow time on surface morphology and quality of AIN and GaN. The AIN and GaN layers are grown on a Si(111) substrate by metal organic chemical vapor deposition. Scanning electron microscopy, atomic force microscopy, x-ray diffraction and optical microscopy are used for analysis. Consequently,we find significant differences in the epitaxial properties of AIN buffer and the GaN layer, which are dependent on the Al preflow time. Al preflow layers act as nucleation sites in the case of AIN growth. Compact and uniform AIN nucleation sites are observed with optimizing Al preflow at an early nucleation stage, which will lead to a smooth AIN surface. Trenches and AIN grain clusters appear on the AIN surface while melt-back etching occurs on the GaN surface with excessive Al preflow. The GaN quality variation keeps a similar trend with the AIN quality, which is influenced by Al preflow. With an optimized duration of Al preflow, crystal quality and surface morphology of AIN and GaN could be improved.     

The influence of SixNy interlayer on GaN film grown on Si(111) substrate

A method to drastically reduce dislocation density in a GaN film grown on an Si(111) substrate is newly developed. In this method, the Si_xN_y interlayer which is deposited on an AlN buffer layer in situ is introduced to grow the GaN film laterally. The crack-free GaN film with thickness over 1.7 micron is grown on an Si(111) substrate successfully. Synthesized GaN epilayer is characterized by X-ray diffraction (XRD), atomic force microscope (AFM), and Raman spectrum. The test results show that the GaN crystal reveals a wurtzite structure with the <0001> crystal orientation and the full width at half maximum of the X-ray diffraction curve in the (0002) plane is as low as 403 arcsec for the GaN film grown on the Si substrate with an Si_xN_y interlayer. In addition, Raman scattering is used to study the stress in the sample. The results indicate that the Si_xN_y interlayer can more effectively accommodate the strain energy. So the dislocation density can be reduced drastically, and the crystal quality of GaN film can be greatly improved by introducing Si_xN_y interlayer.     

GaAs(111)衬底上生长的GaN的极性与生长方法和生长条件的关系

研究了在GaAs(111)衬底上生长的六角相GaN的极性的相关关系.在高Ⅴ/Ⅲ比的条件下用MOVPE和MOMBE方法生长的GaN的极性和GaAs衬底的极性一致;在(111)A-Ga表面上的生长层呈现Ga的极性,而在(111)B-As表面上的生长层呈现N的极性.然而,在低的Ⅴ/Ⅲ比,或采用一个AIN中间层的条件下,用HVPE和MOMBE方法在GaAs(111)B表面上生长的GaN呈现出Ga的极性.目前,其原因尚不清楚,但是这些结果表明采用HVPE生长方法或用一高温AlN阻挡层可以得到高质量的GaN.     

Effect of nitrogen gas flow and growth temperature on extension of GaN layer on Si

The effect of nitrogen flow and growth temperature on extension of GaN on Si substrate has been studied. By increasing the nitrogen flow whose outlet is located in the center of the MOCVD (metal-organic chemical vapor deposition) gas/particle screening flange and by increasing the growth temperature of HT-AlN and AlGaN buffer layers near the primary flat of the wafer, the GaN layer has extended more adequately on Si substrate. In the meantime, the surface morphology has been greatly improved. Both the AlN and GaN crystal quality uniformity has been improved. X-ray diffraction results showed that the GaN (0002) XRD FWHMs (full width at half maximum) decreased from 579 arcsec～ 1655 arcsec to around 420 arcsec.     

Si(111)衬底上生长有多缓冲层的六方GaN晶格常数计算和应变分析

利用卢瑟福背散射/沟道技术和高分辨率X射线衍射技术对在Si(111)衬底上利用金属有机化合物气相外延技术(MOVPE)生长有多缓冲层的六方GaN外延膜进行结晶品质计算、晶格常数计算和应变分析. 实验结果表明：GaN外延膜的结晶品质为χ_min=1.54%，已达到完美晶体的结晶品质(χ_min=1%—2%)；GaN外延膜的水平方向和垂直方向晶格常数分别为：a_epi＝0.31903nm，c_epi=0.51837nm，基本达到G 关键词： GaN 高分辨X射线衍射 卢瑟福背散射/沟道 弹性应变     

Synthesis of ZnAl<Subscript>2</Subscript>O<Subscript>4</Subscript>/α-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> complex substrates and growth of GaN films

With the solid phase reaction between pulsed-laser-deposited (PLD) ZnO film and α-Al₂O₃ substrate, ZnAl₂O₄/α-Al₂O₃ complex substrates were synthesized. X-ray diffraction (XRD) spectra show that as the reaction proceeds, ZnAl₂O₄ changes from the initial (111)-oriented single crystal to poly-crystal, and then to inadequate (111) orientation. Corresponding scanning electron microscope (SEM) images indicate that the surface morphology of ZnAl₂O₄ transforms from uniform islands to stick structures, and then to bulgy-line structures. In addition, XRD spectra present that ZnAl₂O₄ prepared at low temperature is unstable at the environment of higher temperature. On the as-obtained ZnAl₂O₄/α-Al₂O₃ substrates, GaN films were grown without any nitride buffer using light-radiation heating low-pressure MOCVD (LRH-LP-MOCVD). XRD spectra indicate that GaN film on this kind of complex substrate changes fromc-axis single crystal to poly-crystal as ZnAl₂O₄ layer is thickened. For the single crystal GaN, its full width at half maximum (FWHM) of X-ray rocking curve is 0.4°. Results indicate that islands on thin ZnAl₂O₄ layer can promote nucleation at initial stage of GaN growth, which leads to the (0001)-oriented GaN film.     

Influence of AlN Buffer Thickness on GaN Grown on Si(111) by Gas Source Molecular Beam Epitaxy with Ammonia

Hexagonal GaN is grown on a Si(111) substrate with AlN as a buffer layer by gas source molecular beam epitaxy (GSMBE) with ammonia. The thickness of AlN buffer is changed from 9 to 72nm. When the thickness of AlN buffer is 36nm, the surface morphology and crystal quality of GaN is optimal. The in-situ reflection high energy electron diffraction (RHEED) reveals that the transition to a two-dimensional growth mode of AlN is the key to the quality of GaN. However, the thickness of AlN buffer is not so critical to the residual in-plane tensile stress in GaN grown on Si(111) by GSMBE for AlN thickness between 9 to 72nm.     

表面预处理对石墨烯上范德瓦耳斯外延生长GaN材料的影响

基于范德瓦耳斯外延生长的氮化镓/石墨烯材料异质生长界面仅靠较弱的范德瓦耳斯力束缚,具有低位错、易剥离等优势,近年来引起了人们的广泛关注.采用NH_3/H_2混合气体对石墨烯表面进行预处理,研究了不同NH_3/H_2比对石墨烯表面形貌、拉曼散射的影响,探讨了石墨烯在NH_3和H_2混合气氛下的表面预处理机制,最后在石墨烯上外延生长了1.6μm厚的GaN薄膜材料.实验结果表明:石墨烯中褶皱处的C原子更容易与气体发生刻蚀反应,刻蚀方向沿着褶皱进行;适当NH_3/H_2比的混合气体对石墨烯进行表面预处理可有效改善石墨烯上GaN材料的晶体质量.本研究提供了一种可有效提高GaN晶体质量的石墨烯表面预处理方法,可为进一步研究二维材料上高质量的GaN外延生长提供参考.     

梯度铝镓氮缓冲层对氮化镓外延层性质的影响

采用金属有机物化学气相沉积系统在硅面碳化硅衬底的(0001)面上生长氮化铝缓冲层,并通过改变3层梯度铝镓氮(Al_xGa_(1-x)N:x=0.8,0.5,0.2)缓冲层的生长温度和氨气流量,制备出了高质量的氮化镓外延层。分别采用X射线衍射、原子力显微镜、光致发光谱和拉曼光谱对氮化镓外延层进行表征。实验结果表明,随着氮化镓外延层中张应力的降低,样品的晶体质量、表面形貌和光学质量都有显著提高。在最优的梯度铝镓氮缓冲层的生长条件下,氮化镓外延层中的应力值最小,氮化镓(0002)和(1012)面的摇摆曲线半峰宽分别为191 arcsec和243 arcsec,薄膜螺位错密度和刃位错密度分别为7×10~7cm~(-2)和3.1×108cm~(-2),样品表面粗糙度为0.381 nm。这说明梯度铝镓氮缓冲层可以改变氮化镓外延层的应力状态,显著提高氮化镓外延层的晶体质量。     

蓝宝石表面处理对氮化镓薄膜的影响

采用化学方法腐蚀c-面蓝宝石衬底,以形成一定的图案;利用LP-MOCVD在经过不同腐蚀时间的蓝宝石衬底上外延生长GaN薄膜。采用高分辨率双晶X射线衍射（DCXRD）、三维视频光学显微镜（OM）、扫描电子显微镜（SEM）和原子力显微镜（AFM）进行分析。结果表明,对蓝宝石衬底腐蚀50min情况下,外延生长的GaN薄膜晶体质量最优,其（0002）面上的XRD 半峰全宽为202.68arcsec,（10-12）面上的XRD 半峰全宽为300.24arcsec;其均方根粗糙度（RMS）为0.184nm。     

New design of nozzle structures and its effect on the surface and crystal qualities of thick GaN using a horizontal HVPE reactor

High-quality thick GaN films without cracks were achieved by using a new nozzle structure in the reactor grown by the hydride vapor phase epitaxy on sapphire substrates. Optical contrast microscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray double diffraction (XRD) and cathodoluminescence (CL) were carried out to reveal the surface, crystal and optical properties of the GaN epilayer. It was found that the nozzle structure in the reactor has a large effect on the growth rate, surface flat, crystal quality, and the uniformity of the growth. Compared with the old one, the new nozzle structure (denoted as multi-layers nozzle) can improve dramatically the properties of thick GaN. Mirror, colorless and flat GaN thick film was obtained and its (0 0 0 2) FWHM results were reduced from 1000 to 300 arcsec when the new nozzle was used. AFM result revealed a step flow growth mode for GaN layer with the new nozzle. Room-temperature CL spectra on the GaN films showed a strong near-band-edge peak for the new nozzle, but there is only weak emitting peak for the old nozzle. New nozzle structure can improve the uniform of flow field near the surface of substrates compared with the old one, which leads to the improvement of properties of GaN thick film by hydride vapor phase epitaxy (HVPE).