Structural and optical characterization of GaN grown on porous silicon substrate by MOVPE

GaN was grown on porous silicon (PS) substrates by Metalorganic Vapour Phase Epitaxy at temperature of 1050 °C. An additional AlN buffer layer is used between GaN and PS. The crystalline quality and surface morphology of GaN films were studied by X-ray diffraction and scanning electron microscope (SEM), respectively. Preferential growth of hexagonal GaN with 〈00.1〉 direction is observed and is clearly improved when the thickness of AlN buffer layer increases. Morphological changes in PS layer appearing after growth have been also discussed.GaN optical qualities were determined by photoluminescence at low and room temperature (RT).     

AlN缓冲层厚度对脉冲激光沉积技术生长的GaN薄膜性能的影响

在蓝宝石(Al2O3)衬底上应用脉冲激光沉积技术(PLD)生长不同厚度的AlN缓冲层后进行GaN薄膜外延生长。采用高分辨X射线衍射仪(HRXRD)和扫描电子显微镜(SEM)对外延生长所得GaN薄膜的晶体质量和表面形貌进行了表征。测试结果表明: 相比直接在Al2O3衬底上生长的GaN薄膜, 通过生长AlN缓冲层的GaN薄膜虽然晶体质量较差, 但表面较平整; 而且随着AlN缓冲层厚度的增加, GaN薄膜的晶体质量和表面平整度均逐渐提高。可见, AlN缓冲层厚度对在Al2O3衬底上外延生长GaN薄膜的晶体质量和表面形貌有着重要的影响。     

AlN缓冲层厚度对脉冲激光沉积技术生长的GaN薄膜性能的影响

在蓝宝石(Al2O3)衬底上应用脉冲激光沉积技术(PLD)生长不同厚度的AlN缓冲层后进行GaN薄膜外延生长。采用高分辨X射线衍射仪(HRXRD)和扫描电子显微镜(SEM)对外延生长所得GaN薄膜的晶体质量和表面形貌进行了表征。测试结果表明:相比直接在Al2O3衬底上生长的GaN薄膜,通过生长AlN缓冲层的GaN薄膜虽然晶体质量较差,但表面较平整;而且随着AlN缓冲层厚度的增加,GaN薄膜的晶体质量和表面平整度均逐渐提高。可见,AlN缓冲层厚度对在Al2O3衬底上外延生长GaN薄膜的晶体质量和表面形貌有着重要的影响。     

Raman scattering of polycrystalline 3C-SiC film deposited on AlN buffer layer by using CVD with HMDS

This paper presents the Raman scattering characteristics of poly (polycrystalline) 3C-SiC thin films deposited on AlN buffer layer by atmospheric pressure chemical vapor deposition (APCVD) using hexamethyldisilane (MHDS) and carrier gases (Ar+H₂). The Raman spectra of SiC films deposited on AlN layer of before and after annealing were investigated according to the growth temperature of 3C-SiC. Two strong Raman peaks, which mean that poly 3C-SiC admixed with nanoparticle graphite, were measured in them. The biaxial stress of poly 3C-SiC/AlN was calculated as 896 MPa from the Raman shifts of 3C-SiC deposited at 1180 °C on AlN of after annealing.     

Analysis of reactor geometry and diluent gas flow effects on the metalorganic vapor phase epitaxy of AIN and GaN thin films on α(6H)-SiC substrates

The influence of diluent gas on the metalorganic vapor phase epitaxy of AlN and GaN thin films has been investigated. A computational fluid dynamics model using the finite element method was employed to improve film uniformity and to analyze transport phenomena. The properties of AlN and GaN thin films grown on α(6H)-SiC(0001) substrates in H₂ and N₂ diluent gas environments were evaluated. Thin films of AlN grown in H₂ and N₂ had root mean square (rms) roughness values of 1.5 and 1.8 nm, respectively. The surface and defect microstructures of the GaN thin films, observed by scanning and transmission electron microscopy, respectively, were very similar for both diluents. Low temperature (12K) photoluminescence measurements of GaN films grown in N₂ had peak intensities and full widths at half maximum equal to or better than those films grown in H₂. A room temperature Hall mobility of 275 cm²/V·s was measured on 1 μm thick, Si-doped, n-type (1×10¹⁷ cm⁻³) GaN films grown in N₂. Acceptor-type behavior of Mg-doped GaN films deposited in N₂ was repeatably obtained without post-growth annealing, in contrast to similar films grown in H₂. The GaN growth rates were ∼30% higher when H₂ was used as the diluent. The measured differences in the growth rates of AlN and GaN films in H₂ and N₂ was attributed to the different transport properties of these mixtures, and agreed well with the computer model predictions. Nitrogen is shown to be a feasible alternative diluent to hydrogen for the growth of AlN and GaN thin films.     

Effect of AlN buffer layer thickness on the properties of GaN films grown by pulsed laser deposition

The GaN films are grown by pulsed laser deposition (PLD) on sapphire, AlN(30 nm)/Al₂O₃ and AlN(150 nm)/Al₂O₃, respectively. The effect of AlN buffer layer thickness on the properties of GaN films grown by PLD is investigated systematically. The characterizations reveal that as AlN buffer layer thickness increases, the surface root-mean-square (RMS) roughness of GaN film decreases from 11.5 nm to 2.3 nm, while the FWHM value of GaN film rises up from 20.28 arcmin to 84.6 arcmin and then drops to 31.8 arcmin. These results are different from the GaN films deposited by metal organic chemical vapor deposition (MOCVD) with AlN buffer layers, which shows the improvement of crystalline qualities and surface morphologies with the thickening of AlN buffer layer. The mechanism of the effect of AlN buffer layer on the growth of GaN films by PLD is hence proposed.     

Elevated-Temperature Annealing Effects on AlGaN/GaN Heterostructures

The effect of high-temperature annealing of undoped AlGaN/GaN heterostructures on different substrates was systematically studied between 1100°C and 1230°C. An AlN spacer layer was found to add stability to structures on sapphire substrates. AlGaN/GaN heterostructures on SiC substrates demonstrated excellent robustness for the temperature range studied, maintaining their mobility, sheet resistance, and sheet concentration values, even after annealing. A silicon nitride, SiN _x , capping layer was found to assist in minimizing surface roughness during annealing and maintaining the electrical characteristics of the heterostructures. AlGaN/GaN heterostructures on SiC substrates showed a 20% decrease in mobility for uncapped samples compared with SiN _x -capped samples.     

Growth and characterization of ZnO thin films on GaN epilayers

Dense ZnO(0001) films formed at 500°C via coalescence of islands grown via metalorganic vapor phase epitaxy (MOVPE) either on GaN/AlN/SiC(0001) substrates or on initial, coherent ZnO layers. Conical crystallites formed due to thermal expansion-induced stresses between the ZnO and the substrate. Interfaces between the ZnO films on GaN epilayers exposed either simultaneously to diethylzinc and oxygen or only to diethylzinc at the initiation of growth were sharp and epitaxial. Interfaces formed after the exposure of the GaN to O₂ were less coherent, though an interfacial oxide was not observed by cross-sectional transmission electron microscopy (TEM). Threading dislocations and stacking faults were observed in all films.     

Activation annealing of Si-implanted GaN up to 1500°C using a novel RTP technique

A novel rapid thermal processing (RTP) unit called Zapper™ has recently been developed by MHI Inc. and the University of Florida for high temperature thermal processing of semiconductors. This Zapper™ unit is capable of reaching much higher temperatures (>1500°C) than conventional tungsten-halogen lamp RTP equipment and achieving high ramp-up and ramp-down rates. Implant activation annealing studies of Si⁺-implanted GaN thin films (with and without an AlN encapsulation layer) have been conducted using the Zapper™ unit at temperatures up to 1500°C. The measurements of electrical properties of such annealed samples have led to the conclusion that high annealing temperatures and AlN encapsulation are needed for the optimum activation efficiency of Si⁺ implants in GaN. It has clearly been demonstrated that the Zapper™ unit has tremendous potential for RTP annealing of semiconductor materials, especially for wide bandgap compound semiconductors that require very high processing temperatures.     

A novel technique for RTP annealing of compound semiconductors

We introduce for the first time a novel rapid thermal processing (RTP) unit called Zapper™, which has recently been developed by MHI Inc. and the University of Florida, for high temperature thermal processing of semiconductors. This Zapper™ unit is capable of reaching much highertemperatures (>1500°C) than conventional tungsten–halogen lamp RTP equipment and achievinghigh ramp-up and ramp-down rates. We have conducted implant activation annealing studies ofSi⁺-implanted GaN thin films (with and without an AlN encapsulation layer) using the Zapper™ unit at temperatures up to 1500°C. The electrical property measurements of such annealed samples have led to the conclusion that high annealing temperatures and AlN encapsulation are needed for the optimum activation efficiency of Si⁺ implants in GaN. It has clearly been demonstrated that the Zapper™ unit has tremendous potential for RTP annealing of semiconductor materials, especially for wide band-gap (WBG) compound semiconductors that require very high processing temperatures.     

Pendeo-epitaxial growth of gallium nitride on silicon substrates

Pendeo-epitaxy (PE)¹ from raised, [0001] oriented GaN stripes covered with silicon nitride masks has been employed for the growth of coalesced films of GaN(0001) with markedly reduced densities of line and planar defects on Si(111)-based substrates. Each substrate contained previously deposited 3C-SiC(111) and AlN(0001) transition layers and a GaN seed layer from which the stripes were etched. The 3C-SiC transition layer eliminated chemical reactions between the Si and the NH₃ and the Ga metal from the decomposition of triethylgallium. The 3C-SiC and the GaN seed layers, each 0.5 μm thick, were also used to minimize the cracking and warping of the GaN/SiC/silicon assembly caused primarily by the stresses generated on cooling due to the mismatches in the coefficients of thermal expansion. Tilting in the coalesced GaN epilayers of 0.2° was confined to areas of lateral overgrowth over the masks; no tilting was observed in the material suspended above the trenches. The strong, low-temperature PL band-edge peak at 3.456 eV with a FWHM of 17 meV was comparable to that observed in PE GaN films grown on AlN/6H-SiC(0001) substrates.     

Growth optimization and doping with Si and Be of high quality GaN on Si(111) by molecular beam epitaxy

GaN layers have been grown by plasma-assisted molecular beam epitaxy on AlN-buffered Si(111) substrates. An initial Al coverage of the Si substrate of aproximately 3 nm lead to the best AlN layers in terms of x-ray diffraction data, with values of full-width at half-maximum down to 10 arcmin. A (2×2) surface reconstruction of the AlN layer can be observed when growing under stoichiometry conditions and for substrate temperatures up to 850°C. Atomic force microscopy reveals that an optimal roughness of 4.6 nm is obtained for AlN layers grown at 850°C. Optimization in the subsequent growth of the GaN determined that a reduced growth rate at the beginning of the growth favors the coalescence of the grains on the surface and improves the optical quality of the film. Following this procedure, an optimum x-ray full-width at half-maximum value of 8.5 arcmin for the GaN layer was obtained. Si-doped GaN layers were grown with doping concentrations up to 1.7×10¹⁹ cm⁻³ and mobilities approximately 100 cm²/V s. Secondary ion mass spectroscopy measurements of Be-doped GaN films indicate that Be is incorporated in the film covering more than two orders of magnitude by increasing the Be-cell temperature. Optical activation energy of Be acceptors between 90 and 100 meV was derived from photoluminescence experiments.     

Growth of thick gan films on rf sputtered ain buffer layer by hydride vapor phase epitaxy

High crystalline quality thick GaN films were grown by vapor phase epitaxy using GaCl₃ and NH₃. The growth rate was in the range of 10~15 Μm/h. GaN films grown at higher temperatures (960~ 1020?C) were single crystalline with smooth surface morphologies. No chlorine impurity was incorporated in these films during growth. The best crystalline quality and surface morphology of grown films was achieved by sputtering a thin A1N buffer layer, prior to growth. According to reflection high energy electron diffraction and atomic force microscopy measurements, as-sputtered A1N buffer layer was amorphous with root means square roughness of 0.395 nm and then crystallized during the GaN growth. This improved the GaN growth due to more uniform distribution of GaN nucleation. Rutherford backscattering channeling experiments produced the lowest value from the GaN film grown on a-Al₂O₃ with a 500å A1N buffer layer at 1020?C.     

<Emphasis Type="Italic">In Situ</Emphasis> Stress Measurements During GaN Growth on Ion-Implanted AlN/Si Substrates

In situ wafer curvature measurements were used in combination with postgrowth structural characterization to study the evolution of film stress and microstructure in GaN layers grown by metalorganic chemical vapor deposition on N⁺ ion-implanted AlN/Si (111) substrates. The results were compared with growth on identical unimplanted substrates. In situ stress measurements revealed that, for the unimplanted sample, the GaN initiated growth under compressive stress of −1.41 GPa which arose due to lattice mismatch with the AlN buffer layer. In contrast, GaN growth on the ion-implanted sample began at lower compressive stress of −0.84 GPa, suggesting a reduction in epitaxial stress. In both cases, the compressive growth stress was fully relaxed after ~0.7 μm and minimal tensile stress was generated during growth. During post-growth cooling, tensile stress was introduced in the GaN layer of both samples due to thermal expansion mismatch. Post-growth optical microscopy characterization, however, demonstrated that the ion-implanted sample had lower density of channeling cracks compared with the unimplanted sample. Cross-sectional transmission electron microscopy images of the sample grown on ion-implanted Si with no post-implantation nitrogen annealing revealed the formation of horizontal cracks in the implanted region beneath the AlN buffer layer. The weakened layer acts to decouple the GaN film from the Si substrate and thereby reduces the density of channeling cracks in the film after growth.     

N-type implantation doping of GaN

Doping characteristics of N/Si and N/Ge co-implanted GaN have been systematically investigated. N-type regions were produced in undoped GaN films by the co-implantation and subsequent annealing with an SiO₂ encapsulation layer at high temperatures. The annealing procedures above 1100 and 1200°C were required to achieve an n-type activation for N/Si and N/Ge co-implanted GaN, respectively. The both samples show effective activation efficiencies of 50% after annealing at 1300°C. However, actual Si activation seems to be much higher than the Ge activation due to the different behaviors of implantation-induced damage.     

Porous silicon as an intermediate buffer layer for GaN growth on (100) Si

We report preliminary results on the growth of GaN on (100) Si substrate using porous silicon (PS) as an intermediate buffer layer. The growth was in situ monitored by laser beam reflectivity. Analysis of the evolution of the reflectivity signal indicates a change from relatively flat surface to rough one as the growth temperature (T_g) is increased. At a temperature of about 1050°C, the growth rate is very low and the reflected signal intensity is constant. When the growth temperature is varied, no drastic change of the porosity of the intermediate layer was detected. Scanning electron microscope (SEM) observations of the GaN/SP/Si structure revealed a good surface coverage at 500°C. When T_g increases, the structure morphology changes to columnar like structure at 600°C, and well-developed little crystallites with no preferential orientation appear at 800°C. These observations agree well with the X-ray diffraction (XRD) analysis. A preferential hexagonal growth is obtained at low growth temperature, while cubic phase begin to appear at elevated temperatures.     

利用平片蓝宝石衬底制备高功率垂直结构LED

在平片蓝宝石衬底上,通过引入AlN缓冲层,优化成核层与粗糙层的生长条件,生长出了表面平整的GaN薄膜,晶体质量得到显著提升。通过引入AlN缓冲层,将X射线衍射(XRD)下样品(002)面的半高宽(FWHM)由232″降低至148″;通过减薄成核层厚度、提升粗糙层生长压力,将样品(102)面和(100)面的FWHM分别由243″和283″降低至169″和221″。研究了不同成核层和粗糙层的生长参数对GaN薄膜表面形貌的影响,随着(102)面和(100)面FWHM的降低,表面平整度亦得到改善,粗糙度由约3.8 nm下降到约1.6 nm。利用优化后的底层条件生长了高质量GaN薄膜,在3.5 A/mm^2电流密度下,与参考样品相比,制备出的LED样品的光输出功率由863 mW提升至942 mW,提升了约9%。     

Investigations of GaN growth on the sapphire substrate by MOCVD method with different AlN buffer deposition temperatures

The effects of different AlN buffer deposition temperatures on the GaN material properties grown on sapphire substrate was investigated. At relatively higher AlN buffer growth temperature, the surface morphology of subsequent grown GaN layer was decorated with island-like structure and revealed the mixed-polarity characteristics. In addition, the density of screw TD and leakage current in the GaN film was also increased. The occurrence of mixed-polarity GaN material result could be from unintentional nitridation of the sapphire substrate by ammonia (NH₃) precursor at the beginning of the AlN buffer layer growth. By using two-step temperature growth process for the buffer layer, the unintentional nitridation could be effectively suppressed. The GaN film grown on this buffer layer exhibited a smooth surface, single polarity, high crystalline quality and high resistivity. AlGaN/GaN high electron-mobility transistor (HEMT) devices were also successfully fabricated by using the two-step AlN buffer layer.     

利用混合极性制备多孔缓冲层及其在GaN厚膜外延中的应用

使用分子束外延(MBE)技术在(0001)面蓝宝石衬底上生长混合极性的氮化镓(GaN)薄膜,利用不同极性面的GaN薄膜在强碱溶液中腐蚀特性的差异,混和极性样品经腐蚀处理后,得到了一层具有多孔结构的GaN层.以多孔结构的GaN作为缓冲层,用卤化物气相外延(HVPE)方法生长GaN厚膜.X射线双晶衍射和光致发光等测试结果表明,多孔结构的GaN缓冲层可以有效地释放GaN厚膜和衬底之间因热膨胀系数失配产生的应力,使GaN厚膜晶体的质量得到很大提高.     

GaN薄膜表面形貌与AlN成核层生长参数的关系

采用金属有机物化学气相淀积技术生长了以AlN为成核层的GaN薄膜,研究了成核层生长时三甲基铝(TMAl)流量对最终GaN薄膜表面形貌的影响.研究结果表明,高质量GaN薄膜只能在高TMAl流量下获得,采用充足的TMAl源才能形成满足需要的AlN成核点,这是生长高质量GaN薄膜的一个先决条件.