硅衬底氮化镓基LED薄膜转移至柔性黏结层基板后其应力及发光性能变化的研究

本文将硅(Si)衬底上外延生长的氮化镓(GaN)基发光二极管(LED)薄膜转移至含有柔性黏结层的基板上, 获得了不受衬底和支撑基板束缚的LED薄膜. 利用高分辨率X射线衍射仪(HRXRD)研究了薄膜转移前后的应力变化, 同时对其光致发光(PL)光谱的特性进行了研究. 结果表明: 硅衬底GaN基LED薄膜转移至柔性基板后, GaN受到的应力会由转移前巨大的张应力变为转移后微小的压应力, InGaN/GaN量子阱受到的压应力则增大; 尽管LED薄膜室温无损转移至柔性基板其InGaN阱层的In组分不会改变, 然而按照HRXRD倒易空间图谱通用计算方法会得出平均铟组发生了变化; GaN基LED薄膜从外延片转移至柔性基板时其PL谱会发生明显红移.     

InGaN/GaN多量子阱的组分确定和晶格常数计算

采用金属有机化学气相沉积(MOCVD)技术以蓝宝石为衬底在n型GaN单晶层上生长了InGaN/GaN多量子阱结构外延薄膜，利用高分辨X射线衍射(HRXRD)，卢瑟福背散射/沟道(RBS/channeling)，以及光致发光(PL)技术对InGaN/GaN多量子阱结构薄膜分别进行了平均晶格常数计算、In原子替位率计算和In组分的定量分析.研究表明：InGaN/GaN多量子阱的水平和垂直方向平均晶格常数分别为a_epi=0.3195nm，c_epi=0.5198nm，In原子的替位率为99.3%，利用HRXRD和RBS/channeling两种分析技术计算In的组分分别是0.023和0.026，并与样品生长时设定的预期目标相符合，验证了两种实验方法的准确性；而用室温条件下的光致发光谱(PL)来计算InGaN/GaN多量子阱中In的组分是与HRXRD和RBS/channeling的实验结果相差很大，说明用PL测试In组分的方法是不适宜的. 关键词： InGaN/GaN多量子阱 高分辨X射线衍射 卢瑟福背散射/沟道 光致发光     

量子垒生长速率对InGaN基绿光LED性能的影响

利用MOCVD技术在图形化Si(111)衬底上生长了InGaN/GaN绿光LED外延材料。在GaN量子垒的生长过程中,保持NH3流量不变,通过调节三乙基镓(TEGa)源的流量来改变垒生长速率,研究了量子垒生长速率对LED性能的影响。使用二次离子质谱仪(SIMS)和荧光显微镜(FLM)分别对量子阱的阱垒界面及晶体质量进行了表征,使用电致发光测试系统对LED光电性能进行了表征。实验结果表明,垒慢速生长,在整个测试电流密度范围内,外量子效率(EQE)明显提升。我们认为,小电流密度下,EQE的提升归结为量子阱晶体质量的改善;而大电流密度下,EQE的提升则归结为阱垒界面陡峭程度的提升。     

AlN插入层对硅衬底GaN薄膜生长的影响

利用金属有机化合物气相外延沉积技术在2inch(5.08cm)Si(111)图形衬底上生长了GaN外延薄膜,在Al组分渐变AlGaN缓冲层与GaN成核层之间引入了AlN插入层,研究了AlN插入层对GaN薄膜生长的影响。结果表明,随着AlN插入层厚度的增加,GaN外延膜(002)面与(102)面X射线衍射摇摆曲线半峰全宽明显变小,晶体质量变好,同时外延膜在放置过程中所产生的裂纹密度逐渐减小直至不产生裂纹。原因在于AlN插入层的厚度对GaN成核层的生长模式有明显影响,较厚的AlN插入层使GaN成核层倾向于岛状生长,造成后续生长的nGaN外延膜具有更多的侧向外延成分,从而降低了GaN外延膜中的位错密度,减少了GaN外延膜中的残余张应力。同时还提出了一种利用荧光显微镜观察黄带发光形貌来表征GaN成核层形貌和生长模式的新方法。     

湿法刻蚀对Si基片孔点阵及ZnO外延薄膜周期形貌的影响

利用射频等离子体辅助分子束外延法,在刻有周期性孔点阵结构的Si衬底上生长了ZnO二维周期结构薄膜,系统研究了湿法化学刻蚀对孔形点阵Si(100),Si(111)基片表面形貌的影响,以及两种初底上ZnO外延薄膜的结晶质量与周期形貌的差异.X射线衍射及扫描电子显微测试结果表明：Si (111)衬底上生长出的ZnO二维周期结构薄膜具有较好的结晶质量与较好的周期性表面形貌.该研究结果为二维周期结构的制备提供了一种新颖的方法. 关键词： ZnO 分子束外延 Si 湿法刻蚀     

In插入层对硅衬底外延InN晶体质量和光学特性的影响

在Si(111)衬底上分别预沉积0,0.1,0.5,1 nm厚度的In插入层后,采用等离子辅助分子束外延法制备了纤锌矿结构的InN材料,结合X射线衍射(XRD)、扫描电子显微镜(SEM)、吸收谱及光致发光谱研究了不同厚度的In插入层对外延InN晶体质量和光学特性的影响。XRD和SEM的测试结果表明,在Si衬底上预沉积0.5 nm厚的In插入层有利于改善外延InN材料的形貌,提高材料的晶体质量。吸收谱和光致发光谱测试表明,0.5 nm厚In插入层对应的InN样品吸收边蓝移程度最小,光致发射谱半峰宽最窄,并且有最高的带边辐射复合发光效率。可见,引入适当厚度的InN插入层可以改善Si衬底上外延InN材料的晶体质量和光学特性。     

脉冲激光沉积GaN薄膜的结构和光学特性研究

采用准分子脉冲激光,在Si(111)衬底上生长了带有AlN缓冲层的GaN薄膜, 利用X射线衍射(XRD)、原子力显微镜(AFM)和光致发光光谱(PL)等测试手段研究了不同沉积温度所生长的GaN薄膜结构特征和光学性能.研究表明:沉积温度影响GaN薄膜结构和光学性能,黄带发射峰主要与晶体缺陷有关.在400～700℃沉积范围内随着温度升高,GaN薄膜结构和光学性能提高.     

Si掺杂对AlGaInP/GaInP多量子阱性能的影响

采用LP-MOCVD技术在n-GaAs衬底上生长了AlGaInP／GaInP多量子阱红光LED外延片。以X射线双晶衍射技术和光致发光技术对外延片进行了表征,研究了Si掺杂对AlGaInP／GaInP多量子阱性能的影响。研究表明：掺Si能大大提高(Al0．3Ga0.7)0.5In0.5P／Ga0.5In0.5P多量子阱的发光强度。相对于未故意掺杂的样品,多量子阱垒层掺Si使多量子阱的发光强度提高了13倍,阱层和垒层均掺Si使多量子阱的发光强度提高了28倍。外延片的X射线双晶衍射测试表明,Si掺杂并没有使多量子阱的界面质量变差。     

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。     

In插入层对硅衬底外延InN晶体质量和光学特性的影响

在Si（111）衬底上分别预沉积0,0.1,0.5,1 nm厚度的In插入层后,采用等离子辅助分子束外延法制备了纤锌矿结构的InN材料,结合X射线衍射（XRD）、扫描电子显微镜（SEM）、吸收谱及光致发光谱研究了不同厚度的In插入层对外延InN晶体质量和光学特性的影响。XRD和SEM的测试结果表明,在Si衬底上预沉积0.5 nm厚的In插入层有利于改善外延InN材料的形貌,提高材料的晶体质量。吸收谱和光致发光谱测试表明,0.5 nm厚In插入层对应的InN样品吸收边蓝移程度最小,光致发射谱半峰宽最窄,并且有最高的带边辐射复合发光效率。可见,引入适当厚度的InN插入层可以改善Si衬底上外延InN材料的晶体质量和光学特性。     

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。     

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.     

Influence of AlN buffer layer thickness on structural properties of GaN epilayer grown on Si (111) substrate with AlGaN interlayer

We present the growth of GaN epilayer on Si (111) substrate with a single AlGaN interlayer sandwiched between the GaN epilayer and AlN buffer layer by using the metalorganic chemical vapour deposition. The influence of the AlN buffer layer thickness on structural properties of the GaN epilayer has been investigated by scanning electron microscopy, atomic force microscopy, optical microscopy and high-resolution x-ray diffraction. It is found that an AlN buffer layer with the appropriate thickness plays an important role in increasing compressive strain and improving crystal quality during the growth of AlGaN interlayer, which can introduce a more compressive strain into the subsequent grown GaN layer, and reduce the crack density and threading dislocation density in 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.     

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.     

A Comparison of GaN Epilayers with Multiple Buffer Layers and with a Single Buffer Layer Grown on Si（111） Studied by HRXRD and RBS/Channeling

Two hexagonal GaN epilayers （samples A and B） with multiple buffer layers and single buffer layer are grown on Si （111） by metal-organic vapour phase epitaxy （MOVPE）. From the results of Rutherford backscattering （RBS）/channeling and high resolution x-ray diffraction （HRXRD）, we obtain the lattice constant （a and c） of two GaN epilayers （aA = 0.3190 nm, cA = 0.5184 nm and aB = 0.3192 nm, CB = 0.5179 nm）, the crystal quality of two GaN epilayers （ ХminA=4.87%, ХminB =7.35% along 〈1-↑213〉 axis） and the tetragonal distortion eT of the two samples along depth （sample A is nearly fully relaxed, sample B is not relaxed enough）. Comparing the results with the two samples, it is indicated that sample A with multiple buffer layers have better crystal quality than sample B with a single buffer layer, and it is a good way to grow GaN epilayer on Si （111） substrates using multiple buffer layers to improve crystal quality and to reduce lattice mismatch.     

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.     

Influence of Si doping on the structural and optical properties of InGaN epilayers

Influences of the Si doping on the structural and optical properties of the InGaN epilayers are investigated in detail by means of high-resolution X-ray diffraction （HRXRD）, photolumimescence （PL）, scanning electron microscope （SEM）, and atomic force microscopy （AFM）. It is found that the Si doping may improve the surface morphology and crystal quality of the InGaN film and meanwhile it can also enhance the emission efficiency by increasing the electron concentration in the InGaN and suppressing tile formation of V-defects, which act as nonradiative recombination centers in the InGaN, and it is proposed that the former plays a more important role in enhancing the emission efficiency in the InGaN.     

硅衬底GaN基LED薄膜芯片的应力调制

将Si衬底GaN基LED外延薄膜经晶圆键合、去硅衬底等工艺制作成垂直结构GaN基LED薄膜芯片,并对其进行不同温度的连续退火,通过高分辨X射线衍射(HRXRD)研究了连续退火过程中GaN薄膜芯片的应力变化。研究发现:垂直结构LED薄膜芯片在160~180℃下退火应力释放明显,200℃时应力释放充分,GaN的晶格常数接近标准值。继续升温应力不再发生明显变化,GaN薄膜的晶格常数只在标准晶格常数值附近波动。扫描电子显微镜给出的bonding层中Ag-In合金情况很好地解释了薄膜芯片应力的变化。