HgCdTe Molecular Beam Epitaxy Growth Temperature Calibration Using Spectroscopic Ellipsometry

In this work, spectroscopic ellipsometry (SE) is demonstrated as a technique to calibrate growth temperature measurement devices (thermocouples and pyrometers) prior to real mercury cadmium telluride (HgCdTe) growth. A pyrometer is used to control the substrate temperature in molecular beam epitaxy (MBE) for the growth of HgCdTe-based material. It is known that a very narrow optimal growth temperature range exists for HgCdTe, typically ±5°C. A nonoptimal growth temperature will negatively impact on material quality by inducing growth defects, reducing composition uniformity, causing difficulty in controlling doping incorporation, promoting poor electronic properties, and having other adverse effects. Herein, we present a method for measuring and calibrating substrate temperature measurement equipment by using spectroscopic ellipsometry (SE) prior to real HgCdTe growth. This method is easy to implement, nondestructive, and reliable. The proposed method requires one substrate with a surface material with optical properties well known in the temperature range of interest, but not necessarily the same base material as the material to be grown. In the specific case of this work, we use epitaxial CdTe material on top of a Si substrate. This wafer was used to create a database of its optical properties as a function of temperature by using SE. From the collected optical parameters, a model is built and a fit is generated from the SE data collected. The temperature can then be determined by fitting the temperature-dependent SE measurements from this specific CdTe material. The angle offset and surface roughness parameters are also included in the model to account for changes in the average run-to-run angle variations and surface conditions over time. This work does not attempt to obtain an absolute temperature, but rather a reliable and repeatable relative temperature measurement.     

Molecular Beam Epitaxy Growth of HgCdTe on Large-Area Si and CdZnTe Substrates

This paper presents the status of HgCdTe growth on large-area Si and CdZnTe substrates at Raytheon Vision Systems (RVS). The different technological tools that were used to scale up the growth from 4 inch to 6 inch diameter on Si and from 4 cm × 4 cm to 8 cm × 8 cm on CdZnTe without sacrificing the quality of the layers are described. Extremely high compositional uniformity and low macrodefect density were achieved for single- and two-color HgCdTe layers on both Si and CdZnTe substrates. Finally, a few examples of detector and focal-plane array results are included to highlight the importance of high compositional uniformity and uniformly low macrodefect density of the epitaxial layers in obtaining high operability and low cluster outages in single- and two-color focal-plane arrays (FPAs).     

Characterization of HgCdTe Films Grown on Large-Area CdZnTe Substrates by Molecular Beam Epitaxy

Recent advances in growth of Hg_1?x Cd _x Te films on large-area (7 cm × 7.5 cm) CdZnTe (CZT) substrates is presented. Growth of Hg_1?x Cd _x Te with good uniformity on large-area wafers is achieved using a Riber 412 molecular beam epitaxy (MBE) tool designed for growth of Hg_1?x Cd _x Te compounds. The reactor is equipped with conventional CdTe, Te, and Hg sources for achieving uniform exposure of the wafer during growth. The composition of the Hg_1?x Cd _x Te compound is controlled in situ by employing a closed-loop spectral ellipsometry technique to achieve a cutoff wavelength (λ _co) of 14 μm at 78 K. We present data on the thickness and composition uniformity of films grown for large-format focal-plane array applications. The composition and thickness nonuniformity are determined to be <1% over the area of a 7 cm × 7.5 cm wafer. The films are further characterized by Fourier-transform infrared spectroscopy, optical microscopy, and Hall measurements. Additionally, defect maps show the spatial distribution of defects generated during the epitaxial growth of the Hg_1?x Cd _x Te films. Microdefect densities are in the low 10³ cm^?2 range, and void defects are below 500 cm^?2. Dislocation densities less than 5 × 10⁵ cm^?2 are routinely achieved for Hg_1?x Cd _x Te films grown on CZT substrates. HgCdTe 4k × 4k focal-plane arrays with 15 μm pitch for astronomical wide-area infrared imagers have been produced using the recently developed MBE growth process at Teledyne Imaging Sensors.     

Influence of Substrate Orientation on the Growth of HgCdTe by Molecular Beam Epitaxy

An empirical study is reported, wherein HgCdTe was deposited simultaneously on multiple CdZnTe substrates of different orientations by molecular beam epitaxy. These orientations included the following vicinal surfaces: (115)B, (113)B, (112)B, and (552)B. Additionally, growth on (111)B was explored. Growth conditions found to be nearly optimalfor the standard (112)B orientation were selected. Through a series of growth runs, substrate temperature was varied, and the physical properties of the resulting HgCdTe epilayers were measured. These measurements included Nomarski microscopy, infrared transmission, x-ray diffraction, and defect decoration etching. The properties of HgCdTe epilayers as a function of temperature were roughly similar for all vicinal surfaces. Namely, as the temperature increased, the dislocation density decreased. At some critical temperature, the density of void defects increased dramatically. This critical temperature varied with orientation, the (115)B exhibiting the lowest critical temperature and the (112)B and (552)B exhibiting the highest. The (115)B, (113)B, and (112)B orientations exhibited “needlelike” defects on the as-grown HgCdTe surface. The density of these defects decreased with increasing temperature. The (552)B surface exhibited no such defects and growth behavior nearly identical to the (112)B growthsurface.     

低缺陷Si基碲镉汞分子束外延工艺研究

随着焦平面探测器向超大面阵、小像元方向发展,对盲元率尤其连续盲元、均匀性等要求越来越高。材料表面缺陷已经成为抑制Si基碲镉汞分子束外延(Molecular Beam Epitaxial, MBE)技术在更广范围内应用的一个重要因素。通过解决MBE系统束流稳定性、束流测量的精确性和生长温度控制的稳定性共3个MBE生长碲镉汞材料精确控制的关键问题,以及通过正交试验优化生长参数,将Si基碲镉汞材料缺陷密度控制在500 cm^-2以内,最优值达到57.83 cm^-2。     

分子束外延硅基碲镉汞材料技术研究现状

目前,高性能大面阵中波及短波红外探测器已经得到了越来越多的应用。材料参数控制精确、材料质量良好的碲镉汞材料是获得高质量碲镉汞探测器的先决条件。报道了华北光电技术研究所在分子束外延(Molecular Beam Epitaxy, MBE)生长硅基中波及短波碲镉汞材料方面的最新研究进展,并介绍了现阶段MBE生长碲镉汞材料的研究现状。     

Surface Structure of Molecular Beam Epitaxy (211)B HgCdTe

The as-grown molecular beam epitaxy (MBE) (211)B HgCdTe surface has variable surface topography, which is primarily dependent on substrate temperature and substrate/epilayer mismatch. Nano-ripple formation and cross-hatch patterning are the predominant structural features observed. Nano-ripples preferentially form parallel to the \( [\bar {1}11] \) and are from 0 Å to 100 Å in height with a wavelength between 0.1 μm and 0.8 μm. Cross-hatch patterns result from slip dislocations in the three {111} planes intersecting the (211) growth surface. The cross-hatch step height is 4 ± 1 Å (limited data set). This indicates that only a bi-layer slip (Hg/Cd + Te) in the {111} slip plane occurs. For the deposition of MBE (211)B HgCdTe/CdTe/Si, the reorientation of multiple nano-ripples coalesced into “packets” forms cross-hatch patterns. The as-grown MBE (211)B CdTe/Si surface is highly variable but displays nano-ripples and no cross-hatch pattern. Three types of defects were observed by atomic force microscopy (AFM): needle, void/hillock, and voids.     

分子束外延In掺杂硅基碲镉汞研究

利用分子束外延(Molecular Beam Epitaxy, MBE)系统生长了In掺杂硅基碲镉汞(Mercury Cadmium Telluride, MCT)材料。通过控制In源温度获得了不同掺杂水平的高质量MCT外延片。二次离子质谱仪(Secondary Ion Mass Spectrometer, SIMS)测试结果表明,In掺杂浓度在1×10¹⁵～2×10¹⁶ cm^-3之间。表征了不同In掺杂浓度对MCT外延层位错的影响。发现位错腐蚀坑形态以三角形为主(沿<■>方向排列),且位错密度与未掺杂样品基本相当。对不同In掺杂浓度的材料进行汞饱和低温处理后,样品的电学性能均有所改善。结果表明,In掺杂能够提高材料的均匀性,从而获得较高的电子迁移率。     

CdZnTe Substrate Surface Preparation Technology at ASELSAN,Inc. for Molecular Beam Epitaxy Growth of High Quality HgCdTe Epilayers

High quality CdZnTe substrates with 4% ZnTe mole fraction are used for epitaxial growth of HgCdTe infrared detector layers. Molecular Beam Epitaxy (MBE) growth of HgCdTe epilayers requires high quality surface layer with sub-nanometer surface roughness values as well. We report on the development of a CdZnTe substrate surface preparation process for MBE growth of high quality HgCdTe epilayers. Surface preparation processes were performed on both commercially available CdZnTe substrates and substrates obtained from in-house grown CdZnTe boules. We developed a multi-step substrate surface processing flow to achieve sub-nanometer surface roughness, low total thickness variation (TTV), and wax or slurry residue free CdZnTe substrate surfaces. Each process step was optimized with the aim of removing the subsurface damage caused by the previous process step; so that we reduce the amount of damaged layer needed to be etched prior to epitaxy. Our developed surface preparation process can be applicable to commercially available CdZnTe substrates with high surface roughness and high TTV. This process was also optimized for as-cut CdZnTe slices. We are capable of processing typically 25 mm?×?25 mm CdZnTe substrates with achievable surface roughness values (R_rms) down to below 0.5 nm.     

Growth of ZnSnN2 by Molecular Beam Epitaxy

The Zn-IV-N₂ family of materials represents a potential earth abundant element alternative to conventional compound semiconductor materials that are based on gallium and indium. While both ZnSiN₂ and ZnGeN₂ have been studied to some degree, very little is known about the narrow-gap member ZnSnN₂. Here, we investigate the growth dynamics of crystalline ZnSnN₂ through plasma-assisted molecular beam epitaxy. All films exhibit some degree of crystalline order regardless of growth conditions, although significant tin coverage was observed for films grown with low Zn:Sn flux ratio; Zn flux in particular became increasingly problematic at increased substrate temperatures designed to improve crystallinity. Single-crystal material was achieved through careful optimization of growth parameters. Regardless of deposition conditions or substrate choice, however, all films exhibit a monoclinic structure as opposed to the predicted orthorhombic lattice; this can be directly attributed to sublattice disorder.     

基于分子束外延的4 in硅基碲镉汞材料工艺研究

现阶段,大面阵碲镉汞红外焦平面探测器的需求持续增加,面向更大尺寸的碲镉汞材料制备技术成为了研究热点。对4 in硅基碲镉汞材料外延技术进行了研究。通过提升设备参数的稳定性、控制外延片的平整度以及优化材料工艺参数等一系列手段,突破了大尺寸硅基碲镉汞材料工艺的关键技术瓶颈,并制备出了高平整度、高均匀性、低缺陷率、高质量的4 in硅基碲镉汞材料。结果表明,该材料的双晶衍射半峰宽小于等于90 arcsec,表面宏观缺陷密度小于等于100 cm^-2,表面平整度小于等于15 μm。     

CdSeTe分子束外延技术研究

对HgCdTe红外探测器CdSe_xTe_1-x衬底材料的分子束外延生长条件、组分调整等进行了简单介绍。生长条件包括生长结构(主要有CdSe_xTe_1-x/CdTe/ZnTe/Si、CdSe_xTe_1-x/ZnTe/GaAs等)、生长温度(300℃左右)、生长厚度(5μm左右)等。组分调整包括分析Se组分随(J_Se+J_Te)/J_Cd和J_Se/(J_Se+J_Te)的变化。J_Se/(J_Se+J_Te)值较小时,Se组分较难融入外延层;J_Se/(J_Se+J_Te)值较大时,Se组分增长较迅速。同时,若J_Se/(J_Se+J_Te)值较小,则Se组分增长趋势...     

面向第三代红外焦平面的碲镉汞材料器件研究

文章叙述了第三代红外焦平面中所需求的碲镉汞分子束外延(MBE)的一些研究成 果。对GaAs、Si基大面积异质外延、表面缺陷抑制、p 型掺杂等MBE的主要难点问题进行了阐述。研究表明, 3 in材料的组分均匀性良好,组分x的偏差为0. 5%。晶格失配引发的孪晶缺陷可以通过合适的低温成核方法得到有效的抑制。在GaAs和Si衬底上外延的HgCdTe材料的(422) x射线衍射半峰宽( FWHM)的典型值为60～80arc·sec。大于2μm缺陷的表面密度可以控制在小于300cm- 2水平。研究发现As的表面黏附系数很低,对生长温度十分敏感,在170℃下约为1 ×10- 4。通过合适的退火,可以实现As的受主激活。采用碲镉汞多层材料已试制了长波n2on2p与p2on2n型掺杂异质结器件以及双色红外短波/中波焦平面探测器,本文报道了一些初步结果。     

N-型ZnSe:Cl的分子束外延生长

本文报道利用分子束外延(MBE)技术,采用高纯ZnCl_2作掺杂源,成功地进行了n—型ZnSe:Cl的分子束外延生长。n-ZnSe:Cl/p-GaAs异质结构的伏-安(I—V)特性和热探针测试显示外延层呈n型导电特性。反射高能电子衍射(RHEED)和x射线衍散谱测量表明ZnSe:Cl外延层具有较好的晶体质量。     

Progress in the Molecular Beam Epitaxy of HgCdTe on Large-Area Si and CdZnTe Substrates

This paper presents the progress in the molecular beam epitaxy (MBE) growth of HgCdTe on large-area Si and CdZnTe substrates at Raytheon Vision Systems. We report a very high-quality HgCdTe growth, for the first time, on an 8 cm × 8 cm CdZnTe substrate. This paper also describes the excellent HgCdTe growth repeatability on multiple 7 cm × 7 cm CdZnTe substrates. In order to study the percentage wafer area yield and its consistency from run to run, small lots of dual-band long-wave infrared/long-wave infrared triple-layer heterojunction (TLHJ) layers on 5 cm × 5 cm CdZnTe substrates and single-color double-layer heterojunction (DLHJ) layers on 6-inch Si substrates were grown and tested for cutoff wavelength uniformity and micro- and macrovoid defect density and uniformity. The results show that the entire lot of 12 DLHJ-HgCdTe layers on 6-inch Si wafers meet the testing criterion of cutoff wavelength within the range 4.76 ± 0.1 μm at 130 K and micro- and macrovoid defect density of ≤50 cm⁻² and 5 cm⁻², respectively. Likewise, five out of six dual-band TLHJ-HgCdTe layers on 5 cm × 5 cm CdZnTe substrates meet the testing criterion of cutoff wavelength within the range 6.3 ± 0.1 μm at 300 K and micro- and macrovoid defect density of ≤2000 cm⁻² and 500 cm⁻², respectively, on the entire wafer area. Overall we have found that scaling our HgCdTe MBE process to a 10-inch MBE system has provided significant benefits in terms of both wafer uniformity and quality.     

Optical and Structural Properties of CdTe Grown by Molecular Beam Epitaxy at Low Temperature for Resonant-Cavity-Enhanced HgCdTe Detectors

Investigation into resonant-cavity-enhanced (RCE) HgCdTe detectors has revealed a discrepancy in the refractive index of the CdTe layers grown by molecular beam epitaxy (MBE) for the detectors, compared with the reported value for crystalline CdTe. The refractive index of the CdTe grown for RCE detectors was measured using ellipsometry and matches that of CdTe with an inclusion of approximately 10% voids. X-ray measurements confirm that the sample is crystalline and strained to match the lattice spacing of the underlying Hg_(1−x)Cd_(x)Te, while electron diffraction patterns observed during growth indicate that the CdTe layers exhibit some three-dimensional structure. Secondary ion mass spectroscopy results further indicate that there is enhanced interdiffusion at the interface between Hg_(1−x)Cd_(x)Te and CdTe when the Hg_(1−x)Cd_(x)Te is grown on CdTe, suggesting that the defects are nucleated within the CdTe layers.     

碲镉汞的液相外延生长

设计了一种使用良好的石墨舟,建立了一套能进行开管液相外延的系统,并利用此系统在CdZnTe衬底上和在富Te的生长条件下生长了不同x值的HgCdTe外延薄膜.通过对外延生长工艺的控制,外延薄膜的表面形貌有很大的改善,残留母液大为减少,外延薄膜的组分比较均匀,其电学性能得到较大改善,HgCdTe外延薄膜与CdZnTe衬底之间的互扩散非常少,外延膜的晶体结构也较完整.     

碲镉汞的液相外延生长

设计了一种使用良好的石墨舟 ,建立了一套能进行开管液相外延的系统 ,并利用此系统在 Cd Zn Te衬底上和在富 Te的生长条件下生长了不同 x值的 Hg Cd Te外延薄膜 .通过对外延生长工艺的控制 ,外延薄膜的表面形貌有很大的改善 ,残留母液大为减少 ,外延薄膜的组分比较均匀 ,其电学性能得到较大改善 ,Hg Cd Te外延薄膜与Cd Zn Te衬底之间的互扩散非常少 ,外延膜的晶体结构也较完整 .     

Microscopic Origin of Electrical Compensation in Arsenic-Doped HgCdTe by Molecular Beam Epitaxy: Density Functional Study

The understanding of the configurations of the arsenic tetramer (As _t ), dimer (As _d ), and singlet (As _s ) is important to explain the high electrical compensation of molecular beam epitaxy (MBE) samples and the conversion to p-type behavior. In this work, the possible configurations were optimized from density functional calculations for arsenic defects As _n (n = 1, 2, and 4) in as-grown HgTe. According to the dominant electronic contribution to the defect formation energies, which was calculated under Te-rich conditions, the most probable configurations for As _t , As _d , and As _s have been established. The above discussion applies to the neutral arsenic defects. A further study is necessary to consider the entropy contribution to the defect formation energy.