8英寸导电型4H-SiC单晶衬底制备与表征

使用物理气相传输法(PVT)通过扩径技术制备出直径为209 mm的4H-SiC单晶,并通过多线切割、研磨和抛光等一系列加工工艺制备出标准8英寸SiC单晶衬底。使用拉曼光谱仪、高分辨X射线衍射仪、光学显微镜、电阻仪、偏光应力仪、面型检测仪、位错检测仪等设备,对8英寸衬底的晶型、结晶质量、微管、电阻率、应力、面型、位错等进行了详细表征。拉曼光谱表明8英寸SiC衬底100%比例面积为单一4H晶型;衬底(004)面的5点X射线摇摆曲线半峰全宽分布在10.44″~11.52″;平均微管密度为0.04 cm^-2;平均电阻率为0.020 3 Ω·cm。使用偏光应力仪对8英寸SiC衬底内部应力进行检测表明整片应力分布均匀,且未发现应力集中的区域;翘曲度(Warp)为17.318 μm,弯曲度(Bow)为-3.773 μm。全自动位错密度检测仪对高温熔融KOH刻蚀后的8英寸衬底进行全片扫描,平均总位错密度为3 293 cm^-2,其中螺型位错(TSD)密度为81 cm^-2,刃型位错(TED)密度为3 074 cm^-2,基平面位错(BPD)密度为138 cm^-2。结果表明8英寸导电型4H-SiC衬底质量优良,同比行业标准达到行业先进水平。     

切割角蓝宝石基氧化镓薄膜MOCVD外延及日盲紫外光电探测器制备

本文使用金属有机物化学气相沉积(MOCVD)法在不同切割角的c面蓝宝石衬底上外延氧化镓(β-Ga₂O₃)单晶薄膜，揭示了衬底切割角对外延薄膜晶体质量的影响规律。研究表明，当衬底切割角为6°时，β-Ga₂O₃外延膜具有较小的X射线摇摆曲线半峰全宽(1.10°)和最小的表面粗糙度(7.7 nm)。在此基础上，采用光刻、显影、电子束蒸发及剥离工艺制备了金属-半导体-金属结构的日盲紫外光电探测器，器件的光暗电流比为6.2×10⁶,248 nm处的峰值响应度为87.12 A/W,比探测率为3.5×10¹⁵ Jones,带外抑制比为2.36×10⁴,响应时间为226.2μs。     

昆明物理研究所分子束外延碲镉汞薄膜技术进展

碲镉汞(MCT)自从问世以来一直是高端红外(IR)探测器领域的首选材料,分子束外延碲镉汞技术具有低成本异质外延、材料能带精准调控、原位成结等优势,是第三代红外焦平面陈列(FPA)器件研制的重要手段。本文报道了昆明物理研究所分子束外延(MBE)MCT薄膜技术进展,包括材料结构、晶体质量、表面缺陷、材料均匀性、掺杂浓度等参数优化控制的研究结果。异质衬底、碲锌镉衬底上MCT薄膜尺寸分别为4英寸(10.16 cm)及2.5 cm×2.5 cm,材料EPD值分别在1×10⁶ cm^-2附近及(3~30)×10⁴ cm^-2范围,表面宏观缺陷密度分别在30 cm^-2附近及100~300 cm^-2范围,薄膜质量与国内外先进水平相当。采用分子束外延MCT薄膜实现了2 048×2 048中波红外(MWIR)、2 048×2 048短波甚高分辨率红外(SWIR)焦平面、640×512中短双色红外(S-MWIR)、320×256中中双色红外(M-MWIR)FPA探测器的研制和验证。     

无位错Te-GaSb(100)单晶抛光衬底的晶格完整性

采用液封直拉(LEC)法批量生长的直径2英寸(1英寸=2.54 cm)n型Te-GaSb(100)单晶的位错腐蚀坑密度(EPD)通常低于300 cm^-2,达到无位错水平。本文利用X射线摇摆曲线以及倒易空间图(RSM)对这种GaSb单晶抛光衬底的晶格完整性和亚表面损伤情况进行了分析表征,结果表明经过工艺条件优化的化学机械抛光处理,GaSb单晶衬底表面达到原子级光滑,不存在亚表面损伤层。利用分子束外延在这种衬底上可稳定生长出高质量的Ⅱ类超晶格外延材料并呈现出优异的红外探测性能。在此基础上,对CaSb衬底材料的物性、生长制备和衬底加工条件之间的内在关系进行了综合分析。     

高质量N型SiC单晶生长及其器件应用

采用物理气相传输法在(0001)面偏向<11-20>方向4°的籽晶上生长了掺氮低电阻率碳化硅(SiC)单晶.结合碳化硅邻位面生长机制,通过优化温场设计,在近平温场下生长出了晶型稳定、微管密度低、高结晶质量的低电阻率4H-SiC单晶.在加工的“epi-ready”SiC衬底上进行了同质外延,获得了光滑的外延层表面.利用该外延材料研制了600V/10 A SiC肖特基二极管,器件的直流性能与进口衬底结果相当,反向漏电成品率高达67;.另外研制了600 V/50 A SiC肖特基二极管,器件的直流性能也达到了进口衬底水平.     

碳化硅晶圆的表面/亚表面损伤研究进展

表面无损伤、粗糙度低的半导体碳化硅(4H-SiC)衬底是制造电力电子器件和射频微波器件的理想衬底材料，在新能源、轨道交通、智能电网和5G通信等领域具有广阔的应用前景。4H-SiC衬底的加工过程包括切片、减薄、研磨、抛光和清洗，在4H-SiC衬底加工过程中引入的表面/亚表面损伤均严重影响材料性能、同质外延薄膜性质，以及器件性能和可靠性。本文将重点介绍4H-SiC晶片在切片、减薄、研磨、抛光等各个加工环节中表面/亚表面损伤的形成和去除机制，基于4H-SiC晶圆表面/亚表面损伤的检测方法，综述亚表面损伤的形貌和表征参量，并简单介绍三种常见的亚表面损伤的消除方法，分析其技术优势和发展瓶颈，对去除亚表面损伤工艺的发展趋势进行了展望。     

13N超高纯锗单晶的制备与性能研究

13N超高纯锗单晶是制作超高纯锗探测器的核心材料。本文通过还原法获得还原锗锭,再由水平区熔法提纯获得12N高纯锗多晶,最后由直拉法生长得到13N超高纯锗单晶。通过低温霍尔测试、位错密度检测、深能级瞬态谱(DLTS)测试对13N超高纯锗单晶性能进行分析。低温霍尔测试结果显示,晶体头部截面平均迁移率为4.515×10⁴ cm²·V^-1·s^-1,载流子浓度为1.176×10¹⁰ cm^-3,导电类型为p型,位错密度为2 256 cm^-2;尾部截面平均迁移率为4.620×10⁴ cm²·V^-1·s^-1,载流子浓度为1.007×10¹⁰ cm^-3,导电类型为p型,位错密度为2 589 cm^-2。晶体深能级杂质浓度为1.843×10⁹ cm^-3。以上结果...     

4英寸氧化镓单晶生长与性能

本文使用导模法(EFG)制备了4英寸氧化镓(β-Ga₂O₃)单晶,并对晶体物相、结晶质量、缺陷、光学及电学特性进行了研究。晶体不同方向劳厄(Laue)衍射斑点清晰一致,符合β-Ga₂O₃衍射特征。晶体(400)面摇摆曲线半峰全宽(FWHM)为57.57″,通过化学腐蚀获得其腐蚀坑位错密度为1.06×10⁴ cm^-2。晶体在紫外截止边为262.1 nm,对应光学带隙为4.67 eV。通过C-V测试分析获得非故意掺杂晶体中的电子浓度为7.77×10¹⁶ cm^-3。     

p型4H-SiC单晶衬底表征及第一性原理计算

p型4H-SiC是制备高功率电力电子器件的理想衬底材料,但由于工艺技术的制约,国内尚无能力生产高质量、大尺寸、低电阻的p型4H-SiC单晶衬底。本文使用物理气相传输(PVT)法制备了直径为4英寸(1英寸=2.54 cm)Al掺杂的p型4H-SiC单晶衬底。通过KOH腐蚀表征样品位错密度,使用高分辨X射线衍射(HRXRD)表征其晶体质量,利用拉曼光谱扫描确定其晶型,采用非接触式电阻测试仪测试其电阻率。结果表明,衬底整体位错密度较低,结晶质量良好,晶型稳定且衬底全片电阻率小于0.5 Ω·cm。通过第一性原理平面波超软赝势方法对本征4H-SiC及Al元素掺杂后样品的体系进行能带结构、电子态密度的计算。结果表明Al掺杂后样品禁带宽度减小,费米能级穿过价带,体现出p型半导体的特征。研究结果为大规模生产高质量、低电阻的p型4H-SiC衬底提供思路。     

8英寸导电型4H-SiC单晶的生长

采用物理气相传输(PVT)法扩径获得了8英寸(1英寸=2.54 cm)4H-SiC籽晶,用于8英寸导电型4H-SiC晶体生长,并加工出厚度520 μm的8英寸4H-SiC衬底。使用拉曼光谱、全自动显微镜面扫描、非接触电阻率测试仪面扫描和高分辨X射线衍射仪对衬底的晶型、微管、电阻率和结晶质量进行了表征。衬底颜色均一并结合拉曼光谱表明衬底4H-SiC晶型面积比例为100%;衬底微管密度小于0.3 cm^-2;衬底电阻率范围20~23 mΩ·cm,平均值为22 mΩ·cm;(004)面高分辨X射线摇摆曲线半峰全宽为32.7″,表明衬底良好的结晶质量。     

X-ray characterization of detached-grown germanium crystals

Germanium (1 1 1)-oriented crystals have been grown by the vertical Bridgman technique, in both detached and attached configurations. Microstructural characterization of these crystals has been performed using synchrotron white beam X-ray topography (SWBXT) and double axis X-ray diffraction. Dislocation densities were measured from X-ray topographs obtained using the reflection geometry. For detached-grown crystals, the dislocation density is on the order of 10⁴ cm⁻² in the seed region, and decreases in the direction of growth to less than 10³ cm⁻², and in some crystals reaches less than 10² cm⁻². For crystals grown in the attached configuration, dislocation densities were on the order of 10⁴ cm⁻² in the middle of the crystals, increasing to greater than 10⁵ cm⁻² near the edge. The measured dislocation densities are in excellent agreement with etch pit density (EPD) results. Broadening and splitting of the rocking curve linewidths was observed in the vicinity of subgrain boundaries identified by X-ray topography in some of the attached-grown crystal wafers. The spatial distribution of rocking curve linewidths across the wafers corresponds to the spatial distribution of defect densities measured in the X-ray topographs and EPD micrographs.     

多孔坩埚温度梯度法生长Ho,Y∶CaF2晶体及其光谱性能

采用自主设计改造的温梯炉,成功生长了不同浓度Ho³⁺、Y³⁺掺杂的CaF₂及Sr_xCa_1-xF₂晶体,晶体尺寸约为ϕ15 mm×55 mm,生长周期约为6 d,能够实现7种不同浓度晶体的同步生长,并选取其中的4%(原子数分数)Ho,4%Y∶CaF₂晶体进行分析,吸收测试表明,该晶体448 nm和643 nm处吸收峰的吸收截面分别是1.13×10^-20 cm²和0.84×10^-20 cm², J-O理论分析得到了晶场强度参数Ω_t(t=2、4、6)、辐射跃迁几率、荧光分支比和辐射寿命。在448 nm氙灯激发下,经计算得到该晶体在546 nm、650 nm 和752 nm处的发射截面分别为10.450×10^-21 cm²、8.737×10^-21 cm²和5.965×10^-21 cm²,测得⁵F₄和⁵F₅能级的寿命分别为33.5 μs和17.7 μs。在640 nm LD泵浦激发下,经计算得到该晶体2 031 nm处发射截面为5.375×10^-21 cm²,2 847 nm处发射截面为10.356×10^-21 cm²,测得⁵I₇和⁵I₆ 能级的寿命分别为4.37 ms 和1.85 ms。以上结果表明,多孔坩埚温梯法能够大大提高激光晶体稀土离子掺杂浓度筛选的效率,加快新型激光晶体材料的研发速度。     

K2LaBr5∶Pr晶体的生长及发光性能研究

通过高温固相法合成Pr³⁺不同掺杂浓度的K₂LaBr₅多晶料,采用垂直坩埚下降法生长出K₂LaBr₅∶Pr单晶,并对晶体进行一系列加工,得到ø12 mm×5 mm的圆柱透明晶体。该晶体属于正交晶系,晶胞参数为a=1.336 0 nm,b=0.992 7 nm,c=0.846 2 nm,Z=4,晶体密度为3.908 g/cm³,熔点为607 ℃。测试了该晶体的X射线粉末衍射、X射线激发发射光谱、光致发光光谱、透过率等。在紫外光以及X射线的激发下,K₂LaBr₅∶Pr晶体在480~750 nm波长范围内呈现蓝光(³P₁→³H₄)、绿光(³P₀→³H₄,³P₁→³H₅)、橙光(³P₁→³H₆,³P₁→³F₂)、红光(³P₀→³F₂,³P₁→³F₃)、深红光(³P₁→³F₄),及紫光(³P₀→³F₄)等多个可见波长的光输出,表明该晶体具有优良的发光性能。在X射线的激发下,在360~440 nm范围内还观察到一个宽带4f 5d-4f²发射跃迁。稳态瞬态荧光光谱分析仪测出光致衰减时间为10 μs左右,紫外可见分光光度计则测出晶体在可见光波段的透过率达到88%。     

Reduction of the defect density in GaN films using ultra-thin AlN buffer layers on 6H-SiC

A low dislocation density of 10^7–8 cm⁻² in GaN thin films on 6H-SiC(0001) substrates grown by metalorganic chemical vapor deposition was achieved. By considering possible origins of dislocations in the GaN/AlN/Sic structure, two major dislocation reduction routes are proposed; ultra-thin AlN buffer layers and smooth AlN surfaces in an atomic scale. Experimentally, the effects of the surface roughness and structural perfection of the AlN buffer layer on GaN film quality were extensively investigated as a function of AlN film thickness. The reduced dislocation density was realized by using ultra-thin AlN buffer layers having a thickness of 1.5 nm, which is below the critical value for misfit dislocation generation. The smoother surface morphology and enhanced structural quality of ultra-thin AlN buffer layers were found to be the main parameters in reducing the defect density in the GaN film.     

Growth of semi-insulating GaAs crystals in low temperature gradients by using the Vapour Pressure Controlled Czochralski Method (VCz)

The present paper gives a review on fundamentals, modelling, growth, structural and electrical properties of semi-insulating GaAs single crystals, grown in low temperature gradients by the Vapour Pressure Controlled Czochralski Method (VCz), with diameters from 75 up to 150 mm. Special attention is drawn to the investigation of the temperature-fields inside the growing crystals (and thus thermoelastic stress). Additionally, the influence of convective transport of heat within meit and inert gas is investigated by both experiment and modelling. Thermodynamic aspects of arsenic pressure control within the inner VCz chamber as well as the special experimental and technological challenges are discussed. High quality 100 mm (4-inch) crystals with EPD < 10⁴ cm⁻² and low as-grown residual strain are presented. Very low carbon concentrations of ≈10¹⁴ cm⁻³ were obtained for the first time in VCz crystals. This material, as one of the challengers to conventional LEC material, is able to meet similar electrical specifications whilst showing improved structural quality and better parameter homogeneity even in the as-grown state. Initial studies of a VCz crystal grown without boric oxide encapsulant is presented.     

多片导模法蓝宝石晶体的缺陷研究

使用导模法(EFG)生长了多片a面蓝宝石晶体。显微拉曼光谱结合电感耦合等离子体发射光谱(ICP-AES)测试得出晶体的气泡中可能存在含S化合物。晶体表面明显的生长条纹主要与温度、生长速度的波动以及模具的加工精度有关。化学腐蚀分析表明晶体位错密度在4.2×10⁴ cm^-2,未存在小角度晶界缺陷,双晶摇摆曲线半峰宽(FWHM)为70.63″。由于采用石墨保温材料,晶体中存在F心与F⁺色心。晶体在400~3 000 nm波段透过率高于80%,空气中退火后可减弱色心吸收。本文研究结果可为蓝宝石晶体缺陷形成理论研究提供参考,也可为导模法蓝宝石工业生产技术改进提供借鉴。     

Growth, morphological and structural characterization of Pb1−xSnxTe single crystals

Pb_1−xSn_xTe single crystals have been grown by a vertical Bridgman method. They have typical Hall mobilities and carrier concentration values of 10³ cm²/V · s and 10¹⁸ cm^-3, respectively, and change from p- to n-type as the Sn content increases. The ingots were single crystal with a subgrain structure that has a misorientation no higher than 2′. The segregation of Sn has been determined and it suggests that there is a convective flow in the liquid.     

Growth and characterization of CdSe single crystals by modified vertical vapor phase method

Good quality, large single crystals of CdSe were grown by the modified growth method (i.e., vertical unseeded vapor phase growth with multi-step purification of the starting material in the same quartz ampoule without any manual transfer between the steps). Lower temperature gradients (8–9°C/cm) at the growth interface were used for the crystal growth. As-grown CdSe crystals was characterized by X-ray diffraction, scanning electron microscopy, energy dispersive analyzer of X-rays, high-resistance instrument measurement, and etch-pit observation. It is found that there are two cleavage faces of (1 0 0) and (1 1 0) orientations on the crystal, the resistivity is about 10⁸ Ω cm, and the density of etch pits is about 10^3–4/cm². The crystal was cut into wafers and was fabricated into detectors. The detectors were tested using an ²⁴¹Am radiation source. γ-ray spectra at 59.5 keV were obtained. The results demonstrated that the quality of the as-grown crystals was good. The crystals were useful for fabrication of room-temperature-operating nuclear radiation detectors. Therefore, the modified growth technique is a promising, convenient, new method for the growth of high-quality CdSe single crystals.