HFCVD法制备纳米晶体碳化硅薄膜中氢流量对晶粒尺寸的影响

以甲烷、硅烷和氢气为反应气体,采用热丝化学气相沉积(HFCVD)法在单晶硅衬底上沉积纳米晶体碳化硅(SiC)薄膜.通过X射线衍射(XRD)和扫描电子显微镜(SEM)分别对SiC薄膜的晶体结构和表面形貌进行分析.实验发现氢气流量对碳化硅薄膜晶粒尺寸有很大影响,当氢气流量从10SCCM变化到300SCCM时,薄膜晶粒的平均尺寸将由较大的400 nm左右减小到40 nm左右.     

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利用微波电子回旋共振等离子体增强型化学气相沉积(ECR-PECVD)采用一步法直接在K9玻璃上低温沉积制备了多晶硅薄膜.研究了不同实验参数对薄膜沉积的影响,采用X射线衍射(XRD)、拉曼光谱、扫描电子显微镜(SEM)等实验分析方法对不同条件下制备的样品进行了晶体结构和表面形貌分析,并讨论了多晶硅薄膜沉积的最佳条件.实验结果表明,玻璃衬底上多晶硅薄膜呈柱状生长,并有一定厚度的非晶孵化层;较高氢气比例和衬底温度有利于结晶,薄膜的结晶率达到了62％;晶粒团簇的最大尺寸约为500nm.     

在Si(111)上用有机溶胶凝胶甩膜热解法制备(0001)定向的6H-SiC薄膜

在Si(111)衬底上用聚苯乙烯溶胶凝胶甩膜并经950℃真空(10^-3Pa)热解处理法,制备出晶态SiC薄膜.用FTIR,XRD,TEM,RamanXPS等方法研究了SiC薄膜的晶体结构、微结构、组成以及各元素的化学态等性质.结果表明制得的是沿(0001)高度择优取向的晶态6H-SiC薄膜.膜中SiC晶粒沿c轴柱状生长,其最大尺寸约150nm,膜厚约为0.3μm,SiC中的Si/C比约为1.表层有少许污染C(CH和CO)和少量O(Si₂O₃,CO态氧和吸附氧).从对比实验可知,在热解时将甩膜的Si片与另一空白Si片面面相贴可明显增加SiC的生成量. 关键词： 碳化硅 薄膜 溶胶凝胶     

(0001)SiC衬底MgB_2超薄膜的制备和性质研究

利用混合物理化学气相沉积法(Hybrid physical-chemical vapor deposition简称为(HPCVD)在(0001)SiC衬底上制备了干净的MgB2超导超薄膜.在背景气体、压强、载气氢气流量以及B2H6的流量一定的情况下,改变沉积时间,制得一系列MgB2超薄膜样品。通过观察样品的表面形貌变化探究了MgB2超薄膜的生长过程.该系列超薄膜的生长遵循Volmer-Weber岛状生长模式且沿c轴外延生长.以20nm超薄膜作为例子,可知其表面连接性良好,超导转变温度Tc(0)≈38.5K,临界电流密度Jc≈0.82×107 A/cm2,表明了利用HPCVD在(0001)SiC衬底上制备的MgB2超薄膜有很好的性能.这预示其在超导电子器件上具有广阔的应用前景.     

强磁场对不同厚度Fe-Ni纳米多晶薄膜的生长过程及磁性能的影响

有无6 T强磁场条件下, 利用分子束气相沉积方法制备了21 nm和235 nm厚的Fe-Ni纳米多晶薄膜. 研究发现, 0 T时, 21 nm厚的薄膜是晶粒堆叠而成, 晶粒尺寸为6–7 nm; 6 T时, 21 nm厚的薄膜首先在基片表面形成了晶粒相互连接的5 nm平坦层, 晶粒沿基片表面拉长, 随后以6–7 nm尺寸的晶粒堆叠而成; 0 T时, 235 nm厚度的薄膜生长初期平均晶粒尺寸为3.6 nm, 生长中期平均晶粒尺寸为5.6 nm, 生长末期薄膜近似柱状方式生长, 晶粒沿生长方向拉长; 6 T时, 235 nm厚度的薄膜在基片表面也形成了晶粒相互连接的5 nm平坦层, 晶粒沿基片表面拉长, 随后以尺寸均匀的6.1 nm晶粒堆叠而成; 而且, 6 T强磁场使得不同厚度薄膜的面外与面内矫顽力都降低.     

低压下气流对激光沉积纳米硅晶化及尺寸的影响

纳米硅具有明显的光致发光效应和量子尺寸效应,广泛的应用在现代电子工业和太阳能光伏工业中.尺寸影响着纳米硅的实际用途,因此制备尺寸可控的纳米硅晶粒具有很重要的实际意义.本文采用脉冲激光沉积(PLD)技术,在烧蚀点水平方向、距靶2 cm处引入一束流量为5 sccm的氩(Ar)气流,在0.01-0.5 Pa的Ar气压下烧蚀高阻抗单晶硅(Si)靶.在管口正下方1 cm处水平放置衬底来沉积纳米Si薄膜;并用同一装置,在0.08 Pa的Ar气压下分别引入流量为0,2.5,5,7.5,10 sccm的Ar气流沉积纳米Si薄膜.利用原子力显微镜(AFM)、X射线衍射(XRD)、Raman散射对样品表面形貌和微观结构进行分析表征.结果表明:不引入气流时出现纳米Si晶粒的阈值气压是0.1Pa,引入气流后出现纳米Si晶粒的阈值气压为0.05 Pa.晶粒尺寸随着气流流量的增大而减小.     

基片温度对SiNx薄膜结晶状态及机械性能的影响

利用微波电子回旋共振增强磁控反应溅射法在不同基片温度下制备无氢SiNx薄膜.通过傅里叶变换红外光谱、透射电子显微镜、台阶仪、纳米硬度仪等表征技术,研究了基片温度对SiNx薄膜结晶状态、晶粒尺寸、晶体取向等结晶性能以及薄膜的生长速率、硬度等机械性能的影响,并探讨了薄膜结晶性能与机械性能之间的关系.研究结果表明,在基片温度低于300℃时制备的SiNx薄膜以非晶状态存在,硬度值仅为18 GPa左右;基片温度在320-620℃范围内,SiNx薄膜中出现纳米晶粒,且晶粒尺寸随沉积温度的增加而增加,在沉积温度为620℃时达到最大,为20±1.5 nm;当沉积温度为700℃时,SiN<,x>薄膜的晶粒尺寸突然减小,但由于此时晶粒密度为最大,因此薄膜硬度达到最大值(36.7 GPa).     

氢气引入对宽光谱Mg和Ga共掺杂ZnO透明导电薄膜的特性影响

为适应宽光谱高效率硅基薄膜太阳电池的应用需求,本文尝试采用直流磁控溅射技术在553 K衬底温度下生长氢化Mg和Ga共掺杂ZnO(HMGZO)透明导电氧化物(TCO)薄膜.通过对薄膜微观结构、表面形貌、电学以及光学性能的测试和分析,详细地研究了氢气(H2)流量(0—16.0 sccm)对HMGZO薄膜结晶特性及光电性能的影响.实验结果表明:生长获得的HMGZO薄膜均为六角纤锌矿结构的多晶薄膜,择优取向为(002)晶面生长方向.薄膜的生长速率随着氢气流量的增加呈现逐渐减小趋势,主要归因于溅射产额的减小.适当的氢气引入会引起晶粒尺寸的增加.随着氢气流量由0增加至4.0 sccm,ZnO薄膜电阻率从177?·cm急剧减小至7.2×10-3?·cm,主要是由于H施主的引入显著地增加了载流子浓度;然而进一步增加氢气流量(4.0—16.0 sccm)造成电阻率的轻微增加,主要归因于载流子浓度的减小以及过多氢杂质引入造成杂质散射的增加.所有生长获得的HMGZO薄膜平均光学透过率在波长λ～320—1100 nm范围内可达87%以上.由于Mg的作用及Burstein-Moss效应的影响造成了带隙展宽,带隙变化范围～3.49—3.70 eV,其中最大光学带隙Eg可达～3.70 eV.     

N掺杂对a-SiC:H基介质扩散阻挡层结构及性能的影响

用射频等离子增强化学气相沉积技术（RF-PECVD）制备非晶碳化硅（a-SiC:H）和不同掺氮量的碳化硅基（a-SiCN_x:H）介质薄膜.采用傅里叶红外光谱（FIRT）,X射线光电子谱仪（XPS）,纳米压入仪（Nano Indenter^A○R-XP）,Agilent 4294A高精度阻抗分析仪,俄歇能谱仪（AES）和场发射高分辨透射电镜（HRTEM）表征氮掺杂对碳化硅基薄膜化学键组成、微观结构、机械性能、介电常数和阻挡铜扩散性能的影响.实验结果表明：通过控制薄膜的氮含量可实现其介电常数在38—52范围内可调.随着反应源中氨气（NH₃）流量的增加,碳化硅基薄膜中Si—N和C—N化学键比例增加以及由此导致的薄膜微观结构致密化是氮掺杂显著提高碳化硅基薄膜机械性能、热稳定性和阻挡铜扩散性能的机理.     

氢气流量对混合物理化学气相沉积法制备MgB_2超薄膜的影响

用混合物理化学气相沉积法(Hybrid physical-chemical vapor deposition简称为HPCVD)制备了MgB2超薄膜.在背景气体压强、B2H6的流量和成膜时间等条件一定的情况下,当氢气的流量从200到400sccm范围内变化时,观察了其对成膜的影响.结果显示,随氢气流量增大,膜表面粗糙度增大,同时膜面的连接性变好,伴随着样品的超导转变温度得到提高.对于平均厚度是10nm和15nm的样品,氢气流量分别是200sccm和300sccm时,Tc分别是26K和33K与28K和37K.     

氢稀释对高速生长纳米晶硅薄膜晶化特性的影响

以SiH₄与H₂为气源,采用射频等离子体增强化学气相沉积技术,在较高的压强(230Pa)下,研究氢稀释率对纳米晶硅薄膜的生长速率和晶化特性的影响. 实验表明,薄膜的晶化率,晶粒尺寸随着氢稀释率的提高而增加,当氢稀释率为99%,薄膜的晶化率接近70%. 而沉积速率却随着氢稀释率的减小而增加,当氢稀释率从99%减小到95%时,薄膜的沉积速率由0.3nm/s 增加至0.8nm/s. 关键词： 纳米晶硅薄膜 氢稀释 晶化率 硅烷     

碳化硅薄膜脉冲激光晶化特性研究

采用XeCl准分子激光对非晶碳化硅(a-SiC)薄膜的脉冲激光晶化特性进行了研究.通过原子力显微镜（AFM）和Raman光谱技术对退火前后薄膜样品的形貌、结构及物相特性进行了分析.结果表明，选用合适的激光能量采用激光退火技术能够实现a-SiC薄膜的纳米晶化.退火薄膜中的纳米颗粒大小随着激光能量密度的增加而增大；Raman谱分析结果显示了退火后的薄膜的晶态结构特性并给出了伴随退火过程存在的物相分凝现象.根据以上结果并结合激光退火特性，对a-SiC的脉冲激光晶化机理进行了讨论. 关键词： 激光退火 晶化 碳化硅     

射频等离子体增强化学气相沉积SiNx薄膜的研究

采用射频等离子体增强化学气相沉积技术,以N2和SiH4作为反应气体,在P型硅基片上进行SiNx薄膜的沉积.使用椭偏仪对薄膜厚度和光学常量进行了测量, 用傅里叶变换红外光谱仪对SiNx薄膜的化学键合结构进行了分析.研究了基片温度、射频功率以及N2和SiH4的气体流量比率等实验工艺参量对薄膜沉积速率和光学常量的影响.结果表明,射频等离子体增强化学气相沉积技术沉积的SiNx薄膜是低含氢量的SiNx薄膜,折射率在1.65~2.15之间,消光系数k在0.2~0.007之间,当SiNx薄膜为富氮时k≤0.01,最高沉积速率高达6.0 nm/min,N2和SiH4气体流量比率等于10是富硅和富氮SiNx薄膜的分界点.     

高氢稀释制备微晶硅薄膜微结构的研究

采用高氢稀硅烷热丝化学气相沉积方法制备氢化微晶硅薄膜.其结构特征用Raman谱，红外透射谱，小角X射线散射等来表征.结果表明微晶硅的大小及在薄膜中的晶态比χ_c随氢稀释度的提高而增加.而从红外谱计算得到氢含量则随氢稀释度的增加而减少.小角X射线散射结果表明薄膜致密度随氢稀释度的增加而增加.结合红外谱和小角X射线散射的结果讨论与比较了不同相结构下硅网络中H的键合状态.认为随着晶化的发生和晶化程度的提高H逐渐移向晶粒表面，在硅薄膜中H的存在形式从以SiH为主向SiH₂ 关键词：     

The structure and optical properties of SiC film on Si (111) substrate with a ZnO buffer layer by RF-magnetron sputtering technique

We have fabricated a multiply layer SiC/ZnO on Si substrates using the RF-magnetron sputtering technique with the targets of a single crystalline SiC and a polycrystalline ZnO. The as-deposited films were annealed in the temperature range of 600–1000 °C under nitrogen ambient. We have observed a strong ultraviolet (UV) emission (370 nm) from the as-deposited SiC/ZnO film and an intense violet emission (412 nm) from the film annealed at high temperature (1000 °C) under nitrogen ambient. The SiC film quality and the PL intensities are considered to be strongly dependent on the crystalline quality of the ZnO buffer layer. With the increase of the annealing temperature, the crystalline quality of the ZnO buffer layer is improved, resulting in the improvement of the SiC film quality and the increase of the PL intensities. The thin films have been characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) to provide the evidences of photoluminescence (PL). We suggest that the UV emission could be attributed to the nanocrystal silicon particles, that the 395 nm band is related to ZnO buffer layer and has a great relation to the crystalline quality of the ZnO film, and that the violet emission is associated with the emission luminescence from 6H-SiC, which bears on the SiC film quality. The obtained results are expected to have important applications in modern optoelectronic devices.     

Effects of substrate on surface morphology, crystallinity, and photoluminescence properties of sputtered ZnO nano films

Effects of substrate on crystallinity, surface morphology, and luminescence properties of radio frequency sputtered zinc oxide (ZnO) thin films were investigated. A variety of materials such as Si (100), Si (111), Al₂O₃, quartz, and silicon carbide (SiC) wafers were examined as substrates for deposition of ZnO thin films. The results showed smooth and uniform growth of c-axis orientation films. The thickness of the layers was about 50 nm. The average grain sizes of films were about 10, 13, and 12 nm for Si (111), quartz, and SiC samples, respectively. The deposited film on Al₂O₃ showed the largest grain size, about 500 nm. Grazing incidence x-ray diffraction patterns of the samples revealed that sputtered layers on Al₂O₃ and quartz had better crystallinity with higher peak at (002) orientation compared to Si and SiC substrates. Moreover, the Al₂O₃ sample exhibited a weak peak at position of (100) planes of ZnO too. The photoluminescence spectra of the samples showed a typical luminescence behavior with a broad UV band, including a main peak at around 388 nm and a weak shoulder peak at around 381 nm, corresponding with bound excitonic recombination and free excitonic recombination, respectively. The luminescence peak revealed that the intensity of UV emission is not necessarily dependent on the grain sizes and the micro-structural quality of ZnO films.     

Microstructural investigation of nickel silicide thin films and the silicide-silicon interface using transmission electron microscopy

This article discusses the results of transmission electron microscopy (TEM)-based investigation of nickel silicide (NiSi) thin films grown on silicon. Nickel silicide is currently used as the CMOS technology standard for local interconnects and in electrical contacts. Films were characterized with a range of TEM-based techniques along with glancing angle X-ray diffraction. The nickel silicide thin films were formed by vacuum annealing thin films of nickel (50 nm) deposited on (100) silicon. The cross-sectional samples indicated a final silicide thickness of about 110 nm. This investigation studied and reports on three aspects of the thermally formed thin films: the uniformity in composition of the film using jump ratio maps; the nature of the interface using high resolution imaging; and the crystalline orientation of the thin films using selected-area electron diffraction (SAED). The analysis highlighted uniform composition in the thin films, which was also substantiated by spectroscopy techniques; an interface exhibiting the desired abrupt transition from silicide to silicon; and desired and preferential crystalline orientation corresponding to stoichiometric NiSi, supported by glancing angle X-ray diffraction results.     

富硅氮化硅薄膜的制备及其光学带隙研究

采用双极脉冲磁控反应溅射法在不同参数条件下制备了一系列氮化硅薄膜。利用数字式显微镜和紫外-可见光光谱仪研究了沉积薄膜的表面形貌及其光学带隙,利用共焦显微拉曼光谱仪比较了硅衬底、氮化硅薄膜退火前后的拉曼光谱。结果表明,氮气流量对薄膜的光学带隙影响较大,制备的薄膜主要为富硅氮化硅薄膜。原沉积薄膜的拉曼光谱存在明显的非晶硅和单晶硅峰,退火处理后非晶硅峰减弱或消失,表明薄膜出现明显的结晶化;单晶硅峰出现频移现象,表明薄膜中出现硅纳米颗粒,平均尺寸约为6.6 nm。     

Nanostructured core-shell Ni deposition on SiC particles by alkaline electroless coating

In this study, core-shell nanostructured nickel formation on silicon carbide (SiC) ceramic powders was achieved through the electroless deposition method using alkaline solutions. To produce a nano core-shell Ni deposition on the SiC surfaces, process parameters such as pH values, the type of reducer material, deposition temperature, stirring rate and activation procedure among others were determined. Full coverage of core-shell nickel structures on SiC surfaces was achieved with a grain size of between 100 and 300 nm, which was approximately the same deposition thickness on the SiC surfaces. The surface morphology of the coated SiC particles showed a homogenous distribution of nanostructured nickel grains characterized by scanning electron microscopy and X-ray diffraction techniques. The nanostructures of the crystalline Ni coatings were observed to be attractive for achieving both good bonding and dense structure. The thin core shell-structure of Ni on the SiC surfaces was assessed as a beneficial reinforcement for possible metal matrix composite manufacturing.