尺寸可控的纳米硅的生长模型和实验验证

基于经典热力学理论，对a-SiN_x/a-Si:H/a-SiN_x三明治结构或a-Si:H/a-SiN_x多层膜结构中纳米硅成核，以及从球形到鼓形的生长过程进行了研究. 建立了限制性晶化理论模型：在纳米硅生长过程中，由于界面能增大将导致生长停止，给出限制性晶化条件——a-Si:H子层厚度小于34 nm. 在激光晶化和常规热退火两种方法形成的a-SiN_x/nc-Si/a-SiN_x三明治结构和nc-Si/a-SiN_x多层膜结构中验证了该理论模型. 关键词： 非晶硅 纳米硅 激光辐照 结晶     

包含硅量子点的富硅SiNx 薄膜结构与发光特性

采用等离子体增强化学气相沉积法, 以NH₃与SiH₄为反应气体, n型单晶硅为衬底, 低温(220 ℃)沉积了富硅氮化硅(SiN_x)薄膜. 在N₂氛围中, 于500–1100 ℃ 范围内对样品进行了热退火处理. 采用Raman 光谱技术分析了薄膜内硅量子点的结晶情况, 结果表明, 当退火温度低于950 ℃时, 样品的晶化率低于18%, 而当退火温度升为1100 ℃, 晶化率增加至53%, 说明大部分硅量子点都由非晶态转变为晶态. 实验通过Fourier 变换红外吸收(FTIR)光谱检测了样品中各键的键合结构演变, 发现Si–N键和Si–H键随退火温度升高向高波数方向移动, 说明了薄膜内近化学计量比的氮化硅逐渐形成. 实验还通过光致发光(PL)光谱分析了各样品的发光特性, 发现各样品中均有5个发光峰, 讨论了它们的发光来源, 结合Raman光谱与FTIR光谱表明波长位于500–560 nm的绿光来源于硅量子点, 其他峰则来源于薄膜内的缺陷态. 研究了硅量子点的分布和尺寸对发光带移动的影响, 并根据PL峰位计算了硅量子点的尺寸, 其大小为1.6–3 nm, 具有良好的限域效应. 这些结果有助于制备尺寸不同的硅量子点和基于硅量子点光电器件的实现. 关键词： 硅量子点 氮化硅薄膜 光致发光 Fourier 变换红外吸收     

溅射压强对TiN/SiNx纳米多层膜微观结构及力学性能的影响

利用磁控溅射方法在不同溅射压强条件下制备了TiN/SiN_x纳米多层膜.多层膜的微观结构及力学性能分别用X射线衍射仪、原子力显微镜及纳米压痕仪来表征.结果表明随着溅射压强的增大,多层膜的界面变模糊,TiN层的择优取向由(200)晶面过渡到(111)晶面.与此同时,多层膜的表面粗糙度增大,硬度和弹性模量随溅射压强的增大而减小.多层膜力学性能的差异主要是由于薄膜的周期性结构及致密度存在差异所致. 关键词： x多层膜')" href="#">TiN/SiN_x多层膜 界面宽度 表面形貌     

激光限制结晶技术制备nc-Si/SiO2多层膜

在等离子体增强化学气相淀积系统中，采用aSi:H层淀积和原位等离子体氧化相结合的逐层生长技术制备了aSi:H/SiO_2多层膜.在激光诱导限制结晶原理基础上，使用KrF准分子脉冲激光为辐照源，对aSi:H/SiO_2多层膜进行辐照，使纳米级厚度的aSi:H子层晶化.Raman散射谱和电子衍射谱的结果表明，经过激光辐照后纳米Si颗粒在原始的aSi:H子层内形成，晶粒尺寸可以根据aSi:H层的厚度精确控制.还研究了样品的光致发光（PL）特性以及激光辐照能量密度对PL性质的影响. 关键词： 脉冲激光 多层膜 限制结晶     

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SiN_x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SiN_x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SiN_x薄膜以非晶状态存在,硬度值仅为18GPa左右;基片温度 关键词： x')" href="#">SiN_x 磁控溅射 微观结构 硬度     

微波ECR磁控溅射制备SiNx薄膜的XPS结构研究

利用微波电子回旋共振等离子体增强非平衡磁控溅射法在不同N₂流量下制备无氢SiN_x薄膜.通过X光电子能谱、纳米硬度仪等表征技术,研究了不同N₂流量下制备的SiN_x薄膜的化学键结构、化学键含量、元素配比及各元素沿深度分布.研究结果表明,N₂流量是影响SiN_x薄膜化学键结构、元素配比、元素延深度分布等性质的主要因素.在N_{2关键词： x}')" href="#">SiN_x 磁控溅射 XPS 化学键结构     

发光纳米硅/二氧化硅多层膜的特性与氢气氛退火的影响

利用等离子体增强化学气相沉积法制备了氢化非晶硅/二氧化硅多层膜，通过两步热退火的方法获得了尺寸可控的纳米硅/二氧化硅多层结构，晶粒尺寸约为4nm，在室温下观察到了较强的光致可见发光，其发光峰位于750nm.在此基础上，发现合适的氢气氛退火能有效地提高材料的发光强度.电子顺磁共振实验表明氢气氛退火有效地降低了纳米硅中的非辐射复合中心而导致发光效率的提高.     

掺铒Si/Al2O3多层结构中结晶形态对1.54 μm发光的影响

利用脉冲激光沉积的方法制备掺铒 Si/Al₂O₃多层结构薄膜,获得了由纳米结构的Si作为感光剂增强的Er³⁺在1.54 μm高效发光.利用拉曼散射、高分辨透射电镜和光致发光测量研究了在不同退火温度下（600—1000 ℃）纳米结构Si层的结晶形态变化,及对Er³⁺在1.54 μm的发光的影响特征.研究发现最佳发光是在退火温度600—700 ℃.在这个条件下纳米Si的尺寸和密度,Si和Er的作用距离以及Er^{3+ 关键词： 铒 纳米硅 能量转移 氧化铝}     

线性微波化学气相沉积制备SiNx薄膜的微结构及光学性能研究

利用自主研发的线性微波化学气相沉积系统在不同微波功率、微波占空比、基片温度、特气比例条件下制备了SiN_x薄膜. 通过扫描电子显微镜、椭圆偏振仪等表征测量技术, 研究了不同工艺参数对SiN_x薄膜表面形貌、元素配比、折射率、沉积速度的影响, 并探讨了薄膜元素配比、折射率、沉积速度间的关系. 结果表明: 利用线性微波沉积技术, 不同工艺参数下制备的SiN_x薄膜组成元素分布均匀, 同时具有平整的表面状态; 特气比例和微波占空比是影响薄膜折射率的最主要因素, 薄膜折射率在1.92–2.33之间连续可调; 微波功率、微波占空比、沉积温度、特气比例都对SiN_x 薄膜沉积速度影响较大, 制备的SiN_x薄膜最大沉积速度为135 nm·min^-1.     

纳米Si/SiO2多层膜的结构表征及发光特性

采用等离子体化学气相沉积系统生长非晶硅薄膜并用原位等离子体氧化的方法制备出具有不同子层厚度的非晶Si/SiO₂多层膜,然后利用限制性晶化原理使非晶硅层晶化生成纳米硅。利用Raman、TEM等手段对薄膜结构进行了系统表征,在室温下观测到了光致发光信号,其发光峰峰位在750nm附近。进而在样品上下表面蒸镀电极,构建了电致发光原型器件并观测到了室温下的电致发光谱,开启电压约为6V,有两个明显的发光带,分别位于在650nm和520nm处。初步探讨了纳米硅及纳米硅/二氧化硅界面态对发光特性的影响。     

Photo-modification and synthesis of semiconductor nanocrystals

Both photo-oxidation and photosynthesis manifest a strong interaction between nanoparticles and photons due to the large surface area-to-volume ratio. The final sizes of the semiconductor nanocrystals are determined by the photon energy during these phenomena. The photosynthesis is demonstrated in a Si-rich oxide and is similar to thermal synthesis, which involves the decomposition of SiO_x into Si and SiO₂, that is well known and often employed to form Si or Ge nanocrystals embedded in SiO₂ by annealing SiO_x at high temperature. However, photosynthesis is much faster, and allows the low-temperature growth of Si nanocrystals and is found to be pronounced in the SiO nanopowder, which is made by thermal CVD using SiH₄ and O₂. The minimum laser power required for the photosynthesis in the SiO nanopowder is much lower than in the Si-rich oxide formed by the co-sputtering of Si and SiO₂. This is attributed to the weak bond strength of Si-Si and Si-O in the SiO nanopowder. Photosynthesis, which can control the size and position of Si nanocrystals, is a novel nanofabrication technique making the best use of the strong interaction between photons and nanoparticles.     

Effect of laser annealing on crystallinity of the Si layers in Si/SiO2 multiple quantum wells

We report on continuous-wave laser induced crystallisation processes occurring in Si/SiO₂ multiple quantum wells (MQW), prepared by remote plasma enhanced chemical vapour deposition of amorphous Si and SiO₂ layers on quartz substrates. The size and the volume fraction of the Si nanocrystals in the layers were estimated employing micro-Raman spectroscopy. It was found that several processes occur in the Si/SiO₂ MQW system upon laser treatment, i.e. amorphous to nanocrystalline conversion, Si oxidation and dissolution of the nanocrystals. The speed of these processes depends on laser power density and the wavelength, as well as on the thickness of Si-rich layers. At optimal laser annealing conditions, it was possible to achieve ∼100% crystallinity for 3, 5 and 10 nm thickness of deposited amorphous Si layers. Crystallization induced variation of the light absorption in the layers can explain the complicated process of Si nanocrystals formation during the laser treatment.     

Size control of Si nanocrystals by two-step rapid thermal annealing of sputtered Si-rich oxide/SiO2 superlattice

Controllable size of silicon (Si) nanocrystals can be achieved by a two-step rapid thermal annealing technique consisting of rapid annealing at 1000°C in nitrogen ambient and rapid oxidation at 600–800°C of a radio frequency magnetron co-sputtered Si-rich oxide/SiO₂ superlattice structure. The photoluminescence (PL) spectra related to Si nanocrystals were observed in the visible range (600–900 nm). After rapid oxidation, the size of the nanocrystals was reduced and the quality of the Si nanocrystal/SiO₂ interface was improved, resulting in a blue shift and an increase of the PL peak intensity. Finally, annealing in air increases the PL intensity further.     

Formation of Si structure in glass with a femtosecond laser

Mixing metallic Al into the starting material for silicate glass is proposed as a means of forming Si structures in glass. We confirmed that Si nanocrystals are space-selectively deposited in silicate glass via a thermite reaction triggered by femtosecond laser pulses. Small Si particles were transformed into larger, but still micrometer sized, Si particles by laser irradiation. These structures grew to micro-size particles due to the thermite reaction promoted by heat treatment. We discuss what effect the irradiation of the focused laser pulse had on the Si deposition process in the laser-irradiated region. Localized high temperatures and pressures and generation of shock waves appear to be very important in forming Si-rich structures that contribute to the growth of Si particles. The diffusion of calcium ions by the generation of shock waves and the presence of Al-rich structures is important for forming Si-rich structures such as Si clusters, which is achieved by continuously breaking Si–O bonds using localized high temperatures.     

(Si,Er)双注入热氧化硅的光致发光

采用强流金属蒸汽真空弧（MEVVA）离子源注入机，先将Si大束流注入热氧化SiO2/单晶硅，直接形成镶嵌在SiO2中的纳米晶Si，再小束流注入Er。Er离子在掺杂层中的浓度可达10^21cm^-3量级，大大地提高了作为孤立发光中心的Er^3 浓度。在77K和室温下，观察到了Er^3 的1.54цm特征发射。     

用硅离子注入方法制备的纳米硅的拉曼散射研究

在直角散射配置下测量了纳米硅样品的拉曼散射谱及其退火温度的关系。结果表明,在８００℃以下退火的样品只观察到单晶硅衬底的光学声子模,在９００℃以上退火,才观察到纳米硅的特征拉曼散射峰。在１２００℃下退火后,纳米硅的特征拉曼散射峰消失,观察到类似于非晶硅的光学声子特征峰,可能表示纳米硅不能承受这样的高温热退火。这些结果进一步证实了光致发光谱的结果。     

Interfacial reactions of rf-sputtered TiNi thin films on (100) silicon with a SiN diffusion barrier

Silicon nitride (SiN) with a 50?nm thickness on Si(100) as a thermal barrier was obtained by plasma-enhanced chemical vapour deposition (PECVD). TiNi thin films were rf sputtered on a SiN/Si substrate and then annealed at 400–700°C for 30?min. Their interfacial reactions were studied using transmission electron microscopy, X-ray diffraction and Auger electron spectroscopy analyses. Experimental results show that the thickness of reaction layer in TiNi/SiN/Si specimens is clearly reduced, compared with that in TiNi/Si specimens under the same annealing conditions. The significant effect of the SiN layer as a diffusion barrier in TiNi/SiN/Si can be recognized. N and Si atoms diffuse from the SiN layer to react with TiNi films at 500°C and 600°C respectively. The TiN_{1 ? x} phase is formed in specimens annealed at 500°C, and mixed Ti₂Ni₃Si and Ti₄Ni₂O compounds are found at 600°C. In the specimen annealed at 700°C, the reaction layer has sublayers in the sequence TiNi/Ti₄Ni₂O/Ti₂Ni₃Si/TiN_{1 ? x} /SiN/Si. The SiN thermal barrier obtained by PECVD caused quite different diffusion species to cross the interfaces between TiNi/SiN/Si and TiNi/Si specimens during the annealing.     

Structural and photoluminescence properties of silicon nanocrystals embedded in SiC matrix prepared by magnetron sputtering

Si nanocrystals (NCs) embedded in an SiC matrix were prepared by the deposition of Si-rich Si_1?xC_x/SiC nanomultilayer films using magnetron sputtering, subsequently followed by thermal annealing in the range of 800～1200 °C. As the annealing temperature increases to 1000 °C, Si NCs begin to form and SiC NCs also start to emerge at the annealing temperature of 1200 °C. With the increase of annealing temperature, two photoluminescence (PL) peaks have an obvious redshift. The intensity of the low-energy PL peak around 669～742 nm gradually lowers, however the intensity of high-energy PL peak around 601～632 nm enhances. The low-energy PL peak might attribute to dangling bonds in amorphous Si (a-Si) sublayers, and the redshift of this peak might be related to the passivation of Si dangling bonds. Whereas the origin of the high-energy PL peak may be the emergence of Si NCs, the redshift of this peak correlates with the change in the size of Si NCs.     

软X射线Mo/B_4C多层膜应力和热稳定性研究

为了实现7nm波段Mo/B4C多层膜反射镜元件的制备,研究了不同退火方式对Mo/B4C多层膜应力和热稳定性的影响。首先,采用直流磁控溅射方法分别基于石英和硅基板制作Mo/B4C多层膜样品,设计周期为3.58nm、周期数为60,Mo膜层厚度与周期的比值为0.4。其次,采用不同的退火方式对所制作的样品进行退火实验,最高退火温度500℃。最后,分别采用X射线掠入射反射、X射线散射和光学干涉仪的方法对退火前后的Mo/B4C多层膜的周期、界面粗糙度和应力进行测试。测试结果表明采用真空退火方式能够有效降低Mo/B4C多层膜的应力,且退火前后Mo/B4C多层膜的周期和界面粗糙度无明显变化,证明Mo/B4C多层膜在500℃以内具有很好的热稳定性。     

Pulsed laser deposition of Co and growth of CoSi2 on Si(111)

Monolayers of Co were prepared by pulsed laser deposition (PLD) and thermal deposition (TD) on Si(111) substrates. The surface structure and morphology were studied as a function of annealing temperature with scanning tunneling microscopy and low-energy electron diffraction (LEED). Comparing PLD to TD in the monolayer regime, we find surface phases with lower Co content in the top layer for annealing temperatures below 500 °C, indicating an implantation of Co into the Si substrate. The implanted Co leads to an increased intermixing of Co and Si and a higher density of nucleation centers for Co multilayers produced by PLD compared to TD. Multilayer PLD films therefore show an improved film quality, which is detected by an increased intensity of the LEED reflectivity. PACS 68.37.Ef; 61.14.Hg; 68.55.-a