SiNx薄膜中硅纳米粒子的制备及表征

通过等离子增强化学气相沉积(PECVD)法, 以氨气和硅烷为反应气体, P型单晶硅和石英为衬底, 低温下(200℃)制备了含硅纳米粒子的非化学计量比氮化硅(SiN_x)薄膜. 经高温(范围500~950℃)退火处理优化了薄膜结构. 室温下测试了不同温度退火后含硅纳米粒子SiN_x薄膜的拉曼(Raman)光谱、光致发光(PL)光谱及傅立叶变换红外吸收(FTIR)光谱, 对薄膜材料的结构特性、发光特性及其键合特性进行了分析. Raman光谱表明. SiN_x薄膜内的硅纳米粒子为非晶结构. PL光谱显示两条与硅纳米粒子相关的光谱带, 随退火温度的升高此两光谱带峰位移动方向相同. 当退火温度低于800℃时, PL光谱峰位随退火温度的升高而蓝移. 当退火温度高于800℃时, PL光谱峰位随退火温度的升高而红移. 通过SiNx薄膜的三种光谱分析发现薄膜的光致发光源于硅纳米粒子的量子限制效应. 这些结果对硅纳米粒子制备工艺优化和硅纳米粒子光电器件的应用有重要意义.     

CO在U2N3+xOy薄膜表面反应特性研究

采用磁控溅射沉积方法在Si基底表面制备U₂N_3+xO_y薄膜, 采用X光电子能谱(XPS)分析技术观测CO气氛环境下U₂N_3+xO_y薄膜表面腐蚀行为, 以期获得U₂N_3+xO_y薄膜在CO环境下的表面腐蚀机理。结果表明: 超高真空条件下, CO在U₂N_3+xO_y薄膜表面表现为氧化特性; CO在薄膜表面吸附解离生成的C以无定形碳形式聚集在薄膜表面, 深度剖析过程中并未观察到C向U₂N_3+xO_y薄膜内部扩散; 而解离生成的氧在薄膜内扩散并发生氧化反应, 生成高价氧化物或铀氮氧化物和氮。氧化反应生成的氮向薄膜内部扩散, 并在次表面反应生成富氮中间产物。随着CO暴露反应进程的推进, 富氮层逐渐向薄膜内部迁移, 这是导致U4f谱卫星峰变化的主要原因。     

常压化学气相沉积方法制备非晶硅薄膜及其光致发光性能研究

使用改进的常压化学气相沉积(APCVD)系统制备了非晶硅薄膜,测量了样品的光致发光特性,使用Raman光谱和X射线光电子能谱(XPS)谱测量了薄膜的微结构特征.样品在523 nm出现发光峰,Raman光谱和XPS谱表明制备的薄膜结构中存在富氧相和富硅相的分相现象,分析认为相界面的存在是产生发光的原因.Raman光谱分峰结果表明薄膜中存在纳米晶粒.     

硒化锌量子点二维阵列的LB方法制备与表征

以去铁铁蛋白作为生物模板合成了硒化锌量子点,采用Langmuir-Blodgett技术在硅基质表面制备1:4的EA/SMA的LB薄膜并将硒化锌核铁蛋白吸附组装到EA/SMA薄膜上形成二维阵列。用紫外-可见吸收光谱(UV-Vis)、荧光光谱(PL)、傅里叶转换红外光谱(FTIR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)进行表征,结果表明成功制备得到了硒化锌量子点核铁蛋白单分子层二维阵列。这种排列在固体表面的有序微观尺寸的纳米结构由于其独特的光学和生物学特性在生物传感、药物和诊断等领域具有潜在的应用前景。     

nc-Si/a-SiO_x:H复合薄膜的结构及光吸收特性

采用 PECVD技术制备的 a－ SiO_x:H (0 SiO_x:H基质的量子点复合膜（ nc－ Si/a－ SiO_x:H）。利用 TEM技术, Raman散射谱和光吸收谱等 ,较系统地研究了该复合膜的膜结构和光吸收特性。实验结果表明：纳米硅嵌埋颗粒呈多晶结构,颗粒大小随退火温度升高而增大。复合膜光吸收边随纳米硅颗粒尺寸的减小发生了蓝移,表现出明显的量子限域效应。     

气相沉积硅薄膜微结构及悬挂键缺陷研究

在单晶Si(100)基体上利用电子回旋共振等离子体增强化学气相沉积法制备硅薄膜,并采用X射线衍射谱(XRD)、透射电镜(TEM)、Raman光谱、电子自旋共振(ESR)波谱等实验方法研究了不同Ar流量下硅薄膜微结构及悬挂键密度的变化。XRD及TEM实验结果得出,制备的硅薄膜的晶粒尺寸为12~16 nm,属纳晶硅薄膜。薄膜结晶度随镀膜时Ar流量增大而增大,而悬挂键密度则先迅速减小而后缓慢增大。当Ar流量为70 ml/min(标准状态)时,薄膜的悬挂键密度达到最低值4.42×1016cm-3。得出最佳Ar流量值为70 ml/min。     

电弧离子镀Cr1-xAlxN硬质薄膜的成分、结构与性能

采用电弧离子镀的分离靶弧流调控技术在硬质合金基体上制备了4组不同Al含量的Cr_1-xAl_xN硬质薄膜, 采用SEM、XPS、GIXRD、Nanoindenter及划痕仪分别表征了薄膜的形貌、成分、相结构和力学性能。结果表明: 4组薄膜厚度分别为1.28、1.42、1.64和1.79 μm; 成分x随着Al靶的弧流相对增大而增大, 分别为x=0.41、0.53、0.64和0.73; 相结构与成分密切相关, 当x=0.41时, 薄膜呈单一的c-(Cr,Al)N相, 而当x≥0.53时, 则由c-(Cr,Al)N相和hcp-AlN相混相构成; 随着Al含量增加, 晶粒尺寸先减小后增大, 在x=0.64时达到最小值8.9 nm; 相应地硬度则先增大后减小, 在x=0.64时达到峰值35.3 GPa; 4组Cr_1-xAl_xN薄膜的膜基结合良好, 结合力均在60 N以上。综合测试结果发现, 当x=0.53时, Cr_1-xAl_xN薄膜的韧性最佳, 弹性恢复系数最高为57.4%, 同时兼具较高的硬度34.7 GPa, 此时薄膜具有最佳的综合性能。     

退火对两种硅基薄膜的结构及发光影响

采用双离子束共溅射沉积方法制备了两种复合硅基薄膜SiOxCy和SiOxNy薄膜,对两种薄膜进行后退火处理,并分别对样品进行PL、FTIR、XPS谱测试分析,比较退火前后的发光及结构的变化。两种样品的光致发光测试谱(PL)表明:退火前后都有两个发光峰位-都存在470nm的发光峰位,它来自于硅基薄膜中中性氧空位缺陷(O3≡Si-Si≡O3),是由于氧原子配位的二价硅的单态-单态之间的跃迁所致,其发光强度随退火温度的升高而变化。进一步的FTIR和XPS的测试谱表明另外一个发光峰位420nm(SiOxCy薄膜)和400nm(SiOxNy薄膜)分别来自于掺杂杂质(C和N)与硅基薄膜中的Si、O组成的复合结构。而两种样品经过退火处理后掺杂所引起的发光峰位强度随退火温度的升高而增强,说明退火温度的升高有利于发光机制的形成。     

水相制备CdSe量子点及其ZnS核壳结构量子点

因具有较宽的可调控发光范围,CdSe量子点及其ZnS核壳结构量子点受到了研究者们的普遍关注。采用水相回流法合成了CdSe量子点及其ZnS核壳结构量子点,并结合透射电镜(TEM)、X射线衍射(XRD)、紫外-可见光吸收光谱(UV-Vis)和荧光光谱(PL)对样品进行表征。TEM结果表明,合成的量子点粒径分布较宽且结晶度较高;从XRD分析结果可以看出,CdSe量子点为闪锌矿结构,沿着晶面向外生长ZnS壳层后,谱峰向高角度偏移;从UV-Vis和PL分析结果可以看出,CdSe量子点于500 nm处出现吸收肩峰,于644 nm处出现半高宽较宽的缺陷发光峰;随着反应时间的延长,于577 nm处出现本征发光峰。包覆了ZnS壳层后,量子点不仅发光强度明显增大,而且稳定性显著提高。该合成方法节能环保、生产效率高,具有较大的应用空间。     

不同横向尺寸单层Ti3C2Tx纳米片的制备及其电化学性能研究

近年来, 一种新型二维过渡金属碳化物及氮化物(MXene)凭借大的比表面积、良好的亲水性、金属导电性等物理化学性质而广受关注。通过LiF和HCl刻蚀Ti₃AlC₂的Al层, 改变机械剥离强度和方式, 以及离心速率和时间, 可控制备出平均横向尺寸为625 和2562 nm的单层Ti₃C₂T_x型MXene。借助扫描电子显微镜(SEM)、透射电子显微镜(TEM)和X射线衍射仪(XRD)对二维Ti₃C₂T_x进行形貌、结构和成分的表征。使用电化学工作站表征Ti₃C₂T_x的电化学性能。结果表明: 小片层Ti₃C₂T_x(625 nm)的质量比电容高达561.9 F/g, 远高于文献报道的石墨烯、碳纳米管和二氧化锰等电极材料; Ti₃C₂T_x电极在循环测试10 ⁴次后, 其比电容仍保持初始96%的容量。     

Microstructures of microcrystalline silicon thin films prepared by hot wire chemical vapor deposition

Undoped hydrogenated microcrystalline silicon (μc-Si:H) thin films were prepared at low temperature by hot wire chemical vapor deposition (HWCVD). Microstructures of the μc-Si:H films with different H₂/SiH₄ ratios and deposition pressures have been characterized by infrared spectroscopy X-ray diffraction (XRD), Raman scattering, Fourier transform (FTIR), cross-sectional transmission electron microscopy (TEM) and small angle X-ray scattering (SAXS). The crystallization of silicon thin film was enhanced by hydrogen dilution and deposition pressure. The TEM result shows the columnar growth of μc-Si:H thin films. An initial microcrystalline Si layer on the glass substrate, instead of the amorphous layer commonly observed in plasma enhanced chemical vapor deposition (PECVD), was observed from TEM and backside incident Raman spectra. The SAXS data indicate an enhancement of the mass density of μc-Si:H films by hydrogen dilution. Finally, combining the FTIR data with the SAXS experiment suggests that the Si---H bonds in μc-Si:H and in polycrystalline Si thin films are located at the grain boundaries.     

Annealing effects on the structural and optical properties of growth ZnO thin films fabricated by pulsed laser deposition (PLD)

Annealed ZnO thin film at 300, 350, 400, 450 and 500 °C in air were deposited on glass substrate by using pulsed laser deposition. The effects of annealing temperature on the structural and optical properties of annealed ZnO thin films by grazing incident X-ray diffraction (GIXRD), transmittance spectra, and photoluminescence (PL) were investigated. The GIXRD reveal the presence of hexagonal wurtzite structure of ZnO with preferred orientation (002). The particle size is calculated using Debye–Scherrer equation and the average grain size were found to be in the range 5.22–10.61 ± 0.01 nm. The transmittance spectra demonstrate highly transparent nature of the films in visible region (>70 %). The calculation of optical band gap energy is found to be in the range 2.95–3.32 ± 0.01 eV. The PL spectra shows that the amorphous film gives a UV emission only and the annealed films produce UV, violet, blue and green emissions this indicates that the point defects increased as the amorphous film was annealed.     

Thickness dependent structural, electronic, and optical properties of Ge nanostructures

In the present paper, we have investigated structural, optical as well as electronic properties of electron beam evaporated Ge thin films having layer thicknesses ranging from ultra-thin (5 nm) to thick (200 nm). The Raman spectra show that all peaks are shifted towards lower wave number as compared to their bulk counterparts and are considered as a signature of nanostructure formation and quantum confinement effect. The Raman line exhibits transformation from nanocrystalline to microcrystalline phase with a reduction in blue shift of peak position with increase in Ge film thickness (>5 nm). Similarly, the optical absorption spectra corresponding to these films also show reduction in blue shift effect, although Ge 5 nm film shows the absorption behaviour quite different from higher thickness films. The corresponding band gap values obtained from absorption measurements are much larger than bulk Ge and are mainly attributed to the effect of quantum confinement as expected for small size particles calculated from GIXRD patterns. AFM data in each case are correlated and discussed with structural as well as optical results to support the effect of growth morphology on the above-mentioned observations. The results are further supported by photoelectron spectroscopy (PES), photoluminescence (PL) and resistivity measurements and are interpreted in terms of crystallinity and quantum confinement effect.     

Preparation and photoluminescence of nanocrystalline Si-rich silicon oxide films by PECVD

Nanocrystalline Si-rich silicon oxide films were deposited using plasma enhanced chemical vapor deposition technique with the mixture of silane (SiH₄), nitrous oxide (N₂O) and hydrogen (H₂) as gas source on quartz glass substrate at the substrate temperature of 300 °C. The effect of the ratio N₂O/SiH₄ on the oxidation, microstructures and photoluminescence (PL) of the as-deposited Si-rich silicon oxide films was investigated with FTIR, XRD and HRTEM. The results reveal that with the increasing ratio of N₂O/SiH₄, more amounts of oxygen are incorporated in the as-deposited films and more nanosized silicon particles are embedded in the films, forming nanocrystalline Si-rich silicon oxide films. The quantum confinement effect or the cooperation of quantum confinement and luminescence center results in the nanocrystalline Si-rich silicon oxide films of higher PL intensity.     

CdxTe薄膜的共蒸发法制备及其表征

采用CdTe和Te双源共蒸发的方法, 调控CdTe和Te源的蒸发速率, 首次制备出一系列不同x组分的Cd_xTe二元化合物薄膜, 并在N₂气气氛下进行185℃退火处理。通过XRD、SEM、紫外-可见吸收光谱分析及暗电导率-温度关系对Cd_xTe薄膜的结构、形貌、光学和电学性质进行表征。紫外-可见吸收光谱分析表明, 不同x组分的Cd_xTe薄膜, 其禁带宽度可在0.99~1.46 eV之间变化, 随着x值从0.8减小到0.2, 吸收边向长波方向移动, 而且透过率也显著下降。XRD结果表明, x值小于0.6时, 刚沉积的Cd_xTe薄膜为非晶相; 随着x的值逐渐靠近1, 刚沉积的薄膜明显结晶, 沿CdTe(111)方向择优生长, 退火处理促使薄膜从非晶转变为多晶。Cd_xTe薄膜的导电类型为p型, 其暗电导率随温度的上升而增大, 当温度继续升高至临界点时, 薄膜暗电导率-温度关系出现反常。这些结果表明, Cd_xTe薄膜将有望用于CdTe薄膜太阳电池以拓展电池的长波光谱响应。     

Sn对Ge-Se-Te玻璃结构与光学特性的影响

采用熔融淬冷法制备了系列Ge₃Se₅Te₂Sn_x(x=0、0.4、0.8、1.2、1.6、2.0, mol%)硫系玻璃。采用X射线衍射(XRD)图谱、差示扫描量热曲线(DSC)、可见/近红外光谱、傅里叶红外(FTIR)光谱、显微拉曼光谱等手段对玻璃的物化性能及结构进行表征, 研究发现Sn的引入导致Ge-Se-Te玻璃系统物化性能的变化: 玻璃的转变温度T_g降低、红外截止波长发生红移, 并有效地降低了杂质吸收峰对样品红外透过率的影响。利用Philips网络约束理论计算的玻璃平均配位数及拉曼光谱的变化, 讨论了引入Sn对Ge-Se-Te玻璃的影响。     

电子束再结晶法制备的纳米硅薄膜室温光致发光特性

用电子束再结晶的方法对非晶硅氢材料进行快速退火,成功地制备出纳米硅薄膜,在室温下观察到光致红、蓝发光带,峰位约在１．７ｅＶ和２．５ｅＶ处,ＸＲＤ和ＰＬ谱结果表明：晶化程度的变化引起红、蓝光带强度及在整个发光谱中所占比例的改变,在我们的实验中,电子束能量密度２．７Ｗ／ｃｍ＾２的晶化样品具有强的发光带。     

Optical properties of nano-silicon

We investigated the optical properties of silicon clusters and Si nanocrystallites using photolumine-scence (PL) and Raman scattering technique. Broad luminescence band in the red region was observed from Si-doped SiO₂ thin films deposited by co-sputtering of Si and SiO₂ onp-type Si (100) substrates, annealed in Ar and O₂ atmosphere. Nanocrystalline Si particles fabricated by pulsed plasma processing technique showed infrared luminescence from as grown film at room temperature. Raman spectra from these films consisted of broad band superimposed on a sharp line near 516 cm⁻¹ whose intensity, frequency, and width depend on the particle sizes arising from the phonon confinement in the nanocrystalline silicon. We also performed PL, Raman and resonantly excited PL measurements on porous silicon film to compare the optical properties of Si nanostructures grown by different techniques. An extensive computer simulation using empirical pseudo-potential method was carried out for 5–18 atoms Si clusters and the calculated gap energies were close to our PL data. Paper presented at the 5th IUMRS ICA98, October 1998, Bangalore.     

Effects of annealing ambient on the photoluminescence properties of Si-rich oxide/SiO2 multilayer films containing Si-nanocrystals

In this study, Si-nanocrystals (Si-NCs) have been prepared by annealing Si-rich oxide (SRO)/SiO₂ multilayer films in Ar and N₂, and the effects of annealing ambient on the photoluminescence (PL) properties are studied. XPS results show that the chemical compositions for the SRO and SiO₂ layers are SiO_1.1 and SiO₂, respectively. FTIR results show that phase separation between Si and SiO₂ occurs after annealing treatment, and Si-NCs are obtained which have been proved by the TEM images. Large and high density Si-NCs are obtained in the Ar-annealed film, and high structural disorder exists at the interface of Si-NCs. Compared with the film annealed in N₂, a 2.4 times PL enhancement is obtained for the Ar-annealed sample, and the PL peak shifts toward low energy. Two lifetime distribution bands are obtained by fitting the time-resolved PL spectra, and the proportion of slow PL decay component increases from 69.7 to 84.0 %. The PL intensity for the Ar-annealed film is further enhanced by hydrogen passivation, and the slow PL decay component is increased to 87.5 %. Analyses show that both interface states recombination and quantum confinement effect (QCE) related optical transition in the Si-NCs exist in the optical emission process, and intense PL can be obtained only when the QCE become dominant PL mechanism.