硅纳米线/氧化钒纳米棒复合材料的制备与气敏性能研究

采用纳米球光刻和金属辅助刻蚀法以p型单晶硅片制备了硅纳米线阵列, 并以此作为基底, 通过溅射不同时长的金属钒薄膜并进行热退火氧化处理, 制备出硅纳米线/氧化钒纳米棒复合材料. 采用扫描电子显微镜和X射线衍射仪表征了该复合材料的微观特性, 结果表明该结构增大了材料的比表面积, 有利于气体传感, 并且镀膜时间对后续生长的氧化钒纳米棒形貌有明显影响. 采用静态配气法在室温下测试了该复合材料对NO₂的气敏性能, 气敏测试结果表明沉积钒膜的时间对复合材料的气敏性能影响较大. 当选择合适的镀膜时间时, 适量氧化钒纳米棒增加了材料表面积并形成大量pn结结构, 相比纯硅纳米线对NO₂气体的灵敏度有明显提升, 且在室温下表现出优良的选择性. 同时, 对气敏机理做了定性解释, 认为硅纳米线与氧化钒纳米棒之间形成的pn结及能带结构在接触NO₂ 时的动态变化是其气敏响应提升的主要机制.     

n型有序多孔硅基氧化钨室温气敏性能研究

利用电化学腐蚀方法制备了n型有序多孔硅, 并以此为基底用直流磁控溅射法在其表面溅射不同厚度的氧化钨薄膜. 利用X射线和扫描电子显微镜表征了材料的成分和结构, 结果表明, 多孔硅的孔呈柱形有序分布, 溅射10 min的WO₃薄膜是多晶结构, 比较松散地覆盖在整个多孔硅的表面. 分别测试了多孔硅和多孔硅基氧化钨在室温条件下对二氧化氮的气敏性能, 结果表明, 相对于多孔硅, 多孔硅基氧化钨薄膜对二氧化氮的气敏性能显著提高. 对多孔硅基氧化钨复合结构的气敏机理分析认为, 多孔硅和氧化钨薄膜复合形成的异质结对良好的气敏性能起到主要作用, 氧化钨薄膜表面出现了反型层引起了气敏响应时电阻的异常变化. 关键词： 有序多孔硅 氧化钨薄膜 二氧化氮 室温气敏性能     

银纳米膜的电化学制备方法及性能表征

采用电沉积方法在表面活性剂与电解液的界面上制备了银纳米膜。通过对甲磺酸银体系和硝酸银体系中纳米银膜的电沉积速率及纳米银膜颗粒进行比较发现，相同条件下硝酸银体系得到的纳米膜晶粒粒径比较小，膜的生长速率较快。选定硝酸银体系为电沉积体系。考察了槽压、电解液的浓度和温度及溶液的pH值对制备银纳米膜的影响，确立了制备银纳米膜的最佳工艺条件为硝酸银浓度5mmol/L，槽压4V，pH3.0,硬脂酸的质量浓度0.2g/L。实验表明，最佳工艺条件下制备的银纳米膜晶粒粒径均匀，平均粒径在20nm左右，近似球形。本方法制备的银纳米膜将在非线性光学材料方面得到应用。     

介质阻挡放电等离子体沉积多孔硅纳米颗粒膜的光发射及红外光谱

用介质阻挡放电(DBD)等离子体增强化学气相沉积(PECVD)的方法,以硅烷为源气体,在沉积区域加载脉冲负偏压进行调节,在玻璃基片上沉积得到具有荧光特征的多孔硅纳米颗粒膜。沉积过程的发射光谱结果表明,在412 nm处出现S iH*(A2Δ→X2Π0-0)特征峰,证明放电沉积过程中存在不同程度的硅烷裂解。将脉冲负偏压固定在-300 V,当占空比从0.162增大到0.864时,薄膜的红外光谱显示S i—O—S i在1 070cm-1伸缩振动吸收峰与800 cm-1的弯曲振动峰都有所增强,而930 cm-1的S i—H弯曲振动减弱。说明随着占空比的增加,S i—O—S i键的结合越来越明显。     

CdS纳米颗粒填充的自支撑多孔硅光致发光特性

为了研究CdS纳米颗粒填充的自支撑多孔硅的光致发光特性,选用电阻率为0.01~0.02Ω·cm的P型硅片,先采用二步阳极氧化法制备自支撑多孔硅,再利用电泳法将CdS纳米颗粒填充入该自支撑多孔硅中.采用扫描电子显微镜、X射线能谱分析、X射线衍射分析、光致发光谱分析对所制备样品的形貌、相结构、组份及发光性能进行研究.实验结果表明:自支撑多孔硅内部成功填充了CdS纳米颗粒,该CdS纳米颗粒衍射峰为(210);CdS纳米颗粒填充的自支撑多孔硅光致发光峰峰位发生红移,且从570nm转移到740nm;电泳时间直接影响CdS纳米颗粒的填充量,导致相关的发光峰强度及发光峰位明显不同.     

金刚石膜/多孔硅复合材料的性能表征

提出了一种新颖的多孔硅表面钝化技术,即采用微波等离子体辅助的化学气相沉积（MPCVD）方法在多孔硅上沉积金刚石薄膜。采用原子力显微镜（AFM）、扫描电子显微镜（SEM）、X射线衍射仪（XRD）、拉曼光 谱仪和荧光分光度计对多孔硅及金刚石膜的表面形貌、结构和发光特性进行了表征。结果表明采用微波等离子体化学气相沉积法可在多孔硅基片上形成均匀、致密、性能稳定且对可见光具有全透性的金刚石膜。金刚石膜与多孔硅的复合,大大稳定了多孔硅的发光波长和强度,同时增强了多孔硅的机械强度。     

纳米压印多孔硅模板的研究

纳米压印模板通常采用极紫外光刻、聚焦离子束光刻和电子束光刻等传统光刻技术制备,成本较高.寻找一种简单、低成本的纳米压印模板制备方法以提升纳米压印光刻技术的应用成为研究的重点与难点.本文以多孔氧化铝为母模板,采用纳米压印光刻技术对纳米多孔硅模板的制备进行了研究.在硅基表面成功制备出纳米多孔阵列结构,孔间距为350—560 nm,孔径在170—480 nm,孔深为200 nm.在激发波长为514 nm时,拉曼光谱的测试结果表明,相对于单面抛光的硅片,纳米多孔结构的硅模板拉曼光强有了约12倍左右的提升,对提升硅基光电器件的应用具有重要的意义.最后,利用多孔硅模板作为纳米压印母模板,通过热压印技术,成功制备出了聚合物纳米柱软模板.     

超长氧化锌纳米线的制备及其气敏性能和紫外传感应用研究

采用一种无需催化剂和载气的简便碳热还原法制得长度约为100 μm、直径约为500 nm、长径比达到200的超长ZnO纳米线,讨论了Si基底位置、沉积时间以及反应物原料的量对ZnO纳米线形貌的影响。对ZnO纳米线的气敏性能进行研究,结果表明：在工作温度为350 ℃时,ZnO纳米线传感器能够很好地检测酒精气体,具有选择性好、响应恢复快的优点,且最低检测体积分数为5×10^-6。另外,通过一种简单、实用的介电泳法制得基于ZnO纳米线的紫外传感器。在365 nm紫外灯照射下,光电流增加了13%;而在254 nm紫外灯照射时,光电流则没发生变化,说明该传感器对不同波长的紫外光有一定的选择性。     

多孔硅尺寸的理论研究

研究了球形纳米硅的振动特性及Raman谱，建立了Raman移动与尺寸的对应关系．用球形纳米硅来模拟多孔硅，发现多孔硅的尺寸比通常认为的尺度要小得多 关键词：     

外电场极化对纳米氧化锌拉曼活性及气敏性能的影响

采用沉淀法制备了纳米氧化锌粒子,着重对其进行了不同条件(电场强度、极化温度)下的外电场极化处理.以X射线衍射仪和拉曼光谱仪对产物的结构、拉曼位移等进行了表征.测试了氧化锌极化产物在乙醇、丙酮气体中的气敏性能,研究了外电场效应对纳米氧化锌拉曼光谱和气敏性能的影响机制.结果表明,纳米氧化锌样品在外电场中存在着极化电场强度和温度的阈值,当电场强度和温度分别大于9375 V·cm~(-1)和150℃时,纳米氧化锌试片出现明显的漏电现象,极化效应显著降低并消失.在电场强度和温度阈值范围内,外电场极化作用能够导致氧化锌437 cm~(-1)处的拉曼特征峰强度明显降低.随外电场强度和极化温度增加,纳米氧化锌元件在丙酮气体中的灵敏度逐渐升高,在乙醇气体中的灵敏度逐渐降低,即外电场极化可以有效调控纳米氧化锌的气敏选择性.     

Raman of indigo on a silver surface. Raman and theoretical characterization of indigo deposited on silicon dioxide-coated and uncoated silver nanoparticles

Raman, surface-enhanced Raman scattering, and shell isolated nanoparticles-enhanced Raman scattering techniques were used to study the indigo–nanoparticle interaction nature. Silver nanoparticles were employed with and without a silicon dioxide spacer inert layer. The SERS spectral profile, obtained using silver nanoparticles, is different from the Raman one, which led to the proposition that the indigo–silver interaction is in the range of intermolecular interactions. SERS spectral reproducibility suggests identical organization and orientation of the analyte on the metal surface. The shell isolated nanoparticles enhanced Raman scattering spectrum of indigo, obtained by using silicon dioxide coated silver nanoparticles resulted similar to its Raman spectrum. This result indicates that the indigo structure is chemically unmodified by the silicon dioxide-coated silver surface. From the shell-isolated nanoparticles-enhanced Raman scattering experiments, the electromagnetic mechanism is proposed as the reason for the spectral enhancement. Theoretical calculations allow one to infer both the indigo–silver surface interaction nature and the orientation of indigo on the surface.     

Study on structural properties of epitaxial silicon films on annealed double layer porous silicon

In this paper, epitaxial silicon films were grown on annealed double layer porous silicon by LPCVD. The evolvement of the double layer porous silicon before and after thermal annealing was investigated by scanning electron microscope. X-ray diffraction and Raman spectroscopy were used to investigate the structural properties of the epitaxial silicon thin films grown at different temperature and different pressure. The results show that the surface of the low-porosity layer becomes smooth and there are just few silicon-bridges connecting the porous layer and the substrate wafer. The qualities of the epitaxial silicon thin films become better along with increasing deposition temperature. All of the Raman peaks of silicon films with different deposition pressure are situated at 521 cm⁻¹ under the deposition temperature of 1100 °C, and the Raman intensity of the silicon film deposited at 100 Pa is much closer to that of the monocrystalline silicon wafer. The epitaxial silicon films are all (4 0 0)-oriented and (4 0 0) peak of silicon film deposited at 100 Pa is more symmetric.     

Poly(vinylpyrrolidone)‐stabilized silver nanoparticles for strained‐silicon surface enhanced Raman spectroscopy

Poly(vinylpyrrolidone)‐stabilized silver nanoparticles deposited onto strained‐silicon layers grown on graded Si_1−xGe_x virtual substrates are utilized for selective amplification of the Si–Si vibration mode of strained silicon via surface‐enhanced Raman scattering spectroscopy. This solution‐based technique allows rapid, highly sensitive and accurate characterization of strained silicon whose Raman signal would usually be overshadowed by the underlying bulk SiGe Raman spectra. The analysis was performed on strained silicon samples of thickness 9, 17.5 and 42 nm using a 488 nm Ar⁺ micro‐Raman excitation source. The quantitative determination of strained‐silicon enhancement factors was also made. Copyright © 2011 John Wiley & Sons, Ltd.     

硅纳米线尖端阵列的制备及其场发射性能研究

将银镜反应与金属催化化学刻蚀相结合,在室温附近成功地制备出了硅纳米线尖端阵列,其长度为4~7μm,中间部分的直径在100~300nm之间。该方法操作简单、高效、无毒、可控以及低成本,且不需要高温、复杂的设备,对环境也没有特殊要求。性能测试结果显示:该硅纳米材料能够有效实现电子发射,开启电场约为2.7V/μm(电流密度10μA/cm2处);硅纳米尖端阵列的场增强因子约为692,可应用在场发射器件之上。     

硅纳米线尖端阵列的制备及其场发射性能研究

将银镜反应与金属催化化学刻蚀相结合,在室温附近成功地制备出了硅纳米线尖端阵列,其长度为4~7 m,中间部分的直径在100~300 nm之间。该方法操作简单、高效、无毒、可控以及低成本,且不需要高温、复杂的设备,对环境也没有特殊要求。性能测试结果显示：该硅纳米材料能够有效实现电子发射,开启电场约为2.7 V/m（电流密度10 A/cm2处）;硅纳米尖端阵列的场增强因子约为692,可应用在场发射器件之上。     

Effect of silver addition on the formation and deposition of titania nanoparticles produced by liquid flame spray

In this study, liquid flame spray (LFS) was used to produce titania, silver and silver–titania deposits of nanoparticles. Titanium(IV)ethoxide (TEOT) and silver nitrate in ethanol solutions were used as precursors and sprayed into turbulent hydrogen–oxygen flame. Production rates of 1.5–40 mg/min of titania were used with silver additions of 1, 2, 4, and 8 wt% compared to titania. Nanoparticle deposits were collected by thermophoretic sampling at six different axial distances from the flame torch head: 3, 5, 10, 12, 15, and 20 cm, of which the all but the last one occurred inside the flame. The deposit samples were analysed by TEM and SAED analysis. The powder samples of the particles were also collected by electric precipitator to XPS and specific surface area analysis. Particle size and effective density after the flame in the aerosol were analysed with SMPS and ELPI. The results from the previous studies i.e. controlling the particle size by setting the production rates of the particles were seen to apply also for this binary system. Characterisation of the deposits showed that when the substrate is inserted into the flame, in the beginning of the flame the deposit is formed by gas phase deposition whereas further down the flame the particles are first formed in the gas phase and then deposited. The location of the transition from gas phase deposition to gas phase nucleation prior to deposition depends on chemical/physical properties (e.g. thermodynamics and gas phase interactions) of the precursor, precursor concentration in the flame and also flame temperature profile. Therefore, the deposit collection distance from the burner also affected the collected particle size and degree of agglomeration. The two component deposits were produced in two different ways: one-step method mixing both precursors in the same solute, and two-step method spraying each precursor separately. The particle morphology differs between these two cases. In one-step method the primary (d _TEM) and agglomerate particle size (d _SMPS) decreased with the amount of silver addition, verifying the fact that when present, the silver has a clear effect on the titania nanoparticle formation and growth.     

The light-enhanced NO2 sensing properties of porous silicon gas sensors at room temperature

The NO2 gas sensing behavior of porous silicon（PS） is studied at room temperature with and without ultraviolet（UV） light radiation.The PS layer is fabricated by electrochemical etching in an HF-based solution on a p ＋-type silicon substrate.Then,Pt electrodes are deposited on the surface of the PS to obtain the PS gas sensor.The NO2 sensing properties of the PS with different porosities are investigated under UV light radiation at room temperature.The measurement results show that the PS gas sensor has a much higher response sensitivity and faster response-recovery characteristics than NO2 under the illumination.The sensitivity of the PS sample with the largest porosity to 1 ppm NO2 is 9.9 with UV light radiation,while it is 2.4 without UV light radiation.We find that the ability to absorb UV light is enhanced with the increase in porosity.The PS sample with the highest porosity has a larger change than the other samples.Therefore,the effect of UV radiation on the NO2 sensing properties of PS is closely related to the porosity.     

Enzyme-induced growth of silver nanoparticles studied on single particle level

Based on their interesting properties, metal nanoparticles show the potential as an analytical tool in electronic (Burmeister et al. 2004), optical (Yguerabide and Yguerabide 1998), and catalytic applications (Liu 2006). Their characteristics depend on the composition, shape, and size of the single particles. These various properties are utilized in many different approaches such as optics, magnetics (Lang et al. 2007), and laser technology (Csaki et al. 2007). We investigated an alternative method for the synthesis of nanoparticles. In this case, an enzyme, horseradish peroxidase, induces a silver deposition and replaces a metal nanoparticle as the reaction seed. Depending on the reaction time, we could obtain particles in a range of few nanometers up to more than 250 nm. For a better understanding of the enzymatic silver deposition process, the silver particles produced by this process were analyzed by SEM, TEM, and atomic force microscopy (AFM) on a single particle level after different enhancement times. The AFM images were utilized for the characterization of particle height and volume to study the enzyme kinetics, i.e., the particle growth process. Thereby, two different phases are described: a first growth phase probably induced by the enzyme-related growth, and a second, more unspecific growth based on the metal deposition onto the silver deposits. These findings may help to use the enzyme-induced silver deposition in a quantitative manner for bioanalytical applications.