Ti6Al4V表面纳米多孔氧化膜的电解制备及形成机理研究

在(NH4)2SO4/NH4F电解液中,采用阶段升压至预定电压,然后恒压阳极氧化在Ti6Al4V表面制备出纳米多孔氧化膜。利用SEM、XRD对纳米多孔氧化膜进行表征。研究表明,电解液pH值和外加电压对纳米多孔氧化膜形成和形貌影响非常大。电解液的pH值=4.0,恒压为20V时,形成孔均匀规整的纳米多孔氧化膜,孔内径约为85nm。纳米多孔氧化膜形成机理是:首先钛合金表面钝化,在F-作用下钝化表面发生孔蚀而形成原始胚胎孔,然后胚胎孔处氧化膜在电场支持下发生场致溶解而成大孔。     

Ti6A14V表面纳米多孔氧化膜的电解制备及形成机理研究

在(NH4)2SO4/NH4F电解液中,采用阶段升压至预定电压,然后恒压阳极氧化在Ti6A14V表面制备出纳米多孔氧化膜.利用SEM、XRD对纳米多孔氧化膜进行表征.研究表明,电解液pH值和外加电压对纳米多孔氧化膜形成和形貌影响非常大.电解液的pH值=4.O,恒压为20V时,形成孔均匀规整的纳米多孔氧化膜,孔内径约为85nm.纳米多孔氧化膜形成机理是:首先钛合金表面钝化,在F-作用下钝化表面发生孔蚀而形成原始胚胎孔,然后胚胎孔处氧化膜在电场支持下发生场致溶解而成大孔.     

电化学阳极氧化条件对多孔硅及其光催化性能的影响研究

在HF/乙醇电解液中,采用恒电压电化学阳极氧化法,将P型硅片制备成了多孔硅催化剂。以甲基橙模拟废水为目标物,分析了电化学阳极氧化条件对多孔硅光催化甲基橙脱色率的影响。结果表明:随着HF浓度、阳极氧化时间、电流密度和光照时间的增加,甲基橙的脱色率逐渐增大。当V(HF)∶V(乙醇)=1∶1、阳极氧化时间为30min、电流密度为10mA/cm2以及光照时间为60min时,对甲基橙废水的脱色率较好。用十二烷基苯磺酸钠修饰的多孔硅对甲基橙废水有更高的脱色率。同直接催化相比,光催化甲基橙废水的脱色率提高到45.32%。同时对多孔硅表面形貌进行了表征。     

近规整多孔硅电化学制备与表征

电化学阳极氧化条件对多孔硅孔排列的规整度有着显著的影响.提出了一种不需阳极氧化铝模板或预图案化而直接制备近规整多孔硅的电化学方法,分析了氧化时间、电解液组成、HF浓度对多孔硅形态的影响.结果表明,随着阳极氧化时间的增加,多孔硅孔的深度逐渐加大,孔径则呈先增大后稳定的趋势.当氢氟酸(40%)与N-N-二甲基甲酰胺(DMF...     

热氧化多孔硅制备及其干涉特性研究

采用电化学阳极氧化法制备彩色薄层多孔硅,经高温热氧化处理后形成稳定的热氧化多孔硅.研究电化学制备条件对热氧化多孔硅的干涉效应和光学厚度的影响,分析热氧化处理前后多孔硅的稳定性.结果表明,在可见光波长范围内,所制备的热氧化多孔硅反射光谱出现一定规律性的干涉条纹,表现出明显的反射干涉现象;随阳极氧化时间、电流密度和HF浓度增大,热氧化多孔硅光学厚度呈增大趋势,当阳极氧化时间为30s、电流密度为520mA/cm2、v(HF):v(C2H5OH)为2:1～5:2时,制备的热氧化多孔硅干涉条纹均匀且光学厚度较大;热氧化处理后,多孔硅结构中的Si-Hx键被Si-O键所取代,其反射干涉特性非常稳定.     

电化学阳极氧化条件对阵列多孔硅的影响

采用电化学阳极氧化法,将预光刻图案的p型硅片制备成阵列多孔硅.讨论电化学阳极氧化条件对阵列多孔硅形貌的影响.结果表明:随着HF浓度、电流密度、阳极氧化时间的增大,阵列多孔硅的孔深逐渐加大;当HF:C2H5OH:H2O(体积比)为1:1:1～1:2:5,电流密度为1.56mA/cm2,阳极氧化时间为3h时,制备出的阵列多孔硅具有比较规整的阵列孔,并且孔深能够达到50pm;表面活性剂对阵列孔的形成有很大影响,加入表面活性剂后形成的孔才具有一定的规整性以及深宽比.     

纳米多孔铝阳极氧化膜的形成机理研究

为探讨多孔铝阳极氧化膜的形成机理,研究了不同气压条件下铝在磷酸溶液中的阳极氧化过程,发现在真空下进行阳极氧化,氧气析出非常明显。通过测定不同气压下的阳极氧化曲线,分析了致密膜向多孔氧化铝膜的转化和生长过程,结果显示氧气析出是导致氧化膜从致密膜向多孔膜转变的主要原因。提出了在氧化膜/电解液界面上氧气分子的聚集是造成表面条纹的新观点。通过氧化膜断面的SEM形貌表征,首次发现多孔膜的主孔道中存在分孔道。分孔道的产生说明析氧反应不但在致密膜/电解液界面发生,而且在多孔膜孔壁/电解液界面也同时发生。     

混合酸(HNO3+HF)刻蚀法致霾汽车尾气过滤载体材料的设计与研究

以纺织加工过程中废弃的棉短绒为模板,经过溶胶法浸渍形成棉纤维/氧化硅复合体,再经常温树脂固化、低温真空碳化、高温碳热还原反应及液相渗硅等方式制备出SiC/Si复合材料,最后通过混合酸(HNO3+HF)循环氧化腐蚀制备出过滤汽车尾气陶瓷载体材料。扫描电镜(SEM)结果显示,多孔SiC具有不规则且相互连通的孔道结构,其微观形貌特征遗传于棉短绒和酚醛树脂制备的多孔碳;三点弯曲试验表明SiC/Si陶瓷复合材料的强度高达200MPa,多孔SiC的气孔率可达62%,混合酸腐蚀的多孔SiC的弯曲强度和断裂韧性均小于致密SiC/Si复合体,并提出了混合酸循环氧化-腐蚀机制解释游离态Si的腐蚀过程。     

多孔硅层结构和氧含量分布对电子发射特性的影响

为了研究较厚的多孔硅层结构及氧化分布对电子发射特性的影响,采用恒流和脉冲腐蚀制备了单层和多层结构的多孔硅,并对这两种结构的多孔硅分别进行定场强和变场强电化学氧化。根据扫描电子显微镜和X射线能谱仪对多孔硅结构和氧含量分布的测量结果,以及对电子发射特性和所提出的多孔硅电子源模型的比较和分析,结果发现:孔隙率交替变化的多层多孔硅结构可以优化电场分布,变场强的电化学氧化使氧含量分布均匀,电子在发射时可以得到持续加速和收敛。单层结构的多孔硅经过定场强电化学氧化后,氧含量分布上层高而下层低,电子不能得到持续加速且具有散射的特点。变场强氧化的多层多孔硅电子发射特性优于定场强氧化的单层多孔硅电子源。     

激光功率对多孔硅微Raman谱的影响

运用微Raman谱仪以不同功率的激光入射到用阳极脉冲腐蚀制备的多孔硅样品以研究多孔硅的稳定性.用斯托克斯与反斯托克斯散射强度的比率确定样品的温度.观察比较不同温度下多孔硅样品的Raman谱趋向,发现在激光功率和样品温度之间的关系曲线上有3个过程,与Raman频移和Raman强度的曲线相一致.所有现象都可以用Si-O键和非晶Si被氧化的机制进行解释.     

A first step in prediction of the nanoscale structure of porous silicon from processing parameters

The present work addresses the formation of porous silicon layers by means of anodic dissolution of p- and p(+)-type boron-doped (100) silicon wafers in 15, 25, and 35 vol% HF-ethanol solutions. The study concerned the dependence of the porous silicon layer growth rate dh/dt on electric current density i as well as on HF concentration. The formation of a porous silicon layer was found to follow a generic linear relationship, in(dh/dt)--in(i), which holds irrespective of the processing conditions. The combination of two equations, experimental and theoretical, derived from Faraday's equation, allowed us to reach conclusions on the relationship between the growth rate dh/dt and the degree of porosity, constituting a first step in prediction of the nanoporous structure of silicon based on processing parameters. This electrochemical approach complements physical models of silicon pore formation.     

Nanosecond field-induced quenching of the luminescence from Er-doped silicon nanocrystals

Er-doped Si-rich SiO2 gate oxide layers containing silicon nanocrystals are prepared by implantation of Si+ and Er+ into SiO2 thin films. The photoluminescence from both Si nanocrystals around 700-850 nm and Er3+ ions at 1.54 microm is strongly quenched by applying electric field in the Si-rich oxide layer. The quenching time and the recovery time of the photoluminescence from Si nanocrystals are less than 50 ns under pulsed field modulation. The quenching rate of the luminescence increases with increasing the density and reducing the size of the silicon nanocrystals. Our results indicate that the fast quenching process originates from the quantum confined Stark effect and enhanced exciton ionization by carrier tunneling between the silicon nanocrystals under the high electric field.     

电催化金属辅助化学刻蚀法制备硅纳米线/多孔硅复合结构

量子限制效应使硅纳米线具有良好的场致发射特性,结合多孔硅的准弹道电子漂移模型可提高场发射器件的性能。传统的金属辅助化学刻蚀法制备硅纳米线的效率较低,本研究在传统方法的基础上引入恒流源,提出电催化金属辅助化学刻蚀法,高效制备了硅纳米线/多孔硅复合结构。在外加30mA恒定电流的条件下,硅纳米线的平均制备速率可达308nm/min,较传统方法提升了173%。研究了AgNO₃浓度、刻蚀时间和刻蚀电流对复合结构形貌的影响规律;测试了采用电催化金属辅助化学刻蚀法制备样品的场发射特性。结果显示样品的阈值场强为10.83 V/μm,当场强为14.16 V/μm时,电流密度为64μA/cm²。     

Room-temperature formation of low refractive index silicon oxide films using atmospheric-pressure plasma

This study aims to apply atmospheric-pressure (AP) plasma to the fabrication of single-layer anti-reflection (AR) coatings with porous silicon oxide. 150 MHz very high-frequency (VHF) excitation of AP plasma permits to enhance the chemical reactions both in the gas phase and on the film-growing surface, increasing deposition rate significantly. Silicon oxide films were prepared from silane (SiH4) and carbon dioxide (CO2) dual sources diluted with helium. The microstructure and refractive index of the films were studied using infrared absorption and ellipsometry as a function of VHF power density. It was shown that significant increase in deposition rate at room temperature prevented the formation of a dense SiO2 network, decreasing refractive index of the resulting film effectively. As a result, a porous silicon oxide film, which had the lowest refractive index of 1.24 at 632.8 nm, was obtained with a very high deposition rate of 235 nm/s. The reflectance and transmittance spectra showed that the low refractive index film functioned as a quarter-wave AR coating of a glass plate.     

Mechanisms of formation and topological analysis of porous silicon — computational modeling

Porous silicon formation under anodization in HF solution is studied by means of computer simulation, using the model, which takes into account the Si dissolution, thermal generation, diffusion and drift of holes and quantum confinement. Structures of porous layer, obtained in computational experiments at various doping level of initial Si, temperatures, HF concentrations, anode current densities, are shown and analyzed. The porosity and fractal dimension of the obtained porous structures are also analyzed.     

Macroscopic Studies on the Properties of the Anodic Oxide Films on Titanium

The effect of fluoride ions on the formation and dissolution behaviour of anodic oxide films on Ti has been investigated in acidic fluoride media (pH=1) using impedance and galvanostatic techniques. A5 the fluoride ion concentration and temperature increase the rate of oxide film formation decreases while the dissolution process increases. oxide film formed at high tem-perature and formation voltage was found to contain more defect sites in the film than that formed at a lower one. Activation energies are calculated during the oxide film formation and dissolution and found to be 20.76 and 28.72 kJ/mol, respectively. Formation rate and reciprocal capacitance data are reported as a function of polarizing current density. Values are recorded for the electrolytic parameters A and B. Potentiostatic curves are derived from the galvanostatic results.     

Morphology of porous silicon structures formed by anodization of heavily and lightly doped silicon

By computer simulation the growing process of porous silicon under p⁻-Si and p⁺-Si anodization in HF solution is studied. The model of electrochemical etching of p⁺-Si includes the relief selective mechanism, which allows one to establish the relationship between anodization conditions (current density, HF concentration, temperature and doping level) and the topological characteristics of porous silicon (PS). The simulation of p⁻-Si dissolution is based on the model of diffusion limited aggregation (DLA), taking into account the thermal generation of holes and the quantum confinement effect. The various morphology of simulated PS structures exhibits a close resemblance to that of experimental ones formed in p⁺-Si and p⁻-Si wafers. For simulated p⁻-Si-based PS layers the porosity profiles and fractal dimension are calculated. It is shown that PS in p⁻-Si is multifractal with fractal dimension varying monotonously from 0.1 to 3 with size increase.     

Anodic oxide growth on aluminium surfaces modified by cathodic deposition of Ni and Co

Surface conditions similar to those found in aluminium alloys of practical use were assessed by cathodic deposition of transitions metals (Ni and Co) from different electrolytes. Fundamental aspects concerning with the growth of anodic oxide films at potentials lower than 10 V in neutral acetate buffer solution on these modified surfaces were analysed by common electrochemical techniques complemented with scanning electron microscopy and transmission electron microscopy. In both potentiodynamic and galvanostatic modes, the growth of aluminium oxide competes with the dissolution of deposited metal particles. The formation of a thin aluminium barrier oxide film beneath them shifts the dissolution potential over to 1.5 V towards more positive values. Some particles get progressively embedded in the matrix of the growing alumina and act as cation sources, increasing the film conductivity and diminishing the established electric field in the oxide. This effect is more pronounced with Co deposits due to its high active dissolution rate, before passivation occurs. Then, the generation of a two-layer film is explained in terms of the precipitation of metal hydroxide at the solution side on the oxide barrier film.     

Argon-oxygen ion-plasma treatment modifies the surface composition and photoluminescence spectrum of porous silicon

We have studied changes in the surface composition and photoluminescence spectrum of porous silicon (por-Si) during the ion-plasma etching of samples in an argon-oxygen gas mixture. This treatment leads to the passivation of the surface of quantum filaments by residual fluorine and the formation of silicon oxide. The source of fluorine atoms are HF molecules retained in the volume of pores upon the por-Si structure formation by chemical etching. Increase in the fluorine concentration is accompanied by the growth in intensity of the blue-green band and broadening of the red band in the photoluminescence spectrum of por-Si.     

聚硅氧烷转化制备硅氧碳多孔陶瓷的研究进展

硅氧碳多孔陶瓷耐高温,密度低,比强度高,比表面积大,热导率低,介电性能优良,应用前景广阔。聚合物前驱体转化法已成为颇具前景的陶瓷材料制取手段。文章在简要介绍聚硅氧烷的基础上,从聚硅氧烷热解前、热解过程中以及热解后不同阶段形成特定的孔结构出发,重点阐述了通过聚硅氧烷热解制备硅氧碳多孔陶瓷的工艺研究现状,并提出了亟待解决的问题。