垂直生长碳纳米管阵列可见光高吸收比标准研制及其特性表征分析

研究采用原子层沉积(ALD)工艺,利用垂直碳纳米管阵列(VACNTs)的稀疏结构和碳纳米管本身具有的中空结构,探索制备具有超黑性质的垂直生长碳纳米管阵列薄膜,研究测试材料在(500~1000)nm绝对吸收比,调节阵列结构,实现高吸收比标准片的研制。     

喷雾热解法在硅衬底上生长定向碳纳米管阵列(英文)

以向日葵油的甲基酯为碳源,二茂铁为催化剂前驱体,Ar为载气,通过喷雾热解法在硅衬底上合成定向碳纳米管阵列。结果表明,在硅衬底上原位形成Fe催化剂纳米颗粒。由拉曼光谱、透射电镜图和X-射线衍射谱图显示所制定向碳纳米管阵列具有较好的石墨化程度,其直径为1 0～3 0 nm,管壁约为1 0 nm。所制定向碳纳米管阵列中残留的催化剂含量可以忽略。     

原子层沉积技术在纳米光子波导中的应用

原子层沉积(ALD)是一种独特的薄膜沉积方法,能够实现完美的台阶复形和大面积均匀沉积,为薄膜成分和厚度提供原子级控制。本文将ALD的优点与纳米光子学联系起来,总结了ALD膜层在几种硅波导新结构中的性能优化作用,综述了近年来利用ALD制备纳米光子波导器件的一些研究成果。     

空间隔离原子层沉积系统的研究

原子层沉积(ALD)技术制备的薄膜在纳米尺度精确可控,并且各处薄膜厚度具有良好的均匀性。空间隔离原子层沉积(SALD)相比于时间隔离ALD技术,此工艺更易实现大面积基底沉积和连续沉积。由于SALD技术巨大的应用前景,关于SALD技术的研究成为ALD技术研究的热点之一。本文介绍了实验室自主设计搭建的SALD系统平台,以Al2O3生长评估SALD系统,实现Al2O3薄膜线性生长。并对反应温度、基底与前驱体喷头间距这两个重要的工艺参数进行了研究。SALD沉积实验表明,减小基底表面温度波动可以提高薄膜的微观形貌质量。同时,前驱体进气喷头与基底之间的距离会强烈影响基底表面的前驱体压力和前驱体间隔离效果,进而影响薄膜生长。为平衡薄膜生长均匀性和系统密封性的要求,需要选择最优的间距值。     

利用电沉积Ni纳米晶制备无缠绕阵列碳纳米管

以金属Cu基板上脉冲电沉积Ni纳米晶薄膜作为催化剂,在乙醇火焰中制备了直立、无缠绕阵列碳纳米管.利用原子力显微镜(AFM)、扫描电子显微镜(SEM)、透射电镜(TEM)和激光拉曼谱仪(Raman)对不同工艺制备的Ni纳米晶薄膜和阵列碳纳米管的形貌进行了表征.结果表明:通过综合控制脉冲电沉积参数、电沉积时间和火焰中的合成时间,可以获得大面积、密集、均匀、直立、无缠绕、形态良好、重复性高的阵列碳纳米管.脉冲电沉积Ni纳米晶和合成无缠绕阵列碳纳米管的最佳工艺条件是:脉冲电沉积正、负脉冲的工作频率为154Hz、占空比为38.5%、电沉积时间为1min、基板预热至600℃、火焰中停留1min.通过对生长机理的研究发现:当电沉积时间较短时,获得的Ni纳米晶薄膜较薄,具有较高的局域粗糙程度和催化活性,有利于碳纳米管的同时大面积"拥挤生长"形成阵列结构;另外,通过调整脉冲电沉积参数,可以控制Ni纳米晶的大小,从而控制碳纳米管的长径比,当长径比较小时即可获得无缠绕的阵列碳纳米管.     

Fe-Mo/Al_2O_3催化剂催化分解甲烷制备碳纳米管:温度对碳管结构的影响

利用化学气相沉积法,以Fe-Mo/Al_2O_3为催化剂,催化分解甲烷气体制备碳纳米管(CNTs).研究了温度,反应时间和气体流速对碳纳米管结构的影响.结果显示:温度是影响碳纳米管壁厚的关键参数.低温导致壁厚为2 nm～7 nm的多壁碳纳米管(MWCNTs)的生成.相对地,高温有利于双壁碳纳米管(DWCNTs)的生长,而更高的温度促使单壁碳纳米管(SWCNTs)的产生.进一步升高温度,得到了壁厚为3 nm～15 nm的MWCNTs和大的炭颗粒.     

预置镍化学气相沉积法制备定向碳纳米管(英文)

采用化学气相沉积法(CVD),在溅射了镍薄膜的硅基底上制备了定向碳纳米管薄膜。对镍薄膜的氨气预处理过程及其机理进行了研究。结果发现预处理后的岛状区域随着薄膜厚度的增加而增加,纳米粒子区域的变化则与之相反。对5nm的镍薄膜进行预处理能获得细化和均匀分布的纳米粒子,有利于定向碳纳米管的生长。碳纳米管的生长过程及其细微结构与温度有很大关系。碳源的分解、碳原子在催化剂内部的扩散以及催化剂粒子的团聚三者之间的竞争决定了碳纳米管的生长情况。本文分析了碳纳米管的顶部生长模式及该模式下催化剂粒子的形态变化。     

ZnO纳米棒阵列、纳米片及其发光和光催化特性

首先通过溶胶-凝胶法在Si片基底上制备1层ZnO纳米薄膜,作为纳米棒的晶种层,然后利用金属浴沉积法在ZnO纳米薄膜基础上制备择优取向的ZnO纳米棒阵列,最后通过水热法二次成核结晶形成纳米片。研究证明,ZnO纳米棒阵列和纳米片均沿着c轴取向。在Cu2+抑制极性面生长的作用下,形成的ZnO纳米片结构均匀,分布面积广,单片ZnO纳米片的厚度约为8 nm,面积呈平方微米级,较大的有40μm2左右。ZnO纳米结构的生长取向对其物理化学性能具有重要影响。高度沿c轴取向的ZnO纳米棒有利于紫外光发射和激光器的发展,但极性面的缩小不利于光催化反应。     

原子层沉积技术在新型太阳能电池中的应用

原子层沉积技术(ALD)是一项正处于发展之中、在许多领域具有巨大应用前景的新型材料制备技术,该技术在纳米结构和纳米复合结构的制备方面显示出独特的优势,在新型薄膜太阳能电池领域呈现出巨大的发展潜力和前景。首先概述了ALD技术的工作原理,简要介绍了近几年ALD技术在硅基太阳能电池和铜铟镓硒薄膜电池(CIGS)中的应用,然后重点综述了原子层沉积纳米功能薄膜在染料敏化太阳能电池(DSSCs)和有机-无机杂化钙钛矿太阳能电池(PSCs)为代表的新型薄膜太阳能电池中的应用。最后,总结了原子层沉积功能薄膜的特点和优势,展望了ALD在新能源材料与器件领域的应用前景和发展趋势。     

辅助气体对RF-PECVD制备碳纳米管薄膜形貌的影响

采用射频等离子体增强化学气相沉积(RF-PECVD)技术,以Ni为催化剂,经600℃裂解C2H2在Si基底上制备出定向碳纳米管薄膜。采用扫描电子显微镜(SEM)表征了刻蚀后Ni颗粒与沉积的碳纳米管薄膜的形貌。研究了辅助气体对等离子体预处理催化剂与碳纳米管生长的影响。结果表明:辅助气体(H2与N2)流量比对催化剂颗粒尺寸、分布以及碳纳米管生长有显著影响;合适的气体流量比有利于减少碳纳米管薄膜的杂质颗粒,促进其定向生长。预处理过程中气体流量比H2:N2=20:5时,预处理后催化剂Ni颗粒分布密度大、粒径小且分布范围窄,适合碳纳米管均匀着床;沉积生长碳纳米管薄膜时,H2:N2=20:15可得到纯度高、定向性好的碳纳米管。     

Influence of thickness and growth temperature on the properties of zirconium oxide films grown by atomic layer deposition on silicon

ZrO₂ films of thicknesses varied in the range of 3–30 nm were atomic layer deposited from ZrI₄ and H₂O–H₂O₂ on p-Si(100) substrates. The effects of film thickness and deposition temperature on the structure and dielectric properties of ZrO₂ were investigated. At 272 and 325 °C, the growth of ZrO₂ started with the formation of the cubic polymorph and continued with the formation of the tetragonal polymorph. The ratio between the lattice parameters increased with the film thickness and growth temperature. The effective permittivity, determined from the accumulation capacitance of Hg/ZrO₂/Si capacitors, increased with the film thickness, reaching 15–17 in 25-nm-thick films. The permittivity decreased with the increasing growth temperature. The hysteresis of the capacitance–voltage curves was the narrowest for the films deposited at 325 °C, and increased towards both lower and higher deposition temperatures.     

Formation of a highly oriented FeO thin film by phase transition of Fe3O4 and Fe nanocrystallines

A highly oriented FeO thin film was formed from a Fe₃O₄ thin film containing Fe nanocrystallines by post-annealing at 600°C. Fe₃O₄ thin films were grown on Si(100) substrates by ion beam sputter deposition under oxygen ambient. The stoichiometry of the iron oxide thin film could be precisely controlled by in situ X-ray photoelectron spectroscopy (XPS). X-ray diffraction (XRD) pattern of the Fe₃O₄ thin film grown at substrate temperature of 300°C showed a mixed phase of Fe₃O₄ and Fe nanocrystallines with a preferred orientation (110). However, the mixed phase was converted to a highly oriented FeO(200) phase by post-annealing at 600°C. This could be inverted as a result of Ostwald ripening of the Fe₃O₄ and Fe nanocrystallines.     

Magnetic properties and texture of sputteredFe/Fe3O4 multilayer films

Polycrystalline Fe/Fe₃O₄ multilayers have been fabricated with varying Fe/Fe₃O₄ ratios, period (bilayer) thickness, number of periods, and deposition sequence. The films were deposited by RF magnetron sputtering. The coercivity was found to vary in a nonlinear fashion between that of Fe and Fe₃ O₄. For selected multilayer geometries, the coercivity can be increased beyond that of single-layer Fe and Fe₃O₄ films. The magnetic saturation was observed to follow a linear mixture rule. These results suggest that a multilayer approach is useful for designing magnetic thin films and may allow fabrication of new materials for recording media applications. A secondary result was the ability to obtain highly textured polycrystalline films of both Fe and Fe₃O₄ on amorphous substrates for selected multilayer geometries. The texture results, which may be generally applicable, suggest that relatively thin multilayers of only a few periods may provide a means to control polycrystalline film texture on amorphous substrates     

Deposition of BaTiO3 thin films by plasma MOCVD

Barium titanium trioxide (BaTiO₃) thin films were deposited on fused silica or silicon wafer substrate from barium dipivaloylmethanate (II) (Ba(dpm)₂) and titanium tetraisopropoxide (IV) (TTIP) used as precursors in an oxygen microwave plasma. The substrates were dielectrically heated and the substrate temperatures were around 900 K during the film deposition. The deposition was performed for 15 min and the deposits were identified as BaTiO₃ by means of X-ray diffraction, X-ray photoelectron spectroscopy, infrared spectroscopy, and ellipsometry. Oxygen and barium atoms and TiO and CO molecules were identified in the plasma. These species would produce higher deposition rates at lower substrate temperatures than those did in the usual thermal metalorganic chemical vapor deposition (MOCVD). The dielectric constant of the BaTiO₃ thin film that was directly deposited on the silicon wafer substrate was as low as 10¹ order of magnitude. Because the deposit reacted with the substrate and an interdiffusional layer was formed, the platinum layer was coated on the silicon wafer substrate in order to prevent the formation of an interdiffusional layer. The dielectric constant then increased to 10³ order of magnitude.     

TaN薄膜的等离子体增强原子层沉积及其抗Cu扩散性能

使用Ta[N(CH₃)₂]₅和NH₃等离子体作为反物用等离子体增强原子层沉积工艺生长了TaN薄膜,借助原子力显微镜、X射线光电子能谱、四探针和X射线反射等手段研究了薄膜的性能与工艺条件之间的关系。结果表明,TaN薄膜主要由Ta、N和少量的C、O组成。当衬底温度由250℃提高到325℃时Ta与N的原子比由46:41升高到55:35,C的原子分数由6%降低到2%。同时,薄膜的密度由10.9 g/cm³提高到11.6 g/cm³,电阻率由0.18 Ω?cm降低到0.044 Ω?cm。与未退火的薄膜相比,在400℃退火30 min后TaN薄膜的密度平均提高了~0.28 g/cm³,电阻率降低到0.12~0.029 Ω?cm。在250℃生长的3 nm超薄TaN阻挡层在500℃退火30 min后仍保持良好的抗Cu扩散性能。     

纳米金刚石负载Fe2O3的制备及其对高氯酸氨的热分解催化作用

对纳米金刚石（ND）进行羧基化处理以提高其分散性,然后采用沉淀法制备了羧基化ND负载Fe₂O₃的催化剂。利用XRD、TG、BET和TEM对该负载型催化剂进行表征,通过DSC研究其对高氯酸铵(AP)热分解的催化作用。结果表明:ND经过羧基化处理后,在水中的分散性大幅度提高。沉淀法制备了直径5 nm、长50 nm的Fe₂O₃包裹或附着于ND的负载型复合催化剂,该催化剂对AP高温热分解的催化效果优于单一的Fe₂O₃或ND。当Fe₂O₃和ND的质量比为5∶1、在AP中添加质量分数2%的复合催化剂时,AP的高温分解峰温降低约30 ℃,ND负载Fe₂O₃催化剂具有一定的协同催化作用。     

具有固-液转变的磁性Fe3O4纳米流体的制备、结构及性能

Fe3O4纳米粒子与离子型改性剂N,N-二癸基-N-甲基-N-三甲氧基硅正丙基氯化铵进行接枝反应,再采用反离子脂肪醇聚氧乙烯醚磺酸盐的长链阴离子交换Cl-,在Fe3O4纳米粒子表面得到具有阴、阳离子双电层结构的表面处理层,制备出了无溶剂Fe3O4纳米流体。分析结果表明,表面处理鏖已成功地接枝在Fe3O4纳米粒子表面,改...     

Fe2O3对原位制备SiCw/SiC太阳能储热陶瓷的结构与性能的影响

为调控SiC_w/SiC复相陶瓷中原位生长SiC晶须的生长发育和形貌, 以提高SiC复相储热陶瓷的性能, 在CF0配方(SiC 69.31wt%, AlN 20.30wt%, Si 10.39wt%)的基础上添加0.5wt%~2.0wt% Fe₂O₃作为催化剂。研究了Fe₂O₃对晶须形貌、生长机制及SiC复相陶瓷结构与性能的影响。研究结果表明, 引入Fe₂O₃后晶须生长机制由气-固机理转变为气-液-固机理。Fe₂O₃添加量通过调节C元素在Fe-Si熔球中的溶解度, 与烧成温度共同调控晶须形貌。经1500 ℃烧成的CF4(2.0wt% Fe₂O₃)样品性能最佳, 晶须直径50~100 nm, 长度1~6 μm, 其体积密度、抗折强度、比热容分别为2.19 g/cm ³、45.08 MPa、0.95 J/(g·K) (25 ℃), 热导率达18.15 W/(m·K) (25 ℃), 相比于未添加Fe₂O₃的样品增加了169%。气-液-固机理生长的SiC晶须缺陷少、直径大, 可有效降低晶须-基体传输势垒, 具有更好的热学性能。     

低温反应溅射Al+α-Al2O3复合靶沉积α-Al2O3薄膜

低温沉积α-Al₂O₃薄膜是拓展其实际工程应用的关键。本研究以Al、α-Al₂O₃和Al + 15wt% α-Al₂O₃为靶材, 用射频磁控溅射在Si(100)基体上沉积氧化铝薄膜。用掠入射X射线衍射(GIXRD)、透射电子显微镜(TEM)、能谱仪(EDS)对所沉积薄膜的相结构和元素含量进行研究, 用纳米压痕技术测量薄膜硬度。结果表明, 在550 ℃的基体温度下, 反应射频磁控溅射Al+α-Al₂O₃靶可获得单相α-Al₂O₃薄膜。靶中的α-Al₂O₃溅射至基片表面能优先形成α-Al₂O₃晶核, 在550 ℃及以上的基体温度下可抑制γ相形核, 促进α-Al₂O₃晶核同质外延生长, 并最终形成单相α-Al₂O₃薄膜。     

Growth of calcium carbonate by the atomic layer chemical vapour deposition technique

Thin films of CaCO₃ (calcite) have been grown with the atomic layer chemical vapour deposition (ALCVD) technique, using Ca(thd)₂ (Hthd=2,2,6,6-tetramethylheptan-3,5-dione), CO₂, and ozone as precursors. Pulse parameters for the ALCVD-type growth are found and self-limiting reaction conditions are established between 200 and 400 °C. Calcium carbonate films have been deposited on soda-lime glass, Si(100), -Al₂O₃(001), -Al₂O₃(012), -SiO₂(001), and MgO(100) substrates. The observed textures were: in-plane oriented films with [100](001)CaCO₃ [100](001)Al₂O₃ and [100](001)CaCO₃[110](001)Al₂O₃ on -Al₂O₃(001), amorphous films on -Al₂O₃(012) when grown at 250 °C, and columnar oriented films on soda-lime glass, Si(001), -SiO₂(001), and MgO(100) substrates with (00l) and (104) parallel to the substrate plane at 250 and 350 °C, respectively. The film topography was studied by atomic force microscopy and AC impedance characteristics were measured on as-deposited films at room temperature. The films were found to be insulating with a dielectric constant (_r) typically approximately 8. Thin films of CaO were obtained by heat treatment of the carbonate films at 670 °C in a CO₂-free atmosphere, but the thermal decomposition led to a significant increase in surface roughness.