薄膜光学 制膜技术与装置

O484.12006054416LPCVD法制备碳纳米管薄膜及其场发射性能的研究=Deposition of carbon nanotubes fil mby LPCVDand relatedfield emission property[刊,中]/陈婷(华东师范大学纳米功能材料和器件应用研究中心.上海(200062)),孙卓…//光学学报.—2006,26(5).—777-782采用低压化学汽相沉积法(LPCVD)在镍片上直接制备碳纳米管(CNTs)薄膜,系统地研究了生长温度(500~800℃)对碳纳米管薄膜形貌、结构及场发射性能的影响,并对此方法的生长机理进行了分析。当温度从500℃升高到650℃时,碳纳米管的生长速率随着温度升高而增大,而温度继续…     

快速退火对PLD法制备SnS薄膜结构和光学性质的影响

利用脉冲激光沉积(PLD)法在玻璃基片上室温生长SnS薄膜,并在Ar气保护下分别在200,300,400,500,600℃对薄膜进行快速退火处理。利用X射线衍射(XRD)、拉曼光谱仪(Raman)、原子力显微镜(AFM)、场发射扫描电子显微镜( FE-SEM)、紫外-可见-近红外分光光度计( UV-Vis-NIR)、Keithley 4200-SCS半导体参数分析仪研究了快速退火温度对SnS薄膜的晶体结构、表面形貌以及有关光学性质和电学性能的影响。所制备的SnS薄膜样品沿(111)晶面择优取向生长,退火温度为400℃时的薄膜结晶质量最好。薄膜均具有SnS特征拉曼峰。随着退火温度的升高,薄膜厚度逐渐减小,而平均颗粒尺寸逐渐增大。不同退火温度下的SnS薄膜在可见光范围内的吸收系数均为105 cm-1量级,400℃时退火薄膜的直接带隙为1.92 eV。随着退火温度从300℃升高到500℃,电阻率由1.85×104Ω·cm下降到14.97Ω·cm。     

高择优取向Mo薄膜的直流磁控溅射制备及其电学性能

使用直流磁控溅射法在玻璃基底上沉积Mo薄膜,采用X射线衍射仪、原子力显微镜和四探针测试系统研究了溅射工艺对Mo薄膜的结构、形貌和电学性能的影响.结果表明:当基片温度为150 ℃时,薄膜获得(211)晶面择优取向生长,而在低于250 ℃的其它温度条件下,样品则表现为(110)晶面择优取向生长.进一步的表面形貌分析显示:薄膜的粗糙度随基片温度变化不明显,其值大约为0.35 nm,随溅射功率密度的增大而变大|电学性能方面:随着溅射功率密度的升高,薄膜导电性能迅速增强,电阻率呈现近似指数函数衰减|随着基底温度的升高,薄膜的电阻率先减小后增大,当基底温度为150 ℃时,薄膜电阻率降低至最小值2.02×10-5 Ω·cm.     

退火处理对磁控溅射制备LaCoO_3薄膜性能的影响

采用磁控溅射法在硅衬底上制备了LaCoO_3(LCO)薄膜,研究了退火温度对LCO薄膜组织结构、表面形貌及热电特性的影响,并利用X射线衍射仪、原子力显微镜(AFM)、激光导热仪等对LCO薄膜的晶体结构、表面形貌、热扩散系数等进行测量与表征.结果表明:退火温度对LCO薄膜的结晶度、晶粒尺寸和薄膜表面形貌都有较大影响;退火前后LCO薄膜的热扩散系数都随温度的升高而减小,且变化速率逐渐减缓; LCO薄膜的热扩散系数随退化温度的升高先增大后减小.LCO薄膜经过700℃退火后得到最佳的综合性能,其薄膜表面致密、平整,结晶质量最好,热扩散系数最小,热电性能最好.     

蓝宝石衬底上Gd2O3掺杂CeO2氧离子导体电解质薄膜的生长及电学性能

采用反应磁控溅射方法,在(0001)蓝宝石单晶衬底上,制备了纳米多晶Gd2O3掺杂CeO2(GDC)氧离子导体电解质薄膜,采用X射线衍射仪(XRD)、原子力显微镜(AFM)对薄膜物相、结构、粗糙度、表面形貌等生长特性进行了表征,利用交流阻抗谱仪测试了GDC薄膜不同温度下的电学性能;实验结果表明,GDC薄膜为面心立方结构,在所研究的衬底温度范围内,均呈强(111)织构生长;薄膜表面形貌随衬底温度发生阶段性变化:衬底温度由室温升高到300℃时,对应球形生长岛到棱形生长岛的转变,当完全为棱形岛生长时(300℃),生长岛尺寸显著增大;从400℃开始,则发生棱形生长岛到密集球形生长岛的转变,球形生长岛尺寸明显减小.生长形貌的转变反映着薄膜生长初期不同的成核机理,很可能与蓝宝石(13001)面的表面结构随温度变化有关;GDC多晶电解质薄膜的复平面交流阻抗谱主要源于晶界的贡献,根据Arrhenius图求得电导活化能Ea在1.2-1.5 ev范围内,接近于晶界电导的活化能值,并且随衬底温度升高Ea减小(Ea300 > Ea400> Ea600 );电导活化能以及晶粒尺寸不同,导致GDC薄膜电导率随测试温度的变化规律不同.     

高择优取向Mo薄膜的直流磁控溅射制备及其电学性能

使用直流磁控溅射法在玻璃基底上沉积Mo薄膜,采用X射线衍射仪、原子力显微镜和四探针测试系统研究了溅射工艺对Mo薄膜的结构、形貌和电学性能的影响.结果表明:当基片温度为150℃时,薄膜获得(211)晶面择优取向生长,而在低于250℃的其它温度条件下,样品则表现为(110)晶面择优取向生长.进一步的表面形貌分析显示:薄膜的...     

金属诱导生长与超高真空化学气相沉积方法相结合制备多晶锗硅薄膜

采用金属Ni诱导与超高真空化学气相沉积(UHVCVD)相结合的方法，在热氧化硅衬底上生长了多晶锗硅薄膜.利用X射线衍射(XRD)、场发射扫描电镜(SEM)等对多晶锗硅薄膜的质量、表面形貌进行了测试分析，并就生长参数以及金属Ni对薄膜性能的影响进行了研究.结果表明：1)在420—500℃范围内，金属Ni具有明显的诱导作用；2)Ni层厚度对薄膜质量及形貌的影响使得晶粒尺寸随Ni厚度增加存在一极大值.在Ni层厚度为60nm时，能够获得晶粒尺寸均匀，晶粒大小为500—600nm，结晶质量良好的多晶锗硅薄膜. 关键词： 超高真空化学气相沉积 金属诱导 镍 多晶锗硅     

生长温度对碳纳米管阴极场发射性能的影响

碳纳米管(Carbon Nanotubes,CNTs)场发射平面显示器(Field Emission Display,FED)与其他显示器比较显示了其独特优点,被认为是未来理想的平面显示器之一。碳纳米管阴极作为器件的核心部分,其性能的好坏直接影响显示器的性能。针对30~60英寸(76.2~152.4cm)大屏幕显示器所用的厚膜工艺,即采用丝网印刷法制备了碳纳米管阴极阵列,研究了化学气相沉积法在不同温度下生长的CNTs的场发射电流-电压特性,找到了适合FED用碳纳米管的最佳生长温度。结果表明生长温度越高(750℃),CNTs场发射性能越好。并用荧光粉阳极测试这些CNTs的场发射发光显示效果,验证了上述结论。     

阵列碳纳米管的石墨化程度

采用化学气相沉积法制备了阵列碳纳米管薄膜,对阵列碳纳米管的石墨化程度进行了系统研究。利用扫描电子显微镜(SEM)、拉曼光谱(Raman)对样品形貌以及结构进行了表征。探讨了不同实验参数对阵列碳纳米管石墨化程度影响的机理。结果发现,在一定催化剂浓度范围内,催化剂浓度过低时,阵列碳纳米管的石墨化程度较差,而随着催化剂浓度的增加,阵列碳纳米管的石墨化程度逐渐变好;生长石墨化程度较好的阵列碳纳米管需要合适的进液速度,进液速度过低或过高都会使得碳纳米管的石墨化程度变差;此外,生长石墨化程度较好的阵列碳纳米管也需要合适的生长温度,生长温度过低或过高都会使得碳纳米管的石墨化程度变差。     

磁控共溅射法制备的Zn2GeO4多晶薄膜结构及其光致发光研究

用射频控共溅射方法在不同温度的单晶硅基片上生长薄膜,然后在800℃真空环境下对薄膜进行退火处理,成功获得了结晶状态良好的Zn2GeO4多晶薄膜.利用X射线衍射(XRD),X射线光电子能谱(XPS)和原子力显微镜(AFM)对薄膜进行了结构、成分和形貌分析,研究了基片温度对三者的影响.结果显示,当基片温度升高到400℃以上时,薄膜中的Zn2GeO4晶粒在(220)方向上显示出了明显的择优取向.当基片温度在500-600℃范围内,有利于GeO2结晶相的形成.XPS显示薄膜中存在着Zn2GeO4,GeO2,GeO,ZnO四种化合态.同时,随着基片温度的升高,晶粒尺寸增大且薄膜表面趋于平整.薄膜的光致发光在绿光带存在中心波长为530和550 nm两个峰,应该归因于主体材料Zn2GeO4中两个不同的Ge2 的发光中心.     

沉积工艺参数对碳纳米管薄膜场发射性能的影响

利用微波等离子体化学气相沉积(MWPCVD)方法,在不锈钢衬底上直接沉积碳纳米管膜。通过SEM、拉曼光谱和XRD表征,讨论了制备温度和甲烷浓度对碳纳米管膜场发射的影响。结果表明:不同条件下制备的碳纳米管膜的场发射性能有很大差异,保持氢气的流量(100sccm)、生长时间(10min)、反应室压力不变,当甲烷流量为8sccm、温度为700~800℃时,场发射性能最好,开启场强仅为0.8V/μm,发射点分布密集、均匀。     

高能球磨对碳纳米管形貌及场致发射显示特性的影响

用化学气相沉积法制备了碳纳米管,进行了不同时间的球磨处理。用扫描电镜、拉曼光谱对其形貌和结构进行了表征。对不同球磨条件下的碳纳米管制备成阴极,进行了场致发射特性的测试。结果表明,高能球磨会对碳纳米管的形貌、结构及场致发射性能有明显的影响。球磨时间为0．5～1h时,可以使碳纳半管变短而均匀,且场致发射电性能与未处理时相近,即有低的阈值电场和高的发射电流密度,从而使发射时在阳极上产生的荧光点密度大大增加,发光均匀。但研磨时间过长会改变碳纳半管结构,使其非晶化或石墨化,导致其场致发射性能和显示效果变差。     

Improve the field emission uniformity of carbon nanotubes treated by ball-milling process

Carbon nanotubes (CNTs) deposited by chemical vapor deposition (CVD) were treated by ball milling. The morphologies and field emission properties of the treated CNTs depending on milling time were studied. The emission turn-on field is increased, and the field emission current density is reduced, when the milling time increased from 0.5 to 3 h. The as-deposited long CNTs were cut to short CNTs (∼1 h) and micro-particles (>1 h) with increasing of the milling time. It is found that the optimized milling time is 0.5-1 h, the treated CNTs showed excellent field emission properties, such as low turn-on field, high emission current density and uniform luminescence spots distribution.     

Aligned growth and alignment mechanism of carbon nanotubes by hot filament chemical vapor deposition

Carbon nanotubes (CNTs) growth on Inconel sheets was carried out using hot filament chemical vapor deposition (HFCVD) in a gas mixture of methane and hydrogen. Scanning electron microscopy, transmission electron microscopy and field electron emission (FEE) measurement were applied to study the structure and FEE properties of the deposited CNTs. The effect of bias voltage and substrate surface roughness on the growth of vertically aligned carbon nanotubes was investigated. Well-aligned CNTs were synthesized by bias enhanced HFCVD. The results show that a bias of −500 V generates the best alignment. It has been observed that at the early growth stage, aligned and non-aligned CNTs are growing simultaneously on the unscratched sheets, whereas only aligned CNTs are growing on the scratched sheets. The results indicate that tip growth is not necessary for the electric field to align the CNTs, and larger catalyst particles created by scratching before the heat treatment can induce alignment of CNTs at the early growth stage. In addition, tree-like CNTs bundles grown on the scratched substrates exhibit better FEE performances than dense carbon nanotube forest grown on the unscratched substrates due to the reduced screen effect.     

Field emission characteristics of carbon nanotubes post-treated with high-density Ar plasma

The field emission characteristics of carbon nanotubes (CNTs) grown by thermal chemical vapor deposition (CVD) and subsequently surface treated by high-density Ar plasma in an inductively coupled plasma reactive ion etching (ICP-RIE) with the various plasma powers were measured. Results indicate that, after treated by Ar plasma with power between 250 and 500 W, the emission current density of the CNTs is enhanced by nearly two orders of magnitude (increased from 0.65 to 48 mA/cm²) as compared to that of the as-grown ones. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were employed to investigate the structural features relevant to the modified field emission properties of CNTs. The SEM images of CNTs subjected to a 500 W Ar plasma treatment exhibit obvious damages to the CNTs. Nevertheless, the turn-on fields decreased from 3.6 to 2.2 V/μm, indicating a remarkable field emission enhancement. Our results further suggest that the primary effect of Ar plasma treatment might be to modify the geometrical structures of the local emission region in CNTs. In any case, the Ar plasma treatment appears to be an efficient method to enhance the site density for electron emission and, hence markedly improving the electric characteristics of the CNTs.     

Synthesis of carbon nanotubes on diamond-like carbon by the hot filament plasma-enhanced chemical vapor deposition method

Carbon nanotubes (CNTs) have attracted considerable attention as possible routes to device miniaturization due to their excellent mechanical, thermal, and electronic properties. These properties show great potential for devices such as field emission displays, transistors, and sensors. The growth of CNTs can be explained by interaction between small carbon patches and the metal catalyst. The metals such as nickel, cobalt, gold, iron, platinum, and palladium are used as the catalysts for the CNT growth. In this study, diamond-like carbon (DLC) was used for CNT growth as a nonmetallic catalyst layer. DLC films were deposited by a radio frequency (RF) plasma-enhanced chemical vapor deposition (RF-PECVD) method with a mixture of methane and hydrogen gases. CNTs were synthesized by a hot filament plasma-enhanced chemical vapor deposition (HF-PECVD) method with ammonia (NH₃) as a pretreatment gas and acetylene (C₂H₂) as a carbon source gas. The grown CNTs and the pretreated DLC films were observed using field emission scanning electron microscopy (FE-SEM) measurement, and the structure of the grown CNTs was analyzed by high resolution transmission scanning electron microscopy (HR-TEM). Also, using energy dispersive spectroscopy (EDS) measurement, we confirmed that only the carbon component remained on the substrate.     

Synthesis and field emission properties of carbon nanotubes grown in ethanol flame based on a photoresist-assisted catalyst annealing process

Carbon nanotubes (CNTs) have been grown directly on a Si substrate without a diffusion barrier in ethanol diffusion flame using Ni as the catalyst after a photoresist-assisted catalyst annealing process. The growth mechanism of as-synthesized CNTs is confirmed by scanning electron microscopy, high resolution transmission-electron microscopy and energy-dispersive spectroscopy. The photoresist is the key for the formation of active catalyst particles during annealing process, which then result in the growth of CNTs. The catalyst annealing temperature has been found to affect the morphologies and field electron emission properties of CNTs significantly. The field emission properties of as-grown CNTs are investigated with a diode structure and the obtained CNTs exhibit enhanced characteristics. This technique will be applicable to a low-cost fabrication process of electron-emitter arrays.     

Improved emission stability of HfC-coated carbon nanotubes field emitters

Plasma-enhanced chemical vapor deposition (PECVD) method was employed to synthesize the Fe-catalyzed carbon nanotubes (CNTs). Hf films were deposited onto the synthesized CNTs, followed by heat treatment at 1200 °C which could form HfC. Field emission properties indicate that the HfC-coated CNTs have good emission current density due to low work function of HfC and also keep stable emission characteristics under poor vacuum owing to the chemical inertness of HfC. Consequently, field emission characteristics of the CNTs can be improved by the HfC-coated surface treatment compared with the synthesized CNTs.     

Growth of carbon nanotubes on stainless steel substrates by DC-PECVD

We report on the fabrication of carbon nanotubes (CNTs) on Ni-coated stainless steel (SUS) substrates by using dc plasma enhanced chemical vapor deposition. The synthesized CNTs have the diameter of about 30 nm and the length of about 1.2 μm. To verify the effects of SUS substrates on the growth of CNTs, CNTs had also been grown on Ni-coated Si substrates. CNTs grown on the SUS substrates were more uniform compared with those grown on the Si substrates. Field emission properties of the CNT films were measured in the diode configuration, and the turn-on electric field of 3.87 V/μm and field enhancement factor β of about 1737 were obtained from the synthesized CNTs at the gap of 500 μm between the SUS substrate and the anode. These results have not only clarified the effects of the substrate on the growth of CNTs, but also shown the potential of CNTs in field emission applications, especially CNT-based cold-cathode X-ray tubes.