VHF-PECVD制备微晶硅薄膜的微结构研究

用甚高频等离子体化学气相沉积(VHF-PECVD)法在玻璃衬底上低温制备了不同沉积时间微晶硅薄膜.用拉曼散射光谱仪、X射线衍射(XRD)、原子力显微镜(AFM)等表征手段对薄膜的微观结构进行了研究.研究结果表明:随着沉积时间的延长,薄膜呈岛状生长,薄膜晶粒度在微晶核形成后迅速升高并逐渐饱和;其微观结构经历了"非晶相→非晶/微晶混合相→微晶相"的演变过程.本实验制备的微薄膜仍以(111)为优化取向.     

氧等离子体处理硬质合金表面对金刚石薄膜附着性能的影响

本文采用微波氧等离子体刻蚀硬质合金基体表面,再利用热的浓碱溶液清除硬质合金表面所形成的氧化物,通过扫描电镜(SEM)观察了试样表面情况,并通过X射线能谱(EDAX)分析了硬质合金表面各成分变化情况.经过预处理的试样采用热丝化学气相沉积(HFCVD)金刚石薄膜,对所沉积出的金刚石薄膜采用SEM观察及压痕测试,发现经过氧等离子体处理的金刚石刀具较两步酸蚀法处理过的金刚石薄膜涂层,其附着性能有较大提高.     

氧等离子体对以石墨为碳源合成的CVD金刚石颗粒的影响

采用一种新型的金刚石颗粒制备方法,利用微波辅助化学气相沉积技术,向反应室内通入氢气,以固态石墨片同时作为碳源和衬底沉积金刚石颗粒.利用该方法合成的金刚石颗粒具有微米级尺寸,可用作研磨剂、抛光剂、形核剂等.但是合成的金刚石颗粒中仍含有少量的非晶碳,且合成颗粒的尺寸均匀性有待提高.为解决以上问题,本文中在反应不同阶段(初期、中期及末期)通入氧气,形成氧等离子体;研究氧等离子体对合成的金刚石颗粒形貌、尺寸、质量、纯度的影响,以及随氧等离子体添加阶段不同而产生的不同变化情况.结果 表明,经氧等离子体处理的金刚石颗粒形貌略有改变,表面光滑度更好,且金刚石颗粒尺寸的一致性有所提高;经过激光粒度测试发现,金刚石颗粒的尺寸主要集中在25～ 29 μm.添加氧等离子体有助于消除金刚石中的非晶碳,提高金刚石纯度;且在反应初期添加氧等离子体可最大程度提高金刚石颗粒质量.     

催化剂膜厚对碳纳米管薄膜生长的影响

采用射频等离子体增强化学气相沉积技术,以Ni为催化剂,在Si基底上沉积出定向性良好的碳纳米管.用扫描电镜表征了催化剂颗粒大小和相应的碳纳米管形貌.深入研究了催化剂膜厚对碳纳米管牛长的影响.结果表明:不同度的催化剂薄膜经刻蚀形成的颗粒密度、尺寸、分布等对碳纳米管的合成质量起主要作用.催化剂厚度≤5 nm时,形成的颗粒密度较小而且分布不均,制备的碳纳米管产量低、定向性差.催化剂厚度≥15 nm时,形成的颗粒较大,粘连在一起,生长时大部分被非晶碳包覆,几乎没有碳纳米管的生长.催化剂厚度为10 nm时,形成的颗粒密度大、分布较均,制备的碳纳米管纯度高、定向性好.     

沉积温度对硬质合金表面沉积的SiC薄膜的影响

采用强电流直流伸展电弧等离子体CVD技术,以Ar、H2和四甲基硅烷(TMS)为先驱气体,在YG6硬质合金衬底表面制备了SiC薄膜。实验结果表明:随着沉积温度的升高,薄膜的致密性和平整度提高;但当沉积温度过高时,SiC薄膜的表面开始具有含非晶碳球和呈花瓣状的疏松结构。在合适的沉积温度下,SiC薄膜的致密性和平整度较好,且其具有较好的附着力和一定的强度,而这样的SiC薄膜可以阻止在金刚石涂层沉积过程中硬质合金中含有的Co对金刚石相沉积过程的有害作用。     

过渡层对纳米非晶碳薄膜场发射性能的影响

采用微波等离子体化学气相沉积法在经研磨处理后的Si(111)面上制备出了纳米非晶碳薄膜.为改善薄膜的场发射性能,在研磨好的Si基底上运用直流磁控溅射法沉积了一层金属过渡层.本文分别选择三种常见金属:钛(Ti)、鉬(Mo)、镍(Ni)来作对比试验.结果发现用钛作为过渡层时薄膜场发射效果最好,主要表现为开启电场低,同一电场下发射电流大,发射点密度较大且分布均匀等.利用迭代法计算了钛作为过渡层时制备的纳米非晶碳薄膜的有效发射面积和功函数.     

直流电弧等离子体喷射法制备氮化碳薄膜研究

以H2、N2和CF4气体为前驱体,用直流电弧等离子体喷射设备在不同基底温度条件下于钼/金刚石过渡层基底上制备了氮化碳薄膜.利用扫描电子显微镜(SEM)、能谱仪(EDS)、X射线衍射仪(XRD)对表面形貌和组织成分进行了表征.结果表明,当基底温度为900℃时,所沉积材料已初具晶型;所沉积材料含有α-C3N4和β-C3N4相成分.同时,提出在金刚石表面制备氮化碳时金刚石相刻蚀和氮化碳相生长同时进行的模型,较好地解释了不同基底温度条件下的膜材料沉积现象.     

基于氢等离子体处理改善氢化非晶硅/晶体硅界面钝化效果的工艺研究

薄层a-Si∶H钝化技术对于提高硅异质结太阳能电池的效率至关重要,通常有三类工艺可显著改善a-Si∶H薄膜的钝化效果:晶硅表面湿化学处理(薄膜沉积前);氢等离子体处理(薄膜沉积过程中);后退火处理(薄膜沉积后).该论文基于等离子增强型化学气相沉积系统,采用氢等离子处理和后退火处理改善a-Si∶ H/c-Si界面的钝化效果,样品的有效少数载流子寿命最高达到1 ms,并研究了射频功率密度、腔体压力、氢气流量等工艺参数对钝化效果的影响;采用光发射谱、台阶仪等对氢等离子体处理所涉及的物理过程进行研究,得出该工艺对a-Si∶H薄膜具有刻蚀作用;根据钝化效果和刻蚀速率的关系,得出低刻蚀速率由于给予薄膜充足的时间进行结构弛豫或重构,显著改善钝化效果;基于快速热退火方法进一步改善钝化效果,采用傅里叶变换红外光谱对a-Si∶H薄膜的钝化机理进行研究,并基于化学退火模型进行讨论;采用透射电镜研究了a-Si∶ H/c-Si界面的微结构,并没有观测到影响钝化效果的外延生长.     

用MPCVD法制备氮化碳薄膜

用微波等离子体化学气相沉积法(MPCVD)在硅片和铂基片上生长了氮化碳薄膜.扫描电镜(SEM)观察显示,在硅片上形成了多晶的膜;EDX能谱分析表明膜中的碳氮比在1.0～2.0之间;X射线衍射谱表明在硅片和铂片上生长的氮化碳薄膜是由α-C3N4和β-C3N4晶相组成的;XPS峰形分析表明,薄膜中的C、N主要是以共价单键结合的;红外谱中也出现了β-C3N4的特征谱线.因此有足够的证据表明,晶态的氮化碳薄膜已经合成.     

SiNX覆盖层厚度对非晶In-Ga-Zn-O薄膜退火晶化的影响研究

采用射频磁控溅射在二氧化硅衬底上沉积一层厚度200 nm的非晶In-Ga-Zn-O(IGZO)薄膜,并在IGZO膜层上沉积厚度分别为20 nm、50 nm、60 nm、70 nm、90 nm的SiNX薄膜覆盖层,于350℃条件下N2气氛中退火1 h.采用X射线衍射(XRD)、高分辨透射电子显微镜(HRTEM)、能量色散谱仪(EDS)对IGZO薄膜的微观结构及成分进行研究.研究结果表明,退火后无覆盖层的IGZO膜层仍为非晶状态,70 nm以上SiNX覆盖层下的IGZO薄膜不发生晶化.与此不同,20～60 nm的SiNX覆盖层下IGZO膜层与SiNX覆盖层的界面处存在纳米凸起柱,使IGZO薄膜与SiNX覆盖层的接触界面脱离,此厚度的SiNX覆盖层具有诱导非晶IGZO薄膜晶化的作用,IGZO膜层内部的晶粒直径约10 nm.成分分析结果表明,结晶处In原子含量增加,IGZO薄膜中In原子的局域团聚是IGZO薄膜发生晶化的原因.     

[100]定向织构生长金刚石薄膜的红外光学性能研究

采用微波等离子增强化学气相沉积法在(100)镜面抛光的硅片衬底上实现了金刚石薄片[100]定向织构生长.并用扫描电子显微镜、拉曼散射和傅立叶红外光谱仪分析测试了不同工艺得到的金刚石薄片的表面形貌、组成结构和红外性能.结果表明:负偏压辅助定向成核和氢的等离子刻蚀不仅促进了金刚石薄膜的定向织构生长,而且还能刻蚀成核期的非金刚石成分.从而提高了金刚石薄片的红外光透过特性.     

Diamond nanorods from nanocrystalline diamond films

Diamond nanorods (DNRs) have been prepared by hydrogen plasma post-treatment of nanocrystalline diamond films in radio-frequency (RF) plasma-assisted hot-filament chemical vapor deposition. Single-crystal diamond nanorods with diameters of 3–5 nm and with lengths up to 200 nm grow under hydrogen plasma irradiation of nanocrystalline diamond thin film on the Si substrate at high temperatures. The DNRs growth occurs from graphite clusters. The graphite clusters arises from the etching of diamond carbon atoms and from the non-diamond phase present in the parent film. The graphite clusters recrystallized to form nanocrystalline diamonds which further grow for diamond nanorods. The negative applied bias and surface stresses are suggested to support one-dimensional growth. The growth direction of diamond nanorods is perpendicular to the (1 1 1) crystallographic planes of diamond. The studies address the structure and growth mechanism of diamond nanorods.     

Effect of rare-earth elements on the plasma etching behavior of the RE–Si–Al–O glasses

The effect of rare-earth elements on the plasma etching behavior of oxide glasses were investigated to develop the window glass for a plasma processing chamber in the semiconductor industry. Aluminosilicate glasses with various rare-earth elements (Y, Gd and La) were prepared and their optical transmittance and plasma etching depth were evaluated. The plasma etching behavior of the glasses was estimated by X-ray photoelectron spectroscopy analysis at the fluorine plasma exposure surface of the glasses. The rare-earth element in the glass was highly related to various properties such as density, molar volume, mechanical properties and plasma etching depth. The cationic field strength of the rare-earth element more strongly affected the plasma etching depth of the glasses than the sublimation point of the fluorine compounds and this may be related to the plasma etching condition.     

Plasma etching of As2S3 films for optical waveguides

Chalcogenide glasses are good candidate materials for ultra-fast non-linear optic devices. In this work, we present the photolithographic process and the plasma etching of arsenic tri-sulphide (As₂S₃) film. The films were deposited on thermally oxidized silicon substrates by ultra-fast pulsed laser deposition. To protect As₂S₃ film from photo-resist developer, thin resist layer ∼100-200 nm was remained on the UV exposed area by controlling resist development time. After removing the protective layer in oxygen plasma, As₂S₃ waveguides were patterned in inductively coupled plasma reactive ion etching (ICP-RIE) system using CF₄-O₂ gas mixture. We investigated the etch rate and the etch selectivity to photo-resist of As₂S₃ as a function of bias power, induction power, operating pressure, and gas flow rate ratio of CF₄ and O₂. The film is mainly etched by the chemical reaction with fluorine radicals. The content of oxygen in the plasma determines the etched sidewall profiles and nearly vertical profile was obtained at high oxygen content plasma.     

掺氮四配位非晶碳薄膜的拉曼光谱和表面形貌

采用磁过滤真空溅射离子沉积技术,用氩气和氮气共溅射石墨靶,在不同氮气分压下,制备了一组不同氮含量的四配位非晶碳薄膜(ta-C:N).用X射线光电子能谱确定ta-C:N薄膜中的氮含量;研究了氮含量对ta-C薄膜的拉曼光谱和表面形貌的影响.结果表明:不含氮的ta-C薄膜的拉曼光谱是中心在1580cm-1、范围从1200cm-1至2000cm-1的类高斯峰,表面均匀光滑;含氮的ta-C:N薄膜,其拉曼光谱分裂为1360 cm-1的D带和1580 cm-1的G带,且D带与G带的最大强度比, 以及薄膜的表面粗糙度随氮含量的增加而增大.最后讨论了氮含量对ta-C薄膜的微结构的影响.     

Growth and optical property characterization of textured barium titanate thin films for photonic applications

We have investigated the growth of barium titanate thin films on bulk crystalline and amorphous substrates utilizing biaxially oriented template layers. Ion beam-assisted deposition was used to grow thin, biaxially textured, magnesium oxide template layers on amorphous and silicon substrates. Growth of highly oriented barium titanate films on these template layers was achieved by molecular beam epitaxy using a layer-by-layer growth process. Barium titanate thin films were grown in molecular oxygen and in the presence of oxygen radicals produced by a 300 W radio frequency plasma. We used X-ray and in situ reflection high-energy electron diffraction (RHEED) to analyze the structural properties and show the predominantly c-oriented grains in the films. Variable angle spectroscopic ellipsometry was used to analyze and compare the optical properties of the thin films grown with and without oxygen plasma. We have shown that optical quality barium titanate thin films, which show bulk crystal-like properties, can be grown on any substrate through the use of biaxially oriented magnesium oxide template layers.     

自支撑氮化硅膜结构制备工艺优化

自支撑氮化硅膜结构一般是基于微纳加工技术来制备的。为了提高膜结构的品质,本文分别对自支撑氮化硅膜结构制备中的干法刻蚀参数和各向异性湿法腐蚀参数进行了研究和优化,其中干法刻蚀参数主要包括反应气体配比和刻蚀时间,各向异性湿法腐蚀参数主要包括腐蚀剂浓度和腐蚀温度。在不同的参数组合下进行实验,使用光学显微镜观察并比较不同样品的表面形貌,得到了较理想的参数组合。在干法刻蚀的反应气体中加入少量O₂可改善刻蚀效果,反应气体配比V(SF₆)∶V(CHF₃)∶V(O₂)=6∶37∶3,刻蚀时间2 min。湿法腐蚀中腐蚀剂在质量分数25%处达到最大的硅腐蚀速率,同时氮化硅表面形貌也较理想。     

用PECVD在低温衬底上制备类金刚石碳膜

本文报道用 RF PECVD在低温衬底上制备了类金刚石碳(DLC)膜.研究了氢稀释、气体压力和 RF 功率对薄膜性质的影响. 用光透射率、红外吸收谱和小角度X射线衍射谱分析了DLC膜的结构和光学性质.结果表明,这样制备的DLC膜是无定形态的,包含了大量的C-H键,具有良好的透明性.厚度为230nm的DLC膜在480nm后的可见光区和近红外区的透过率大于83;,所导出的Tauc光学带隙在2.7eV和3.7eV之间.本文还探讨了应用这种DLC膜作为二次电子发射材料的可能性.     

Atmospheric aging and thermal annealing effects in a-C:H thin films

Atmospheric aging and thermal annealing effects have been studied in hydrogenated amorphous carbon (a-C:H) thin films deposited using a dc saddle field glow discharge technique with different ion energies (85–225 eV) during deposition. The a-C:H films grown with low ion energies showed aging effects when they were exposed to the ambient atmosphere. Infrared (IR) absorption due to O–H and C=O vibration modes increased while the IR absorption due to C–H vibrations decreased with aging. The absence of absorption due to O–D vibrations in deuterated films indicates that the films reacted with water rather than oxygen when exposed to the atmosphere. The C–H and O–H bond concentrations decreased when the a-C:H films which had been exposed to the atmosphere for a one month period were thermally annealed. The a-C:H films grown with high ion energies exhibited neither atmospheric aging nor thermal annealing effects.