准动态柱腔充气靶制备工艺研究

主要研究了聚酰胺酸的合成和成膜,聚酰亚胺的热环化,柱腔充气靶的组装和检测,柱腔充气系统的研制,靶场装配和测量,采用准动态充气方式的充气工艺等。研究表明,在二胺和二酐按摩尔比1.01∶1~1.02∶1,反应温度0~5 ℃,反应时间2~3 h条件下,可以制备出厚度0.2~1.0 μm的聚酰亚胺薄膜;薄膜表面光洁度达0.3～0.4 nm,厚度起伏小于5％,薄膜厚度均匀性和表面光洁度都能满足充气靶端口膜的需要,可承受0.1 MPa的压力差;利用柱腔充气系统,可以实现打靶现场配气与充气,并准确控制和测量靶内的气压,测量的误差小于0.1%。     

气相沉积法制备聚酰亚胺薄膜不同单体配比的表征及其性能影响

聚酰亚胺微球作为惯性约束聚变的重要候选靶丸之一,其力学性能和热学性能的提高对于实现聚变点火有重要意义.本文以均苯四甲酸二酐和二氨基二苯醚为原料,采用气相沉积法制备了不同单体配比的聚酰胺酸薄膜,研究了制备聚酰胺酸薄膜过程中不同单体蒸发温度对薄膜组成的影响,并对聚酰胺酸薄膜进行热环化处理.采用红外光谱仪分析了聚酰胺酸薄膜和聚酰亚胺薄膜的组成,结果表明:随着二酐蒸发温度的增加,聚酰胺酸薄膜中过量二酐单体的红外吸收振动特征峰(1780 cm~(-1),1850 cm~(-1)强度增加,单体配比由二胺过量到二酐二胺配比均衡再到二酐过量.热环化处理的过程中,薄膜中过量单体会再次蒸发,其红外图谱显示最终产物只有聚酰亚胺,但单体配比接近样品聚酰亚胺红外特征振动峰(1380 cm~(-1))强度更大.X射线衍射图谱显示配比接近的样品具有更高的晶化程度,说明过量单体的存在抑制了聚酰胺酸分子链的生长,造成分子量降低.采用纳米压痕仪和热重分析仪分别测量了聚酰亚胺薄膜的弹性模量和硬度以及失重曲线,结果表明分子量的降低会造成聚酰亚胺薄膜的弹性模量和硬度的降低,同时热稳定性也变差.扫描电子显微镜图像显示聚酰亚胺薄膜呈层状结构,单体配比接近的样品表面状况更好,这一点与聚酰亚胺分子的生长规律相符合.     

气相沉积法制备聚酰亚胺微球的均匀性及性能

为满足惯性约束聚变(ICF)对聚酰亚胺(PI)靶丸的要求,研究了气相沉积过程单体加热温度对PI薄膜厚度的影响并测试其均匀性,测试了脉冲敲击模式下复合微球的表面质量。研究了薄膜热环化过程中的结构变化,并对所得PI薄膜进行了热稳定性分析。研究结果表明:脉冲敲击下制备所得复合微球表面粗糙度均方根值波动在29~45nm之间,在相同时间内其薄膜厚度随单体加热温度的增加而增加,通过调节不同单体加热温度,可将薄膜厚度控制在一定范围;薄膜厚度测试发现其较为均匀,横向和纵向各点厚度相差不足1μm;热环化后聚酰胺酸转化为PI,CONH与COOH结合形成C-N键;热重分析数据显示PI薄膜热稳定性较好,600℃左右才开始大量分解。     

充气塑料柱腔的制备与保气半寿命

 研究了聚苯乙烯塑料柱腔的两种制备方法：采用聚苯乙烯溶液旋转涂层和熔体浸涂。聚苯乙烯熔融后浸涂制备的塑料柱腔存在一定的结晶取向和很多气泡,去掉铜芯轴后,塑料柱腔因缺陷太多几乎不能保气,成品率非常低,不到10％。利用聚苯乙烯溶液通过多次旋转涂层和烘干过程制备的塑料柱腔具有很低的表面粗糙度,柱腔厚度为10～30 m,表面粗糙度5～20 nm,采用0.3～0.4 μm聚酰亚胺膜封口保气,气体介质为氪气,通过X射线荧光谱仪测量柱腔保气半寿命约24 h。采用保气罐储存和运输无源塑料柱腔充气靶,打靶时腔内气体密度可保持在初始状态的92％左右。     

分层蒸镀制备聚酰亚胺自支撑膜及其特性研究

 采用分层蒸镀法,在玻璃基片上依次蒸镀二氨基二苯醚（ODA）和均苯四甲酸二酐（PMDA）两种单体,然后在空气环境中对样品进行不同温度和时间的热亚胺化处理,使二者在交界面上反应生成聚酰亚胺。经加热150 ℃ 1 h然后经350 ℃ 2 h处理的样品,在脱膜后能制备出直径1.8 cm,厚度为100 nm的聚酰亚胺自支撑薄膜。用FTIR测量了自支撑薄膜的红外光谱,特征吸收峰的分析表明薄膜已基本上完全亚胺化。用原子力显微镜分析了浮法玻璃衬底上聚酰亚胺薄膜的表面形貌,结果表明以ODA作为内层制备的膜层表面更光滑平整。     

聚酰亚胺LB膜的研究：Ⅰ聚酰胺酸N,N—二甲基十八胺前聚物的LB膜

聚酰胺酸Ｎ，Ｎ－二甲基十八胺是制备本身不具备两亲性的聚酰亚胺ＬＢ膜的前聚物。合成制备了均苯四酸二酐－４，４’－二胺基二苯酸Ｎ，Ｎ－二甲基十八胺，研究了它单分子膜的各异性，比较了伯胺和叔胺膜的不同，并用低角Ｘ射线衍射研究这前聚物ＬＢ膜分子的详细排列。     

气袋靶制备技术

为了研究柱腔内气体对激光-等离子体相互作用及内爆对称性的影响,详细给出了气袋靶制备及其在神光-Ⅱ靶场的应用情况。对气袋靶的靶型设计、靶材料选择及薄膜制备和充气工艺进行了系统的研究。制备的气袋靶主要由厚度为400 nm的聚酰亚胺薄膜和厚度为400 m的铝支撑环构成,利用装配在支撑环上的充气管实现对气袋靶的充气,当充气完成后,整个气袋靶膨胀为球状。     

用粉末靶在玻璃和PI衬底上制备AZO/Ag/AZO薄膜

室温下在玻璃和聚酰亚胺两种不同衬底上, 采用射频磁控溅射法溅射掺铝氧化锌(AZO)粉末靶和固体Ag靶, 制备了两组AZO/Ag/AZO 3层透明导电薄膜, 研究了AZO层厚度对不同衬底3层膜结构和光电性能的影响.结果表明:不同衬底的两组AZO/Ag/AZO薄膜均为多晶膜.当Ag层厚度不变时, 随着AZO层厚度的增加, 两组薄膜电学性能变化不大, 透射峰向长波方向移动.玻璃和PI衬底上制备的AZO(30 nm)/Ag(14 nm)/AZO(30 nm)薄膜, 在550 nm处的透光率分别为85%和70%, 方块电阻分别为2.6 Ω/□和4.6 Ω/□.     

对超声波作用下的化学浴沉积方法制备CdS薄膜的谱学分析

用化学浴沉积法制备了CdS薄膜 ,并研究了加超声波对CdS薄膜生长过程的影响。利用卢瑟福背散射 ,X 射线粉末衍射和扫描电子显微镜对薄膜的厚度、晶相和表面形貌进行了表征。结果表明施加超声波的作用能有效地改善薄膜的质量 ,制备出均匀、致密的有较好的晶体结构CdS薄膜。同时 ,通过时间的控制可以精确地控制薄膜在 5 0nm左右 ,以满足制备太阳能电池的特殊要求。     

WS2纳米薄膜厚度依赖的三阶非线性吸收特性研究

利用液相剥离法制备了WS2纳米片,结合真空抽滤技术,控制上清液体积制备了不同厚度的WS2薄膜.在此基础上,使用800 nm飞秒激光的Z扫描技术表征了WS2纳米薄膜的三阶非线性吸收特性.研究发现,制备的不同厚度的WS2都表现出可饱和吸收特性,可饱和吸收主要是由于单光子吸收所引起的泡利阻塞效应引起;随着厚度的增加,饱和强度...     

Properties of Cu film and Ti/Cu film on polyimide prepared by ion beam techniques

Cu film and Ti/Cu film on polyimide substrate were prepared by ion implantation and ion beam assisted deposition (IBAD) techniques. Three-dimension white-light interfering profilometer was used to measure thickness of each film. The thickness of the Cu film and Ti/Cu film ranged between 490 nm and 640 nm. The depth profile, surface morphology, roughness, adhesion, nanohardness, and modulus of the Cu and Ti/Cu films were measured by scanning Auger nanoprobe (SAN), atomic force microscopy (AFM), and nanoindenter, respectively. The polyimide substrates irradiated with argon ions were analyzed by scanning electron microscopy (SEM) and AFM. The results suggested that both the Cu film and Ti/Cu film were of good adhesion with polyimide substrate, and ion beam techniques were suitable to prepare thin metal film on polyimide.     

Surface roughness analysis and magnetic property studies of nickel thin films electrodeposited onto rotating disc electrodes

Ni films were electrodeposited onto polycrystalline gold substrates mounted on a rotating disc electrode. The effects of rotation speed, film thickness and current density on the kinetic roughening and magnetic properties of the films were investigated. The film surface roughness was imaged using an atomic force microscope (AFM). The results indicate that the film roughness increases as the film thickness or deposition current density increases. We found that the electrodeposited Ni films exhibit anomalous scaling since both local and large-scale roughnesses show a power-law dependence on the film thickness. The effect of electrode rotation speed on the film surface roughness was also investigated. Scanning electron microscopy studies (SEM) had a good agreement with the AFM results. The average crystalline size of the film surfaces is also calculated from X-ray line broadening using (220) peak and Debye–Scherrer formula. The obtained results agree with that of AFM and SEM. The Ni thin films which are grown at different deposition current densities and rotation speeds exhibit in-plane magnetization with coercivities less than 110 Oe.     

Effect of substrate curvature on thickness distribution of polydimethylsiloxane thin film in spin coating process

The polymer spin coating is critical in flexible electronic manufaction and micro-electro-mechanical system(MEMS)devices due to its simple operation, and uniformly coated layers. Some researchers focus on the effects of spin coating parameters such as wafer rotating speed, the viscosity of the coating liquid and solvent evaporation on final film thickness.In this work, the influence of substrate curvature on film thickness distribution is considered. A new parameter which represents the edge bead effect ratio(re) is proposed to investigate the influence factor of edge bead effect. Several operation parameters including the curvature of the substrate and the wafer-spin speed are taken into account to study the effects on the film thickness uniformity and edge-bead ratio. The morphologies and film thickness values of the spin-coated PDMS films under various substrate curvatures and coating speeds are measured with laser confocal microscopy. According to the results, both the convex and concave substrate will help to reduce the edge-bead effect significantly and thin film with better surface morphology can be obtained at high spin speed. Additionally, the relationship between the edge-bead ratio and the thin film thickness is like parabolic curve instead of linear dependence. This work may contribute to the mass production of flexible electronic devices.     

A Comparative Investigation of Thermal and Tribological Properties of Thermoplastic and Thermosetting Polyimides with Similar Structural Formulae

Polymerization of monomer reactants (PMR)-type polyimide was synthesized and the homogeneous matrix resin solution (30–40% solid) was used to prepare film blocks for tribological tests. Compared with a thermoplastic polyimide with similar molecular formula and similar behavior of weight loss under heating, the high glass transition (Tg) and char yield of the PMR polyimide can be attributed to the self-reaction of phenylethynyl groups to result in a cross-linked structure. Tribological studies on both PMR type thermosetting polyimide and thermoplastic one showed that the friction coefficient and wear rate of the former polyimide were lower than that of the latter one under both similar and even more critical conditions. Scanning electron microscope examinations of worn surfaces and wear debris show that the wear type of the thermoplastic polyimide was adhesive wear and that of the thermosetting one was fatigue wear. In terms of all good tribological properties, this PMR-type thermosetting polyimide, due to its high PV limit, could be a potential candidate for tribo-material in dry sliding against steel under high speed and large load.     

全息光栅掩模应力控制研究

通过干涉法并应用Stoney公式计算的结果，对SiO2基底上光刻胶薄膜的应力进行了研究。采用干涉显微镜在同一样品、不同直径上多点测量的方法，初步得出光刻胶薄膜膜厚均匀性的分布规律。发现在匀胶转速相同的前提下，光刻胶薄膜应力值随加速度的降低而减小，光刻胶薄膜的均匀性随加速度的增加而变好。在4000rpm的低转速时，光刻胶薄膜样品的膜厚均匀性好。因此，在全息光栅匀胶工艺中，要选择适当的转速的加速度，以得到应力较小和均匀性较好的光刻胶薄膜。     

空间多能电子辐照聚合物充电过程的稳态特性

空间同步轨道上多能电子辐照聚合物的充电过程及其稳态特性是研究和抑制通信卫星静电放电的基础.在同步电子散射-输运微观模型的基础上,采用具有10—400 keV积分能谱分布的多能电子辐照聚酰亚胺样品,进行了多能电子辐照聚酰亚胺充电过程的数值模拟,获得了空间电荷密度、空间电位、空间电场分布和聚合物样品参数条件下的表面电位和最大场强.结果表明,多能电子与样品发生散射作用并沉积在样品内形成具有高密度的电荷区域分布,同时在迁移和扩散的作用下输运至样品底部形成样品电流;充电达到稳态、电子迁移率较小时(小于10-10cm2·V-1·s-1),表面电位绝对值和充电强度随电子迁移率的降低明显加强,捕获密度较大时(大于1014cm-3),表面电位绝对值和充电强度随捕获密度的增大明显加强;聚合物样品厚度对表面电位和充电强度的影响大于电子迁移率、捕获密度和相对介电常数的影响.研究结果对于揭示空间多能电子辐照聚合物的充电现象及微观机理、提高航天器故障机理研究水平具有重要科学意义和价值.     

Effect of corona ageing on the structure changes of polyimide and polyimide/Al2O3 nanocomposite films

In order to investigate the corona ageing mechanism of polyimide and polyimide/Al₂O₃ nanocomposites, effects of corona ageing on the structure changes of the two polymers were studied. The physical and chemical changes were studied by Atomic Force Microscope (AFM), Scanning Electron Microscope (SEM) and Fourier Transform Infrared Spectroscope (FTIR) respectively. Modified isothermal discharge current method (MIDC) was used to investigate the trap level distribution before and after corona ageing. AFM images showed that there are large amounts of nano-clusters on the surface of polyimide nanocomposite before corona ageing. The surface roughness parameters of the nanocomposite is much larger than that of the pure polyimide, and that is slightly decreased for polyimide nanocomposite and largely increased for pure polyimide after corona ageing. FTIR spectra analysis showed that possible chemical changes due to the decomposition of C–O–C bond and C–N bond occurred during corona ageing for both polyimide and its nanocomposite. Pulse corona ageing can introduce even larger structure changes than the AC corona ageing for 100HN, while 100CR was just the opposite. IDC measurements showed that the trap level density was increased evidently after corona ageing and become larger for longer ageing time in 100HN film, whereas for 100CR, the trap level density was decreased with ageing time extended. Thus conclusions can be drawn that, corona ageing is a combined process leading to physical and chemical degradation of PI film. The more serious ageing the specimen suffers, the more changes of the trap level density and the surface roughness occurs. The deposition of inorganic nanoparticles on the surface of nanocomposite can form a flat block layer for corona ageing, which can decrease both the surface roughness and the physical trap level density.     

提拉法SiO_2化学膜厚度与折射率的变化规律研究

采用提拉法在硅基底上制备了多孔溶胶凝胶SiO2膜,用椭偏法测量薄膜的厚度与折射率,考察了提拉速度和胶体浓度对膜层厚度与折射率的影响。对厚度与提拉速度的关系进行线性与幂函数拟合,并比较分析两种拟合的关系及其对工艺流程的作用。比较了不同浓度胶体所得到的同一厚度薄膜的折射率变化规律。结果表明:对于同一胶体浓度下薄膜厚度与提拉速度的正相关关系,线性拟合相比幂函数拟合可以更好地解释实验结果的规律性。同时,折射率在一定范围内也会随着提拉速度的增加而减小。镀同一厚度膜时,浓度大的胶体膜层折射率大。通过对提拉速度和胶体浓度的控制可以得到理想的薄膜厚度与折射率。     

A study of direct- and pulse-current chromium electroplating on rotating cylinder electrode (RCE)

Direct- and pulse-current (DC and PC) chromium electroplating on Cr-Mo steel were performed in a sulfate-catalyzed chromic acid solution at 50 °C using a rotating cylinder electrode (RCE). The electroplating cathodic current densities were at 30, 40, 50 and 60 A dm⁻², respectively. The relationship between electroplating current efficiency and the rotating speed of the RCE was studied. The cross-sectional microstructure of Cr-deposit was examined by transmission electron microscope (TEM). Results showed that DC-plating exhibited higher current efficiency than the PC-plating under the same conditions of electroplating current density and the rotating speed. We found the critical rotating speed of RCE used in the chromium electroplating, above this rotating speed the chromium deposition is prohibited. At the same plating current density, the critical rotating speed for DC-plating was higher than that for PC-plating. The higher plating current density is, the larger difference in critical rotating speeds appears between DC- and PC-electroplating. Equiaxed grains, in a nanoscale size with lower dislocation density, nucleate on the cathodic surface in both DC- and PC-electroplating. Adjacent to the equiaxed grains, textured grains were found in other portion of chromium deposit. Fine columnar grains were observed in the DC-electroplated deposit. On the other hand, very long slender grains with high degree of preferred orientation were detected in PC-electroplated deposit.