磁场对电弧离子镀深管内壁沉积TiN薄膜的影响

用电弧离子镀设备在一端封口的Φ50 mm×200 mm×5 mm不锈钢深管内壁上沉积TiN薄膜,镀膜前在管子上方布置一个0.4 T的永磁体,以考察附加磁场对深管内壁沉积TiN薄膜的影响。对薄膜的厚度、表面形貌、相结构、显微硬度等随管子深度的变化进行了分析与测试,结果表明,薄膜的厚度及显微硬度都随管子的深度而下降,但在距管开口处前120 mm范围内下降明显慢于未加磁场的,说明磁场对内孔沉积具有促进作用;按照显微硬度不低于20 GPa划分,本实验的镀膜深径比达到了2.0,比未加磁场时提高了40%。     

脉冲偏压对电弧离子镀深管内壁沉积TiN薄膜的影响

用电弧离子镀设备,分别采用直流偏压和脉冲偏压的沉积工艺,在一端封口的50 mm×200 mm×5 mm的不锈钢深管内壁上沉积TiN薄膜,对薄膜的厚度、表面形貌、相结构、硬度和磨损性能等随管子深度的变化进行了对比测试.结果表明,两种工艺下薄膜的厚度、硬度以及耐磨性能都随管子的深度而下降,但与直流偏压相比,脉冲偏压能够提高薄膜厚度和硬度,减少大颗粒的尺寸和数量,提高耐磨性能;按照硬度不低于20 GPa的标准划分,脉冲偏压使镀膜深度提高了40%,即从直流偏压的50 mm提高到70 mm.     

脉冲真空弧源沉积类金刚石薄膜耐磨特性研究

本文利用脉冲真空弧源沉积技术在Cr17Ni14Cu4不锈钢和Si(100)基体上制备了类金刚石(DLC)薄膜,研究在不同基体偏压下,DLC薄膜的结构与性能.采用拉曼光谱和X射线光电子能谱(XPS)研究DLC薄膜的原子结合状态,利用CSEM销盘摩擦磨损试验机研究其耐磨性,利用HXD1000B显微硬度仪测试其显微硬度,并采用压痕法评价其结合力.研究结果表明:DLC薄膜与基体结合牢固.随着基体偏压的提高,DLC薄膜内sp3键含量增大,薄膜硬度提高.Cr17Ni14Cu4不锈钢表面沉积DLC薄膜后,耐磨性大幅度提高,本文探讨了DLC薄膜的耐磨机理.     

沉积温度对ZrO2薄膜结构及表面形貌的影响

采用反应磁控溅射方法,在室温～550℃的沉积温度下,在Si(100)和玻璃基片上沉积了厚度在纳米量级的ZrO2薄膜.通过高分辨电子显微镜、原子力显微镜和透射光谱分析,研究了沉积温度对ZrO2薄膜的相结构、表面形貌和折射率的影响.研究结果表明沉积温度低于250℃时,ZrO2薄膜的结构完全呈非晶态,但250℃沉积的薄膜有比较高的致密度;随着沉积温度的升高,薄膜出现了明显的结晶现象,主要为单斜ZrO2相;沉积温度为450℃时,ZrO2薄膜晶化不完全,在晶粒堆砌处有非晶ZrO2相存在;沉积温度为550℃时,ZrO2薄膜完全晶化,在晶粒堆砌处有四方ZrO2相存在.此外,根据薄膜相结构和表面形貌的研究结果,探讨了沉积温度对薄膜生长行为的影响及其物理机制.     

离子束增强沉积氮化硅薄膜的超显微硬度

利用测试负荷小于１０＾－１Ｎ的ＵＭＨＴ－３型超显微度测量仪，测试了不厚度的离子束增强沉积氮化硅薄膜的硬度。详细了薄膜和其底对在工测试的影响，并提出了临界负荷的概念，只有当测试负荷小于监界负荷时，才能获得薄膜的真空硬度。对三种不同厚度的氮化硅薄膜，给出了相应的监界负荷值。     

纳米Ti-Si-N薄膜的高温热稳定性

用直流等离子体增强化学气相沉积(PCVD)方法在不锈钢基体上制备了Ti-Si-N硬质纳米复合薄膜,研究了Si含量对薄膜硬度的影响及高温退火对薄膜晶粒尺寸及其硬度的影响.结果表明:薄膜的硬度随着Si含量的增加有先增大后减小的趋势,最大硬度可达70 GPa以上.薄膜表现出了较高的热稳定性能,对于晶粒尺寸在4 nm以下的薄膜,Ti-Si-N薄膜的纳米结构和硬度可以维持在1000℃以上.沉积态薄膜的晶粒尺寸是影响薄膜再结晶温度的主要因素.薄膜的高热稳定性是由于沉积过程中发生的自发调幅分解形成了纳米复合结构,偏析使得纳米晶晶界具有强的热力学稳定性.     

中频脉冲非平衡磁控溅射技术制备类金刚石膜的结构与性能

利用中频脉冲非平衡磁控溅射技术在载玻片上制备了类金刚石(DLC)薄膜,研究了沉积气压对薄膜厚度、微观结构、机械性能和光学性能的影响。厚度测试结果表明,DLC膜厚度随沉积气压的增加而增加。X射线光电子能谱测试结果表明,当沉积气压由0.18Pa增加到1.50Pa时,DLC薄膜中sp~3杂化碳含量随沉积气压的增加而减少。纳米压痕和椭偏仪测试结果表明,DLC膜的纳米硬度、折射率均随沉积气压的增加而减小。采用浅注入模型分析了沉积气压对薄膜生长和键合结构的影响。以上结果表明,沉积气压对DLC膜的厚度、sp~3杂化碳含量、机械与光学性能具有较大的影响。     

多弧离子镀制备硬质梯度薄膜技术

介绍了多弧离子镀在金属陶瓷表面沉积硬质梯度薄膜的技术,用X射线衍射法对表面形成的薄膜进行了物相分析,并对材料的金相显微组织、显微硬度、抗弯强度以及膜与基体的结合力进行了测试和分析.结果表明:多弧离子镀处理能在金属陶瓷表面形成硬质梯度薄膜,膜与基体的结合力良好,表面硬度大大提高,而材料的抗弯强度却没有发生变化.     

直流反应磁控溅射在3003铝箔表面制备薄膜的研究

为有效提高3003铝箔表面光泽度、比面积及强硬度,采用直流反应磁控溅射的方法.在一定溅射参数条件下,选用高纯钼靶和钛靶对3003铝箔进行溅射实验,分别在铝箔表面主要沉积出AlMo3、Al3Mo薄膜和TiAl、(Ti,Al)N薄膜,利用X射线衍射、扫描电镜分析相组成及微观组织结构,并测试了显微硬度和薄膜厚度,实验结果表明:制备出的AlMo3、Al3Mo薄膜和TiAl薄膜结晶良好,与基底结合良好,铝箔表面美观漂亮、硬度增高及比表面积得到一定提高.     

工艺参数对Ni-W-P-CeO2-SiO2纳米复合薄膜材料微观组织及性能的影响

通过Ni,W,P和CeO2,SiO2纳米颗粒的脉冲共沉积,在普通碳钢表面制备了Ni-W-P-CeO2-SiO2纳米复合薄膜材料,研究了电解液pH值和电解液温度对纳米复合薄膜材料电沉积过程的影响,采用化学组成、沉积速率、显微硬度和微观组织进行表征.结果表明:增加电解液pH值和电解液温度,纳米复合材料晶粒得到细化,沉积速率和显微硬度增加.当电解液pH值为5.5、电解液温度为60℃时,纳米复合薄膜材料晶粒细小,沉积速率最快,为28.87μm/h,显微硬度最高,为Hv673,若继续增加电解液pH值和电解液温度,沉积速率和显微硬度又开始降低.     

Effects of silicon nitride interlayer on phase transformation and adhesion of TiNi films

TiNi films with different Ti/Ni ratios were deposited on Si substrates with and without silicon nitride interlayer. Near-equiatomic TiNi films were found to have the lowest residual stress and the highest recovery stress regardless of the existence of silicon nitride interlayer. The addition of silicon nitride interlayer between film and Si substrate did not cause much change in phase transformation behavior as well as adhesion properties. X-ray photoelectron spectroscopy (XPS) analysis revealed that there is significant interdiffusion of elements and formation of Ti-N and Si-Si bonds at TiNi film/silicon nitride interface. Scratch test results showed that adhesion between the TiNi film and substrate was slightly improved with the increase of Ti content in TiNi films.     

反应溅射Ti-Si-N纳米晶复合薄膜的微结构与力学性能

采用Ar、N2 和SiH4混合气体反应溅射制备了一系列不同Si含量的Ti Si N复合膜 ,用EDS、XRD、TEM和微力学探针研究了复合膜的微结构和力学性能。结果表明 ,通过控制混合气体中SiH4分压可以方便地获得不同Si含量的Ti Si N复合膜。当Si含量为 (4～ 9)at%时 ,复合膜得到强化 ,最高硬度和弹性模量分别为 34 2GPa和 398GPa。进一步增加Si含量 ,复合膜的力学性能逐步降低。微结构研究发现 ,高硬度的Ti Si N复合膜呈现Si3 N4界面相分隔TiN纳米晶的微结构特征 ,其中TiN纳米晶的直径约为 2 0nm ,Si3 N4界面相的厚度小于 1nm。     

Si-N-O薄膜结构对薄膜血液相容性的影响

采用非平衡磁控溅射(UBMS450)法在(100)单晶硅表面制备Si-N-O薄膜.利用X射线光电子能谱(XPS)表征薄膜的成分结构;用血小板粘附试验表征薄膜结构对薄膜血液相容性的影响.研究结果表明,以无机Si为主的Si-N-O薄膜,其血液相容性较差;键合少量O的Si3N4薄膜,其血液相容性较佳.Si-N-O薄膜中N含量和O含量的变化,是导致薄膜结构变化的重要因素.     

Single and multiple doping effects of silicon–boron and fluorine on ZnO thin films deposited with sol–gel spin coating technique

Undoped, Si and B single doped, Si–B co-doped and Si–B–F triple doped ZnO thin films were grown by sol–gel spin coating method. Effects of these doping elements on microstructural, morphological and optical properties were investigated. X-ray diffraction studies showed that all films had hexagonal wurtzite structure. Although Si doping increased crystallinity of ZnO, single boron doping, Si–B co-doping and Si–B–F triple doping gave rise to a decreasing in crystallinity. Scanning electron microscope micrographs indicated that the grain size and morphological characters of ZnO depended on doping element type and their concentrations. The micrographs also demonstrated that Si doping deteriorated grain size and their distribution on film surface of ZnO structure. Although single B, doubly Si–B and triple Si–B–F doping at low contents improved grain distribution and film morphology, when their content increased, film morphology started to deteriorate. Optical band gap value of undoped film increased with Si doping irrespective of Si doping content. Although single B, doubly Si–B and triple Si–B–F doping at low contents caused an increase in optical band gap of undoped ZnO, more doping content brought about a decrease in optical band gap. From the optical parameters such as absorption coefficient, the Urbach energy values of the films were calculated by using ln α vs. photon energy graphs. In generally, Urbach energies of the films changed reversely with the band gap energies of the films.     

溅射靶功率对氮化碳薄膜结构的影响

利用双放电腔微波ECR等离子体增强非平衡磁控溅射技术,在Si(100)上制备氮化碳薄膜,并对薄膜进行了拉曼(Raman)、原子力显微镜(AFM)、X射线光电子谱(XPS)等结构的表征.发现溅射靶功率对制膜工艺、薄膜的结构和表面形貌产生很大影响.随着溅射靶功率的增大,薄膜的沉积速率减小,表面粗糙度增大,薄膜结构中的sp2含量增加.     

Preferred growth of epitaxial TiN thin film on silicon substrate by pulsed laser deposition

Epitaxial TiN thin films on silicon substrates were prepared by pulsed excimer laser (KrF, 34 ns) ablation of a hot-pressed TiN target in nitrogen gas atmosphere. X-ray diffraction (XRD) showed that the preferred orientations of TiN thin films did not change with substrate temperatures, nitrogen gas pressure and film thickness; however, they did change with the orientations of substrates. The epitaxial orientation relationships between high-quality epitaxial TiN thin films and silicon substrates [2 4 2] TiN [2 4 2] Si, (1 1 1) TiN(1 1 1) Si and [3 1 1] TiN [3 1 1] Si, (1 0 0) TiN(1 0 0) Si. The full-width at half-maximum (FWHM) of the rocking curve of XRD and the minimum channelling yield of Rutherford backscattered spectroscopy (RBS) of the epitaxial TiN thin film were estimated to be 0.3 ° and 7.3%, respectively, indicating excellent crystalline quality of the grown film. X-ray photoelectron spectroscopy confirmed that the binding energies of Ti 2p 3/2 and N 1s core levels in epitaxial thin film were 455.2 and 397.1 eV, respectively, corresponding to those of TiN bulk. By calibrating the RBS spectra, the chemical composition of TiN thin films was found to be titanium-rich. The typical surface roughness of TiN thin film observed by scanning probe microscopy was about 1.5 nm. © 1998 Chapman & Hall     

（Ba0.6Sr0．4）Ti1-xZnxO3薄膜的介电调谐性能

利用溶胶-凝胶法在Pt／TiO2/SiO2/Si衬底上制备了（Ba0．6Sr0．4）Ti1-xZnxO3（BSTZ）薄膜,用X射线衍射和扫描电镜分析测定了BSTZ的微结构和薄膜的表面形貌,研究Zn掺杂量对其介电调谐性能的影响,结果表明,随Zn含量的增加BSTZ物相无明显变化,其介电常数、调谐量先增加后降低,但介电损耗却先降低后增加。在室温1MHz下,1．5m01％Zn掺杂BSTZ薄膜有最大的调谐量54．26％;2．5mol％Zn掺杂BSTZ薄膜有最低的介电损耗0．0148和最大的优值因子30．3。     

不同电极形式对掺镧钛酸铅铁电薄膜的介电性能的影响

采用射频磁控溅射技术在Si(100) 基底和Pt/Ti/SiO2/Si(100)基底上生长了掺镧钛酸铅[(Pb0.9,La0.1)TiO3, PLT10]铁电薄膜.用X射线衍射技术(XRD)研究了PLT10薄膜结晶性能.使用光刻工艺在Si(100) 基底的PLT10薄膜上制备了叉指电极,测试了PLT10薄膜的介电性能.在室温下,测试频率为1kHz时,PLT10薄膜的介电常数为386.而采用相同工艺条件制备的具有平行电极结构的PLT10薄膜, 其介电常数为365.但利用叉指电极测试的PLT10薄膜的介电常数和介电损耗随频率的下降比利用平行电极测试的PLT10薄膜的快些.这是因为叉指电极结构引入了更多的界面态影响的缘故.     

Structure and optical properties of Zr1−xSixN thin films on sapphire

A series of zirconium silicon nitride (Zr_1−xSi_xN) thin films were grown on r-plane sapphire substrates using reactive RF magnetron co-sputtering of Zr and Si targets in a N₂/Ar plasma. X-ray diffraction pole figure analysis, X-ray reflectivity, X-ray photoelectron spectroscopy (XPS), optical microscopy, and optical absorption spectroscopy were used to characterize the film stoichiometries and structures after growth at 200 °C and post-deposition annealing up to 1000 °C in ultra-high vacuum. The atomically clean r-plane sapphire substrates induce high quality (100) heteroepitaxy of ZrN films rather than the (111) orientation observed on steel and silicon substrates, but the addition of Si yields amorphous films at the 200 °C growth temperature. After the annealing treatment, films with Si content x < 0.15 have compressive stress and crystallize into a polycrystalline structure with (100) fiber texture. For x > 0.15, the films are amorphous and remain so even after ultra-high vacuum annealing at 1000 °C. XPS spectra indicate that the bonding changes from covalent to more ionic in character as Si―N bonds form instead of Zr―N bonds. X-ray reflectivity, atomic force microscopy (AFM) and optical microscopy data reveal that after post-deposition annealing the 100 nm thick films have an average roughness < 2 nm, except for Si content near x = 0.15 corresponding to where the film becomes amorphous rather than being polycrystalline. At this stoichiometry, evidence was found for regions of film delamination and hillock formation, which is presumably driven by strain at the interface between the film and sapphire substrate. UV-visible absorption spectra also were found to depend on the film stoichiometry. For the amorphous Si-rich films (x > 0.15), the optical band gap increases with Si content, whereas for Zr-rich films (x < 0.15), there is no band gap and the films are highly conductive.     

Crystalline β-C3N4 synthesized by MPCVD

Carbon nitride films were grown on Si and Pt substrates by microwave plasma chemical vapor deposition (MPCVD) method. Scanning electron microscope (SEM) observations show that the films deposited on Si substrates consisted of densely populated hexagonal crystalline rods. Energy dispersive X-ray (EDX) analyses show that N/C ratios of the rods were in the range of 1.0 to 2.0 depending on deposition condition. X-ray diffraction experiments show that the films consisted of crystalline phase -C₃N₄. Comparison with films grown on Pt substrate show that the main X-ray diffraction peaks of -C₃N₄ are existed in films deposited on both substrate. XPS study showed that carbon and nitride atoms are covalent bounded to each other. IR results show that the film is predominantly C-N bonded. Raman measurement showed characteristic peaks of -C₃N₄ in the low wave number region. Temperature dependent growth experiments show that the amount of Si₃N₄ in the films grown on Si substrates can be significantly reduced to negligible amount by controlling the substrate temperature.