后天抑制剂取向硅钢析出物的研究

采用"后天抑制剂法"制备取向硅钢,通过TEM研究热轧、常化、脱C和渗N阶段析出物的类型和分布。结果表明,热轧、常化和脱C板中的析出物主要是AlN颗粒,AlN颗粒在热轧、常化和脱C板中分布密度低;渗N后钢中形成非晶态Si3N4颗粒,非晶态Si3N4颗粒有多边形大块状和规则小四方形2种形貌,多边形大块状Si3N4颗粒分布在晶界,规则小四方形Si3N4颗粒主要分布在晶内。     

氮化硅薄膜材料的表面结构和热稳定性研究

研究了三种方法制备的氮化硅薄膜的组成、表面结构、热氧化稳定性以及抗离子束损伤等性能。研究发现APCVD法制备氮化硅薄膜的Si3N4含量最高，PRSD法制备的薄膜次之，而PECVD法制备的薄膜Si3N4含量最低。在PRSD薄膜中没有N－H键存在，仅有少量的Si－H键存在，薄膜的热氧化稳定性和抗离子束损伤性能最好。APCVD薄膜中含有少量的N－H和Si－H键，虽然膜层的热稳定性很好，但由于膜层具有较多的缺陷，因此其抗氧化性较差，抗离子束损伤性能也不好。对于PECVD薄膜，由于其形成温度较低，膜层中含有大量的N－H和Si－H键，因此膜层的热稳定性和抗离子束损伤性能最差。此外，还发现XPS获得的N／Si原子比和膜层的真实成分校一致，而RBS和AES由于离子束损伤效应，其结果偏低。氮化硅薄膜热稳定性差和离子束损伤的本质均因氯化硅的脱氮分解。热氧化的本质是膜层中自由硅和气氛中残余氧的氧化反应。     

金属有机化学气相沉积法生长AlN/Si结构界面的研究

采用金属有机化学气相沉积法在Si(111)衬底上生长了AlN外延层.高分辨透射电子显微镜显示在AlN/Si界面处存在非晶层,俄歇电子能谱测试表明Si有很强的扩散,拉曼光谱测试表明存在Si-N键,另外光电子能谱分析表明非晶层中存在Si3N4.研究认为MOCVD高温生长造成Si的大量扩散是非晶层存在的主要原因,同时非晶Si3N4层也将促使AlN层呈岛状生长.     

低应力Si_3N_4介质膜的制备工艺优化

低应力Si3N4介质膜对于制作微结构传感器是非常重要的。本文通过采用正交试验设计,优化出Si3N4介质膜制备的低应力工艺参数,并给出了Si3N4薄膜应力的测试方法和测试结果。     

Si_3N_4球表面DLC膜在干摩擦条件下的摩擦学性能分析

采用非平衡磁控溅射技术在Si3N4球及高速钢基体上制备了类金刚石(DLC)膜。采用UMT-II型球盘式摩擦磨损试验机分别考察了Si3N4球、镀DLC膜Si3N4球及GCr15球的摩擦学性能,并分析了不同滑动速度和载荷下Si3N4球表面DLC膜的摩擦学性能。研究结果表明:Si3N4球的摩擦系数及磨损率约为GCr15球的一半,但因Si3N4球脆性较大,在摩擦过程中摩擦接触表面容易剥落;Si3N4球表面镀DLC膜能有效地改善Si3N4球脆性大的弱点,并具有良好的减摩作用;Si3N4球表面DLC膜所组成摩擦副的平均摩擦系数随着载荷的增加而增大;随着速度的增加摩擦副的摩擦系数先增大而后减小,滑动速度对摩擦副摩擦系数的影响比载荷明显。实验结果表明Si3N4球表面镀DLC膜适合于高速轻载的工况。     

反应溅射HfC/Si3N4纳米多层膜的微结构与力学性能

通过反应磁控溅射制备了一系列不同Si3N4层厚的HfC/Si3N4纳米多层膜,采用X射线光电子能谱、X射线衍射、扫描电子显微镜和微力学探针表征了多层膜的微结构、硬度与弹性模量,研究了Si3N4层厚度变化对纳米多层膜微结构与力学性能的影响。结果表明,溅射的Si3N4粒子不与C2H2气体反应,因NaCl结构HfC晶体调制层的模板效应,溅射态为非晶的Si3N4层在厚度小于约1 nm时被强制晶化,并与HfC晶体层形成共格外延生长结构,多层膜呈现强烈的(111)择优取向柱状晶,其硬度和弹性模量显著上升,最高值分别达到38.2 GPa和343 GPa。进一步增加Si3N4层的厚度后,Si3N4层转变为以非晶态生长,多层膜的共格外延生长结构受到破坏,其硬度和模量也相应降低。     

自蔓延燃烧合成β-Si3N4棒晶

采用自蔓延高温合成（SHS），在高压氮气中成功地合成了β－Si3N4棒晶，研究了中不同量Y2O3对自蔓延燃烧合成β－Si3N4棒晶长径比的影响。结果表明，Y2O3添加量有一个最佳范围，当Y2O3的添加量在2wt％－5wt％时，棒晶生长均匀，长径比约为8．通过铜坩埚吸热淬火的方法，观察到β－Si3N4棒晶不同生长阶段的显微形貌，从而推测其生长机理为VLS和VS两种机理协同作用的结果。本文对β－Si3N4棒晶生长的反应历程也进行了阐述。     

TiN/Si3N4纳米多层膜的生长结构与超硬效应

采用磁控溅射方法制备了一系列不同Si3N4和TiN层厚的TiN/Si3N4纳米多层膜,采用X射线衍射、高分辨电子显微分析和微力学探针表征了薄膜的微结构和力学性能,研究了Si3N4和TiN层厚对多层膜生长结构和力学性能的影响.结果表明:当Si3N4层厚小于0.7 nm时,原为非晶的Si3N4在TiN的模板作用下晶化并与之形成共格外延生长的柱状晶,使TiN/Si3N4多层膜产生硬度和弹性模量异常升高的超硬效应.最高硬度和弹性模量分别为34.0 GPa和353.5 GPa.当其厚度大于1.3 nm时,Si3N4呈现非晶态,阻断了TiN的外延生长,多层膜的力学性能明显降低.此外,TiN层厚的增加也会对TiN/Si3N4多层膜的生长结构和力学性能造成影响,随着TiN层厚的增加,多层膜的硬度和弹性模量缓慢下降.     

ADC12铝合金表面氮化铝(AlN)涂层的制备及其耐磨性能研究

为了提高ADC12铝合金材料的耐磨性能，利用多功能离子渗氮炉在ADC12铝合金表面进行离子渗氮，制备氮化铝(AlN)涂层。通过X射线衍射仪、扫描电子显微镜对表面AlN涂层的相结构与微观形貌进行表征；利用WS-2005涂层附着力自动划痕仪、WTM-2E可控气氛微型摩擦磨损试验仪和3D光学显微镜研究AlN涂层与基体的膜基结合力、摩擦系数、比磨损率和摩擦磨损机理。结果显示：表面AlN涂层的相结构为面心立方，没有发现有Al₂O₃衍射峰存在。随着渗氮时间的延长和渗氮温度的升高，表面AlN涂层的厚度逐渐增大，膜基结合力先增大再减小，在510℃、4 h时膜基结合力最大，为56.60 N。相对于基体来说，AlN涂层样品在负载1 N、进行摩擦磨损试验10 min后，摩擦系数变小，比磨损率降低，表面AlN涂层厚度越厚，减缓磨损效果越明显。ADC12铝合金表面离子渗氮所得氮化铝(AlN)涂层具有优异的耐磨损性能。     

纳米陶瓷颗粒填充PTFE基复合材料的干摩擦磨损性能

利用MM-200型环-块摩擦磨损试验机研究了纳米陶瓷颗粒SiC、Si3N4、AlN和TiN对聚四氟乙烯(PTFE)复合材料在干摩擦条件下与45#钢对磨时的摩擦磨损性能的影响,借助于扫描电子显微镜观察分析了试样磨损表面形貌,并探讨了磨损机理。结果表明:添加纳米TiN减少了PTFE的摩擦系数,而添加纳米SiC、Si3N4增大了PTFE的摩擦系数。与纯PTFE相比,PTFE复合材料的耐磨性能显著提高,其中以纳米AlN的减磨效果最好,纳米Si3N4的减磨效果最差。纯PTFE的磨损机制主要表现为粘着磨损和疲劳磨损,而纳米粒子填充PTFE基复合材料的磨损机制主要表现为不同程度的粘着磨损、犁沟效应和塑性变形特征。     

Si3N4薄膜的成分与结构研究

通过PECVD方法,在Si基体表面制备了Si3N4薄膜,给出了XRD、TEM、AES、DPS的分析结果,表明Si3N4是非晶态结构,薄膜的主要成分是Si3N4,SEM分析结果显示Si3N4薄膜与基体材料的结合强度高,薄膜致密性好.     

Interracial Bonding Strength of TiN Film Coated on Si3N4 Ceramic Substrate

The fraction of TiN/Si3N4 in the cross section was observed with scanning electric microscope （SEM）, and residual stresses of TiN coated on the surface of Si3N4 ceramic were measured with X-ray diffraction （XRD）.The hardness of TiN film was measured, and bonding strength of TiN film coated on Si3N4 substrate was measured by scratching method. The formed mechanism of residual stress and the failure mechanism of the bonding interface in the film were analyzed, and the adhesion mechanism of TiN film was investigated preliminarily. The results show that residual stresses of TiN film are all behaved as compressive stress, and TiN film is represented smoothly with brittle fracture, which is closely bonded with Si3N4 substrate. TiN film has high hardness and bonding strength of about 500 MPa, which could satisfy usage requests of the surface of cutting Si3N4 ceramic.     

Interfacial Bonding Strength of TiN Film Coated on Si3N4 Ceramic Substrate

The fraction of TiN/Si3N4 in the cross section was observed with scanning electric microscope (SEM), and residual stresses of TiN coated on the surface of Si3N4 ceramic were measured with X-ray diffraction (XRD).The hardness of TiN film was measured, and bonding strength of TiN film coated on Si3N4 substrate was measured by scratching method. The formed mechanism of residual stress and the failure mechanism of the bonding interface in the film were analyzed, and the adhesion mechanism of TiN film was investigated preliminarily. The results show that residual stresses of TiN film are all behaved as compressive stress, and TiN film is represented smoothly with brittle fracture, which is closely bonded with Si3N4 substrate. TiN film has high hardness and bonding strength of about 500 MPa, which could satisfy usage requests of the surface of cutting Si3N4 ceramic.     

Effect of chain conformation on micro-mechanical behaviour of MEH–PPV thin film

The morphology, photoluminescent properties and micro-mechanical character of poly[2-methoxy-5-(2′-ethylhexyloxy)-p-phenylene vinylene] (MEH–PPV) thin films prepared from toluene (T film) and chloroform (C film) were studied by transmission electron microscopy (TEM), absorption, photoluminescence spectrophotometry and nanoindentation test. The morphological feature of worm-like entities which appeared in T film was ~10–20 nm in length and 3–5 nm in width. The C film displayed the continuous cotton fibre-shaped morphology. In contrast with C film, the band-edge absorption and maximum emission for T film shifted to the longer wavelength. An analysis from TEM photograph, absorption and photoluminescence spectra indicated that different chain conformation presented in these two kinds of films. The nanoindentation test showed that the elastic modulus and indentation hardness of T film under the same experimental parameter (load: 50–200 μN, loading rate: 20 μN/s and holding time: 20 s) decreased by 33·3 ± 0·3 and 8·9 ± 0·5%, respectively comparing with C film. In addition, critical bending radius of these two films based on the flexible base was also evaluated from the obtained experimental results.     

Si3N4薄膜的表面微观特性

利用偏心静电单探针诊断了反应室内的等离子体密度的空间分布;在不同的工艺条件下制备了Si3N4薄膜,由STM和Telystep-Hobbso轮廓仪研究了ECR－PECVD制备的Si3N4薄膜的表面微观特性,分析了沉积温度对ECR－PECVD制备的Si3N4薄膜表面平整度特性影响的物理机理;结果表明ECR－PECVD制备的薄膜是一种表面均匀致密的纳米Si3N4薄膜。     

微波ECR-PCVD技术制备Si3 N4薄膜的研究与应用

受电子器件芯片铝电极耐温性能的限制和钝化膜沉积工艺中高能粒子对芯片辐射损伤等因素的影响，一般的沉积方法难以用到要求较高的浅结器件的钝化工艺中。微波ECR-PCVD技术没有高能粒子对芯片的辐射损伤，可以在较低的温度条件下沉积出均匀致密、性能优良的Si_3N_4薄膜，因而成为微电子器件沉积钝化膜的最佳工艺。     

Properties of silicon nitride films prepared by plasma-enhanced chemical vapour deposition of SiH4-N2 mixtures

The refractive indices and IR absorption spectra are measured for silicon nitride films plasma deposited from SiH₄-N₂-H₂ gas mixtures. The composition of the film (N:Si ratio) is derived from the value of the refractive index and the concentration of bonded hydrogen as Si-H and N-H in the film is estimated from the absorption intensities in the IR spectrum. The optimum deposition conditions for giving excellent insulating silicon nitride films are confirmed to be same as the conditions for giving films with stoichoimetric composition and the lowest amount of incorporated hydrogen.     

SiC和Si_3N_4粉体的太赫兹时域光谱研究

采用太赫兹时域光谱装置测试SiC和Si3N4粉体在0.4～2.4 THz的透射光谱,研究SiC和Si3N4粉体对太赫兹波的吸收性能与其电导率的关系,分析SiC和Si3N4粉体对太赫兹波的散射特性。结果表明,SiC是一种半导体材料,其内部含有较多可以自由移动的载流子,对太赫兹波的吸收较强;Si3N4是绝缘性很好的材料,对太赫兹波的吸收很小;SiC和Si3N4粉体对太赫兹波的散射作用属于瑞利散射,但是测试波长比粉体粒径大得多,散射效果不明显。     

氮化碳薄膜的结构与特性

采用射频等离子体增强化学气相沉积（ＣＶＤ）＋负偏压热丝辅助方法直接在Ｓｉ（１００）衬底上制备了多晶Ｃ_３Ｎ_４薄膜．Ｘ射线衍射测试表明,薄膜同时含有α－和β-Ｃ_３Ｎ_４晶相以及未知结构,没有观测到石墨衍射峰．利用扫描电子显微镜观测到线度约２μｍ、横截面为六边形的β－Ｃ_３Ｎ_４晶粒．纳米压痕法测得薄膜的硬度达７２．６６ ＧＰａ．     

纳米SiC纤维改性短切碳纤维增强Si_3N_4陶瓷介电响应及吸波性能

以甲基三氯硅烷为原料,采用催化化学气相沉积(CCVD)工艺在短切碳纤维(C_(fd))表面制备了纳米SiC纤维(nano SiC_f)改性层,并采用凝胶注模-无压烧结工艺制备了nano SiC_f-C_(fd)/Si_3N_4和C_(fd)/Si_3N_4复合材料。使用矢量网络分析仪研究了nano SiC_f-C_(fd)和C_(fd)对Si_3N_4陶瓷在X波段(8.2~12.4GHz)的介电响应和吸波性能的影响。结果表明:nano SiC_f-C_(fd)/Si_3N_4和C_(fd)/Si_3N_4复合材料的复介电常数和介电损耗角正切值(tanδ)均随纤维添加量增加而增大;相同纤维含量时,nano SiC_f-C_(fd)/Si_3N_4复合材料的介电常数实部比C_(fd)/Si_3N_4复合材料有所降低,但损耗角正切升高。反射损耗结果表明:nano SiC_f-C_(fd)/Si_3N_4复合材料拥有更优的电磁波吸收效果。nano SiC_f-C_(fd)含量为2wt%、d=2.5mm时,出现最大吸收峰-14.95dB,反射损耗优于-5dB,波段频宽达3.5GHz。nano SiC_f界面改性能有效提高C_(fd)/Si_3N_4复合材料的吸波性能。