玻璃微球表面辉光等离子体聚合物涂层的热稳定性研究

采用辉光放电聚合技术,在不同工作压强条件下在直径为350—400 μm,厚度为2.5—3 μm的玻璃微球上制备了辉光放电聚合物 (GDP)涂层,并对玻璃/GDP微球模拟充气过程进行了热稳定性实验.利用傅里叶变换红外光谱仪、元素分析仪、热重法、体视显微镜和X射线照相技术对GDP涂层的内部结构及其化学键、热稳定性、微球形貌和厚度进行了表征.结果表明:GDP涂层中的碳氢比、不饱和键和C C含量随着制备压强的增大而减小,低压的热稳定性较好,GDP涂层与玻璃微球的结合力提高,流变、起泡和脱层现象也得到明显改善.微球 关键词： 玻璃微球 GDP涂层 热稳定性 结合力     

Cu空心微球的精密连接技术

以Cu作为代用材料,通过分解实验方法,研究了扩散连接各工艺条件对靶丸参数的影响关系,获得适宜的工艺参数(温度小于600℃,压强小于6 MPa,时间60 min)。据此,实际连接Cu半球并制备出Cu空心微球。采用白光干涉仪、扫描电子显微镜、微米X射线断层扫描机等仪器对样品进行测试,结果显示连接界面无明显缺陷,内表面粗糙度小于50 nm,内球面直径差值小于20μm,连接强度满足机械加工要求。     

侧照明实验用平面调制微靶的制备及参数测量

 介绍了用于侧照明实验研究瑞利-泰勒流体力学不稳定性(Rayleigh-Taylor instability)实验的聚苯乙烯和铝平面调制微靶的制备工艺。通过图形转移，靶型切割和装配工艺的控制，结合靶参数测量，获得了厚度在几十μm、表面具有波长50 μm和55 μm、振幅从几到几十μm、微靶宽度约为200 μm、剖面正弦调制图形清晰的两种靶型。     

4H-SiC压力敏感膜片的低损伤飞秒激光加工

采用飞秒激光加工4H-SiC压力敏感膜片,研究了飞秒激光深度方向步进间距、扫描路径方向、单脉冲能量、扫描线间距等参数对4H-SiC烧蚀形貌和烧蚀速率的影响。实验结果表明,飞秒激光加工4H-SiC样品表面孔洞的形成主要与激光诱导微沟槽的重叠有关,激光能量分布更均匀能够有效减少4H-SiC被烧蚀表面的激光诱导微沟槽的数量,增大激光扫描路径与激光偏振方向的夹角能够有效降低激光诱导微沟槽的重叠概率,从而抑制孔洞的形成。采用优化后的飞秒激光加工工艺参数,制备出直径为1 600μm、厚度为100μm的4H-SiC压力敏感膜片。所制备的4H-SiC压力敏感膜片表面无明显孔洞,边缘过烧蚀深度小于10μm,实现了4H-SiC压力敏感膜片的低损伤飞秒激光加工。     

类金刚石微球的高温高压制备

通过对化学气相沉积方法获得的碳膜微球进行高温高压处理,在约8GPa、1 600℃的条件下制备了类金刚石异质实心微球样品,芯轴为钼球。根据金刚石和钼的体积随压力及温度的变化规律,设计并优化了样品制备的温度-压力路径,以降低因类金刚石膜层与钼球的体弹模量及热膨胀系数差异而导致的残余应力。拉曼光谱测试结果表明,样品膜层具有明显的1 332cm~(-1)金刚石特征峰,高温高压有效地消除了存在于初始碳膜微球中的反式聚乙炔,同时降低了膜中残余应力,产生了有利于提高类金刚石膜强度的压应力;扫描电子显微镜测试结果表明,样品球形度良好,平均直径约2mm,类金刚石膜表面平均晶粒尺寸约为100nm,膜厚约为20μm;原子力显微镜测试结果表明,类金刚石膜层的表面粗糙度为647nm。     

跳动模式对微球CH涂层表面粗糙度的影响

 采用低压等离子体化学气相沉积方法（LPPCVD）,结合反弹盘系统制备了微球CH涂层,研究了跳动模式对微球CH涂层表面形貌的影响。利用光学显微镜和扫描电镜(SEM)对微球涂层表面形貌进行了分析;利用原子力显微镜（AFM）测定了微球CH涂层表面均方根粗糙度（RMS）并对球形度进行了表征;利用X光照相技术对同心度进行了表征。结果表明：采用间歇跳动模式可有效改善微球CH涂层的表面形貌,降低中高模数的粗糙度。在间歇跳动模式下,减小占空比,可使CH涂层的表面粗糙度得到进一步降低。在占空比为1/4的间歇跳动模式下制备的厚度为30 mm的CH涂层,其表面均方根粗糙度低于30 nm,碳氢-聚苯乙烯（CH-PS）微球的球形度与同心度均优于99%。     

导流型热蒸发沉积制备微球表面聚酰胺酸涂层

 在自行研制的导流型热蒸发沉积装置上开展了微球表面聚酰胺酸（PAA）涂层制备工艺研究。探讨了单体原料处理和改变升温过程对沉积速率的影响。两种单体分别采用两个相互独立的蒸发源加热蒸发,使用两个晶振膜厚测量探头,通过对膜厚探头、样品盘和导流管端头三者的空间位置和对称关系的调整和实验标定,实现了两种单体近似等化学计量比的沉积。采用间歇性压电振动或敲击配合样品盘的旋转作为微球运动的激励方式,在聚-α-甲基苯乙烯（PAMS）微球上制备出均匀的表面质量好的PAA涂层。     

电沉积枝状微针翅铜的池沸腾传热特性

微纳表面在沸腾传热领域得到广泛的关注和研究。本文通过电化学沉积方法制备了枝状微针翅铜表面,并测试了其池沸腾换热特性。实验表明,在较低热流密度时,样品厚度对沸腾强化效果的影响不明显;但热流密度较大时,沸腾强化效果随样品厚度的减小而增大,其中厚度为110μm的样品在热流密度为140 W·cm~(-2)时,有最大传热系数143kW·m~(-2)·℃~(-1)。CHF随样品厚度增大而增大,厚度为460μm时的CHF约250 W·cm~(-2)。     

球壳结构金阴极及其X射线光电发射特性

以聚苯乙烯微球为模板, 采用种子-生长法在聚苯乙烯微球表面镀覆金球壳层, 以不同浓度旋涂分散在阴极衬底上, 热处理去除聚苯乙烯模板, 初步制备出表面具有金球壳结构的反射式金阴极样品, 通过金相显微镜和扫描电镜研究其表面形貌, 结果表明: 阴极表面球壳的直径约为10 μm, 高温去除聚苯乙烯微球模板后金沉积层具有良好的自支撑性, 球壳厚度约70-90 nm, 球壳表面主要由30-60 nm的晶粒突起组成. X射线光电发射测试表明, 反射式球壳结构阴极在200-1500 eV波段光电效率相对于平面薄膜阴极有明显提升, 其量子效率可达到平面阴极的3倍以上, 理论分析表明: 球壳结构阴极特殊的表面结构引起光电发射面积的增大和表面势垒的降低, 是阴极光电发射效率提高的主要原因.     

组装条件对涂布法制备SiO2结构色涂层光谱性质影响研究

为了实现结构色涂层在纸张表面的快速制备，研究不同组装条件对SiO₂结构色涂层呈色效果的影响，采用快速涂布的方法，在纸张表面制备出了大面积且具有随角异色特性的结构色涂层。探讨SiO₂微球粒径、分散液浓度及涂布次数等因素对结构色涂层光学特性的影响，通过优化自组装条件和分析周期性结构构筑类型，阐明快速涂布法构建的SiO₂微球在激光打标纸上的自组装过程及结构色呈色机理。应用数码相机、3D激光共聚焦形貌测量显微镜等仪器对样品的颜色外观和微观结构进行测量，表征样品的呈色性能及表面结构。使用X-Rite MA68Ⅱ多角度分光光度仪及光纤光谱仪测量反射光谱，进而用CIEL*a*b*色度值对制备的结构色涂层的光学性能进行分析。结果表明，通过快速涂布自组装法制备所得的结构色涂层，SiO₂微球粒径尺度对样品色调影响显著，随着微球粒径的增加，反射光谱中心波长发生红移，且该涂层有角度依赖特性，当固定入射角度为45°时，随着探测方向与镜面反射方向夹角的增大，中心波长发生红移；微球溶液的浓度可以调控结构色涂层反射光谱曲线的半高宽及反射率峰值，进而影响样品的亮度和彩度，而对于光子带隙的位置无明显影响。微球浓度为4%时，样品表面呈现出基材本身的黑色，微球浓度为8%时，200，220和250 nm粒径的样品表面分别可以呈现彩度较低的蓝色、绿色、黄色，微球浓度增加到10%时，纸张表面的结构色涂层彩度提高，色调不变；随着涂布次数的增加，反射光谱曲线的半高宽变窄，且反射峰位发生蓝移，涂布次数达到3次时，反射峰位最接近于根据布拉格定律计算出的理论值，但涂布次数的增加也使得结构色涂层表面产生白色的不均匀现象。     

Preparation and in vitro characterization of aerosol-deposited hydroxyapatite coatings with different surface roughnesses

Hydroxyapatite (HA) coatings with different surface roughnesses were deposited on a Ti substrate via aerosol deposition (AD). The effect of the surface roughness on the cellular response to the coating was investigated. The surface roughness was controlled by manipulating the particle size distribution of the raw powder used for deposition and by varying the coating thickness. The coatings obtained from the 1100 °C-heated powder exhibited relatively smooth surfaces, whereas those fabricated using the 1050 °C-heated powder had network-structured rough surfaces with large surface areas and were superior in terms of their adhesion strengths and in vitro cell responses. The surface roughness (R_a) values of the coatings fabricated using the 1050 °C-heated powder increased from approximately 0.65 to 1.03 μm as the coating thickness increased to 10 μm. The coatings with a rough surface had good adhesion to the Ti substrate, exhibiting high adhesion strengths ranging from 37.6 to 29.5 MPa, depending on the coating thickness. The optimum biological performance was observed for the 5 μm-thick HA coating with an intermediate surface roughness value of 0.82 μm.     

Fabrication and electrical properties of metal-coated acrylate rubber microspheres by electroless plating

Electroless copper plating on micron-scale acrylate rubber (ACM) microspheres was studied. The core-shell structured Cu-coated ACM microspheres with high conductivity and low density were fabricated by introducing a reaction control method. Via multi-times activating treatment, the acrylate rubber (ACM) microspheres were implanted with more Ag catalytic active centers on the surfaces to promote the formation of coatings. The surface-coating structures and the electrical properties of Cu-coated ACM microspheres were investigated. It was found that the Cu-coated ACM microspheres were a kind of elastic particles. The different coating structures could be produced by controlling the extent of plating reaction. The coated microspheres with different coating structures were conductive, and their volume resistivities decreased remarkably with the increasing of applied pressure and varied with the temperature according to their surface coating structures.     

节瘤缺陷平坦化提高高反射膜的激光损伤阈值

探究了节瘤缺陷平坦化技术中平坦化层(刻蚀层)厚度和种子源尺寸之间的刻蚀规律,同时解释了平坦化技术提高节瘤缺陷的损伤阈值的机制。在双离子束溅射系统中,使用SiO₂微球模拟真实的种子源置于基板上,镀制1064 nm HfO₂/SiO₂高反膜,制备人工节瘤缺陷。对类似于实际种子源的SiO₂微球一系列不同刻蚀程度的实验得出了节瘤缺陷平坦化技术的刻蚀规律:只要平坦化层(刻蚀层)的厚度稍大于节瘤缺陷的种子源粒径,就可以将种子源完全平坦化。使用时域有限差分法(FDTD)模拟不同平坦化程度的节瘤缺陷内电场增强的结果与节瘤缺陷的损伤形貌进行对比实验,将损伤形貌和损伤阈值与电场强度分布之间建立联系,表明平坦化技术可以改变节瘤缺陷原有的几何结构,有效抑制节瘤缺陷的电场增强效应。最后,通过对未经平坦化和经过平坦化处理后的节瘤缺陷进行损伤阈值测试,对比结果直接验证了节瘤缺陷平坦化技术可以实现对节瘤缺陷的调控,大幅度提高了节瘤缺陷的损伤阈值。     

Fabrication of protective tantalum carbide coatings on carbon fibers using a molten salt method

Protective tantalum carbide (TaC) coatings were fabricated successfully on carbon fibers in the temperature range of 950-1100 °C using a molten salt method. A salt mixture composed of LiCl-KCl-KF was used as a reaction medium in which the tantalum and the carbon fiber substrates reacted to form the TaC coatings. The structure and morphology of the TaC coatings were characterized by XRD, SEM and EDX analyses. The results show that the reaction temperature and time have significant influence on the thickness, integrity and surface morphology of the TaC coatings. A uniform, adherent and crack-free TaC coating can be obtained by controlling the reaction temperature and time. Thermo-gravimetric analysis indicated that the oxidation resistance of the carbon fibers was improved remarkably by coating them with a high-quality TaC layer.     

稀土永磁薄膜材料

简要地介绍在纳米复合稀土永磁薄膜材料、各向异性稀土永磁薄膜材料方面的进展。在纳米复合稀土永磁薄膜材料中实现磁性交换耦合和剩磁增强效应，系统地研究了其结构与磁性的关系。制备成功高磁能积的各向异性稀土永磁薄膜材料，比较了Ti或Mo缓冲层对Nd-Fe-B薄膜的表面形貌、磁畴结构和磁性能的影响。发现薄膜的表面形貌强烈地依赖于缓冲层的厚度。由于它极大地影响薄膜的成分，溅射速率被证明是控制薄膜的显微结构、表面形貌和磁性能的一个重要因素。在微磁学模型的基础上，通过分析从5到300K的矫顽力温度依赖关系。研究了各向异性Pr-Fe-B薄膜的矫顽力机制。在晶粒表面，由于磁各向异性的降低和局域退磁场的提高导致的反转畴的形核被确定为控制各向异性Pr-Fe—B薄膜的磁化反转过程的首要机制。     

工作压强对空心玻璃微球表面形貌和性能的影响

采用化学气相沉积-氧化烧结法,在不同工作压强条件下,制备了惯性约束聚变靶用空心玻璃微球(HGM)。利用扫描电子显微镜、原子力显微镜、VMR显微镜系统和能谱仪对HGM的表面形貌、球形度、壁厚均匀性以及成分进行了表征。分析了工作压强对HGM表面形貌、球形度、壁厚均匀性和成分的影响以及相互关系。研究表明:HGM的表面形貌随工作压强的增大而变得平滑致密,表面均方根粗糙度逐渐减小。随工作压强增大,HGM的球形度没有发生明显变化,而壁厚均匀性得到不断提高,微球中C元素浓度逐渐降低,Si元素浓度不断升高,O元素浓度基本保持不变。     

Adhesion properties of a silicon-containing calcium phosphate coating deposited by RF magnetron sputtering on a heated substrate

Silicon-containing hydroxyapatite coatings 400–700 nm in thickness are prepared by means of radio-frequency (RF) magnetron sputtering on a heated (to 200°C) titanium substrate chemically etched and treated with a pulsed electron beam. The morphology and phase composition of the coating are studied. The morphology and roughness of the composite “calcium-phosphate coating-titanium substrate” differ depending on the treatment procedure of the substrate before deposition. The scratch test method is used to assess the adhesion strength of the coatings formed at different values of bias potential applied to the substrate. It is observed that the adhesion strength of the coating changes with decreasing crystallite size.     

Study of physicochemical and biological properties of calcium phosphate coatings prepared by RF magnetron sputtering of silicon-substituted hydroxyapatite

Coatings based on pure silicon and silicon-substituted hydroxyapatite were grown by RF magnetron sputtering. The coating surface morphology, phase and elemental composition were studied by scanning electron microscopy, energy-dispersive X-ray analysis, and infrared spectroscopy. It was found that coatings are X-ray-amorphous, their elemental composition being controlled by the sputtered target composition. The distribution of elements over the coating surface is homogeneous. Medical and biological properties of coatings were studied in vivo and in vitro. Osteogenic properties of coatings were studied. Coatings grown by sputtering of a stoichiometric hydroxyapatite target are biocompatible without osteoinductive activity. The introduction of silicate ions into the hydroxyapatite structure that forms an electrode target significantly enhances the in vivo effect of CaP magnetron coatings on the osteogenic activity and stromal bone-marrow stem cells.     

The structure and tribological behaviors of CrN and Cr-Ti-N coatings

The Cr-Ti-N coatings with different composition were deposited in a medium frequency magnetron sputtering system on Si (1 1 1) substrates. The structures, surface morphology and wear properties were measured. The binary CrN coatings, formed a single-phase fcc structure with nearly random (1 1 1), (2 0 0) and (2 2 0) orientation, while for the Ti was introduced, coatings show a preferred orientation of (2 0 0). Cr-Ti-N coating shows a much smoother surface than CrN coating. Cr-Ti-N coating with 31.75% Ti content shows the best wear behavior. The excellent tribological properties of this composition coating are corresponding to the solid solution nitride structures.     

溅射功率对Mo薄膜微结构和性能的影响

 实验采用直流磁控溅射沉积技术在不同溅射功率下制备Mo膜,研究了不同溅射功率下Mo膜的沉积速率、表面形貌及晶型结构,并对其晶粒尺寸和应力进行了研究。利用原子力显微镜观察样品的表面形貌发现随着溅射功率的增加,薄膜表面粗糙度逐渐增大。X射线衍射分析表明薄膜呈立方多晶结构,晶粒尺寸为14.1～17.9 nm;应力先随溅射功率的增大而增大,在40 W时达到最大值(2.383 GPa),后随溅射功率的增大有所减小。