Bottom and top AF/FM interfaces of NiFe/FeMn/NiFe trilayers

X-ray reflectivity analyses were performed in the Si/WTi (7 nm)/NiFe (30 nm)/FeMn (13 nm)/NiFe (10 nm)/WTi (7 nm) exchange-biased system prepared by magnetron sputtering under three different argon working pressures. Layer-by-layer analyses were realized in order to obtain the interfacial roughness parameters quantitatively. For a fixed argon pressure, the root-mean-square roughness (including the atomic grading) of the upper (FeMn/NiFe) interface are greater than that for the lower one in all studied samples. Argon working pressure also has severe influence over the NiFe/FeMn interfaces, being more pronounced at the upper interfaces.     

“天光”一号MOPA系统光学元件加工与镀膜的进展

本文阐述了在中国原子能科学研究院“天光一号”ＫｒＦ激光核聚变实验装置上，ＭＯＰＡ系统光学元件加工与镀膜研究工作的进展。实验测量结果表明，加工后的基片表面均方根粗糙度对于Ｋ９光学玻璃与熔融石英玻璃来说分别为σｒｍｓ＝１．８±０．５ｎｍ，σｒｍｓ＝２．０±０．４ｎｍ。镀ＨｆＯ２／ＳｉＯ２高反射膜的光学元件的反射率与破坏阈值分别为Ｒ＞９９．５％，Ｅｔｈ＝１．３０～１．３３Ｊ／ｃｍ２。镀Ａｌ２Ｏ３／ＭｇＦ２增透膜的光学元件的透射率与破坏阈值分别为Ｔ＞９９．５％，Ｅｔｈ＝１．３～１．９７Ｊ／ｃｍ２。     

Ti-B-C-N纳米复合薄膜结构及力学性能研究

利用反应磁控溅射方法在单晶硅和高速钢(W18Cr4V)基片上制备出不同C含量Ti-B-C-N纳米复合薄膜. 使用X射线衍射和高分辨透射电子显微镜研究了Ti-B-C-N纳米复合薄膜的组织和微观结构,用纳米压痕仪测试了它们的硬度和弹性模量. 结果表明,利用往真空室通入C₂H₂气体的方法制备得到的Ti-B-C-N纳米复合薄膜中,在所研究成分范围内只发现TiN基的纳米晶. 当C₂H₂流量较小时,C元素的加入可以促进Ti-B-C 关键词： Ti-B-C-N薄膜 磁控溅射 微观结构 力学性能     

离子束溅射制备低应力深紫外光学薄膜

采用离子束溅射制备了Al F3、Gd F3单层膜及193 nm减反和高反膜系,分别使用分光光度计、原子力显微镜和应力仪研究了薄膜的光学特性、微观结构以及残余应力。在优选的沉积参数下制备出消光系数分别为1.1×10~(-4)和3.0×10~(-4)的低损耗AlF_3和GdF_3薄膜,对应的折射率分别为1.43和1.67,193 nm减反膜系的透过率为99.6%,剩余反射几乎为零,而高反膜系的反射率为99.2%,透过率为0.1%。应力测量结果表明,AlF_3薄膜表现为张应力而GdF_3薄膜具有压应力,与沉积条件相关的低生长应力是AlF_3和GdF_3薄膜残余应力较小的主要原因,采用这两种材料制备的减反及高反膜系应力均低于50 MPa。针对平面和曲率半径为240 mm的凸面元件,通过设计修正挡板,250 mm口径膜厚均匀性均优于97%。为亚纳米精度的平面元件镀制193 nm减反膜系,镀膜后RMS由0.177 nm变为0.219 nm。     

Characteristics of ZrC/ZrN and ZrC/TiN multilayers grown by pulsed laser deposition

ZrC/ZrN and ZrC/TiN multilayers were grown on (1 0 0) Si substrates at 300 °C by the pulsed laser deposition (PLD) technique using a KrF excimer laser. X-ray diffraction investigations showed that films were crystalline, the strain and grain size depending on the nature and pressure of the gas used during deposition. The elemental composition, analyzed by Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS), showed that films contained a low level of oxygen contamination. Simulations of the X-ray reflectivity (XRR) curves acquired from films indicated a smooth surface morphology, with roughness below 1 nm (rms) and densities very close to bulk values.Nanoindentation results showed that the ZrC/ZrN and ZrC/TiN multilayer samples exhibited hardness values between 30 and 33 GPa, slightly higher than the values of 28-30 GPa measured for pure ZrC, TiN and ZrN films.     

MPCVD方法制备军用光学元件纳米金刚石膜

介绍了用MPCVD方法制备纳米金刚石膜的工艺。用MPCVD方法实验研究了在光学玻璃上镀纳米金刚石膜:膜层厚度为0 4551μm,粒度小于200nm,表面粗糙度小于29 5nm,最大透过率为80%;平均显微硬度为34 9GPa,平均体弹性模量为238 9GPa,均接近天然金刚石的力学性能。与衬底材料表面应力-2 78GPa相比,具有较好的抗压和耐磨效果。     

水窗波段反射式偏振光学元件的设计和制作

水窗波段是软X射线进行生物活细胞显微成像的最佳波段,因此对于水窗波段偏振光学元件的研究有着非常重要的意义。用菲涅耳公式计算出在水窗波段内不同材料组合对应不同波长的最大反射率,模拟分析了多层膜周期和表界面粗糙度对多层膜偏振光学元件性能的影响。用超高真空磁控溅射镀膜设备,制作出2．40nm、3．00nm和4．30nm波长处W／B4C多层膜偏振元件,并用X射线衍射仪对元件的周期厚度进行了测量,得到的测量结果与设计值偏差很小,可以进行实际应用。为水窗波段反射式偏振光学元件的研究提供了理论依据,同时也为相应偏振光学元件的制备确定了合适的工艺参量。     

退火温度对溅射铝膜结构与电性能的影响

 采用直流磁控溅射方法成功地制备了Al膜,研究了退火温度对Al膜表面形貌、晶体结构、应力、择优取向及反射率的影响。研究表明：不同退火温度的薄膜晶粒排布致密而光滑,均方根粗糙度小。XRD测试表明：不同温度退火的铝膜均成多晶状态,晶体结构为面心立方,退火温度升高到400 ℃时,Al膜的应力最小达0.78 GPa,薄膜平均晶粒尺寸由18.3 nm增加到25.9 nm;随着退火温度的升高,(200)晶面择优取向特性变好。薄膜紫外-红外反射率随着退火温度的升高而增大。     

碳纳米管/丙烯酸酯涂料的制备及其红外吸波性能

"利用表面改性剂对碳纳米管进行表面改性来防止其颗粒的团聚,从而制得分散性较好的碳纳米管浆料,在此基础上来制备碳纳米管/丙烯酸酯涂料,并研究了它在近红外波段的反射率．分析了PVC浓度、表面改性剂的种类及浓度以及碳纳米管的管长,对碳纳米管/丙烯酸酯涂料在?=930 nm处反射率的影响,并对涂料工艺进行了优化设计,最终制备出了吸收性能优良的碳纳米管/丙烯酸酯涂料．它在840~950 nm的近红外波段的反射率为均在0.1%以下并且透射率均在1.0%以下．"     

Chemical composition of ZrC thin films grown by pulsed laser deposition

ZrC films were grown on (1 0 0) Si substrates by the pulsed laser deposition (PLD) technique using a KrF excimer laser working at 40 Hz. The nominal substrate temperature during depositions was set at 300 °C and the cooling rate was 5 °C/min. X-ray diffraction investigations showed that films deposited under residual vacuum or under 2 × 10⁻³ Pa of CH₄ atmosphere were crystalline, exhibiting a (2 0 0)-axis texture, while those deposited under 2 × 10⁻² Pa of CH₄ atmosphere were found to be equiaxed and with smaller grain size. The surface elemental composition of as-deposited films, analyzed by Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS), showed the usual high oxygen contamination of carbides. Once the topmost 2-4 nm region was removed, the oxygen concentration rapidly decreased, down to around 3-8% only in bulk. Simulations of the X-ray reflectivity (XRR) curves indicated a smooth surface morphology, with roughness values below 1 nm (rms) and films density values of around 6.30-6.45 g/cm³, very close to the bulk density. The growth rate, estimated from thickness measurements by XRR was around 8.25 nm/min. Nanoindentation results showed for the best quality ZrC films a hardness of 27.6 GPa and a reduced modulus of 228 GPa.     

两种常用碳化硅反射镜基底表面改性的研究

利用霍尔离子源辅助电子束蒸发方法,分别在反应烧结碳化硅(RB-SiC)和常压烧结碳化硅(Sintered SiC,S-SiC)基底材料上制备了Si改性膜层,并进行了相关性能测试和分析。经过表面改性,两种基底的表面粗糙度(rms)大幅地降低,镀银后的反射率有较大地提高,基底表面光学质量已满足工程应用要求。在相同工艺条件下,S-SiC基底改性后效果好于RB-SiC基底的情况,主要是因为Si膜在两种基底表面生长情况不同所致。     

Role of argon in its mixture with nitrogen in deposition of nitride condensates in the Ti-Si-N system and in vacuum arc deposition processes

Arc vacuum deposition of nitride coatings in the Ti-Si-N system is carried out in an argonnitrogen mixture with variable gas concentration ratios. The resulting condensates are studied by fractographic analysis, X-ray diffraction analysis, and high-resolution scanning electron microscopy. Studied also are the elemental composition and microhardness of the condensates. At gas mixture pressure p > 5 × 10^?3 Torr, conditions are found under which the hardness of the condensates is maximal, and the dependence of the hardness on the argon percentage in the mixture is obtained. At an argon percentage of 8–12%, the hardness of the coatings reaches 50 GPa. This value is 1.7 times higher than the hardness of coatings obtained in a nitrogen atmosphere. This superhard state is explained by the nanometer size (25–30 nm) of nitride grains and a specific growing texture with a family of {100} planes that is parallel to the growth plane. Such a configuration minimizes the surface energy. Mechanisms that may increase the ionization of film-forming particles and activate chemical bonds in the presence of argon are discussed.     

高精细度光学参考腔的自主化研制

高精细度超稳光学参考腔是获得超窄线宽激光的核心部件.本文报道了面向空间应用的高精细度球形超稳光学参考腔自主化研制及其初步测试结果.设计球形腔体直径为80 mm,腔长78 mm,采用平-凹腔镜结构,凹镜曲率半径为0.5 m.使用有限元方法计算了该参考腔的震动敏感度,最佳支撑位置的震动敏感度小于1×10~(-10)/g.采用超光滑表面三级抛光技术实现光学表面粗糙度小于0.4 nm(rms)的超精密加工,采用双离子束溅射法实现工作波长反射率大于99.999%、损耗小于4 ppm腔镜镀膜,干式光胶方法键合腔体和腔镜.利用扫腔线宽法和腔衰荡法对参考腔的线宽和精细度进行了测量,结果表明该参考腔的精细度约为195000,线宽为9.8 kHz.将698 nm半导体激光器锁定到该参考腔上测得其损耗5 ppm.与实验室进口同类型参考腔相比较,主要性能指标与其相当.     

Study and simulation of the growth of solid lubricant MoSe<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> coatings during pulsed laser deposition

The chemical composition and tribological properties of the thin-film diselenide molybdenum coatings deposited by pulsed laser deposition in vacuum and a rarefied inert gas (argon) atmosphere are studied. Upon deposition in a gas at a pressure of ∼2 Pa, stoichiometric coatings with improved antifriction properties as compared vacuum-deposited coatings form. However, a too strong increase in the argon pressure (to ∼10 Pa) degrades the tribological properties of the coating. Structure formation in the MoSe _x coatings grown by pulsed laser deposition on an unheated substrate is investigated. Deposition in vacuum or argon at a pressure of 2 Pa leads to formation of rather smooth coatings with a dense amorphous structure containing molybdenum nanoinclusions. Deposition at a high argon pressure results in a developed surface relief and a loose coating structure. A mathematical model is developed using the kinetic Monte Carlo method in order to describe structure formation in the coatings that grow during physical deposition of an atomic flux. A comparative analysis demonstrates satisfactory agreement between the simulated and experimentally studied structures in the coatings created by pulsed laser deposition at various gas pressures.     

Sputtering pressure effects on the structural and mechanical properties of TiVCr alloy coatings

In this study, TiVCr alloy coatings were deposited on Si substrates by magnetron sputtering system at different working pressures (0.33-1 Pa). The TiVCr coatings have a composite structure with amorphous and body-centered cubic (bcc) crystal phases comprised of bundles of fine fibrous structures and V-shaped columnar structures, respectively. Compared with the amorphous zone, the crystalline zone has a denser and more compact structure. The coating microstructure became more porous as working pressure increased. Consequently, the crystal zones of the deposited coatings at 0.33 Pa obtained higher hardness (11.6 GPa) while the deposited coatings at 1 Pa achieved lower hardness (4.5 GPa).     

Influence of superalloy substrate roughness on adhesion and oxidation behavior of magnetron-sputtered NiCoCrAlY coatings

The present study has been conducted in order to determine the influence of superalloy substrate roughness on adhesion and oxidation behavior of magnetron-sputtered NiCoCrAlY coatings. Six types of coating samples with different substrate roughness were tested. The surface roughness and real surface area of both the substrates and coatings were studied by atomic force microscopy (AFM) techniques. The scratch tests performed at progressive loads were employed to evaluate the adhesion of the coatings. Cyclic oxidation tests were performed at 1100 °C in air for 50 cycles, each cycle consisting of 1 h heating in the tube furnace followed by 15 min cooling in the open air. The AFM measurements exhibit that the surface roughness of the sputtered NiCoCrAlY coating increases with the increasing of the superalloy substrate roughness. The NiCoCrAlY coatings present slightly lower roughness than the corresponding superalloy substrate. The scratch adhesion tests indicate that the coatings on substrates with a smoother surface possess better adhesion than on those with a rougher surface. Both the real surface area and oxidation weight gain of the coatings decrease with the decreasing of the superalloy substrate roughness. The NiCoCrAlY coating sputtered on the superalloy substrate with lower roughness provides relatively higher antioxidant protection than that provided by the coating with rougher substrate.     

Microstructure and mechanical properties of reactive magnetron sputtered Ti-B-C-N nanocomposite coatings

Ti-B-C-N nanocomposite coatings with different C contents were deposited on Si (1 0 0) and high speed steel (W18Cr4V) substrates by closed-field unbalanced reactive magnetron sputtering in the mixture of argon, nitrogen and acetylene gases. These films were subsequently characterized ex situ in terms of their microstructures by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM), their nanohardness/elastic modulus and facture toughness by nano-indention and Vickers indentation methods, and their surface morphology using atomic force microscopy (AFM). The results indicated that, in the studied composition range, the deposited Ti-B-C-N coatings exhibit nanocomposite based on TiN nanocrystallites. When the C₂H₂ flow rate is small, incorporation of small amount of C promoted crystallization of Ti-B-C-N nanocomposite coatings, which resulted in increase of nano-grain size and mechanical properties of coatings. A maximum grain size of about 8 nm was found at a C₂H₂ flux rate of 1 sccm. However, the hardness, elastic modulus and fracture toughness values were not consistent with the grain size. They got to their maximum of 35.7 GPa, 363.1 GPa and 2.46 MPa m^1/2, respectively, at a C₂H₂ flow rate of 2 sccm (corresponding to about 6 nm in nano-grain size). Further increase of C content dramatically decreased not only grain size but also the mechanical properties of coatings. The presently deposited Ti-B-C-N coatings had a smooth surface. The roughness value was consistent with that of grain size.     

高反射率Mo/B4C多层膜设计及制备

 运用遗传算法优化设计了Mo/B₄C多层膜结构。入射光入射角度取10°时,设计的理想多层膜膜对数为150,周期为3.59 nm,Gamma值（Mo膜厚与周期的比值）为0.41,峰值反射率为33.29%。采用恒功率模式直流磁控溅射方法制作Mo/B₄C多层膜。通过在Mo/B4C多层膜与基底之间增加15 nm厚的Cr粘附层,提高多层膜与基底的粘附力。另外,还采用调整多层膜Gamma值的方法减小其内应力,调整后多层膜结构周期为3.59 nm, Mo膜厚1.97 nm, B4C膜厚1.62 nm,峰值反射率26.34％。制备了膜对数为150的Mo/B₄C膜并测量了其反射率,在波长7.03 nm处,Mo/B₄C多层膜的近正入射反射率为21.0％。最后对测量结果进行了拟合,拟合得到Mo/B₄C多层膜的周期为3.60 nm,Gamma值0.60,界面粗糙度为0.30 nm。     

Peculiarities of structural phase and elastic stress states of superhard TiN-based nanocomposite coatings

A new concept of designing nanocomposite coatings is proposed. The concept consists in microstructural self-organization through simultaneous nucleation of islands of different mutually insoluble or slightly soluble phases at the stage of coating formation. Physical principles on which to select compositions of the coatings were developed and were experimentally verified on multicomponent nanocomposite coatings. With a Sprut magnetron arc plasma complex, superhard (H _μ > 40 GPa) multicomponent nanocomposite coatings of the system Ti-Al-Si-Cr-Ni-Cu-O-C-N were obtained. The peculiarities of structural phase and elastic stress states of the multicomponent coatings before and after annealing at a temperature of up to 1000 °C were studied by transmission electron microscopy, X-ray diffraction analysis, microhardness measurements and scratch tests. The study reveals a wide range of lattice bending-torsion (up to 200° μm^?1) of nanosized (less than 30 nm) coherent scattering regions in the two-level coating structure and of individual (up to 15 nm) TiN nanocrystals. Annealing of the coatings causes the two-level grain structure to relax with the formation of TiN-based nanocrystals of size less than 30–40 nm and with a decrease in lattice bending-torsion down to 40°–50° μm^?1. Comparative analysis of acoustic emission signals and tracks of the multicomponent and TiN coatings in scratch tests points to an increase in fracture ductility in the multicomponent coatings.     

温度和压力对Au反射特性影响及动高压下的测温应用分析

基于金属电子气模型,进行了温度、压力对Au反射率变化影响的研究与分析。利用DAC装置开展了压力对Au反射率变化测量实验,以及激光加热的动态温升条件下温度对Au反射率变化测量实验,获得了探测光束波长为488 nm条件下,温度(室温至350 ℃)和压力(11 GPa范围内)对Au反射特性影响的实验结果。结果表明:在11 GPa压力范围内,与温度因素相比,压力对Au的反射率变化影响可忽略;Au对488 nm波长激光的反射率变化趋势为单调递增,变化幅值达约10%,且具有反射率与温度的一一对应特性。通过动高压加载下材料温度瞬态测量要求分析,认为基于Au在488 nm波长下的反射变化特性,可建立一种适用于动高压加载下低温段(低于1000 K)的瞬态测温方法,用于解决材料动高压领域的瞬态测温技术难点。