电子束与电阻复合蒸发法制备Zr-Cu非晶薄膜及性能表征

主要采用电子束蒸发与电阻蒸发复合镀膜系统制备Zr-Cu二元非晶薄膜,衬底基板无冷却装置。通过X射线衍射仪(XRD)、场发射透射电子显微镜(FE-TEM)、场发射扫描电子显微镜(FE-SEM)、微控四探针测量仪等仪器,系统地研究了样品沉积时间对薄膜厚度、微观结构、表面形貌以及电学性能的影响,另外还分析了与磁控溅射制备的Zr-Cu非晶样品的区别。结果显示,该复合镀膜技术制备的ZrxCu100-x非晶薄膜玻璃形成成分范围为x=30~85;薄膜的结构与性能对沉积时间比较敏感。样品随沉积时间的延长从非晶结构逐渐向非晶纳米晶复合结构转变;相比磁控溅射制备的薄膜样品,复合蒸发法制备的薄膜表面呈现较大尺寸的"团簇"形貌;样品的电阻率和方块电阻随沉积时间的延长逐渐减小。     

磁控溅射工艺参数对Cu,Al薄膜与Gd基底附着性的影响

为了探讨Gd表面溅射保护膜的附着性能,利用直流磁控溅射技术在Gd基体上分别镀Cu和Al膜.用扫描电镜(SEM)和能谱仪对薄膜进行表征,用引拉法测定了薄膜的附着强度.结果表明:A1膜表面质量好,Al/Gd界面结合好,附着强度高,在优化工艺参数条件下薄膜附着强度可达到27.60 MPa;Cu膜表面质量较差,Cu/Gd界面结合差,附着强度低,在优化工艺参数条件下薄膜附着强度最高仅为3.02 MPa.     

Interface cracking between functionally graded coatings and a substrate under antiplane shear

Coating technology plays a significant role in a number of applications such as high temperatures, corrosion, oxidation, wear, and interface. In this paper, we investigate the interface cracking between ceramic and/or functionally graded coatings (FGM coatings) and a substrate under antiplane shear. Four coating models are considered, namely single layered homogeneous coating, double layered piece-wise homogeneous coating, single layered FGM coating and double layered coating with an FGM bottom coat. Mode III stress intensity factors (SIFs) are calculated for the different coating models. In the case of μ_L > μ₀ where μ₀ is the shear modulus of the substrate and μ_L the shear modulus of the material at the surface of the coating, it is found that the single layered FGM coating reduces SIF slightly, whereas the coating system with a top homogeneous layer and a thin FGM bottom layer reduces SIF significantly. In the case of μ_L < μ₀ the SIF is found to be larger for the FGM coatings than for the homogeneous coatings. The FGM coating, however, may still be superior to homogeneous coatings in this case as FGM coatings usually provide better bonding strength between the coating and substrate. Finally, the applicability of the SIF concept in the fracture of FGM coatings is discussed. Large modulus gradients in thin coatings may seriously restrict the application of SIFs as the SIF-dominant zone may fall into the crack tip nonlinear deformation and damage zone. The same argument exists for some interphase models in interface crack solutions.     

The production of porous and chemically reactive coatings by magnetron sputtering

High surface area materials can have a number of applications including use as pyrophoric devices, sensors, laser mirrors, filters, thermal barriers and catalysts. The aim of this work was to deposit highly porous thin films capable of undergoing a spontaneous pyrophoric reaction and igniting a suitable substrate material. Magnetron sputtering was the chosen deposition technique as it enables reproducible deposition of coatings, with closely controlled, almost uniform, thickness and morphologies over extended surfaces.A number of magnetron magnetic configurations were investigated and deposition conditions were varied in order to control the surface area of the films and, thereby, optimise the pyrophoric behaviour. As a consequence, pyrophoric coatings were produced with ignition temperatures dependent on the deposition conditions and substrate material/topography. When deposited on combustible substrates, these coating/substrate systems formed simple pyrotechnic devices in a one-stage process. The main thermal signal emitted by these devices was dependent on the substrate material only.     

磁控溅射TiAlSiN膜的抗氧化性能

目前,针对TiAlN和TiAlSiN薄膜在800~1 000℃高温氧化时的硬度及抗氧化性能研究较少。利用磁控溅射技术,在高速钢W18Cr4V表面制备了TiAlN和TiAlSiN薄膜,当Al靶功率为100 W、Si靶溅射电流为0.20 A时,TiAlSiN薄膜硬度及弹性模量达到最大值,对此条件下的膜层进行了大气高温氧化试验。采用激光共聚焦显微镜、扫描电子显微镜(SEM)和能谱仪(EDS)、X射线衍射仪(XRD)等检测手段,研究了800,900,1 000℃下2种薄膜的抗氧化性。结果表明:经相同温度氧化处理后,TiAlSiN薄膜的表面粗糙度明显小于TiAlN薄膜的;在TiAlN中引入Si元素形成Si3N4包裹TiN纳米晶的复合结构,抑制了膜层中裂纹的形成,使TiAlSiN薄膜在相同氧化温度下的抗氧化性能比TiAlN薄膜更加优异。     

Three dimensional imaging of deformation modes in TiN-based thin film coatings

A TiN thin film coating, approximately 4 μm in thickness, deposited on a ductile steel substrate, was subject to surface deformation via nanoindentation using a spherical indenter, 5 μm in radius, with loads up to 500 mN. Pop-ins were observed during loading, which are characteristic of the onset of cracking and the formation of shear steps at the coating-substrate interface. Focused ion beam microscopy was used to prepare cross-sections through the indentation that revealed the presence of both intercolumnar and inclined cracks. Three-dimensional reconstructions of the deformation zone beneath the indentation were performed using a dual-beam focus ion beam instrument. These constructions provided more detailed images of the morphology of cracks, which were observed to be consistent with theoretical models of plastic deformation of such brittle coatings.     

锆合金表面磁控溅射制备SiC/Cr复合涂层的研究

通过直流磁控溅射方法在锆合金基体表面沉积Cr涂层, 再在Cr层上射频磁控溅射制备SiC涂层, 探索了基体预处理方式、射频溅射功率对涂层结合力、厚度和表面质量的影响。采用扫描电镜及能谱仪, 红外光谱和X射线衍射仪对SiC/Cr复合涂层样品进行成分分析, 结果表明所制备的涂层Cr层为晶态, SiC层为非晶态。高温水蒸汽氧化实验表明Cr作为锆合金与SiC涂层之间的过渡层, 不仅能够缓解SiC层和锆合金基体的热膨胀系数差异, 提高涂层结合力, 还能增加涂层的延展性, 减少基体在高温水蒸气环境下的氧化和断裂。     

磁控溅射法制备HAF/YSZ梯度复合涂层及生物性能研究

采用射频磁控溅射技术在Ti6Al4V基体上成功制备了含氟羟基磷灰石梯度复合涂层(HAF/YSZ)。利用X射线光电子能谱(XPS)、电子探针(EDX)、扫描电镜(SEM)等对涂层的成分分布、形貌、界面结合进行表征。通过模拟体液(SBF)实验,分析和评价了HAF/YSZ涂层在模拟人体条件下的生物性能。结果表明,所制备涂层表面粗糙,呈多孔岛状结构,有利于新生骨组织的生长;涂层与基体结合紧密,各层间相互扩散,整体一致性较好;经模拟体液浸泡后,涂层表面有新生物质沉积,表现出较好的生物活性及稳定性;梯度复合涂层较氟含量单一的氟羟基磷灰石涂层具有更好的抗体液溶解能力及稳定性。     

Highly adhesive hydroxyapatite coatings on titanium alloy formed by ion beam assisted deposition

A compact crystalline hydroxyapatite coating on Ti–6Al–4V substrate with an atomic intermixed coating/substrate interface about 27 nm in width was synthesized by ion beam assisted deposition (IBAD) and a following post-treatment. The coating after post-treatment was identified by X-ray diffraction as crystalline hydroxyapatite. The interface between coatings and substrates was studied by Auger electron spectroscopy. The adhesive strength between coatings and substrates was measured by scratch tester. The results showed that the adhesive strength of IBAD coatings is nearly twice that of ion beam sputtered coatings. The study also showed that coatings prepared by IBAD eliminated the interfacial deficiencies existing in plasma-sprayed coatings.     

Ion-beam etching for the precise manufacture of optical coatings

We propose using ion-beam etching as an additional tool for the accurate control of the thickness of thin films during the manufacture of sensitive optical multilayer coatings. We use a dual ion-beam sputtering system in the deposition and etch modes. In the deposition mode both the assist and sputtering ion beams are used to produce dense films at deposition rates in the range of 0.1-0.3 nm/s. In the etch mode, only the assist ion beam is used to remove material at a rate of less than 0.1 nm/s. A very high precision in the layer thicknesses can be obtained by alternating between deposition and etch modes. We observed that etching did not significantly affect the surface quality and the uniformity of the coatings. We introduced etching into our current manufacturing process and demonstrated its potential for the fabrication of several optical multilayer systems with performances that are very sensitive to the thickness of their layers.     

注入氮离子的SiC涂层阻氢性能研究

利用离子束混合－离子注入（Ar^ ）和磁控溅射相结合的实验技术在HR－1不锈钢基体上制备了注入N^ 的SiC涂层，并用表面分析手段对所制备涂层的表面形貌，剖面形貌、相结构，表面成分，表面元素的化学态进行了分析，结果表明：制备的涂层结构致密，表面平整、膜层成分均匀；涂层与基体之间形成了一明显的过渡层，增强了涂层和基体之间的结合力，用二次离子质谱（SIMS）对充氘涂层的阻氢性能进行了定性分析，结果表明，涂层元素与氢形成稳定的化学键，抑制了氢的扩散和迁移，使得涂层具有一定的阻氢能力。     

离子束溅射沉积羟基磷灰石涂层钛种植体材料的制备和表征

采用Ａｒ＾＋离子束溅射沉积技术和钛基体上沉积羟基磷灰石薄膜涂层,Ａｒ＾＋离子束的能量分别为０．９ｋｅＶ、１．２ｋｅＶ和１．５ｋｅＶ。利用Ｘ射线衍射（ＸＲＤ）、扫描电（ＳＥＭ０、透射电镜（ＴＥＭ）和红外光谱（ＦＴＩＲ）等检测方法,对制备的羟基磷灰石薄膜涂层进行了表征。Ｘ射线衍射和透射电结果表明该薄膜涂层为非晶态;红外光谱中无羟基（ＯＨ）特征峰存在,ＣＯ３根吸收峰的出现说明制备过程中会引入ＣＯ３根;扫     

Hard coatings on light-metal components under mechanical surface loading

In this work the behaviour of hard coated light-metal components was investigated when they are mechanically loaded. Three lightmetal alloys, Ti-6Al-4V, AlSi7Mg and AlMgSi0.5 and 100Cr6 steel (as a reference material) were coated by two different physical vapour deposition processes: radio frequency magnetron sputtering and electron beam evaporation. The coating materials utilised were CrN and TiN. Standard test methods with different loading conditions were used to evaluate the substrate/coating-combinations: the hardness test (applying a static normal load), the scratch test (applying a combination of a static normal and a static tangential force) and the impact test (applying a dynamic normal load). It was observed that the load support of coated materials depends on the loading conditions. The coated aluminium alloys showed poor load support under all loading test conditions but produced a higher surface hardness than uncoated steel. Coated Ti-6Al-4V showed very good load support properties, similar to coated steel. All coated light-metal substrates demonstrated significant improvement in load support behaviour with an increase in coating thickness. The results of the scratch test, which is commonly used to asses adhesion properties of thin coatings, showed an immediate indenter-breakthrough on the aluminium alloy substrates, but causing no coating delamination. Due to this behaviour, the scratch test is not suitable to evaluate adhesion properties on coated soft light-metals. Yet the impact test allowed assessment of coating delamination on the aluminium alloys, proving its usefulness for adhesion measurement even on soft substrates. The study indicates that substitution of steel with coated lightmetal alloys is a viable proposition for certain applications.     

Study on behavior of NiAl coating with different Ni/Al ratios

β-NiAl coatings with different Ni/Al ratios were deposited on K403 superalloy substrates via magnetron sputtering. The phase transformation and diffusion phenomenon of the NiAl/Ni-based superalloy system after vacuum annealing at 900 and 1000 °C were analyzed using X-Ray diffraction (XRD), field emission scanning electron microscope (FE-SEM) and energy dispersive X-ray spectrometry (EDS). The effect of coating concentrations on the outward diffusion behavior of substrate elements was discussed. The high Cr concentrations in the Al-rich NiAl coatings were caused by the intense interdiffusion between Al and Cr. The Ti, W and Mo partitioned to γ′-Ni₃Al in the coatings. Several possible reasons for the formation of γ′-Ni₃Al at the surface of Ni-rich NiAl coating were identified, including: diffusion behavior of W and Mo in β-NiAl, destabilizing effect of substrate elements on β-NiAl, and diffusion rates of Ni and Al in β-NiAl. The volume change in β ⇛ γ′ transformation process shows Ni uphill diffused to the γ′-Ni₃Al islands at the surface of Ni-rich NiAl coatings. The IDZ (interdiffusion zone) thickness and precipitates in IDZ were related to the Al initial concentrations in the coatings.     

Microstructure and mechanical properties of CrAlN coatings deposited by modified ion beam enhanced magnetron sputtering on AISI H13 steel

CrAlN coatings were deposited on silicon and AISI H13 steel substrates using a modified ion beam enhanced magnetron sputtering system. At the modified ion beam bombardment, the effects of bias voltage and Al/(Cr + Al) ratio on microstructure and mechanical properties of the coatings were studied. The X-ray diffraction data showed that all CrAlN coatings were crystallized in the cubic NaCl B1 structure, showing the (111), (200), and (220) preferential orientation. It is noted that the (111) diffraction peak intensity decreased and the peaks broadened as the bias voltage increased at the same ratio of Al/Cr targets power, which is attributed to the variation in the grain size and microstrain. The microstructure observation of the coatings by field emission scanning electron microscopy cross-section morphology shows that the columnar grain became more compact and dense with increasing substrate bias voltage and Al concentration. At a substrate bias voltage of −120 V and a Al/(Cr + Al) ratio of 40%, the coating had the highest hardness (33.8 GPa) and excellent adhesion to the substrate.     

Multilayer DLC coatings via alternating bias during magnetron sputtering

To combat the high residual stress problem in monolayer diamond-like carbon coatings, this paper fabricated multilayer diamond-like carbon coatings with alternate soft and hard layers via alternating bias during magnetron sputtering. The surface, cross sectional morphology, bonding structures and mechanical properties are investigated. The atomic force microscopy images indicate low bias results in rougher surface with large graphite clusters and voids suggesting low coating density. The multilayered coatings demonstrate relatively smooth surface stemming from higher bias. The cross sectional images from field emission scanning electron microscopy indicate coating thickness decreases as substrate bias increases and confirm that higher bias results in denser coating. Delamination is observed in monolayer coatings due to high residual stress. The trend of sp³/sp² fraction estimated by X-ray photoelectron spectroscopy is consistent with that of I_D/I_G ratios from Raman spectra, indicating the change of bonding structure with change of substrate bias. Hardness of multilayer diamond-like carbon coating is comparable to the coatings deposited at low constant bias but the adhesion strength and toughness are significantly improved. Alternately biased sputtering deposition provides an alternative when combination of hardness, toughness and adhesion strength is needed in an all diamond-like carbon coating.     

ZnO/Al2O3 coatings for the photoprotection of polycarbonate

ZnO and ZnO/Al₂O₃ thin films were deposited by r.f. magnetron sputtering on polycarbonate (PC) films in order to protect this polymer against photodegradation. The composition, structure and optical properties of the ceramic coatings were characterised. CO₂-plasma treatments were applied to PC in order to improve the coating adhesion. The PC surface energy was characterised by wettability measurements and the chemical bonds were analysed by XPS.It was found that ZnO coatings improve the stability of PC to UV radiations and that an intermediate alumina coating inhibits the photocatalytic oxidation of PC at the PC/ZnO interface. Additionally an external alumina coating brings a high hardness to the coating.     

车载抬头显示光学系统塑料元件反射膜的研制

为了提高抬头显示系统中投影镜和反射镜的耐环境性和光学性能,以聚碳酸酯(PC)作为基底,采用电子束蒸发技术,使用过渡层和连接层技术以及渐增式离子源工艺,解决了薄膜与基底的附着力问题;利用真空退火,改善了环境测试过程中薄膜的膜裂现象;通过调节最外层SiO₂的离子源工艺,改善了水煮测试过程中薄膜因水汽渗透而导致的反射率下降的问题。制备了耐环境性能强的平均反射率大于95%的金属-介质结构的高反射膜。实际样品满足抬头显示系统的要求,并通过了多项环境测试。     

镍基625合金电子束熔覆TiC涂层表面改性研究

目的 采用电子束表面改性技术对Inconel 625镍基合金进行电子束表面合金化(EBSA)处理,制备性能良好的TiC涂层,提高Inconel 625镍基合金的表面性能。方法 采用不同的电子束扫描速度(80、100、120 mm/min)在Inconel 625镍基合金表面制备TiC涂层,使用扫描电镜(SEM)拍摄合金区横截面进行EDS能谱分析,使用电子背散射衍射仪(EBSD)对合金层进行EBSD表征分析,使用显微硬度仪测量EBSA后的表面硬度,使用摩擦磨损试验机(RTEC)测试表面耐磨性、生成摩擦曲线并拍摄磨损表面的三维形貌。结果 从宏观形貌上来看,在80 mm/min扫描速度下涂层成形质量最好。微观组织测试结果表明,随着扫描速度的增大,平均晶粒尺寸增大。显微硬度测试结果表明,随着扫描速度的增大,表面硬度呈现降低的趋势,但涂层表面硬度均高于基材硬度。当扫描速度为80 mm/min时,TiC强化颗粒较多分布在表面,其表面硬度最高,为457HB,与基材相比,表面硬度提高了1.936倍。耐磨性测试结果表明,当扫描速度为80 mm/min时,磨损体积和磨损率最低,分别为0.913 1 mm<...     

A coatings application for fusion research

A large stainless steel toroidal inner vacuum liner, with a major radius of 79.5 cm and minor radius of 23.5 cm, has been coated with gold to minimize gas adsorption and to provide an inert surface for the plasma in ORMAK, a fusion experiment. A thin platimum film, deposited prior to the gold coating, acts as a diffusion barrier and prevents many of the constituents of the steel from diffusing through the gold to the surface.In a fusion reactor the walls exposed to the plasma will be bombarded by highly energetic neutrals and a gold surface may not be suitable because of its relatively high sputtering yield. Several other materials, some of which may be more suitable for use as a “first wall” surface than gold, have been identified but many of these candidates are expected to be impractical to use in their bulk form. A solution is a composite wall consisting of a suitable coating on a substrate chosen for its strength and ease of fabrication. The techniques employed to deposit several of these candidate materials onto stainless steel substrates as thick coatings are described.