铝表面改性SiOx薄膜力学性能研究

采用常压化学气相沉积（APCVD）技术在铝基底上成功制备了改性SiOx陶瓷薄膜。通过显微硬度测试与涂层附着力自动划痕测试定量研究了薄膜显微硬度和膜基结合强度，利用光学显微镜（0M）和扫描电子显微镜（SEM）观察了薄膜的原始表面以及压痕、划痕形貌。结果表明，SiOx膜层由大小不均匀的等轴状颗粒团聚堆垛而成，退火处理时长大或融合成片状；SiOx薄膜有效提高纯铝表面的硬度，并能通过SiOx薄膜变形以松弛表层应力，抑制脆性裂纹产生；划痕测试证明基底和薄膜具有很高的结合强度，薄膜与基底发生塑性变形而不剥离。     

双槽电沉积法制备Cu/Ag纳米多层膜

双槽电沉积法制备了不同调制波长的Cu/Ag金属多层膜(Cu膜和Ag膜等厚),用扫描电子显微镜观察了多层膜的层状结构,并研究了不同调制波长下多层膜的显微硬度变化.结果表明:双槽电沉积法制备的Cu/Ag多层膜层状结构明显.当调制波长大于100 nm时,显微硬度随调制波长减小而增加;当小于100 nm时,硬度随调制波长减小而...     

调制周期对磁控溅射WB2/CrN多层薄膜力学性能的影响

目的研究调制周期对磁控溅射WB_2/CrN多层膜结构及性能的影响。方法通过双靶直流磁控溅射法,在硅片、石英玻璃片及不锈钢上,制备Al B_2型WB_2薄膜与CrN薄膜及其多层复合薄膜,采用X射线衍射及扫描电子显微镜对其相结构及形貌进行观察和分析,使用维氏显微硬度仪及划痕仪对多层膜的硬度及膜基结合力进行研究。结果磁控溅射WB_2/CrN多层薄膜呈现出柱状生长趋势,且层状结构明显,仅当调制周期大于317 nm时,多层膜中才出现WB_2晶体的衍射峰。结论多层膜中的WB_2薄膜在本实验条件下的临界结晶厚度大于150 nm。随着调制周期的减小,CrN层生长取向发生由(200)晶面向多晶面的转变,WB_2层生长取向由(101)晶面向(001)晶面转变。多层膜硬度随调制周期的减小大体呈下降趋势,在调制周期为317 nm时达到最大值。结合力变化趋势与硬度相反,CrN层及多层界面有助于复合薄膜膜基结合强度的提高。     

Cr/CrN/CrNC/CrC/Cr-DLC梯度膜层的研究

采用中频磁控溅射结合离子源技术沉积Cr／CrN／CrNC／CrC／Cr-DLC膜层。利用扫描电镜（SEM）、电子能谱（EDS）、Raman光谱和俄歇深层剥层分别对膜层微观形貌、成分组成、键结构及梯度成分深层分布进行分析；采用努氏显微硬度计、摩擦磨损试验机、划痕仪及洛氏硬度计测评膜层机械性能。结果表明：采用中频磁控溅射可沉积出大面积Cr／CrN／CrNC／CrC／Cr-DLC梯度膜层；Cr溅射功率对C键结构影响不大，但表层DLC中Cr的含量和膜层厚度随中频功率增大而增大；随DLC中掺Cr量增多，膜层硬度及摩擦因数略有上升；采用梯度过渡层及掺入金属Cr提高了膜层附着力，但过高的中频功率使沉积离子能量偏高，膜层压应力增加反而降低了膜层附着性能。     

铝表面改性SiOx薄膜力学性能研究

采用常压化学气相沉积(APCVD)技术在铝基底上成功制备了改性SiOx陶瓷薄膜.通过显微硬度测试与涂层附着力自动划痕测试定量研究了薄膜显微硬度和膜基结合强度,利用光学显微镜(OM)和扫描电子显微镜(SEM)观察了薄膜的原始表面以及压痕、划痕形貌.结果表明,SiOx膜层由大小不均匀的等轴状颗粒团聚堆垛而成,退火处理时长大或融合成片状;SiOx薄膜有效提高纯铝表面的硬度,并能通过SiOx薄膜变形以松弛表层应力,抑制脆性裂纹产生;划痕测试证明基底和薄膜具有很高的结合强度,薄膜与基底发生塑性变形而不剥离.     

调制周期对CrAlN/ZrN纳米多层膜韧性的影响

目的研究调制周期对纳米多层膜性能的影响。方法采用磁控溅射方法制备了CrAlN与ZrN的固定厚度比为2.6,不同调制周期(Λ为6,8,10,20 nm)的CrAlN/ZrN纳米多层膜。利用场发射扫描电镜(FESEM)表征薄膜的形貌、结构。用Dektak150型台阶仪测薄膜表面粗糙度。用Agilent Technologies G200纳米压痕仪检测涂层的硬度和弹性模量。用划痕仪测薄膜/基材的结合力,同时,引入抗裂纹扩展系数(CPR)表征纳米多层膜的韧性。结果 CrAlN/ZrN纳米多层膜断面皆为穿晶柱状结构,调制周期为20 nm时,多层膜层与层之间的界面清晰;多层膜表面呈致密的花椰菜状,厚度均约为2μm。调制周期为8 nm时,硬度为20.4 GPa,进一步增大调制周期,硬度下降。调制周期为8 nm的多层膜临界载荷L_(c2)为18 N,CPR值为73.2,L_(c2)与CPR值均高于其他调制周期的多层膜。在临界载荷L_(c2)处,裂纹扩展导致薄膜发生了严重的片状剥落,露出了亮白的热轧钢基底,薄膜失去了保护作用。结论实验表明,在多层膜厚度、调制比不变的条件下,改变调制周期能够改变多层膜的韧性。随着调制周期的增大,韧性呈先上升、后下降的趋势。调制周期为8 nm时,纳米多层膜的硬度最高,韧性最好,综合性能良好。     

调制周期对TiN/Ti多层膜组织结构和结合力的影响

为了阐明调制周期对薄膜微观组织及薄膜与基体结合力的影响,采用反应磁控溅射在Ti6Al4V基板上交替沉积了Ti层及TiN层制备了TiN/Ti多层膜。利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、显微硬度仪和划痕仪测量分析了薄膜的晶体结构、微观组织、硬度以及薄膜与基体之间的结合力。研究结果表明:TiN/Ti多层膜中均存在TiN,Ti和Ti2N 3种相。TiN/Ti多层膜均以柱状晶方式生长,在调制周期较大(5层)时,TiN和Ti层的界面清晰;随着调制周期的减小(层数增加),TiN和Ti层的界面逐渐消失。与单层TiN薄膜相比,多层TiN/Ti薄膜的硬度显著提高;但随着薄膜层数的增加,多层TiN/Ti薄膜硬度略微降低。当调制周期为80nm(30层)时,薄膜与基体的结合力明显提高,达到73N。     

调制周期对Cr/CrN多层膜结构及性能的影响

采用电弧离子镀技术在6Cr13Mo低碳马氏体不锈钢基材表面沉积不同调制周期的Cr/CrN多层膜。利用扫描电镜、显微硬度仪、划痕仪、压痕仪、摩擦磨损试验机、3D轮廓仪研究Cr/CrN多层膜的结构和性能。结果表明:调制周期的变化对Cr/CrN多层膜硬度影响较小;随着调制周期的减小,Cr/CrN多层膜致密性逐渐提高;不同调制周期下,Cr/CrN多层膜与基体结合力均在100 N以上,其中调制周期为321 nm的Cr/CrN多层膜的韧性及与基体结合性能最优;调制周期为569 nm的Cr/CrN多层膜的磨损率最低。     

调制周期对Cr/CrN纳米多层膜的结构与性能的影响

采用多弧离子镀技术在65Mn钢表面制备了不同调制周期的Cr/CrN纳米多层膜.采用俄歇能谱仪(AES)、扫描电子显微镜(SEM)、X射线衍射仪(XRD)、纳米硬度仪、轮廓仪和划痕仪,分析了不同调制周期Cr/CrN纳米多层膜的成分分布、微观结构、力学性能、残余应力和结合强度.结果表明,Cr/CrN纳米多层膜的表面平整致密,截面层状调制结构清晰,其调制结构为Cr层-过渡层-CrN层的"三明治"结构,调制比约为1∶ 1.多层膜由CrN、Cr2N和Cr相组成,在CrN(200)方向上出现择优取向.当调制周期为80 nm时,多层膜的硬度值相对较高.随调制周期的增大,Cr/CrN多层膜的残余应力值减小,结合强度值先增大后减小.当调制周期为120 nm时,涂层的划痕临界载荷值相对较高,为69 N.     

电流密度对7075铝合金微弧氧化膜层组织与性能的影响

在硅酸盐电解液体系中对7075铝合金表面采用微弧氧化(MAO)法制备陶瓷膜层,并借助扫描电镜、三维立体显微镜、X射线衍射仪、显微硬度计、涂层附着力划痕仪和摩擦磨损实验机等对微弧氧化膜层的形貌及性能进行研究。结果表明:电流密度对微弧氧化膜层的组织与性能有较大影响。α-Al_2O_3是微弧氧化膜层的主要组成相,微弧氧化膜层具有较好的显微硬度及耐磨性能。当电流密度达到10 A/dm~2时,膜层的显微硬度与耐磨性能最优。     

Tribological behavior of CrN/WN multilayer coatings grown by ion-beam assisted deposition

CrN monolayer coating and CrN/WN multilayer coatings were deposited on the silicon (100) substrate by ion-beam assisted deposition process. The bilayer period of these coatings was controlled at 8 nm and 30 nm. The cross-sectional morphology of nanoscaled multilayer coatings was characterized by scanning electron microscopy and transmission electron microscopy. The wear resistance of CrN/WN multilayer coatings and CrN monolayer coating was investigated using a pin-on-disc tribometer. The surface roughness (Ra) of the coatings was evaluated by atomic force microscopy, and that of CrN and WN monolayer coating was 6.7 and 5.9 nm, respectively. The employment of multilayer configuration in CrN/WN coating with bilayer period of 8 nm and 30 nm effectively reduced the surface roughness down to 1.9 and 2.2 nm, respectively. The friction coefficient of CrN monolayer coating and CrN/WN multilayer film with a bilayer period of 30 nm was 0.63 and 0.31, respectively. Owing to the high hardness/elastic modulus ratio, as well as the dense structure and the smooth surface roughness, the CrN/WN multilayer coatings exhibited better wear resistance in the consideration of friction coefficient and the worn surface morphology.     

Synthesis and characterization of multilayer CrN/ZrN coatings

In this study, multilayer CrN/ZrN coatings with various bi-layer periods (δ) were deposited by closed-field unbalanced magnetron sputtering and their compositions, crystalline structures and morphologies were characterized by auger electron spectroscopy (AES), X-ray diffraction (XRD) and transmission electron microscopy (TEM). Additionally, the mechanical properties of the coatings were characterized by nano-indentation and wear tests. The XRD results showed that the diffraction peak of multilayer CrN/ZrN coatings is observable between the CrN (111) and the ZrN (111). This peak has a strong tendency to increase the intensity and sharpen the width as the substrate rotation speed increases, indicating that the grain size of the multilayer CrN/ZrN coatings gradually increases. The hardness of films was dependent on the bi-layer period (δ), and the maximum hardness and elastic modulus were approximately 31.8 GPa and 321.5GPa, respectively. Moreover, the results of the wear tests showed that the multilayer CrN/ZrN coatings exhibited greatly improved wear resistance compared to the monolithic CrN coatings.     

Preparation of TiAlN/ZrN and TiCrN/ZrN multilayers by RF magnetron sputtering

Titanium-based nitride coatings on cutting tools, press molds and dies can be used to prolong their life cycle because of their superior corrosion and oxidation resistance. TiAlN/ZrN and TiCrN/ZrN multilayer coatings were prepared by RF magnetron sputtering, and their microstructural evolution and corrosion resistance during heat treatment were investigated. The TiAlN/ZrN and TiCrN/ZrN multilayer coatings are degraded by heating up to 600 °C with the formation of oxides particles on the surface. During the heat treatment, the TiCrN/ZrN and TiAlN/ZrN multilayer coatings show the lowest corrosion current density and the highest polarization resistance at temperature range of 400–500 °C. Consequently, the TiAlN/ZrN and TiCrN/ZrN multilayer coatings show good corrosion resistance at temperature range of 400–500 °C during heating.     

Mechanical and tribological properties evaluation of cathodic arc deposited CrN/ZrN multilayer coatings

Five nanostructured CrN/ZrN multilayer coatings were deposited periodically by cathodic arc evaporation. The bilayer periods of the CrN/ZrN multilayer coatings were controlled in the range of 5 to 30 nm. The structures and bilayer period of the multilayer coatings were characterized by an X-ray diffractometer. The microstructures of thin films were examined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. Nanoindentation, scratch tests, Daimler–Benz Rockwell-C (HRC-DB) adhesion tests, microhardness and pin-on-disk wear tests were used to evaluate the hardness, adhesion, indentation toughness and tribological properties of thin films, respectively. It was found that the hardness and tribological properties were strongly influenced by the bilayer period of the CrN/ZrN multilayer coatings. An optimal combination of mechanical properties and excellent tribological behavior was found for a coating with a critical bilayer period of 30 nm.     

调制结构对TiN/TaN多层膜的生长行为及力学性能的影响

利用反应磁控溅射方法,制备了调制周期相同而调制比不同的TiN／TaN多层膜．利用XRD,HRTEM和纳米压痕仪分别对多层膜的结构、微观状态和力学性能进行了系统研究．结果表明：调制结构不仅改变多层膜的生长速率,而且能导致多层膜择优生长取向的变化;界面应力的存在使得薄膜生长速率随沉积层厚度的增加而下降;在TiN／TaN多层膜中存在着各自独立外延生长的[111]和[100]两种取向的调制结构,且具有不同的调制周期;调制周期为6nm左右的TiN／TaN多层膜的硬度与弹性模量分别提高约50％与30％;在调制比为3：1时,硬度最大值为34．2GPa,弹性模量为344．9GPa;根据结构和力学性能的分析结果,讨论了TiN／TaN多层膜的硬化机制．     

Characterization and wear properties of nanoscaled TiN/TaN multilayer coatings

The structural, morphological, mechanical and tribological characterization of nanoscaled multilayer TiN/TaN coatings deposited by magnetron sputtering technology were investigated by low angle X-ray diffractometry, high angle X-ray diffractometry, atomic force microscopy, microhardness, pin-on-disc testing and 3-D surface profiler. The results show that the TiN/TaN coatings exhibit good modulation period and sharp interface between TiN and TaN layers. In mutilayered TiN/TaN coatings, TiN layers have cubic structure, but hexagonal structure emerged among TaN layers besides cubic structure as modulation period is beyond 8.5 nm. The mierohardness is affected by modulation period and the maximum hardness value of 31.5 GPa appears at a modulation period of 8.5 rim. The coefficient of friction is high and the wear resistance is improved for TiN/TaN coatings compared with those of TiN coating; the wear mechanism exhibits predominantly ploughing, material transfer and localized spallation.     

气相沉积 Ti / TiN 多层薄膜的力学及耐腐蚀性能研究

目的研究多层薄膜的界面对薄膜性能的影响。方法通过直流磁控溅射法在45#钢表面制备Ti N及Ti/Ti N多层薄膜,采用扫描电镜和XRD衍射分析仪对薄膜表面形貌及相结构进行观察和分析,使用纳米压痕仪、电子薄膜应力分布测试仪对Ti N及Ti/Ti多层薄膜的力学性能以及残余应力大小进行研究,并运用电化学设备对Ti N及不同调制周期的Ti/Ti多层薄膜的耐腐蚀性能进行研究。结果制备的Ti N及Ti/Ti N多层薄膜表面光滑且结构致密,Ti N晶粒细小且为非晶相;薄膜力学性能良好,内部均存在残余压应力。随着调制周期的减小,弹性模量和硬度先减小后增大,内部残余应力逐渐减小且分布不均匀程度逐渐增大。薄膜在H_2SO_4中的腐蚀试验表明:当Ti/Ti N多层薄膜调制周期为1μm时,多层薄膜的耐腐蚀性能不如Ti N薄膜,随着Ti/Ti N多层薄膜随调制周期的减小,多层薄膜的耐腐蚀性能逐渐升高;当调制周期为0.5μm时,Ti/Ti N多层薄膜的耐蚀性能已超过Ti N薄膜。结论 Ti/Ti N多层薄膜界面的增多有助于减小薄膜的残余应力,并且可提高薄膜的耐蚀性能。     

磁控溅射CrTiN涂层和PECVD DLC涂层在银币压印模上的应用

在ASSAB 635冷作模具钢试样表面分别采用磁控溅射物理气相沉积技术（PVD）和等离子增强化学气相沉积技术（PECVD）涂覆了厚度约为2μm的CrTiN涂层和DLC涂层。用扫描电镜（SEM）、X射线衍射仪（XRD）和激光拉曼光谱仪（LRS）对涂层的微观结构及物相进行了分析。采用维氏硬度试验。划痕和压坑试验分析了涂层厚度和涂层与基体的结合力。对涂覆CrTiN、DLC涂层的银币模具进行了应用试验。研究结果表明：CrTiN涂层的主要组成为CrN相和TiN相;DLC涂层（类金刚石）主要为SP^3键和SP^2键的混合结构,其中SP^2键的含量较高。两种涂层表面平滑致密,结合力的临界载荷大于60N;显微硬度分别为1967 HV0．01和2883 HV0．01。与传统化学镀铬相比较,磁控溅射CrTiN涂层能有效延缓模具表面“闪金光”现象的出现,模具寿命提高3倍以上。     

Microstructure, mechanical and tribological properties of CrN/W2N multilayer films deposited by DC magnetron sputtering

CrN/W₂N multilayer films with various bilayer periods of 15-85 nm were deposited on high speed steel (W18Cr4V) substrates by means of DC closed field unbalanced magnetron sputtering. The morphology and microstructure of the multilayer films were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM). The mechanical and tribological properties were evaluated using a nanoindentor, Rockwell and scratch tests and a conventional ball-on-disk tribometer, respectively. There were some transverse grains at the layer interface and the interface between the CrN and W₂N layers was not so sharp owing to atom diffusion through the interface. In the bilayer period range, the microhardness, elastic modulus and adhesive strength of the CrN/W₂N multilayer films increased with the decrease of bilayer period. The CrN/W₂N multilayer film with a bilayer period of 15 nm showed the highest hardness (29.2 GPa), elastic modulus (376 GPa) and best adhesion strength, it also had the highest wear resistance and lowest friction coefficient.