Multilayered gradient CrN/ZrN coatings synthesized by magnetron sputtering

The multilayer gradient CrN/ZrN coatings were synthesized by a dual cathode DC magnetron sputtering.The influence of different species of reaction gases and partial pressures on structure and mechanical properties was investigated using XRD, AES, XPS, and nanoindentation. The results show that N2-NH3 mixture process gas is of benefit to the synthesis of superhard multilayered gradient CrN/ZrN coatings. The presence of the preferred orientations of CrN(111), (200) and ZrN (111), (220) in the structure is a main reason for superhardness of multilayered gradient coatings.     

直流、射频磁控溅射制备钌薄膜的微观结构及电学性能分析

为了探索直流和射频磁控溅射制备钌薄膜的微观结构及性能差异,进而指导薄膜制备工艺优化。采用直流和射频磁控溅射法在SiO2/Si(100)衬底上沉积不同时间和温度的钌薄膜;通过高分辨场发射扫描电镜、X射线衍射仪、原子力显微镜、四探针等方法研究不同溅射电源下制备的钌薄膜的微观结构和电学性能。结果表明,在相同溅射条件下,DC-Ru薄膜的结晶性优于RF-Ru薄膜;其厚度大于RF-Ru薄膜,满足tDC≈2tRF;其沉积速率高于RF-Ru薄膜,满足vDC≈2vRF。然而,其电阻率却高于RF-Ru薄膜,这主要得益于RF-Ru薄膜的致密度较高,从而降低了电子对缺陷的散射效应。     

采用中频反应磁控溅射技术沉积氮化锆薄膜

采用中频反应磁控溅射技术沉积ZrN薄膜,在真空镀膜机内对称安装了3对矩形孪生靶.利用等离子体发射光谱和质谱仪QMS200分别实时监控真空炉内靶材表面的谱线变化和各种气氛的分压强,并通过控制系统氮气流量自动调控,从而消除了靶中毒和打火现象,确保了溅射镀膜的稳定进行.通过对氮化锆膜层的显微组织观察、X射线衍射和俄歇半定量分析,沉积的氮化锆薄膜膜层致密,与基体的结合牢固.结果表明:当炉内氮气分压强为45%,控制靶电压200V,靶电流为25A,逐步调节Ar与N2比例,可获得成分均匀,膜层致密,结合力较好的金黄色氮化锆薄膜.     

磁控溅射温度与时间对ZrN薄膜附着力的影响

采用非平衡磁控溅射技术在1Cr18Ni9Ti不锈钢上制备了ZrN薄膜。用SEM、EDS观察并分析了薄膜的表面形貌和成分,用光电轮廓仪测量了膜层厚度。并采用划格法测试不同溅射时间和温度制备的薄膜附着力大小。分析不同溅射时间和温度对薄膜附着力的影响规律。结果表明,通过调节磁控溅射时间和温度可以得到具有一定厚度,成分稳定,结构致密的ZrN薄膜,且溅射时间在1～20 min范围内时间越长薄膜附着力越大,溅射时间超过20 min,附着力趋于稳定;溅射温度在30～90℃范围内温度越高薄膜附着力越大,超过90℃溅射温度继续升高附着力减小。     

Influence of bilayer period and thickness ratio on the mechanical and tribological properties of CrSiN/TiAlN multilayer coatings

Nanostructured CrSiN/TiAlN multilayer coatings were deposited by a bipolar asymmetric reactive pulsed DC magnetron sputtering system. The thickness ratio of CrSiN to TiAlN layers was fixed at 1:1. The bilayer periods of the coatings were controlled to be from 6 to 40 nm. Furthermore, two CrSiN/TiAlN multilayer coatings with the same bilayer period (20 nm) but different CrSiN/TiAlN thickness ratios (2:8 and 8:2) were also deposited to explore the influence of thickness ratio on the mechanical properties of the multilayer coatings. The crystalline structures of the coatings were determined by a glancing angle X-ray diffractometer. The microstructures of thin films were examined by a scanning electron microscopy and a transmission electron microscopy, respectively. A nanoindenter, a micro Vickers hardness tester, and a pin-on-disk wear tester were used to evaluate the hardness, the toughness and the tribological properties of the thin films, respectively. The maximum hardness of the multilayers was obtained when the bilayer period was at 10 nm for the coating with the same thickness ratio of CrSiN to TiAlN layers (1:1). Meanwhile, the thickness ratio of CrSiN to TiAlN layer had great influence on the hardness and the toughness properties of the multilayer coatings. The hardness and the toughness of the CrSiN/TiAlN multilayer coatings increased as the individual TiAlN layer thickness increased.     

Microstructures and mechanical properties evaluation of TiAlN/CrSiN multilayered thin films with different bilayer periods

The Ti_0.45Al_0.55N/Cr_0.75Si_0.25N nanoscale multilayered coatings were deposited periodically by a bipolar asymmetric pulsed DC reactive magnetron sputtering technique. The structures and bilayer period of multilayer coatings were characterized by an X-ray diffractometer. The surface and cross-sectional morphologies of thin films were examined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. The surface roughness of thin films was explored by atomic force microscopy (AFM). A nanoindenter, a micro Vickers hardness tester and pin-on-disk wear tests were used to evaluate the hardness, fracture toughness and tribological properties of the thin films, respectively. Six coatings with bilayer period ranges from 6 nm to 40 nm were produced in this work. It was observed that the hardness increased with increasing bilayer period and reached the maximum at 12 nm and then leveled off at periods larger than 12 nm. An optimal hardness, and plastic deformation resistance, as well as adequate tribological behaviors were found on the coating with a critical bilayer period of 12 nm.     

痕法测定 TiAlN 涂层结合强度的研究

采用磁控溅射法在不锈钢表面制备了TiAlN涂层,采用压入法及划痕法表征了涂层的结合强度。分析表明,压入法只能作为一种定性的测定方法,该法测得TiAlN涂层的结合强度达到HF3。划痕法结合了声信号、摩擦力信号和划痕微观形貌,可以定量测定结合强度,该法测得在压头曲率半径为200μm的情况下,TiAlN涂层的临界载荷达到13 N,比传统TiN涂层提高了45%。     

基于X射线反射研究溅射工艺对CrAlN/TiAlN周期膜界面结构的影响

为研究X射线反射技术在纳米多层膜界面微结构表征中的应用,采用反应磁控溅射技术在单晶硅基片上制备CrAlN/TiAlN纳米周期膜,利用X射线反射技术系统研究溅射工艺参数对CrAlN/TiAlN纳米周期膜界面微结构的影响规律。结果表明:增加铝靶功率可提高膜层的溅射速率和降低膜层的界面粗糙度,然而较高的铝靶功率会使膜层界面出现严重的弥散;较大和较小的负偏压都不利于形成完整的周期膜调制结构和光滑的界面;提高Ti/Cr靶电流可有效改善周期膜的调制界面结构,但太大的靶电流会导致膜层间扩散加重,形成弥散界面。N2流量与Ar流量对膜层界面粗糙度具有相反的影响作用。试验得到的优化工艺参数为:铝靶功率80W,溅射负偏压-200 V,Ti/Cr靶电流0.2A,N2流量30cm~3/min,Ar流量10cm~3/min。     

Cu互连中Zr嵌入层对ZrN阻挡层热稳定性的影响

在不同的衬底偏压下,用射频反应磁控溅射的方法在Si(100)衬底和Cu膜间制备了ZrN/Zr/ZrN堆栈结构的阻挡层。研究了Zr层的插入对ZrN扩散阻挡性能的影响,结果表明:随着衬底偏压的升高,阻挡层的电阻率降低,ZrN呈(111)择优取向;Zr层的插入使ZrN阻挡层的失效温度至少提高100℃,750℃仍能有效地阻止Cu的扩散,阻挡性能提高的主要原因可能是高温退火时形成的ZrO2阻塞了Cu快速扩散的通道。     

Modified TiAlN coatings prepared by d.c. pulsed magnetron sputtering

Coatings like TiN or TiAlN are well established as hard and wear resistant tool coatings. These coatings often are prepared by PVD techniques like arc evaporation or d.c. magnetron sputtering. Typical micro hardness values of such hard coatings are in the range of 30 GPa. Compared to d.c. magnetron sputtering processes the pulsed magnetron sputter deposition technique could be shown as a clear advancement. Furthermore pure TiAlN hard coatings as well as TiAlN coatings modified by addition of elements like Si and Cr were prepared in order to improve the coating properties using the pulsed magnetron sputter technique in a batch coater equipped with 4 targets. Coatings prepared with the pulsed sputter process showed both high hardness and high wear resistance. The application potential of pulsed sputtered TiAlN coatings is demonstrated by turning test results of coated cemented carbide cutting inserts.Beside hardness and wear, other properties like adhesion or high temperature stability were determined. Cross sectional SEM images revealed the growth structure in dependence of the applied substrate bias and of the added elements. The chemical composition of the coatings was investigated by electron microprobe analysis and the phase and crystal size were determined by X-ray diffraction. Using the pulsed magnetron sputter process the coating properties, especially the hardness and the morphology, could be significantly improved. With indentation hardness values in the range of 40 GPa the region of super hard materials could be reached.     

退火处理对不同RF功率下制备ZnO薄膜的结晶性能的影响

采用RF磁控溅射法,在不同溅射功率下在玻璃衬底上制备了ZnO薄膜,并对所制备的ZnO薄膜在空气气氛中进行了不同温度（350-600℃）的退火处理.利用X射线衍射仪（XRD）、扫描电子显微镜（SEM）等研究了退火对不同溅射功率条件下制备的ZnO薄膜晶体性能和应力状态的影响.研究表明,在衬底没有预热的情况下,较低功率（190W）下制备的ZnO薄膜,当退火温度为500℃时,能获得单一c轴择优取向和最小半高宽,张应力在350℃退火时最小;较高功率（270W）下,薄膜最佳c轴取向和晶粒度在600℃退火温度获得,张应力最小的退火温度在350-500℃之间.当衬底预热至300℃时,退火处理对两种功率下制备的薄膜的结晶性能和应力的影响基本一致.     

TiAlN/CrN多层膜的组织结构及耐蚀性机理

目的研究Ti AlN/CrN多层膜及Ti AlN、Cr N单一膜层的微观组织和电化学性能区别,分析不同结构薄膜材料的耐腐蚀性影响因素。基于电化学参数、组织结构和腐蚀形貌特征,为开发新型腐蚀性薄膜提供理论依据。方法采用多弧离子镀方法,在316不锈钢基底上先沉积150 nm Cr薄膜作为过渡层,然后交替沉积Cr N薄膜和Ti AlN薄膜,制备单层厚度为10 nm的Ti AlN/CrN多层膜。作为对比,制备单一Ti AlN、CrN薄膜。通过SEM、XRD表征薄膜断面形貌、组织结构,并分析耐蚀机理,结合极化曲线和阻抗谱对三种涂层进行电化学性能分析,最后对涂层进行浸泡腐蚀试验。结果 Ti Al N/Cr N纳米多层膜为面心立方结构,呈现共格外延生长,且呈(200)择优取向。纳米多层膜的动电位极化曲线测量结果与不锈钢基体和单层薄膜相比,其腐蚀电位正移为-0.36 V,腐蚀电流密度降低为0.501μA/cm²,极化电阻为120 kΩ·cm²。阻抗谱试验结果表明,相比较于单层膜和基体,Ti Al N/Cr N多层膜的CPE值最低,为29.83×10^...     

Effect of NbN and ZrN films formed by magnetron sputtering on Ti and porcelain bonding

Niobium nitride (NbN) and zirconium nitride (ZrN) were deposited on Ti substrates by direct-current (DC) reactive magnetron sputtering; the deposited NbN and ZrN films served as intermediate layers of a Ti and porcelain interface. X-ray diffraction (XRD) results proved that the deposited NbN and ZrN films were polycrystalline with a cubic microstructure. The Ti and porcelain bonding strength of the samples in Group Control (27.2 ± 0.75 MPa), Group NbN (43.1 ± 0.59 MPa), and Group ZrN (52.4 ± 0.80 MPa) were measured. The surface roughness in the case of Group Control (1.863 ± 0.10 μm), Group NbN (2.343 ± 0.07 μm), and Group ZrN (2.346 ± 0.10 μm) was also investigated. Statistical analysis showed that both films helped improve the Ti and porcelain bonding strength and increase the surface roughness. Scanning electron microscopy (SEM) results showed that no apparent oxide layer was formed at the Ti and porcelain interface in both Group NbN and Group ZrN. Energy-dispersive X-ray spectroscopy (EDS) results showed that ZrN was more effective in preventing Ti oxidation than was NbN. Overall, the experimental results showed that the deposition of both NbN and ZrN films helps improve the Ti and porcelain bonding strength and that ZrN films are more effective.     

Effect of the PbOx thickness on the microstructure and electrical properties of PLT thin films prepared by RF magnetron sputtering

The (Pb_0.90La_0.10)Ti_0.975O₃ (PLT) thin films with different thicknesses of PbO_x buffer layers were deposited on the Pt(111)/Ti/SiO₂/Si(100) substrates by RF magnetron sputtering technique. The PbO_x buffer layer leads to the (100) orientation of the PLT thin films. Effects of the PbO_x thickness on the microstructure and electrical properties of the PLT thin films were investigated. The experimental results show that the PbO_x thickness plays an important role on the orientation, phase purity, domain structure, and electrical properties of the PLT thin films. The PLT thin films with proper PbO_x thickness possess highly (100) orientation, high phase purity, strong intensity of out of plane polarization, and good electrical properties. It is concluded that the PbO_x thickness between PLT thin films and Pt coated Si substrate is very critical to obtain good electrical properties.     

非平衡磁控溅射Cp/AlSn镀层组织结构与性能

利用非平衡磁控溅射离子镀技术在铝基轴承合金表面沉积Cp/Al Sn复合镀层。采用原子力显微镜(AFM)和扫描电子显微镜(SEM)对镀层的微观形貌进行观察,并对镀层的维氏硬度和摩擦学性能进行了测试。结果表明,非平衡磁控溅射离子镀Cp/Al Sn镀层,当碳靶电流在0.2~0.8 A范围内,镀层呈等轴结构生长,随碳靶电流增大,镀层晶粒逐渐细化,且致密度增加;在Cp/Al Sn复合镀层中,Al、Sn和C元素分别以单质形式存在,且随掺碳量增加,Cp/Al Sn复合镀层非晶特征逐渐增强;随碳靶电流增加,镀层硬度增加,摩擦系数减小,电流为0.8 A时,镀层硬度最高为230 HV0.025。摩擦系数最低为0.09,磨损率先减小后增大,碳靶电流为0.4 A时,镀层的磨损率最低为6.6×10-16m3/(N·m),其磨损机制逐渐由粘着磨损转变为磨粒磨损。     

Characteristic comparison of metal films coated onto the cenosphere by chemical and magnetron sputtering methods

Metal-coated cenospheres have been widely used in Industries. Different coating methods result in different characteristic metal films. Hie metal film on the cenosphere by chemical coating does not appear to be very smooth, exhibiting metal piled up and pin holes on the surface and leaving some spots uncoated. Meanwhile, the metal film is not tightly absorbed onto cenospheres and is easy to peel off. However, the metal film prepared by magnetron sputtering is compact, smooth and without pin holes. The film has good affinity to the cenosphere surface. Such films do not separate with it even when the cenosphere is crushed. Both the metal films give the same XRD patterns, indicating tnat the crystal structure of the metal films by these two methods is the same. Chemical coating is a complex process and harmful to the environment, but it fits ultrafine powder coating (the particle size can be less than 2 μm). The magnetron sputtering method is environmental friendly and works quickly, but this method requires specially designed equipment and does not work for ultrafine powders. If the particle size is less than 30 μm, the coating process is hard to carry on.     

反应磁控溅射制备Ti-Si-N薄膜的摩擦磨损性能

用反应磁控溅射方法,在不锈钢表面沉积Ti-Si-N薄膜.用原子力显微镜观察薄膜的表面形貌,Ti-Si-N颗粒尺寸小于0.1 μm,用亚微压入仪测试薄膜硬度,当硅的摩尔分数为9.6%时,薄膜硬度出现最大值47 GPa.球-盘式摩擦磨损结果表明,Ti-Si-N薄膜的耐磨性能明显优于TiN薄膜,加入少量硅元素后,TiN薄膜的抗磨损性能有显著提高,但Ti-Si-N薄膜的室温摩擦系数较高(0.6～0.8),高温下摩擦系数也仅轻微降低(550℃,0.5～0.6).由于Ti-Si-N薄膜的摩擦系数可能与磨损中氧化物生成量的增加有关,常温下Ti-Si-N薄膜的摩擦系数随硅摩尔分数的增加而增大,而高温下Ti-Si-N薄膜的摩擦系数随硅含量上升而降低.     

Magnetron sputtering deposition of [FePt/Ag]n multilayers for perpendicular recording

[FePt/Ag]n multilayers were deposited on glass substrates by RF magnetron sputtering and ex situ annealed at 550℃ for 30 min. The effects of inserted Ag layer thickness and the number of bilayer repetitions （n） on the structure and magnetic properties of the multilayers were investigated. It was found that the difference between in-plane and out-of-plane coercivities varied with an increase of inserted Ag layer thickness in the [FePt 2 nm/Ag x nm]10 multilayers. The ratio of out-of-plane coercivity to in-plane coercivity reached the maximum value with the Ag layer thickness of 5 nm, indicating that the Ag layer thickness plays an important role in obtaining perpendicular orientation. For the [FePt 2 nm/Ag 5 um]n multilayers, perpendicular orientation is also influenced by n. The maximum value of the ratio of out-of-plane coercivity to in-plane coercivity appeared when n was given as 8. It was found that the [FePt 2 nm/Ag 5 nm]8 had a high perpendicular coercivity of 520 kA/m and a low in-plane one of 88 kA/m, which shows a strong perpendicular anisotropy.     

Effects of Ag layers on the SiO2/FePt thin films deposited by magnetron sputtering

The effects of Ag layers with different locations and thicknesses on the structural and magnetic property of SiO2/FePt multilayer films were investigated.The non-magnetic Ag layer plays an important role in inducing（001） orientation and ordering of FePt grains,as well as the SiO2-doping reducing the grain size and the magnetic exchange coupling between grains.When the 10 nm Ag layer is moved from the bottom to the top of the SiO2/FePt multilayer film,the coercivity gradually decreases;the largest difference between the out-of-plane coercivity and the in-plane one is obtained in the sample of [SiO2（2 nm）/FePt（3 nm）]3/Ag（10 nm）/[SiO2（2 nm）/FePt（3 nm）]2.Furthermore,the location of Ag layers was fixed and the thickness was changed.The XRD curves suggest that the intensity of the（001） peak becomes the strongest with the addition of 10 nm Ag layers.