Characterization and properties of CrN films deposited by ion-source-enhanced middle frequency magnetron sputtering

CrN films with deposition rates of 130-180 nm/min were deposited on Si (111) and carbamide alloy substrates by an ion-source-enhanced middle frequency magnetron sputtering system. Increasing of ion source voltages promoted the growth of CrN films with preferred orientation of (200). The deposited CrN films are composed of nanocrystalline particles with sizes of ∼20 nm embedded in polycrystalline matrix. The hardness of the CrN films increases from 1300 Kg/mm² without ion source bombardment to 2400 Kg/mm² with ion source voltages of 1000 V. Origins for the increasing of hardness can be attributed to dislocation strengthening and densification effects.     

偏压对反应磁控溅射TiN薄膜结构以及性能的影响

本文采用直流反应磁控溅射技术,以Ar和N2为反应前驱气体制备了TiN功能装饰薄膜.重点研究了衬底负偏压对沉积TiN薄膜的色泽、性能及微结构的影响.采用台阶轮廓仪、X射线衍射仪、EDS能谱仪、纳米压痕仪等分析了薄膜的粗糙度、晶相、组分、纳米硬度以及弹性模量.结果表明,采用适宜的衬底负偏压调控轰击离子能量,能够有效阻止薄膜结构中空位以及缺陷的产生,从而有效避免薄膜表面的紫黑色氧化钛的生成,有利于表面光滑的金黄色TiN薄膜制备,同时使薄膜具备更优异的力学性能.实验结果还表明基体偏压可显著影响TiN薄膜的择优生长取向:随偏压增加,薄膜由(111)晶相择优生长转变为(200)晶相的择优生长,(200)晶相的薄膜比(111)晶相薄膜具有更佳的力学性能.     

Microstructures and corrosion behaviors of Zr modified CrN coatings deposited by DC magnetron sputtering

Zirconium modified chromium nitride coatings with various Zr contents have been prepared by a DC reactive magnetron sputtering technique. The detailed investigations in terms of composition, phase structure, morphology and corrosion properties have been performed by GDOES, XRD, SEM and electrochemical measurements, respectively. The as-deposited coatings with Zr contents ranging from 0 to 3.2 at. % form nanocrystalline solid solutions, where Zr substitute Cr in the CrN lattice. With increasing Zr contents, the lattice parameters increase but the grain sizes show little effects. All the coatings exhibit dense compact columnar structures in SEM cross-sectional observations. Electrochemical measurements in 3.5% NaCl solutions revealed that the additions of Zr into CrN coatings improved their chemical inertness. The coated samples with much low corrosion current densities in nA/cm² range show their excellent protective characteristics to the stainless steel substrates. The corrosion mechanism, however, was due to the slight pitting corrosions, which were mainly localized in the growth defects.     

溅射法生长 MgxZn1- xO薄膜的结构和光学特性

用射频磁控溅射法在不同衬底上制备出了MgxZn1-xO薄膜。X射线衍射(XRD)和原子力显微镜(AFM)研究结果表明,薄膜为六角纤锌矿结构,具有(002)方向择优取向;随氧分压增加,(002)衍射峰的角度变大,表征薄膜表面粗糙程度的方均根粗糙度减小。室温光致发光谱中有多个紫外及可见光致发光峰,其中344nm发光峰应来源于近带边发射。室温透射谱表明薄膜在可见光区具有极高的透过率,薄膜的吸收边位于340nm附近,进而估算出Mg、Zn1-xO薄膜的带隙宽度为3．59eV,与光致发光结果一致。     

负偏压对Be上磁控溅射离子镀Al膜结构影响的研究

以Be为基体，采用磁控溅射离子镀的在其上镀制Al膜，研究了负偏压对Al膜微结构的影响；研究表明，不加基体负偏压，Al膜在（111）面择优生长；随着基体负偏压升高Al膜在（111）面择优生长趋势减北，Al膜在（200）面生长趋势加强；当基体负偏压超过150V后，Al膜在（111）面择优生长的趋势又得到加强。晶粒在低负偏压时随负偏压增加而细化，当较高的负偏压引起基体温度升高时，此时晶粒又变大了。     

Effect of substrate temperature on the structure and optical properties of ZnO thin films deposited by reactive rf magnetron sputtering

Zinc Oxide films were deposited on quartz substrates by reactive rf magnetron sputtering of zinc target. The effect of substrate temperature on the crystallinity and band edge luminescence has been studied. The films deposited at 300 °C exhibited the strongest c-axis orientation. AFM and Raman studies indicated that the films deposited at 600 °C possess better overall crystallinity with reduction of optically active defects, leading to strong and narrow PL emission.     

非平衡磁控溅射沉积CrN用于液压杆件的研究

目前液压杆件基本上采用电沉积的方法在基体表面沉积一层Cr膜,以此来满足其耐热、耐磨和抗腐蚀要求,但电沉积Cr不但浪费能源而且对环境和人体健康有着极大的伤害.本文利用非平衡磁控溅射的方法在45#钢表面获得6μm左右的Cr-CrN多层膜,通过对膜层进行物理性能测试、盐雾试验以及装车磨损寿命试验,结果表明利用非平衡磁控溅射方法在液压杆件基体上沉积CrN不仅可取代电沉积Cr,而且使用寿命大大提高.     

Influence of substrate bias voltage on properties of Pt thin films deposited by non-mass separated ion beam deposition method

Pt thin films were deposited on Si substrates by applying a negative substrate bias voltage using a non-mass separated ion beam deposition method. The effect of the substrate bias voltage on the properties of the deposited films was investigated. In the case of Pt thin films deposited without the substrate bias voltage, a columnar structure and small grains were observed. The electrical resistivity of the deposited Pt films was very high (49.3 ± 0.65 µΩ cm). By increasing the substrate bias voltage, no clear columnar structure was observed. At the substrate bias voltage of − 75 V, the resistivity of the Pt film showed a minimum value of 16.9 ± 0.2 µΩ cm closed to the value of bulk (10.6 µΩ cm).     

Preparation of CrN thick films by high-rate middle-frequency unbalanced magnetron sputtering

A middle-frequency (MF) unbalanced magnetron sputtering system equipped with an electron source was designed and used for deposition of CrN thick films under various MF power (1.4–14 kW) at fixed temperature, pressure, and gas flow rate. The deposition rate was increased with increasing MF power and the structure and N/Cr ratio of the deposited CrN films exhibited a complicated behavior, where the CrN films were a polycrystalline structure and the films deposited under optimized conditions exhibited a dense columnar structure and a micro-hardness of 16 GPa. The dependence of the structure and micro-hardness on MF power was interpreted by the power deposition efficiency.     

Mn-doped ZnO transparent conducting films deposited by DC magnetron sputtering

Mn-doped zinc oxide (ZnO:Mn) thin films with low resistivity and relatively high transparency were firstly prepared on glass substrate by direct current (DC) magnetron sputtering at room temperature. Influence of film thickness on the properties of ZnO:Mn films was investigated. X-ray diffraction (XRD) and scanning electron microscopy (SEM) show that all the deposited films are polycrystalline with a hexagonal structure and have a preferred orientation along the c-axis perpendicular to the substrate. As the thickness increases from 144 to 479 nm, the crystallite size increases while the electrical resistivity decreases. However, as the thickness increases from 479 to 783 nm, the crystallite size decreases and the electrical resistivity increases. When film thickness is 479 nm, the deposited films have the lowest resistivity of 2.1 × 10^− 4 Ω cm and a relatively high transmittance of above 84% in the visible range.     

非平衡磁控溅射类金刚石碳膜的性能

用非平衡磁控溅射的方法在室温下制备了光滑、均匀、致密的类金刚石(DLC)薄膜,分析和研究了DLC膜的形貌、结构和摩擦特性.结果表明,靶工作电流对DLC膜的沉积有重要的影响.随着工作电流的增大,薄膜的沉积速率增大,薄膜中sp3键的含量增加.薄膜的摩擦系数随着工作电流的增加略有增大,在摩擦的初始阶段,摩擦系数较高,随着摩擦循环次数的增加,摩擦系数逐渐减小,并逐渐趋于稳定.     

Effect of substrate temperature and bias voltage on the crystallite orientation in RF magnetron sputtered AlN thin films

The crystal orientation and residual stress of AlN thin films were investigated using X-ray diffraction and substrate curvature method. The AlN films were deposited on Si(100) by RF magnetron sputtering in a mixed plasma of argon and nitrogen under various substrate negative bias V_s (up to − 100 V) and deposition temperature T_s up to 800 °C. The results show that lower temperature and moderate bias favor the formation of (002) plane parallel to the substrate surface. On the contrary, strong biasing beyond − 75 V and deposition temperature higher than 400 °C lead to the growth of (100) plane. At the same time nanoindentation hardness and compressive stress measured by substrate curvature method showed significant enhancement with substrate bias and temperature. The biased samples develop compressive stress while unbiased samples exhibit tensile or compressive stress depending on plasma power and temperature. The relationships between deposition conditions and crystallographic orientation of the films are discussed in terms of surface energy minimization and ion bombardment effects.     

Influence of annealing on thermoelectric properties of bismuth telluride films grown via radio frequency magnetron sputtering

Bismuth telluride films were prepared via radio frequency magnetron sputtering. Mixed powders with different composition were used as sputtering targets. Influence of the annealing temperature on surface topography, crystal structure and thermoelectric properties of the films has been investigated. It was found that the grain size increased and the surface roughness decreased with a rising annealing temperature. X-ray diffraction analysis revealed an improved crystallization after the annealing, and that crystal planes perpendicular to c-axis became prominent. High temperature treatments resulted in a decrease of Seebeck coefficient and an increase of electrical conductivity. The highest power factor was obtained after being annealed at 300 °C.     

硅靶中频反应磁控溅射二氧化硅薄膜的特性研究

报道了中频双靶反应磁控溅射制备二氧化硅（SiO2)薄膜的装置、工艺及薄膜特性。对制备的SiO2薄膜的化学配比和元素化学态进行了SAM和XPS分析，测试了膜层对钠离子（Na^ )阻挡性能、光学折射率和可见光的透过率。研究表明作者开发的中频双靶反应磁控溅射沉积SiO2薄膜的设备和工艺可以高速率、大面积制备高质量的SiO2膜。     

Structural characterization of ZnO thin films deposited by dc magnetron sputtering

In this work we present recent results on ZnO thin films grown by dc magnetron sputtering technique at room temperature (RT), focusing on structural and surface characterization using conventional cross-section transmission electron microscopy (XTEM) and high resolution cross section transmission electron microscopy (HRXTEM) in an attempt to understand the thickness influence on film, mechanical and optical properties as well as photoreduction/oxidation conductivity changes. Films were found to be polycrystalline with a columnar mode of growth. For films with thickness over 100 nm, XTEM and HRTEM analysis evidenced the presence of a small grains transition layer near interface with the substrate, feature which plays an important role in ZnO thin films for gas sensing application. The control of such structural parameters is proved to be critical for the improvement of their gas sensing performance.     

Influence of annealing temperature on the properties of ZnO:Zr films deposited by direct current magnetron sputtering

Transparent conducting zirconium-doped zinc oxide (ZnO:Zr) films were deposited on quartz substrates by direct current (DC) magnetron sputtering at room temperature. The influence of post-annealing temperature on the structural, morphological, electrical and optical properties of ZnO:Zr films were investigated. When annealing temperature increases from room temperature to 573 K, the resistivity decreases obviously due to an improvement of the crystallinity. However, with further increase in annealing temperature, the crystallinity deteriorates leading to an increase in resistivity. The films annealed at the optimum annealing temperature of 573 K in vacuum have the lowest resistivity of 9.8 × 10⁻⁴ Ω cm and a high transmittance of above 92% in the visible range.     

中频磁控反应溅射AlN薄膜及微观结构研究

采用中频磁控反应溅射工艺进行了氮化铝薄膜的制备,对沉积速率、晶体结构和表面形貌与氮气流量和溅射功率之间的变化关系进行了研究。结果表明,通过调节N2流量和溅射功率选择性地获得非晶态和沿着c轴方向择优生长的晶态AlN薄膜。在化合物沉积模式下,增加溅射功率和增加反应气体流量均有利于获得非晶态AlN薄膜,并且减小薄膜表面粗糙度,获得光滑的AlN薄膜,并采用薄膜生长原理对这种现象进行了解释。     

非平衡磁控溅射DLC薄膜应力研究

类金刚石（DLC）薄膜可用作红外增透保护膜,高的薄膜残余应力造成薄膜附着力下降是目前应用中存在的主要问题之一。本文从DLC薄膜作为红外增透保护膜的需求出发,采用非平衡磁控溅射技术生长DLC薄膜。实测了薄膜的残余应力,分析研究了薄膜残余应力在不同工艺条件下的变化情况。探讨了薄膜残余应力与薄膜厚度、光学透过率、离子能量、沉积速率以及能流密度之间的关系。研究结果表明,薄膜残余应力平衡值在0．9～2．2GPa之间,相应的单面镀膜样片的透过率在4μm波长处为69％～63％,随工艺的不同而变化。工艺优化后薄膜残余应力显著下降。硅基底上薄膜与基底剥离的力的临界值大于2160GPa．nm,最大薄膜厚度≥2400nm;锗基底上最大薄膜厚度≥2000nm,可以满足整个红外波段的需求。     

The phase and microstructure of CrAlN films deposited by pulsed dc magnetron sputtering with synchronous and asynchronous bipolar pulses

CrAlN films have been deposited from a Cr target and an Al target using pulsed dc magnetron sputtering. The Cr and Al targets were pulsed in asynchronous and synchronous pulsing modes at different pulsing frequencies and duty cycles. The ion energy distributions of the plasma were characterized by a Hiden mass spectrometer. The pulsed plasma contains a wide range of energetic ions. The ion energies depend on the pulsing parameters and the pulsing mode of the two targets. The ion energy and ion flux increased as the pulsing frequency was increased. The plasma exhibited higher ion energies and ion fluxes in the synchronous pulsing mode than those in the asynchronous pulsing mode for the same pulsing frequency and duty cycle. A decrease in the N content and an increase in the Al/(Cr + Al) ratio were observed as the pulsing frequency was increased in both pulsing modes. When the pulsing frequency was increased to 350 kHz, the films deposited in the asynchronous pulsing mode exhibited a NaCl cubic structure, whereas a mixture of the cubic and hexagonal phases was formed in the films deposited in the synchronous pulsing mode. The hardness of the films increased with an increase in the pulsing frequency in the asynchronous pulsing mode. In contrast, a decrease in the hardness was found in the synchronously deposited films as the pulsing frequency was increased due to the formation of hexagonal AlN phase and the stress relaxation in the films.     

Dependence of the electrical and optical properties on the bias voltage for ZnO:Al films deposited by r.f. magnetron sputtering

Aluminum-doped zinc oxide (ZnO:Al) thin films were deposited on glass, polycarbonate (PC), and polyethylene terephthalate (PET) substrates by r.f. magnetron sputtering. The substrate dc bias voltage varied from 0 V to 50 V. Structural, electrical and optical properties of the films were investigated. The deposition rate of ZnO:Al films on glass substrate initially increased with the bias voltage, and then decreased with further increasing bias voltage. It was found that the best films on glass substrate with a low as 6.2 × 10^− 4 Ω cm and an average transmittance over 80% at the wavelength range of 500-900 nm can be obtained by applying the bias voltage of 30 V. The properties of the films deposited on polymer substrate, such as PC and PET, have a similar tendency, with slightly inferior values to those on glass substrate.