Characterization and properties Ti-Al-Si-N nanocomposite coatings prepared by middle frequency magnetron sputtering

TiN-containing amorphous Ti-Al-Si-N (nc-TiN/a-Si₃N₄ or a-AlN) nanocomposite coatings were deposited by using a modified closed field twin unbalanced magnetron sputtering system which is arc assisted and consists of two circles of targets, at a substrate temperature of 300 °C. XRD, XPS and High-resolution TEM experiments showed that the coatings contain TiN nanocrystals embedded in the amorphous Si₃N₄ or AlN matrix. The coatings exhibit good mechanical properties that are greatly influenced by the Si contents. The hardness of the Ti-Al-Si-N coatings deposited at Si targets currents of 5, 8, 10, and 12 A were 45, 47, 54 and 46 GPa, respectively. The high hardness of the deposited Ti-Al-Si-N coatings may be own to the plastic distortion and dislocation blocking by the nanocrystalline structure. On the other hand, the friction coefficient decreases monotonously with increasing Si contents. This result would be caused by tribo-chemical reactions, which often take place in many ceramics, e.g. Si₃N₄ reacts with H₂O to produce SiO₂ or Si(OH)₂ tribolay-layer.     

GaN films deposited by middle-frequency magnetron sputtering

GaN films were deposited on Si (111) substrates by middle-frequency magnetron sputtering. X-ray diffraction revealed preferential GaN (0 0 0 2) orientation normal to the substrate surface for all the films deposited. The diffraction intensity and N contents were found to depend strongly on the total gas pressure. Good quality films were only obtained at pressures in the range of 0.4-1.0 Pa. Little diffraction of GaN (0 0 0 2) could be observed either at total pressures below 0.4 Pa or above 1.0 Pa. The GaN films produced under the optimized conditions have an N:Ga ratio of 1:1 as determined by energy-dispersive X-ray spectroscopy.     

Deposition and characterization of TiAlSiN nanocomposite coatings prepared by reactive pulsed direct current unbalanced magnetron sputtering

This work reports the performance of high speed steel drill bits coated with TiAlSiN nanocomposite coating at different Si contents (5.5-8.1 at.%) prepared using a four-cathode reactive pulsed direct current unbalanced magnetron sputtering system. The surface morphology of the as-deposited coatings was characterized using field emission scanning electron microscopy. The crystallographic structure, chemical composition and bonding structure were evaluated using X-ray diffraction, energy-dispersive X-ray analysis, X-ray photoelectron spectroscopy, respectively. The corrosion behavior, mechanical properties and thermal stability of TiAlSiN nanocomposite coatings were also studied using potentiodynamic polarization, nanoindentation and Raman spectroscopy, respectively. The TiAlSiN coating thickness was approximately 2.5-2.9 μm. These coatings exhibited a maximum hardness of 38 GPa at a silicon content of approximately 6.9 at.% and were stable in air up to 850 °C. For the performance evaluation, the TiAlSiN coated drills were tested under accelerated machining conditions by drilling a 12 mm thick 304 stainless steel plate. Under dry conditions the uncoated drill bits failed after drilling 50 holes, whereas, TiAlSiN coated drill bits (Si = 5.5 at.%) drilled 714 holes before failure. Results indicated that for TiAlSiN coated drill bits the tool life increased by a factor of more than 14.     

磁控溅射(Ti,N)/Al纳米复合薄膜的微结构和力学性能

采用Al和TiN靶通过磁控共溅射方法, 制备了一系列Ti:N≈1的不同(Ti, N) 含量的铝基纳米复合薄膜, 利用X射线能量分散谱仪、X射线衍射仪、透射电子显微镜和纳米力学探针表征了薄膜的成分、 微结构和力学性能, 研究了(Ti, N)含量对复合薄膜微结构和力学性能的影响. 结果表明: Ti, N原子的共同加入使复合薄膜形成了同时具有置换固溶和间隙固溶特征的"双超过饱和固溶体", 薄膜的晶粒随着溶质含量的增加逐步纳米化, 并进一步形成非晶结构, 晶界区域形成溶质原子的富集区. 相应地, 复合薄膜的硬度在含1.8 at.%(Ti, N) 时就可迅速提高到3.9 GPa; 随着TiN含量的增加, 薄膜的硬度进一步提高到含17.1 at.%(Ti, N)时的8.8 GPa. 以上结果显示出Ti和N"双超过饱和固溶"对Al薄膜极其显著的强化效果.     

磁控反应溅射法制备渐变折射率薄膜的模型分析

阐述了磁控反应溅射法制备渐变折射率薄膜的机理;探讨了磁控反应溅射法制备渐变折射率薄膜的理论模型,给出了渐变折射率薄膜的折射率与反应气体分压的关系,在一定的沉积参数下,由要得到的膜层折射率随膜层几何厚度的变化规律可推导出反应气体分压比随时间的变化规律;最后以制备折射率线性变化的薄膜为例说明了如何推导得到反应气体分压比随时间的变化规律. 关键词： 渐变折射率 磁控反应溅射 模型     

直流磁控溅射法在管道内壁镀TiZrV薄膜

用氩气作为放电气体,采用直流磁控溅射法,成功地在不锈钢管道内壁获得了TiZrV薄膜。分别利用能量弥散X射线谱和X射线光电子能谱测量薄膜的成分组成,应用扫描电子显微镜和X射线衍射仪对薄膜进行了测试,并对TiZrV的二次电子产额进行了测量。测试结果表明:TiZrV的成分基本保持在Ti原子分数为30%,Zr原子分数为30%,V原子分数为40%左右,位于“低激活温度区”内;薄膜具有无定形的结构,由微小的纳米晶粒组成;加热激活后TiZrV的二次电子产额有所下降,其峰值由2.03降到1.55,低于不锈钢和无氧铜。     

脉冲磁控溅射法制备单斜相氧化铒涂层

用中频脉冲反应磁控溅射法,在溅射功率为78 W,93 W和124 W以及衬底温度分别为室温,500 ℃及677 ℃下制备了氧化铒涂层.采用原子力显微镜、纳米压痕、X射线衍射和掠入射X射线衍射法研究了涂层的形貌、力学性能及物相结构.测量了涂层的电学性能.结果显示,脉冲磁控溅射沉积氧化铒涂层具有较高的沉积速率.实验制备得到了单斜相结构的氧化铒涂层.提高溅射功率时,沉积速率从28 nm/min增大至68 nm/min,涂层的结晶质量显著下降.提高衬底温度至500 ℃和677 ℃时,单斜相衍射峰强度下降.分析认为 关键词： 氧化铒 脉冲磁控溅射 单斜晶相     

Color and optical characteristics of carbon coatings produced by magnetron sputtering

The color parameters of carbon coatings deposited by magnetron sputtering of a graphite target onto substrates of stainless steel without a sublayer and with a titanium sublayer are calculated. By numerical modeling, the refractive indices and extinction coefficients for the titanium sublayer and carboniferous film as well as the volume content of titanium dioxide in the sublayer are determined. Physico-Technical Institute of the Academy of Sciences of Belarus, 4, Zhodinskaya St., Minsk, 220141, Belarus. Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 64, No. 3, pp. 374–385, May–June, 1997.     

Synthesis and characterization of tantalum nitride films prepared by cathodic vacuum arc technique

Tantalum nitride films were deposited on silicon wafer and steel substrates by cathodic vacuum arc in N₂/Ar gas mixtures. The chemical composition, crystalline microstructure and morphology of the films were investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM), respectively. According to the results, film composition and microstructure depends strongly on the N₂ partial pressure and the applied negative bias (V_s).     

Mechanical properties of the plasma-enhanced magnetron sputtering Si-C-N coatings

The mechanical properties of plasma-enhanced magnetron sputtering Si-C-N hard coatings with various compositions are characterized. The effect of chemical composition on the microstructure and properties of coating is investigated. The results show that the microstructure and mechanical properties of Si-C-N coatings are very sensitive to chemical composition. The nanocrystalline/amorphous composite structure is beneficial to the coating's mechanical properties. It also reveals that Si-C-N coating with low Si and high C concentrations has the highest hardness (≥40 GPa) and the best wear property with dry friction coefficient about 0.2.     

Structural and mechanical properties of multi-element (TiVCrZrHf)N coatings by reactive magnetron sputtering

In this study, (TiVCrZrHf)N multi-component coatings with quinary metallic elements were deposited by reactive magnetron sputtering system. The composition, structure, and mechanical properties of the coatings deposited at different N₂ flow rates were investigated. The (TiVCrZrHf)N coatings deposited at N₂ flow rates of 0, 1, and 2 SCCM showed an amorphous structure, whereas those deposited at N₂ flow rates of 4 and 6 SCCM showed a simple face-centered cubic solid solution structure. A saturated nitride coating was obtained for N₂ flow of 4 SCCM and higher. By increasing N₂ flow to 4 SCCM, the hardness and modulus reached a maximum value of 23.8 ± 0.8 and 267.3 ± 4.0 GPa, respectively.     

磁控溅射制备微球表面金属Mo涂层的研究

利用磁控溅射制备了各种工艺参数不同的微球表面金属Mo涂层样品,并通过白光干涉仪和扫描电子显微镜对样品的表面及剖面进行了系统的测试分析。分别探究了溅射工作气压和沉积制备时间对微球表面Mo涂层表面形貌以及结晶质量的影响规律。结果表明通过优化工艺参数可制备微球直径约为800μm、涂层厚度为3.5μm到14.1μm、厚度均匀性良好的微球表面Mo涂层。Mo涂层中的晶粒呈现出柱状结构致密堆积在一起,且随涂层的厚度增加晶粒间空隙增大。     

直流磁控溅射法在管道内壁镀TiZrV薄膜

用氩气作为放电气体,采用直流磁控溅射法,成功地在不锈钢管道内壁获得了TiZrV薄膜。分别利用能量弥散X射线谱和X射线光电子能谱测量薄膜的成分组成,应用扫描电子显微镜和X射线衍射仪对薄膜进行了测试,并对TiZrV的二次电子产额进行了测量。测试结果表明:TiZrV的成分基本保持在Ti原子分数为30%,Zr原子分数为30%,V原子分数为40%左右,位于"低激活温度区"内;薄膜具有无定形的结构,由微小的纳米晶粒组成;加热激活后TiZrV的二次电子产额有所下降,其峰值由2.03降到1.55,低于不锈钢和无氧铜。     

溅射功率对直流磁控溅射Ti膜结构的影响

 采用直流磁控溅射方法制备了纯Ti膜,研究了不同功率下Ti膜的沉积速率、表面形貌及晶型结构,并对其应力进行了研究。研究表明：薄膜的沉积速率随溅射功率的增加而增加,当溅射功率为20 W时,原子力显微镜(AFM)图像显示Ti膜光洁、致密,均方根粗糙度最小可达0.9 nm。X射线衍射(XRD)分析表明薄膜的晶体结构为六方晶型,Ti膜应力先随溅射功率增大而增大,在60 W时达到最大值（为945.1 MPa）,之后随溅射功率的增大有所减小。     

溅射功率对直流磁控溅射Ti膜结构的影响

采用直流磁控溅射方法制备了纯Ti膜,研究了不同功率下Ti膜的沉积速率、表面形貌及晶型结构,并对其应力进行了研究。研究表明：薄膜的沉积速率随溅射功率的增加而增加,当溅射功率为20 W时,原子力显微镜(AFM)图像显示Ti膜光洁、致密,均方根粗糙度最小可达0.9 nm。X射线衍射(XRD)分析表明薄膜的晶体结构为六方晶型,Ti膜应力先随溅射功率增大而增大,在60 W时达到最大值（为945.1 MPa）,之后随溅射功率的增大有所减小。     

Raman studies on nanocomposite silicon carbonitride thin film deposited by r.f. magnetron sputtering at different substrate temperatures

Raman studies of nanocomposite SiCN thin film by sputtering showed that with increase of substrate temperature from room temperature to 500 °C, a transition from mostly sp² graphitic phase to sp³ carbon took place, which was observed from the variation of I_D/I_G ratio and the peak shifts. This process resulted in the growth of C₃N₄ and Si₃N₄ crystallites in the amorphous matrix, which led to increase in hardness (H) and modulus (E) obtained through nanoindentation. However, at a higher temperature of 600 °C, again an increase of sp² C concentration in the film was observed but the H and E values showed a decrease due to increased growth of the graphitic carbon phase. The whole process got reflected in a modified four‐stage Ferrari–Robertson model of Raman spectroscopy. Copyright © 2010 John Wiley & Sons, Ltd.     

磁控溅射制备极紫外高反射率多层膜应力研究

为制备硼边附近6.7 nm波长的极紫外高反射率多层膜反射镜,研究了Mo2C/B4C,Mo/B4C周期多层膜,重点解决薄膜应力难题。采用直流磁控溅射技术制备了膜层厚度为30 nm的Mo,Mo2C,B4C单层膜,周期厚度为3.5 nm,30对的Mo2C/B4周期多层膜。利用台阶仪测试了镀膜前后基底面形,计算并比较了不同薄膜样品的应力值。结果表明Mo2C/B4C多层膜压应力要远小于Mo/B4C多层膜,且成膜质量与Mo/B4C相当。因此Mo2C/B4C是应用于6.7 nm反射镜较好的多层膜材料组合。C,Mo/B4C     

磁控溅射制备极紫外高反射率多层膜应力研究

为制备硼边附近6.7 nm波长的极紫外高反射率多层膜反射镜,研究了Mo_2C/B_4C,Mo/B_4C周期多层膜,重点解决薄膜应力难题。采用直流磁控溅射技术制备了膜层厚度为30 nm的Mo,Mo_2C,B_4C,单层膜,周期厚度为3.5 nm,30对的Mo_2C/B_4C,Mo/B_4C周期多层膜。利用台阶仪测试了镀膜前后基底面形,计算并比较了不同薄膜样品的应力值。结果表明Mo_2C/B_4C多层膜压应力要远小于Mo/B_4C多层膜,且成膜质量与Mo/B_4C相当。因此Mo_2C/B_4C是应用于6.7 nm反射镜较好的多层膜材料组合。     

利用等离子体辅助脉冲磁控溅射实现 多晶硅薄膜的低温沉积

本文报道了利用电感耦合等离子体辅助中频直流脉冲磁控溅射在温度300 ℃ 以下沉积氢化多晶硅薄膜的制备方法. 利用拉曼散射、X射线衍射、透射电子衍射和傅里叶红外光谱对多晶硅薄膜进行了表征. 详细研究了氢气在沉积过程中所起的作用, 并结合Langmuir探针和发射光谱等等离子体诊断方法, 对辅助等离子体源在多晶硅薄膜制备过程中所起到的作用进行了讨论.     

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用射频等离子体增强非平衡磁控溅射在Si100基底上沉积了金属Cu膜。研究了偏压,射频功率和磁场等沉积参数对膜性能的影响。用扫描电子显微镜(SEM)、原子力显微镜(AFM)、X射线衍射(XRD)和电子能谱(EM)检测了膜的表面形貌,结构和成分。结果表明,射频放电有利于表面均匀光滑、电导率高的Cu沉积膜的形成;沉积参数对沉积膜的性能有重要的影响。