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首页> 外文期刊>Materials Science and Engineering. B, Solid-State Materials for Advanced Technology >Superhard nanocomposite Ti-Al-Si-N films deposited by reactive unbalanced magnetron sputtering
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Superhard nanocomposite Ti-Al-Si-N films deposited by reactive unbalanced magnetron sputtering

机译：反应性不平衡磁控溅射沉积超硬纳米复合Ti-Al-Si-N薄膜

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摘要

Nanocomposite Ti-Al-Si-N films (Al content ranging from 0 to 16.7 at.% and Si from 0 to 11.8 at.%, respectively) were prepared on Si(100) substrates at 500℃ by reactive close-field unbalanced magnetron sputtering in an Ar-Ni mixture. The chemical composition, bonding structure, surface morphology, microstructure, stress and mechanical properties of these films were systematically investigated by means of energy dispersive spectrometry (EDS), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), X-ray diffraction (XRD), optical interference system and nanoindentation measurements. The XPS measurements reveal evolution of chemical composition and bonding structure of the deposited Ti-Al-Si-N films. The observed nonlinear peak shift of Ti 2p and N 1 s indicates the bonding evolution of crystalline TiN. The spectra from Al 2p at 73.7 eV and Si 2p at 101.1 eV indicates the evolution of film composition from TiSiN to TiAlN with the incorporation of Al, and also implies that their chemical states are mainly in the form of SiN_x and AlN, respectively. The (111) diffraction peak from the XRD θ-2θ patterns shows a variation either on peak width or on peak position, indicating the variation of grain size and lattice constant. The calculated lattice constant reveals a mixture of different phases whose structures are similar to TiN. The nonlinear variation of grain size and lattice constant is considered due to the competition between two processes, i.e. Al addition and the underlying Si reduction. In order to further understand the microstructure evolution, the XRD spectra and corresponding calculations of the Ti-Al-Si-N films without heating during deposition are also shown for comparison. The effect of substrate heating is discussed. The present results show that the influence of Si and Al addition on the grain growth is different. The surface roughness of Ti-Al-Si-N films also exhibits a nonlinear variation, which is due to the variation of grain size and the competitive growth of different phases. The influence of stress on the hardness can be ignored due to its relatively low value (1-2 GPa) compared with the super-hardness of the films. All the quaternary Ti-Al-Si-N films show enhanced mechanical properties when compared with the nanocomposite Ti-Si-N and Ti-Al-N films deposited under the same condition. The best hardness, reaching superhard, is obtained for the Ti-Al-Si-N film with 7.5 at.% Al and 6 at.% Si. The combined effect of vacancy hardening and some of extrinsic hardening are considered responsible for the enhanced mechanical properties of Ti-Al-Si-N films.
机译：利用反应性近场不平衡磁控管在500℃的Si（100）衬底上制备了纳米复合Ti-Al-Si-N薄膜（Al含量分别在0至16.7 at。％和Si在0至11.8 at。％）。在Ar-Ni混合物中进行溅射。通过能量色散光谱（EDS），X射线光电子能谱（XPS），原子力显微镜（AFM），X-射线能谱等系统地研究了这些薄膜的化学组成，键合结构，表面形态，微观结构，应力和力学性能。射线衍射（XRD），光学干涉系统和纳米压痕测量。 XPS测量揭示了沉积的Ti-Al-Si-N膜的化学成分和键合结构的演变。观察到的Ti 2p和N 1 s的非线性峰位移表明晶体TiN的键演化。来自Al 2p在73.7 eV和Si 2p在101.1 eV的光谱表明，随着Al的掺入，薄膜成分从TiSiN演化为TiAlN，也暗示它们的化学态分别主要为SiN_x和AlN形式。来自XRDθ-2θ图案的（111）衍射峰在峰宽或峰位置均显示出变化，表明晶粒尺寸和晶格常数的变化。计算出的晶格常数揭示了结构类似于TiN的不同相的混合物。考虑到晶粒尺寸和晶格常数的非线性变化是由于两个过程之间的竞争，即Al添加和下面的Si还原。为了进一步了解显微组织的演变，还显示了在沉积过程中不加热的Ti-Al-Si-N薄膜的XRD光谱和相应的计算方法，用于比较。讨论了基板加热的影响。目前的结果表明，添加硅和铝对晶粒长大的影响是不同的。 Ti-Al-Si-N薄膜的表面粗糙度也表现出非线性变化，这是由于晶粒尺寸的变化和不同相的竞争性生长所致。应力对硬度的影响可以忽略不计，因为与薄膜的超硬度相比，应力值较低（1-2 GPa）。与在相同条件下沉积的纳米复合Ti-Si-N和Ti-Al-N薄膜相比，所有四元Ti-Al-Si-N薄膜均显示出增强的机械性能。对于具有7.5at。％的Al和6at。％的Si的Ti-Al-Si-N膜，获得了达到超硬的最佳硬度。空位硬化和一些非本征硬化的综合作用被认为是增强Ti-Al-Si-N薄膜机械性能的原因。

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