多组分合金靶材在服役期间发生的成分和结构变化

L. Shaginyan, M. Mironov, S. Firstov, Nicolay A. Krapivka, Valery V. Kremetsky, V. N. Novichenko
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摘要

摘要磁控溅射(MS)技术的主要部分是作为薄膜/涂层材料来源的靶材。靶材的性能直接影响ms沉积薄膜/涂层的性能,靶材的组成和微观结构在其开发过程中可能发生变化,特别是当靶材具有复杂的成分时,例如多组分合金。然而,在MS中,只有一小部分目标作为成膜颗粒的来源。这是一个侵蚀区,一个环形槽,随着时间的推移,在目标的离子轰击(IB)下形成。通常,槽面积约为目标方的25%,其余方保持不变。随着沟槽的发展,成膜颗粒的组成和膨胀角度发生了变化,影响了成膜颗粒的组成和厚度均匀性。因此,在目标的使用期限结束时,凹槽的组成和微观结构的信息可以预测薄膜性能可能发生的变化。有鉴于此,我们利用SEM和显微分析对CoCrCuFeNi、CoCrCuFeMnNi、AlCoCrCuFeNiV高熵合金靶材服役初期和结束时的凹槽组织和组成进行了研究。所有靶材的初始微观结构均为光滑平坦,由基体和内含物均匀分布于基体中组成。凹槽底部和侧壁的微凸度不同,且与IB强度有关。在强IB区域,微凸度呈现熔化表面特征。在中IB区,微地形在不同方向上被不同长度和宽度的微沟交叉。结果表明,这些微沟的形状和分布与原始靶表面的夹杂物一致。结果还表明,在使用期限结束时,沟槽的成分被生成焓最大的元素耗尽。对所得结果的分析得出以下结论:(1)靶材表面的熔化迹象表明其温度接近合金的熔化温度;(2)建立了一种新型的优先溅射效应。其存在的主要条件是以微夹杂物的形式存在于第二相的靶组分中,其溅射产率明显高于第一相的组分;(iii)具有DC质谱典型能量的离子在IB靶表面上形成特定微纹是高温和溅射两个因素共同作用的结果。关键词:直流质谱,靶,高熵合金,成分,结构
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Variations in composition and structure occurring in multicomponent alloy targets during their service term
Abstract. Main part of the magnetron sputtering (MS) technology is a target that serves as a source for film/coating material. The target properties directly influence the properties of a film/coating deposited by MS. The target composition and microstructure may change during its exploitation, especially if the target has complex composition, e.g., multicomponent alloy. However, only a small part of the target in the MS serves as a source of film-forming particles. This is an erosion zone, an annular groove, which forms over time under the ion bombardment (IB) of the target. Usually, the groove area is about 25% of the target square while the rest square remains unchanged. As the groove develops, the composition and angle of expansion of the film-forming particles change, that affects the composition and thickness uniformity of the film. Therefore, the information of the composition and microstructure of the groove at the end of the target's service term allows predicting the possible changes in the properties of the film. In view of the told above, we used SEM and microanalysis to study the structure and composition of the grooves of CoCrCuFeNi, CoCrCuFeMnNi, AlCoCrCuFeNiV high entropy alloy targets at the beginning and at the end of their service. Initial microstructure of the surface of all targets was smooth and flat and composed of matrix and inclusions homogenously distributed in the matrix. The microrelief of the bottom and side walls of the grooves was different and depended on the intensity of the IB. In the area of strong IB the microrelief acquired features of a melted surface. In the area of moderate IB the microrelief was crossed in various directions by micro-trenches of various length and width. It was revealed that the shapes and distribution of these micro-trenches coincided with those of the inclusions observed on the original targets surfaces. It was also revealed that at the end of the service term the composition of the grooves became depleted with elements with maximal enthalpy of formation. Analysis of the obtained results led us to the following conclusions: (i) the signs of melting on the targets surfaces indicate that its temperature is close to the melting temperatures of the alloys; (ii) a new type of the effect of preferential sputtering has been established. The main condition for its existence is the presence in the target composition of the second phase in the form of microinclusions, which sputtering yield is noticeably higher than of the components of the first phase; (iii) the formation of specific microrelief on the targets surfaces upon IB with ions with energy typical for DC MS is a result of the combined action of two factors: high temperature and sputtering. Key words: DC MS, target, high entropy alloys, composition, structure
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