Structural and optical characterization of titanium nitride thin films deposited by magnetron sputtering

G. Negrea, V. Merie, A. Molea, V. N. Burnete, B. Neamțu
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A negative polarization of the substrate leads to the formation of small sized crystallites. Regarding the optical properties, the films showed good semiconductor properties and a low reflectivity. Introduction Titanium nitride (TiN) thin films were studied by many researchers due to their excellent properties, especially mechanical and tribological properties, corrosion resistance, wear resistance and thermodynamic stability [1–3]. Due to these properties, titanium nitride thin films can be used in a wide range of applications like: diffusion barriers for micro-electric devices, optical coatings with antireflection and antistatic properties, electrodes, biomedicine and hard coatings for tools and so on [4–9]. The most often used methods to obtain titanium nitride films are: reactive magnetron sputtering, laser ablation, ion beam deposition or plasma assisted chemical vapor deposition and so on [10–14]. The physical-chemical and mechanical/tribological properties of titanium nitride films depend on the deposition parameters. In this regard, different researches present the influence of some deposition parameters such as the deposition rate, deposition time, substrate, the heating or the polarization of the substrate on the topographical, mechanical, tribological, adhesion properties for titanium nitride thin films deposited by DC (direct current) magnetron sputtering. All the results are pointing out a change in these properties with the change in deposition parameters. A possible explanation for this change can be the growth of the deposited films after different preferential orientations. The present paper is a study concerning the deposition of titanium nitride thin films by DC magnetron sputtering on silicon substrates at different deposition parameters (substrate Powder Metallurgy and Advanced Materials – RoPM&AM 2017 Materials Research Forum LLC Materials Research Proceedings 8 (2018) 134-142 doi: http://dx.doi.org/10.21741/9781945291999-15 135 temperature, substrate bias voltage, deposition time) and the structural and optical characterization of the obtained thin films. Materials and Methods Deposition of titanium nitride thin films The deposition of titanium nitride films was done by direct current reactive magnetron sputtering method, using 99.99 % purity titanium target and silicon Si (100) substrate. The experimental procedure details are presented in previously published work of the authors [4]. The parameters for titanium nitride films deposition were: (i) deposition time (10, 20 and 40 minutes) with the substrate (RT) at room temperature, (ii) deposition time (20 minutes) with the substrate at a temperature of 300 °C and (iii) deposition time (20 minutes) and polarization of the substrate at 40 V and -90 V. These studies were conducted in order to determine the influence of the deposition conditions on the structural and optical properties of titanium nitride films destined for MEMS devices applications. Characterization of titanium nitride thin films X-ray diffraction analysis was carried out with an Inel Equinox 3000 diffractometer using a cobalt radiation (λ1=1.7889 Å, λ2=1.7928 Å). The patterns were evaluated using JPCDS 87-0633. The mean crystallite size and lattice strain were calculated using the Williamson-Hall method. According to this method, the broadening of the diffraction line, β, is given by the sum of the broadening introduced by the crystallite size, βd, and the broadening introduced by the internal strain, βε (equation (1)). These two parameters can be calculated using the equations (2) and (3) as follows [15]:","PeriodicalId":20390,"journal":{"name":"Powder Metallurgy and Advanced Materials","volume":"32 1","pages":""},"PeriodicalIF":0.0000,"publicationDate":"2018-11-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"4","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Powder Metallurgy and Advanced Materials","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.21741/9781945291999-15","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 4

Abstract

Titanium nitride applicability covers different industries such as microelectronics, biomedicine and so on. This paper presents the analysis of the structural and optical properties of titanium nitride thin films for different deposition conditions. The samples were deposited by direct current magnetron sputtering on silicon substrates. The deposition was done at room temperature, on substrates preheated at 300 °C or on substrates that were polarized at -40 V and 90 V respectively. The results indicate a dependency of the structural orientation with respect to the deposition process when this takes place at room temperature. When the deposition was done on a preheated substrate there was no structural orientation. A negative polarization of the substrate leads to the formation of small sized crystallites. Regarding the optical properties, the films showed good semiconductor properties and a low reflectivity. Introduction Titanium nitride (TiN) thin films were studied by many researchers due to their excellent properties, especially mechanical and tribological properties, corrosion resistance, wear resistance and thermodynamic stability [1–3]. Due to these properties, titanium nitride thin films can be used in a wide range of applications like: diffusion barriers for micro-electric devices, optical coatings with antireflection and antistatic properties, electrodes, biomedicine and hard coatings for tools and so on [4–9]. The most often used methods to obtain titanium nitride films are: reactive magnetron sputtering, laser ablation, ion beam deposition or plasma assisted chemical vapor deposition and so on [10–14]. The physical-chemical and mechanical/tribological properties of titanium nitride films depend on the deposition parameters. In this regard, different researches present the influence of some deposition parameters such as the deposition rate, deposition time, substrate, the heating or the polarization of the substrate on the topographical, mechanical, tribological, adhesion properties for titanium nitride thin films deposited by DC (direct current) magnetron sputtering. All the results are pointing out a change in these properties with the change in deposition parameters. A possible explanation for this change can be the growth of the deposited films after different preferential orientations. The present paper is a study concerning the deposition of titanium nitride thin films by DC magnetron sputtering on silicon substrates at different deposition parameters (substrate Powder Metallurgy and Advanced Materials – RoPM&AM 2017 Materials Research Forum LLC Materials Research Proceedings 8 (2018) 134-142 doi: http://dx.doi.org/10.21741/9781945291999-15 135 temperature, substrate bias voltage, deposition time) and the structural and optical characterization of the obtained thin films. Materials and Methods Deposition of titanium nitride thin films The deposition of titanium nitride films was done by direct current reactive magnetron sputtering method, using 99.99 % purity titanium target and silicon Si (100) substrate. The experimental procedure details are presented in previously published work of the authors [4]. The parameters for titanium nitride films deposition were: (i) deposition time (10, 20 and 40 minutes) with the substrate (RT) at room temperature, (ii) deposition time (20 minutes) with the substrate at a temperature of 300 °C and (iii) deposition time (20 minutes) and polarization of the substrate at 40 V and -90 V. These studies were conducted in order to determine the influence of the deposition conditions on the structural and optical properties of titanium nitride films destined for MEMS devices applications. Characterization of titanium nitride thin films X-ray diffraction analysis was carried out with an Inel Equinox 3000 diffractometer using a cobalt radiation (λ1=1.7889 Å, λ2=1.7928 Å). The patterns were evaluated using JPCDS 87-0633. The mean crystallite size and lattice strain were calculated using the Williamson-Hall method. According to this method, the broadening of the diffraction line, β, is given by the sum of the broadening introduced by the crystallite size, βd, and the broadening introduced by the internal strain, βε (equation (1)). These two parameters can be calculated using the equations (2) and (3) as follows [15]:
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磁控溅射沉积氮化钛薄膜的结构和光学特性
氮化钛的适用性涵盖了微电子、生物医药等不同行业。本文分析了不同沉积条件下氮化钛薄膜的结构和光学性能。采用直流磁控溅射法在硅衬底上沉积样品。沉积分别在室温、300℃预热和-40 V和90 V极化的衬底上进行。结果表明,当沉积过程发生在室温下时,结构取向与沉积过程有关。当沉积在预热的衬底上时,没有结构取向。衬底的负极化导致小尺寸晶体的形成。在光学性能方面,薄膜具有良好的半导体性能和较低的反射率。氮化钛(TiN)薄膜由于其优异的性能,特别是机械和摩擦学性能、耐蚀性、耐磨性和热力学稳定性,受到了许多研究者的研究[1-3]。由于这些特性,氮化钛薄膜可用于广泛的应用,如:微电子器件的扩散屏障,具有抗反射和抗静电性能的光学涂层,电极,生物医学和工具硬涂层等[4-9]。获得氮化钛薄膜最常用的方法有:反应磁控溅射、激光烧蚀、离子束沉积或等离子体辅助化学气相沉积等[10-14]。氮化钛薄膜的物理化学和机械/摩擦学性能取决于沉积参数。在这方面,不同的研究提出了沉积速率、沉积时间、衬底、衬底加热或极化等沉积参数对直流(直流)磁控溅射沉积氮化钛薄膜的形貌、力学、摩擦学、粘附性能的影响。结果表明,这些性能随沉积参数的变化而变化。对这种变化的一种可能的解释是,在不同的优先取向后,沉积膜的生长。本论文研究了不同沉积参数下硅衬底上的直流磁控溅射沉积氮化钛薄膜(衬底粉末冶金和先进材料- RoPM&AM 2017材料研究论坛LLC材料研究进展8 (2018)134-142 doi: http://dx.doi.org/10.21741/9781945291999-15 135温度,衬底偏置电压,沉积时间)以及所获得薄膜的结构和光学特性。氮化钛薄膜的沉积材料和方法采用直流反应磁控溅射法,以纯度为99.99%的钛为靶材,硅Si(100)为衬底,制备了氮化钛薄膜。实验过程细节见作者先前发表的作品[4]。氮化钛薄膜的沉积参数为:(i)室温下与衬底(RT)的沉积时间(10,20和40分钟),(ii)在300℃下与衬底的沉积时间(20分钟),(iii)沉积时间(20分钟)和衬底在40 V和-90 V下的极化情况。这些研究是为了确定沉积条件对用于MEMS器件的氮化钛薄膜结构和光学性能的影响。利用Inel Equinox 3000衍射仪进行了氮化钛薄膜的x射线衍射分析,采用钴辐射(λ1=1.7889 Å, λ2=1.7928 Å)。使用JPCDS 87-0633对模式进行评价。采用Williamson-Hall法计算了平均晶粒尺寸和晶格应变。根据这种方法,衍射线的展宽β由晶体尺寸引起的展宽βd和内部应变引起的展宽βε(式(1))之和给出。这两个参数可由式(2)、(3)计算得出[15]:
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