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Advances in Thin Films Materials: Properties, Characterization, Physical Vapor Deposition and Application

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A special issue of Materials (ISSN 1996-1944). This special issue belongs to the section "Thin Films and Interfaces".

Deadline for manuscript submissions: closed (10 October 2024) | Viewed by 10491

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Special Issue Editors

Dr. Yue Liu

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Guest Editor

State Key Laboratory of Metal Matrix Composites, School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai, China
Interests: physical vapor deposition of thin films; oxide and nitride nanocomposites; metal matrix composites; multi-scale characterization and modeling
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Dr. Jian Song

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Guest Editor

School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai, China
Interests: physical vapor deposition and properties of ceramic thin films

Dr. Kunming Yang

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Guest Editor

Institute of Materials, China Academy of Engineering Physics, Beijing, China
Interests: deposition and properties of metallic thin films

Special Issue Information

Dear Colleagues,

The mechanical and functional properties of thin-film materials generally differ substantially from those of their bulk counterparts due to the well-known defect, strain, dimensional and interface effects. For example, thin-film materials have higher strength and wear resistance, owing to the presence of nano-sized interfaces. Additionally, interface-related strains can induce strong interplays between the crystal lattice, orbital, charge and spin degrees of freedom, which create emerging electronic or magnetic states and consequently lead to novel functionalities. These unique properties enable an incredible expansion of technological applications of thin-film materials in a range of fields, from electronics to biomedicine to optical devices. Recent advances in physical vapor deposition (PVD) have furthered the compositional and structural design of thin films. Introducing structural/compositional complexity during PVD involves profuse interface and phase coupling, and thereby significantly enhances thin films’ properties. As a consequence, new materials have emerged in the development of next-generation structural and functional materials, such as ceramics, oxides, nanocomposite thin films and multilayers. In order to develop materials with desired microstructure and properties and to facilitate their development, efforts to explore material deposition and growth, defect and microstructure control, property characterization and applications, as well as the establishment of an in-depth understanding of structure–property relationships, are necessary.

Correspondingly, this Special Issue will be devoted to all aspects related to PVD films, including but not limited to thin film growth, microstructure characterization and thin film properties and applications, presenting state-of-the-art advances in this rapidly developing field.

Dr. Yue Liu
Dr. Jian Song
Dr. Kunming Yang
Guest Editors

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Keywords

physical vapor deposition
thin films
interfaces
functional properties
mechanical properties

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Published Papers (7 papers)

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Research

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14 pages, 2706 KiB

Open AccessArticle

Evolution of Chemical, Structural, and Mechanical Properties of Titanium Nitride Films with Different Thicknesses Fabricated Using Pulsed DC Magnetron Sputtering

by Wei Mao, Runze Qi, Jiali Wu, Zhe Zhang and Zhanshan Wang

Materials 2024, 17(24), 6067; https://doi.org/10.3390/ma17246067 - 12 Dec 2024

Viewed by 497

Abstract

Considering the application of titanium nitride (TiN) films as a release layer in producing Wolter-I X-ray telescope mirror shells by the electroformed nickel replication (ENR) technique, this research pays attention to the influence of nanometer-scale thickness variation in the microstructure and physical properties of TiN films deposited by the pulsed direct current (DC) magnetron sputtering method. This topic has received limited attention in the existing literature. TiN films (9.8 nm to 42.9 nm) were fabricated to comprehensively analyze the evolution in microstructure, depth distribution of elements, surface morphology, and intrinsic stress. With increasing thickness, TiN transitioned from amorphous to (200) and (111)–(200) mixed-oriented crystallization, explaining inflection points in the increasing roughness curve. Elements (C, N, O, Si, and Ti) and chemical bond proportions (Ti-N, Ti-N-O, and Ti-O) varied with film depth, and the fitting of film density can be optimized according to these variations. Crystallite size increased with thickness, which led to a reduction in intrinsic stress. It is evident that as film thickness increases, TiN forms a stable crystal structure, thereby reducing intrinsic stress, but resulting in increased roughness. Considering the impact of changes in thin film thickness on physical properties such as roughness, crystallinity, and intrinsic stress, a TiN film with a thickness of approximately 25 nm is deemed suitable for application as a release layer. Full article

(This article belongs to the Special Issue Advances in Thin Films Materials: Properties, Characterization, Physical Vapor Deposition and Application)

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27 pages, 6259 KiB

Open AccessArticle

Real-Time Spectroscopic Ellipsometry for Flux Calibrations in Multi-Source Co-Evaporation of Thin Films: Application to Rate Variations in CuInSe₂ Deposition

by Dhurba R. Sapkota, Balaji Ramanujam, Puja Pradhan, Mohammed A. Razooqi Alaani, Ambalanath Shan, Michael J. Heben, Sylvain Marsillac, Nikolas J. Podraza and Robert W. Collins

Materials 2024, 17(16), 4048; https://doi.org/10.3390/ma17164048 - 14 Aug 2024

Viewed by 830

Abstract

Flux calibrations in multi-source thermal co-evaporation of thin films have been developed based on real-time spectroscopic ellipsometry (RTSE) measurements. This methodology has been applied to fabricate CuInSe₂ (CIS) thin film photovoltaic (PV) absorbers, as an illustrative example, and their properties as functions of deposition rate have been studied. In this example, multiple Cu layers are deposited step-wise onto the same Si wafer substrate at different Cu evaporation source temperatures (T_Cu). Multiple In₂Se₃ layers are deposited similarly at different In source temperatures (T_In). Using RTSE, the Cu and In₂Se₃ deposition rates are determined as functions of T_Cu and T_In. These rates, denoted R_eff, are measured in terms of effective thickness which is the volume per planar substrate area and accounts for surface roughness variations with deposition time. By assuming that all incident metal atoms are incorporated into the films and that the atomic concentrations in the deposited material components are the same as in single crystals, initial estimates of the Cu and In atom fluxes can be made versus T_Cu and T_In. Applying these estimates to the co-evaporation of a set of CIS films from individual Cu, In, and Se sources, atomic concentration corrections can be assigned to the Cu and In₂Se₃ calibration films. The corrections enable generation of a novel calibration diagram predicting the atomic ratio y = [Cu]/[In] and rate R_eff within the T_Cu-T_In plane. Using this diagram, optimization of the CIS properties as a PV absorber can be achieved versus both y and R_eff. Full article

(This article belongs to the Special Issue Advances in Thin Films Materials: Properties, Characterization, Physical Vapor Deposition and Application)

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13 pages, 8022 KiB

Open AccessCommunication

Hydrothermal Growth and Orientation of LaFeO₃ Epitaxial Films

by Guang Xian, Tongxin Zheng, Yaqiu Tao and Zhigang Pan

Materials 2024, 17(11), 2758; https://doi.org/10.3390/ma17112758 - 5 Jun 2024

Cited by 1 | Viewed by 1014

Abstract

LaFeO₃ thin films were successfully epitaxially grown on single-crystalline SrTiO₃ substrates by the one-step hydrothermal method at a temperature of 320 °C in a 10 mol/L KOH aqueous solution using La(NO₃)₃ and Fe(NO₃)₃ as the raw materials. The growth of the films was consistent with the island growth mode. Scanning electronic microscopy, elemental mapping, and atomic force microscopy demonstrate that the LaFeO₃ thin films cover the SrTiO₃ substrate thoroughly. The film subjected to hydrothermal treatment for 4 h exhibits a relatively smooth surface, with an average surface roughness of 10.1 nm. X-ray diffraction in conventional Bragg–Brentano mode shows that the LaFeO₃ thin films show the same out-of-plane orientation as that of the substrate (i.e., (001)_LaFeO3||(001)_SrTiO3). The in-plane orientation of the films was analyzed by φ-scanning, revealing that the orientational relationship is [001]_LaFeO3||[001]_SrTiO3. The ω-rocking curve indicates that the prepared LaFeO₃ films are of high quality with no significant mosaic defects. Full article

(This article belongs to the Special Issue Advances in Thin Films Materials: Properties, Characterization, Physical Vapor Deposition and Application)

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13 pages, 10556 KiB

Open AccessEditor’s ChoiceArticle

Influence of HiPIMS Pulse Widths on the Structure and Properties of Copper Films

by Xincheng Liu, Heda Bai, Yongjie Ren, Jin Li and Xiangli Liu

Materials 2024, 17(10), 2342; https://doi.org/10.3390/ma17102342 - 15 May 2024

Cited by 1 | Viewed by 1160

Abstract

High-power pulse magnetron sputtering is a new type of magnetron sputtering technology that has advantages such as high peak power density and a high ionization rate compared to DC magnetron sputtering. In this paper, we report the effects of different pulse widths on the current waveform and plasma spectrum of target material sputtering, as well as the structure and properties of Cu films prepared under the same sputtering voltage and duty cycle. Extending the pulse width can make the sputtering enter the self-sputtering (SS) stage and improve the ion quantity of sputtered particles. The Cu film prepared by HiPIMS with long pulse width has higher bond strength and lower electrical resistivity compared to the Cu film prepared by short pulse width. In terms of microstructure, the Cu film prepared by HiPIMS with the long pulse width has a larger grain size and lower micro-surface roughness. When the pulse width is bigger than 200 μs, the microstructure of the Cu film changes from granular to branched. This transformation reduces the interface on the Cu film, further reducing the resistivity of the Cu film. Compared to short pulses, long pulse width HiPIMS can obtain higher quality Cu films. This result provides a new process approach for preparing high-quality Cu films using HiPIMS technology. Full article

(This article belongs to the Special Issue Advances in Thin Films Materials: Properties, Characterization, Physical Vapor Deposition and Application)

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14 pages, 4372 KiB

Open AccessArticle

Effects of HiPIMS Duty Cycle on Plasma Discharge and the Properties of Cu Film

by Yongjie Ren, Heda Bai, Xincheng Liu, Jin Li and Xiangli Liu

Materials 2024, 17(10), 2311; https://doi.org/10.3390/ma17102311 - 13 May 2024

Cited by 1 | Viewed by 1621

Abstract

In this paper, Cu thin films were deposited on Si (100) substrates by the high−power impulse magnetron sputtering (HiIPMS) technique, and the effects of different duty cycles (from 2.25% to 5.25%) on the plasma discharge characteristics, microstructure, and electrical properties of Cu thin films were investigated. The results of the target current test show that the peak target current remains stable under 2.25% and 3% duty cycle conditions. Under the conditions of a 4.5% and 5.25% duty cycle, the target peak current shows a decreasing trend. The average power of the target shows a rising trend with the increase in the duty cycle, while the peak power of the target shows a decreasing trend with the increase in the duty cycle. The results of OES show that with the increase in the duty cycle, the total peak intensity of copper and argon emissions shows an overall increasing trend. The duty cycle from 3% to 4.5% change in copper and argon emission peak total intensity change is not obvious. The deposition rate and surface morphology of the copper film were investigated by scanning electron microscopy, and the deposition rate of the copper film increased with the increase in the duty cycle, which was mainly due to the increase in the average power. The surface roughness of the copper film was evaluated by atomic force microscopy. X−ray diffraction (XRD) was used to analyze the grain size and texture of the Cu film, and the results showed that the average grain size of the Cu film increased from 38 nm to 59 nm on the (111) and (200) crystal planes. Four−probe square resistance test copper film resistivity in 2.25%, 3% low duty cycle conditions of the copper film resistivity is generally higher than 4.5%, 5.25% high duty cycle conditions, the copper film resistivity shows the trend of change is mainly affected by the copper film grain size and the (111) face of the double effect of the optimal orientation. The lowest resistivity of the copper film measured under the 4.5% duty cycle condition is 1.7005 μΩ·cm, which is close to the intrinsic resistivity of the copper film of 1.67 μΩ·cm. Full article

(This article belongs to the Special Issue Advances in Thin Films Materials: Properties, Characterization, Physical Vapor Deposition and Application)

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13 pages, 6048 KiB

Open AccessArticle

Two-Step Thermal Transformation of Multilayer Graphene Using Polymeric Carbon Source Assisted by Physical Vapor Deposited Copper

by Yong Huang, Jiamiao Ni, Xiaoyu Shi, Yu Wang, Songsong Yao, Yue Liu and Tongxiang Fan

Materials 2023, 16(16), 5603; https://doi.org/10.3390/ma16165603 - 13 Aug 2023

Cited by 2 | Viewed by 1459

Abstract

Direct in situ growth of graphene on dielectric substrates is a reliable method for overcoming the challenges of complex physical transfer operations, graphene performance degradation, and compatibility with graphene-based semiconductor devices. A transfer-free graphene synthesis based on a controllable and low-cost polymeric carbon source is a promising approach for achieving this process. In this paper, we report a two-step thermal transformation method for the copper-assisted synthesis of transfer-free multilayer graphene. Firstly, we obtained high-quality polymethyl methacrylate (PMMA) film on a 300 nm SiO₂/Si substrate using a well-established spin-coating process. The complete thermal decomposition loss of PMMA film was effectively avoided by introducing a copper clad layer. After the first thermal transformation process, flat, clean, and high-quality amorphous carbon films were obtained. Next, the in situ obtained amorphous carbon layer underwent a second copper sputtering and thermal transformation process, which resulted in the formation of a final, large-sized, and highly uniform transfer-free multilayer graphene film on the surface of the dielectric substrate. Multi-scale characterization results show that the specimens underwent different microstructural evolution processes based on different mechanisms during the two thermal transformations. The two-step thermal transformation method is compatible with the current semiconductor process and introduces a low-cost and structurally controllable polymeric carbon source into the production of transfer-free graphene. The catalytic protection of the copper layer provides a new direction for accelerating the application of graphene in the field of direct integration of semiconductor devices. Full article

(This article belongs to the Special Issue Advances in Thin Films Materials: Properties, Characterization, Physical Vapor Deposition and Application)

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Review

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21 pages, 6468 KiB

Open AccessReview

Comparison of CrN Coatings Prepared Using High-Power Impulse Magnetron Sputtering and Direct Current Magnetron Sputtering

by Heda Bai, Jin Li, Jialai Gao, Jinyang Ni, Yaxiong Bai, Jie Jian, Lin Zhao, Bowen Bai, Zeyun Cai, Jianchao He, Hongsheng Chen, Xuesong Leng and Xiangli Liu

Materials 2023, 16(18), 6303; https://doi.org/10.3390/ma16186303 - 20 Sep 2023

Cited by 12 | Viewed by 2817

Abstract

Chromium Nitride (CrN) coatings have widespread utilization across numerous industrial applications, primarily attributed to their excellent properties. Among the different methods for CrN coating synthesis, direct current magnetron sputtering (DCMS) has been the dominant technique applied. Nonetheless, with the expanded applications of CrN coatings, the need for enhanced mechanical performance is concurrently escalating. High-power impulse magnetron sputtering (HiPIMS), an innovative coating deposition approach developed over the past three decades, is gaining recognition for its capability of yielding coatings with superior mechanical attributes, thereby drawing significant research interest. Considering that the mechanical performance of a coating is fundamentally governed by its microstructural properties, a comprehensive review of CrN coatings fabricated through both techniques is presented. This review of recent literature aims to embark on an insightful comparison between DCMS and HiPIMS, followed by an examination of the microstructure of CrN coatings fabricated via both techniques. Furthermore, the exploration of the underlying factors contributing to the disparities in mechanical properties observed in CrN coatings is revealed. An assessment of the advantages and potential shortcomings of HiPIMS is discussed, offering insight into CrN coating fabrication. Full article

(This article belongs to the Special Issue Advances in Thin Films Materials: Properties, Characterization, Physical Vapor Deposition and Application)

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