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Advances in Synthesis, Characterization, and Application of Thin Films

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A special issue of Crystals (ISSN 2073-4352). This special issue belongs to the section "Inorganic Crystalline Materials".

Deadline for manuscript submissions: closed (20 June 2024) | Viewed by 14392

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Dr. Miłosz Grodzicki

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1. Department of Semiconductor Materials Engineering, Faculty of Fundamental Problems of Technology, Wrocław University of Science and Technology, Wybrzeże Wyspiańskiego 27, Wrocław, Poland
2. Łukasiewicz Research Network – PORT Polish Center for Technology Development, 54-066 Wrocław, Poland
Interests: surface science; thin-films; PVD; MBE
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Dr. Damian Wojcieszak

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Division of Thin Film Technologies, Department of Electronic and Photonic Metrology, Faculty of Electronics, Photonics and Microsystems, Wrocław University of Science and Technology, Wybrzeże Wyspiańskiego 27, Wrocław, Poland
Interests: thin film technology; fucntional coatings; bioactive multilayers; transparent electronics

Dr. Michał Mazur

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Special Issue Information

Dear Colleagues,

Thin films have a wide range of applications across various fields due to their unique properties, but their application is dependent on their composition, morphology, microstructure, etc. They find practical applications in electronics and optoelectronics, sensors, energy conversions, magnetic storages, and optical coatings. In recent years, significant progress has been made in the advancement of thin films, leading to the development of novel materials and devices. For this purpose, various thin film growth techniques are being used. These include magnetron sputtering (MS), molecular beam epitaxy (MBE), physical vapor deposition (PVD), metal–organic chemical vapor deposition (MOCVD), and pulsed laser deposition (PLD), which have been developed and upgraded over the years.

The objective of this Special Issue is to gather high-quality articles that specifically concentrate on thin film materials, coatings, and devices as well as techniques of deposition. The aim is to explore the diverse range of functional films, including metallic, organic, inorganic, hybrid, and composite materials, with the goal of advancing various types of devices. These devices may include transistors, sensors, photodetectors, photovoltaic devices, and light-emitting devices.

Dr. Miłosz Grodzicki
Dr. Damian Wojcieszak
Dr. Michał Mazur
Guest Editors

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Keywords

thin film fabrication
thin film growth
thin film characterization
thin film applications
surfaces and interfaces
thin film modeling
thin film materials in catalysis, electronics, optics, and coatings

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Published Papers (10 papers)

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Research

15 pages, 4176 KiB

Open AccessArticle

Study on the Simulation and Experimental Impact of Substrate Holder Design on 3-Inch High-Quality Polycrystalline Diamond Thin Film Growth in a 2.45 GHz Resonant Cavity MPCVD

by Shuai Wu, Kesheng Guo, Jie Bai, Jiafeng Li, Jingming Zhu, Lei Liu, Lei Huang, Chuandong Zhang and Qiang Wang

Crystals 2024, 14(9), 821; https://doi.org/10.3390/cryst14090821 - 20 Sep 2024

Viewed by 1264

Abstract

In this study, three different substrate holder shapes—trapezoidal, circular frustum, and adjustable cyclic—were designed and optimized to enhance the quality of polycrystalline diamond films grown using microwave plasma chemical vapor deposition (MPCVD). Simulation results indicate that altering the shape of the substrate holder leads to a uniform distribution of the electric field on the surface, significantly suppressing the formation of secondary plasma. This design ensures a more even distribution of the temperature field and plasma environment on the substrate holder, resulting in a heart-shaped distribution. Polycrystalline diamond films were synthesized under these three different substrate holder conditions, and their morphology and crystal quality were characterized using optical microscopy, Raman spectroscopy, and high-resolution X-ray diffraction. Under conditions of 5 kW power and 90 Torr pressure, the adjustable cyclic substrate holder produced high-quality 3-inch diamond films with low stress and narrow Raman full width at half maximum (FWHM). The results confirm the reliability of the simulations and the effectiveness of the adjustable cyclic substrate holder. This approach provides a viable method for scaling up the size and improving the quality of polycrystalline diamond films for future applications. Full article

(This article belongs to the Special Issue Advances in Synthesis, Characterization, and Application of Thin Films)

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17 pages, 4121 KiB

Open AccessArticle

Plasma-Enhanced Atomic Layer Deposition of Hematite for Photoelectrochemical Water Splitting Applications

by Thom R. Harris-Lee, Andrew Brookes, Jie Zhang, Cameron L. Bentley, Frank Marken and Andrew L. Johnson

Crystals 2024, 14(8), 723; https://doi.org/10.3390/cryst14080723 - 13 Aug 2024

Viewed by 1759

Abstract

Hematite (α-Fe₂O₃) is one of the most promising and widely used semiconductors for application in photoelectrochemical (PEC) water splitting, owing to its moderate bandgap in the visible spectrum and earth abundance. However, α-Fe₂O₃ is limited by short hole-diffusion lengths. Ultrathin α-Fe₂O₃ films are often used to limit the distance required for hole transport, therefore mitigating the impact of this property. The development of highly controllable and scalable ultrathin film deposition techniques is therefore crucial to the application of α-Fe₂O₃. Here, a plasma-enhanced atomic layer deposition (PEALD) process for the deposition of homogenous, conformal, and thickness-controlled α-Fe₂O₃ thin films (<100 nm) is developed. A readily available iron precursor, dimethyl(aminomethyl)ferrocene, was used in tandem with an O₂ plasma co-reactant at relatively low reactor temperatures, ranging from 200 to 300 °C. Optimisation of deposition protocols was performed using the thin film growth per cycle and the duration of each cycle as optimisation metrics. Linear growth rates (constant growth per cycle) were measured for the optimised protocol, even at high cycle counts (up to 1200), confirming that all deposition is ‘true’ atomic layer deposition (ALD). Photoelectrochemical water splitting performance was measured under solar simulated irradiation for pristine α-Fe₂O₃ deposited onto FTO, and with a α-Fe₂O₃-coated TiO₂ nanorod photoanode. Full article

(This article belongs to the Special Issue Advances in Synthesis, Characterization, and Application of Thin Films)

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10 pages, 3664 KiB

Open AccessArticle

Deposition and Structural Characterization of Mg-Zn Co-Doped GaN Films by Radio-Frequency Magnetron Sputtering in a N₂-Ar₂ Environment

by Erick Gastellóu, Rafael García, Ana M. Herrera, Antonio Ramos, Godofredo García, Gustavo A. Hirata, José A. Luna, Jorge A. Rodríguez, Mario Robles, Yani D. Ramírez and Iván E. García

Crystals 2024, 14(7), 618; https://doi.org/10.3390/cryst14070618 - 4 Jul 2024

Viewed by 1020

Abstract

Mg-Zn co-doped GaN films were deposited by radio-frequency magnetron sputtering in an N₂-Ar₂ environment at room temperature, using a target prepared with Mg-Zn co-doped GaN powders. X-ray diffraction patterns showed broad peaks with an average crystal size of 13.65 nm and lattice constants for a hexagonal structure of a = 3.1 Å and c = 5.1 Å. Scanning electron microscopy micrographs and atomic force microscopy images demonstrated homogeneity in the deposition of the films and good surface morphology with a mean roughness of 1.1 nm. Energy-dispersive spectroscopy and X-ray photoelectron spectroscopy characterizations showed the presence of gallium and nitrogen as elemental contributions as well as of zinc and magnesium as co-doping elements. Profilometry showed a value of 260.2 nm in thickness in the Mg-Zn co-doped GaN films. Finally, photoluminescence demonstrated fundamental energy emission located at 2.8 eV (430.5 nm), which might be related to the incorporation of magnesium and zinc atoms. Full article

(This article belongs to the Special Issue Advances in Synthesis, Characterization, and Application of Thin Films)

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9 pages, 3463 KiB

Open AccessArticle

High-Temperature (Cu,C)Ba₂Ca₃Cu₄O_y Superconducting Films with Large Irreversible Fields Grown on SrLaAlO₄ Substrates by Pulsed Laser Deposition

by Yugang Li, Zhiyong Liu, Ping Zhu, Jinyu He and Chuanbing Cai

Crystals 2024, 14(6), 514; https://doi.org/10.3390/cryst14060514 - 28 May 2024

Cited by 1 | Viewed by 1321

Abstract

(Cu,C)Ba₂Ca₃Cu₄O_y is a nontoxic cuprate superconducting material with a superconducting transition temperature of about 116 K. Recently, it was found that bulk samples of this material synthesized under high pressure hold the highest irreversibility line among all the superconductors, which is very promising for its application in the liquid nitrogen temperature field. In this work, high-temperature (Cu,C)Ba₂Ca₃Cu₄O_y superconducting films with large irreversible fields were prepared on SrLaAlO₄(00l) substrates by pulsed laser deposition. The substrate temperature during deposition proved to be the most important parameter determining the morphology and critical temperature of the superconductors, with 680 °C considered to be the optimum temperature. X-ray diffraction (XRD) results showed that the (Cu,C)Ba₂Ca₃Cu₄O_y films prepared under optimal conditions exhibited epitaxial growth with the a-axis perpendicular to the film surface and the b- and c-axes parallel to the substrate, with no evidence of any other orientation. In addition, resistivity measurements showed that the onset transition temperature (T_c^onset) was approximately 116 K, the zero-resistance critical temperature (T_c₀) was around 53 K, and the irreversible field (H_irr) was about 9 T at 37 K for (Cu,C)Ba₂Ca₃Cu₄O_y films under optimal temperature. This is the first example of the successful growth of superconducting (Cu,C)Ba₂Ca₃Cu₄O_y films on SrLaAlO₄(00l) substrates. This will facilitate high-performance applications of (Cu,C)Ba₂Ca₃Cu₄O_y superconducting materials in the liquid nitrogen temperature field. Full article

(This article belongs to the Special Issue Advances in Synthesis, Characterization, and Application of Thin Films)

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12 pages, 3197 KiB

Open AccessArticle

Ultrahigh Responsivity In₂O₃ UVA Photodetector through Modulation of Trimethylindium Flow Rate

by Yifei Li, Tiwei Chen, Yongjian Ma, Yu Hu, Li Zhang, Xiaodong Zhang, Jinghang Yang, Lu Wang, Huanyu Zhang, Changling Yan, Zhongming Zeng and Baoshun Zhang

Crystals 2024, 14(6), 494; https://doi.org/10.3390/cryst14060494 - 24 May 2024

Cited by 1 | Viewed by 1096

Abstract

Oxygen vacancies (V_o) can significantly degrade the electrical properties of indium oxide (In₂O₃) thin films, thus limiting their application in the field of ultraviolet detection. In this work, the V_o is effectively suppressed by adjusting the Trimethylindium (TMIn) flow rate (f_TMIn). In addition, with the reduction of the f_TMIn, the background carrier concentration and the roughness of the film decrease gradually. And a smooth In₂O₃ thin film with roughness of 0.44 nm is obtained when the f_TMIn is 5 sccm. The MSM photodetectors (PDs) are constructed based on In₂O₃ thin films with different f_TMIn to investigate the opto-electric characteristics of the films. The dark current of the PDs is significantly reduced by five orders from 100 mA to 0.28 μA with the reduction of the f_TMIn from 50 sccm to 5 sccm. In addition, the photo response capacity of PDs is dramatically enhanced. The photo-to-dark current ratio (PDCR) increases from 0 to 2589. Finally, the PD with the f_TMIn of 5 sccm possesses a record-high responsivity of 2.53 × 10³ AW⁻¹, a high detectivity of 5.43 × 10⁷ Jones and a high EQE of 9383 × 100%. Our work provides an important reference for the fabrication of high-sensitivity UV PDs. Full article

(This article belongs to the Special Issue Advances in Synthesis, Characterization, and Application of Thin Films)

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11 pages, 6554 KiB

Open AccessArticle

Influence of the Incorporation of Nd in ZnO Films Grown by the HFCVD Technique to Enhance Photoluminiscence Due to Defects

by Marcos Palacios Bonilla, Godofredo García Salgado, Antonio Coyopol Solís, Román Romano Trujillo, Fabiola Gabriela Nieto Caballero, Enrique Rosendo Andrés, Crisóforo Morales Ruiz, Justo Miguel Gracia Jiménez and Reina Galeazzi Isasmendi

Crystals 2024, 14(6), 491; https://doi.org/10.3390/cryst14060491 - 23 May 2024

Cited by 1 | Viewed by 788

Abstract

In this work, optical–structural and morphological behavior when Nd is incorporated into ZnO is studied. ZnO and Nd-doped ZnO (ZnO-Nd) films were deposited at 900 °C on Silicon n-type substrates (100) by using the Hot Filament Chemical Vapor Deposition (HFCVD) technique. For this, pellets were made by from powders of ZnO(s) and a mixture of ZnO(s):Nd(OH)₃(s). The weight percent of the mixture ZnO:Nd(OH)₃ in the pellet is 1:3. The gaseous precursor generation was carried out by chemical decomposition of the pellets using atomic hydrogen which was produced by a tungsten filament at 2000 °C. For the ZnO film, diffraction planes (100), (002), (101), (102), (110), and (103) were found by XRD. For the ZnO-Nd film, its planes are displaced, indicating the incorporation of Nd into the ZnO. EDS was used to confirm the Nd in the ZnO-Nd film with an atomic concentration (at%) of Nd = 10.79. An improvement in photoluminescence is observed for the ZnO-Nd film; this improvement is attributed to an increase in oxygen vacancies due to the presence of Nd. The important thing about this study is that by the HFCVD method, ZnO-Nd films can be obtained easily and with very short times; in addition, some oxide compounds can be obtained individually as initial precursors, which reduces the cost compared to other techniques. Something interesting is that the incorporation of Nd into ZnO by this method has not yet been studied, and depending on the method used, the PL of ZnO with Nd can increase or decrease, and by the HFCVD method the PL of the ZnO film, when Nd is incorporated, increases more than 15 times compared to the ZnO film. Full article

(This article belongs to the Special Issue Advances in Synthesis, Characterization, and Application of Thin Films)

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27 pages, 16687 KiB

Open AccessArticle

The Influence of Variations in Synthesis Conditions on the Phase Composition, Strength and Shielding Characteristics of CuBi₂O₄ Films

by Dauren B. Kadyrzhanov, Medet T. Idinov, Dmitriy I. Shlimas and Artem L. Kozlovskiy

Crystals 2024, 14(5), 453; https://doi.org/10.3390/cryst14050453 - 10 May 2024

Viewed by 1448

Abstract

This paper presents the results of the influence of variation of the synthesis conditions of CuBi/CuBi₂O₄ films with a change in the applied potential difference, as well as a change in electrolyte solutions (in the case of adding cobalt or nickel sulfates to the electrolyte solution) on changes in the phase composition, structural parameters and strength characteristics of films obtained using the electrochemical deposition method. During the experiments, it was found that, in the case of the addition of cobalt or nickel to the electrolyte solutions, the formation of films with a spinel-type tetragonal CuBi₂O₄ phase is observed. In this case, a growth in the applied potential difference leads to the substitution of copper with cobalt (nickel), which in turn leads to an increase in the structural ordering degree. It should be noted that, during the formation of CuBi/CuBi₂O₄ films from solution–electrolyte №1, the formation of the CuBi₂O₄ phase is observed only with an applied potential difference of 4.0 V, while the addition of cobalt or nickel sulfates to the electrolyte solution results in the formation of the tetragonal CuBi₂O₄ phase over the entire range of the applied potential difference (from 2.0 to 4.0 V). Studies have been carried out on the strength and tribological characteristics of synthesized films depending on the conditions of their production. It has been established that the addition of cobalt or nickel sulfates to electrolyte solutions leads to an increase in the strength of the resulting films from 20 to 80%, depending on the production conditions (with variations in the applied potential difference). During the studies, it was established that substitution of copper with cobalt or nickel in the composition of CuBi₂O₄ films results in a rise in the shielding efficiency of low-energy gamma radiation by 3.0–4.0 times in comparison with copper films, and 1.5–2.0 times for high-energy gamma rays, in which case the decrease in efficiency is due to differences in the mechanisms of interaction of gamma quanta, as well as the occurrence of secondary radiation as a result of the formation of electron–positron pairs and the Compton effect. Full article

(This article belongs to the Special Issue Advances in Synthesis, Characterization, and Application of Thin Films)

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15 pages, 5678 KiB

Open AccessArticle

Design and Study of Composite Film Preparation Platform

by Chao Li, Wenxin Li, Guangqin Wu, Guojin Chen, Junyi Wu, Niushan Zhang, Yusen Gan, Dongqi Zhang and Chang Chen

Crystals 2024, 14(5), 389; https://doi.org/10.3390/cryst14050389 - 23 Apr 2024

Cited by 1 | Viewed by 995

Abstract

This study aims to develop equipment for the preparation of composite films and successfully implement a film thickness prediction function. During the research process, we segmented the mechanical structure of the composite thin film preparation equipment into distinct modules, completed the structural design of the core module, and validated the stability of the process chamber, as well as the reasonableness of the strength and stiffness through simulation. Additionally, we devised a regression model for predicting the film thickness of composite films. The input features for the model included the sputtering air pressure, sputtering current, and sputtering time for magnetron sputtering process samples, as well as the evaporation volume and evaporation current for vacuum evaporation process samples. Simultaneously, the output features were the film thickness for both process samples. Subsequently, we established the designed composite film preparation equipment and conducted experimental verification. During the experiments, we successfully prepared Cr-Al composite films and utilized AFM for surface morphology analysis. The results confirmed the excellent performance of the Cr-Al composite films produced by the equipment, demonstrating the reliability of the equipment. Full article

(This article belongs to the Special Issue Advances in Synthesis, Characterization, and Application of Thin Films)

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13 pages, 8452 KiB

Open AccessArticle

Growth and Properties of Ultra-Thin PTCDI-C8 Films on GaN(0001)

by Katarzyna Lament, Miłosz Grodzicki, Radosław Wasielewski, Piotr Mazur and Antoni Ciszewski

Crystals 2024, 14(3), 201; https://doi.org/10.3390/cryst14030201 - 20 Feb 2024

Cited by 1 | Viewed by 1726

Abstract

Ultra-thin PTCDI-C8 films are vapor-deposited under ultra-high vacuum (UHV) conditions onto surfaces of p- or n-doped GaN(0001) samples. The X-ray photoelectron spectroscopy (XPS) results reveal a lack of strong chemical interaction between the PTCDI-C8 molecule and the substrate. Changes in the electronic structure of the substrate or the adsorbed molecules due to adsorption are not noticed at the XPS spectra. Work function changes have been measured as a function of the film thickness. The position of the HOMO level for films of thicknesses 3.2–5.5 nm has been determined. Energy diagrams of the interface between p- and n-type GaN(0001) substates and the PTCDI-C8 films are proposed. The fundamental molecular building blocks of the PTCDI-C8 films on GaN(0001), assembled by self-organization, have been identified. They are rows of PTCDI-C8 molecules stacked in “stand-up” positions in reference to the substrate, supported by the π–π bonds which are formed between the molecular cores of the molecules and monomolecular layers constituted by rows which are tilted in reference to the layer plane. The layers are epitaxially oriented. The epitaxial relation between the rows and the crystallographic directions of the substrate are determined. A model of the PTCDI-C8 film’s growth on GaN(0001) substrate is proposed. The 3D islands of PTCDI-C8 molecules formed on the substrate surface during film deposition are thermodynamically unstable. The Volmer–Weber type of growth observed here is a kinetic effect. Rewetting processes are noticeable after film aging at room temperature or annealing at up to 100 °C. Full article

(This article belongs to the Special Issue Advances in Synthesis, Characterization, and Application of Thin Films)

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15 pages, 6390 KiB

Open AccessEditor’s ChoiceArticle

Sol–Gel Synthesis of ZnO:Li Thin Films: Impact of Annealing on Structural and Optical Properties

by Tatyana Ivanova, Antoaneta Harizanova, Tatyana Koutzarova, Benedicte Vertruyen and Raphael Closset

Crystals 2024, 14(1), 6; https://doi.org/10.3390/cryst14010006 - 20 Dec 2023

Cited by 3 | Viewed by 2185

Abstract

A sol–gel deposition approach was applied for obtaining nanostructured Li-doped ZnO thin films. ZnO:Li films were successfully spin-coated on quartz and silicon substrates. The evolution of their structural, vibrational, and optical properties with annealing temperature (300–600 °C) was studied by X-ray diffraction (XRD), Fourier Transform Infrared (FTIR), UV-VIS spectroscopic, and field emission scanning electron microscopic (FESEM) characterization techniques. It was found that lithium doping maintains the wurtzite arrangement of ZnO, with increasing crystallite sizes when increasing the annealing temperature. Analysis of the FTIR spectra revealed a broad main absorption band (around 404 cm⁻¹) for Li-doped films, implying the inclusion of Li into the ZnO lattice. The ZnO:Li films were transparent, with slightly decreased transmittance after the use of higher annealing temperatures. The porous network of undoped ZnO films was transformed to a denser, grained, packed structure, induced by lithium doping. Full article

(This article belongs to the Special Issue Advances in Synthesis, Characterization, and Application of Thin Films)

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