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21 pages, 8435 KiB

Open AccessArticle

Influence of Co-Content on the Optical and Structural Properties of TiO_x Thin Films Prepared by Gas Impulse Magnetron Sputtering

by Patrycja Pokora, Damian Wojcieszak, Piotr Mazur, Małgorzata Kalisz and Malwina Sikora

Coatings 2023, 13(5), 955; https://doi.org/10.3390/coatings13050955 - 19 May 2023

Cited by 2 | Viewed by 1101

Abstract

Nonstoichiometric (Ti,Co)Ox coatings were prepared using gas-impulse magnetron sputtering (GIMS). The properties of coatings with 3 at.%, 19 at.%, 44 at.%, and 60 at.% Co content were compared to those of TiO_x and CoO_x films. Structural studies with the aid of [...] Read more.

Nonstoichiometric (Ti,Co)Ox coatings were prepared using gas-impulse magnetron sputtering (GIMS). The properties of coatings with 3 at.%, 19 at.%, 44 at.%, and 60 at.% Co content were compared to those of TiO_x and CoO_x films. Structural studies with the aid of GIXRD indicated the amorphous nature of (Ti,Co)Ox. The fine-columnar, homogeneous microstructure was observed on SEM images, where cracks were identified only for films with a high Co content. On the basis of XPS measurements, TiO₂, CoO, and Co₃O₄ forms were found on their surface. Optical studies showed that these films were semi-transparent (T > 46%), and that the amount of cobalt in the film had a significant impact on the decrease in the transparency level. A shift in the absorption edge position (from 337 to 387 nm) and a decrease in their optical bandgap energy (from 3.02 eV to more than 2.60 eV) were observed. The hardness of the prepared films changed slightly (ca. 6.5 GPa), but only the CoO_x film showed a slightly lower hardness value than the rest of the coatings (4.8 GPa). The described studies allowed partial classification of non-stoichiometric (Ti,Co)Ox thin-film materials according to their functionality. Full article

(This article belongs to the Special Issue Advances in Thin Film Fabrication by Magnetron Sputtering)

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15 pages, 7170 KiB

Open AccessArticle

Particle-in-Cell Simulations for the Improvement of the Target Erosion Uniformity by the Permanent Magnet Configuration of DC Magnetron Sputtering Systems

by Young Hyun Jo, Cheongbin Cheon, Heesung Park and Hae June Lee

Coatings 2023, 13(4), 749; https://doi.org/10.3390/coatings13040749 - 07 Apr 2023

Viewed by 1519

Abstract

Improving the target erosion uniformity in a commercial direct current (DC) magnetron sputtering system is a crucial issue in terms of process management as well as enhancing the properties of the deposited film. Especially, nonuniform target erosion was reported when the magnetic flux [...] Read more.

Improving the target erosion uniformity in a commercial direct current (DC) magnetron sputtering system is a crucial issue in terms of process management as well as enhancing the properties of the deposited film. Especially, nonuniform target erosion was reported when the magnetic flux density gradient existed. A two-dimensional (2D) and a three-dimensional (3D) parallelized particle-in-cell (PIC) simulation were performed to investigate relationships between magnetic fields and the target erosion profile. The 2D PIC simulation presents the correlation between the heating mechanism and the spatial density profiles under various magnet conditions. In addition, the 3D PIC simulation shows the different plasma characteristics depending on the azimuthal asymmetry of the magnets and the mechanism of the mutual competition of the E × B drift and the grad-B drift for the change in the electron density uniformity. Full article

(This article belongs to the Special Issue Advances in Thin Film Fabrication by Magnetron Sputtering)

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13 pages, 2199 KiB

Open AccessArticle

Improved Methodology of Cross-Sectional SEM Analysis of Thin-Film Multilayers Prepared by Magnetron Sputtering

by Malwina Sikora, Damian Wojcieszak, Aleksandra Chudzyńska and Aneta Zięba

Coatings 2023, 13(2), 316; https://doi.org/10.3390/coatings13020316 - 31 Jan 2023

Cited by 4 | Viewed by 3485

Abstract

In this work, an improved methodology of cross-sectional scanning electron microscopy (SEM) analysis of thin-film Ti/V/Ti multilayers was described. Multilayers with various thicknesses of the vanadium middle layer were prepared by magnetron sputtering. The differences in cross sections made by standard fracture, focused [...] Read more.

In this work, an improved methodology of cross-sectional scanning electron microscopy (SEM) analysis of thin-film Ti/V/Ti multilayers was described. Multilayers with various thicknesses of the vanadium middle layer were prepared by magnetron sputtering. The differences in cross sections made by standard fracture, focused ion beam (FIB)/Ga, and plasma focused ion beam (PFIB)/Xe have been compared. For microscopic characterization, the Helios NanoLab 600i microscope and the Helios G4 CXe with the Quanta XFlash 630 energy dispersive spectroscopy detector from Bruker were used. The innovative multi-threaded approach to the SEM preparation itself, which allows us to retain information about the actual microstructure and ensure high material contrast even for elements with similar atomic numbers was proposed. The fracture technique was the most noninvasive for microstructure, whereas FIB/PFIB results in better material contrast (even than EDS). There were only subtle differences in cross sections made by FIB-Ga and PFIB-Xe, but the decrease in local amorphization or slightly better contrast was in favor of Xe plasma. It was found that reliable information about the properties of modern nanomaterials, especially multilayers, can be obtained by analyzing a two-part SEM image, where the first one is a fracture, while the second is a PFIB cross section. Full article

(This article belongs to the Special Issue Advances in Thin Film Fabrication by Magnetron Sputtering)

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18 pages, 6052 KiB

Open AccessArticle

P-type (CuTi)Ox Thin Films Deposited by Magnetron Co-Sputtering and Their Electronic and Hydrogen Sensing Properties

by Ewa Mańkowska, Michał Mazur, Jarosław Domaradzki and Damian Wojcieszak

Coatings 2023, 13(2), 220; https://doi.org/10.3390/coatings13020220 - 17 Jan 2023

Cited by 1 | Viewed by 1300

Abstract

Thin films of copper oxide (Cu_xO), titanium oxide (TiO_x), and several mixtures of copper and titanium oxides ((CuTi)Ox) were deposited using magnetron sputtering. X-ray diffraction analysis of the as-deposited TiO_x thin film revealed the presence of TiO crystallites, [...] Read more.

Thin films of copper oxide (Cu_xO), titanium oxide (TiO_x), and several mixtures of copper and titanium oxides ((CuTi)Ox) were deposited using magnetron sputtering. X-ray diffraction analysis of the as-deposited TiO_x thin film revealed the presence of TiO crystallites, while in the case of (CuTi)Ox with the lowest amount of copper, metallic Cu crystallites were found. In the case of (Cu_0.77Ti_0.23)Ox and Cu_xO thin films, characteristic peaks for metallic copper and copper oxides were observed in their diffractograms. It was found that post-process annealing at 473 K considerably affects the microstructure of (CuTi)Ox thin films. After annealing, anatase phase was observed in (Cu_0.23Ti_0.77)Ox and (Cu_0.41Ti_0.59)Ox thin films. In turn, the (Cu_0.77Ti_0.23)Ox and Cu_xO films were formed only in the copper oxide phase. The (Cu_0.77Ti_0.23)Ox film annealed at 473 K showed the best opto-electronic performance, as it had the highest transmission and the lowest resistivity. However, the greatest advantage of this thin film was the p-type semiconducting behavior, which was the strongest of all of the thin films in this work, as indicated by the measurement of the Seebeck coefficient. All deposited thin films were sensitive to hydrogen exposure, while the best sensor response of 10.9 was observed for the (Cu_0.77Ti_0.23) Ox thin film annealed at 473 K. Full article

(This article belongs to the Special Issue Advances in Thin Film Fabrication by Magnetron Sputtering)

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20 pages, 8497 KiB

Open AccessArticle

Synthesis of Magnetron-Sputtered TiN Thin-Films on Fiber Structures for Pulsed-Laser Emission and Refractive-Index Sensing Applications at 1550 nm

by Omar Gaspar Ramírez, Manuel García Méndez, Ricardo Iván Álvarez Tamayo and Patricia Prieto Cortés

Coatings 2023, 13(1), 95; https://doi.org/10.3390/coatings13010095 - 04 Jan 2023

Viewed by 1400

Abstract

In this work, a set of titanium nitrides thin-films was synthesized with the technique of reactive RF and DC magnetron-sputtering. To demonstrate the versatility and effectiveness of the deposition technique, thin films were deposited onto different fiber structures varying the deposition parameters for [...] Read more.

In this work, a set of titanium nitrides thin-films was synthesized with the technique of reactive RF and DC magnetron-sputtering. To demonstrate the versatility and effectiveness of the deposition technique, thin films were deposited onto different fiber structures varying the deposition parameters for optical applications as saturable absorbers in passively q-switched fiber lasers and as lossy mode resonance fiber refractometers. After deposition, optical and electronical properties of samples were characterized by UV–Vis and XPS spectroscopies, respectively. Samples presented coexisting phases of Ti nitride and oxide, where the nitride phase was non-stoichiometric metallic-rich, with a band gap in the range of E_g = 3.4–3.7 eV. For all samples, glass substrates were used as templates, and on top of them, optical fibers were mounted to be covered with their respective titanium compounds. Full article

(This article belongs to the Special Issue Advances in Thin Film Fabrication by Magnetron Sputtering)

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13 pages, 3376 KiB

Open AccessArticle

Microstructure and Properties of MAO-Cu/Cu-(HEA)N Composite Coatings on Titanium Alloy

by Zhao Wang, Nan Lan, Yong Zhang and Wanrong Deng

Coatings 2022, 12(12), 1877; https://doi.org/10.3390/coatings12121877 - 03 Dec 2022

Cited by 2 | Viewed by 1411

Abstract

In this paper, MAO-Cu/Cu-(HEA)N composite coatings on TC4 titanium alloy were prepared by combining micro arc oxidation (MAO) with magnetron sputtering (MS) to enhance the wear resistance and antibacterial ability of the substrate in simulated seawater. The number of micropores on the surface [...] Read more.

In this paper, MAO-Cu/Cu-(HEA)N composite coatings on TC4 titanium alloy were prepared by combining micro arc oxidation (MAO) with magnetron sputtering (MS) to enhance the wear resistance and antibacterial ability of the substrate in simulated seawater. The number of micropores on the surface of the composite coatings decreased with increasing CuSO₄ concentration in the electrolyte, causing the surfaces to be flat and smooth. XPS and EDS analyses revealed that the MAO-Cu/Cu-(HEA)N composite coatings predominately contained TiO₂, Cu₂O, and (HEA)N. Moreover, the addition of CuSO₄ increased the growth rate of the MAO coatings. Comparatively, the MAO-Cu/Cu-(HEA)N composite coating with 5 g/L CuSO₄ showed superior wear resistance, reduced friction coefficient (approximately 0.2), and shallow and narrow grinding cracks were observed compared to the other coatings. Antibacterial experiments showed that the MAO-Cu/Cu-(HEA)N composite coatings had better bacterial killing effects than the TC4 substrate, which is of great significance to the antifouling abilities of titanium alloys in marine applications. Full article

(This article belongs to the Special Issue Advances in Thin Film Fabrication by Magnetron Sputtering)

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14 pages, 3269 KiB

Open AccessFeature PaperArticle

On the Control of Hot Nickel Target Magnetron Sputtering by Distribution of Power Pulses

by Rafal Chodun, Bartosz Wicher, Katarzyna Nowakowska-Langier, Roman Minikayev, Marlena Dypa-Uminska and Krzysztof Zdunek

Coatings 2022, 12(7), 1022; https://doi.org/10.3390/coatings12071022 - 19 Jul 2022

Cited by 4 | Viewed by 1742

Abstract

This paper presents the experimental results of high-temperature sputtering of nickel targets by the Gas Injection Magnetron Sputtering (GIMS) technique. The GIMS technique is a pulsed magnetron sputtering technique that involves the generation of plasma pulses by injecting small doses of gas into [...] Read more.

This paper presents the experimental results of high-temperature sputtering of nickel targets by the Gas Injection Magnetron Sputtering (GIMS) technique. The GIMS technique is a pulsed magnetron sputtering technique that involves the generation of plasma pulses by injecting small doses of gas into the zone of the magnetron target surface. Using a target with a dedicated construction to limit heat dissipation and the proper use of injection parameters and electrical power density, the temperature of the target during sputtering can be precisely controlled. This feature of the GIMS technique was used in an experiment with sputtering nickel targets of varying thicknesses and temperatures. Plasma emission spectra and current-voltage waveforms were studied to characterize the plasma process. The thickness, structure, phase composition, and crystallite size of the nickel layers produced on silicon substrates were investigated. Our experiment showed that although the most significant increase in growth kinetics was observed for high temperatures, the low sputtering temperature range may be the most interesting from a practical perspective. The excited plasma has the highest energy in the sputtering temperature range, just above the Curie temperature. Full article

(This article belongs to the Special Issue Advances in Thin Film Fabrication by Magnetron Sputtering)

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10 pages, 6356 KiB

Open AccessArticle

Thermal Stability of the Copper and the AZO Layer on Textured Silicon

by Ping-Hang Chen, Wen-Jauh Chen and Jiun-Yi Tseng

Coatings 2021, 11(12), 1546; https://doi.org/10.3390/coatings11121546 - 16 Dec 2021

Cited by 4 | Viewed by 2309

Abstract

Transparent conductive oxide (TCO) film is the most widely used front electrode in silicon heterojunction (SHJ) solar cells. A copper metallization scheme can be applied to the SHJ process. The abundance of zinc in the earth’s crust makes aluminum-doped zinc oxide (AZO) an [...] Read more.

Transparent conductive oxide (TCO) film is the most widely used front electrode in silicon heterojunction (SHJ) solar cells. A copper metallization scheme can be applied to the SHJ process. The abundance of zinc in the earth’s crust makes aluminum-doped zinc oxide (AZO) an attractive low-cost substitute for indium-based TCOs. No work has focused on the properties of the copper and AZO layers on the textured silicon for solar cells. This work deposited an aluminum-doped zinc oxide layer and copper metal layer on textured (001) silicon by a sputtering to form Cu/AZO/Si stacks. The structures of Cu/AZO/Si are characterized by scanning electron microscope (SEM), scanning transmission electron microscope (STEM), and energy-dispersive X-ray spectrometer (EDS). The results show that the copper thin film detached from AZO in the valley of the textured silicon substrate at a temperature of 400 °C. Additionally, the gap between the copper and AZO layers increases as temperature increases, and the 65 nm thickness AZO layer was found to be preserved up to 800 °C. Full article

(This article belongs to the Special Issue Advances in Thin Film Fabrication by Magnetron Sputtering)

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8 pages, 1991 KiB

Open AccessArticle

Annealing Studies of Copper Indium Oxide (Cu₂In₂O₅) Thin Films Prepared by RF Magnetron Sputtering

by Giji Skaria, Ashwin Kumar Saikumar, Akshaya D. Shivprasad and Kalpathy B. Sundaram

Coatings 2021, 11(11), 1290; https://doi.org/10.3390/coatings11111290 - 24 Oct 2021

Cited by 4 | Viewed by 1993

Abstract

Copper indium oxide (Cu₂In₂O₅) thin films were deposited by the RF magnetron sputtering technique using a Cu₂O:In₂O₃ target. The films were deposited on glass and quartz substrates at room temperature. The films [...] Read more.

Copper indium oxide (Cu₂In₂O₅) thin films were deposited by the RF magnetron sputtering technique using a Cu₂O:In₂O₃ target. The films were deposited on glass and quartz substrates at room temperature. The films were subsequently annealed at temperatures ranging from 100 to 900 °C in an O₂ atmosphere. The X-ray diffraction (XRD) analysis performed on the samples identified the presence of Cu₂In₂O₅ phases along with CuInO₂ or In₂O₃ for the films annealed above 500 °C. An increase in grain size was identified with the increase in annealing temperatures from the XRD analysis. The grain sizes were calculated to vary between 10 and 27 nm in films annealed between 500 and 900 °C. A morphological study performed using SEM further confirmed the crystallization and the grain growth with increasing annealing temperatures. All films displayed high optical transmission of more than 70% in the wavelength region of 500–800 nm. Optical studies carried out on the films indicated a small bandgap change in the range of 3.4–3.6 eV during annealing. Full article

(This article belongs to the Special Issue Advances in Thin Film Fabrication by Magnetron Sputtering)

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15 pages, 4355 KiB

Open AccessArticle

Physical Properties of Fe₃Si Films Coated through Facing Targets Sputtering after Microwave Plasma Treatment

by Nattakorn Borwornpornmetee, Peerasil Charoenyuenyao, Rawiwan Chaleawpong, Boonchoat Paosawatyanyong, Rungrueang Phatthanakun, Phongsaphak Sittimart, Kazuki Aramaki, Takeru Hamasaki, Tsuyoshi Yoshitake and Nathaporn Promros

Coatings 2021, 11(8), 923; https://doi.org/10.3390/coatings11080923 - 01 Aug 2021

Cited by 5 | Viewed by 2127

Abstract

Fe₃Si films are deposited onto the Si(111) wafer using sputtering with parallel facing targets. Surface modification of the deposited Fe₃Si film is conducted by using a microwave plasma treatment under an Ar atmosphere at different powers of 50, 100 [...] Read more.

Fe₃Si films are deposited onto the Si(111) wafer using sputtering with parallel facing targets. Surface modification of the deposited Fe₃Si film is conducted by using a microwave plasma treatment under an Ar atmosphere at different powers of 50, 100 and, 150 W. After the Ar plasma treatment, the crystallinity of the coated Fe₃Si films is enhanced, in which the orientation peaks, including (220), (222), (400), and (422) of the Fe₃Si are sharpened. The extinction rule suggests that the B₂–Fe₃Si crystallites are the film’s dominant composition. The stoichiometry of the Fe₃Si surfaces is marginally changed after the treatment. An increase in microwave power damages the surface of the Fe₃Si films, resulting in the generation of small pinholes. The roughness of the Fe₃Si films after being treated at 150 W is insignificantly increased compared to the untreated films. The untreated Fe₃Si films have a hydrophobic surface with an average contact angle of 101.70°. After treatment at 150 W, it turns into a hydrophilic surface with an average contact angle of 67.05° because of the reduction in the hydrophobic carbon group and the increase in the hydrophilic oxide group. The hardness of the untreated Fe₃Si is ~9.39 GPa, which is kept at a similar level throughout each treatment power. Full article

(This article belongs to the Special Issue Advances in Thin Film Fabrication by Magnetron Sputtering)

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11 pages, 3134 KiB

Open AccessArticle

Properties of RF Magnetron-Sputtered Copper Gallium Oxide (CuGa₂O₄) Thin Films

by Ashwin Kumar Saikumar, Sreeram Sundaresh, Shraddha Dhanraj Nehate and Kalpathy B. Sundaram

Coatings 2021, 11(8), 921; https://doi.org/10.3390/coatings11080921 - 01 Aug 2021

Cited by 10 | Viewed by 2456

Abstract

Thin films of CuGa₂O₄ were deposited using an RF magnetron-sputtering technique for the first time. The sputtered CuGa₂O₄ thin films were post-deposition annealed at temperatures varying from 100 to 900 °C in a constant O₂ ambience [...] Read more.

Thin films of CuGa₂O₄ were deposited using an RF magnetron-sputtering technique for the first time. The sputtered CuGa₂O₄ thin films were post-deposition annealed at temperatures varying from 100 to 900 °C in a constant O₂ ambience for 1.5 h. Structural and morphological studies were performed on the films using X-ray diffraction analysis (XRD) and a Field Emission Scanning Electron Microscope (FESEM). The presence of CuGa₂O₄ phases along with the CuO phases was confirmed from the XRD analysis. The minimum critical temperature required to promote the crystal growth in the films was identified to be 500 °C using XRD analysis. The FESEM images showed an increase in the grain size with an increase in the annealing temperature. The resistivity values of the films were calculated to range between 6.47 × 10³ and 2.5 × 10⁸ Ωcm. Optical studies were performed on all of the films using a UV-Vis spectrophotometer. The optical transmission in the 200–800 nm wavelength region was noted to decrease with an increase in the annealing temperature. The optical bandgap value was recorded to range between 3.59 and 4.5 eV and showed an increasing trend with an increase in the annealing temperature. Full article

(This article belongs to the Special Issue Advances in Thin Film Fabrication by Magnetron Sputtering)

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Review

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18 pages, 2395 KiB

Open AccessReview

Sputtering Process of Sc_xAl_1−xN Thin Films for Ferroelectric Applications

by Jacob M. Wall and Feng Yan

Coatings 2023, 13(1), 54; https://doi.org/10.3390/coatings13010054 - 28 Dec 2022

Cited by 4 | Viewed by 2001

Abstract

Several key sputtering parameters for the deposition of Sc_xAl_1−xN such as target design, sputtering atmosphere, sputtering power, and substrate temperature are reviewed in detail. These parameters serve a crucial role in the ability to deposit satisfactory films, achieve the [...] Read more.

Several key sputtering parameters for the deposition of Sc_xAl_1−xN such as target design, sputtering atmosphere, sputtering power, and substrate temperature are reviewed in detail. These parameters serve a crucial role in the ability to deposit satisfactory films, achieve the desired stoichiometry, and meet the required film thickness. Additionally, these qualities directly impact the degree of c-axis orientation, grain size, and surface roughness of the deposited films. It is systematically shown that the electric properties of Sc_xAl_1−xN are dependent on the crystal quality of the film. Although it is not possible to conclusively say what the ideal target design, sputtering atmosphere, sputtering power, and substrate temperature should be for all sputtering processes, the goal of this paper is to analyze the impacts of the various sputtering parameters in detail and provide some overarching themes that arise to assist future researchers in the field in quickly tuning their sputtering processes to achieve optimum results. Full article

(This article belongs to the Special Issue Advances in Thin Film Fabrication by Magnetron Sputtering)

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