Reactive Magnetron Sputtering of ZrO 2 /Al 2 O 3 Coatings: Alumina Content and Structure Stability (original) (raw)
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Thermal stability of zirconia/alumina thin coatings produced by magnetron sputtering
Surface and Coatings Technology, 1997
Thin Zr02-A1103-YL03 coatings were deposited by reactive magnetron sputtering technique onto steel substrates. Annealing at 1273 K the ceramic ZrO*-A120j mixtures in air crystallise in the tetragonal phase and grain growth is observed. The A&O3 content limits the maximum observed grain size between 25 and 30 nm during the observation time of this study of about 1.8 x 10" s (500 h). In contrast, the ZrO-YL03 coatings revealed tetragonal grains with a size of about 200 nm. Diffusion processes cause the grain growth as well as the observed decrease of the intrinsic coating stress. Zirconia coatings stabilised by A1203 (without YZO,) generally show tetragonal grains but prolonged annealing at 1273 K decreases the effect of the rigid A&O3 matrix and the zirconia transforms into its monoclinic phase modification. Multilayered coatings of ZrOL with layer thickness lower to 6 nm also retained the tetragonal phase. Nevertheless, l-nm thick A1?03 spacing layers are not sufficient to suppress the diffusion. growth and subsequent phase transformation of the zirconia. 0 1997 Elsevier Science S.A.
Surface & Coatings Technology, 1999
In order to investigate the structure of PVD alumina coatings as a function of substrate temperature and deposition conditions, Al 2 O 3 films have been deposited by reactive magnetron sputtering at deposition temperatures between 100 and 600°C on cemented carbide and high speed steel substrates using aluminum targets, which were sputtered in an argon-oxygen plasma in RF, DC and pulsed mode, respectively. The influence of deposition temperature and sputtering conditions upon the crystal structure of the films has been investigated by X-ray diffraction, the hardness by microindentation. Furthermore, a correlation between film growth rate and oxygen partial pressure has been determined. The analyses revealed that the oxygen partial pressure during film deposition had strong influence on the resulting deposition rate and crystallinity, which is also significantly influenced by the deposition temperature. The process window for the deposition of crystalline coatings is very narrow for DC sputtering, while it is larger with RF and pulsed plasma sources. Depending on the process parameters oxygen partial pressure and plasma source, amorphous or crystalline c-Al 2 O 3 films with thicknesses in the range from 1 to 8 mm and hardness values up to 25 GPa have been deposited. Very low oxygen partial pressures led to the co-deposition of aluminum, while none of the chosen process parameters resulted in the formation of crystalline a-Al 2 O 3 .
Crystalline alumina coatings by reactive AC magnetron sputtering
Alumina coatings were deposited on silicon ͑111 orientation͒ substrates by reactive ac magnetron sputtering. Film deposition was done using Al targets and three O 2 / Ar gas flow rate ratios at 5 kW power. X-ray diffraction studies showed that films were crystalline and contained several phases of alumina. Secondary ion mass spectroscopy analyses were used to measure O / Al atomic ratio and Ar and H concentrations in the films. Hydrogen content in the coatings depended on the O 2 partial pressure used during sputtering and also on the arrival rate of Al and O species on the substrates and seemed to influence the crystallinity of the coatings.
The analysis of Al[2]O[3] coatings obtained by magnetron sputtering
2011
With the use of AFM, nanohardness and elastic modulus measuring, as well as measurements of the forces of cohesion, friction coefficient by means of a scratch test, oxide coatings of Al2O3, obtained by magnetron sputtering of Al were investigated. The hardness of the coating Al2O3, nanostructured film deposited on TiN, increased as compared with the coating deposited on steel. A comparison of the morphology of samples obtained by reactive magnetron sputtering synthesis and a source of RF plasma using oxygen ions was carried out. The mechanical characteristics of hardness, elastic modulus, adhesion strength and friction coefficient of obtained coatings were investigated.
Reactive dc magnetron sputter deposited Al2O3: large area coatings for industrial application
Surface and Coating Technology, 1999
O 3 films are produced with a pure Al source in the metallic state in an O 2 +Ar gas mixture using reactive d.c. magnetron sputtering. Substrates as large as 70×100 cm2 are uniformly coated at room temperature while moving in front of the cathode. The key to the success lies in utilizing a sufficiently high working gas pressure and a sufficiently large source-tosubstrate distance. Monte Carlo simulations are used to estimate the latter. The process is extremely stable, and despite the large target size, no arcing is detected.
Zr±B±O coatings were deposited on both construction steel and stainless steel substrates by magnetron sputtering of ZrB 2 targets in reactive Ar±O 2 gaseous mixtures. In this paper, the deposition rate and the structural and mechanical properties of Zr±B±O ®lms will be investigated as a function of the inlet oxygen¯ow rate. We will show that two domains are available owing to the sputtering phenomena. In the former, the coating enrichment is quite proportional to the oxygen¯ow rate. Even for a weak oxygen enrichment, amorphization of the Zr±B±O ®lms is observed which also decreases both their intrinsic internal stress and microhardness, thus improving the physical quality of the coatings. As the oxygen¯ow rate increases, the amorphous coatings, initially composed of a single-phase ZrB 22x O x solid solution, present an increasing fraction of amorphous ZrO 2 , and then, of amorphous B 2 O 3 simultaneously with the disappearance of the metallic solid solution. Higher oxygen¯ow rates allow the synthesis of optically transparent amorphous oxide mixture ®lms, the composition and mechanical properties of which become independent of the inlet oxygen¯ow rate. q 1999 Elsevier Science S.A. All rights reserved.
Characterization of bi-phased Zr 2 ON 2–ZrO 2 coatings deposited by RF magnetron sputtering
The aim of this work is to develop zirconium oxynitride coatings by RF magnetron sputtering on silicon substrates. The film properties were analyzed as a function of oxygen flux percentage in two different inert gas atmospheres namely argon and helium. At low oxygen flux percentage, Zr 2 ON 2 and ZrO 2 phases are observed from the structural characterization by X-ray diffraction. The atomic ratio of nonmetallic to metallic atoms (N + O)/Zr content varies from 1.22 to 2.03 for zirconium oxynitride films deposited in argon atmosphere and from 1.43 to 2.33 for films deposited in helium atmosphere. The thickness of the film was measured by surface profiler and the growth rate decreases from 11.33 to 5.1 nm/min for films deposited in argon atmosphere and from 7.01 to 3.75 nm/min for films deposited in helium atmosphere with increase in oxygen flux percentage. The films deposited are hydrophobic and the contact angle was measured by contact angle measuring system. Higher surface roughness and maximum contact angle values of 100°and 103°are observed for films deposited in argon and helium atmosphere respectively at low oxygen flux percentage (2.5%). The surface energy of films was calculated by two methods: Owens-Wendt's geometric mean and Wu's harmonic mean approach. The elevated surface energy values were observed with increase in oxygen flux percentage. The stress measurements of the deposited films were done by sin 2 ψ X-ray diffraction method which depends on the variation of Zr 2 ON 2 and m-ZrO 2 phases.
Surface and Coatings Technology, 1999
Stoichiometric Al 2 O 3 films are produced with a pure Al source in the metallic state in an O 2 +Ar gas mixture using reactive d.c. magnetron sputtering. Substrates as large as 70×100 cm2 are uniformly coated at room temperature while moving in front of the cathode. The key to the success lies in utilizing a sufficiently high working gas pressure and a sufficiently large source-tosubstrate distance. Monte Carlo simulations are used to estimate the latter. The process is extremely stable, and despite the large target size, no arcing is detected.
Applied Surface Science, 2015
17 ZrO x N y /ZrO 2 thin films were deposited on stainless steel using two different methods: 18 ultrasonic spray pyrolysis-nitriding (SPY-N) and the DC unbalanced magnetron sputtering 19 technique (UBMS). Using the first method, ZrO 2 was initially deposited and subsequently 20 nitrided in an anhydrous ammonia atmosphere at 1023 K at atmospheric pressure. For 21 UBMS, the film was deposited in an atmosphere of air/argon with a Φair/ΦAr flow ratio of 22 Page 2 of 23 A c c e p t e d M a n u s c r i p t 2 steel's resistance to corrosion using both techniques. The protective efficacy was evaluated 33 using electrochemical techniques based on linear polarization (LP). The results indicated 34 that the layers provide good resistance to corrosion when exposed to chloride-containing 35 media. 36 37 Keywords: 38 Physical vapor deposition (PVD), corrosion, zirconium oxynitride, coatings, X-ray photo-39 emission spectroscopy (XPS) 40 41 Page 3 of 23 A c c e p t e d M a n u s c r i p t 3 sputtering, with its variations: balanced DC magnetron sputtering, unbalanced DC 65 magnetron sputtering (UBMS), and sputtering with radio frequency [12,13], have been 66 those traditionally used because they require short times of deposit and cleaning is easy, 67 and because of the reproducibility of the layer formed under strictly controlled conditions. 68 However, they are costly and difficult to apply on a large scale. It is because of this that 69 Page 4 of 23 A c c e p t e d M a n u s c r i p t 4 polar organic solvents: dichloromethane, acetone, and isopropanol. ZrO x N y coatings were 97 deposited using the UBMS technique. A high purity Zr target (99.99%) was used, and the 98 target-substrate distance was 50 mm. Non-commercial equipment was employed to grow 99 the ZrO x N y films via the UBMS technique, described in a previous paper [9]. The 100 substrates were placed in a chamber which was initially subjected to a process of 101 evacuation to about 4 × 10− 1 Pa using a mechanical pump. Then, with the help of a turbo 102 molecular pump, the vacuum was increased, reaching a pressure of 1.0 × 10 −3 Pa. The flow 103 of the gas was controlled and measured using an MKS mass flow controller. The argon had 104 a constant flow rate of 9.0 standard cubic centimeters per minute (sccm), and air flow rates 105 were 3.0 sccm. Discharge power was 350 W, and plasma current was 170 mA. All coatings 106 were grown at room temperature for 40 min. Under these experimental conditions, films 107 were deposited with a thickness of approximately 710 nm. See Figure 1a. 108 109