High Power Impulse Magnetron Sputtering Research Articles

Microstructure and mechanical properties of Ti-Nb alloys: comparing conventional powder metallurgy, mechanical alloying, and high power impulse magnetron sputtering processes for supporting materials screening

AbstractAt the interface of thin film development and powder metallurgy technologies, this study aims to characterise the mechanical properties, lattice constants and phase formation of Ti-Nb alloys (8–30 at.%) produced by different manufacturing methods, including conventional powder metallurgy (PM), mechanical alloying (MA) and high power impulse magnetron sputtering (HiPIMS). A central aspect of this research was to investigate the different energy states achievable by each synthesis method. The findings revealed that as the Nb content increased, both the hardness and Young’s modulus of the PM samples decreased (from 4 to 1.5 and 125 to 85 GPa, respectively). For the MA alloys, the hardness and Young’s modulus varied between 3.2 and 3.9 and 100 to 116 GPa, respectively, with the lowest values recorded for 20% Nb (3.2 and 96 GPa). The Young’s modulus of the HiPIMS thin film samples did not follow a specific trend and varied between 110 and 138 GPa. However, an increase in hardness (from 3.6 to 4.8 GPa) coincided with an increase in the β2 phase contribution for films with the same chemical composition (23 at.% of Nb). This study highlights the potential of using HiPIMS gradient films for high throughput analysis for PM and MA techniques. This discovery is important as it provides a way to reduce the development time for complex alloy systems in biomaterials as well as other areas of materials engineering. Graphical abstract

Achieving a High Thermally Conductive One Micron AlN Deposition by High Power Impulse Magnetron Sputtering plus Kick.

High-power impulse magnetron sputtering (HiPIMS) plus kick is a physical vapor deposition method that employs bipolar microsecond-scale voltage pulsing to precisely control the ion energy during sputter deposition. HiPIMS plus kick for AlN deposition is difficult since nitride deposition is challenged by low surface diffusion and high susceptibility to ion damage. In this current study, a systematic examination of the process parameters of HiPIMS plus kick was conducted. Under optimized main negative pulsing conditions, this study documented that a 25 V positive kick biasing for AlN deposition is ideal for optimizing a high quality film, as shown by X-ray diffraction and transmission electron microscopy as well as optimal thermal conductivity while increasing high speed deposition (25 nm/min) and obtaining ultrasmooth surfaces (rms roughness = 0.5 nm). HiPIMS plus kick was employed to deposit a single-texture 1 μm AlN film with a 7.4° rocking curve, indicating well oriented grains, which correlated with high thermal conductivity (121 W/m·K). The data are consistent with the optimal kick voltage enabling enhanced surface diffusion due to ion-substrate collisions without damaging the AlN grains.

Friction and Wear of Hard Yet Tough TiN Coatings Deposited Using High-Power Impulse Magnetron Sputtering

The friction and wear response of hard coatings is complex, which largely depends on a good combination of hardness and toughness, and their service life is difficult to predict. Hence, in this work, hard yet tough TiN coatings were deposited using high-power impulse magnetron sputtering at 5–10 kW. With increasing sputtering power, the coatings showed a transition in crystal texture from (200) to (111), along with a refinement in microstructure, leading to an improvement in hardness (H) of 29.8–31.2 GPa and an effective Young’s modulus (E*) of 310–365 GPa. The hard yet tough TiN coatings deposited at 6.5 kW exhibited the highest H/E* and H3/E*2 ratios of 0.097 and 0.29, respectively, as well as the highest fracture toughness of 2.1 MPa·m1/2 and elastic recovery of 42.5%. Accordingly, the coatings possessed an enhanced adhesion and cohesion, in terms of micro-scratch critical load (LC3 = 19.67 N) and HF Rockwell HF1 level. The friction and wear response of hard yet tough TiN coatings under the normal load of 1–10 N were investigated to explore their durability and predict their critical load up to failure. Wear mechanisms changed from oxidative to severe abrasive wear, with load increasing from 1 to 10 N. At 2–5 N, a combination of oxidative and abrasive wear was observed. The coatings maintained their integrity up to the critical load of 9.4 N before failure event, with a maximum wear track depth of 1.8 μm, indicating their durability under the loading conditions.

Enhancement of hole mobility in high-rate reactively sputtered Cu2O thin films induced by laser thermal annealing

In presented work, a reactive high-power impulse magnetron sputtering (r-HiPIMS) was used for high-rate deposition (≈ 170 nm/min) of Cu2O films. Films were deposited on a standard soda-lime glass (SLG) substrate at a temperature of 190 °C. As-deposited films exhibit poor hole mobility in the orders of ≈ 1 cm2/Vs. We have systematically studied the effect of laser thermal annealing (LTA) procedure performed using high-power infrared laser under different laser parameters (number of pulses, length of the pulse). We have found, LTA procedure could significantly enhance the hole mobility (up to 24 cm2/Vs in our case). We have also fitted the results of a temperature-dependent Hall measurement to clarify the mechanism of the reported increase in hole mobility. Moreover, we have discussed the effect of the LTA procedure on microstructure (crystallinity, surface morphology) and on the value of optical band gap.

Investigating different carbon-based target materials: Can we improve ionization in HiPIMS for the deposition of diamondlike carbon films?

Investigating different carbon-based target materials: Can we improve ionization in HiPIMS for the deposition of diamondlike carbon films?

2D analysis of sputtered species transport in high-power impulse magnetron sputtering (HiPIMS) discharge

Among the numerous advantages of the high-power impulse magnetron sputtering (HiPIMS) technique, the most important is the enhanced ionization degree of sputtered species contributing to the film growth. Consequently, the quality of deposited thin films is highly improved. Still, the optimization process is challenging due to the complexity associated with the intricate transport of the sputtered species, ionized or neutrals. The scarce knowledge available on the spatial distribution of these species when operating a HiPIMS discharge makes the quantitative prediction of any deposition feature particularly difficult. In this paper, we discuss the influence of experimentally controllable quantities, such as gas pressure and target current density, on the transport of sputtered titanium in non-reactive (argon) HiPIMS, namely, on the behavior of metal atoms and metal ion fluxes intercepting the substrate. Systematic quantitative measurements were performed in a diameter normal plane on a circular planar target. Hence, the 2D spatial distribution of the ionized flux fraction (IFF) and the total flux of titanium sputtered particles (deposition rate) are evaluated by biasing a quartz crystal microbalance equipped with an electron magnetic filter. The wide range of parameters we examined allows us to predict and optimize the flux of sputtered species based on complete mapping of the IFF of sputtered particles.

Effect of titanium and deposition parameters on microstructure and mechanical properties of W-Ti-B thin films deposited by High Power Impulse Magnetron Sputtering

Tungsten diboride alloyed with transition metals provides an opportunity to obtain exceptional mechanical, physical, and chemical properties. We report a strategy for designing and synthesizing of superhard and low-compressible ceramic thin films with increased toughness and lowered residual stresses (σ < −0.9 GPa) deposited with high-power impulse magnetron sputtering (HiPIMS) from one target. The addition of 7–12 % titanium promotes additional strengthening mechanisms of the layers in one material, leading to the improvement of wear resistance compared to an alloyed WB2-z yet at even higher hardness 43.8 ± 2.1 GPa and nanoindentation toughness 4.9 ± 0.2 MPa√m. The compression of the micropillar shows that titanium addition changed the type of nanoindentation from cracking along the slip plane to bulging on the top of the pillar and next the crack initiation along column boundaries. The highest adhesion of the layers is obtained for addition of 7 % titanium and in all cases the wear has abrasive character. The controlled use of 200 μs pulses during synthesis with HiPIMS allows for an increase in the deposition rate and maintaining exceptional mechanical properties of the layers even at a substrate temperature of 300 °C.

On double-layer and reverse discharge creation during long positive voltage pulses in a bipolar HiPIMS discharge

Time-resolved Langmuir probe diagnostics at the discharge centerline and at three distances from the target ( 35mm , 60mm , and 100mm ) was carried out during long positive voltage pulses (a duration of 500μs and a preset positive voltage of 100V ) in bipolar high-power impulse magnetron sputtering of a Ti target (a diameter of 100mm ) using an unbalanced magnetron. Fast-camera spectroscopy imaging recorded light emission from Ar and Ti atoms and singly charged ions during positive voltage pulses. It was found that during the long positive voltage pulse, the floating and the plasma potentials suddenly decrease, which is accompanied by the presence of anode light located on the discharge centerline between the target center and the magnetic null of the magnetron’s magnetic field. These light patterns are related to the ignition of a reverse discharge, which leads to the subsequent rise in the plasma and the floating potentials. The reversed discharge is burning up to the end of the positive voltage pulse, but the plasma and floating potentials have lower values than the values from the initial part of the positive voltage pulse. Secondary electron emission induced by the impinging Ar+ ions to the grounded surfaces in the vicinity of the discharge plasma together with the mirror configuration of the magnetron magnetic field are identified as the probable causes of the charge double-layer structure formation in front of the target and the ignition of the reverse discharge.

The structure and properties of high-entropy (MoTaNbZrHf)-Si-B coatings deposited by DCMS and HIPIMS methods using the multilayer target

This article reports the results of comparative studies of the composition, structure, high-temperature oxidation resistance, mechanical and tribological properties of (MoTaNbZrHf)-Si-B coatings prepared at an identical average power of 1 kW by direct current magnetron sputtering (DCMS) and high-power impulse magnetron sputtering (HIPIMS). Switching from the DCMS to the HIPIMS mode is found to increase adhesion and crack resistance of the coatings and their wear resistance under friction sliding and cyclic impact conditions, as well as reduce the depth of oxidation at 1300 °C threefold. The record-breaking values of high-temperature oxidation resistance at 1500 °C are achieved due to formation of a surface film based on the borosilicate glass (a-Si:B:O) containing crystallites of the t-HfSiO4, o-Ta2O5, m-HfO2, and m-ZrO2 phases.

Deuterium retention in tungsten co-deposits with neon and argon inclusions

Deuterium (D) retention in tungsten (W) co-deposited layers, in the presence of neon (Ne) and argon (Ar), was investigated using the bipolar High Power Impulse Magnetron Sputtering (BP-HiPIMS) technique. The deposited layers have a polycrystalline structure, with a preferential growth of W(110) phase. The concentration of D and noble gases (Ne and Ar) is almost constant throughout the depth of the layers. In a D2-Ar discharge, the deposited layers exhibit compressive stress, indicating that Ar is mostly incorporated into the interstitial sites of the W crystal lattice. D retention increases when Ne is added in the discharge, especially when the deposited layer is bombarded with highly energetic ions. Low energy Ne ions (below the W damaging threshold) induce compressive stress, indicating that Ne atoms occupy interstitial sites in the W crystal lattice. High energy Ne ions induce tensile stress, a sign that Ne is trapped in the grain boundaries as inert-gas-vacancy defects, leading to a grain-boundary relaxation. In the presence of Ne, the ion acceleration towards the layer from 0 V to 300 V results in an increase of the D content of about three times, from 3.2 at.% to 8.6 at.%.

The Enhanced Performance of Oxide Thin-Film Transistors Fabricated by a Two-Step Deposition Pressure Process.

It is usually difficult to realize high mobility together with a low threshold voltage and good stability for amorphous oxide thin-film transistors (TFTs). In addition, a low fabrication temperature is preferred in terms of enhancing compatibility with the back end of line of the device. In this study, α-IGZO TFTs were prepared by high-power impulse magnetron sputtering (HiPIMS) at room temperature. The channel was prepared under a two-step deposition pressure process to modulate its electrical properties. X-ray photoelectron spectra revealed that the front-channel has a lower Ga content and a higher oxygen vacancy concentration than the back-channel. This process has the advantage of balancing high mobility and a low threshold voltage of the TFT when compared with a conventional homogeneous channel. It also has a simpler fabrication process than that of a dual active layer comprising heterogeneous materials. The HiPIMS process has the advantage of being a low temperature process for oxide TFTs.

Dielectric properties of hafnium oxide film prepared by HiPIMS at different O2/Ar ratios and their influences on TFT performance

High-k hafnium oxide (HfO2) film was prepared by high power impulse magnetron sputtering (HiPIMS). The influences of oxygen supply on the plasma state, film properties and TFT performance were investigated. The films are near-stoichiometric and preferentially (−1 1 1)-orientated. When the oxygen supply increased from 1% to 3%, the excitation/ionization rate of the plasma species increased, leading to higher crystallinity, higher density, and lower oxygen vacancy defect concentration of the film, therefore improving the dielectric properties of the film. When the oxygen supply further increased to 5%, the excitation/ionization rate decreased, thereby leading to lower crystallinity, lower density, and higher oxygen vacancy defect concentration of the film, therefore deteriorating the dielectric properties of the film. The film deposited at 3% oxygen supply exhibited the best dielectric properties with the highest k value of 24 and the highest breakdown-electric field (4.7 MV/cm), which should be attributed to the high crystallinity, high density and low oxygen vacancy defect concentration of the film. Finally, transparent thin film transistors (TFTs) with ITO gate electrode, HfO2 gate dielectric layer and indium-gallium-zinc oxide channel were fabricated on flexible colorless polyimide substrate at full room temperature by all HiPIMS process. The fixed positive charges and k value of HfO2 film have significant effects on the TFT performance. The best TFT exhibited good electrical performance, featuring a remarkably low subthreshold swing of 0.13 V/decade. It also exhibited fair stability against bending and gate bias stress.

Tribological Properties of Hard TiB2 Thin Films Prepared at Low Temperatures Using HiPIMS

Magnetron-sputtered WS2 composite thin films are solid lubricants with excellent performances. However, the low hardness of the WS2 thin films necessitates the further improvement of their wear resistance. For this purpose, an effective strategy is to alternately deposit or code posit WS2 and a hard phase, such as TiB2, to form hard lubricant thin films. Herein, a TiB2 thin film was prepared under the same conditions as those used for depositing the WS2 thin film with a dense structure and excellent tribological properties. Because of the high deposition energy of high-power impulse magnetron sputtering (HiPIMS), the TiB2 thin film possesses a dense structure and leather-like flat surface (hardness = 24.17 GPa). The friction coefficient of the film under different loads ranges between 0.6 and 0.8. The wear rate of the thin film increases with load, mainly because of fatigue wear and abrasive wear. Under high loads, obvious furrow-like wear marks are observed. At different sliding frequencies, except 8 Hz, the friction coefficient of the film ranges from 0.6 to 0.8. The main wear mode is fatigue wear, particularly at increasing sliding frequencies. Although the film possesses a relatively high friction coefficient, its wear resistance is excellent (minimum wear rate = 1.96 × 10−6 mm3/(N·m)).

Materials’ properties of low temperature deposited Cu/W and Cu/Cr multilayer thin films using high power impulse magnetron sputtering

In this study, copper/tungsten (Cu/W) and copper/chromium (Cu/Cr) multilayers were created by stacking bilayer films in a 3:1 ratio, with layer thicknesses ranging from 400 to 800 nm, deposited on Si (100) substrates using high power impulse magnetron sputtering (HiPIMS). The microstructural and surface properties of these films were examined through x-ray diffraction, atomic force microscopy, and scanning electron microscopy. Electrical properties were assessed using a four-point probe, while mechanical properties were measured via nanoindentation. Both multilayer systems showed a decrease in the hardness accompanied by an increase in the elastic modulus with each stacking bilayer. The Cu/W system experienced a gradual hardness reduction (down to 19%), compared to the Cu/Cr system, which exhibited a similar decrease (14.5%). The Cu/W and Cu/Cr multilayer film samples consistently demonstrate a softer nature compared to their bilayer counterparts due to the influence of the underlying Cu soft layers. A distinctive surface smoothness in these multilayer systems correlates with the elastic modulus in a manner unlike that with hardness. These multilayer films also demonstrated altered electrical resistivity, enhancing our understanding and capabilities in fabricating films with an increased number of layers.

Deposition of Fe2O3:Sn semiconducting thin films by reactive pulsed HiPIMS + ECWR co-sputtering from Fe and Sn targets

Semiconducting Fe2O3 thin films were deposited on SnO2:F (FTO) and Pt substrates by reactive high-power impulse magnetron sputtering combined with electron cyclotron wave resonance plasma (HiPIMS + ECWR). Fe2O3 films were fabricated either by sputtering from a single Fe target or by co-sputtering from an additional Sn target. Plasma parameters during co-sputtering were measured by an RF probe system enabling the comparison between HiPIMS + ECWR and only HiPIMS conditions used for the film deposition. As deposited Fe2O3 films were post-annealed in air at 450 °C and 650 °C, respectively. It was shown that as deposited Fe2O3 films were amorphous but became crystalline after post-annealing at 450 °C. Further increase of annealing temperature to 650 °C did not improve significantly the crystalline structure of the Fe2O3 film. All post-annealed Fe2O3 films exhibited photocurrents in the anodic region; generally, hematite films annealed at 650 °C exhibited higher photocurrents than those annealed at 450 °C. Films doped by Sn co-sputtering had higher photocurrents than films only doped by Sn diffusion during post-annealing from the FTO substrate. Hematite films on Pt substrate doped by Sn co-sputtering and post-annealed at 650 °C exhibited the highest photocurrents. It was verified by XPS analysis with ion sputtering depth profiling that Pt atoms also diffuse from the Pt substrate into the Fe2O3 film during the post-annealing at 650 °C and can, similar to Sn in the case of an FTO substrate, act as a dopant.

Anisotropic dielectric dispersions and thermal behaviors in highly textured BN thin films for heat self-dissipating electronics

Mainstream high-k gate materials, such as SiO2, Al2O3, and HfZrO2, are in demand for modern electronics. However, these dielectrics possess lower thermal conductivity, significantly limiting thermal dissipation in electronic devices. Herein, we propose the utilization of complementary metal-oxide semiconductor- (CMOS) compatible high power impulse magnetron sputtering (HiPIMS) for the mass production of highly textured hexagonal boron nitride (h-BN) on (100)-, (110)-, and (111)-oriented SrTiO3 substrates. The as-prepared films exhibit distinct vertical alignments, as evidenced by HRTEM and FTIR analysis. Notably, the R value, ranging from 0.46 to 0.50, is associated with the stress in the film. Importantly, distinct anisotropies in thermal conductivity, dielectric constant, and optical band gap are observed. Furthermore, the values of thermal conductivity in these highly textured h-BN films are 4.5, 5.7, and 5.3 Wm−1K−1, which is almost three times larger than those of SiO2 (1.4 Wm−1K−1) and Al2O3 (1.35 Wm−1K−1), and even an order of magnitude larger than that of HfZrO2 (0.67 Wm−1K−1). The combination of excellent dielectric characteristics, favorable thermal conductivity, and superior stability over a broad temperature range makes this novel material outperform conventional dielectric gate materials in high-power electronics applications.

Fabrication of (TiZrNbSiMo)1-xNx high entropy alloy coatings using a high power impulse magnetron sputtering technique: Effects of nitrogen addition

Due to the outstanding mechanical and physical properties of high entropy alloy (HEA) coatings, the global academic and industrial communities have made significant research efforts in recent years, aiming to expand their industrial applications. In this study, TiZrNbSiMo and (TiZrNbSiMo)1-xNx HEA nitride coatings with different nitrogen contents were fabricated using a high power impulse magnetron sputtering (HiPIMS) system. By varying the nitrogen flow rates, the nitrogen contents of coatings increased from 0 to 48.8 at. %. The deposition rate decreased with increasing nitrogen content due to the target poisoning effect. Very fine and dense microstructure can be seen for each coating. The amorphous structure was obtained as the nitrogen content was lower than 19.1 at.%, whereas a nanocrystalline FCC structure was formed when the nitrogen content reached 34.9 at. %. Furthermore, the corrosion resistance of TiZrNbSiMo and four TiZrNbSiMoN HEA coatings in 0.5 M H2SO4 aqueous solution were superior to uncoated 304 stainless steel. We can conclude that the nanocrystalline TiZrNbSiMoN HEA coatings with a nitrogen content of 34.9 at. % exhibited a high hardness of 15.6 GPa, an electrical resistivity of 766.5 μΩ·cm, and an excellent corrosion polarization resistance of 9.71 × 105 Ω·cm2, 610.7 times higher than 304SS. This study provides valuable insights for future promising applications of (TiZrNbSiMo)1-xNx HEA nitride coatings in severely corrosive environments, such as the protective coatings on stainless steel bipolar plates in proton exchange membrane fuel cells.

Effect of magnetron sputtering C-doped CrN film on the conductivity and corrosion resistance of 304 stainless steel bipolar plates

Using a high-power impulse and direct current (DC) magnetron sputtering approach, C-doped CrN films with various C-target pulse frequencies are created on the surface of SS 304. The microstructure, corrosion resistance and conductivity of the films are examined. With the decreases of C-target pulse frequency, the roughness of the CrCN films decreases and the density increases. The results of XPS and TEM analyses demonstrate that C atoms are either present in CrN lattice as interstitial atoms or precipitate at grain boundaries to form amorphous carbon, which facilitates the increase of film density and conductivity. In the potentiodynamic tests, the CrCN-1000 Hz film exhibits the lowest corrosion current density 0.54 μA/cm2 at 0.6 V vs. Ag/AgCl potential. The values of icorr and Ecorr are 0.11 μA/cm2 and 0.427 V, respectively. Furthermore, the CrCN-1000 Hz film has the lowest interface contact resistance (ICR) under a compaction force of 140 N/cm2 after potentiostatic polarization test, indicating that C doping is beneficial to improve the corrosion resistance and conductivity of CrN film.

Increasing the wear resistance of hip prostheses components using micro-nanostructured thin layers

Evaluation of micro-nanostructured thin layers applicability for increasing the lifetime of rehabilitation systems, mainly hip prostheses, is the aim of the present research. This because, the final objective of the complete project is to improve the quality of human prostheses using micro-nanostructured thin layers. In order to realize these researches, 0.5, 1, and 1.5 µm thick thin layers of TiN and TiO2, were deposited on substrates made of materials currently used for hip prostheses – M30NW steel and CoCr – using physical deposition methods, respectively Cathodic Arc (CA), Direct Current (DC) sputtering and High-Power Impulse Magnetron Sputtering (HiPIMS). After tribological and nanoindentation tests, the 1.5 μm thick TiN and TiO2 thin layers deposited on the steel and CoCr substrates using the DC sputtering method presented superior mechanical properties. Functional characterization of a total hip prosthesis, that have had components coated with these thin layers presented an increased resistance to fatigue wear. After comparative analysis, the main conclusion of the realized researches was that TiN layers with a thickness of 1.5 μm have an increased resistance to fatigue wear in comparison with TiO2 layers, when both are deposited by DC sputtering on M30NW steel and CoCr substrates. It was observed that 1.5 μm thick TiN layers ensures a prolongation by 15% of the lifetime of femoral heads compared to those uncoated.

Evaluation of chromium coatings deposited by standard and bipolar high-power impulse magnetron sputtering (HiPIMS & B-HiPIMS) for nuclear power applications

Chromium coatings, as deposited onto Zircaloy-4 through direct current magnetron sputtering (DCMS) and high-power impulse magnetron sputtering (HiPIMS), are evaluated for usage in advanced nuclear fuel applications. While traditional magnetron sputtering has been documented extensively in literature, HiPIMS remains relatively novel and unexplored within this application space, especially when the sputtering source voltage waveform is modified with the addition of a positive “kick pulse”, as in the case of bipolar HiPIMS (B-HiPIMS). Rigorous analysis of the microstructure and residual stress state of these coatings are correlated to electrochemical observations and 84-day, 360 °C autoclave weights gains to predict the performance of the films within a non-irradiated pressurized water reactor (PWR) environment. Under this scrutiny, differences and similarities are revealed between DCMS, HiPIMS, and B-HiPIMS. It is demonstrated that monolithic Cr coatings deposited by HiPIMS and B-HiPIMS outperform those deposited by DCMS, while exhibiting an order of magnitude reduction in autoclave weight gain relative to the Zircaloy-4 nuclear grade material.