Control of morphology (ZrN crystallite size and SiNx layer thickness) in Zr-Si-N nanocomposite thin films

DC reactive magnetron sputtering was used for the deposition of Zr-Si-N thin films. Four series of samples have been deposited at various substrate temperatures T_S: 300 K, 510 K, 710 K and 910 K. Depending on T_S, different N₂ partial pressures p_N2 were required to obtain nearly stoichiometric ZrN films. Si content (C_Si) was varied in each series by changing the power applied on the Si target, whereas the power on the Zr target was kept constant. The microstructure of the coatings was examined by XRD and in cross-section by transmission electron microscopy (TEM). Depending on T_S and p_N2, the deposition rate showed significant variations from 0.04 to 0.18 nm/s. The correlation between film morphology (preferential orientation of crystallites, grain size, column dimensions, thickness of the SiN_x layer covering ZrN crystallites) and the deposition conditions (power applied on Si target, temperature, nitrogen partial pressure and deposition rate) provides useful information for optimizing the deposition process.     

Formation of composite ternary nitride thin films by magnetron sputtering co-deposition

Thin films of M-X-N (M stands for early transition metal and X = Si, Ge, Sn) are studied as protective coatings. To extend the knowledge about the formation of nanocomposite films, various M-X-N systems have been compared. Ti-Si-N, Ti-Ge-N, Ti-Sn-N, Nb-Si-N, Zr-Si-N and Cr-Si-N thin films were deposited by reactive magnetron sputtering, from confocal targets in a mixed Ar/N₂ atmosphere. The chemical reactivity of germanium and tin with nitrogen is significantly lower than that of Si and Ti. Therefore, the Ti-Ge-N and Ti-Sn-N systems are different from Ti-Si-N. Important changes in the morphology and structure of M-X-N films are induced by X addition. Nanocrystalline composite films are formed in all these investigated ternary systems.As a function of increasing X content (C_X), the size of the crystallites D in the Ti-Si-N, Ti-Ge-N, Nb-Si-N and Zr-Si-N films decreases (from tens of nm to 2 nm) following the relationship C_X ∼ 1 / D. The segregation of X atoms on the MN crystallite surface is responsible for the limitation of their growth. It results in the formation of a SiN_y or TiGe_y amorphous phase on the crystallite surfaces. In the case of Nb-Si-N and Zr-Si-N systems, Si atoms can substitute metal atoms in the cubic MN lattice up to a critical concentration (solubility limit). Ti-Si-N, Ti-Ge-N and Ti-Sn-N systems are different: no solubility of Si, Ge and Sn in the TiN lattice is observed. For every composite film, the morphology changes result in a maximum hardness value at a typical concentration 2 ≤ C_X ≤ 12 at.%. Resistivity measurements provide experimental mean for determining the limit of Si solubility in M-Si-N ternary systems and for following the thickness evolution of the SiN_y coverage layer in the composite films.     

磁控溅射偏压对Zr-Si-N扩散阻挡层组织结构的影响

用反应磁控溅射法在不同偏压下沉积了Zr-Si-N扩散阻挡层.结果表明:Zr-Si-N膜的成分、电阻率和结构均随偏压的改变而不同;随着溅射偏压的增加,Zr-Si-N膜的表面粗糙度值增大;Zr/Si比值也随着偏压的增加而增大;电阻率随偏压的增加显著降低;Zr-Si-N膜的结构为类似Si3N4的氮硅化物非晶相与ZrN组成的复合结构,随着偏压的升高ZrN由非晶转变为纳米晶,而且ZrN晶体相增加.     

不同氮分压制备纳米复合Zr-Si-N薄膜的组织与性能研究

利用射频反应磁控溅射设备在不同N2分压下制备了Zr-Si-N 纳米复合薄膜.研究了N2分压对薄膜组织和性能的影响.结果表明:随着N2分压的增加,薄膜中Zr、Si元素含量比降低,且薄膜方电阻增加;Zr-Si-N薄膜的微观组织由纳米晶ZrN嵌入SiNx非晶基体构成,在低N2分压条件下,有少量Zr2Si 形成.Zr2Si 的形成与低N反应活性相关.在0.03 Pa N2分压条件下,Zr-Si-N薄膜硬度达到22.5 GPa的最大值.高N2分压制备薄膜硬度较低可能与Si原子造成的晶格畸变相关.     

Oxidation resistance and mechanical property of cosputtered quasi-amorphous Ta-Si-N films under vacuum rapid thermal annealing

The oxidation resistance and mechanical properties of Ta-Si-N films at high temperature are important issues for application. In this paper, quasi-amorphous Ta-Si-N thin films were fabricated by using reactive magnetron co-sputtering at different Si/Ta power ratios and nitrogen flow ratios (FN₂% = FN₂/(FAr + FN₂) × 100%). Vacuum rapid thermal annealing at 600-900 °C at 2.6 Pa was performed to investigate the oxidation resistance of films. At the higher Si/Ta power ratio and increased FN₂%, there is low oxygen fraction (O/(O + N) ≤ 0.2) of films at high annealing temperature which corresponds to benefit oxidation resistance. The crystalline δ-Ta₂O₅ phase was formed at 900 °C for all films. The islands of oxide were formed on the surface of films at low-Si-content (≤ 20 at.%) after 900 °C annealing. The hardness of all as-deposited Ta-Si-N films was between 16 and 24 GPa. The low-Si-content Ta-Si-N films has higher hardness than high-Si-content (≥ 20 at.%) ones due to lower fraction of soft amorphous SiN_x. The effect of annealing temperature on the correlation among process parameters, microstructure, phase transformation and hardness is discussed. The Ta-Si-N formed at 6 FN₂% and Si/Ta power ratio of 2/1 can be the best candidate for good oxidation resistance with appropriate mechanical property.     

Heat treatment induced phase separation and phase transformation of ZrNxOy thin films deposited by ion plating

Nanocrystalline ZrN_xO_y thin films were deposited on p-type Si (100) substrates using hollow cathode discharge ion-plating (HCD-IP) and the films were annealed at 700 and 900 °C in the controlled atmosphere. The purpose of this study was to investigate the phase separation, phase transformation and the accompanying change of properties of the heat-treated ZrN_xO_y films deposited by ion plating. With the increase of oxygen flow rate ranging from 0 to 10 sccm, the primary phase of the as-deposited films evolved from ZrN to nearly amorphous structure and further to monoclinic ZrO₂ (m-ZrO₂). After heat treatment at 700 and 900 °C, phase transformation occurred in the samples deposited at 8 and 10 sccm O₂, where a stoichiometric crystalline Zr₂ON₂ was found to derive from m-ZrO₂ with dissolving nitrogen (m-ZrO₂(N)). The hardness of the ZrN_xO_y thin films could be correlated to the fraction of Zr₂ON₂ + m-ZrO₂. The film hardness decreased significantly as the fraction of ZrO₂ + Zr₂ON₂ exceeded ~ 60%, which was due to phase transition by increasing oxygen flow rate or phase transformation induced by heat treatment. The phase separation of m-ZrO₂ from ZrN with dissolving oxygen (ZrN(O)) may relieve the residual stress of the ZrN_xO_y specimens deposited at 5 and 8 sccm O₂, while direct formation of m-ZrO₂ increased the stress of the film deposited at 10 sccm O₂. On the other hand, the phase transformation from m-ZrO₂(N) to Zr₂ON₂ by heat treatment at both 700 and 900 °C may effectively relieve the residual stress of the ZrN_xO_y films.     

Phase transition and mechanical properties of ZrNxOy thin films on AISI 304 stainless steel

ZrN_xO_y thin films were deposited on AISI 304 stainless steel (304SS) substrates by reactive magnetron sputtering. The specimens were produced by sputtering a Zr target at 500 °C and the reactive gasses were N₂ and O₂ at various flow rates (ranging from 0 to 2 sccm). The purpose of this study was to investigate the effect of oxygen flow rate on the phase transition and accompanying mechanical properties of the ZrN_xO_y thin films. The oxygen contents of the thin films increased significantly with increasing oxygen flow rate. X-ray diffraction (XRD) revealed that the characteristics of the films can be divided into three zones according to the major phase with increasing oxygen content: Zone I (ZrN), Zone II (Zr₂ON₂) and Zone III (m-ZrO₂). The hardness of the ZrN_xO_y films decreased with increasing oxygen content due to the formation of the soft oxide phase. Modified XRD sin²ψ method was used to respectively measure the residual stresses of ZrN, Zr₂ON₂ and m-ZrO₂ phases. The results showed that the residual stress in ZrN was relieved as the oxygen content increased, and Zr₂ON₂ and m-ZrO₂ were the phases with lower residual stress. Compositional depth profiles indicated that there was a ZrO₂ interlayer near the film/substrates interface for all samples except the mononitride ZrN specimen. Contact angle was used as an index to assess the wettability of the film on substrate. The contact angles of ZrN, Zr₂ON₂ and m-ZrO₂ on stainless steel were indirectly measured using Owens-Wendt method. The results showed that ZrO₂ possessed the lowest wettability on 304SS among the three ZrN_xO_y phases, indicating that the ZrO₂ interlayer may account for the spallation of the ZrN_xO_y films after salt spray tests.     

Mechanical properties and corrosion resistance of nanocrystalline ZrNxOy coatings on AISI 304 stainless steel by ion plating

Transition metal oxynitrides have become emerging decorative coating materials due to their adjustable coloration and high hardness and corrosion resistance. This research studied the effect of oxygen content on the coloration, mechanical properties and corrosion resistance of ZrN_xO_y thin films deposited on AISI 304 stainless steel using hollow cathode discharge ion plating (HCD-IP). The Zr/N/O ratios of the ZrN_xO_y films were determined using X-ray photoelectron spectroscopy (XPS). The color of the ZrN_xO_y thin film changed from golden yellow to blue and then slate blue with increasing oxygen content. X-ray diffraction (XRD) patterns revealed that phase separation of ZrN and m-ZrO₂ occurred as the oxygen content reached 31.2 at.%. ZrN(O) (ZrN with dissolving oxygen) is dominant at oxygen content less than 18.1 at.%, while m-ZrO₂ phase was prevailed at oxygen content above 40.3 at.%. Phase separation lowered the hardness of the ZrN_xO_y films as the fraction of ZrO₂ was less than 40%. The residual stresses in ZrN phase was higher than that in ZrO₂, and the residual stress decreased for the specimen containing 30 to 37% ZrO₂. For the samples containing more than 44% ZrO₂, the average residual stress was close to that in ZrO₂ phase. The corrosion resistance was evaluated by salt spray test and potentiodynamic scan in two solutions: 0.5MH₂SO₄ + 0.05 M KSCN and 5% NaCl solutions. The results showed consistent trend in the two solutions. From the results of potentiodynamic scan, corrosion resistance increased as the packing density of the film increased, whereas the film thickness was not a crucial factor on corrosion current; moreover, the electrical conductivity of the film may be one of the significant factors in corrosion resistance. Results of salt spray tests suggested that the corrosion of ZrN_xO_y in NaCl may play an important role in corrosion resistance.     

Lanthanum silicate thin films for SOFC electrolytes synthesized by magnetron sputtering and subsequent annealing

Thin films of La and Si with Si/(La + Si) atomic ratios ranging from 0.36 to 0.44 were produced by magnetron sputtering in pure Ar. For all compositions, the apatite-like La_9.33Si₆O₂₆ phase was formed during annealing in air at 900 °C. A preferential orientation was developed during annealing of the films with higher silicon content while formation of oxide impurities was detected for the films with less silicon. Silicon segregation to the thin film/substrate interface was observed after annealing for thin films with higher Si/(La + Si) atomic ratios. The higher ionic conductivity values were obtained with the films with lower silicon content (2.81 × 10^− 3 Scm^− 1 at 800 °C for the film with Si/(La + Si) atomic ratio of 0.36). This film presented the lower activation energy E_a (0.94 eV).     

X-ray photoelectron spectroscopy analysis of zirconium nitride-like films prepared on Si(100) substrates by ion beam assisted deposition

Thin zirconium nitride films were prepared on Si(100) substrates at room temperature by ion beam assisted deposition with a 2 keV nitrogen ion beam. Arrival rate ratios ARR(N/Zr) used were 0.19, 0.39, 0.92, and 1.86. The chemical composition and bonding structure of the films were analyzed with X-ray photoelectron spectroscopy (XPS). Deconvolution results for Zr 3d, Zr 3p_3/2, N 1s, O 1s, and C 1s XPS spectra indicated self-consistently the presence of metal Zr⁰, nitride ZrN, oxide ZrO₂, oxynitride Zr₂N₂O, and carbide ZrC phases, and the amounts of these compounds were influenced by ARR(N/Zr). The chemical composition ratio N/Zr in the film increased with increasing ARR(N/Zr) until ARR(N/Zr) reached 0.92, reflecting the high reactivity of nitrogen in the ion beam, and stayed almost constant for ARR(N/Zr) ≥ 1, the excess nitrogen being rejected from the growing film. A considerable incorporation of contaminant oxygen and carbon into the depositing film was attributed to the getter effect of zirconium.     

Internal structure of clusters of partially coherent nanocrystallites in Cr-Al-N and Cr-Al-Si-N coatings

Nano-sized clusters consisting of strongly preferentially oriented, partially coherent nanocrystallites were observed in Cr-Al-N and Cr-Al-Si-N coatings deposited using cathodic arc evaporation. Microstructure analysis of the coatings, which was done using the combination of X-ray diffraction (XRD) and transmission electron microscopy with high resolution (HRTEM), revealed furthermore stress-free lattice parameters, size and local disorientation of crystallites within the nano-sized clusters in dependence on the aluminium and silicon contents, mean size of these clusters and the kind of structure defects. Within the face-centred cubic (fcc) Cr_{1 − x − y}Al_xSi_yN phase, the stress-free lattice parameter was described by the equation a = (0.41486 − 0.00827 · x + 0.034 · y) nm. The size of individual crystallites decreased from ∼ 11 nm in Cr_0.92Al_0.08N to ∼ 4 nm in Cr_0.24Al_0.65Si_0.10N. These nanocrystallites formed clusters with the mean size between 36 and 56 nm. The mutual disorientation of the partially coherent nanocrystallites forming the clusters increased with increasing aluminium and silicon contents from 0.5° to several degrees. The disorientation of neighbouring nanocrystallites was explained by the presence of screw dislocations and by presence of phase interfaces in coatings containing a single fcc phase and several phases, respectively.     

Characterisation of R.F. magnetron sputtered Cr-N,Cr-Zr-N and Zr-N coatings

Binary Cr-N, Zr-N and Cr-Zr-N films were synthesised using a R.F. reactive magnetron sputtering technique by co-sputtering Cr and Zr. The crystalline structure, morphology, mechanical and tribological properties of the films as a function of Zr content were characterised by X-ray diffraction, microanalysis X (WDS, EDS), X-ray photoelectron spectroscopy, scanning electron microscopy, atomic force microscopy, nanoindentation, scratch adhesion and pin-on-disc sliding wear tests. The residual stress was calculated with the Stoney formula. The Cr-Zr-N films exhibit a two-phase microstructure, containing a cubic (CrN, ZrN) with hexagonal (Cr₂N, Zr₂N) phases, as shown by X-ray diffraction. As the Zr content increased, a columnar and compact structure is developed with a low surface roughness. The results reveal that the mechanical and tribological properties of the films were found to depend on the Zr content and the hardness (maximum 26.3?GPa) is greatly improved in comparison with CrN and ZrN films, especially at 31?at.-% Zr. In the scratch test, the hardest film (Cr_0.18Zr_0.31N_0.47) exhibited an adhesive failure at Lc_2?=?34.3?N.     

Nanomechanical and electrochemical properties of ZrN coated NiTi shape memory alloy

Zirconium nitride (ZrN) thin films were deposited on NiTi and Si substrates in the 23–570 °C temperature range by direct current reactive magnetron sputtering using N₂/Ar gas mixture. The film hardness, corrosion behavior, phase composition, and texture were determined. The deposited films were composed mainly by the cubic ZrN phase, whose texture varies with substrate temperature, changing progressively from (111) to (200) texture as the temperature increases. The hardness of the films is influenced by the texture and has a linear relationship with the ratio of the texture coefficients P(111)/P(200). The higher hardness is obtained for ZrN thin films with (200) texture. Electrochemical tests show that NiTi coated with (200)-oriented ZrN films has higher tendency to passivation and greater stability of the passive film as compared to (111)-oriented ZrN films, despite no abrupt changes was observed when the texture changes from (111) to (200).     

Effect of nitrogen content in amorphous SiCxNyOz thin films deposited by low temperature reactive magnetron co-sputtering technique

Amorphous silicon oxycarbonitride (SiC_xN_yO_z) films have been deposited on Si substrates by low temperature reactive magnetron co-sputtering of silicon and graphite targets in mixed Ar/N₂ atmosphere. Our studies are focused on the influence of nitrogen incorporation on deposition rate, film composition, film structure, chemical bonds, and electrical resistivity of SiC_xN_yO_z films investigated by profilometry, Rutherford Backscattering Spectrometry (RBS), X-ray diffraction (XRD), Raman spectroscopy, X-ray Photoelectron Spectroscopy (XPS), and four-point probe method. RBS results show that all samples contain significant amounts of oxygen (up to 16 at.%) which led to the formation of SiC_xN_yO_z. Further, XPS results show that most of this oxygen is located in the film surface. With the addition of N₂ gas in the plasma, the carbon, and nitrogen contents in the films increase. The increased carbon content is due to the contribution of chemically driven sputtering of the graphite target and the reduction of the sputtering rate of the silicon target owing to poisoning by nitrogen. Raman spectra suggest that the films contain amorphous phases and that the a-C clusters suffer a graphitization with increased N₂ gas flow rate. The XRD analysis confirmed the amorphous structure of these films. According to the XPS analysis, the increase in nitrogen content leads to an increase in SiN and CN bonds, decreasing the SiC, SiSi, and CC bonds. Finally, the films electrical resistivity depends mainly on the nitrogen content, which makes it possible to obtain semiconductor or insulator SiC_xN_yO_z films only by adjusting the N₂ concentration in the gas phase during the deposition process.     

Si-doped multifunctional bioactive nanostructured films

Si-doped multifunctional bioactive nanostructured films (MuBiNaFs) were deposited by DC magnetron sputtering of composite TiC_0.5 + CaO + Si (A) and TiC_0.5 + CaO + Si₃N₄ (B) targets produced by self-propagating high-temperature synthesis method. The films were characterized in terms of their structure, elemental and phase composition using X-ray diffraction, scanning and transmission electron microscopy, electron energy loss spectroscopy, glow discharge optical emission spectroscopy, Raman, and IR spectroscopy. The Ti-Si-Ca-P-C-O-(N) films consisted of TiC(N) as a main phase with a minor amount of TiO_x, SiN_x, SiO_x, SiC, and CaO phases probably mainly in amorphous state at the grain boundaries and COO- groups on the film surface. The excess of carbon atoms in the Ti-Si-Ca-P-C-O-N film (target A) precipitated in a DLC form. The films showed hardness in the range of 26-31 GPa, reduced Young's modulus of 200-270 GPa, and high percentage of elastic recovery of 60-71%. The best Ti-Si-Ca-C-O-N films exhibited low friction coefficient both in physiological solution and Dulbecko modified Eagle medium with fetal calf serum, hydrophilic properties, improved electrochemical characteristics, and excellent impact resistance. Nevertheless, the wear resistance of the Ti-Si-Ca-C-O-N films against Al₂O₃ ball was lower compared with the best Si-free MuBiNaFs. In vitro studies showed that the Si-doped Ti-Ca-C-O-N films possess improved osteoconductive characteristics during early stage of cell/material interaction. The film surface was highly adhesive for IAR-2 epithelial and MC3T3-E1 osteoblastic cells. The films revealed a high level of biocompatibility and biostability in experiments in vivo. The Ti-Si-Ca-C-O-N film (target A) did not show any bactericidal activity during cultivation of bacterial strains both on solid and in liquid Luria Bertani mediums. The film did not reveal any bactericidal and toxic activity against macrophages and therefore did not change bacterial status and defence system of macro-organisms.     

Structure and mechanical properties of TiAlSiN/Si3N4 multilayer coatings

TiAlSiN/Si₃N₄ multilayer coatings which have different separate layer thicknesses of TiAlSiN or Si₃N₄ were deposited onto glass sheets, single-crystal silicon wafers and polished WC-Co substrates by reactive magnetron co-sputtering. The morphology, crystalline structure and thickness of the as-prepared multilayer coatings were characterized by TEM, SEM, XRD and film thickness measuring instrument. The mechanical properties of the coatings were evaluated by a nanoindenter. The effects of monolayer thickness on the microstructure and properties of TiAlSiN/Si₃N₄ multilayer coatings were explored. The coatings showed the highest hardness when the thickness of Si₃N₄ and TiAlSiN monolayers was 0.33 nm and 5.8 nm, respectively. The oxidation characteristics of the coatings were studied at temperatures ranging from 700 °C to 900 °C for oxidation time up to 20 h in air. It was found that the coatings displayed good oxidation resistance.     

Microstructure and tribological properties of CrN and CrSiCN coatings

Three CrN based coatings were deposited on 17-4PH precipitation hardening stainless steel substrate using plasma enhanced magnetron sputtering (PEMS) technique. The three coatings evaluated in this study assumed the nominal compositions of Cr_0.68N_0.32 (sample CrN), Cr_0.55Si_0.013C_0.14N_0.3 (sample CrSiCN-1), and Cr_0.43Si_0.034C_0.25N_0.29 (Sample CrSiCN-2)_. The microstructure, mechanical properties and wear and erosion resistance of the coatings were evaluated to examine the effect of Si and C additions to CrN. The results indicated that with the incorporation of Si and C, the microstructure transformed from hexagonal Cr₂N (for CrN coating) to B1 structure containing crystalline Si₃N₄ (for CrSiCN-2). The initial addition of Si (1.3 at.%) and C resulted in increase of hardness (H), Young's modulus (E) and the ratio of H³/E². With further increase in Si (3.4 at.%) and C, the hardness and Young's modulus decreased. The coefficient of friction was observed to decrease with the addition of Si and C, irrespective of microstructure changes. The combination of reduced coefficient of friction and microstructure modifications has resulted in improved wear resistance for sample CrSiCN-2 (with a wear rate ∼ 60% lower than CrN). The erosion resistance test results showed brittle erosion characteristics for samples CrN and CrSiCN-1 where erosion rate increased with erodent impingement angle and reached the highest rate at 75° and 90°, respectively. CrSiCN-2 coating, while exhibiting higher erosion rate at low impingement angle, demonstrated reduced erosion rate at higher angle due to the ductile nature of the coating under erosion test condition.     

Preparation and electrochemical performance of copper foam-supported amorphous silicon thin films for rechargeable lithium-ion batteries

Amorphous Si thin films, which have been deposited on copper foam by radio-frequency (rf) magnetron sputtering, are employed as anode materials of rechargeable lithium-ion batteries. The morphologies and structures of the as-prepared Si thin films are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray powder diffraction (XRD). Electrochemical performance of lithium-ion batteries with the as-prepared Si films as the anode materials is investigated by cyclic voltammetry and charge-discharge measurements. The results show that the electrode properties of the prepared amorphous Si films are greatly affected by the deposition temperature. The film electrode deposited at an optimum temperature of 300 °C can deliver a specific capacity of ∼2900 mAh/g and a coulombic efficiency above 95% at charge/discharge current density of 0.2C after 30 cycles. The Li⁺ diffusion coefficiency in copper foam-supported Si thin films is determined to be 2.36 × 10⁻⁹ cm²/s.     

Investigation of metal distribution and carbide crystallite formation in metal-doped carbon films (a-C:Me, Me = Ti, V, Zr, W) with low metal content

Metal-doped amorphous carbon films (a-C:Me) were deposited at room temperature by magnetron sputtering using a metal (Me = Ti, V, Zr, W) and a graphite target. The metal distribution and the temperature-induced carbide crystallite formation were analyzed by X-ray diffraction (XRD), electron microscopy (TEM, STEM) and X-ray absorption spectroscopy (EXAFS, XANES), focusing on low metal concentrations between 6.5 and 9.5%. In as-deposited samples, the metal atoms are atomically distributed in the carbon matrix without significant formation of carbide particles. With annealing to 900 K the local atomic environment around the metal atoms becomes similar to the carbide. The carbide crystallites grow with annealing up to 1300 K, their size is dependent on the metal type: V > Ti > Zr≈W. W₂C and WC_1 − x crystallites were identified for W-doped films, whereas the monocarbides are formed for the other metals. It is demonstrated, that EXAFS and high resolution electron microscopy are required to get a correct picture of the structure of the analyzed a-C:W films.     

Cathodic arc plasma deposition of nano-multilayered ZrN/AlSiN thin films

Thin films of ZrN/AlSiN were deposited on SKD 11 tool steel substrate using Zr and AlSi cathodes in an Ar/N₂ gas mixture in a cathodic arc plasma deposition system. The influence of the AlSi cathode arc current and the substrate bias voltage on the mechanical and structural properties of the films was investigated. X-ray diffraction, electron probe micro-analysis, high resolution transmission electron microscopy, nanoindentation and profilometry were used to characterize the films. The ZrN/AlSiN thin films had a multilayered structure by rotating the substrate in which nano-crystalline ZrN layers alternated with amorphous AlSiN layers. The hardness of the films increased as the AlSi cathode arc current was raised from 35 to 40 A, and then decreased with a further increase of the current. The hardness of the films increased with the increase of the bias voltage from − 50 to − 100 V. Further increase in the bias voltage decreased the hardness. The films exhibited a maximum hardness of 38 GPa. With the increase of bias voltage, the residual stress of the films correlated well with the hardness.