Zirconium Nitride Thin Films Research Articles

Innovative process to obtain thin films and micro-nanostructured ZrN films from a photo-structurable ZrO2 sol-gel using rapid thermal nitridation

Zirconium nitride (ZrN) is widely used in many industrial sectors for its outstanding performances including its mechanical properties, high chemical and thermal stability. Associated with its plasmonic behavior, these properties make ZrN a suitable candidate for optical applications at high temperature or in extreme environments. The authors present an innovative, easy-to-use and rapid process for producing ZrN thin films from a photo-structurable ZrO2 sol-gel using a rapid thermal nitridation (RTN) process. In this process, a ZrO2 sol-gel layer is converted into a ZrN thin film in a few minutes by rapid thermal annealing (RTA) under ammonia gas. Compared to physical or chemical vapor deposition, usually used to produce ZrN thin films, the advantages of the sol-gel method include suitability for non-planar and large substrates and the possibility of nanotexturing of crystallized ZrN surfaces in considerably less time, at a larger scale and at a lower cost. The ZrO2 and ZrN thin films were characterized by Raman spectroscopy, X-ray diffraction and Transmission Electron Microscopy, to confirm complete nitridation. The optical, electrical and tribological properties were also investigated. Finally, the nitridation method was also used on structured ZrO2 layers and showed the versatility of the process e.g. enabling the production of micro-nanostructured ZrN films without using any etching techniques.

Reusability, Long‐Life Storage and Highly Sensitive Zirconium Nitride (ZrN) Surface‐Enhanced Raman Spectroscopy (SERS) Substrate Fabricated by Reactive Gas‐Timing Rf Magnetron Sputtering

AbstractTransition metal nitrides (TMN) are promising material alternative to replace noble metals in the field of plasmonic applications, especially surface‐enhanced Raman spectroscopy (SERS). Here we demonstrate a practical surface enhanced Raman spectroscopy (SERS) substrate using zirconium nitride (ZrN) thin films grown by reactive gas‐timing (RGT) rf magnetron sputtering. The tailored properties of ZrN thin film exploited for SERS activity could be achieved to obtain a highly sensitive ZrN thin film SERS substrate with the enhancement factor (EF) of 1.24 × 106 and 4.8 %RSD at 1626 cm‐1 toward methylene blue (MB) analyte which are comparable to the optimized Au sputtered thin films (EF=1.18 × 106 and with 5.1%RSD). We find that the spatial plasmonic hotspots on the surface of ZrN SERS substrate controlled by the turn‐on timing of Ar:N2 sputtered gas sequence, leading to the discrete conductive surface profile, strongly relates to non‐stoichiometric composition and the degree of (200)‐oriented texture at the surface of ZrN thin film. Furthermore, ZrN thin film SERS substrates exhibit an excellent recyclability more than 30 cycles with simple cleaning process and a storage time longer than 6 months. The detection and reusability of ZrN SERS substrate on the low concentration of trinitrotoluene (TNT) for homeland security are also performed.

Optimization of Electron-Beam Evaporation Process Parameters for ZrN Thin Films by Plasma Treatment and Taguchi Method

This study presents the optimal process parameters of zirconium nitride (ZrN) thin films prepared by ion-assisted deposition (IAD) technology combined with electron-beam evaporation based on plasma surface treatment and the Taguchi method. We use Minitab statistical software (Version 20.2.0) and L9 orthogonal array parameter design combined with the response surface method (RSM). The quadratic polynomial regression equation was optimized by the RSM. Based on the control factor screening test of the Taguchi method, we determined the most critical factor combination for the process and derived the optimized process parameters of the ZrN thin films. In the coating experiments, we successfully achieved the optimal combination of good refractive index, adequate residual stress, and lower surface roughness on B270 glass substrates. These results indicate that the optimized preparation process can simultaneously achieve several desirable properties, improving the performance and application of ZrN thin films. Furthermore, our research method not only reduces the number of experiments and costs but also improves the efficiency of research and development. By screening key factors and optimizing process parameters, we can find the best process parameter more rapidly, reduce the demand for expenses given materials and equipment costs, and contribute to improving the electron-beam evaporation process. According to the experimental results, it can be observed that under certain conditions, the properties of ZrN thin films reached optimal values. These results are highly useful for optimizing the process parameters of ZrN thin films and provide a basis for further improvement of the thin film properties.

Influence of nitrogen environment on wettability and optical properties of sputtered zirconium nitride thin film

This article aims to examine how changing the nitrogen flow rate affects Zirconium coatings. By using RFmagnetron sputtering to deposit zirconium nitride (ZrN) on silicon wafers and glass while adjusting the nitrogen flow rate from 2 to 10 sccm, well-crystalline zirconium nitride films are produced. X-ray diffraction (XRD) and atomic force microscopy were used to investigate the structure and topography of the thin films, respectively. XRDanalysis revealed that the film's atomic structure corresponded to the orthorhombic phase of Zr3N4, with a peak in the (011) plane. Zr3N4 film's optical transmittance was studied from 300 nm to 2500 nm. The observed transmission value was around 65%. The deposited films' surface energy and contact angles were evaluated with the use of contact angle measuring instruments. Contact angles measured werebetween 95.1° and 104.9°. The deposited coatings become hydrophobic and have a contact angle of 90° or more when the flow rate of nitrogen is high.

An Accurate Quantitative X-ray Photoelectron Spectroscopy Study of Pure and Homogeneous ZrN Thin Films Deposited Using BPDMS

A quantitative X-ray Photoelectron Spectroscopy (XPS) study has been undertaken on different experimental data sets of ZrN thin films deposited using reactive Bipolar Pulsed Dual-Magnetron Sputtering (BPDMS) on silicon/stainless steel substates, to obtain dense, pure and homogeneous coatings, free from morphological defects. Zirconium nitride (ZrN) occupies a central role within the class of transition metal nitrides (TMN) for its excellent properties, such as high hardness, low resistivity and chemical/thermal stability when its stoichiometric ratio is 1:1. Many deposition techniques, reported in the literature, tried to obtain oxygen-free and defect-free structures, but they proved a hard task. In this paper it has been demonstrated, using quantitative XPS, that stoichiometric, pure and homogeneous ZrN films have been grown at certain deposition conditions, optimized also via optional accessories mounted on the deposition apparatus. Almost all the films considered for microanalytical characterization resulted as completely oxygen-free, pure (with a lowest-detection limit of 1%) and homogeneous. Apart from these features, a stoichiometric ratio (N/Zr) close to one was calculated for six samples of the ten investigated, with a precision of ± 0.01. In this frame XPS, widely known for being a highly surface-sensitive technique (average depth resolution of 20–30 Å), and powerful for characterizing the chemical composition of materials, has been extensively employed to extract information both in the surface regions and in depth. A cluster ion beam Ar+ 2500 facility on our main XPS chamber has not proved adequate for depth-profiling acquisitions. Therefore, Ar+ ion sputtering was performed instead. To the best of our best knowledge, the results achieved in the present paper possess a level of accuracy never reached before. Rigorous calibration procedures before and during experimental spectrum acquisitions and a careful and scrupulous data processing using software CasaXps v.2.3.24PR1 were carried out to ensure a low percentage error. Progress has also been made for shake-up satellite extraction and interpretation from Zr 3d high-resolution spectra with the help of the literature milestones reported in the text. The total absence of oxygen inside most of the films prevented the formation of zirconium oxide compounds during deposition, which are generally resonant with the binding energy of the shake-up satellite peaks and hide them. A little summary about the experimental shake-up satellite peaks revealed and extracted from the Zr 3d region, after Shirley background subtraction and data processing, will be presented in the last subparagraph of the “Results” section for the ZrN samples analyzed. Figures of Zr 3d deconvoluted spectra for in-depth area analysis have been reported. The quantitative satellite contribution to the Zr 3d total area would not be included in stoichiometric calculations.

Refractory Plasmonic Hafnium Nitride and Zirconium Nitride Thin Films as Alternatives to Silver for Solar Mirror Applications.

Harnessing solar energy by employing concentrated solar power (CSP) systems requires materials with high electrical conductivity and optical reflectivity. Silver, with its excellent optical reflectance, is traditionally used as a reflective layer in solar mirrors for CSP technologies. However, silver is soft and expensive, quickly tarnishes, and requires a protective layer of glass for practical applications. Moreover, supply-side constraints and high-temperature instability of silver have led to the search for alternative materials that exhibit high solar and infrared reflectance. Transition metal nitrides, such as titanium nitride, have emerged as alternative plasmonic materials to gold starting from a spectral range of ∼500 nm. However, to achieve high solar reflection (∼320-2500 nm), materials with epsilon-near-zero starting from the near-ultraviolet (UV) spectral region are required. Here, we show the development of refractory epitaxial hafnium nitride (HfN) and zirconium nitride (ZrN) thin films as excellent mirrors with a solar reflectivity of ∼90.3% and an infrared reflectivity of ∼95%. Low-loss and high-quality epsilon-near-zero resonance at near-UV (∼340-380 nm) spectral regions are achieved in HfN and ZrN by carefully controlling the stoichiometry, leading to a sharp increase in the reflection edge that is on par with silver. Temperature-dependent reflectivity and dielectric constants are further measured to demonstrate their high-temperature suitability. The development of refractory epitaxial HfN and ZrN thin films with high solar and infrared reflectance makes them excellent alternative plasmonic materials to silver and would pave their applications in CSP, daytime radiative cooling, and others.

The mechanism of phase transition induced by oxygen doping in zirconium nitride thin films

The mechanism of phase transition induced by oxygen doping in zirconium nitride thin films

MOCVD growth of ZrN thin films on GaN/Si templates and the effect of substrate temperature on growth mode, stress state, and electrical properties

Zirconium nitride (ZrN) is a candidate for contact metal and diffusion barrier in ohmic contacts for GaN-based devices due to its superior electrical conductivity and corrosion resistance. This paper reported ZrN films deposited on GaN/Si templates using metal-organic chemical vapor deposition (MOCVD) and analyzed the effect of substrate temperature (T s) on its growth mode, film stress, as well as electrical properties. Firstly, the surface morphology and film roughness of the resultant ZrN epilayers were investigated, which were found to vary dramatically with T s. Then, a temperature-dominated crystal formation process was reasonably proposed, revealing the transfer from the island to layer growth mode and the augmentation of the growth rate of ZrN with elevated T s. Stress information was obtained from the position of XRD diffraction peaks, indicating large in-plane lattice stretching in ZrN film and the presence of compressive stress in the GaN/Si template. The stress states can be related to island merger and thermal mismatch between ZrN and GaN, which proved satisfyingly advantageous in preventing the GaN layer from cracking during the subsequent preparation procedure. In addition, XPS surface and interface investigations were performed to identify the chemical state and the atomic content of the ZrN film, which also implied a relatively clear interface between the ZrN epilayer and GaN/Si template. Furthermore, Hall tests proved the resistivity of ZrN thin film can reach a minimum of 2.28 × 10−4 Ω cm, owing to the grain boundary chaining and flat film surface at high temperatures. Overall, it appears to have promising prospects for its application in the contact layer and diffusion barrier of ohmic contact in GaN-based devices.

Structural and corrosion resistance properties of sputtered zirconium nitride thin films as electrode material for supercapacitor

In this paper, the surface morphology, crystal structure and corrosion resistance of the magnetron sputtered zirconium nitride (ZrN) thin films were evaluated and investigated. The results show that the surface of the prepared films is homogeneous and dense, and the root-mean-square surface roughness (Rq) are 21.0 nm (ZrN0.45), 1.8 nm (ZrN0.4), and 2.0 nm (ZrN0.35), respectively. With the increase of nitrogen partial pressure, the content of Zr3N4 in the ZrN films increased gradually. Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) measurements demonstrate that all samples enhance the corrosion performance of ZrN-coated 304 SS. ZrN0.4 possesses a best corrosion resistance in 0.5 M Na2SO4 solution, which maintains complete and dense surface morphologies after 50 h immersion. The underlying related corrosion mechanism was explored and discussed, and the excellent corrosion resistance of ZrN0.4 film on 304 SS can be ascribed to a lower density of pin-hole defects and the dense passive layer of ZrO2.

Effect of Zr content on the structure and morphology of CrZrN thin films prepared by reactive DC magnetron co-sputtering method

In this research, nanostructured chromium zirconium nitride (CrZrN) thin film has been deposited on Si(100) substrates by reactive DC magnetron co-sputtering method without in situ substrate heating and post-deposition annealing. The effects of Zr content on thin film structure and morphology were investigated. The Zr content in the films were varied by applied the sputtering current of Zr target (Izr) in the range of 300 to 900 mA, whereas the current of Cr target was kept at 300 mA. The crystal structure, microstructure, morphology, thickness, and chemical composition were characterized by glancing angle X-ray diffraction (GA-XRD), field emission scanning electron microscopy (FE-SEM), and energy-dispersive X-ray spectroscopy (EDS) techniques, respectively. The results showed that the increase of Izr not only increased the deposition rate, but also increased the Zr content of the as-deposited film ranging from 3.9 to 26.5 at%. The as-deposited thin films were formed as a (Cr,Zr)N solid solution, with fcc structure in (111) and (200) plane, where Cr atoms were replaced by Zr atoms in the CrN lattice. The 2θ diffraction peaks were shifted to the lower value as increase of Zr content which was obtained by increased Izr. The nanocrystalline CrZrN structure with crystal sizes smaller than 10 nm structure were calculated for as-deposited thin films. The lattice parameters increased from 4.187 to 4.381 Å, whereas the crystal size decreased from 8.3 to 6.4 nm. The FE-SEM images of all the CrZrN films exhibited compact columnar with dense morphology as a function of Zr content. Moreover, the thickness of the CrZrN thin films was increased of 302 – 421 nm.

Morphological and mechanical evolution of nanostructured ZrN thin films under 165 keV argon ions irradiation

Zirconium nitride is a promising candidate ceramic material to be adopted as an inert matrix for transuranic fuel, a new fuel concept having as targets the closing of the nuclear fuel cycle, and reduce the environmental impact of nuclear waste. Nevertheless, the comprehension of radiation tolerance of zirconium nitride still limited. In this paper, we have studied the radiation stability of nanostructured zirconium nitride (ZrN) thin films using 165 keV argon-ions (Ar2+) irradiation at room temperature. After irradiation, the microstructural, morphological and mechanical properties of the irradiated ZrN films were investigated and compared to an un-irradiated reference film. The grazing incidence X-ray diffraction tests (GI-XRD) revealed a (100) ZrN textured films, the atomic force microscope (AFM) and the scanning electron microscope (SEM) images showed that the as-deposited ZrN films were nano-crystalline with spherical grains of about 50 nm in size and rms surface roughness of about 1.175 nm. After irradiation, the estimate grains size was found to increase to 72 and 86 nm for films irradiated to 2.3 and 22.3 (dpa) respectively, indicating grains coalescence. The nano-hardness of the irradiated films compared to the un-irradiated film was decreased for both doses, while the XRD patterns demonstrate a crystalline ZrN even at the higher dose of 22.3 (dpa), suggesting along with AFM and SEM results grain growth without amorphisation.

Zirconium Nitride: Optical Properties of an Emerging Intermetallic for Plasmonic Applications

Finding new plasmonic materials with prominent optical properties and unique physical and chemical characteristics, which are merits of traditional gold and silver, is of great interest to many applications. This work uses a series of powerful numerical methods, such as density functional theory (DFT) and electromagnetic modeling approaches, to predict the plasmonic response of a mechanically well‐known material, zirconium nitride (ZrN). DFT first delivers an electronic analysis and optical dispersion data between 1 and 8 eV, experimentally verified in the lower energy regime (), and extremely valuable for any subsequent optical modeling. Subsequent electromagnetic modeling steps, including the transfer matrix method (TMM) and Mie theory, demonstrate the excitation of surface plasmon polaritons and localized surface plasmon resonances in ZrN thin films and nanoparticles. Furthermore, the finite‐difference time‐domain (FDTD) method exhibits the excitation of distinct electric (plasmon) and magnetic (LC) resonances in a periodic array of u‐shaped ZrN split‐ring resonators (SRRs). The findings showcase an optical behavior comparable with structures made from noble metals such as gold and silver and support the introduction of ZrN as a new and appropriate candidate for plasmonic applications, specifically in technological applications where optical and mechanical properties are of simultaneous concern.

Influence of Protection Layers on Thermal Stability of Nitride Thin Films

Nitrides are commonly studied for their properties relevant to numerous coating applications, and have been recently used to synthesize newly predicted materials in thin‐film form. However, the thermodynamic stability of such nitride materials is difficult to experimentally evaluate, due to the limited thermal budget of thin films. Herein, it is shown that the thermal stability of nitride films can be extended using protection layers. Specifically, it is found that zirconium nitride (ZrN) thin films are stable up to at least 1200 °C annealing temperature in N2 atmosphere, if aluminum nitride (AlN) diffusion barriers and capping layers are used. X‐ray diffraction (XRD) measurements show the expected thermodynamically stable rocksalt structure of ZrN, and scanning electron microscopy (SEM) confirms the compact microstructure of these ZrN films. Without such protection layers, the transient bixbyite Zr2ON2 phase and high‐temperature ZrSi2 phase are observed after annealing by XRD, SEM, and Auger electron spectroscopy (AES), due to side reaction with the native surface oxide (ZrOx) and the substrate (Si), respectively. These results demonstrate that protection layers are beneficial to increase the thermal budget of nitride thin films, for evaluating rgw thermodynamic stability of new nitride materials, for capturing transient metastable phases during crystallization, and for using functional nitride coatings in extreme environments.

Structural and physical characteristics of sputter deposited zirconium nitride thin films by sputtering at various time in Ar-N2 atmosphere

Zirconium nitride films were deposited by RF reactive magnetron sputtering at room temperature in an N2 and Ar ambient. The X-ray diffraction analysis indicated that the growth of ZrN with preferred orientations (111) and (200) on the soda-lame glass substrates was reached. The particle size formed on the surface of the synthesized layers increases from 15.9 to 42.1 nm as deposition time increases. The N/Zr ratio decreases from 2.0 to 1.43 with increasing deposition time from 10 to 30, and the average surface roughness increased from 0.88 to 5.58 nm. Increasing the deposition time reduced the bandgap from 2.91 to 2.06 eV and also increased the resistance from 19.84 × 10–6 to 40.69 × 10−6Ω cm. The thermal coefficient of resistance was 9.27 × 10–8 $$\frac{{\Omega \cdot {\text{cm}}}}{{^{ \circ } K}}$$ for the thickest sample and 5.26 × 10–8 $$\frac{{\Omega \cdot {\text{cm}}}}{{^{ \circ } K}}$$ for the thinnest sample. At a wavelength of 600 nm, the refractive index was 2.028 and 0.889 for the samples deposited for 10 and 30 min, respectively.

Effect of hafnium contaminant present in zirconium targets on sputter deposited ZrN thin films

Zirconium nitride thin films deposited by reactive magnetron sputtering recurrently present small amounts of hafnium (~1 at.%) in their composition derived from an inherent impurity existing in Zr targets. Hf presence in ZrN coatings is neglected by most of the researchers despite its known potential to modify properties of thin films. In this work, pure ZrN (0.9 at.% Hf contaminant) and ZrHfN thin films with intentional hafnium addition of 1.8, 3.7 and 5.5 at.% were deposited by reactive magnetron sputtering and characterized by RBS, GAXRD, SEM, nanohardness and high temperature oxidation tests. Based on the results, it is suggested that inherent hafnium presence in zirconium targets contributes for the good hardness values and oxidation resistance at 773 K registered for ZrN thin films.

Nanocrystalline ZrN thin film development via atomic layer deposition for U-Mo powder

Zirconium nitride (ZrN) thin film deposited via thermal atomic layer deposition (ALD) has been recently chosen as a candidate technology for application of a diffusion barrier coating on the low enriched uranium alloy powder considered in the NNSA research reactor conversion program. Reported here is the first instance of using ALD for coating actinide materials. For this study, a modified ALD system was constructed to produce one micron thick zirconium nitride (ZrN) coating over spherical particulate of natural uranium-molybdenum (U-Mo) based fuel. The ALD system was designed to have a rotating drum system, with provisions for facilitating sequential exposures of chemicals such as tetrakis dimethyl amido zirconium (TDMAZr) and ammonia (NH3) in order to deposit ZrN. The ALD system was successful in developing a highly conformal ZrN coating covering every individual U-7Mo particle. This article describes the ZrN film synthesis details and reports the produced microstructure and composition of the ALD ZrN as deposited on fuel particulates. The as-fabricated coating was determined to have a nanocrystalline structure in the cubic-ZrN (cF8) phase. It exhibited a dense microstructure with adequate interfacial bonding. TEM-EELS characterization demonstrated that the coating contains a very low amount of oxygen impurity. To understand the potential microstructural evolution for ALD ZrN during reactor operation, an in-situ heavy ion (Kr) irradiation experiment was performed at the IVEM-Tandem facility. A total fluence of 7.5 × 1015 ions/cm2 (∼10 dpa) was achieved, and apart from minor grain coarsening in the ALD ZrN coating, no significant radiation effects were observed.

Surface, structural, electrical and mechanical modifications of pulsed laser deposited ZrN thin films by implantation of MeV carbon ions

Atomic Force Microscope (AFM), X-ray Diffraction (XRD), four point probe and micro hardness techniques are utilized for studying the surface, structural, electrical and mechanical properties of ions beam irradiated nanostructured zirconium nitride (ZrN) thin films. Pulsed laser deposition technique is employed for the growth of ZrN thin films by using Nd:YAG laser (532 nm, 140 mJ, 6 ns, 10 Hz). The deposited films were irradiated with 2 MeV carbon (C+) ions at fluences ranging from 0.2 × 1015 to 1.8 × 1015 ions/cm2 by using Pelletron accelerator. AFM analysis reveals the formation of ion induced nano hillocks whose density and size are dependent upon ion irradiation fluence. The growth of these nanostructure is explained on the basis of thermal spike model. XRD analysis depicts higher angular shifting which leads to unit cell contraction along with evaluation of crystallite size, lattice parameter, strain and stresses at different ion fluences. The ion induced phase transition from metastable Zr3N4 to stable ZrN phase and the formation of new ZrC phase is also observed. The electrical resistivity explored by four point probe method is decreased after ion irradiation and is found to be dependent upon phase transformation as well as irradiation fluence. The ion irradiation induced increase in surface microhardness at different fluences is attributed to the change in crystallite size, formation of point defects and ZrC phases. The modifications in electrical and mechanical properties are well correlated with ion irradiation induced structural modification.

Study of the structural and electrical properties of silicon ion irradiated zirconium nitride thin films

In this work, modification in structural and electrical properties of zirconium nitride (ZrN) thin films induced by silicon-ion irradiation is studied. ZrN thin films are grown on glass substrate over Zirconium (Zr) layer using cathodic arc evaporation method. The samples of the film are irradiated with silicon ions of energy 2.08 MeV at different fluences ranging from [Formula: see text] ions/cm[Formula: see text] to [Formula: see text] ions/cm[Formula: see text]. The structural and electrical properties of the prepared films are investigated using X-ray diffraction (XRD), Raman spectroscopy and four-point probe method. XRD analysis shows significant shift in the peak corresponding to (111) crystallographic plane of ZrN at low fluence ([Formula: see text] ions/cm[Formula: see text]) while modest peak shift at high fluence rate ([Formula: see text] ions/cm[Formula: see text]) is observed. Under the electrical properties point of view, it is observed that the decrease in resistivity is small at high ion fluence as compared to that at low ion fluence. At highest fluence of [Formula: see text] ions/cm[Formula: see text], resistivity of the irradiated sample approaches the resistivity of the un-irradiated sample indicating very small changes in structure at very high dose irradiance.

An XPS study on oxidation of exposed-to-air Cr1−xZrxN film surfaces

Chromium zirconium nitride (CrZrN) thin films were prepared on Si (100) substrates with various Zr contents by using co-sputtering technique. The Zr content was varied by variation of the Zr sputtering current from 0.2 to 0.8 A while the Cr current and the N2 flow rate were kept at 0.8 A and 6.0 sccm, respectively, to fix the concentration of Cr and N atoms. An oxidation caused by exposure to air of the Cr1−xZrxN thin films were studied by using X-ray photoelectron spectroscopy (XPS). Chemical composition analysis of XPS spectra revealed that oxygen detected on the film surfaces was increased with the rise in the Zr content. Deconvolutions of O 1s photoemission lines revealed bonding separately of O atoms to Cr and Zr atoms. Moreover, the fraction of the O–Cr bond was increased with the increasing Zr content.

Effects of nitrogen gas ratio on the structural and corrosion properties of ZrN thin films grown on biodegradable magnesium alloy by ion-beam sputtering

Studies on the corrosion resistance of magnesium alloys, which are widely applied as biomaterials, have increased in recent years. In this work, zirconium nitride (ZrN) coatings were deposited on AZ91 magnesium alloy through ion-beam sputtering at 473 K with 0.3, 0.4, 0.5, and 0.6 nitrogen proportions [F(N2)] in ionized gas. X-ray diffraction, profilometry, hardness tests, scanning electron microscopy, and potentiodynamic polarization techniques were used to analyze the structure, thickness, adhesion, microstructure, and corrosion resistance of coated samples, respectively. Results showed that the (111) crystalline orientation dominated in all coatings. Williamson–Hall technique revealed that the crystallite size of ZrN films decreased from 73 to 20 nm with increasing F(N2), and compressive microstrain increased from 0.004 to 0.030. Film thicknesses were inversely correlated with N2 amount and significantly decreased from 1.7 to 0.8 µm. The maximum dP/dr ratio, a dependent factor of adhesion, was 0.04 kg/cm for the film deposited under the F(N2) value of 0.5. The corrosion potential of coated samples was not significantly different from that of uncoated AZ91. Under the F(N2) value of 0.6, corrosion current density slightly decreased from 14 to 9.7 µA/cm2 and significantly increased to 13.5 µA/cm2. Results indicated that ZrN film deposited under the F(N2) value of 0.5 showed high adhesion and corrosion resistance.