Diffraction Intensity Research Articles

A boundary integration method for calculating diffraction intensity of crystalline materials with planar deformation

Defects and strain states in crystals can be investigated using X-ray and neutron diffraction, two types of penetrating, non-destructive detection techniques. Various approximations are frequently employed to minimize the amount of computation in the practical calculations because the present Fourier transform approach, established by Warren, Averbach et al. based on the Kinematic diffraction theory, has a huge computational cost. This paper develops a numerical method to precisely calculate diffraction intensity by integrating kinematic diffraction amplitude over the boundary, which is applicable to crystals with planar deformation. The precision of this method is assessed by contrasting it with Wilson's analytical equations for the X-ray diffraction results of a single screw dislocation. As an example, the difference in diffraction spots on a single edge dislocation irradiated by different incident X-ray widths are calculated and analyzed. When compared to the X-ray diffraction spots of an ideal material with a dislocation core dug out, the results indicate that if lattice information close to the dislocation core is to be retrieved by X-ray diffraction, the X-ray irradiation area should be restricted.

Three-dimensional refractive index microscopy based on the multi-layer propagation model with obliquity factor correction

Multi-layer propagation model-based intensity diffraction tomography (IDT) is a three-dimensional (3D) microscopy imaging technique to reveal the structural information of optically thick or multiple scattering samples. However, the performance of existing multi-layer propagation models deteriorates with increasing illumination angle, which can prevent good 3D refractive index (RI) imaging. To overcome this limitation, we incorporate the obliquity factor (OF) into the multi-layer propagation model. Numerical simulation validates that the forward propagation and the RI reconstruction both can be considerably improved. Then, the 3D RI reconstruction performance is quantitatively and qualitatively validated by optical experiments on polystyrene microspheres and peony pollen grains, respectively. In addition, excellent optical sectioning and high spatial resolution are experimentally demonstrated on various unlabeled fixed and living samples, including an Arabidopsis root, HeLa and HCT-116 cells. Time-lapse 3D imaging of living samples is performed for the first time for multi-layer propagation model-based IDT, demonstrating its potential application to some biological and medical studies.

Effect of high-pressure treatment on the rheological properties of Alyssum homolocarpum seed gum/grass pea protein isolate dispersions and comparison with heat-induced gels

The effects of high-pressure (HP) treatment at 400 MPa for 15 min on rheological properties of dispersions and gels of grass pea protein isolate (10% GPPI) containing different concentrations of Alyssum homolocarpum seed gum (0.2, 0.4 and 0.6% AHSG) were investigated. With the addition of AHSG, the amount of α-helix, β-sheet, and random coils in pre-treated GPPI decreased, whereas after HP treatment, α-helix and β-turn content increased. For AHSG-GPPI mixtures, it was found that HP treatment increased the intensity of X-ray diffraction peaks at 2θ = 11 and 26°, which had previously been found to decrease and become flatter with increasing gum concentration. The thermal degradation temperature (Td) and enthalpy (ΔH) increased after the addition of AHSG and following HP treatment. All mixed solutions had shear thinning behavior before and after HP treatment. When AHSG was added to GPPI, η0 and η∞ increased for both HP-treated and untreated samples, while after the treatment, the magnitude of η0 and η∞ slightly decreased. G′ values were higher than G″ values for all AHSG-GPPI dispersions, indicating a gel-like behavior for these mixtures. With increasing gum concentrations, G′ and G″ values of dispersions increased; however, these moduli decreased after exposure to HP treatment, though they were not statistically significant. The addition of AHSG significantly decreased the gelation temperature, increased the G′ value, and made the system more elastic during conventional heating and cooling ramps. When the HP treated samples were heated, the G′ value increasing trend was almost identical to that of the untreated samples, but during the cooling stage, the value of G′ for the HP treated samples were significantly higher.

2D Helium Atom Diffraction from a Microscopic Spot.

A method for measuring helium atom diffraction with micron-scale spatial resolution is demonstrated in a scanning helium microscope (SHeM) and applied to study a micron-scale spot on the (100) plane of a lithium fluoride (LiF) crystal. The positions of the observed diffraction peaks provide an accurate measurement of the local lattice spacing, while a combination of close-coupled scattering calculations and MonteCarlo ray-tracing simulations reproduce the main variations in diffracted intensity. Subsequently, the diffraction results are used to enhance image contrast by measuring at different points in reciprocal space. The results open up the possibility for using helium microdiffraction to characterize the morphology of delicate or electron-sensitive materials on small scales. These include many fundamentally and technologically important samples which cannot be studied in conventional atom scattering instruments, such as small grain size exfoliated 2D materials, polycrystalline samples, and other surfaces that do not exhibit long-range order.

Structure and Properties of Cationic Chitosan Derivative Modified Bombyx mori

Abstract Cationic modification of silk fabric can highly improve its antibacterial property, but cationic modification may change the microstructure of silk fiber, and further affect its properties, thus O-methyl acrylamide quaternary ammonium salt of chitosan (NMA-HTCC), which is a kind of strong cationic chitosan derivative, was used for the modification on Bombyx mori silk fiber. The combination structure between NMA-HTCC and silk fiber was characterized by FT-IR. The surface morphology and structure of silk fiber after being treated by NMA-HTCC were investigated by SEM and XPS analysis. The crystalline structure and thermal stability of silk fibers before and after being treated were determined by XRD and DSC analysis, respectively. Then the breaking strength, breaking elongation and antibacterial properties of the silk yarns were also determined. The results indicated that the NMA-HTCC modified silk fiber clearly showed two characteristic absorption peaks at 1535 cm-1 and 1670 cm-1 due to the N-H bending and C=O stretch of the secondary amide in the acrylamidomethyl group of the NMA-HTCC molecule. The successful combination of NMA-HTCC and silk fiber was also confirmed by XPS and SEM analysis. Compared with the untreated silk sample, the diffracted intensity of the characteristic absorption peak and crystallinity of the NMA-HTCC modified silk fiber were both increased; the internal aggregation structure of the silk fiber treated with NMA-HTCC was much closer and its thermal stability was enhanced obviously. The breaking strength and elongation of silk fibers after being treated with NMA-HTCC were also significantly increased. Silk fibers treated with NMA-HTCC had excellent durable antibacterial properties against S. aureus and E. coli, even after 50 repeated launderings, with the bacterial reduction rate of the silk fibers maintained at over 95 %. The results in this research can provide the theoretical basis for the application of NMA-HTCC in the modifications of silk fabric.

Fabrication of ultra-low porosity plasma electrolytic oxidation coating on Ta-12W alloys and its formation mechanism

The sealing of pores in plasma electrolytic oxidation (PEO) coatings is critical to further enhance the protection of the underlying substrate and maintain the mechanical performance of coatings. This study focuses on the modification of the surface microstructure of PEO coatings on Ta-12W alloy by introducing NH4F additive into a mixed silicate-phosphate electrolyte. As a result, ultra-low porosity coating with a surface porosity of less than 1 % is effectively prepared. Detailed investigations have been conducted to study the effects of NH4F content and treatment duration on various coating characteristics, including microscopic morphology, elemental distribution, thickness, and phase composition. It is found that optimizing the concentration of NH4F eliminates the large pore structures and promotes the development of Ta-rich structures resembling pancakes on the coating surface. Furthermore, the intensities of diffraction peaks from different crystal faces of Ta2O5 in coatings exhibit variations, and selective growth is observed specifically on its (110) crystal plane. After a 20-minute treatment of Ta-12W alloys in the electrolyte containing 4 g/L NH4F, the surface of the coating displays predominantly pancake-like structures with sealed pore/non-pore features. The formation process of these specific structures is discussed based on the evolution of coating morphology with oxidation time. It is proposed that the increase in anodic voltage and gas production in the late stage favors the breakdown of gas bubbles, leading to the creation of non-porous pancake-like structures on the surface. In addition, the breakdown of the dielectric layer at the periphery of gas bubbles results in the influx of film-forming materials into pores, which causes the formation of pancake-like structures with sealed pores.

Investigation of dynamical X-ray back diffraction at grazing incidence

We report a theoretical investigation of X-ray back diffraction at grazing incidence. Based on the framework of the dynamical theory of X-ray diffraction, the grazing incidence for Si (12 4 0) back diffraction is taken as an example to resolve the eigenvalue problem inside the crystal. The dispersion surface and the resulting diffraction intensities are strongly affected by the miscut angle as well as the diffraction geometry of grazing incidence. The kinematical relationship between the incident angle and the miscut angle is well explained by Snell’s law. While only the two-beam diffraction is considered, our treatment can be further extended to include the cases for multiple diffractions as well.

Characteristic of Natural and Acid-activated Clay From Hatu Village, Mollucas Province: FTIR, XRD, XRF, SEM-EDX, TEM, and BET Analysis

Research on the chemical and physical characteristics of natural and acid-activated clay from Hatu Village had been carried out using FTIR, XRD, XRF, SEM-EDX, TEM, and BET surface area analyzer instruments. The natural clay had activated with 0.25 M sulfuric acid for 3 hours using the reflux method, then calcined with 700 Watt microwave radiation for 10 minutes. Overall, FTIR data show tetrahedral and octahedral functional groups that create clay minerals. There is a decrease in absorption intensity due to acid's influence, which dissolves cations in the octahedral and interlayer clay. The XRD analysis shows the Hatu natural clay contains montmorillonite, alumina, kaolinite, quartz, and illite minerals. Broadening and decreasing the intensity of diffraction peaks due to treatment by acid and calcination. SEM images of natural clay before and after activation-calcination shows the morphology of porous and layered material, while the mapping of the surface of natural clay shows irregular and rough material topography. The EDX spectra showed four elements with the most extensive composition: O, Si, Al, and Fe. XRF data confirmed three components that have the highest mass percent, namely SiO2, Al2O3, and Fe2O3. Dealumination occurs at 0.95% due to activation by sulfuric acid along with calcination. TEM images clearly show the multilayered silicate materials. The higher nitrogen gas uptake by activated-calcinated natural clay is proportional to the large surface area and total pore volume.

Hydrogenetic and Diagenetic Controls on the Specific Surface Area of Polymetallic Nodules in Deep Ocean Basins

Polymetallic nodules (nodules) are a predominant deep-sea mineral resource due to theirenrichment with critical metals, such as Co, Ni, and Cu, and rare earth elements (REEs). The loose and porous nature of nodules contributes to their adsorption and enrichment in trace metals from seawater and pore water. Consequently, the specific surface area (SSA) of nodules is a key factor requiring further study. However, controls on the SSA of nodules with various genetic types remain poorly characterized. This study aimed to investigate controls on nodule SSA by analyzing the transition metals, REEs, mineralogy, and SSA of nodules recovered from basins in the Atlantic, Indian, and Pacific oceans, including the Northwest Pacific Basin (NPB), Bauer Basin (BB), Tiki Basin (TB), Wharton Basin (WB), Central Indian Basin (CIB), and Angola Basin (AB). Nodule SSAs were compared among the various basins by calculating the BET SSA (based on the equation proposed by Brunauer, Emmett, and Teller, 1938). The results suggest thatnodules from the PNB, WB, CIB, and AB are mainly hydrogenetic, and those nodules have a relatively high SSA, high Co, low Ni and Cu, positive Ce anomalies, and low X-ray diffraction (XRD) intensities at ~10 Å. The nodules from the BB and TB are mainly diagenetic in origin, characterized by a relatively low SSA, low Co, high Ni and Cu, negative Ce anomalies, and high XRD intensities at ~10 Å. The SSAs of nodules were significantly positively correlated with Co, δCe, and light REEs (LREEs), and negatively correlated with the XRD intensity at ~10 Å, Ni, and Cu. The SSAs of nodules from the NPB ranged from 329.440 m2/g to 418.711 m2/g, comparable to the SSAs of Co-rich crusts on seamounts. This study proposes that nodule SAA is regulated by nodule genesis and that hydrogenetic nodules have a higher SSA.

Order-disorder (OD) polytypism of K3FeTe2O8(OH)2(H2O)1+x.

K3FeTe2O8(OH)2(H2O)2 was synthesized under hydrothermal conditions from Te(OH)6, FeSO4·7H2O and 85 wt% KOH in a 1:2:6 molar ratio. The crystal structure is built of a triperiodic network. One disordered water molecule per formula unit is located in a channel and can be partially removed by heating. Systematic one-dimensional diffuse scattering indicates a polytypic character, which is best described by application of the order-disorder theory. The major polytype is monoclinic with pseudo-orthorhombic metrics. It is interrupted by fragments of an orthorhombic polytype. The diffraction intensities are analyzed using structure factor calculations.

Dehydroxylation of Kaolinite and Halloysite-Rich Samples: An In Situ Study of the Texture and Structural Evolutions

Halloysite and kaolinite are dioctahedral TO phyllosilicates that drive the interest of scientists for formulating environmentally friendly materials, and consequently in the field of ceramics. The main scope of this study was the understanding of the texture evolution upon the dehydroxylation reaction and the influence of the presence of halloysite. In situ synchrotron (002) and (111) poles figures were recorded on the DiffAbs beamline at SOLEIL Synchrotron, from room temperature to 1000 °C, on kaolinite and/or halloysite-rich samples shaped by tape casting. Commercial kaolins and halloysite provided by Imerys company were used. The samples were labeled KRG100, KCS100, H100, KRG50H50 and KRG59H50 in relation with the wt. % of kaolin (KRG, KCS) or halloysite (H) clays. In samples KCS100 and KRG100, a strong texture was observed until in situ annealing at 700 °C, with respect to the c-axis of kaolinite. On the contrary, the texture with respect to the c-axis of halloysite for the sample H100 was weak whatever the temperature was. Moreover, this weak texture disappeared before the complete dehydroxylation of halloysite. This is due to the opening of some halloysite tubes. When considering the samples KRG50H50 and KCS50H50, a significant texture was observed with the c-axis preferentially oriented perpendicular to the sample surface. The presence of kaolinite platelets predominated onto the alignment of halloysites tubes. Furthermore, it was noted that the halloysite influenced the (002) diffracted intensity into the temperature range 20 °C to 400 °C. Above 400 °C, the behavior obtained for the (002) reflection in samples KRG50H50 and KCS50H50 was similar to the behavior noticed for pure kaolins KRG100 and KCS100, respectively. The dehydroxylation temperature range appeared to be relevant with combined effect of kaolinite and halloysite transformations arising from KRG100 or KCS100 and H100 samples. Therefore, the onset point of dehydroxylation is 550 °C ± 25 °C for KRG100, KCS100, KRG50H50 and KCS50H50. For the pure halloysite H100 sample, the dehydroxylation starts at the lower temperature 475 °C. It was also noted that during the dehydroxylation of kaolinite, the characteristic portion of ring related to the diffracted intensity of the (111) reflection located at χ = 45° tended to disappear above 550 °C and led to the formation of a new transitory phase with a (111) reflection with perpendicular alignment to the c-axis. Indeed, an epitaxial relationship with the (111) kaolinite reflection could be assumed. Further X-ray scattering experiments allowed highlighting the effective offset temperature of the dehydroxylation, which was identified as close to 720 °C. The metakaolinite achieved structural transformation to another transitory phase at 1000 °C.

Semi-quantitative analysis study of the impact of microwave treatment on fly ash

Pre-processing provides an effective way for fly ash's high value-added utilization. However, the shortcomings of pre-processing methods such as grinding and flotation are apparent, with many disadvantages that make it more challenging to use efficiently. Microwave heating helps the SiO2-Al2O3 bond break, not only can make the structural change of the material can also promote the chemical reaction process. In the article, XRD, SEM, FT-TR, ammonia nitrogen adsorption, and other methods were used to analyze the changes in the properties of fly ash before and after microwave pre-treatment, the change of adsorption performance of fly ash before and after microwave treatment was analyzed. The study found that under microwave conditions of 600W and 15min, the adsorption rate of ammonia nitrogen by fly ash reached the maximum of 29.67%. The intensity of mullite and amorphous diffraction peaks decreased after 20 minutes at 600W. The Si-O-(Si, Al) and Si-O-(Si) bonds showed significant changes at 15 and 20 minutes under 600W conditions. Based on the results, microwave conditions were selected at 600W for different periods, and semi-quantitative analysis was carried out by XRD-Rietveld, infrared peak fitting, and nuclear magnetic resonance. The XRD-Rietveld analysis showed that the amorphous phase content reached 46.18% at 15 minutes. In the infrared peak fitting, the fitting area at 1300-900cm-1 and 600-400cm-1 peaks reaches 56.92% at 25 minutes and 17.5% at 15 minutes, respectively. The silicon-oxygen network's degree of connection and polymerization is reduced after 15 minutes of microwave treatment for the nuclear magnetic resonance analysis.

Simulation of ultrafast electron diffraction intensity under coherent acoustic phonons.

Ultrafast electron diffraction has been proven to be a powerful tool for the study of coherent acoustic phonons owing to its high sensitivity to crystal structures. However, this sensitivity leads to complicated behavior of the diffraction intensity, which complicates the analysis process of phonons, especially higher harmonics. Here, we theoretically analyze the effects of photoinduced coherent transverse and longitudinal acoustic phonons on electron diffraction to provide a guide for the exploitation and modulation of coherent phonons. The simulation of the electron diffraction was performed in 30-nm films with different optical penetration depths based on the atomic displacements obtained by solving the wave equation. The simulation results exhibit a complex relationship between the frequencies of the phonons and diffraction signals, which highly depends on the laser penetration depth, sample thickness, and temporal stress distribution. In addition, an intensity decomposition method is proposed to account for the in-phase oscillation and high harmonics caused by inhomogeneous excitation. These results can provide new perspectives and insights for a comprehensive and accurate understanding of the lattice response under coherent phonons.

Transformation of the structure of the polyimide film during deformation: The effect of thickness

The effect of the thickness of the amorphous polymerized films of poly-4,4'-diphenylene oxide pyromellitimide on the structure after deformation by stretching at 293 K and 77 K was studied. The evolution of the macromolecular structure was concluded based on the results of the redistribution of the intensity diffraction peaks. It was established that the structure of films with a thickness of 75 μm is homogeneous and does not cardinal changes after deformation. Deformation of polymer films with a thickness of 125 μm leads to the appearance of regions with long-range order in the sample.

Enhancing Contrast of Spatial Details in X-ray Phase-Contrast Imaging through Modified Fourier Filtering

In-line X-ray phase contrast imaging, which is simple to experiment with, provides significantly higher sensitivity, compared to conventional X-ray absorption imaging. The inversion of the relationship between recorded Fresnel diffraction intensity and the phase shift induced by the object is called phase retrieval. The transport of intensity equation (TIE), a simple method of phase retrieval, which is solved by the fast Fourier transform algorithm proposed by Paganin et al., has been widely adopted. However, the existing method suffers from excessive suppression of high-frequency information, resulting in loss of image details after phase retrieval, or insufficient detail contrast, leading to blurry images. Here, we present a straightforward extension of the two-distance FFT-TIE method by modifying the Fourier filter through the use of a five-point approximation to calculate the inverse Laplacian in a discrete manner. Additionally, we utilize a combination of continuous Fourier transform and a four-point approximation to compute the gradient operator. The method is evaluated by simulating samples with a shape similar to the resolution test map and by using a photograph of a dog for further evaluation. The algorithm that incorporates the modified gradient operator and the algorithm that solely utilizes the continuous Fourier transform for gradient computation were compared with the results obtained using the two-distance FFT-TIE method. The comparisons were conducted using the results obtained from two distances from the sample to the detector. The results show that this method improves the contrast of spatial details and reduces the suppression of high spatial frequencies compared to the two-distance FFT-TIE method. Furthermore, in the low-frequency domain, our algorithm does not lose much information compared to the original method, yielding consistent results. Furthermore, we conducted our experiments using carbon rods. The results show that both our method and the FFT-TIE method exhibit low-frequency distortion due to the requirement of close proximity between the absorption maps and the detector. However, upon closer inspection, our proposed method demonstrates superior accuracy in reproducing the finer details of the carbon rod fibers.

Beam Effects on Atomic Dynamics in Metallic Glasses Studied With Electron Correlation Microscopy.

Electron correlation microscopy (ECM) is used to investigate atomic dynamics in metallic glasses (MG) close to metastable equilibrium. It temporally correlates diffracted intensities of a time series of dark-field images to deduce a metric for structural decays. The measurement parameters, such as time and temperature, must be chosen according to the material of interest. In this work, ECM was extended to measurements at room temperature. To ensure, or select, a time window with quasi-thermodynamic equilibrium/steady-state measurement conditions, two-time correlation functions of diffracted intensities were calculated. The dynamics at room temperature are partly driven by the electron beam, thus affecting the material and the results. A systematic analysis of the influence of the electron beam is presented, revealing an inverse relation between electron dose rate and intensity correlation decay times at 300 kV acceleration voltage. However, the underlying dynamical mechanisms, described by a stretching exponent, are found to be independent of the applied electron dose rate for a Pd40Ni40P20 MG. An extrapolation of the results to infinite long measurement times and zero dose rate agrees with X-ray photon correlation spectroscopy data and justifies the application of beam-driven ECM at room temperature to study the dynamics of disordered systems.

Effects of freeze-thaw cycles on in-vitro digestive properties of myofibrillar protein in mirror carp (Cyprinus carpio L.), based on protein degradation, oxidation, and structural properties

The in-vitro digestive properties of myofibrillar protein (MP) in mirror carp (Cyprinus carpio L.) after freeze-thaw (F-T) cycles were analyzed in terms of the relationship between protein degradation, oxidation, and structural properties. The F-T samples exhibited a significant increase in glucosidase activity, N-acetyl-β-d-glucosidase activity, total protease activity, and non-protein nitrogen content. α-aminoadipate semialdehyde and γ-glutamate semialdehyde contents increased by 23.17% and 123.12%, respectively. Furthermore, 53.97% decrease in the total nitrogen content and changes in the content of different soluble proteins were observed. X-ray diffraction intensity, thermal stability, free amine content, hydrolysis degree, and digestibility of the MP samples decreased, and the 2θ angle and zeta potential were reversed. Besides, changes in the amide band wavenumbers were also detected. Therefore, the protein structure was unfolded and aggregates were formed through degradation and oxidation induced by the F-T cycles, ultimately making the in-vitro digestion of MP difficult.

Scanning precession electron diffraction data analysis approaches for phase mapping of precipitates in aluminium alloys

Mapping the spatial distribution of crystal phases with nm-scale spatial resolution is an important characterisation task in studies of multi-phase materials. One popular approach is to use scanning precession electron diffraction which enables semi-automatic phase mapping at the nanoscale by collecting a single precession electron diffraction pattern at every probe position over regions spanning up to a few micrometers. For a successful phase mapping each diffraction pattern must be correctly identified. In this work four different approaches for phase mapping of embedded precipitates in an Al-Cu-Li alloy are compared on a sample containing three distinct crystal phases. These approaches are based on: non-negative matrix factorisation, vector matching, template matching and artificial neural networks. To evaluate the success of each approach a ground truth phase map was manually created from virtual images based on characteristic phase morphologies and compared with the deduced phase maps. The percentage accuracy of all methods when compared to the ground truth was satisfactory, with all approaches obtaining scores above 98%. The optimal method depends on the specific task at hand. Non-negative matrix factorisation is suitable with limited prior data knowledge but performs best with few unique diffraction patterns and requires substantial post-processing. It has the advantage of reducing the dimensionality of the dataset and handles weak diffracted intensities well given that they occur repeatedly. The current vector matching implementation is fast, simple, based only on the Bragg spot geometry and requires few parameters. It does however demand that each Bragg spot is accurately detected in each pattern and the current implementation is limited to zone axis patterns. Template matching handles a large range of orientations, including off-axis patterns. However, achieving successful and reliable results often require thorough data pre-processing and do require adequate diffraction simulations. For artificial neural networks a substantial setup effort is demanded but once trained it excels for routine tasks, offering fast predictions. The implemented codes and the data used are available open-source. These resources and the detailed assessment of the methods will allow others to make informed decisions when selecting a data analysis approach for 4D-STEM phase mapping tasks on other material systems.

Mathematical uniqueness of multimode ptychographic imaging.

By writing diffracted intensities as a set of linear equations with the self-correlation of sample's Fourier components as unknown terms and the self-correlation of illumination's Fourier components as coefficients, it was found that the number of unknown terms to be determined is much larger in partially coherent PIE than that in purely coherent PIE. When a partially coherent illumination composed of N modes was applied a unique reconstruction can be determined by scanning the sample to at least 4N positions and recording 4N frames of diffraction patterns. While mathematically illustrating the physical mechanism of multimode ptychography and numerically demonstrating its capability in generating unique reconstruction under partially coherent illumination, this study showed for the first time that multimode ptychography could be an analytic imaging method.

Growth and stability of epitaxial zirconium diboride thin films on silicon (111) substrate

The epitaxial growth of boron rich hexagonal zirconium diborides (h-ZrB2+δ) thin films on Si(111) substrates using the magnetron co-sputtering technique with elemental zirconium and boron is reported. The effect of process temperature (700–900 °C) on the compositions and epitaxy quality was investigated. The chemical composition of the films was found to have a higher boron to zirconium ratio than the ideal stoichiometric AlB2-type ZrB2 and was observed to be sensitive to process temperature. Films deposited at 700 °C exhibited intense diffraction peaks along the growth direction corresponding to (000ℓ) of h-ZrB2 using both lab and synchrotron-based x-ray diffractograms. The thermal and compositional stability of the epitaxial h-ZrB2+δ film was further evaluated under a nitrogen-rich environment through isothermal annealing which showed a reduction in in-plane misorientation during thermal annealing. The relative stability of deviating compositions and the energetics of impurity incorporations were analyzed using density functional theory simulations, and the formation of native point defects or impurity incorporation in h-ZrB2 was found to be endothermic processes. Our experimental results showed that an epitaxial thin film of h-ZrB2+δ can be grown on Si(111) substrate using a magnetron co-sputtering technique at a relatively low processing temperature (700 °C) and has the potential to be used as a template for III-nitride growth on Si substrates.