Chemical Vapor Deposition Reactor Research Articles

Understanding the competing growth of 2D and 3D transition metal dichalcogenides in a chemical vapor deposition (CVD) reactor

The competing growth of two-dimensional (2D) and three-dimensional (3D) crystals of layered transition metal dichalcogenides (TMDCs) has been reproducibly observed in a large variety of chemical vapor deposition (CVD) reactors and demands a comprehensive understanding in terms of involved energetics. 2D and 3D growth is fundamentally different due to the large difference in the in-plane and out-of-plane binding energies in TMDC materials. Here, an analytical model describing TMDC growth via CVD is developed. The two most common TMDC structures produced via CVD growth (2D triangular flakes and 3D tetrahedra) are considered, and their formation energies are determined as a function of their growth parameters. By calculating the associated energies of 2D triangular or 3D tetrahedral flakes, we predict the minimum sizes of the critical nuclei of 2D triangular and 3D morphologies, and thereby determine the minimum realizable dimensions of TMDC, in the form of quantum dots. Analysis of growth rates shows that CVD favors 2D growth of MoS2between 820 K and 900 K and 3D growth over 900 K. Our model also suggests that the flow rates of TMDC precursors (metal oxide and sulfur) in a long, cylindrical CVD reactor are important parameters for attaining uniform growth. Our model provides a compressive analysis of TMDC growth via CVD. Therefore, it is a critical tool for helping to achieve reproducible growth of 2D and 3D TMDCs for a variety of applications.

Free-standing n-type phosphorus-doped diamond

n-type diamond substrates are highly desired for diamond electronics and quantum technology based on NV centers. In this work, we investigate the high growth rates obtained using plasma with high-power densities in a commercial bell-jar chemical vapor deposition reactor equipped with a gas panel for diamond doping with phosphorus impurities. We evidence that the diamond growth rate is increased by adding phosphorus precursor in the gas mixture, up to 21.6 μm/h. We found conditions for growing extremely thick (up 580 μm) phosphorus doped (100) diamond homoepilayers keeping a n-type character as shown by optical spectroscopy. From such films we succeed in slicing a free-standing phosphorus-doped diamond plate, showing the feasibility of n-type diamond substrate fabrication for further use in optoelectronics and quantum devices.

Homoepitaxial growth of device-grade GaAs using low-pressure remote plasma CVD

We have achieved the growth of high-quality, homoepitaxial 100 GaAs thin films at 0.5 mbar and 500 °C using a Remote Plasma Chemical Vapor Deposition (RP-CVD) reactor. With this process, we demonstrate a film growth rate up to 3 μm/h, comparable to the conventional MOCVD technique. The resulting films exhibit structural characteristics close to those of commercial GaAs wafers, with excellent crystalline quality as confirmed by SAED patterns and XRD rocking-curve measurements for the 004 peak with a FWHM of 0.004°. AFM measurements reveal a surface roughness of 0.2 nm, similar to that of a polished wafer. Analysis of the chemical composition – as determined through XPS surface and depth-profiled measurements – indicates that the film is homogeneous, with a constant III/V ratio of 1 throughout the whole layer, and has no detectable carbon or oxygen contamination. Additionally, the films demonstrate a sharp photoluminescence peak (FWHM of 55 meV), a p-type doping concentration of 1.1018 cm−3, and a hole mobility of 172 cm2 V⁻1.s⁻1. This work thus demonstrates a cost-effective growth method for III-V devices, enabled by the reduced gas consumption (only a few sccm, compared to tens of L/min in MOCVD) in RP-CVD operation at low pressure.

Controlling the Crystalline Quality and Yield of Single‐Walled Carbon Nanotubes via Floating Catalyst Chemical Vapor Deposition Synthesis

AbstractCarbon nanotubes (CNTs) were synthesized by floating catalyst chemical vapor deposition (FCCVD) reactions. The complicated processing parameters that included a precursor solution composition, reaction temperature, flow rate of the carrier gas, weak oxidants, and injection rate of the precursor solution were controlled to synthesize single‐walled carbon nanotubes (SWCNTs) during the reaction process. The effects of the processing parameters were analyzed with respect to the formation of SWCNTs, yield, and the crystallinity in the CNTs structure. The SWCNTs were characterized by the Raman spectroscopy, scanning electron microscope, high‐resolution transmission electron microscopy, and thermogravimetric analysis. A high reaction temperature, high H2 flow rate, low injection rate of solution precursor, and low concentrations of iron catalysts in the reaction were important factors to improve the crystalline quality of the SWCNTs. The purity of the initial product grown by the standard process was more than 90 wt %, with a yield of 0.5 g/h. The average G/D ratio of the initial product was 178, and it had a distinct RBM peak. HRTEM confirmed that the synthesized SWCNTs had high purity and crystallinity. The SWCNTs could be tunable to meet a particular application by varying the reaction conditions.

Online Three-Dimensional Fuzzy Reinforcement Learning Modeling for Nonlinear Distributed Parameter Systems

Distributed parameter systems (DPSs) frequently appear in industrial manufacturing processes, with complex characteristics such as time–space coupling, nonlinearity, infinite dimension, uncertainty and so on, which is full of challenges to the modeling of the system. At present, most DPS modeling methods are offline. When the internal parameters or external environment of DPS change, the offline model is incapable of accurately representing the dynamic attributes of the real system. Establishing an online model for DPS that accurately reflects the real-time dynamics of the system is very important. In this paper, the idea of reinforcement learning is creatively integrated into the three-dimensional (3D) fuzzy model and a reinforcement learning-based 3D fuzzy modeling method is proposed. The agent improves the strategy by continuously interacting with the environment, so that the 3D fuzzy model can adaptively establish the online model from scratch. Specifically, this paper combines the deterministic strategy gradient reinforcement learning algorithm based on an actor critic framework with a 3D fuzzy system. The actor function and critic function are represented by two 3D fuzzy systems and the critic function and actor function are updated alternately. The critic function uses a TD (0) target and is updated via the semi-gradient method; the actor function is updated by using the chain derivation rule on the behavior value function and the actor function is the established DPS online model. Since DPS modeling is a continuous problem, this paper proposes a TD (0) target based on average reward, which can effectively realize online modeling. The suggested methodology is implemented on a three-zone rapid thermal chemical vapor deposition reactor system and the simulation results demonstrate the efficacy of the methodology.

Polycrystalline inclusion-free growth of thick, lattice-matched SiGeC with high substitutional Carbon concentrations up to 2%

Lattice-matched SiGeC with ~20% of Ge was grown at 550°C, 10 Torr on a 300 mm Si substrate in an industrial standard Reduced Pressure Chemical Vapor Deposition reactor using commercially available Si2H6/GeH4/SiH3CH3 precursors. Thicknesses exceeding 250 nm resulted in cluster formation in SiGeC with [C]Sub~2.0% and [C]Int~0.4%, with a surface density up to 6.13x106 µm-2. Room temperature photoluminescence measurements showed that the clusters were non-radiative defects and Transmission Electron Microscopy, using the ASTAR system, proved they were polycrystalline with random orientation. Cluster-free growth was achieved for 1 µm thick SiGeC with [C]Sub~1.0% and no interstitial carbon atoms, however, without lattice-matched growth on a Si substrate. Injecting HCl during a co-flow process resulted in a smooth surface with a RMS roughness of 0.23 nm and a reduction of [C]Intfrom ~0.7% down to ~0.1%, close to the detection limit of X-ray Photoelectron Spectroscopy at 0.1%. This led to a significant cluster surface density reduction down to 1.15x104 µm-2. The injection of HCl caused an increase in the Ge concentration from 19.7% up to 28.9% and a non-lattice-matched growth. A Cyclic Deposition Etch (CDE) process resulted in no [C]Int reduction, but significantly reduced the cluster surface density down to 4.60x104 µm-2. CDE-grown SiGeC was lattice-matched to the Si substrate and yielded a smooth surface with a RMS roughness of 0.22 nm. This enabled the growth of high crystalline quality, thick, lattice-matched layers on a 300 mm Si substrate with material properties beyond pure Si.

Boron Delta-Doping in Si : B Stacks By RP-CVD Epitaxy

Low resistivity materials are required for advanced MOS or equivalent technologies. High boron in-situ doped Si epitaxy is known to create defects that increase the resistivity. Boron delta-doping (Si:B epitaxy alternating with boron saturation layers) is a potential solution to overcome this limitation. Using the delta-doping process at 750 °C in a Reduced Pressure Chemical Vapor Deposition reactor, a resistivity two times lower than that without delta-doping (8.9x10-4 Ω.cm and 1.86x10-3 Ω.cm respectively) was achieved. SIMS characterization measured a total boron concentration of 3.3x1021 at.cm-3. However, the delta-doping processes , as a function of the soaking volume (product of B2H6 flow and saturation time), resulted in low crystal quality and highly stressed layers. Moreover, thin layers were observed by TEM likely due to the formation of the SiBx phase at each saturation layer. For an equivalent soaking volume, a better crystal quality was obtained with a high B2H6 flow and short saturation time.

Opto-electronic responses of large area WSe2 layers synthesized by chemical conversion of WO3 thin films

Atomically thin tungsten diselenide (WSe2) has drawn much interest due to its remarkable optical properties and potential applications in next-generation optoelectronics and energy harvesting devices. High-quality, wafer-scale synthesis of such two-dimensional (2D) semiconductors is necessary for their practical applications. Chemical vapor deposition (CVD) is a promising method for synthesizing large-area thin films of 2D materials where the constituent elements are of widely different vapor pressure. Herein, we demonstrate large-area synthesis of the 2H phase of WSe2 with a precise control over the 2D film thickness. The first step of this process is the deposition of tungsten trioxide (WO3) films of a well-defined thickness by thermal evaporation over large areas. The subsequent selenization of these films in an atmospheric pressure CVD reactor, yields high-quality uniform films of WSe2. The quality of these films is ascertained by measuring their characteristic Raman active vibrational modes and layer thickness dependent optical absorption and photoluminescence. The photoconductivity (PC) of these films has been measured with 405, 532 and 915 nm laser excitation. We note an increase in the PC of the films with their thickness. The best photoresponsivity and detectivity obtained are 11.3 mA/W and 1.42 × 108 Jones respectively. These results are promising to create photo-transistor arrays over large areas using such WO3 processed films.

High-Yield WS2 Synthesis through Sulfurization in Custom-Modified Atmospheric Pressure Chemical Vapor Deposition Reactor, Paving the Way for Selective NH3 Vapor Detection.

Nanostructured transition metal dichalcogenides have garnered significant research interest for physical and chemical sensing applications due to their unique crystal structure and large effective surface area. However, the high-yield synthesis of these materials on different substrates and in nanostructured films remains a challenge that hinders their real-world applications. In this work, we demonstrate the synthesis of two-dimensional (2D) tungsten disulfide (WS2) sheets on a hundred-milligram scale by sulfurization of tungsten trioxide (WO3) powder in an atmospheric pressure chemical vapor deposition reactor. The as-synthesized WS2 powders can be formulated into inks and deposited on a broad range of substrates using techniques like screen or inkjet printing, spin-coating, drop-casting, or airbrushing. Structural, morphological, and chemical composition analysis confirm the successful synthesis of edge-enriched WS2 sheets. The sensing performance of the WS2 films prepared with the synthesized 2D material was evaluated for ammonia (NH3) detection at different operating temperatures. The results reveal exceptional gas sensing responses, with the sensors showing a 100% response toward 5 ppm of NH3 at 150 °C. The sensor detection limit was experimentally verified to be below 1 ppm of NH3 at 150 °C. Selectivity tests demonstrated the high selectivity of the edge-enriched WS2 films toward NH3 in the presence of interfering gases like CO, benzene, H2, and NO2. Furthermore, the sensors displayed remarkable stability against high levels of humidity, with only a slight decrease in response from 100% in dry air to 93% in humid environments. Density functional theory and Bayesian optimization simulations were performed, and the theoretical results agree with the experimental findings, revealing that the interaction between gas molecules and WS2 is primarily based on physisorption.

Development of GeSn epitaxial films with strong direct bandgap luminescence in the mid-wave infrared region using a commercial chemical vapor deposition reactor

Germanium tin (GeSn) is a material of interest for electronic and photonic device applications, but its development and commercialization have been limited by material quality issues and lack of availability from epitaxy suppliers. In this paper, we report initial studies in optimizing GeSn films deposited on a Ge buffer layer grown on 200-mm diameter silicon (Si) substrates with an ASM Epsilon 2000 chemical vapor deposition reactor designed for commercial production. Using a single-step growth process, a Sn content up to 22% near the surface of a GeSn film was achieved due to the increase in Sn incorporation via strain relaxation. A two-step growth process resulted in a bilayer structure with a nearly 100% relaxation on the first layer, followed by a higher quality GeSn layer with 18% Sn as evident by a high photoluminescence intensity emitting in the mid-wave infrared region at 3.2 μm at 20 K.

(Dielectric Science & Technology Thomas Callinan Award) Rare-Earth Luminescence in Silicon-Based Thin Film Structures

For Si-based materials to be used in solid-state lighting and silicon photonics schemes it is necessary to have precise control of the optical emission from these materials. This can be accomplished using rare earth dopants such as Ce, Tb, and Eu to obtain blue, green, and red emissions, respectively. In this talk, we first will provide a review of our work in this field and then focus on Eu-doped films, which are particularly attractive for silicon photonic applications due to their intense emission in the visible spectral region [1]. We will also discuss the benefits of introducing a novel hybrid radio frequency (RF) magnetron sputtering source in the electron cyclotron resonance (ECR) plasma enhanced chemical vapour deposition (PECVD) reactor chamber [2], using the example of Tb-doped SiON films [3]. This approach contrasts with traditional doping methods which use metal-organic precursors or ion implantation to introduce rare-earth dopant species into the host matrix.[1] F. Azmi et al., “Tunable Emission from Eu:SiOxNy Thin Films Prepared by Integrated Magnetron Sputtering and Plasma Enhanced Chemical Vapor Deposition”, J. Vac. Sci. Technol. A 40, 043402 (2022); DOI: 10.1116/6.0001761[2] J.W. Miller et al., “Integrated ECR-PECVD and Magnetron Sputtering System for Rare-Earth-Doped Si-Based Materials”, Surface and Coatings Technology 336, 99 (2018); DOI: 10.1016/j.surfcoat.2017.08.051[3] Z. Khatami et al., "A comprehensive calibration of integrated magnetron sputtering and plasma enhanced chemical vapor deposition for rare-earth doped thin films", J. Mater. Res. (2023); DOI: 10.1557/s43578-023-01207-2

Influence of high-temperature thermal annealing on paramagnetic point defects in silicon-rich silicon nitride films formed in a single-wafer-type low-pressure chemical vapor deposition reactor

The influence of high-temperature thermal annealing on silicon dangling bonds called K centers in Si-rich silicon nitride films grown in a single-wafer-type low-pressure chemical vapor deposition reactor with the SiH2Cl2-NH3 system at 750 °C has been investigated by combining thermal desorption spectroscopy (TDS), Fourier transform infrared spectroscopy-attenuated total reflection, spectroscopic ellipsometry, and electron spin resonance. In the TDS analysis, H2 desorption from the nitride films was detected above about 600 °C. It is found that thermal annealing at 750 and 900 °C caused a slight decrease in the K center density and a change in the g value of K centers, which are considered to be caused by changes in the atomic structure of the nitride films. On the other hand, thermal annealing at 1050 °C resulted in a substantial decrease in the K center density and the generation of paramagnetic defects with unprecedented characteristics. The findings in this study are expected to provide important guidelines for the design of manufacturing processes of nonvolatile memories.

Growth of Carbon Nanofibers and Carbon Nanotubes by Chemical Vapour Deposition on Half-Heusler Alloys: A Computationally Driven Experimental Investigation.

The possibility of directly growing carbon nanofibers (CNFs) and carbon nanotubes (CNTs) on half-Heusler alloys by Chemical Vapour Deposition (CVD) is investigated for the first time, without using additional catalysts, since the half-Heusler alloys per se may function as catalytic substrates, according to the findings of the current study. As a carbon source, acetylene is used in the temperature range of 700-750 °C. The n-type half-Heusler compound Zr0.4Ti0.60.33Ni0.33Sn0.98Sb0.020.33 is utilized as the catalytic substrate. At first, a computational model is developed for the CVD reactor, aiming to optimize the experimental process design and setup. The experimental process conditions are simulated to investigate the reactive species concentrations within the reactor chamber and the activation of certain reactions. SEM analysis confirms the growth of CNFs with diameters ranging from 450 nm to 1 μm. Raman spectroscopy implies that the formed carbon structures resemble CNFs rather than CNTs, and that amorphous carbon also co-exists in the deposited samples. From the characterization results, it may be concluded that a short reaction time and a low acetylene flow rate lead to the formation of a uniform CNF coating on the surface of half-Heusler alloys. The purpose of depositing carbon nanostructures onto half-Heusler alloys is to improve the current transfer, generated from these thermoelectric compounds, by forming a conductive coating on their surface.

Spatial and Chemical Dual Nano‐Confined Ultrastable Perovskite Quantum Dots Glass Manifesting Exciton Modulation

AbstractNano‐confined synthesis of perovskite quantum dots (QDs) in solid matrix is emerging as a promising route to solve their long‐standing stability problem. Utilizing sol‐gel derived nanoporous glass as matrix that has high flexibility in chemical composition and pore size, a novel spatial and chemical dual nano‐confined strategy is presented for the synthesis of ultrastable perovskite QDs with tunable composition and bandgap in glass. The findings reveal that the Pb─O bonding is formed at perovskite QDs/glass interface during a nano‐confined chemical vapor deposition (CVD) reaction. In particular, the presence of interfacial chemical bonding is discovered to be critical for passivating surface traps and stabilizing the perovskite QDs during the final densification process (related photoluminescence intensity maintained ≈100% after immersed in aqueous solution for 30 days). Series optical spectroscopy unravels the exciton modulation (80 meV) of perovskite QDs in nanoporous and densified glass related to the unique combination of dual physical and chemistry nano‐confined effect. By shedding light on the nano‐confined growth of functional nanocrystals, the research offers the key paths for fabricating high‐performance perovskite devices.

Formation of Diamond Films with Different Grain Sizes on TiO2 Nanotubes and Its Field Emission Properties

Diamond films with different grain sizes are deposited on TiO2 nanotube (TNT) arrays prepared by anodic oxidation using a microwave plasma chemical vapor deposition reactor. The scanning electron microscope, X‐Ray diffractometer, and Raman results indicate that the diamond film is successfully deposited and that the substrate undergoes a phase transition due to the diamond deposition temperature, resulting in the rutile phase becoming dominant with lower energy bandgap and work function. Notably, after 5 h of deposition, a relatively continuous microcrystalline film is formed on the TNTs, and the diamond grains change from spherical to pyramidal and show excellent electron field emission behavior, with a low turn‐on field of 0.5 V μm−1 and a current density of 85.9 μA cm−2. In addition, the deposition environment of the nanocrystalline diamond has a large impact on the substrate morphology, resulting in a blocked electron transport path, which reduces the overall field emission performance. The enhanced performance is attributed to the synergistic effect between the highly efficient 1D electron path of the TNTs, the negative electron affinity of the diamond surface, and the lower work function of rutile TiO2.

Estimation of Junction Temperature in Single 228 nm‐Band AlGaN Far‐Ultraviolet‐C Light‐Emitting Diode on c‐Sapphire Having 1.8 mW Power and 0.32% External Quantum Efficiency

The increasing resistance of methicillin‐resistant Staphylococcusaureus to antibiotics is a major challenge faced by mankind in thehistory of medical science and according to United Nations, 700‐000 patients worldwide die every year from an infection with multidrug‐resistant organisms (MROs). Aluminum gallium nitride‐based 228 nm Far‐ultraviolet‐C (Far‐UVC) lightsources can be safely used as a germicidal application in both manned as wellas in unmanned environments against these MROs. Previously, the 228 nm Far‐UVC light‐emitting diode (LED) with emission power of 1 mW was reported by ourgroup, however, the value of external quantum efficiency (EQE) was not reportedusing conventional thick Ni (20 nm)/Au (100 nm) p‐electrode. Herein, animproved Far‐UVC LED on c‐Sapphire is attempted using a special technique in SR4000 type of metal‐organic chemical vapor deposition reactor to control the Al composition in n‐AlGaN buffer and across the 2 inch‐wafer. As a result, the light emission power of 1.8 mW and EQE of 0.32% in 228 nm Far‐UVC LED aresuccessfully achieved using very thin p‐electrode (Ni/Au). However, arelatively high junction temperature of ≈100°C around thejunction of Far‐UVC LED is observed. Finally, some simple heat‐sink modules forheat dissipation of Far‐UVC LED panel with light power of 30 mW are implemented.

Effects of CaCO3/MgO on Fe-Co-Mo catalyst in the reprocessing of recycled polypropylene to carbon nanotubes

In recent times, there has been a global discourse on the menace of plastic waste (PW) materials on the ecosystem and ways for effective management of PW. This has resulted in the utilization of PW in the research arena in the synthesis of smart nanomaterials of high value as a sustainable solution. In this study, the catalytic-pyrolysis procedure was used to develop carbon nanotubes (CNTs) from recycled polypropylene (PP) plastic in a one-step chemical vapour deposition (CVD) reactor. The impacts of CaCO3 and MgO as supports for Fe-Co-Mo catalysts in the production of CNTs were studied. Kinetic and thermodynamic parameters were determined from the thermal profile of the catalysts to establish the nature of the reaction in CNTs synthesis. Transmission electron microscopy (TEM), energy Dispersive X-ray (EDX), selected area electron diffraction pattern, particle size distribution (PSD), thermogravimetric analysis (TGA), Raman spectroscopy, Fourier transforms infrared (FTIR) and X-ray diffraction (XRD) were employed to characterize the catalysts and CNTs. The results obtained showed the impact of the supports on the yield, quality, and morphology of the synthesized CNTs. The CNTs yield from catalysts supported with CaCO3 and MgO were 35.12 % and 37.24% respectively. The average outer diameters of CNTs produced over the catalyst with CaCO3 and MgO supports were 36 and 29 nm respectively. The ID/IG ratio for CaCO3 and MgO supports were 0.6724 and 0.8401 respectively. The change in entropy for all phases were −274.41 and −1032.97 J/mol/K and −213.0, −318.48 and −1022.13 J/mol/K for CaCO3 and MgO supported catalyst respectively which confirmed non-spontaneous endothermic reaction. It was observed that MgO support showed better catalytic activity toward CNTs growth in terms of yield while those with CaCO3 support showed higher graphitization.

Towards a mechanistic understanding of the floating catalyst CVD of CNTs: Interplay between catalyst particle nucleation, growth and deactivation

The chemical vapor deposition (CVD) of carbon nanotubes (CNTs) with the floating catalyst technique, using ferrocene as catalyst, is computationally investigated from its mechanistic perspective. The present work presents a novel model dealing with the phenomena taking place in the bulk of a floating catalyst CVD reactor. The developed model incorporates the gas flow, heat transfer and species transport phenomena, coupled with reaction mechanisms and kinetics, as well as the catalyst particle formation and growth dynamics. The novelty of the approach lies on the inclusion of carbon species deposition on the catalyst particle surface, which have a crucial effect on the particle growth and catalyst deactivation, leading to the termination of CNT growth on the particles. The model predictions are directly compared with experimental results from the literature for the same process and for a range of process parameters, showing a very good agreement. The computational model not only successfully predicts the experimental behavior but also reveals the effect of individual mechanisms on the inhibition of particle growth, catalyst deactivation and CNT growth. In this way, the model provides an in-depth mechanistic understanding of the mechanisms in the reactor bulk, which is currently missing, thus paving the way towards the knowledge-based process design and optimization and the possibility of using more sustainable or environmentally-friendly precursors and catalysts which have not been studied experimentally in detail.

Research on the Influence of Carbon Sources and Buffer Layers on the Homogeneous Epitaxial Growth of 4H-SiC.

In this study, a 4H-SiC homoepitaxial layer was grown on a 150 mm 4° off-axis substrate using a horizontal hot wall chemical vapor deposition reactor. Comparing C3H8 and C2H4 as C sources, the sample grown with C2H4 exhibited a slower growth rate and lower doping concentration, but superior uniformity and surface roughness compared to the C3H8-grown sample. Hence, C2H4 is deemed more suitable for commercial epitaxial wafer growth. Increasing growth pressure led to decreased growth rate, worsened thickness uniformity, reduced doping concentration, deteriorated uniformity, and initially improved and then worsened surface roughness. Optimal growth quality was observed at a lower growth pressure of 40 Torr. Furthermore, the impact of buffer layer growth on epitaxial quality varied significantly based on different C/Si ratios, emphasizing the importance of selecting the appropriate conditions for subsequent device manufacturing.

Synthesis and growth mechanism of silicon-based nanostructures from polysiloxane via CVD process

The work is concerned with the deposition of ceramic layers of various morphologies, containing silicon and nitrogen, from a polysiloxane precursor in the chemical vapor deposition (CVD) process. The experiments involved the saturation of nitrogen as a gaseous carrier with polysiloxane molecules in the CVD reaction. Saturated nitrogen was supplied to the reaction zone and depending on the synthesis temperature (1000–1800 °C) and the concentration of resin in gas phase, various nanocrystalline and amorphous deposits were obtained on graphite foil, including polygranulated SiOC powders, fibrous layers composed of nanofibers (NFs) containing silicon and nitrogen, nanochains and composite fibrous components. The morphology, structure and chemical composition of the deposits formed in the CVD reaction changed with increasing temperature. Above 1300 °C, oxygen in the silicon oxycarbide deposits was gradually replaced by nitrogen, creating SiN bonds. The dominant phase in the deposits obtained in the temperature range of 1700–1800 °C were two-phase silicon oxynitride NFs. The core of these NFs consisted of a polycrystalline structure surrounded by an amorphous shell. These structures grew preferentially in the [111] direction through heterogeneous nucleation in the vapor-solid process (VS). The changes in deposits morphology were influenced by the CVD temperature and the resin content in the gas carrier. The activation energy of the crystallization process of silicon oxynitride nanofibers was approximately 96 kJ/mol.