Chemical Vapor Deposition Process Research Articles

CO2 plasma inducing steel-slag with active sites for efficient growth of carbon nanotubes for the high-performance microwave absorption

As a solid waste generated in the metallurgical process, the highly efficient catalysis of steel-slag for carbon nanotube (CNT) growth remains a huge challenge. Herein, a CO2 plasma-inducing approach for modifying the steel-slag catalyst with rich active sites was developed for CNT growth in the chemical vapor deposition (CVD) process. Furthermore, the high-energy CO2 plasma refines the particles on the steel-slag surface, reducing the particle size on the surface of steel-slag effectively increasing the active sites of the catalyst. In addition, the thermal effect generated by the gas molecule ionization process under CO2 increases the background temperature of the steel-slag, and the interaction between the oxygen-active substances produced and the iron oxide on the surface of steel-slag undergoes an oxidation reaction upon full contact with high-energy particles, which greatly improves the catalytic efficiency of the steel-slag as a catalyst for CNT, and increases the catalytic efficiency by 50 % compared with the non-plasma modified steel-slag as a catalyst for catalyzing CNTs. In addition, catalytically grown CNTs encapsulate magnetic steel-slag catalysts to form a three-dimensional CNT network structure, with high-performance electromagnetic wave absorption. The composite absorbing material with a thickness of only 3.55 mm has a minimum absorption rate of −64.08 dB for electromagnetic waves at a frequency of 7.9 GHz. The dielectric and the magnetic loss of steel-slag lead to enhanced electromagnetic wave absorption. Therefore, this study provides an inexpensive and environmentally friendly idea for the design of high-efficiency CNT growth and solid waste catalyst modification synthesized with high-performance absorbers.

Multiscale Models of CVD Process: Review and Prospective.

Chemical vapor deposition (CVD) is a crucial technique in the preparation of high-quality thin films and coatings, and is widely used in various industries including semiconductor, optics, and nuclear fuel, due to its operation simplicity and high growth rate. The complexity of the CVD process arises from numerous parameters, such as precursor chemistry, temperature, pressure, gas flow dynamics, and substrate characteristics. These multiscale parameters make the optimization of the CVD process a challenging task. Numerical simulations are widely used to model and analyze the CVD complex systems, and can be divided into nanoscale, mesoscale, and macroscale methods. Numerical simulation is aimed at optimizing the CVD process, but the inter-scale parameters still need to be extracted in modeling processes. However, multiscale coupling modeling becomes a powerful method to solve these challenges by providing a comprehensive framework that integrates phenomena occurring at different scales. This review presents an overview of the CVD process, the common critical parameters, and an in-depth analysis of CVD models in different scales. Then various multiscale models are discussed. This review highlights the models in different scales, integrates these models into multiscale frameworks, discusses typical multiscale coupling CVD models applied in practice, and summarizes the parameters that can transfer information between different scales. Finally, the schemes of multiscale coupling are given as a prospective view. By offering a comprehensive view of the current state of multiscale CVD models, this review aims to bridge the gap between theory and practice, and provide insights that could lead to a more efficient and precise control of the CVD process.

Flexible All-Carbon Nanoarchitecture Built from In Situ Formation of Nanoporous Graphene Within "Skeletal-Capillary" Carbon Nanotube Networks for Supercapacitors.

It is difficult for carbonaceous materials to combine a large specific surface area with flexibility. Here, a flexible all-carbon nanoarchitecture based on the in situ growth of nanoporous graphene within "skeletal-capillary" carbon nanotube (CNT) networks has been achieved by a chemical vapor deposition (CVD) process. Multi-path long-range conductivity is established, and the porous graphene provides a large specific surface area for charge storage. The flexibility of the films allows them to be directly used as binder-free electrodes for supercapacitors. Since the polymeric binders are saved, the supercapacitors exhibit a higher overall storage density.

Toward crack-free AlN growth on silicon (111) by introducing boron incorporated buffer layer via MOCVD

High-quality aluminum nitride (AlN) films on silicon substrates are crucial for various applications due to their inherent properties as wide-bandgap semiconductors, cost-effectiveness, and compatibility with silicon-based circuits. Nonetheless, producing high-quality and crack-free AlN on silicon presents significant challenges due to the stress caused by lattice and thermal expansion mismatches. This study introduces a method to mitigate these challenges by incorporating a boron precursor during the metalorganic chemical vapor deposition process to form a BAlN buffer layer. Analytical techniques, such as secondary ion mass spectrometry, atomic force microscopy imaging, XRD rocking curves, reciprocal space map, and Raman spectroscopy, indicate that the BAlN buffer layer promotes the enlargement of seed crystal size, which effectively delays AlN coalescence, mitigates accumulated tensile stress, and enhances the overall crystal quality. Employing this technique has produced a 520 nm thick, crack-free AlN film on silicon (111) with high crystal quality, achieving full width at half maximum values of only 0.2° and 0.3° for XRC (002) and (102), respectively.

Dielectric behavior and defects of nitrogen-containing single crystal diamond films

Single crystal diamond (SCD) film, as a new substrate material, has attracted growing attention because of its low dielectric loss. The nitrogen was usually introduced into microwave plasma chemical vapor deposition (MPCVD) process in order to enhance the growth rate of SCD films. So SCD films with nitrogen were prepared by MPCVD compared with the undoped film. The impurities and defects of diamond films were characterized by Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR) and photoluminescence spectroscopy (PL). The dielectric behavior of SCD films was measured using the LCR measurement in the frequency range of 1 kHz to 110 MHz. The results indicate that the primary dielectric loss in SCD films is conductivity loss and space charge polarization below 1 MHz, while the main dielectric loss is dipole orientation polarization and electronic relaxation polarization in the frequency range of 1 MHz to 110 MHz. Point defects like substitutional N+, NV− and SiV− exert a significant influence on polarization loss. This is essential to improve the growth of SCD with excellent dielectric properties.

Autoregressive distributed lag-based dynamic uniformity modeling and monitoring approaches for superconductor manufacturing

ABSTRACT High-temperature superconductors (HTS), known for their high efficiency and low energy loss, have found profound applications across various fields, driving the demand for long, uniformly performing tapes. However, ensuring uniform performance over extended lengths of HTS tapes, often characterized by the consistency of critical current, remains challenging due to fluctuations in growth conditions during manufacturing. To elucidate the mechanisms underlying variations in tape uniformity and enable real-time monitoring of associated parameters, we propose an Autoregressive Distributed Lag (ADL)-based Dynamic Uniformity Modeling and Monitoring (ADUM2) approach. This method integrates uniformity measurement, the identification of critical process parameters and real-time monitoring within the manufacturing process. The ADUM2 approach is applied to the advanced metal organic chemical vapor deposition (A-MOCVD) process, a pilot-scale method for superconductor manufacturing. Our model demonstrates superior performance compared to benchmark methods, accounting for over 80% of the total variance in the data and identifying 13 key process parameters influencing the uniformity of HTS tapes. This study offers significant insights into the high-temperature superconductor manufacturing process and holds the potential to facilitate the production of cost-effective, uniformly performing long superconducting tapes in the future.

Growth of single crystalline GeSn alloy epilayer on Gd2O3/Si (111) engineered insulating substrate using RF sputtering and solid phase epitaxy

The article showcases a low-cost, low-temperature deposition andHVMtechnique to develop single crystalline GeSn alloy epilayers on Gd2O3/Si (111) substrate. First, GeSn alloy amorphous layer is deposited on the insulating substrates using an Radio Frequency (RF) sputtering apparatus. Subsequently, an inductively coupled plasma-assisted chemical vapor deposition (ICP-CVD) process is used to deposit a SiO2 capping layer to protect against Sn out-diffusion during heat treatment. The samples are then subjected to solid phase epitaxy (SPE) at 450 °C, 550 °C, and 650 °C. Sample processed for SPE at 450 °C has weak crystallinity and only shows Type-A stacking. Those processed for SPE at 550 °C and 650 °C, on the other hand, have revealed formation of the single-crystalline GeSn alloy epilayer with Type-A and Type-B stacking. However, SPE at 650 °C revealed tin out-diffusion and segregation effects. This work is significant for enabling the preparation of high-Sn-content GeSn alloy epilayers on insulating Gd2O3/Si (111) substrates, as it requires the initial deposition of a GeSn amorphous alloy epilayer using RF sputtering. This advancement promises benefits which includes advantages such as lower operating voltage, reduced leakage current, and minimized parasitic and short-channel effects, making it ideal for advancing RF technology.

The Corrosion Characteristics of Graphite Coatings on Nickel Foam and Their Applications in High-Temperature Proton Exchange Membrane Fuel Cells

This study investigates the effectiveness of graphite coatings on nickel foam for use in high-temperature proton exchange membrane fuel cells (HT-PEMFCs). Nickel foam, known for its high porosity and good conductivity, serves as an advantageous alternative to traditional flow channels but faces corrosion challenges in HT-PEMFCs, especially from phosphoric acid leakage. Graphite coatings are used as the protection layer and compared with nitride coatings. Chemical vapor deposition process parameters are first optimized for graphite growth. Corrosion polarization curves are then measured using a high-temperature phosphoric acid three-electrode system simulating HT-PEMFC conditions, followed by an analysis of the surface morphology of the samples. Subsequently, the performance and durability of the nickel foams with different coatings are evaluated after being assembled in single fuel cells. The results highlight the superior corrosion resistance of graphite coating under HT-PEMFC conditions, demonstrating its performance over other coatings. Graphite-coated foams showed a significant reduction in corrosion current, approximately 58% lower than uncoated foams and 21% lower than the TiN coated foams. In practical applications, an HT-PEMFC single cell with graphite-coated nickel foam demonstrated a current density of 763 mA/cm2 at 0.6 V under conditions of 180 oC and 2 atm H2/air. The current density is 40% higher than that of the uncoated nickel foam. The results show notable long-term durability under constant current holding tests at 160 oC. The voltage decay rate in the graphite-coated cell was 48% lower compared to the cell with uncoated nickel forms.

Molecular Transformations for Direct Synthesis of Thorium Dioxide Films

New Th(IV) complexes with high volatility were synthesized and applied as molecular single‐source precursors for chemical vapor deposition (CVD) of ThO2 thin films. The change in the steric profile of alkoxide ligands and concomitant reduction in the molecular weight of [Th(L)2(OR)2] (1‐OR, R = iso‐propyl (1‐OiPr) or tert‐butyl (1‐OtBu), L = N‐(4,4,4‐trifluorobut‐1‐ene‐3‐one)‐methoxyethylamide)) had a profound effect on the vapor pressure (at 10‐5 mbar) evident in the drop in sublimation temperature to 100 °C for the iso‐propoxide derivative against 130 °C observed for the tert‐(1‐OtBu). Hirshfeld surface analysis of both complexes showed different degrees of intermolecular H⋅⋅⋅F interactions responsible for the observed differences in the volatilities of the two complexes. Both mixed‐ligand compounds (1‐OiPr, 1‐OtBu) were applied in the CVD process to deposit thorium oxide thin films without any carrier or reactive gas that verified their suitability as single‐source precursors to ThO2 coatings. Thin films of ThO2 were grown at 500 °C and 600 °C on Si/SiO2 substrates, which showed presence of C, N, and F presumably originating from the incorporation of ligand fragments in the growing CVD deposits. Subsequent calcination of CVD‐grown ThO2 films at 800 °C in air led to phase pure ThO2 coatings with uniform morphology.

Fluidized Bed Chemical Vapor Deposition of Copper on Micronic Alumina Powders

AbstractUniformly coating micronic particles with metals is of main interest for a broad range of applications. This study demonstrates the feasibility of depositing pure copper on the surface of micronic alumina particles by the fluidized bed chemical vapor deposition process from the cheap and nontoxic copper acetylacetonate precursor. Thanks to the development of a preconditioning protocol, a complete fluidization of the particles organized as porous agglomerates was reached. The coating of the individual particles was favored by using conditions involving low deposition rates. The influence of key operating parameters on the process behavior and on the characteristics of the deposit was studied. The deposited copper was of cubic crystal structure without carbon nor oxide contamination.

Integration of carbon microsheets and helical carbon nanocoils for efficient microwave absorption

The integration of multi-dimensional materials is a powerful approach for the construction of high-performance microwave absorbers. In this work, 2D-like carbon microsheets (CMSs) have been directly synthesized on the surfaces of 3D helical carbon nanocoils (CNCs) through a Cu catalyzed chemical vapor deposition process. The junctions formed between CMSs and CNCs create numerous polarization sites, which enhances interfacial polarization. The planar morphology of CMSs is beneficial to enhance the multiple scattering of microwave, while the 3D helical CNCs prevent the aggregation of 2D-like CMSs and simultaneously enhance the conductive loss and cross-polarization loss. By controlling the growth time, the morphologies of CMS are precisely tailored and their impedance matching is adjusted. Consequently, CMS/CNC demonstrates exceptional microwave absorption (MA) performance with a broad effective bandwidth of 6.5 GHz and a minimum reflection loss of −39.3 dB at a remarkably low filling ratio of 4 wt%. This study provides a novel multi-dimensional integrated structure for efficient MA.

A first-principles investigation into the adsorption behavior and deposition mechanism of boron-containing gases on Si(100) surfaces during chemical vapor deposition

Polysilicon serves as a primary raw material in the production of solar cells and semiconductors. However, its impurity content, particularly boron, poses significant challenges during the chemical vapor deposition (CVD) process. Therefore, it is essential to investigate the behavior of boron impurities during CVD. In this study, we conducted first-principles calculations to explore the adsorption behavior and deposition mechanism of boron-containing gases (BCl3, BHCl2, B2H6) on the Si(100) surface. We considered different adsorption sites and performed a systematic analysis of various adsorption systems' adsorption energy, charge transfer, and electronic properties. Our findings indicate that BCl3, BHCl2, and B2H6 molecules undergo dissociative chemisorption at specific adsorption sites. Moreover, charge transfer analysis confirms that each of these adsorbed molecules functions as an electron acceptor. Subsequent analyses, including total charge density (TCD), charge density difference (CDD), total density of states (TDOS), and projected density of states (PDOS), collectively underscore the robust electronic interactions between the gaseous molecules and the Si(100) surface. Through the computation of transition states and energy barriers across three potential reaction pathways, we identify a predominant sequence: BCl3→BCl2+Cl→BCl+Cl→B+Cl, that governs boron impurity formation on the Si(100) surface during CVD. Our work elucidates the underlying microscopic mechanisms of boron-containing gas adsorption and deposition in the CVD context.

Impact of Diamond-like Carbon Films on Reverse Torque: Superior Performance in Implant Abutments with Internal Conical Connections

The loosening or fracture of the prosthetic abutment screw is the most frequently reported complication in implant dentistry. Thin diamond-like carbon (DLC) films offer a low friction coefficient and high wear resistance, functioning as a solid lubricant to prevent the weakening of the implant–abutment system. This study evaluated the effects of DLC nanofilms on the reverse torque of prosthetic abutments after simulated chewing. Abutments with 8° and 11° taper connections, with and without DLC or silver-doped DLC coatings, were tested. The films were deposited through the plasma enhanced chemical vapor deposition process. After two million cycles of mechanical loading, reverse torque was measured. Analyses with scanning electron microscopy were conducted on three samples of each group before and after mechanical cycling to verify the adaptation of the abutments. Tribology, Raman and energy-dispersive spectroscopy analyses were performed. All groups showed a reduction in insertion torque, except the DLC-coated 8° abutments, which demonstrated increased reverse torque. The 11° taper groups experienced the most torque loss. The nanofilm had no significant effect on maintaining insertion torque, except for the DLC8 group, which showed improved performance.

Integrating supervised and unsupervised learning approaches to unveil critical process inputs

This study introduces a machine learning framework tailored to large-scale industrial processes characterized by a plethora of numerical and categorical inputs. The framework aims to (i) discern critical parameters that influence the output and (ii) generate accurate out-of-sample qualitative and quantitative predictions of production outcomes. Specifically, we address the pivotal question of the significance of each input in shaping the process outcome, using an industrial Chemical Vapor Deposition (CVD) process as an example. The initial objective involves merging subject matter expertise and clustering techniques exclusively on the process output, here, coating thickness measurements at various positions in the reactor. This approach identifies groups of production runs that share similar qualitative characteristics, such as film mean thickness and standard deviation. In particular, the differences of the outcomes represented by the different clusters can be attributed to differences in specific inputs, indicating that these inputs are potentially critical to the production outcome. Shapley value analysis corroborates the formed hypotheses. Leveraging this insight, we subsequently implement supervised classification and regression methods using the identified critical process inputs. The proposed methodology proves to be valuable in scenarios with a multitude of inputs and insufficient data for the direct application of deep learning techniques, providing meaningful insights into the underlying processes.

Galling-Free Forging of Titanium Using Carbon-Supersaturated SiC Coating Dies

The thermal chemical vapor deposition (CVD) process was utilized to fabricate 6H-structured SiC coating dies with carbon control. The carbon-rich clusters along the SiC grain boundaries acted as a pinning site to suppress irregular crystal growth and to homogenize the fine-grained structure. These massive carbon-supersaturated (MCSed) SiC dies with a thickness of 4 mm were utilized for upsetting pure titanium bars in dry and cold conditions. Under a stress gradient from the contact interface to the depth of the SiC coating, the carbon solute isolated from these carbon clusters diffused through the grain boundaries and formed free carbon agglomerates on the contact interface to the pure titanium bars. These in situ-formed free carbon agglomerates acted as a solid lubricant to sustain the friction coefficient at 0.09 at the hot spots on the contact interface and to protect the dies and bars from severe adhesive wearing.

Influence of the Acetylene Flow Rate and Process Pressure on the Carbon Deposition Behavior by Thermal Chemical Vapor Deposition Process

We used the chemical vapor deposition process to deposit carbon film at a high temperature (900 °C). The carbon films were deposited on AISI 1006 foils using an acetylene gas. We analyzed the carbon film deposited on the surface using Raman spectroscopy, scanning electron microscopy, and high-resolution transmission electron microscopy to define changes in the bonding structure of the carbon film. The results of Raman spectroscopy and high-resolution transmission electron microscopy revealed that as the acetylene flow rate increased, the shape of the deposited carbon film changed from graphene to graphite. In addition, in order to compare the quality of the carbon film in terms of mechanical and electrical properties, carbon films treated under various conditions were closely analyzed using nano-indenter and a sheet resistance meter. Therefore, the optimal condition (1 Torr-50 sccm) was selected in which graphene was uniformly deposited and had the lowest electrical resistance (500 Ω/sq) and highest hardness (12 GPa).

Superhydrophobic Stainless Steel Mesh through Chemical Vapour Deposition of TMCS for Effective Oil-Water Separation

Aim: To Fabricate the superhydrophobic Stainless Steel (SS) mesh using Trimethylchlorosilane (TMCS) through a Chemical Vapor Deposition (CVD) method for the oil-water mixture separation Background: The frequent oil spills have a devastating impact on marine ecosystems and the environment. The porous materials with superhydrophobic properties have been created to separate oil and water effectively. Due to their ability to effectively separate oil and water, superhydrophobic coatings have gained significant attention. Methods: The cleaned stainless-steel mesh was put on a stand and covered with a glass container. Within the container, 50 mL of hexane, which contained 1 mL of TMCS, was added. The mesh was then left for 3 h to undergo the CVD process Results: The silane content with low surface energy creates a highly rough structure on the mesh surface. The optimal mesh coating is superhydrophobic, having a strong affinity to oil and a water contact angle of 162 ± 2°. The coated mesh has shown a separation efficiency of over 97.8% for different oil-water mixtures. The coatings sustain their superhydrophobicity up to 30 tape peels and 40 times sandpaper abrasion, indicating good mechanical durability. Conclusion: The study concludes that the S-3 sample is mechanically stable and can withstand various tests such as adhesive tape peeling, sandpaper abrasion, bending, folding, and twisting. It efficiently separates oil and water mixtures on a large scale with high efficacy

Preparation and loss analysis of Ge on Si SWIR optical strip waveguides

On-chip integrated photonics with operating wavelength at short-wave infrared region is becoming popular for its potential advantages in extending the telecommunication bandwidth and the application in gas sensing. As an important component of integrated optoelectronic chips, high-performance waveguides have attracted widespread attention. In this work, high-performance Ge waveguides were designed and fabricated on the Ge-on-Si platform, in which germanium films were epitaxially grown by the chemical vapor deposition process. The propagation loss for the waveguide was measured to be 2.34 dB/cm at the wavelength of 2 μm through the cut-back method. The quantitative relationship between the waveguide propagation loss and sidewall roughness as well as material defect density was established by introducing an empirical coefficient m. The m value was calculated to be 3.8 × 10−4 dB for the waveguide with a fixed Ge thickness of 1.5 μm by fitting the experimental propagation loss data at an operating wavelength of 2 μm. This formula provides a significant reference for future design of waveguide dimension structures, where defect induced absorption loss is non-negligible.

IFN-γ and IL-10 Immunosensor with Vertically Aligned Carbon Nanotube Interdigitated Electrodes toward Pen-Side Cattle Paratuberculosis Monitoring.

Highly sensitive vertically aligned carbon nanotube arrays (VANTAs) interdigitated electrode (IDE) arrays are developed for electrochemical biosensing of two cytokines (i.e., interleukin-10 (IL-10) and interferon-gamma (IFN-γ)) that are useful for early detection Johne's disease (Bovine Paratuberculosis) in cattle. The high aspect ratio VANTA-IDEs (50-60µm in height) are grown through a chemical vapor deposition process from an iron (Fe) catalyst that is lithographically patterned on a silicon wafer with equal finger width and inter-finger spacing of 25µm. After functionalization with distinct antibodies the VANTA-IDEs are capable of selective detection of both IL-10 and IFN-γ within an actual biological matrix (i.e., diluted bovine implant supernatant) over concentration ranges of 0.1 to 30 pgmL-1 (limit of detection - LOD: 0.0911 pgmL-1) and 50-500 pgmL-1 (LOD: 24.17 pgmL-1), respectively with a response time of <35 min. Results demonstrate important initial steps for rapid, pen-side identification of cattle with stage-I Mycobacterium avium subspecies paratuberculosis infection before physical symptoms of Johne's disease are present. Such a rapid pen-side diagnostic test can be used on cattle at an auction or before they are introduced to a herd to ensure the larger population does not become infected with Johne's disease.

Exploring joining techniques for diamond chips on metallized substrates: Micro- and nano-scale mechanical testing approach

This paper aims to comprehensively evaluate the shear strength of various junctions between diamond chips and double copper bonded ceramic substrates. The study involves several stages, beginning with the deposition of Ti/Ni/Ag metallization system on diamond chips using a chemical vapor deposition (CVD) process. These metallization systems are selected to determine their suitability as ohmic contacts on diamond. In parallel, Ni/Au and Ni/Ag layers are electroplated onto the thick copper metallization of the ceramic substrate. Following these depositions, junctions are created for both Cu/Cu and C/Cu assemblies using different techniques: reflow process for AuGe solder joints, reflow-diffusion process for Ag-In joints, and a thermomechanical process for Ag nanoparticle joints. To assess the effectiveness of these techniques, the shear strength of the junctions is measured using a micro-shear test, which is analogous to a classical micro-scratching test. Additionally, the mechanical behaviors of the layers adjacent to the assemblies are analyzed through nano-indentation tests. Finally, the fracture surfaces are examined using scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX) spectrometry to identify the microstructure and damage modes. The work described in the paper exhibits several innovative aspects. It introduces the novel combination of Ti/Ni/Ag metallization system on diamond chips, evaluated for its suitability as ohmic contacts, potentially leading to improved electrical and thermal performance in diamond substrate applications. The study employs diverse junction creation techniques, such as reflow for AuGe solder joints, reflow-diffusion for Ag-In joints, and a thermomechanical process for Ag nanoparticle joints, allowing for a thorough comparison and identification of the most effective method for different scenarios. We have also introduced an integrated testing methodology, which combines micro-shear tests and nano-indentation tests and provides a robust framework for assessing both the shear strength and mechanical properties of the junctions and adjacent layers, enhancing the reliability and depth of the evaluation. The specific focus on metallization system and junctions suitable for diamond, known for its exceptional thermal and electrical properties, positions this work as highly relevant for advanced electronic and thermal management applications.