Chemical Deposition Research Articles

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.

Plasma enhanced chemical vapor deposition (PECVD) of SiOx thin films on Portuguese limestone: An experimental study

Plasma Enhanced Chemical Vapor Deposition (PECVD) of SiOx thin films has been applied to the stone surface under laboratory conditions in order to assess its feasibility as an alternative method for stone protection. SiOx thin layers were deposited on oolitic limestone lithologies known to have been used for the construction and restoration of the Batalha Monastery in Portugal surface by PECVD from tetraethoxysilane (TEOS) as the reaction precursor, in capacitively coupled parallel-plate reactor. The thickness, morphologies and chemical properties of the deposited film were characterized by attenuated total reflectance -Fourier transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM+EDS). Laboratory simulated decay and natural aging tests were implemented to evaluate the protective effect of the deposited micron-size SiOx thin films. Results suggested that, due to the good barrier effect, SiOx films were able to isolate the stones from aggressive acidic solution, thus reducing possible dissolution-related damage. Natural aging tests proved that SiOx thin films were also able to inhibit to a high extent bio-colonization while, at the same time reducing soiling of the stone appearance. Durability and wetting property of this SiOx thin film were preliminarily assessed. This research tested, for the first time, the feasibility of applying micron-size SiOx film quickly and directly via cold plasma deposition and its versatile protection performance on carbonate stone.

Nanoparticle doping as a way to enhance holmium fiber lasers efficiency

Highly-doped holmium fibers have been prepared using modified chemical vapor deposition in combination with nanoparticle-doping method. Within a series of various Al2O3 and Ho3+ concentrations, relations between fibers composition and their fluorescence and laser parameters have been studied. Al/Ho molar ratio equal to at least 50 was found to be the key factor for fibers with outstanding parameters. Fibers with slope efficiency above 80%, laser threshold below 100 mW and fluorescence lifetime up to 1.6 ms have been prepared. Thanks to high Al2O3 concentrations, obtained through nanoparticle doping, we were able to achieve high-performance fibers in a wide range of Ho3+ concentrations. An output power of 19 W with 81% slope efficiency was reached using fiber with almost 4000 ppm of Ho3+ and 10 mol.% of Al2O3. This result is encouraging for highly efficient high-power cladding-pumped holmium fiber lasers, and studied relations between fibers composition and their laser parameters will be used in the designing of such laser sources.

AlN/AlGaN heterojunction field-effect transistors with a high-AlN-mole-fraction Al0.72Ga0.28N channel grown on single-crystal AlN substrate by metalorganic chemical vapor deposition

This paper presents research results on AlN/AlGaN heterojunction field-effect transistors (HFETs) with a high-AlN-mole-fraction Al0.72Ga0.28N channel grown on a single-crystal AlN substrate by metalorganic chemical vapor deposition. Material evaluation results confirmed that the grown AlGaN layer was 100% coherently grown for the underlying AlN substrate and thereby had superior crystal quality as well as the substrate. The fabricated AlGaN-channel HFETs with a gate length of 2 μm exhibited pinch-off characteristics with the max. current density (I DS_MAX) of 21 mA mm−1, the on-state resistance of 250 Ωmm, the peak transconductance of 4.5 mS mm−1 with the threshold voltage of –4.6 V, and the on/off ratio of 4 × 10−5. The temperature dependence of DC characteristics confirmed that the I DS_MAX decreased by 15% and the off-leakage current increased from 60 nA mm−1 to 10 μA mm−1 within the temperature range from room temperature to 200 °C.

The synthesis, characterization, and thermal properties of a titanium (III) amidinate compound and its potential as a single chemical vapor deposition precursor for N/C-doped TiO2 film

A titanium(III) amidinate compound had been successfully obtained using a salt elimination reaction between TiCl3(3THF) and [Li(i Prn BuAMD)] in a 65% yield, and the characterization of the compound was conducted using various characterization methods. The reported compound’s thermal performances were studied through thermal gravimetric analysis (TGA), and the result indicated that the reported titanium(III) amidinate compound exhibited a suitable volatility, high thermal stability, and sufficient vapor pressure. Furthermore, film material deposit was performed in a CVD reactor under low pressure, and a N/C-doped TiO2 film was successfully deposited.

Improve wear resistance of C/C composites as artificial bone using diamond-like carbon coatings

In this study, diamond-like carbon (DLC) coatings and silicon-doped diamond-like (Si-DLC) coatings were prepared on the surface of C/C composites by a combination of plasma-enhanced chemical vapor deposition (PECVD) and magnetron sputtering processes. The film composition, microstructure and atomic bond structure were characterized using X-ray photoelectron spectroscopy, field-emission scanning electron microscopy and Raman spectroscopy. The mechanical properties and friction behavior related to the Si element were investigated using nanoindentation and HT-1000 high temperature friction and wear tester. The biocompatibility of the materials was also evaluated by the MG-63 proliferation test. The results indicate that Si elements were successfully incorporated into the DLC films, bonding with C and O atoms, which altered the thermal stability and microstructure of the coatings, reduced the internal stress of the films, and increased disorder. Compared to C/C composites, all coated layers exhibited lower coefficients of friction, with the formation of transfer layers and graphitization induced by friction contributing to the excellent tribological performance. Both coatings showed no cytotoxicity and demonstrated good biocompatibility. Both coatings are effective in reducing wear and chip losses in C/C composites when used as artificial bones. This work suggests that diamond-like carbon coated C/C composites can be excellent structural materials for human body in biomedical science.

9.4 μm Emitting Quantum Cascade Lasers Grown by MOCVD: Performance Improvement Obtained through AlInAs Composition Adjustment

Metal-organic chemical vapor deposition (MOCVD) is a prevalent technique for the epitaxial growth of quantum cascade lasers (QCLs), with the material quality being paramount to the overall device performance. Previous studies have indicated that the actual aluminum (Al) content in InAlAs barrier layers grown via MOCVD often diverges from the specified design values, particularly for layers with a thickness below 1 nm. To address this discrepancy, the Al content within the InAlAs layers can be fine-tuned by modifying the MOCVD growth parameters. This study undertakes an exhaustive analysis of QCL devices, comparing those with and without aluminum content compensation, through a combination of simulation and experimental approaches. The results demonstrate that the implementation of the Al compensation methodology facilitates the alignment of the QCL device wavelength with the intended design value. This approach also enhances the laser transition efficiency and gain coefficient of the QCL device, thereby improving its slope efficiency and threshold current density. The final QCL device exhibits a wavelength of 9.4 μm, with a maximum continuous wave (CW) and pulsed optical power and wall-plug efficiency (WPE) of 1.26 W and 7.4% and 2.08 W and 10.1%.

Integrated sensor chip of a resonant cavity light emitter and photon detector for wearable optical medicine

This work presents an integrated chip of a resonant cavity light emitter and photon detector (RCLEPD) to address the requirements of wearable optical medical devices for compact size, high efficiency, and interference resistance sensors. The optical radiation pattern and light extraction efficiency of the resonant cavity light emitting diode (RCLED) as well as the optical absorption spectrum of the resonant cavity enhanced photon detector (RCEPD) are theoretically simulated. Additionally, the wavelength selectivity of the RCEPD absorption spectrum is analyzed. Material epitaxial growth of RCLEPD was performed using metal-organic chemical vapor deposition (MOCVD), and an integrated sensing chip with an area of 2 × 2 mm2 was fabricated. Experimental results demonstrate that RCLED achieves a maximum external quantum efficiency of 10.206%, consistent with the simulation results, while maintaining a peak wavelength at 677.5 nm within a current range of 0-20 mA. Furthermore, the RCEPD exhibits a peak response wavelength at 678 nm, matching that of the RCLED. Utilizing RCLEPD as the sensor, photoplethysmography (PPG) signals are collected from the human wrist under different RCLED driving currents resulting in an average period of 977 ms which aligns with a human pulse frequency of 61 beats/min. With further processing techniques applied to PPG signals, RCLEPD is expected to be used as a sensor in wearable blood pressure and glucose monitoring devices.

Effect of thermal annealing on the luminescent and structural properties of the SiOxCy thin films by organic catalytic chemical vapor deposition

Photoluminescent silicon oxycarbide (SiOxCy) thin films were deposited on n-type (100) silicon substrates using the organic catalytic chemical vapor deposition (O-Cat-CVD) technique employing tetra-ethyl orthosilicate (TEOS) as an organic-based precursor. These films were annealed at a temperature of 500, 800 and 1000°C for 30 minutes in a nitrogen (N2) environment. The as-deposited and annealed SiOxCy films were analyzed using optical and structural characterizations, such as photoluminescence (PL), Fourier transform infrared (FTIR), X-ray photoelectron spectroscopy (XPS), Secondary ion mass spectrometry (SIMS) and scanning electron microscopy (SEM). The PL spectrum of the as-deposited film showed emission in the blue-green region, while the annealed SiOxCy films showed strong emission from blue to near-infrared. The PL in all the films was attributed to different structural defects related to oxygen and carbon that act as radiative centers in the SiOxCy network. The annealed films showed an increase in the emission intensity, where the annealed film at 800°C displayed the highest emission intensity. This is related to an increase in the amount of radiative defects in the films due to structural and compositional changes after the thermal annealing (TA). XPS and SIMS measurements showed an oxygen incorporation with the TA, increasing from 54.59 at. % to 63.5 at. % for the as-deposited and annealed at 1000°C films, respectively. FTIR spectra showed an increase in the Si-O-C and Si-O-Si bonds and the hydrogen and other radicals desorption. These results support the creation of radiative centers due to structural changes in the films after the thermal annealing.

Temperature-driven structural and morphological changes in nitrogen-doped carbon nanofibers synthesized via LaNi5Pt1.0 intermetallic catalyst

In the modern world, heteroatom-doped carbon allotropes play a pivotal role in both fundamental and applied nanotechnology advancements. Due to their exceptional electrical, thermal, chemical, and mechanical properties, which are strongly influenced by the synthesis method, they are highly suitable for a wide range of applications. Catalytic chemical vapor deposition (CCVD) is the leading synthesis technique for producing nitrogen-doped carbon nanofibers (NCNFs) with controlled morphology and structural properties. This report emphasizes the significant influence of reaction temperature on synthesizing CNFs using a LaNi5Pt1.0 intermetallic catalyst. The LaNi5Pt1.0 catalysts prepared through an arc melting process, acted as templates for the catalytic conversion of carbon precursors into solid material via the CCVD method. Additionally, this study provides valuable insights into the temperature-dependent phase transitions and carbon diffusion during the synthesis of NCNFs. The surface segregation mechanism driving phase changes in the catalyst plays a crucial role in the active formation of NCNFs. The segregation of metallic nickel into the CNF structure significantly impacts N-CNF formation, highlighting the intricate dynamics involved in CNF synthesis. Overall, these findings offer a deeper understanding of the synthesis process and the structural evolution of N-CNFs across different growth temperatures.

Rapid preparation of Cu(111) foil with large single-crystal grains through a graphene induction and contactless annealing method

There is a growing interest in preparing large-size Cu(111) foil for achieving high performance in various applications. In this work, a simple two-step method using graphene induction and contactless annealing was designed to rapidly prepare Cu(111) foil with large single-crystal grains. The graphene film grown on the Cu surface in the first step by chemical vapor deposition serves as a template for the orientation transition of the Cu foil in a subsequent high-temperature annealing. The (111) orientation transformation of the entire Cu foil was achieved within 20 min with single-crystal grains in size of above 30 cm2, and the corresponding speed is ten times higher than that prepared in traditional annealing process. This work provides a facile and rapid fabrication approach for preparing Cu(111) foil with large grains.

Investigation of Electrochemical Fingerprints for Buzhong Yiqi Tang Extract Granules Using Diamond-Graphene Composite Electrode

This study presents a novel electrochemical fingerprinting method for Buzhong Yiqi Tang extract granules using a diamond-graphene composite electrode. The electrode was fabricated through chemical vapor deposition of graphene on high-pressure high-temperature synthetic diamond, resulting in a few-layer graphene coating as confirmed by Raman spectroscopy (I₂D/IG ratio ≈ 1.2) and XPS analysis (78% sp² C-C signal). Cyclic voltammetry revealed four anodic and three cathodic peaks, while differential pulse voltammetry provided enhanced resolution with eight distinct oxidation peaks. The method demonstrated high sensitivity (LODs 0.08-0.15mg/mL) and good linearity (R² > 0.995) over a concentration range of 0.5-10mg/mL. Comparison of fingerprints from individual herb extracts (Astragalus membranaceus, Panax ginseng, and Glycyrrhiza uralensis) elucidated the origins of major peaks in the Buzhong Yiqi Tang profile. Principal component analysis of fingerprints successfully differentiated between samples from three manufacturers, accounting for 87.3% of total variance. Strong correlations (r > 0.92) were observed between key DPV peak intensities and HPLC-determined concentrations of traditional chemical markers. The rapid analysis time, minimal sample preparation, and holistic representation of multiple electroactive components make this approach a promising complement to existing chromatographic methods for quality assessment of traditional Chinese medicine formulations.

Ammonia-free quasi-atmospheric MOCVD of InN/Al2O3 (0001)

We demonstrate ammonia-free quasi-atmospheric metal–organic chemical vapor deposition (AFQA-MOCVD) of InN grown on c-plane sapphire (Al2O3) substrate using high-density nitrogen (N2) microstrip-line microwave plasma. Dependence of growth temperature (Tg) and N2 plasma power on structural properties were examined. Increasing Tg and N2 plasma power markedly improved surface morphology of InN. An atomically smooth surface with layer-by-layer growth mode was realized at Tg of 750 °C under N2 plasma power of 80 W. Fully strain-relaxed InN was grown on in-plane crystal rotation by 30° with respect to the Al2O3 (0001). N-polar InN on Al2O3 (0001) was revealed by scanning transmission electron microscopy. AFQA-MOCVD enables to expand growth windows by increasing Tg and V/III ratio compared to the standard MOCVD using NH3.

4 inch 11 μm high-quality AlN thick films grown on nanopatterned sapphire substrates

A high-quality AlN thick film with 11 μm thickness and low defect density was grown on a 4 inch hexagonal hole nano-patterned sapphire substrate by metal oxide chemical vapor deposition. The density of dislocation etch pits in the AlN heteroepitaxial film reached 1.1 × 107 cm−2. The surface and microstrcutres of the AlN thick film were characterized in detail. The dislocation evolution mechanism and stress evolution of AlN were investigated. Dislocations were mainly generated at the interface between the sapphire and AlN, and the voids above the patterned region were generated by the undesirable grain boundaries caused by the lateral epitaxy of AlN and the substrate during the growth process, which prompted a large number of screw dislocations to bend and merge, and while some mixed dislocations to merge and extend upwards, resulting in a high-quality AlN thick film.

Effect of Ce co-doping on radiation resistance behavior and laser performance of Er/Yb/Ce co-doped high-phosphorous polarization-maintaining silica fiber

Er/Yb/Ce co-doped high-phosphorus silica fiber core glasses with varying Ce2O3 concentrations were prepared and systematically studied. Based on this research, optimized Er/Yb/Ce co-doped high-phosphorus polarization-maintaining silica fibers were subsequently fabricated using the modified chemical vapor deposition (MCVD) technique and hole drilling method. The study confirmed that there is an optimal range of Ce doping concentrations for spectral performance, Ce doping effectively suppressing the formation of P-related defects during X-ray irradiation, and the dynamic valence state transformation of Ce3+/Ce4+ ions during irradiation enhanced the radiation-resistant properties, as demonstrated through radiation-induced absorption (RIA), electron paramagnetic resonance (EPR), and L3-edge X-ray absorption near edge structure (XANES) spectra. The homemade fiber, with optimized element concentrations, exhibited high laser efficiency comparable to commercial high-power fibers. Furthermore, the radiation-induced background loss of the fiber was 0.16 dB/m under 60 krad γ-rays at a low dose rate of 100 rad/h, and the radiation-induced gain variation (RIGV) was 0.019 dB/krad.

Gradient Mo1−xWxSe2 monolayer Alloys: Synthesis and multifunctional applications

With the continuous and rapid development of electronic information technology, the demand for new materials with miniaturization, high integration, high performance, and multifunction is becoming increasingly urgent. However, it is difficult for existing photodetectors based on a single material to achieve multi-functionality while maintaining excellent performance, and the devices based on heterostructures are faced with complex preparation and compatibility problems. In this work, gradient Mo1−xWxSe2 monolayer alloys with high crystal quality have been synthesized by an evaporation-assisted chemical vapor deposition method. The composition of the synthesized Mo1−xWxSe2 monolayer alloys varies gradually with x ranging from 0 to 1. The Mo1−xWxSe2 based photodetector shows superior photoresponse performance in the visible wavelength with maximum responsivity of 26 A/W and external quantum efficiency up to 6320 % under 520 nm laser irradiation. Besides, the Mo1−xWxSe2 device is capable of high-resolution imaging, which can be used as image sensor. Moreover, nonvolatile memory function has also been realized in the device because the band gap of Mo1−xWxSe2 can be effectively adjusted by the gradient distribution of the component and the deep energy levels caused by Se vacancies can be modulated to shallow energy levels. A thrilling discovery is that the gradient Mo1−xWxSe2 alloy device can simulate the biological synapses successfully, including paired-pulse facilitation, short-term plasticity, long-term plasticity and learning process. The realization of high-performance photodetection, visualization, nonvolatile memory and synaptic simulation based on a single gradient crystal offers a new type of material to develop advanced optoelectronic devices with multiple functions.

Quantum chemical study of trimethylindium and trimethylgallium gas-phase reaction pathways in InGaN MOCVD growth

Density functional theory was used to analyze the formation of InGaN from trimethylindium (TMIn) and trimethylgallium (TMGa) by metalorganic chemical vapor deposition in ammonia in terms of the reaction between trimethyl compounds and NH3, as well as the subsequent reactions of the key amino species DMInNH2. The calculation model is established in GAUSSIAN 09, and the results obtained by the calculation model are proved to be reliable by comparing with the previous research results. Reaction pathways were assumed and the Gibbs free energy and activation free energy calculation were conducted at different temperatures. TMIn and TMGa can undergo adduct reactions with the first NH3 molecule at reaction temperatures below 596 K and 465 K, respectively, but they cannot further react with the second NH3 molecule to form additional products. The temperature range for adduct reactions between TMIn and NH3 is wider compared to TMGa and NH3. In the absence of H radicals in the reaction chamber, DMInNH2 does not undergo spontaneous CH3 radical elimination reactions or CH4 elimination reactions. Instead, DMInNH2 is more inclined to undergo dimerization reactions and CH4 elimination reactions with NH3, leading to the formation of subsequent products, In(NH2)3 and dimers. However, in the presence of H radicals in the reaction chamber, H radicals can facilitate the CH3 radical elimination reaction of DMInNH2 and also promote the NH2 radical elimination reaction of In(NH2)3, In(NH2)2 and InNH2, enabling these reactions to occur spontaneously within the studied temperature range. Consequently, the subsequent products of DMInNH2 become indium atoms and dimers.

Zirconia encrusted ceramic composite membrane for uremic toxins removal: Fabrication and assessment of biocompatibility

In this study, tubular zirconia composite membranes (ZM1-ZM3) were developed using low-cost tubular substrate which was prepared utilizing naturally available clay materials by an extrusion approach. The zirconia nanoparticles were encrusted on a low-cost tubular substrate using spray pyrolysis technique. The membranes were investigated for their biocompatibility in addition to pore size, chemical stability, water permeability, porosity, contact angle, thermogravimetric (TGA), and X-ray diffraction (XRD). Water permeability, pore size and porosity of optimized membrane (ZM3) were 3.05 × 10-4 ± 0.03 L.m-2.h-1.Pa-1, 119 ± 0.57 nm and 36 ± 0.12 %, respectively. Platelets adhesion and protein adsorption were measured to be 4630 ± 46 platelets.mm-2, and 1.05 ± 0.02 μg.cm-2 respectively, while the activated partial thromboplastin time (APTT) and prothrombin time (PT) were 80 ± 0.51 s and 27 ± 0.26 s, respectively. Complement activation C3 and C4 concentrations were assessed to be 76.2 ± 0.88 mg.dL-1 and 21.57 ± 0.80 mg.dL-1, respectively and hemolysis ratio was 0.31 ± 0.01 %. Moreover, the membrane had a considerable antifouling nature with a flux recovery ratio of 89.22 ± 0.58 %. Protein retention was found to be 81.14 ± 0.58 %, in addition to outstanding sieving coefficients of uremic toxins like urea (0.95 ± 0.005), creatinine (0.93 ± 0.004), and phosphate (0.90 ± 0.004). These findings suggest that the produced tubular zirconia composite membrane has the potency for hemofiltration.

Effect of flame temperature on structure and CO oxidation properties of Pt/CeO2 catalyst by flame-assisted spray pyrolysis

Flame synthesis offers the potential for the synthesis of structure-controlled catalysts. In this study, Pt/CeO2 nanoparticles were synthesized via flame-assisted spray pyrolysis (FASP) and used as CO oxidation catalysts. The catalysts were synthesized using a burner diffusion flame at three different flame temperatures (maximum flame temperatures, Tf = 1556, 1785, and 2026 K), and their particle structure and CO oxidation activity were evaluated. The synthesized Pt/CeO2 catalysts had a bimodal structure containing 100 nm-scale CeO2 loaded with 10 nm-scale Pt and fine CeO2 less than 10 nm loaded with highly dispersed Pt (less than 1 nm). As the flame temperature increases from 1556 to 2026 K, the formation of fine CeO2 particles dominates, resulting in an increase in BET specific surface area from 7.97 to 112 m2/g and Pt dispersion from 4.67 to 20.6%. Insight into the particle formation routes that determine the catalyst structure is provided by numerical simulation of droplet evaporation in a burner flame. CO oxidation experiments showed that the temperature at which CO conversion reached 100% (T100) decreased from 513 to 378 K with increasing flame temperature in FASP. In addition, the thermal stability test showed that the Pt dispersion after thermal degradation was higher for Pt/CeO2 catalyst made by FASP at Tf = 2026 K than that prepared by the impregnation method, and the T100 for CO oxidation was lower by 20 K.

Influence of growth temperature on the structural and optical characteristics of PbZnS thin films

Ternary thin films have garnered significant attention due to their adjustable band gap characteristics, making them suitable for many applications. In this research, we examined the structural and optical characteristics of PbZnS thin films fabricated onto glass substrates employing the spray pyrolysis techniuqe. The films were fabricated at different temperatures ranging from 300 to 400°C. X-ray diffraction (XRD) analysis indicated that all films displayed a cubic structure with a preferred orientation along the (200) plane. From the analysis of XRD peaks, it was observed that the crystal structure initially improved with increasing temperature but then began to degrade. These films demonstrated strong absorption in the range of 350–1600 nm. The optical bandgap (Eg) values, calculated based on the relationship between the absorption coefficient and photon energy, showed slight variations around 2 eV. Notably, the band gap decreased with growth temperatures up to 350°C, then increased at higher temperatures. These fluctuations are attributed to factors such as thermal expansion, strain, defects, surface/interface effects, and changes in doping or composition.