Large Nuclear Detector Array Interconnection by Direct-Write Laser Chemical Vapor Deposition (CVD)
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46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
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Laser velocimetry measurements in non-isothermal CVD systems
Researchers at the NASA Langley Research Center are applying laser velocimetry (LV) techniques to characterize the fluid dynamics of non-isothermal flows inside fused silica chambers designed for chemical vapor deposition (CVD). Experimental issues involved in the application of LV techniques to this task include thermophoretic effects on the LV seed particles, seeding the hazardous gases, index of refraction gradients in the flow field and surrounding media, optical access, relatively low flow velocities, and analysis and presentation of sparse data. An overview of the practical difficulties these issues represent to the use of laser velocimetry instrumentation for CVD applications is given. A fundamental limitation on the application of LV techniques in non-isothermal systems is addressed which involves a measurement bias due to the presence of thermal gradients. This bias results from thermophoretic effects which cause seed particle trajectories to deviate from gas streamlines. Data from a research CVD reactor are presented which indicate that current models for the interaction of forces such as Stokes drag, inertia, gravity, and thermophoresis are not adequate to predict thermophoretic effects on particle-based velocimetry measurements in arbitrary flow configurations.
Johnson, E. J.↗
Emerging continuous SiC fibers for high-temperature applications
Silicon carbide (SiC) fibers are responsible for the ultimate strength and toughness of SiC-fiber reinforced composites in harsh environments. The development of a new generation of continuous SiC fibers continues to advance the mechanical properties of composite materials. Tyranno™ SA4 fiber was recently released as a successor of Tyranno™ SA3 fiber. Laser-driven chemical vapor deposition (LCVD) has been adopted as an alternative fiber processing route to synthesizing high-strength SiC fiber with tailorable small diameters and chemical compositions. Both Tyranno™ SA4 and laser-driven CVD fibers show very high tensile strength, about 4 GPa in the as-fabricated condition. The degradation of thermal stability and strength due to annealing in an inert environment were similar for Tyranno™ SA3 and SA4 fibers because of their similar carbon-rich, crystalline microstructure. Silicon-rich fibers produced by LCVD possessed heterogeneous crystallinity, which was attributed to laser power distribution and showed microstructural instability at 1500 °C and above. Finally, the new SiC fibers demonstrated an increase in as-fabricated strength but faced the same challenges in environmental resistance as the traditional SiC fibers do.
36 MATERIALS SCIENCE↗
Current challenges and potential directions towards precision microscale additive manufacturing – Part III: Energy induced deposition and hybrid electrochemical processes
The Part III of the four-part series of articles discusses the challenges and opportunities in microscale additive manufacturing processes, specifically focusing on energy-induced deposition and electrochemical processes. Compared to the direct ink write (DIW) and laser-based processes, the energy-induced deposition methods can fabricate high-resolution, high aspect ratio and complex parts, while the hybrid electrochemical process can be used to fabricate complex parts using a wide range of conductive and photoactive materials. However, the volumetric throughput of these processes is lower than their DIW and laser-based counterparts. The processes that have been explored in this process are Focused-ion Beam Induced Deposition (FIBID), Laser Chemical Vapor Deposition (LCVD), Menicus-confined Electrodeposition (MCED) and Laser-Enabled Electrochemical Printing (LECP). The range of processable materials, feature-size resolution, geometry and volumetric throughput are used as factors to evaluate the current state-of-the-art for these processes. Finally, novel approaches have been proposed in the article to address these challenges associated with microscale AM processes.
42 ENGINEERING↗
Epitaxial Growth of Ga2O3: A Review
Beta-phase gallium oxide (β-Ga2O3) is a cutting-edge ultrawide bandgap (UWBG) semiconductor, featuring a bandgap energy of around 4.8 eV and a highly critical electric field strength of about 8 MV/cm. These properties make it highly suitable for next-generation power electronics and deep ultraviolet optoelectronics. Key advantages of β-Ga2O3 include the availability of large-size single-crystal bulk native substrates produced from melt and the precise control of n-type doping during both bulk growth and thin-film epitaxy. A comprehensive understanding of the fundamental growth processes, control parameters, and underlying mechanisms is essential to enable scalable manufacturing of high-performance epitaxial structures. This review highlights recent advancements in the epitaxial growth of β-Ga2O3 through various techniques, including Molecular Beam Epitaxy (MBE), Metal-Organic Chemical Vapor Deposition (MOCVD), Hydride Vapor Phase Epitaxy (HVPE), Mist Chemical Vapor Deposition (Mist CVD), Pulsed Laser Deposition (PLD), and Low-Pressure Chemical Vapor Deposition (LPCVD). This review concentrates on the progress of Ga2O3 growth in achieving high growth rates, low defect densities, excellent crystalline quality, and high carrier mobilities through different approaches. It aims to advance the development of device-grade epitaxial Ga2O3 thin films and serves as a crucial resource for researchers and engineers focused on UWBG semiconductors and the future of power electronics.
Chemistry↗
Raman Laser-Induced Structural Modification in CVD-Grown Monolayer MoS 2 for Multi-Purposed Nanofabrication
Molybdenum disulfide (MoS 2 ) has been extensively explored to be utilized as an electronic material in a variety of device applications. In particular, the tunability of MoS 2 enhances its electrical properties making it an intriguing candidate for field-effect transistors (FETs), while also extending beyond electrical properties to structural phase engineering. Laser-induced modifications, particularly with Raman lasers, offer a straightforward method to modulate materials via thermal processes with precise patterning control and energy-level flexibility. However, most studies on the modification of MoS 2 have focused on multilayered structures or have been conducted under low-power laser conditions, leaving the feasibility of structural modifications in monolayer MoS 2 elusive. In this study, we fundamentally elucidated the effects of high-power Raman laser irradiation on the surface of chemical vapor deposition (CVD)-grown monolayer MoS 2 under ambient conditions and uncovered the underlying mechanisms of laser-induced modifications by applying intense photon energy with highly interactive reactions. Our results revealed both etching and deposition phenomena in two discernible regions, and it can be demonstrated by intensity regimes based on the spatial distribution of laser irradiance within the laser-irradiated spot. Furthermore, phase transition was found to be inhibited due to the promoted oxidation and the deposition of hydrogenated amorphous carbon (a-C:H), and p-type doping was observed, likely occurring in the region beneath the a-C:H deposition as substitutional doping on the 2H phase of MoS 2 . To compare the thermal effects, MoS 2 modifications were further analyzed using simplified heat transfer estimations. In conclusion, these findings deepen our understanding of how Raman laser irradiation modifies MoS 2 under ambient conditions, providing guidelines for optimizing its modification processes.
36 MATERIALS SCIENCE↗
Effect of CO{sub 2}-laser power density on the absorption coefficient of polycrystalline CVD diamonds
The effect of 1-s irradiation of an uncooled polycrystalline CVD diamond plate by a focused cw CO{sub 2} laser beam with a power density of 300 – 800 kW cm{sup −2} is investigated. The absorption coefficient of the sample at a power density of 800 kW cm{sup −2} is found to be 0.035 cm{sup −1} larger as compared with that at 300 kW cm{sup −2}, which is related to the temperature dependence of its phonon-induced absorption with a change in temperature from 44 to 100 °C. It is shown that polycrystalline diamond, in contrast to other optical materials, does not exhibit nonlinear (avalanche-like) rise in absorption at high CO{sub 2}-laser power densities, at least up to 800 kW cm{sup −2}. (paper)
36 MATERIALS SCIENCE↗
AlGaAs/GaAs transverse junction stripe lasers with distributed feedback
Transverse junction stripe (TJS) lasers with periodic feedback were fabricated in two geometries. An interferometric and wet chemical etching technique was used to create a feedback grating across the entire pumping region for the distributed feedback (DFB) TJS laser and to create the separate distributed Bragg reflectors/DBR) for the TJS/DBR laser. The TJS/DFB laser was a double heterostructure device grown by liquid phase epitaxy (LPE) and had a third order grating etched in the top ALO.2GaO.8As layer. The grating was buried by growing an ALO.35GaO.65As layer on the grating by metal organic chemical vapor deposition (MO-CVD). The TJS/DBR laser was also fabricated in an LPE double heterostructure. The top AlGaAs layer was thinned to 0.1 micron over more than half of the laser so that the grating would be close to the GaAs active layer and optical field. Single mode operation in both configurations was obtained. The thermal shift of the laser wavelength in both cases was less than 1 Angstrom/deg K, compared to the 3 Angstrom/deg K shift of the spontaneous emission peak.
Hafich, M. J.↗
Design of Inorganic Water Repellent Coatings for Thermal Protection Insulation on an Aerospace Vehicle
In this report, thin film deposition of one of the model candidate materials for use as water repellent coating on the thermal protection systems (TPS) of an aerospace vehicle was investigated. The material tested was boron nitride (BN), the water-repellent properties of which was detailed in our other investigation. Two different methods, chemical vapor deposition (CVD) and pulsed laser deposition (PLD), were used to prepare the BN films on a fused quartz substrate (one of the components of thermal protection systems on aerospace vehicles). The deposited films were characterized by a variety of techniques including X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The BN films were observed to be amorphous in nature, and a CVD-deposited film yielded a contact angle of 60 degrees with water, similar to the pellet BN samples investigated previously. This demonstrates that it is possible to use the bulk sample wetting properties as a guideline to determine the candidate waterproofing material for the TPS.
Fuerstenau, D. W.↗
Selected Area Deposition of PtC x Nanostructures: Implications for Functional Coatings of 3D Nanoarchitectures
Here, we report that selected area deposition of 3D nanostructures is induced via a pyrolytic laser chemical vapor deposition (CVD) process where selected area heating results from the unique photothermal transport regime that is intrinsic to 3D nanostructures. PtC x composite nanostructures were deposited by focused electron beam-induced deposition (FEBID) and used as 3D templates. Subsequent simultaneous localized delivery of an organometallic PtC x precursor and pulsed 915 nm laser irradiation to the pre-defined nanostructures results in selected area deposition on the FEBID features. Results indicate the ability to initiate the process on sub-diffraction-limit nanoscale features. To elucidate the mechanisms that are operative in the selected area deposition, we analyze the effects of the laser repetition rate, power, and pulse duration. Thermal simulations corroborate that the pseudo-1D thermal transport of the nanostructure geometry coupled with the optical and thermal properties of the nanostructure governs the CVD reaction. The results demonstrated here suggest that controlling the thermal transport in nanomaterial architectures could be a useful means to spatially control localized photothermally stimulated chemical reactions and induce selected area reactions.
36 MATERIALS SCIENCE↗
Diamond films for laser hardening
Laser-damage experiments were performed on free-standing polycrystalline diamond films prepared by plasma-enhanced CVD. The high laser-induced stress resistance found for this material makes it useful for thin-film coatings for laser optics. Results for diamond-coated silicon substrates demonstrate the enhanced damage threshold imparted by diamond thin-film coatings to materials susceptible to laser damage.
Albin, S.↗
Production and Characterization of Carbon Nanotubes and Nanotube-Based Composites
The Nobel Prize winning discovery of the Buckuball (C60) in 1985 at Rice University by a group including Dr. Richard Smalley led to the whole new class of carbon allotropes including fullerenes and nanotubes. Especially interesting from many viewpoints are single-walled carbon nanotubes, which structurally are like a single graphitic sheet wrapped around a cylinder and capped at the ends. This cylinders have diameter as small as 0.5 - 2 nm (1/100,000th the diameter of a human hair) and are as long as 0.1 - 1 mm. Nanotubes are really individual molecules and believed to be defect-free, leading to high tensile strength despite their low density. Additionally, these fibers exhibit electrical conductivity as high as copper, thermal conductivity as high as diamond, strength 100 times higher than steel at one-sixth the weight, and high strain to failure. Thus it is believed that developments in the field of nanotechnology will lead to stronger and lighter composite materials for next generation spacecraft. Lack of a bulk method of production is the primary reason nanotubes are not used widely today. Toward this goal JSC nanotube team is exploring three distinct production techniques: laser ablation, arc discharge and chemical vapor deposition (CVD, in collaboration with Rice University). In laser ablation technique high-power laser impinges on the piece of carbon containing small amount of catalyst, and nanotubes self-assemble from the resulting carbon vapor. In arc generator similar vapor is created in arc discharge between carbon electrodes with catalyst. In CVD method nanotubes grow at much lower temperature on small catalyst particles from carbon-containing feedstock gas (methane or carbon monoxide). As of now, laser ablation produces cleanest material, but mass yield is rather small. Arc discharge produces grams of material, but purity is low. CVD technique is still in baby steps, but preliminary results look promising, as well as perspective of scaling the process up. We are also working on necessary purification of nanotubes. Applications of nanotubes are in such various fields as lightweight composites, molecular electronics, energy storage (electrodes in Li ion batteries), flat panel displays, conductive polymers, etc. JSC nanotube team is focused on development of lightweight materials. We work on the injection thermoset epoxies reinforced with nanotubes. Early results show good wetting of nanotube surface with epoxy, which is very important. More research will be possible as more nanotubes become available.
Nikolaev, Pavel↗
Controlled Patterning and Growth of Single Wall and Multi-wall Carbon Nanotubes
Method and system for producing a selected pattern or array of at least one of a single wall nanotube and/or a multi-wall nanotube containing primarily carbon. A substrate is coated with a first layer (optional) of a first selected metal (e.g., Al and/or Ir) and with a second layer of a catalyst (e.g., Fe, Co, Ni and/or Mo), having selected first and second layer thicknesses provided by ion sputtering, arc discharge, laser ablation, evaporation or CVD. The first layer and/or the second layer may be formed in a desired non-uniform pattern, using a mask with suitable aperture(s), to promote growth of carbon nanotubes in a corresponding pattern. A selected heated feed gas (primarily CH4 or C2Hn with n=2 and/or 4) is passed over the coated substrate and forms primarily single wall nanotubes or multiple wall nanotubes, depending upon the selected feed gas and its temperature. Nanofibers, as well as single wall and multi-wall nanotubes, are produced using plasma-aided growth from the second (catalyst) layer. An overcoating of a selected metal or alloy can be deposited, over the second layer, to provide a coating for the carbon nanotubes grown in this manner.
Lance D Delzeit↗
A study on sub-bandgap photoexcitation in nitrogen- and boron-doped diamond with interdigitated device structure
Diamond is an ultrawide-bandgap semiconductor suitable for high power devices that require high current carrying capacity, high blocking voltages, and smaller form factors. We investigated various diamond structures for extrinsic photoconductive semiconductor switches, including an insulating high-pressure high-temperature type Ib (highly nitrogen-doped) substrate, a chemical vapor deposited (CVD) type IIa (unintentionally doped) substrate, a CVD grown semiconducting boron-doped epilayer on a type IIa substrate, and boron-implanted type Ib and IIa substrates. Using these samples, we fabricated and characterized planar interdigitated photoconductive switches with 30 μm, electrode gaps. 532 and 1064 nm Nd:YAG laser pulses with energies up to 3.5 mJ/pulse were used to trigger the switches. Photoresponses were measured at bias voltages ranging from 10 to 100 V, corresponding to electric fields of 3.3–33 kV/cm. In this field range, the type Ib device exhibited the highest average on/off-state current ratio, on the order of 10 11 , when triggered with 0.8 mJ/pulse, 532 nm laser pulses. However, only the CVD grown boron-doped epilayer and boron implanted IIa devices showed decent sensitivity to 1064 nm.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
In-Situ Laser Diagnostics to Understand Plasma-Surface Interactions in Titanium Thin Film Deposition
During the current project period the following tasks were completed: (1) We demonstrated the feasibility of a new way of measuring CH3 radicals in a plasma environment using a single, femtosecond (fs) pulsed laser for the first time, in a CH4 + Ar flow. A single fs pulsed Ti:Sa laser was split into two beams and with beam conversion using crystals we generatedtwo beams of 275 nm and 205 nm. The 275 nm was used to predissociate the CH3 radicals to CH2+H, followed by 205 nm Two Photon Laser Induced Fluorescence (TALIF) detection of H atoms, with a 11 ns delay from 275 nm predissociation pulse. (2) We demonstrated preliminary CH3 concentration measurements with spatial (< 100 µm) and time resolution (< 10 ns) by image processing of H and Kr TALIF signal images. (3) The methodology to quantify CH3 concentrations was developed. (4) Preliminary measurements of laser dissociation cross sections for CH4 and CH3 to (CH3+H), and (CH2+H), respectively, were conducted. (5) 275 nm laser dissociation of CH4 is a multiphoton process, and the CH4 dissociation cross section is a more sensitive function of the laser pulse energy than CH4 concentration. In the coming months, we will make more precise measurements of the dissociation cross sections, 𝑘275, 𝐶𝐻4 and 𝑘275, 𝐶𝐻3, by varying the laser energy while keeping the flow composition and conditions constant. This will enable more precise quantification of CH3 radical concentrations. More detailed measurements of CH3 radicals will be conducted in the following months of 2025 (Sept-Dec) in a Titanium Isopropoxide (TIP) + H2 + Ar flow meant for pure phase Ti thin film deposition by Chemical Vapor Deposition (CVD). More precise measurements of 275 nm laser dissociation cross sections for CH4 (to CH3 + H) and CH3 (to CH2 + H) will be conducted in the future. Detailed 275 nm laser predissociation cross sections for CH4 and CH3 dissociation to (CH3+H), and (CH2+H), respectively, as a function of gas heating, plasma power, and laser pulse energy will be evaluated. This will enable quantification of CH3 concentrations in the precursor flow over a substrate with time and spatial resolution. Comparison of the concentrations with 2D numerical simulations can lead to understanding of plasma surface interactions during pure metallic Ti thin film deposition using environmentally safer non-halogen TIP precursor. Flow conditions for pure Ti thin film deposition using non-halogen precursor (TIP) will be identified in the following months.
Uddi, Mruthunjaya [Advanced Cooling Technologies, ↗
Gravitational and thermal effects in CVD flow and deposition
A three-phased approach is used to investigate the transport phenomena occurring in horizontal CVD reactors. The three phases are made up of laser velocimetry experimental investigations, numerical CFD modeling, and metal-organic chemical vapor deposition experimental studies. Laser velocimetry measurements of flow in a horizontal reactor with a cylindrical flow channel and tilted susceptor demonstrate velocity components arising from thermal expansion and buoyancy effects that significantly exceed the velocity components due to the external applied flow. MOCVD of InP and GaAs thin films in a horizontal reactor channel with a rectangular cross section and a tilted susceptor has also been examined.
Clark, I. O.↗
Laser damage threshold of diamond films
The possibility that diamond films may inhibit laser-induced damage to optical components in laser systems films was investigated by measuring laser damage thresholds of free-standing diamond film windows, diamond films deposited on silicon substrates, and bare silicon substrate. Polycrystalline diamond films were deposited using a dc plasma-enhanced CVD process. It was found that free-standing diamond films had the highest laser damage threshold at 1064 nm. For a diamond film of 630 nm, the damage threshold was found to be 7 J/sq cm, as compared to a damage threshold of 4.5 J/sq cm for bare silicon, and a low value of 1.5 J/sq cm for the film/substrate combination. The damage mechanism is considered to involve melting or dielectric breakdown induced by laser radiation. The low value of the film/substrate combination is attributed to film stress and conditions of film deposition.
Albin, Sacharia↗
Pre-Finishing of SiC for Optical Applications
13 Manufacturing & Prototyping A method is based on two unique processing steps that are both based on deterministic machining processes using a single-point diamond turning (SPDT) machine. In the first step, a high-MRR (material removal rate) process is used to machine the part within several microns of the final geometry. In the second step, a low-MRR process is used to machine the part to near optical quality using a novel ductile regime machining (DRM) process. DRM is a deterministic machining process associated with conditions under high hydrostatic pressures and very small depths of cut. Under such conditions, using high negative-rake angle cutting tools, the high-pressure region near the tool corresponds to a plastic zone, where even a brittle material will behave in a ductile manner. In the high-MRR processing step, the objective is to remove material with a sufficiently high rate such that the process is economical, without inducing large-scale subsurface damage. A laser-assisted machining approach was evaluated whereby a CO2 laser was focused in advance of the cutting tool. While CVD (chemical vapor deposition) SiC was successfully machined with this approach, the cutting forces were substantially higher than cuts at room temperature under the same machining conditions. During the experiments, the expansion of the part and the tool due to the heating was carefully accounted for. The higher cutting forces are most likely due to a small reduction in the shear strength of the material compared with a larger increase in friction forces due to the thermal softening effect. The key advantage is that the hybrid machine approach has the potential to achieve optical quality without the need for a separate optical finishing step. Also, this method is scalable, so one can easily progress from machining 50-mm-diameter samples to the 250-mm-diameter mirror that NASA desires.
Rozzi, Jay↗