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At least 469 records · Page 26

Oblique angle deposition of boron carbide films by magnetron sputtering

Many applications of boron carbide (B4C) films entail deposition on non-planar substrates, necessitating a better understanding of oblique angle deposition phenomena. Here, we systematically study the effect of substrate tilt on properties of B 4 C films with thicknesses up to 10 μm deposited by direct current magnetron sputtering. Results show that all films are amorphous and columnar with an average column width of ~100 nm, independent of substrate tilt. Column tilt angles are limited to ~20° even for substrate tilt of 80°. Film density, residual stress, and the refractive index weakly (within ≲20%) depend on substrate tilt. Furthermore, oxygen impurities bond preferentially with carbon atoms in inter-columnar regions. Substrate tilt has a major effect on mechanical properties that decrease by ~50%, suggesting weak interconnection between nano-columns. Implications of these observations for the deposition onto non-planar substrates are discussed.

36 MATERIALS SCIENCE↗

Experimental evidence of disordered crystalline premixing in sputter-deposited Ni(V)/Al multilayers

The sputter deposition of alternating layers of Ni(V) and Al forms a reactive multilayer known to undergo self-propagating formation reactions when ignited. The sequential deposition process leads to nanometer-scale premixing of reactants at each included interface, which ultimately affects multilayer exothermicity. This work performs the direct measurement of a disordered face-centered cubic (FCC) solid solution premixed phase at the interfaces of Ni(V)/Al multilayers via scanning transmission electron microscopy. The crystallinity of the observed phase differs from previously reported a priori predictions of an amorphous interlayer. The disordered FCC phase retains its symmetry after annealing for 16 h at 135 ± 5 °C, but the lattice parameter shifts consistently with an Al-rich composition. The existence of a crystalline premix in Ni(V)/Al is attributed to the electronic contribution to the entropy of crystallization. The importance of electronic entropy to the phase formation of energetic materials motivates its inclusion when constructing digital twins for atomistic kinetics and ignition sensitivity.

Crystal structure↗

Broad-range tuning of ferroelectric switching of La x Bi 1−x FeO 3 epitaxial films via digital doping using off-axis co-sputtering

To investigate the scope of ferroelectric behavior in La-substituted BiFeO 3 films, La x Bi 1−x FeO 3 epitaxial films were synthesized using off-axis co-sputtering on SrTiO 3 (001) and DyScO 3 (110) substrates with a SrRuO 3 bottom electrode layer. A digital-doping deposition method was used to enable precise control and continuous tuning of La concentration in high-quality LaxBi 1−x FeO 3 films across a wide range of x = 0.05–0.60, which was systematically investigated using piezoresponse force microscopy. Robust and reversible out-of-plane ferroelectric switching has been observed up to x = 0.35, while films with x ≥ 0.37 exhibit no measurable ferroelectric behavior, indicating a sharp ferroelectric-to-paraelectric phase transition between x = 0.35 and 0.37. This represents the highest reported La concentration in LaxBi 1−x FeO 3 films that retains ferroelectric ordering, highlighting opportunities to engineer ferroelectric and multiferroic properties in complex oxide heterostructures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Development of New Magnetron Sputter Deposition Processes for Laser Target Fabrication

Magnetron sputter deposition is an enabling technology for laser target fabrication. Solutions are readily available for the deposition of most sub-micron-thick elemental films on planar substrates. However, major challenges still remain for the development of robust deposition processes in regimes of ultrathick (over ~10 μm) coatings and nonplanar substrates. These challenging deposition regimes are directly relevant to laser target applications, including both sphero-cylindrical hohlraums and spherical ablators for inertial confinement fusion (ICF) targets. Understanding underlying physical mechanisms for a specific material system is crucial for process development, given the overall complexity of the deposition process, its nonlinear dependence on deposition parameters, and a very large process space, often precluding conventional process optimization approaches. Here, we describe our approach to developing new deposition processes and give practical advice with examples of new results from our ongoing studies of glassy boron carbide ceramics for next-generation ICF ablators and nonequilibrium gold-tantalum alloys for hohlraums for magnetized ICF schemes. Emphasis is given to two major challenges of ultrathick coatings related to achieving process stability and reducing residual stress.

36 MATERIALS SCIENCE↗

High-Rate Sputter Deposition of Ultrathick Boron Carbide Coatings on Rolling Spherical Substrates

Amorphous boron carbide (B 4 C) is a promising next-generation ablator material for inertial confinement fusion. However, the deposition of ultrathick B4C coatings with submicron-scale density uniformity on spherical substrates, as required for ablator shell fabrication, remains challenging. Here, in this study, we use direct current magnetron sputtering to deposit B 4 C onto 2-mm-diameter Si spheres rolling in a dish-shaped substrate holder. High deposition rates of ∼3 μm/h are achieved. Ultrathick films have a columnar microstructure, with the column width determined by the density of nodular defects. Nodular defect nucleation is dominated by the pickup of particulates from the holder during substrate rolling. We demonstrate the fabrication of a hollow B 4 C spherical shell with a wall thickness of 80 μm. Also demonstrated is the laser machining of holes in the B 4 C coating, which is necessary for both the chemical removal of the Si template and the attachment of a fusion fuel fill tube.

Inertial confinement fusion targets↗

High-Power Impulse Magnetron Sputter Deposition of Ultrathick Amorphous Carbon

Diamond-like carbon (DLC) is a material of interest for inertial confinement fusion (ICF) ablators. However, the deposition of ultrathick DLC coatings, as required for ICF ablator fabrication, remains a challenge. Here, in this study, we use high-power impulse magnetron sputtering to deposit DLC and demonstrate a set of process parameters leading to high-purity, amorphous DLC coatings with a low compressive residual stress of <400 MPa. Coatings with thicknesses of up to 80 μm are demonstrated.

amorphous carbon↗

Combinatorial Deposition of Ultrathick Ta-W-Au-Bi High-Entropy Alloys for Next-Generation Hohlraums by Direct-Current Magnetron Sputtering

Hohlraum temperature calculations with the model by J. H. Hammer and M. D. Rosen predict a higher X-ray drive from Ta-W-Au-Bi high-entropy alloys compared to pure Au and recently developed Ta 4 Au and Au-Bi hohlraums. Here, we study the microstructure and properties of 25-75−µm-thick Ta-W-Au-Bi alloy films deposited via combinatorial direct-current magnetron sputtering. All of the films have promising physical properties, including high electrical resistivity, that satisfy the requirements for magnetically assisted inertial confinement fusion experiments. While porosity tends to increase with increasing Bi content, we also found that films with Bi content > 44 at. % exhibited densification close to the substrate/film interface and formed a single-phase alloy. In conclusion, these findings provide a potential path forward for the development of Ta-W-Au-Bi alloys for next-generation hohlraum materials.

Magnetron sputtering↗

High figure-of-merit p -type transparent conductor, Cu alloyed ZnS via radio frequency magnetron sputtering

p-type transparent conducting Cu alloyed ZnS thin films from Cu$_{{x}}$ Zn$_{{1-x}}$ S targets ($x = 0.1$ , 0.2, 0.3, 0.4, and 0.5) were deposited on glass substrates via radio frequency sputtering. x-ray diffraction and TEM–SAED analysis show that all the films have sphalerite ZnS as the majority crystalline phase. In addition, films with 30% and 40% Cu show the presence of increasing amounts of crystalline Cu2S phase. Conductivity values ≥400 S ${\rm cm}^{-1}$ were obtained for the films having 30% and 40% Cu, with the maximum conductivity of 752 S ${\rm cm}^{-1}$ obtained for the film with 40% Cu. Temperature dependent electrical transport measurements indicate metallic as well as degenerate hole conductivity in the deposited films. The reflection-corrected transmittance of this Cu alloyed ZnS (40% Cu) film was determined to be ≥75% at 550 nm. In conclusion, the transparent conductor figure of merit ($\Phi_{{\rm TC}}$ ) of the Cu alloyed ZnS (40% Cu), calculated with the average value of transmittance between 1.5 to 2.5 eV, was ≈276 $\mu{\rm S}$ .

36 MATERIALS SCIENCE↗

Sputtered Au–Ta films with tunable electrical resistivity

Gold–tantalum alloy films are attractive for hohlraums used in indirect drive magnetized inertial confinement fusion. A high electrical resistivity of over ~100 µΩ cm at cryogenic temperatures is an essential requirement for allowing an externally imposed pulsed magnetic field to soak through a hohlraum and magnetize the fusion fuel. In this work, we systematically study properties of Au–Ta alloy films in the entire compositional range from pure Au to pure Ta with thicknesses up to 30 µm. These films are made by direct current magnetron co-sputtering on planar substrates. Films are characterized by a combination of high-energy ion scattering, x-ray diffraction, electron microscopy, nanoindentation, and electrical transport measurements. Results show that an alloy with ~80 at.% of Ta forms a metallic glass exhibiting a maximum electrical resistivity of ~300 µΩ cm with a weak temperature dependence in the range of 5–400 K. The deposition of a film with ~80 at.% of Ta onto a sphero-cylindrical substrate for hohlraum fabrication is also demonstrated.

36 MATERIALS SCIENCE↗

Sputter-Deposited Oxides for Interface Passivation of CdTe Photovoltaics

Commercial CdTe PV modules have polycrystalline thin films deposited on glass, and devices made in this format have exceeded 22% efficiency. Devices made by the authors with a magnesium zinc oxide window layer and tellurium back contact have achieved efficiency over 18%, but these cells still suffer from an open-circuit voltage far below ideal values. Oxide passivation layers made by sputter deposition have the potential to increase voltage by reducing interface recombination. CdTe devices with these passivation layers were studied with photoluminescence (PL) emission spectroscopy and time-resolved photoluminescence (TRPL) to detect an increase in minority carrier lifetime. Because these oxide materials exhibit barriers to carrier collection, micropatterning was used to expose small point contacts while still allowing interface passivation. TRPL decay lifetimes have been greatly enhanced for thin polycrystalline absorber films with interface passivation. Device performance was measured and current collection was mapped spatially by light-beam-induced current.

14 SOLAR ENERGY↗

Phase transformation and growth mechanism of RF sputtered ferroelectric lead scandium tantalate (PbSc 0.5 Ta 0.5 O 3 ) films

Lead scandium tantalate (PbSc 0.5 Ta 0.5 O 3 , PST), an order/disorder ferroelectric, is a potential candidate for electrocaloric cooling and pyroelectric infrared (IR) detector. In this work, we report the phase transformation kinetics from two series of samples containing pure amorphous and mixture of amorphous and pyrochlore to desired perovskite phase using postdeposition rapid thermal processing (RTP) as well as growth mechanism of RF sputtered PST thin films using excess lead target on platinized silicon (Pt/Ti/SiO 2 /Si) substrates. We find that small changes in the temperature ramp have a large effect on the degree of perovskite conversion (ferroelectric phase), orientation (crystallographic texture), and long-range order parameter (< S 111 >). Through isothermal annealing, we obtained optimal perovskite phase at ≥700°C temperature. The phase transformation is characterized by spontaneous formation of center-type in-plane radial rosette-like structures revealed by scanning electron microscopy. The PST perovskite crystallites were found to coexist with pyrochlore in RTP annealed films. The volume fractions for perovskite and pyrochlore phase were obtained from the analysis of “rosettes” and respective X-ray diffraction intensities which helped to determine various parameters associated with phase kinetics (n, k, and activation energy, Ea) and accompanying growth. The effective activation energies of perovskite transition and growth were found to be 332 ± 11 kJ/mol (345 ± 11 kJ/mol) and 114 ± 10 kJ/mol (122 ± 10 kJ/mol), respectively, for pure amorphous only (and mixed amorphous and pyrochlore) phase following nucleation-growth controlled Avrami's equation. A linear growth rate (n~1) for the perovskite phase indicates predominant interface-controlled process and diffusion-limited phenomena thus inhibiting rosette size owing to reactant depletion and soft impingement at the grain boundary. However, the growth behavior is isotropic in two-dimension parallel to the plane of the substrates for both sample series. Furthermore, lead loss was severe for in-situ growth and RTP combined with conventional furnace annealing than those of RTP only films, which were closer to stoichiometric albeit with excess lead and marginal oxygen vacancies (V o ).

36 MATERIALS SCIENCE↗

Characterizing the composition, structure, and mechanical properties of magnetron sputtering physical vapor deposition TiN and TiSiN coatings

Ti(Si)N coatings were deposited on Si wafers via magnetron sputtering physical vapor deposition technique. Scanning electron microscopy and atomic force microscopy were used to study the morphologies, grain size, and thicknesses of the different films. X-ray diffraction confirmed the formation of the titanium nitride cubic phase. X-ray photoelectron spectroscopy (XPS) was used to study the silicon and oxygen levels in the films, and high resolution XPS was used to determine the surface oxide to nitride ratios as well as the silicon–nitrogen environment. The hardness of these films was then determined with nanoindentation. It was shown that grain size and film density could be controlled by the Si level and the ion bombardment to eliminate the oxygen level in the nitride coatings, which led to the harder films. It was suggested that due to the miscibility of Si, a ternary TiSiN solid solution was formed. Stronger (200) orientation of the TiN B1-NaCl crystals was associated with increased hardness of the coatings. In conclusion, this crystalline structure was preserved after incorporating Si.

36 MATERIALS SCIENCE↗

Boron carbide films with reduced nodular defect density deposited by full-face erosion radio-frequency magnetron sputtering

Boron carbide coatings deposited by sputtering with conventional planar magnetrons exhibit nodular growth defects. Here, we demonstrate that the density of nodular defects in B 4 C films can be greatly reduced by using a full-face-erosion magnetron source that achieves a more uniform target erosion by sweeping the confining magnetic field over the target surface. Here, we systematically study properties of B 4 C films deposited on substrates with different tilt angles and demonstrate deposition of ultrathick films with compressive residual stress below 200MPa.

36 MATERIALS SCIENCE↗

Parameters of ZnO films with p-type conductivity deposited by high-frequency magnetron sputtering

It is demonstrated that a reduction in the defect concentration in ZnO films formed by high-frequency magnetron sputtering allows effective doping with acceptor impurities both in the cation (Li) and anion (N{sup +}) sublattices and p-type conductivity with reproducible charge-carrier parameters (concentration and mobility) to be obtained. ZnO films are doped with nitrogen by annealing in a high-frequency gas discharge atmosphere. Hall measurements by the Van der Pauw technique show that the deposition of thin Eu layers on the ZnO film surface increases the concentration and mobility of majority charge carriers. The embedding of metal impurities with different ionic radii (Ag and Au) in the cation sublattice of the ZnO films to compensate misfit stresses makes it possible to enhance the concentration of radiative-recombination centers.

36 MATERIALS SCIENCE↗

Formation of Cu{sub 2}O and ZnO Crystal Layers by Magnetron Assisted Sputtering and Their Optical Characterization

Copper (I) oxide and zinc oxide films are formed on silicon and glassy quartz substrates by magnetron assisted sputtering. The thickness of the films is tens and hundreds of nanometers. The films are grown at different substrate temperatures and different oxygen pressures in the working chamber. The film samples are studied by the X-ray diffraction technique, scanning electron microscopy, and optical methods. It is established that an increase in the substrate temperature yields a change in the surface morphology of copper (I) oxide films towards the formation of well-pronounced crystallites. The reflectance and Raman spectra suggest that the quality of such films is close to that of bulk Cu{sub 2}O crystals produced by the oxidation of copper. As concerns ZnO films, an increase in the substrate temperature and an increase in the partial oxygen pressure make it possible to produce films, for which a sharp exciton structure is observed in the reflectance spectra and the emission of excitons bound at donors is observed in the luminescence spectra.

36 MATERIALS SCIENCE↗

Formation of Luminescence Spectra and Emission Intensity in the UV and Visible Spectral Regions for n-ZnO/p-GaN and n-ZnO/p-ZnO Structures when Depositing ZnO Films by High-Frequency Magnetron Sputtering

The emission spectra of structures based on ZnO films deposited by high-frequency magnetron sputtering are studied. Clearly pronounced emission lines associated with the recombination of free (λ = 363 nm) and bound excitons (λ = 377, 390, 410 nm) are observed in the PL (photoluminescence) spectra (T = 300 K) of n-ZnO/p-GaN:Mg structures, and no substantial emission is observed in the impurity PL region λ = 450–600 nm. Only emission lines characteristic of n-ZnO (λ = 374 nm) are observed in the EL (electroluminescence) spectra of n-ZnO/p-ZnO structures (T = 300 K).

36 MATERIALS SCIENCE↗

Luminescence and Stimulated Emission of Polycrystalline Cu(In,Ga)Se{sub 2} Films Deposited by Magnetron-Assisted Sputtering

The stimulated emission of Cu(In,Ga)Se{sub 2} alloy thin films formed by magnetron-assisted sputtering onto a sodium-fluoride layer deposited onto a molybdenum layer on a glass substrate is observed. The structural and optical parameters of the films are determined by scanning electron microscopy, local X-ray spectral microanalysis, X-ray structural analysis, and low-temperature luminescence (T = 10 K) measurements in the range of excitation levels of 1.6–75 kW cm{sup –2} provided by nanosecond nitrogen-laser pulses. The stimulated emission threshold corresponds to ~25 kW cm{sup –2}. Comparative analysis of the emission of Cu(In,Ga)Se{sub 2} thin films suggests that the introduction of sodium results in significant improvement of the structural quality, specifically, in a decrease in the density of energy states in the band tails and in a decrease in the concentration of nonradiative-recombination centers.

36 MATERIALS SCIENCE↗

Effect of the Temperature of Photonic Annealing on the Structural and Optical Properties of ZnO Films Synthesized by Dual Magnetron-Assisted Sputtering

Zinc-oxide films 1.4 μm in thickness are deposited onto glassy substrates by the dual magnetron-assisted sputtering of zinc targets in an argon and oxygen gas atmosphere. The dependences of the structural and optical characteristics of the ZnO films on the temperature of postdeposition photonic annealing are studied. It is established that an increase in the annealing temperature yields an increase in the degree of crystallinity of the films. Electron microscopy shows that the deposited ZnO coatings are columnar in structure and the microstructure density and crystallite size increase upon annealing. It is found that, at an annealing temperature of 450–650°C, the optical transmittance increases to >90% in the spectral range 400–1100 nm. The experimental results show that the temperature of vacuum photonic annealing has the most profound effect on the final properties of ZnO coatings.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗