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All sourcesNASA NTRSDOE OSTI
NASA NTRS2015

Achieving Zero Stress in Iridium, Chromium, and Nickel Thin Films

We examine a method for achieving zero intrinsic stress in thin films of iridium, chromium, and nickel deposited by magnetron sputter deposition. The examination of the stress in these materials is motivated by efforts to advance the optical performance of light-weight x-ray space telescopes into the regime of sub-arc second resolution that rely on control of the film stress to values within 10-100 MPa. A characteristic feature of the intrinsic stress behavior in chromium and nickel is their sensitivity to the magnitude and sign of the intrinsic stress with argon gas pressure, including the existence of a critical pressure that results in zero film stress. This critical pressure scales linearly with the film's density. While the effect of stress reversal with argon pressure has been previously reported by Hoffman and others for nickel and chromium, we have discovered a similar behavior for iridium. Additionally, we have identified zero stress in iridium shortly after island coalescence. This feature of film growth is used for achieving a total internal stress of -2.89 MPa for a 15.8 nm thick iridium film. The surface roughness of this low-stress film was examined using scanning probe microscopy (SPM) and x-ray reflectivity (XRR) at CuKα and these results presented and discussed.

X-ray↗
NASA NTRS1984

Corrosion behavior of magnetron sputter-deposited (Mo/0.6/Ru/0.4/)82B18 and Mo82B18 amorphous metal films

Amorphous metallic films of Mo49Ru33B18 and Mo82B18 have been prepared by magnetron sputtering, and their corrosion behavior was investigated and compared with amorphous liquid-quenched Mo49Ru33B18 and crystalline Mo i acidic and basic solutions. Sputtered Mo49Ru33B18 showed lower corrosion rates compared with liquid-quenched Mo49Ru33B18, owing to the superior surface smoothness and uniformity of the former. Amorphous Mo82B18 showed low corrosion rates in both acidic and basic aqueous solutions. Comparison of the corrosion properties of Mo49Ru33B18 with Mo82B18 and Mo demonstrates the roles of the alloys' constituents. Ru significantly extends the passive region to high-anodic potentials, but, at less-anodic potentials, Mo82B18 has the lowest corrosion rate.

Williams, R. M.↗
DOE OSTI2023

Commissioning of a two-target DC cylindrical magnetron sputter coater for depositing Nb 3 Sn film on Nb superconducting radiofrequency cavities

A DC cylindrical magnetron sputter coater was commissioned and used to coat Nb 2.6 GHz superconducting radiofrequency (SRF) cavity with Nb 3 Sn. The sputter coater has two identical cylindrical magnetrons that can move, with a controlled speed, along the axis of the SRF cavity to coat the inside surface of the cavity. The design of the sputter coater is discussed, along with its performance. Initially, a sample holder that allows coating on flat substrates at positions similar to the equator and beam tubes of a 2.6 GHz SRF cavity was used to test conditions for fabricating Nb 3 Sn layers. Multilayers of Nb and Sn were sequentially sputtered on flat Nb and sapphire substrates mounted on the equivalent positions of the cavity's beam tubes and the equator using the two identical cylindrical magnetrons. Then, the Nb/Sn multilayers were annealed at 950 °C for 3 h. Here, the ~1.2 μm thick Nb 3 Sn film did not show any other Nb–Sn compounds and had a superconducting transition temperature of 17.61–17.76 K. The 2.6 GHz SRF cavity was coated using similar conditions as flat samples. Cryogenic RF testing of the Nb 3 Sn-coated cavity demonstrated a quality factor of 3.2 × 10 8 at an accelerating gradient of 5 MV/m at 4.4 K.

43 PARTICLE ACCELERATORS↗
DOE OSTI2022

Lithium nitride coatings deposited by magnetron sputtering on sulfide electrolytes for solid-state batteries

Lithium nitrides have been considered as promising candidates for interfacial layers in solid-state lithium batteries (SSBs). Previously reported lithium nitride (Li 3 N) coatings were mostly prepared by the reaction between lithium metal and nitrogen gas, which makes it challenging for their thickness control and integration in SSBs. In this study, we prepare Li 3 N via magnetron sputtering for the first time, and apply the resulting coating directly on sulfide solid-state electrolyte. A much smaller impedance increase associated with improved cycling performance is observed in lithium metal symmetric cell. These results demonstrate the feasibility of depositing Li 3 N via magnetron sputtering and its application in SSBs.

25 ENERGY STORAGE↗
DOE OSTI2022

Tantalum Suboxide Films with Tunable Composition and Electrical Resistivity Deposited by Reactive Magnetron Sputtering

Tantalum-based films with tailored composition, density, and electrical resistivity are of interest for next generation hohlraums for magnetized indirect-drive inertial confinement fusion. Here, we use reactive direct-current magnetron sputtering to deposit tantalum suboxide films with O content in the range of 46–71 at.%. In contrast to a common approach involving varying reactive gas contents, compositional control is achieved kinetically by changing the total chamber pressure and the deposition rate, while keeping the working gas mix of Ar-5%O2 constant. The resultant films are X-ray amorphous with electrical resistivity varying by over seven orders of magnitude. The dominant conduction mechanism changes from metallic to activated tunneling above ∼55 at.% of O, which is characterized by a sharp increase in resistivity and a decrease in the carrier density at low temperatures.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Effects of sample bias on adhesion of magnetron sputtered Cr coatings on SiC

Swelling of SiC at 300 C due to in-service neutron irradiation causes tensile residual stresses in coatings which are expected to adversely affect the performance of coated SiC composite fuel cladding for light water reactors. Matching the coating swelling with the substrate, a solution common for thermal expansion, is not practical in the case of neutron irradiation. Biasing samples during magnetron sputtering deposition induces compressive residual stress which may counteract this. In this study, chromium coatings were deposited on SiC by DC magnetron sputtering with no external heating at bias voltages of –50V, –75V, and –100V. The effects of the bias voltage on morphology, residual stress, microstrain, texture, and adhesion are shown. The low deposition temperature resulted in the coating microstructure evolution following an energetic particle bombardment dominated trend. Additionally, at the two lower bias voltages knock-on implantation dominated increasing the residual stress and microstrain while at the highest bias voltage, thermal spike migration allowed for defect relaxation. When the knock-on induced compressive residual stress exceeded 0.8 GPa microcrack formation in the SiC substrate decreased coating adhesion. While no microcracks formed at the lowest bias voltage, insufficient atomic mobility during coating growth lead to voids forming in the coating. A balance is needed to form void-free coatings that have high compressive residual stress.

36 MATERIALS SCIENCE↗
NASA NTRS1990

Investigation of buried homojunctions in p-InP formed during sputter deposition of both indium tin oxide and indium oxide

While dc magnetron sputter deposition of indium tin oxide leads to the formation of a buried homojunction in single crystal p-type InP, the mechanism of type conversion of the InP surface is not apparent. In view of the recent achievement of nearly 17-percent global efficiencies for cells fabricated solely by sputter deposition of In2O3, it is presently surmised that tin may not be an essential element in type conversion. A variety of electrical and optical techniques are presently used to evaluate the changes at both indium tin oxide/InP and indium oxide/InP interfaces. Such mechanisms as the passivation of acceptors by hydrogen, and sputter damage, are found to occur simultaneously.

Gessert, T. A.↗
NASA NTRS1990

Buried homojunction solar cells formed in p-InP during sputter deposition and hydrogen plasma processing

Although it is apparent that direct current (DC) magnetron sputter deposition of indium tin oxide (ITO) leads to the formation of a buried homojunction in single-crystal p-type InP, the actual mechanism of type conversion of the InP surface is not clear. Since sputter deposition of In2O3 has also led to high-quality cells, it appears that Sn is not the cause of type conversion. To investigate the junction formation process further, experiments involving the use of a pure hydrogen plasma have been performed, resulting in type conversion of Fe-doped InP surfaces and in solar cells with efficiencies over 16 percent (global). The results confirm that sputter deposition is not necessary to form this type of buried homojunction solar cell, and they suggest a fabrication process that may be used with other relevant photovoltaic materials.

Gessert, T. A.↗
DOE OSTI2023

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↗
DOE OSTI2024

Commissioning of a modulated pulse-power magnetron sputtering system for depositing niobium thin films

A modulated pulse-power magnetron sputtering system (MPPMS) was commissioned and used to deposit niobium on copper. MPPMS utilizes a modulated pulse train with high peak-to-average energy ratios, thereby increasing the energy density leading to the production of the energetic ions. The MPPMS modulator was designed and constructed based on large voltage/current IGBT modules, which can be externally modulated, produce bi-polar waveforms, and are readily available. A high voltage power supply provides moderate current to the IGBT module to create the precise pulse structure. The MPPMS system was used to deposit ~1 mm thick, niobium film on a copper substrate held at ~77 K to minimize Nb atom surface diffusion and maximize intrinsic film energy. Finally, the Nb film had an average grain size of ~8 nm.

42 ENGINEERING↗
NASA NTRS1999

Pressure Effect in ZnO Films Using Off-Axis Sputtering Deposition

ZnO films are deposited on (0001) sapphire, (001) Si and quartz substrates using the off-axis reactive magnetron sputtering deposition. Based on film thickness measurements, three transport regions of sputtered particles are observed when films are deposited in the pressure regions of 5 mtorr - 150 mtorr. X-ray diffraction, scanning probes microscopy, and electrical measurements are also used to characterize these films. The full width at half maximum of theta rocking curves for epitaxial films is less than 0.5 deg. In textured films, it rises to several degrees. The epitaxial films deposited at high pressure reveal a flat surface with some hexagonal facets. The density of hexagonal facets decreases when the growth pressure is reduced. The resistivity of these epitaxial films also depends on the growth pressures. A relationship between the pressure effects and film properties are discussed.

Zhu, Shen↗
DOE OSTI2021

Functionalized carbon nanotubes for thermionic emission and cooling applications

Barium strontium oxide-coated carbon nanotubes (CNTs) were implemented as a work function lowering and field enhancing functional coating on a coiled tungsten filament to create a new thermionic cathode. This cathode resembles conventional oxide cathodes in structure. It has the same coiled tungsten filament as a conventional oxide cathode but uses barium strontium oxide-coated CNTs instead of the traditional barium strontium calcium oxide powder mixture as an emissive coating. The cathode produces a strong thermionic emission. At 1395 K and 2.5 V/μm, the thermionic emission current of 0.87 A or current density of 2.9 A/cm 2 was obtained from this oxide-coated CNT cathode. This level of emission is about three times as large as a conventional oxide cathode operating at similar temperature and field strength. Strong thermionic emissions from the cathode also lead to a large thermionic cooling effect. Temperature reduction as large as 90° was observed from the cathode surface when it was emitting electrons. Strong thermionic emission and a large cooling effect obtained are the result of the combination of the low work function of barium strontium oxide (1.6 eV) and the large field effect induced by the CNTs. Plasma enhanced chemical vapor deposition was used to grow CNTs, and magnetron sputtering deposition was used to deposit the barium strontium oxide functional coating; details of the cathode fabrication are presented to illustrate both the versatility of the processing techniques and the adaptability of barium strontium oxide-coated CNTs as a functional coating. Finally, measurements on thermionic emission and thermionic cooling of the cathode are also presented.

36 MATERIALS SCIENCE↗
NASA NTRS1986

Influence of process parameter variation on the reflectivity of sputter-deposited W-C multilayer diffraction gratings

Multilayer W-C diffraction gratings with nominal d spacings of 35 A have been fabricated by magnetron sputter deposition. The peak and integrated reflectivities of these films have been measured with Al K-alpha X-rays and compared to theoretical values. The rms surface roughness has been evaluated. The influence of several sputtering-system process parameters on the reflectivities has been investigated.

Sager, B.↗
DOE OSTI2020

Sputter-deposited low-stress boron carbide films

Significant challenges have been faced in the manufacturing of low-stress B 4 C films. Here, we demonstrate a set of process parameters for direct-current magnetron sputter deposition of smooth, high-purity, amorphous B 4 C films with near-zero total residual stress and with thicknesses up to 10 μm. Films are characterized by a combination of high-energy ion scattering, x-ray diffraction, electron microscopy, and stress measurements based on substrate curvature. In order to facilitate the process transfer to other sputtering geometries, the favorable deposition conditions are correlated with distributions of landing energies and incident angles of depositing species estimated by Monte Carlo simulations of ballistic collisions and gas phase atomic transport. Based on such simulations, a decrease in compressive stress with increasing Ar working gas pressure is attributed to the corresponding broadening of the angular distribution of depositing species and associated atomic shadowing effects.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Sputter deposition of high electrical resistivity Au-Ta alloy coatings on rotating substrates

Sputter deposition of gold-tantalum alloy coatings is a key process for manufacturing hohlraums for magnetically-assisted inertial confinement fusion implosions. In this report we describe direct current magnetron sputter deposition of ~ 10 - μ~ 10 - μm-thick films of Au-80 at.% Ta onto rotating sphero-cylindrical hohlraum and planar Si witness substrates. Emphasis is given to how film microstructure and properties are affected by main deposition parameters, including argon working gas pressure, substrate bias, and the source composition (a single alloyed target compared to co-sputtering from two elemental targets). Experimental findings are correlated with distributions of landing energies and incident angles of depositing species calculated by Monte Carlo simulations of ballistic collisions and gas phase atomic transport. Deposition conditions characterized by low energetics of depositing species favor the formation of a β-Ta-like phase. Implications of these results to hohlraum fabrication are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Preparation of ultrathin sputtered gold films on palladium as efficient oxygen reduction electro-catalysts

Herein, we present the preparation of ultrathin gold (Au) films on different M (M = Pd, Pt, Rh, Ir, and Ru) electrodes (Au/M) using magnetron sputtering deposition for oxygen reduction reaction (ORR). The ORR electro-catalytic activities of prepared Au/M catalysts increase as follows: Au/Ru < Au/Ir < Au/Rh < Au/Pt < Au/Pd. Accordingly, the oxygen reduction catalytic behaviors of the Au-modified palladium (Au/Pd) thin films with various Au thicknesses (0.16, 0.24, 0.5, and 1 nm) are investigated in acidic environments. It is found that Au modifications can promote oxygen reduction performances due to the development of more catalytic active sites on the Pd catalyst through the existence of Au atoms. Noticeably, Au/Pd samples exhibit a connection in oxygen reduction ability as a function of Au thickness, with the ultrathin 0.16 nm Au/Pd being the most active ORR catalyst. Significantly, the 0.16 nm Au/Pd material demonstrates superior stability after 1000 potential cycles compared with the 0.16 nm Pt/Pd owing to the influence of Au coating and structurally stable surfaces. Therefore, surface modification with the deposition of Au films on Pd represents a favorable technique to boost both the ORR capability and stability of the electro-catalysts.

Magnetron sputtering↗
NASA NTRS1983

Influence of the microstructure on the corrosion behavior of magnetron sputter-quenched amorphous metallic alloys

The microstructure and corrosion behavior of magnetron sputter deposited amorphous metallic films of (Mo6ORu40)82B18 under varying sputtering atmospheres have been investigated. The microstructural details and topology of the films have been studied by scanning electron microscopy and correlated with the deposition conditions. By reducing the pressure of pure argon gas, the characteristic features of rough surface and columnar growth full of vertical voids can be converted into a mirror-smooth finish with very dense deposits. Films deposited in the presence of O2 or N2 exhibit columnar structure with vertical voids. Film deposited in pure argon at low pressure show remarkably high corrosion resistance due to the formation of a uniform passive surface layer. The influence of the microstructure and surface texture on the corrosion behavior is discussed.

Thakoor, A. P.↗