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At least 397 records · Page 22

Sputtering of Metals by Mass-Analyzed N2(+) and N(+)

Low-energy sputtering studies were conducted with the help of a specially designed ion accelerator. A high-intensity rf ion source was developed for use in conjunction with electrostatic acceleration and magnetic mass separation of ion beams in the 0 to 8 kev energy range. Beams of N(+) or N2(+) ions have been produced with intensities of 200 to 500 micro-a (approx. 1 sq cm in cross section) and energy half-widths of about 20 ev. The sputtering yields of five metals (Cu, Ni, Fe, Mo, and W) were obtained as a function of energy (0-8 kev), bombarding ion (N(+) and N2(+)), and angle of incidence (normal and 450). Results are presented and some of their theoretical implications are discussed.

Bader, Michel↗

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↗

\A Gravity-Related Transport in Reactive Off-Axis Sputtering Deposition

An experiment was designed to investigate the transport characterization of reactive off- axis sputtering deposition. Three transport regions were observed when the growth pressures vary from 5 mtorr to 150 mtorr. A new gravity-related phenomenon was revealed in film growth at relatively high growth pressures. This effect is related to the collision process or thermalization of transport species. This study also suggests a design for the substrate holder orientation in the off-axis sputtering system.

Zhu, Shen↗

Gravity-Related Transport Process in Off-Axis Sputtering Deposition

In the synthesis of epitaxial oxide films, reactive off-axis sputtering deposition techniques have demonstrated the advantages of fabricating high quality epitaxial films. Due to the collisions between the sputtered species and the residue gases, the kinetic energy of species was reduced and the transport of depositing species changed from a ballistic movement to a diffusive drift in which the transport species were almost thermalized. A gravity effect could appear in the transport process. Three transport regimes were observed when the growth pressures vary from 5 mTorr to 150 mTorr. Film growth rate, depositing orientations, crystal structure, surface morphology, and compositions were characterized. A gravity related phenomenon was revealed in film growth at the relative low growth pressures.

Zhu, Shen↗

Fluoropolymer Films Deposited by Argon Ion-Beam Sputtering of Polytetrafluoroethylene

The FT-IR, XPS and UV spectra of fluoropolymer films (SPTFE-I) deposited by argon ion-beam sputtering of polytetrafluoroethylene (PTFE) were obtained and compared with prior corresponding spectra of fluoropolymer films (SPTFE-P) deposited by argon rf plasma sputtering of PTFE. Although the F/C ratios for SPTFE-I and -P (1.63 and 1.51) were similar, their structures were quite different in that there was a much higher concentration of CF2 groups in SPTFE-I than in SPTFE-P, ca. 61 and 33% of the total carbon contents, respectively. The FT-IR spectra reflect that difference, that for SPTFE-I showing a distinct doublet at 1210 and 1150 per centimeter while that for SPTFE-P presents a broad, featureless band at ca. 1250 per centimeter. The absorbance of the 1210-per centimeter band in SPTFE-I was proportional to the thickness of the film, in the range of 50-400 nanometers. The SPTFE-I was more transparent in the UV than SPTFE-P at comparable thickness. The mechanism for SPTFE-I formation likely involves "chopping off" of oligomeric segments of PTFE as an accompaniment to "plasma" polymerization of TFE monomer or other fluorocarbon fragments generated in situ from PTFE on impact with energetic Ar ions. Data are presented for SPTFE-I deposits and the associated Ar(+) bombarded PTFE targets where a fresh target was used for each run or a single target was used for a sequence of runs.

Golub, Morton A.↗

Loss of atmosphere from Mars due to solar wind-induced sputtering

Because Mars does not have a strong intrinsic magnetic field, the atmosphere is eroded by interactions with the solar wind. Early solar-system conditions enhanced the sputtering loss. It is calculated that approximately 3 bars of carbon dioxide (CO2) have been sputtered over the last 3.5 billion years. This significant increase over the previous estimate by Luhmann et al. of approximately 0.14 bar of CO2 is the result of the development of a more complete model. The model also predicts slightly greater loss of water--approximately 80 meters instead of the approximately 50 meters predicted by Luhmann et al. Because estimates of CO2 on early Mars range from 0.5 to 5 bars, the 0.14-bar estimate is insignificant but the approximately 3-bar estimate will have a large effect on our understanding of the planet's evolution.

NASA Discipline Exobiology↗

Transport of Sputtered Carbon During Ground-Based Life Testing of Ion Thrusters

High voltage, high power electron bombardment ion thrusters needed for deep space missions will be required to be operated for long durations in space as well as during ground laboratory life testing. Carbon based ion optics are being considered for such thrusters. The sputter deposition of carbon and arc vaporized carbon flakes from long duration operation of ion thrusters can result in deposition on insulating surfaces, causing them to become conducting. Because the sticking coefficient is less than one, secondary deposition needs to be considered to assure that shorting of critical components does not occur. The sticking coefficient for sputtered carbon and arc vaporized carbon is measured as well as directional ejection distribution data for carbon that does not stick upon first impact.

Marker, Colin L.↗

Kinetic and Potential Sputtering Enhancements of Lunar Regolith Erosion: The Contribution of the Heavy Multicharged (Minority) Solar Wind Constituents

We report preliminary results for H+, Ar+1, Ar+6 and Ar+9 ion sputtering of JSC-1A lunar regolith simulant at solar wind velocities, obtain ed at the ORNL Multicharged Ion Research Facility using quadrupole ma ss spectrometry. The multi-charged Ar ions were used as proxies for i ntermediate mass solar wind multicharged ions. Prior to the Ar beam e xposures, the sample was exposed to high fluence H+ irradiation to si mulate H-loading due to the dominant solar wind constituent. A x80 en hancement of oxygen sputtering by Ar+ over same velocity H+ was measu red and an additional x2 increase for Ar+9 over same velocity Ar+ was demonstrated, giving clear evidence of the importance of potential s puttering by multicharged ions. This enhancement was observed to pers ist to the maximum fluences investigated (approx 10(exp 16)/sq cm). As discussed in a companion abstract by N. Barghouty, such persistent s puttering enhancement has significant implications on weathering and aging of lunar regolith. In addition, XPS measurements showed strong evidence of Fe reduction for those target areas that had been exposed to high fluence Ar+ and Ar+8 beams. Preferential oxidation of the Fe -reduced beam-exposed regions during transfer to the XPS system led t o enhanced O concentrations in those regions as well. On the basis of these very promising preliminary results, a NASA-LASER project on mo re extensive measurements was recently selected for funding. The prop osal expands the collaboration with NASA-MSFC for the simulation effort, and adds a new collaboration with NASA-GSFC for lunar mission-rele vant measurements.

Meyer, F. W.↗

A Magnetron Sputter Deposition System for the Development of Multilayer X-Ray Optics

The proposal objective is to establish the capability to deposit multilayer structures for x-ray, neutron, and EUV optic applications through the development of a magnetron sputtering deposition system. A specific goal of this endeavor is to combine multilayer deposition technology with the replication process in order to enhance the MSFC's position as a world leader in the design of innovative X-ray instrumentation through the development of full shell replicated multilayer optics. The development of multilayer structures is absolutely necessary in order to advance the field of X-ray astronomy by pushing the limit for observing the universe to ever increasing photon energies (i. e. up to 200 keV or higher); well beyond Chandra (approx. 10 keV) and NuStar's (approx. 75 keV) capability. The addition of multilayer technology would significantly enhance the X-ray optics capability at MSFC and allow NASA to maintain its world leadership position in the development, fabrication and design of innovative X-ray instrumentation which would be the first of its kind by combining multilayer technology with the mirror replication process. This marriage of these technologies would allow astronomers to see the universe in a new light by pushing to higher energies that are out of reach with today's instruments.To this aim, a magnetron vacum sputter deposition system for the deposition of novel multilayer thin film X-ray optics is proposed. A significant secondary use of the vacuum deposition system includes the capability to fabricate multilayers for applications in the field of EUV optics for solar physics, neutron optics, and X-ray optics for a broad range of applications including medical imaging.

Broadway, David↗

A Magnetron Sputter Deposition System for the Development of X-Ray Multilayer Optics

The project objective is to establish the capability to deposit multilayer structures for x-ray, neutron, and extreme ultraviolet (EUV) optic applications through the development of a magnetron sputtering deposition system. A specific goal of this endeavor is to combine multilayer deposition technology with the replication process in order to enhance NASA Marshall Space Flight Center's (MSFC's) position as a world leader in the design of innovative x-ray instrumentation through the development of full shell replicated multilayer optics. The development of multilayer structures are absolutely necessary in order to advance the field of x-ray astronomy by pushing the limit for observing the universe to ever-increasing photon energies (i.e., up to 200 keV or higher), well beyond Chandra's (approx.10 keV) and NuStar's (approx.75 keV) capability. The addition of multilayer technology would significantly enhance the x-ray optics capability at MSFC and allow NASA to maintain its world leadership position in the development, fabrication, and design of innovative x-ray instrumentation, which would be the first of its kind by combining multilayer technology with the mirror replication process. This marriage of these technologies would allow astronomers to see the universe in a new light by pushing to higher energies that are out of reach with today's instruments. To this aim, a magnetron vacuum sputter deposition system for the deposition of novel multilayer thin film x-ray optics is proposed. A significant secondary use of the vacuum deposition system includes the capability to fabricate multilayers for applications in the field of EUV optics for solar physics, neutron optics, and x-ray optics for a broad range of applications including medical imaging.

Broadway, David↗

First Results From Nb3Sn Coatings of 2.6 GHz Nb SRF Cavities Using DC Cylindrical Magnetron Sputtering System

A DC cylindrical magnetron sputtering system has been commissioned and operated to deposit Nb3Sn onto 2.6 GHz Nb SRF cavities. After optimizing the deposition conditions in a mock-up cavity, Nb-Sn films are deposited first on flat samples by multilayer sequential sputtering of Nb and Sn, and later annealed at 950°C for 3 hours. X-ray diffraction of the films showed multiple peaks for the Nb3Sn phase and Nb (substrate). No peaks from any Nb- Sn compound other than Nb3Sn were detected. Later three 2.6 GHz Nb SRF cavities are coated with ~1 μm thick Nb3Sn. The first Nb3Sn coated cavity reached close to Eacc = 8 MV/m, demonstrating a quality factor Q0 of $3.2 \times 108$ at Tbath = 4.4 K and Eacc = 5 MV/m, about a factor of three higher than that of Nb at this temperature. Q0 was close to $1.1 \times 109$, dominated by the residual resistance, at 2 K and Eacc = 5 MV/m. The Nb3Sn coated cavities demonstrated Tc in the range of $17.9 -- 18$ K. Here we present the commissioning experience, system optimization, and the first results from the Nb3Sn fabrication on flat samples and SRF cavities.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

First Results from Nb3Sn Coatings of 2.6 GHz Nb SRF Cavities Using DC Cylindrical Magnetron Sputtering System

A DC cylindrical magnetron sputtering system has been commissioned and operated to deposit Nb3Sn onto 2.6 GHz Nb SRF cavities. After optimizing the deposition conditions in a mock-up cavity, Nb-Sn films are deposited first on flat samples by multilayer sequential sputtering of Nb and Sn, and later annealed at 950 {\deg}C for 3 hours. X-ray diffraction of the films showed multiple peaks for the Nb3Sn phase and Nb (substrate). No peaks from any Nb3Sn compound other than Nb3Sn were detected. Later three 2.6 GHz Nb SRF cavities are coated with ~1 $\mu$m thick Nb3Sn. The first Nb3Sn coated cavity reached close to Eacc = 8 MV/m, demonstrating a quality factor Q0 of 3.2 x 108 at Tbath = 4.4 K and Eacc = 5 MV/m, about a factor of three higher than that of Nb at this temperature. Q0 was close to 1.1 x 109, dominated by the residual resistance, at 2 K and Eacc = 5 MV/m. The Nb3Sn coated cavities demonstrated Tc in the range of 17.9 - 18 K. Here we present the commissioning experience, system optimization, and the first results from the Nb3Sn fabrication on flat samples and SRF cavities.

43 PARTICLE ACCELERATORS↗

Superlattice-Structured Films by Magnetron Sputtering as New Era Electrodes for Advanced Lithium-ion Batteries

Sustaining sound structures in Si-based anodes is extremely challenging because of the high volumetric expansion that occurs upon cycling. To maintain high capacities over cycles, new designs rely on engineering-specific hierarchical geometries and/or optimized composite compositions such that at least one of the multiple elements serves as buffer and/or electron conductive pathways in the electrodes. In this paper, we report an innovative design in which alternating layers of periodic atomic structures involving multiple elements form a new anode material for lithium-ion batteries. In this work, a superlattice-structured amorphous film made using Si, Mo, and Cu is fabricated by a simple and scalable magnetron sputtering process for the first time. This continuous and repetitive superlattice formation along the film thickness provides a homogeneous stress-strain distribution. The Mo-Cu layer in the superlattice acts as an inactive-conductive layer and as a backbone to handle the volume expansion of active Si upon cycling. This nano-functional superlattice approach enables harnessing the high energy density of Si while maintaining its structural stability. As a result, the electrode exhibits high specific capacity and capacity retention even at high cycling rates. The possible use of the film in a full cell is also evaluated by cycling it vs. the LiMn 1.5 Ni 0.5 O 4 cathode. The full cell maintains a stable capacity of about 900 mAh g anode -1 over 150 cycles, at ~600 mA g -1 rate. The remarkable performance of this nano-functional superlattice film is found to be promising as anodes for applications that require high energy, long calendar life, and excellent abuse tolerance such as electric vehicle batteries.

25 ENERGY STORAGE↗

Reactive phosphine combinatorial co-sputtering of cation disordered ZnGeP2 films

The discovery of new materials by coupling high-throughput synthesis with computational screening is being increasingly adopted. However, thus far, phosphides have been largely overlooked for both computational screening and high-throughput synthesis. In this paper, we report on the use of a high-throughput synthesis technique, reactive combinatorial co-sputtering with PH 3 , to deposit ZnGeP 2 thin films. We grew amorphous films over a wide range of compositions and found an upper limit in growth temperature determined by Zn and P volatility. We found that depositing in a Ge-limited regime could be utilized to slow the growth rate to compensate for the desorption of the Zn and P. Crystalline films were achieved by depositing films at higher temperatures in this Ge-limited regime with a reduced deposition rate. X-ray diffraction revealed that the films had crystallized in the zinc blende, cation-disordered structure. The crystalline films exhibited optical absorption energy threshold values ranging from 0.8 to 1.3 eV. Increased Ge content was found in films that exhibited a decreased absorption onset energy. Native defect calculations were used to gain an understanding of the off-stoichiometry seen in these films. This work provides the first high-throughput investigation of ZnGeP 2 , demonstrating the ability to grow amorphous and cation disordered ZnGeP 2 over a wide range of compositions with varying optical properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Experimental and theoretical study of hole scattering in RF sputtered p-type Cu 2 O thin films

One of the key materials of interest for p-type oxide semiconductor thin film electronics is cuprous oxide (Cu 2 O), due to its relatively high hole mobility. Here, in this work, we use experiments, analytical models, and density functional theory calculations to study the scattering mechanisms that determine Hall mobility in two Cu 2 O samples. First, we examine a polycrystalline Cu 2 O thin film deposited by RF magnetron sputtering, and second, a single-crystalline Cu2O bulk substrate. Temperature-dependent Hall measurements indicate that neutral impurity and grain boundary scattering are dominant for the polycrystalline Cu 2 O thin film, while phonon scattering is dominant for single-crystalline Cu 2 O. Our first-principles calculations show that the room-temperature intrinsic hole mobility of Cu 2 O is 106 cm 2 V –1 s –1 , indicating the great promise of the material for p-type electronic devices. This intrinsic mobility is limited by phonon scattering, with the most dominant scattering modes having phonon energies of 88.4 and 17.1 meV. These results indicate that the key pathways to increase the hole mobility in Cu 2 O thin films are by reducing the impurity concentration and by increasing grain size. Our work thus sets the stage for the future development of high performance Cu 2 O-based p-type thin film transistors.

36 MATERIALS SCIENCE↗

Nanocolumnar Pt:Ni Alloy Thin Films by High Pressure Sputtering for Oxygen Reduction Reaction

Self-supported nanocolumnar Pt:Ni thin films (TFs) with varying Pt:Ni atomic ratios and Pt mass loadings were produced on a microporous layer (MPL)-like surface composed of carbon particles by high pressure sputtering and examined as oxygen reduction reaction (ORR) electrocatalysts for polymer electrolyte membrane fuel cells. Cauliflower-like microstructures were observed from scanning electron microscopy imaging. Various Pt:Ni atomic ratios were obtained by simply changing the relative deposition power between Pt and Ni source and investigated by X-ray diffraction and quartz crystal microbalance analysis. Additionally, electrochemical characterization of the Pt:Ni-TF/MPL-like-layer/glassy-carbon samples was conducted through benchtop cyclic voltammetry and rotating disk electrode measurements. The electrochemically active surface area (ECSA) was found to be between 22–42 m 2 g -1 for different Pt:Ni atomic ratios. Lower Pt mass loadings exhibited a higher ECSA and the catalytic activity of all Pt:Ni ratios increased with the increase in Pt mass loading. The ORR activity of the Pt:Ni-TFs increased in the order of 3:1 < 1:1 < 1:3 with exhibiting a specific activity of 1781 μA cm -2 and mass activity of 0.66 A mg -1 for the Ni-rich film with 1:3 ratio. The catalytic performance of Pt:Ni-TFs were higher than traditional high surface area carbon supported Pt nanoparticles, elemental Pt nanorods, and Pt-Ni nanorods.

08 HYDROGEN↗

Boron Phosphide Films by Reactive Sputtering: Searching for a P‐Type Transparent Conductor

Abstract With an indirect band gap in the visible and a direct band gap at a much higher energy, boron phosphide (BP) holds promise as an unconventional p‐type transparent conductor. This work reports on reactive sputtering of amorphous BP films, their partial crystallization in a P‐containing annealing atmosphere, and extrinsic doping by C and Si. The highest hole concentration to date for p‐type BP (5 × 10 20 cm −3 ) is achieved using C doping under B‐rich conditions. Furthermore, bipolar doping is confirmed to be feasible in BP. An anneal temperature of at least 1000 °C is necessary for crystallization and dopant activation. Hole mobilities are low and indirect optical transitions are stronger than that predicted by theory. Low crystalline quality probably plays a role in both cases. High figures of merit for transparent conductors might be achievable in extrinsically doped BP films with improved crystalline quality.

36 MATERIALS SCIENCE↗

Understanding Reproducibility of Sputter‐Deposited Metastable Ferroelectric Wurtzite Al 0.6 Sc 0.4 N Films Using In Situ Optical Emission Spectrometry

High‐Sc Al 1– x Sc x N thin films are of tremendous interest because of their attractive piezoelectric and ferroelectric properties, but overall film quality and reproducibility are widely reported to suffer as x increases. In this study, structural and electrical properties of metastable Al 0.6 Sc 0.4 N films are connected with plasma changes during film growth, identified via glow discharge optical emission spectroscopy (GD‐OES), and linked to the target mode changes. This in situ GD‐OES technique uses changes in the N 2 (I) intensity, correlated with DC bias hysteresis behavior of a Al 0.6 Sc 0.4 target in metallic and poisoned modes, to identify films that subsequently exhibit unacceptable structural and electrical performance. Two representative samples deposited under identical conditions but possessing distinct properties related to phases present in the films are focused on. Films sputtered under a poisoned target mode produce pure wurtzite ferroelectric Al 0.6 Sc 0.4 N with a reversible 80 μC cm −1 polarization and 3.1 MV cm −1 coercive field. When identical chamber settings are used but the process starts in metallic mode, a mixed wurtzite/rocksalt film is deposited which exhibits nanometer‐scale changes to the film microstructure and a nonferroelectric response. These results illustrate the utility of optical emission spectroscopy for tracking target mode fluctuations when fabricating metastable materials such as high‐Sc Al 1– x Sc x N films.

36 MATERIALS SCIENCE↗