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At least 217 records · Page 12

Deposition of diamond-like films by ECR microwave plasma

Hard amorphous hydrogenated carbon, diamond-like films are deposited using an electron cyclotron resonance microwave plasma with a separate radio frequency power bias applied to a substrate stage. The electron cyclotron resonance microwave plasma yields low deposition pressure and creates ion species otherwise unavailable. A magnetic mirror configuration extracts special ion species from a plasma chamber. Different levels of the radio frequency power bias accelerate the ion species of the ECR plasma impinging on a substrate to form different diamond-like films. During the deposition process, a sample stage is maintained at an ambient temperature of less than 100.degree. C. No external heating is applied to the sample stage. The deposition process enables diamond-like films to be deposited on heat-sensitive substrates.

Shing, Yuh-Han↗

The use of metalorganics in the preparation of semiconductor materials. VIII - Feasibility studies of the growth of Group III-Group V compounds of boron by MOCVD

The MOCVD growth of B-As and B-P films on Si, sapphire, and Si-on-sapphire substrates is described; in this process, trimethylborane (TMB) or triethylborane (TEB) is pyrolyzed in the presence of AsH3 or PH3 in an H2 atmosphere. The procedures employed are outlined, and the results are presented in graphs, tables, and micrographs. It is found that the growth rate of the primarily amorphous films is dependent on the TMB or TEB concentration but approximately constant for TEB and AsH3 at 550-900 C. The nominal compositions of films grown using TMB are given as B(12-16)As2 and B(1-1.3)P. Carbon impurities and significant stress, bowing, and crazing are observed in the films grown on Si substrates, with the highest carbon content in the films grown from TMB and PH3.

Manasevit, H. M.↗

Thermal conductivity measurement of the interaction layer between UMo and Al produced by high-energy heavy ion irradiation

In this work, we report the first direct thermal conductivity measurement results for Al-UMo interaction layer (IL), which is typically observed in UMo/Al dispersion fuel plates under irradiation. The investigated IL was formed by irradiating Al coated UMo substrate using 80 MeV iodine ions at 180 degrees C up to 3.03 x 10 17 ions/cm 2 fluence. Microstructural characterization indicated that the induced IL is amorphous with an approximately (U 0.8 ,Mo 0.2 )Al 5.3 stoichiometry, which is similar to that formed under in-pile irradiation. Focused ion beam (FIB) was used to prepare nine specimens of various lengths from the IL that could be suspended across a microfabricated device for thermal conductivity measurement. The measured thermal conductivity values of the IL were significantly lower than the values for both the original UMo fuel and the Al. The successful measurement of the Al-UMo IL provides valuable information for the development and qualification of UMo/Al dispersion fuels for research and test reactor conversion applications, and further demonstrates the promising capabilities of utilizing the suspended bridge method in nuclear fuel research.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

First Demonstration on Direct Laser Fabrication of Lunar Regolith Parts

Establishment of a lunar or Martian outpost necessitates the development of methods to utilize in situ mineral resources for various construction and resource extraction applications. Fabrication technologies are critical for habitat structure development, as well as repair and replacement of tools and parts at the outpost. Herein we report the direct fabrication of lunar regolith simulant parts, in freeform environment, using lasers. We show that raw lunar regolith can be processed at laser energy levels as a low as 2.12 J mm-2 resulting in nanocrystalline and/or amorphous microstructures. Potential applications of laser based fabrication technologies to make useful regolith parts for various applications including load bearing composite structures, radiation shielding, and solar cell substrates is described.

Balla, Vamsi Krishna↗

Photovoltaic properties of ferroelectric BaTiO3 thin films RF sputter deposited on silicon

Ferroelectric thin films of BaTiO3 have been successfully deposited on n-type silicon substrates at temperatures above 500 C by RF sputtering in an O2/Ar atmosphere. Analysis by X-ray diffraction patterns show that films deposited at room temperature are amorphous. At temperatures above 500 C, crystalline BaTiO3 films with a tetragonal structure are obtained. The polarization-electric field (P-E) hysteresis loops and a broad peak in the dielectric constant versus temperature curve at Curie point indicate that the RF sputtered BaTiO3 films are ferroelectric. An anomalous photovoltaic effect is observed in these thin films which is related to the remanent polarization of the material. The results on open-circuit and short-circuit measurements provide an important basis for a better understanding of the role of photovoltaic field, photovoltaic current, and the pyroelectric properties in photoferroelectric domain switching.

Dharmadhikari, V. S.↗

Study of the Staebler-Wronski degradation effect in a-Si:H based p-i-n solar cell

Conversion of solar energy into electricity using environmentally safe and clean photovoltaic methods to supplement the ever increasing energy needs has been a cherished goal of many scientists and engineers around the world. Photovoltaic solar cells on the other hand, have been the power source for satellites ever since their introduction in the early sixties. For widespread terrestrial applications, however, the cost of photovoltaic systems must be reduced considerably. Much progress has been made in the recent past towards developing economically viable terrestrial systems, and the future looks highly promising. Thin film solar cells offer cost reductions mainly from their low processing cost, low material cost, and choice of low cost substrates. These are also very attractive for space applications because of their high power densities (power produced per kilogram of solar cell pay load) and high radiation resistance. Amorphous silicon based solar cells are amongst the top candidates for economically viable terrestrial and space based power generation. Despite very low federal funding during the eighties, amorphous silicon solar cell efficiencies have continually been improved - from a low 3 percent to over 13 percent now. Further improvements have been made by the use of multi-junction tandem solar cells. Efficiencies close to 15 percent have been achieved in several labs. In order to be competitive with fossil fuel generated electricity, it is believed that module efficiency of 15 percent or cell efficiency of 20 percent is required. Thus, further improvements in cell performance is imperative. One major problem that was discovered almost 15 years ago in amorphous silicon devices is the well known Staebler-Wronski Effect. Efficiency of amorphous silicon solar cells was found to degrade upon exposure to sunlight. Until now their is no consensus among the scientists on the mechanism for this degradation. Efficiency may degrade anywhere from 10 percent to almost 50 percent within the first few months of operation. In order to improve solar cell efficiencies, it is clear that the cause or causes of such degradation must be found and the processing conditions altered to minimize the loss in efficiency. This project was initiated in 1987 to investigate a possible link between metallic impurities, in particular, Ag, and this degradation. Such a link was established by one of the NASA scientists for the light induced degradation of n+/p crystalline silicon solar cells.

Naseem, H. A.↗

Synthesis and characterization of amorphous Fe2.75Dy-oxide thin films demonstrating room-temperature semiconductor, magnetism, and optical transparency

Recently, amorphous/disordered oxide thin films made from Fe and lanthanides like Dy and Tb have been reported to have a rich set of magnetic, optical, and electronic properties, as well as room-temperature magneto-electric coupling with multiferroics [A. Malasi et al., Sci. Rep. 5, 18157 (2015); H. Taz et al., Sci. Rep. 6, 27869 (2016); and H. Taz et al., Sci. Rep. 10, 1–10 (2020)]. Here, we report the synthesis and detailed characterization of Fe2.75Dy-oxide thin films prepared on various substrates using electron beam co-evaporation. The structure, chemistry, electric, magnetic, and optical properties were studied for the as-prepared and annealed (373 K, in air, 1 h) films of thickness 40 nm. High resolution transmission electron microscopy and electron diffraction study showed that the films were amorphous in both the as-prepared and annealed states. The electron energy-loss spectroscopy studies quantified that metal oxygen stoichiometry changed from Fe2.75Dy-O1.5 to Fe2.75Dy-O1.7 upon annealing. Synchrotron-based x-ray absorption spectroscopy investigation confirmed that the as-prepared films were highly disordered with predominantly metallic Fe and Dy states that became slightly oxidized with annealing in air. The as-prepared amorphous films demonstrated significantly high value of ordinary (∼10 cm2/V s) and anomalous (∼102 cm2/V s) Hall mobility and high electrical conductivity of ∼103 S/cm at room temperature. The cryogenic magnetic property measurement shows two-step magnetization below 200 K, suggesting exchange-spring magnetic interaction. The nature of the field cooled and zero-field cooled curves suggested a spin-glass like transition between 78 K and 80 K, with a characteristic broad peak. The Tauc plot analysis from optical transmission spectra confirms the existence of an optical bandgap of ∼2.42 eV that increased slightly to ∼2.48 eV upon annealing. This rich set of transport, optical, and magnetic properties in these thin films is very exciting and points to potential applicability in low-cost multifunctional devices requiring a combination of transparent, semiconducting, and magnetic responses, such as in spintronics.

Prasad Koirala, Krishna (ORCID:000000029137917X)↗

Sliding Wear and Fretting Wear of DLC-Based, Functionally Graded Nanocomposite Coatings

Improving the tribological functionality of diamondlike carbon (DLC) films--developing, good wear resistance, low friction, and high load-carrying capacity-was the aim of this investigation. Nanocomposite coatings consisting of an amorphous DLC (a-DLC) top layer and a functionally graded titanium-titanium carbon-diamondlike carbon (Ti-Ti(sub x) C(sub y)-DLC) underlayer were produced on AISI 440C stainless steel substrates by the hybrid technique of magnetron sputtering and pulsed-laser deposition. The resultant DLC films were characterized by Raman spectroscopy, scanning electron microscopy, and surface profilometry. Two types of wear experiment were conducted in this investioation: sliding friction experiments and fretting wear experiments. Unidirectional ball-on-disk sliding friction experiments were conducted to examine the wear behavior of an a-DLC/Ti-Ti(sub x) C(sub y)-DLC-coated AISI 440C stainless steel disk in sliding contact with a 6-mm-diameter AISI 440C stainless steel ball in ultrahigh vacuum, dry nitrogen, and humid air. Although the wear rates for both the coating and ball were low in all three environments, the humid air and dry nitrogen caused mild wear with burnishing, in the a-DLC top layer, and the ultrahigh vacuum caused relatively severe wear with brittle fracture in both the a-DLC top layer and the Ti-Ti(sub x) C(sub y)-DLC underlayer. For reference, amorphous hydrogenated carbon (H-DLC) films produced on a-DLC/Ti-Ti(sub x) C(sub y)-DLC nanocomposite coatings by using an ion beam were also examined in the same manner. The H-DLC films markedly reduced friction even in ultrahigh vacuum without sacrificing wear resistance. The H-DLC films behaved much like the a-DLC/Ti-Ti(sub x) C(sub y)-DLC nanocomposite coating in dry nitrogen and humid air, presenting low friction and low wear. Fretting wear experiments were conducted in humid air (approximately 50% relative humidity) at a frequency of 80 Hz and an amplitude of 75 micron on an a-DLC/Ti-Ti(sub x) C(sub y)-DLC-coated AISI 440C disk and on a titanium-6 wt % aluminum-4 wt% vanadium (Ti-6Al-4V) flat, both in contact with a 9.4-mm-diameter, hemispherical Ti-6Al-4V pin. The resistance to fretting wear and damage of the a-DLC/Ti-6Al-4V materials pair was superior to that of the Ti-6Al-4V/Ti-6AI-4V materials pair.

Miyoshi, K.↗

New Approaches to Low-Cost Scalable Doping of Interdigitated back Contact Silicon Solar Cells (Final Report)

The goal of this project was to develop novel approaches to patterning of dopants in the rear fingers of interdigitated back contact (IBC) Si solar cells to reduce the cost of manufacturing this high-efficiency-potential cell architecture. The work throughout this project can be divided into four categories: (a) development of dopant patterning technique using laser scribed Si contacts masks that are mechanically aligned with ~10 μm resolution to the underlying Si substrate; (b) measuring dopant spreading profiles in the isolation region between n- and p-type dopant fingers during plasma-enhanced chemical vapor deposition (PECVD) of doped hydrogenated amorphous silicon (a-Si:H) via shadow masks, and dopant desorption and re-adsorption during high-temperature annealing; (c) understanding the role of dopant compensation on the shunt resistance in contaminated isolation regions through analysis of defect-enhanced compensation; and (d) simulation and fabrication of passivated two-sided grid and back-contact solar cells to demonstrate the use of direct dopant patterning in cell fabrication. For the passivated two-sided grid solar cells, masked deposition was used to demonstrate an improvement in the blue response of the cell by creating a shallow front emitter. During development of the masked PECVD patterning process, we measured 3-D dopant profiles using secondary ion mass spectrometry. After deposition, in the masked region, the phosphorus dopant tail was >100 µm at concentrations >10 19 cm -3 while the boron dopant tail was shorter. During high-temperature crystallization of doped a-Si:H films to polycrystalline Si (poly-Si), phosphorus atoms spread by desorbing from the poly-Si surface and re-adsorbing onto intrinsic poly-Si on adjacent wafers that were separated by several millimeters. These contamination mechanisms resulted in a decrease in resistivity from ~10 5 Ω·cm for intrinsic poly-Si to ~10 -1 Ω·cm for contaminated poly-Si. Mitigation strategies for each contamination mechanism were developed to maintain a resistivity of ~10 5 Ω·cm between doped fingers. During fabrication of the 209 cells created during this project, it was found that despite contamination of the IBC gap through the abovementioned mechanisms, high shunt resistances and FF ~75% were still reached. Investigation into this led to the discovery of defect-enhanced compensation which exists within highly defective poly-Si when net doping concentrations reach the value of defect density (~10 18 cm -3 for many poly-Si films). Simulations guided us in the fabrication of IBCs and the cells fabricated were able to meet the year-end goals for BP 2 and 3 of 15% and 17% IBC cell efficiency, as well as the BP 4 goal of a 1% absolute increase in efficiency for PERC-like devices. However, the most efficient cell created during this project of 18.6% fell short of the 21% final project target. While the champion device fell short in V oc and J sc , many devices fabricated were able to reach the necessary goals of ~40 mA/cm 2 , ~700 mV, and ~75% FF required for a 21% device. The results generated from this project were disseminated through 11 conference presentations and proceedings. Presentations included oral talks at 2019 IEEE PVSC, 2019 MRS Fall Meeting, 2020 PVSEC-30 and 2021 IEEE PVSC, as well as poster presentations at 2020 IEEE PVSC and 2021 SiPV. The project resulted in 2 peer reviewed publications – one published in IEEE Journal of Photovoltaics and one in ACS Applied Energy Materials. The information gained in this project will aid in development of improved processes for fabrication of high-efficiency solar cells and other areas of the semiconductor device industry as well. The IBC cells will also pave the way for higher efficiency tandem devices. Through further manufacturing of high-efficiency solar cells, more of the world’s energy demands can be met through renewable sources, helping to stave off the worst effects that may come about from global climate change.

14 SOLAR ENERGY↗

Exploratory study on microanalysis of thin films by backscattering techniques

Solid phase epitaxial growth of Si layers was studied by backscattering spectrometry for controllable electrical characteristics. Samples were fabricated by vacuum deposition on a thin layer of Sb before deposition of the amorphous Si layer. Analysis of the resulting SPEG layer showed that Sb was present in the SPEG layer of Si. The characteristic of the SPEG layer against the Si substrate was rectifying. A scanning microprobe picture of a cleaved sample established the presence of a depletion region more than 1 micron below the surface. Hall effect data indicated that the SPEG layer was n-type, with average free carrier concentration of about 10 to the 19th power cm/3 and average electron mobility of about 40 sq cm/Vs. SPEG with Pd silicide or Ni silicide transport layers showed fast initial transient growth regimes with slower growth in the steady state regimes.

Mayer, J. W.↗

Lightweight, Flexible Solar Cells on Stainless Steel Foil and Polymer for Space and Stratospheric Applications

The availability of low-cost, lightweight and reliable photovoltaic (PV) modules is an important component in reducing the cost of satellites and spacecraft. In addition, future high-power spacecraft will require lightweight PV arrays with reduced stowage volume. In terms of the requirements for low mass, reduced stowage volume, and the harsh space environment, thin film amorphous silicon (a-Si) alloy cells have several advantages over other material technologies (1). The deposition process is relatively simple, inexpensive, and applicable to large area, lightweight, flexible substrates. The temperature coefficient has been found to be between -0.2 and -0.3 %/degC for high-efficiency triple-junction a-Si alloy cells, which is superior for high temperature operation compared to crystalline Si and triple-junction GaAs/InGaP/Ge devices at 0.53 %/degC and 0.45 %/degC, respectively (2). As a result, the reduction in efficiency at high temperature typical in space conditions is less for a-Si alloy cells than for their crystalline counterparts. Additionally, the a-Si alloy cells are relatively insensitive to electron and proton bombardment. We have shown that defects that are created by electrons with energies between 0.2 to 2 MeV with fluence up to 1x10(exp 15) e/sq cm and by protons with energy in the range 0.3 MeV to 5 MeV with fluence up to 1x10(exp 13) p/sq cm can be annealed out at 70 C in less than 50 hours (1). Further, modules incorporating United Solar s a-Si alloy cells have been tested on the MIR space station for 19 months with only minimal degradation (3). For stratospheric applications, such as the high altitude airship, the required PV arrays are typically of considerably higher power than current space arrays. Airships typically have a large area available for the PV, but weight is of critical importance. As a result, low cost and high specific power (W/kg) are key factors for airship PV arrays. Again, thin-film a-Si alloy solar cell technology is well suited to such applications.

Beernink, Kevin↗

Pinhole-free growth of epitaxial CoSi.sub.2 film on Si(111)

Pinhole-free epitaxial CoSi.sub.2 films (14') are fabricated on (111)-oriented silicon substrates (10) with a modified solid phase epitaxy technique which utilizes (1) room temperature stoichiometric (1:2) codeposition of Co and Si followed by (2) room temperature deposition of an amorphous silicon capping layer (16), and (3) in situ annealing at a temperature ranging from about 500.degree. to 750.degree. C.

Lin, True-Lon↗

Far-Infrared Properties of Cyclic Olefin Copolymer

Cyclic olefin copolymer (COC) is an amorphous thermoplastic with desirable dielectric and mechanical characteristics for optical applications. In particular, its low refractive index, overall mechanical strength, and absence of strong absorption features make it a promising substrate material for far-infrared applications, which include frequency-selective surfaces, scattering filters, and windows. The dielectric properties of selected COC formulations are surveyed from ≈10−700 per.cm (1000−14µm), and representative usage as a thin film membrane structure in optical filters is presented.

Wollack, Edward J.↗

Thin-Film Solar Cells on Polymer Substrates for Space Power

Photovoltaic arrays have played a key role in power generation in space. The current technology will continue to evolve but is limited in the important mass specific power metric (MSP or power/weight ratio) because it is based on bulk crystal technology. Solar cells based on thin-film materials offer the promise of much higher MSP and much lower cost. However, for many space applications, a 20% or greater AM0 efficiency (eta) may be required. The leading thin-film materials, amorphous Si, CuInSe, and CdTe have seen significant advances in efficiency over the last decade but will not achieve the required efficiency in the near future. Several new technologies are herein described to maximize both device eta and MSP. We will discuss these technologies in the context of space exploration and commercialization. One novel approach involves the use of very lightweight polyimide substrates. We describe efforts to enable this advance including materials processing and device fabrication and characterization. Another approach involves stacking two cells on top of each other. These tandem devices more effectively utilize solar radiation by passing through non-absorbed longer wavelength light to a narrow-bandgap bottom cell material. Modeling of current devices in tandem format indicates that AM0 efficiencies near 20% can be achieved with potential for 25% in the near future. Several important technical issues need to be resolved to realize the benefits of lightweight technologies for solar arrays, such as: monolithic interconnects, lightweight array structures, and new ultra-light support and deployment mechanisms. Recent advances will be stressed.

Hepps, A. F.↗

Lattice-Matched Semiconductor Layers on Single Crystalline Sapphire Substrate

SiGe is an important semiconductor alloy for high-speed field effect transistors (FETs), high-temperature thermoelectric devices, photovoltaic solar cells, and photon detectors. The growth of SiGe layer is difficult because SiGe alloys have different lattice constants from those of the common Si wafers, which leads to a high density of defects, including dislocations, micro-twins, cracks, and delaminations. This innovation utilizes newly developed rhombohedral epitaxy of cubic semiconductors on trigonal substrates in order to solve the lattice mismatch problem of SiGe by using trigonal single crystals like sapphire (Al2O3) as substrate to give a unique growth-orientation to the SiGe layer, which is automatically controlled at the interface upon sapphire (0001). This technology is different from previous silicon on insulator (SOI) or SGOI (SiGe on insulator) technologies that use amorphous SiO2 as the growth plane. A cubic semiconductor crystal is a special case of a rhombohedron with the inter-planar angle, alpha = 90 deg. With a mathematical transformation, all rhombohedrons can be described by trigonal crystal lattice structures. Therefore, all cubic lattice constants and crystal planes (hkl) s can be transformed into those of trigonal crystal parameters. These unique alignments enable a new opportunity of perfect lattice matching conditions, which can eliminate misfit dislocations. Previously, these atomic alignments were thought to be impossible or very difficult. With the invention of a new x-ray diffraction measurement method here, growth of cubic semiconductors on trigonal crystals became possible. This epitaxy and lattice-matching condition can be applied not only to SiGe (111)/sapphire (0001) substrate relations, but also to other crystal structures and other materials, including similar crystal structures which have pointgroup rotational symmetries by 120 because the cubic (111) direction has 120 rotational symmetry. The use of slightly miscut (less than plus or minus 10 deg.) sapphire (0001) substrate can be used to improve epitaxial relationships better by providing attractive atomic steps in the epitaxial process.

Choi, Sang↗

Low Temperature Growth of Nanostructured Diamond Films on Metals

The field of nanocrystalline diamond and tetrahedral amorphous carbon films has been the focus of intense experimental activity in the last few years for applications in field emission display devices, optical windows, and tribological coatings, The choice of substrate used in most studies has typically been silicon. For metals, however, the thermal expansion mismatch between the diamond film and substrate gives rise to thermal stress that often results in delamination of the film. To avoid this problem in conventional CVD deposition low substrate temperatures (less than 700 C) have been used, often with the incorporation of oxygen or carbon monoxide to the feedgas mixture. Conventionally grown CVD diamond films are also rough and would require post-deposition polishing for most applications. Therefore, there is an obvious need to develop techniques for deposition of well-adhered, smooth nano-structured diamond films on metals for various tribological applications. In our work, nanostructured diamond films are grown on a titanium alloy substrate using a two-step deposition process. The first step is performed at elevated temperature (820 C) for 30 minutes using a H2/CH4/N2 gas mixture in order to grow a thin (approx. 600 nm) nanostructured diamond layer and improve film adhesion. The remainder of the deposition involves growth at low temperature (less than 600 C) in a H2/CH4/O2 gas mixture. Laser reflectance Interferometry (LRI) pattern during growth of a nanostructured diamond film on Ti-6Al-4V alloy. The first 30 minutes are at a high temperature of 820 C and the rest of the film is grown at a low temperature of 580 T. The fringe pattern is observed till the very end due to extremely low surface roughness of 40 nm. The continuation of the smooth nanostructured diamond film growth during low temperature deposition is confirmed by in-situ laser reflectance interferometry and by post-deposition micro-Raman spectroscopy and surface profilometry. Similar experiments performed without the starting nanostructured diamond layer resulted in poorly adhered films with a more crystalline appearance and a higher surface roughness. This low temperature deposition of nanostructured diamond films on metals offers advantages in cases where high residual thermal stress leads to delamination at high temperatures.

Baker, Paul A.↗

Enhanced superconducting qubit performance through ammonium fluoride etch

The performance of superconducting qubits is often limited by dissipation and two-level systems (TLS) losses. The dominant sources of these losses are believed to originate from amorphous materials and defects at interfaces and surfaces, likely as a result of fabrication processes or ambient exposure. Here, we explore a novel wet chemical surface treatment at the Josephson junction-substrate and the substrate-air interfaces by replacing a buffered oxide etch (BOE) cleaning process with one that uses hydrofluoric acid followed by aqueous ammonium fluoride. We show that the ammonium fluoride etch process results in a statistically significant improvement in median $\text{T}_1$ by $\sim22\%$ (p = 0.002), and a reduction in the number of strongly-coupled TLS in the tunable frequency range. Microwave resonator measurements on samples treated with the ammonium fluoride etch after niobium deposition and etching also show $\sim33\%$ lower TLS-induced loss tangent compared to the BOE treated samples. As the chemical treatment primarily modifies the Josephson junction-substrate interface and substrate-air interface, we perform targeted chemical and structural characterizations to examine materials differences at these interfaces and identify multiple microscopic changes that could contribute to decreased TLS losses.

36 MATERIALS SCIENCE↗

Structural characterizaiton and gas reactions of small metal particles by high-resolution, in-situ TEM and TED

The existing in-situ transmission electron microscopy (TEM) facility was improved by adding a separately pumped mini-specimen chamber. The chamber contains wire-evaporation sources for three metals and a specimen heater for moderate substrate temperatures. A sample introduction device was constructed, installed, and tested, facilitating rapid introduction of a specimen into the mini-chamber while maintaining the background pressure in that chamber in the 10(-9) millibar range. Small particles and clusters of Pd, grown by deposition from the vapor phase in an in-situ TEM facility on amorphous and crystalline support films of alumina and on ultra-thin carbon films, were analyzed by conventional high-resolution TEM and image analysis in terms of detectability, number density, and size distribution. The smallest particles that could be detected and counted contained no more than 6 atoms; size determinations could be made for particles 1 nm in diameter. The influence of various oxygen plasma treatments, annealing treatments, and of increasing the substrate temperature during deposition was investigated. The TEM technique was employed to demonstrate that under otherwise identica l conditions the lattice parameter of Pd particles in the 1 to 2 nm size range and supported in random orientation on ex-situ prepared mica films is expanded by some 3% when compared to 5 nm size particles. It is believed that this expansion is neither a small-particle diffraction effect nor due to pseudomorphism, but that it is due to a annealing-induced transformation of the small as-deposited particles with predominantly composite crystal structures into larger particles with true f.c.c. structure and thus inherently smaller lattice parameter.

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