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A composite electrode prepared from silicon-graphene material and conductive polymer binder poly (1-pyrenemethyl methacrylate-co-methacrylic acid) for use in lithium-ion batteries.
Non-oxide ceramics such as silicon carbide (SiC), silicon nitride (Si3N4), and silicon borides (SiB4, SiB6) have thermal stability, oxidation resistance, hardness, and varied electrical properties. All these materials can be prepared in a fiber form from a suitable polymer precursor. The above mentioned fibers, when tested over a temperature range from 25 to 1400 C, experience degradation at elevated temperatures. Past work in ceramic materials has shown that the strength of ceramics containing both carbides and borides is sustained at elevated temperatures, with minimum oxidation. The work presented here describes the formation of ceramic fibers containing both elements, boron and silicon, prepared via the polymer precursor route previously reported by the authors, and discusses the fiber mechanical properties that are retained over the temperature range studied.
This report summarizes results from research on high performance polymers. The research areas proposed in this report include: 1) Effort to improve the synthesis and to understand and replicate the dielectric behavior of 6HC17-PEK; 2) Continue preparation and evaluation of flexible, low dielectric silicon- and fluorine- containing polymers with improved toughness; and 3) Synthesis and characterization of high performance polymers containing the spirodilactam moiety.
Silicon carbide made by pyrolizing polymers. Method conceived for preparation of poly(decamethylcyclohexasilanes) as precursors for preparation of silicon carbide at high yield. Technical potential of polysilanes as precursors of SiC ceramics being explored. Potential limited by intractability of some polysilanes; formation of small, cyclic polycarbosilane fragments during pyrolysis; and overall low char yield and large shrinkage in conversion to ceramics.
This report summarizes results obtained from research funded through Research Cooperative Agreement No. NCC-1-01033-"Low Dielectric Polymers" (from 5/10/01 through 5/09/02). Results are reported in three of the proposed research areas (Tasks 1-3 in the original proposal): (1) Repeat and confirm the preparation and properties of the new alkyl-substituted PEK, 6HC17-PEK, (2) Prepare and evaluate polymers derived from a highly fluorinated monomer, and (3) Prepare and evaluate new silicon and/or fluorine-containing polymers expected to retain useful properties at low temperature.
Production of strong lightweight membrane structure by applying a thin reflective coating such as aluminum to a rotating cylinder, applying a mesh material such as nylon over the aluminum coating, coating the mesh overlying the aluminum with a polymerizing material such as a para-xylylene monomer gas to polymerize as a film bound to the mesh and the aluminum, and applying an emissivity increasing material such as chromium and silicon monoxide to the polymer film to disperse such material colloidally into the growing polymer film, or applying such material to the final polymer film, and removing the resulting membrane structure from the cylinder. Alternatively, such membrane structure can be formed by etching a substrate in the form of an organic film such as a polyimide, or a metal foil, to remove material from the substrate and reduce its thickness, applying a thin reflective coating such as aluminum on one side of the substrate and applying an emissivity increasing coating such as chromium and silicon monoxide on the reverse side of the substrate.
To determine whether sputter etching may provide substantial polymer surface texturing with insignificant changes in chemical and mechanical properties, an 8 cm beam diameter, electron bombardment, argon ion source was used to sputter etch (ion-texture process) nine biomedical polymers. The materials included silicone rubber, 32% carbon impregnated polyolefin, polyoxymethylene, polytetrafluoroethylene, ultrahigh molecular weight (UHMW) polyethylene, UHMW polyethylene with carbon fibers (10%), and several polyurethanes (bioelectric, segmented, and cross linked). Ion textured microtensile specimens of each material except UHMW polyethylene and UHMW polyethylene with 10% carbon fibers were used to determine the effect of ion texturing on tensile properties. Scanning electron microscopy was used to determine surface morphology changes, and electron spectroscopy for chemical analysis was used to analyze the near surface chemical changes that result from ion texturing. Ion energies of 500 eV with beam current densities ranging from 0.08 to 0.19 mA/sq cm were used to ion texture the various materials. Standard microtensile specimens of seven polymers were exposed to a saline environment for 24 hours prior to and during the tensile testing. The surface chemical changes resulting from sputter etching are minimal in spite of the often significant changes in the surface morphology.
Prompted by its overwhelming benefits, silicon (Si) has evolved as one of the most promising anode materials for high-capacity lithium-ion batteries (LIBs). However, some of the intrinsic drawbacks such as low ionic conductivity and inevitable volume change during the alloying/dealloying process seriously hamper the commercialization of Si-based anodes in LIBs. Among the several strategies to overcome the challenges of the Si anode, the development of designed polymeric binders is imperative for enabling stable and satisfactory performance. The improved cell performance due to the designed binders is recognized as an economical and practical approach, especially from the industrial perspective. In addition to their conventional role in integrating electrode components, binders also play a significant role in alleviating the unfavorable phenomenon of volume expansion, and ultimately stabilizing the Si anode and Si-electrolyte interphase. The polymer architecture of the binders significantly influences the binder performance, and three-dimensional (3D) network binders are generally more effective at coping with the stress resulting from the huge volume change of the Si anode. To develop advanced 3D binders, substantial research efforts have been made including various crosslinking strategies in the past decade. In this review, we focus on diverse crosslinking methods including chemical-, physical-, and topological-crosslinking for rationally designing network binders for Si anodes and take a glance at dynamic interactions to construct healable binders for long-term stability.
Silicon is a promising anode material for lithium-ion batteries with its superior capacity. However, the drastic volume changes during lithiation/delithiation cycles hinder the cycling performance, resulting in particle pulverization, conductivity loss, and an unstable electrode-electrolyte interface. In this work, a series of synthetic polymeric binders, poly(acrylic acid-co-tetra(ethylene glycol) diacrylate)-featuring a poly(acrylic acid) (PAA) backbone branched via tetra(ethylene glycol) diacrylate (TEGDA)-are developed that edge toward evidencing well-balanced properties to confront capacity fading in Si-based electrodes. The incorporation of ether chain not only leads to the branching architecture of the PAA backbone, thus affecting its mechanical properties, but also promotes the conductivity of Li ions. As a result, a synergistic performance improvement is observed in both half and full cells. The best-performing cell using a branched PAA binder (bPAA) with a feeding molar ratio ([TEGDA]:[acrylic acid(AA)]) of 0.2 results in a 10% increase in initial capacity and a 31% increase in capacity retention over 100 cycles compared to the linear PAA cell. The cross-sectional microscopic images of the cycled electrodes reveal that bPAA binders can drastically reduce the electrode expansion. This improvement results from the well-balanced properties of the polymer design, which could guide further development for more advanced binder materials.
Here, we report the synthesis of five new examples of ladder cyclohexasilanes, possessing up to three consecutive fused rings and differing in relative ring fusion configuration and side chain structure. By coupling a 1,4-dipotassiooligosilyl dianion to a cyclohexasilane, we obtained bi- and tricyclic ladder cyclohexasilanes. Combined experimental and theoretical studies suggested that annulation could favor the cis configuration under kinetic control, while the trans configuration predominates under thermodynamic control. Computational studies show that with each additional ring in the trans-diastereomeric series, the predicted onset of light absorption shifts to longer wavelengths.
Block copolymer-directed self-assembly (DSA) remains promising for improving pattern quality and reducing the stochastic variations that challenge high numerical aperture extreme ultraviolet lithography. Equally critical is refining pattern transfer methods for accurately transferring the rectified DSA features to the underlying substrate. We compare two atomic layer deposition (ALD)-based techniques: sequential infiltration synthesis (SIS) and dry liftoff, applied to polystyrene-block-poly(methyl methacrylate) (PS-b-PMMA) DSA patterns. Both methods utilize aluminum oxide hard masks, with one synthesized through infiltration into the PMMA domains and the other through conformal ALD coating. High-resolution scanning electron micrographs were analyzed to measure line edge, width, and placement roughness for both the line (PMMA) and space (PS) features. Although both methods yielded similar overall 3σ rms roughness, they differed significantly in the frequency-dependent power spectral density (PSD) profiles. SIS reduced line placement roughness at length scales associated with the polymer pitch, but increased space width roughness at low frequencies, whereas dry liftoff mimicked the frequency content of the original guiding pattern. This study underscores the importance of PSD evaluation in selecting optimal pattern transfer strategies for specific applications.
The use of composites in aircraft structures is often limited by material and manufacturing costs which, for some designs and applications, are prohibitively high. To increase the frequency of application of composites in primary airframe components alternative manufacturing processes are sought that reduce cost and/or enhance structural efficiency. One alternative process involves the use of THERM-Xsm as the pressure transfer medium during autoclave curing. THERM-Xsm, a silicon-based flow able polymer which behaves like a liquid under autoclave presssure, transmits quasi-hydrostatic pressure to all contacting surfaces of the part to be cured. Once the autoclave pressure is relieved, THERM-Xsm reverts back to the powdery solid state and can be reused many times. The THERM-Xsm process to be evaluated is depicted and consists of (1) enclosing the tool and part to be cured by a set of frames that create a box, (2) pouring THERM-Xsm powder onto the part and filling the box, and (3) placing a vacuum bag over the box assembly. In this program, a separating non-porous film (Teflon) was placed between the part to be cured and THERM-Xsm powder to avoid any contamination. The use of THERM-Xsm has two significant advantages over conventional manufacturing procedures. First, it eliminates complicated hard tooling since it guarantees uniform pressure transfer and thus, good compaction at complex structural details (such as frame-stiffener intersections and corners). Second, it greatly simplifies vacuum bagging, since once the part to be cured is covered by THERM-Xsm powder, the vacuum bag need only conform to a relatively flat shape reducing significantly the number of pleats required. A program is on-going at Sikorsky Aircraft to evaluate the structural performance of complex composite fuselage structures made with this THERM-Xsm process and to quantify the impact of THERM-Xsm on manufacturing labor hours and cost. The program involves fuselage panel optimization analysis, a building block test program where structural details representative of the full-scale article are analyzed and tested, and static and fatigue test/analysis of the full-scale test articles. The main results of this program are reported.
Future concepts of ultra large space telescopes include segmented silicon mirrors and inflatable polymer mirrors. Primary mirrors for these systems cannot meet optical surface figure requirements and are likely to generate over several microns of wavefront errors. In order to correct for these large wavefront errors, high stroke optical quality deformable mirrors are required. JPL has recently developed a new technology for transferring an entire wafer-level mirror membrane from one substrate to another. A thin membrane, 100 mm in diameter, has been successfully transferred without using adhesives or polymers. The measured peak-to-valley surface error of a transferred and patterned membrane (1 mm x 1 mm x 0.016 mm) is only 9 nm. The mirror element actuation principle is based on a piezoelectric unimorph. A voltage applied to the piezoelectric layer induces stress in the longitudinal direction causing the film to deform and pull on the mirror connected to it. The advantage of this approach is that the small longitudinal strains obtainable from a piezoelectric material at modest voltages are thus translated into large vertical displacements. Modeling is performed for a unimorph membrane consisting of clamped rectangular membrane with a PZT layer with variable dimensions. The membrane transfer technology is combined with the piezoelectric bimorph actuator concept to constitute a compact deformable mirror device with a large stroke actuation of a continuous mirror membrane, resulting in a compact A0 systems for use in ultra large space telescopes.
The purpose of this article is to present additional information about the flow-velocity sensors described briefly in the immediately preceding article. As noted therein, these sensors can be characterized as artificial hair cells that implement an approximation of the sensory principle of flow-sensing cilia of fish: A cilium is bent by an amount proportional to the flow to which it is exposed. A nerve cell at the base of the cilium senses the flow by sensing the bending of the cilium. In an artificial hair cell, the artificial cilium is a microscopic cantilever beam, and the bending of an artificial cilium is measured by means of a strain gauge at its base (see Figure 1). Figure 2 presents cross sections of a representative sensor of this type at two different stages of its fabrication process. The process consists of relatively- low-temperature metallization, polymer-deposition, microfabrication, and surface-micromachining subprocesses, including plastic-deformation magnetic assembly (PDMA), which is described below. These subprocesses are suitable for a variety of substrate materials, including silicon, some glasses, and some polymers. Moreover, because it incorporates a polymeric supporting structure, this sensor is more robust, relative to its silicon-based counterparts.
A series of studies evaluating the effects of added elastomers on the properties of a high-temperature addition polyimide adhesive is reviewed. First, thermoset polyimides containing various butadiene/acrylonitrile and silicone elastomers were synthesized either as physical polybends or by chemically reacting the elastomers directly onto the polymer backbone. The modified adhesive resins were characterized for thermomechanical properties, fracture toughness and adhesive strength. A second series of elastomer-containing polyimides was also prepared in order to study the effects of the elastomer chain length on polymer properties. Aromatic amine-terminated silicone rubbers with repeat units varying from n = 10 to 105 were reacted onto the polyimide backbone, and the resulting polymers were characterized for their adhesive properties.
The potential for a three step SiF2 polymer transport purification process was examined. The process involves reacting low cost mg silicon with SiF4 to yield SiF2 gas which is condensed to form polymeric (SiF2)x. The polymer is then heated above 400 C to yield Si, SiF4 and higher Si sub n F sub 2n+2 homologues. This report presents and discusses continuing progress on (1) observations on (SiF2)x polymer formation and depolymerization on the small coil, (2) mass balance studies, (3) partial pressures of SiF2 and SiF4, (4) AlF3 mass spectral studies, and (5) material analysis studies.
This report summarizes results obtained through our current research effort entitled 'Low Dielectric Polymers'. Results are reported in four areas: (1) Development of an alkyne containing a crosslinking agent for 12F-PEK and its analogues; (2) Preparation and evaluation of new silicon- and/or fluorine-containing polymers for low temperature applications; (3) Polymers derived from a new highly fluorinated monomer; and (4) Continued evaluation of the scale-up of the preparation of 6FC11- and 6FC17-PEKs.