A new levitation apparatus coupled to a synchrotron-derived x-ray source has been developed to study the structure of liquids at temperatures up to 3000 K. The levitation apparatus employs conical nozzle levitation using aerodynamic forces to stably position solid and liquid specimens at high temperatures. A 270 W CO2 laser was used to heat the specimens to desired temperatures. Two optical pyrometers were used to record the specimen temperature, heating curves, and cooling curves. Three video cameras and a video recorder were employed to obtain and record specimen views in all three dimensions. The levitation assembly was supported on a three-axis translation stage to facilitate precise positioning of the specimen in the synchrotron radiation beam. The levitation system was enclosed in a vacuum chamber with Be windows, connections for vacuum and gas flow, ports for pyrometry, video, and pressure measurements. The vacuum system included automatic pressure control and multi-channel gas flow control. A phosphor screen coupled to a high-resolution video microscope provided images of the x-ray beam and specimen shadow which were used to establish the specimen position. The levitation apparatus was integrated with x-ray diffractometers located at X-6B and X-25 beamlines at the National Synchrotron Light Source. X-ray structural measurements have been obtained on a number of materials including Al2O 3, Ni, Si, Ge, and other metallic and ceramic materials in the liquid state.
High energy x-ray diffraction measurements have been performed on
CaO–Al2O3 liquids
suspended in a flow of pure argon for six compositions containing 50–67 mol% CaO. The results indicate
that AlO4
tetrahedra dominate the liquid structure. The radial distribution functions show a
significant broadening of the Ca–O peak occurs in the liquid compared to the
corresponding glass and, on average, each Ca is surrounded by approximately five oxygen
atoms in the melt at a distance of 2.3 Å. It is also found that the structure for the eutectic
(64% CaO) liquid does not change measurably with temperature between 1600 and
1970 °C.
Currently, carbon fibers (CFs) from the solution spinning, air oxidation, and carbonization of polyacrylonitrile impose a lower price limit of ≈$10 per lb, limiting the growth in industrial and automotive markets. Polyethylene is a promising precursor to enable a high-volume industrial grade CF as it is low cost, melt spinnable and has high carbon content. However, sulfonated polyethylene (SPE)-derived CFs have thus far fallen short of the 200 GPa tensile modulus threshold for industrial applicability. Here, a graphitization process is presented catalyzed by the addition of boron that produces carbon fiber with >400 GPa tensile modulus at 2400 °C. Wide angle X-ray diffraction collected during carbonization reveals that the presence of boron reduces the onset of graphitization by nearly 400 °C, beginning around 1200 °C. The B-doped SPE-CFs herein attain 200 GPa tensile modulus and 2.4 GPa tensile strength at the practical carbonization temperature of 1800 °C.
This paper presents a structure-property model for carbon fiber derived from a polyethylene (PE) precursor that relates tensile modulus to the elastic properties and angular distribution of constituent graphitic layers, as measured using wide-angle x-ray diffraction of individual carbon fiber filaments. The observed relationship and interpretation of data using a uniform-stress model has revealed fundamental differences in the nature of the microstructure present in carbon fiber produced from polyethylene compared to carbon fiber produced from polyacrylonitrile (PAN) or pitch precursors. Specifically, it was found that the shear modulus, indicative of the shear between adjacent graphitic layers of the carbonized fiber is lower for polyethylene-derived carbon fiber than for PAN-or pitch-derived carbon fiber, suggesting that the covalent CC sp 3 crosslink density connecting adjacent graphitic layers in PE-derived carbon fiber is reduced. This structure that is less crosslinked is anticipated to be easier to orient during carbonization and high-temperature graphitization processes, yielding a highly oriented structure necessary for high tensile modulus.
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