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(12) Patent Application Publication (10) Pub. No.: US 2016/0237595 A1 Maxwell Et Al

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(12) Patent Application Publication (10) Pub. No.: US 2016/0237595 A1 Maxwell Et Al US 20160237595A1 (19) United States (12) Patent Application Publication (10) Pub. No.: US 2016/0237595 A1 MaxWell et al. (43) Pub. Date: Aug. 18, 2016 (54) HIGH-STRENGTH REFRACTORY FIBROUS (52) U.S. Cl. MATERLALS CPC ................ D0IF 9/12 (2013.01): D0IF 9/1272 (2013.01): D0IF 9/1277 (2013.01); D10B (71) Applicant: Dynetics, Inc., Huntsville, AL (US) 2101/14 (2013.01); D10B2505/00 (2013.01); D10B 2401/04 (2013.01) (72) Inventors: James I. Maxwell, Scottsboro, AL (57) ABSTRACT (US); Nicholas Webb, Madison, AL (US); Ryan Hooper, Madison, AL (US); The disclosed materials, methods, and apparatus, provide James Allen, Huntsville, AL (US) novel ultra-high temperature materials (UHTM) 1. fibrous s s forms/structures; such “fibrous materials' can take various forms, such as individual filaments, short-shaped fiber, tows, (21) Appl. No.: 14/931,564 ropes, Wools, textiles, lattices, nano/microstructures, mesos tructured materials, and sponge-like materials. At least four (22) Filed: Nov. 3, 2015 important classes of UHTM materials are disclosed in this invention: (1) carbon, doped-carbon and carbon alloy mate Related U.S. ApplicationO O Data rials,(3) RA (2) materials within within the silicon-carbon-nitride-X the boron-carbon-nitride-X S. system, and (63) Continuation-in-part of application No. 14/827,752, (4) highly-refractory materials within the tantalum-hafnium filed on Aug. 17, 2015. carbon-nitride-X and tantalum-hafnium-carbon-boron-ni tride-X system. All of these material classes offer com (60) Provisional application No. 62/074,703, filed on Nov. pounds/mixtures that melt or Sublime attemperatures above 4, 2014, provisional application No. 62/074,739, filed 1800° C.—and in some cases are among the highest melting on Nov. 4, 2014, provisional application No. 62/038, point materials known (exceeding 3000° C.). In many 705, filed on Aug. 18, 2014. embodiments, the synthesis/fabrication is from gaseous, Solid, semi-solid, liquid, critical, and Supercritical precursor Publication Classification mixtures using one or more low molar mass precursor(s), in combination with one or more high molar mass precursor(s). (51) Int. Cl. Methods for controlling the growth, composition, and struc DOIF 9/12 (2006.01) tures of UHTM materials through control of the thermal DOIF 9/127 (2006.01) diffusion region are disclosed. Patent Application Publication Aug. 18, 2016 Sheet 1 of 25 US 2016/0237595 A1 Patent Application Publication Aug. 18, 2016 Sheet 2 of 25 US 2016/0237595 A1 Patent Application Publication Aug. 18, 2016 Sheet 3 of 25 US 2016/0237595 A1 Patent Application Publication Aug. 18, 2016 Sheet 4 of 25 US 2016/0237595 A1 FIG. 4 Patent Application Publication Aug. 18, 2016 Sheet 5 of 25 US 2016/0237595 A1 Patent Application Publication Aug. 18, 2016 Sheet 6 of 25 US 2016/0237595 A1 Patent Application Publication Aug. 18, 2016 Sheet 7 of 25 US 2016/0237595 A1 FIG. 7(a) Patent Application Publication Aug. 18, 2016 Sheet 8 of 25 US 2016/0237595 A1 FIG. 7(b) Patent Application Publication Aug. 18, 2016 Sheet 9 of 25 US 2016/0237595 A1 Patent Application Publication Aug. 18, 2016 Sheet 10 of 25 US 2016/0237595 A1 FIG. 8(b) 125 Patent Application Publication Aug. 18, 2016 Sheet 11 of 25 US 2016/0237595 A1 FIG. 9(a) 130 Patent Application Publication Aug. 18, 2016 Sheet 12 of 25 US 2016/0237595 A1 FIG. 9(b) 110 Patent Application Publication Aug. 18, 2016 Sheet 13 of 25 US 2016/0237595 A1 FIG. I.) Patent Application Publication Aug. 18, 2016 Sheet 14 of 25 US 2016/0237595 A1 FIG. II Direction of Fibers Drawn Fiber Growth at Nominal H- 8 Growth Rate Spooling NRate Patent Application Publication Aug. 18, 2016 Sheet 15 of 25 US 2016/0237595 A1 FIG. I2 240 - Cooling Fluid FOW 240 Patent Application Publication Aug. 18, 2016 Sheet 16 of 25 US 2016/0237595 A1 FIG. I.3 Mixture Growth Rates Relative to Pure Methane CN O r 0.1 100 Ratio of CH4 to Carbon-based HMMP Partial Pressures Patent Application Publication Aug. 18, 2016 Sheet 17 of 25 US 2016/0237595 A1 FIG. I.4 FIG. I5 Patent Application Publication Aug. 18, 2016 Sheet 18 of 25 US 2016/0237595 A1 FIG. 16(a) FIG. 16(b) FIG. 16(c) FIG. I. 7 FIG, 18(a) FIG. 18(b) Patent Application Publication Aug. 18, 2016 Sheet 19 of 25 US 2016/0237595 A1 FIG. I9 FIG. 20 Patent Application Publication Aug. 18, 2016 Sheet 20 of 25 US 2016/0237595 A1 s& F}{#Export-Controiesinistration Patent Application Publication Aug. 18, 2016 Sheet 21 of 25 US 2016/0237595 A1 FF. Patent Application Publication Aug. 18, 2016 Sheet 22 of 25 US 2016/0237595 A1 FIG. 23 Patent Application Publication Aug. 18, 2016 Sheet 23 of 25 US 2016/0237595 A1 : ...S33: . ... 3. Patent Application Publication Aug. 18, 2016 Sheet 24 of 25 US 2016/0237595 A1 FIG. 25 3. i030/2015 cur spot FA 1818 AM 5.00 kW 27 pA 4.5 ED 127m iOOOx 9.8 m Patent Application Publication Aug. 18, 2016 Sheet 25 of 25 US 2016/0237595 A1 FIG. 26 2000 OOOO 8000 w 6000 4000 2000 O 0.00 0.05 0.10 0.5 0.20 0.25 0.30 0.35 Extension (mm) US 2016/0237595 A1 Aug. 18, 2016 HIGH-STRENGTH REFRACTORY FIBROUS tors and motors, and carbon batteries, among other products. MATERALS In the early 1960s, the Union Carbide Co. used rayon as a precursor to produce the first commercial carbon fiber. In the CROSS-REFERENCE TO RELATED latter portion of the 20th century, various approaches were APPLICATIONS developed to produce high-strength carbon fibers from rayon, 0001. This application is a continuation-in-part of, and polyacrylonitrile (PAN), and Pitch. In these cases, carbon claims priority to, and the benefit of, U.S. application Ser. No. bearing precursors are spun/drawn into long strands and Sub 14/827,752 titled “Method and Apparatus of Fabricating sequently stabilized/oxidized, carbonized, and (optionally) Fibers and Microstructures from Disparate Molar Mass Pre graphitized. While very high-strength-to-density fibers and cursors.” filed Aug. 17, 2015; U.S. Application Ser. No. fibrous materials can be created in this manner, the precursors 62/074,703 titled “Doped Carbon Fibers and Carbon-Alloy employed must be synthesized and/or purified prior to use— Fibers and Method of Fabricating Thereof from Disparate and are relatively expensive. This is one factor that contrib Molecular Mass Gaseous-, Liquid, and Supercritical Fluid utes to the cost of carbon fiber production today. Mixtures, filed Nov. 4, 2014; and U.S. Application Ser. No. 0005. The strength of PAN/Pitch carbon fibers derives 62/074,739 titled “Method and Apparatus for Recording largely from the pre-alignment of the precursor molecules Information on Modulated Fibers and Textiles and Device for along the axis of the fibers, with carbonization at very small Reading Same filed Nov. 4, 2014, the entire contents of fiber cross-sections, to create a consistent microstructure over which are herein incorporated by reference. the cross-section of the fiber. In general, this approach pro vides fibers with graphitic planes running parallel to the fiber STATEMENT REGARDING FEDERALLY axis, mixed with some amorphous and fine-grained carbon SPONSORED RESEARCH ORDEVELOPMENT phases. Note that these graphitic sheets provide great strength along the axis, but less So perpendicular to the fiber axis (as 0002 N/A the graphitic planes can shear relative to each other), which leads to anisotropic properties of the fibers. This approach is BACKGROUND OF THE INVENTION also generally limited to small-diameter fibers to obtain the Field of the Invention necessary uniformity and densification of the carbon mate rial. Thus, untwisted filament bundles, or tows, of thousands 0003. The present invention is in the technical field offiber of fibers are necessary to obtain large Volume coverage with and/or fibrous material production and specifically relates to requisite quality, which also adds to the complexity and cost the synthesis of ultra-high temperature materials (UHTMs) in of carbon fiber production and use. In many applications, it fibrous forms/structures. Such "fibrous materials' can take would be preferable to use fewer high quality fibers that are of various forms, such as individual filaments, short-shaped larger diameter, e.g. during the weaving of carbon fiber cloth, fiber, tows, ropes, wools, textiles, lattices, nano/microstruc where useful strands could have diameters of up to 1-2 mm. tures, mesostructured materials, and Sponge-like materials. In 0006 Current commercial production of carbon fiber does addition, four important classes of materials specifically not produce fully-dense, void-free, and porosity-free fibers. relate to this invention: (1) carbon, doped-carbon and carbon For example, the range of density for high-strength PAN alloy materials, (2) materials within the boron-carbon-ni fibers is generally 1.80-1.94 g/cm and that for pitch fibers is tride-X system, (3) materials within the silicon-carbon-ni generally 2.10-2.16 g/cm while for comparison, the theo tride-X system, and (4) highly-refractory materials within the retical density for crystalline graphite is 2.267 g/cm. The tantalum-hafnium-carbon-nitride-X system. All of these difference between theory and the PAN/Pitch fibers is due to material classes offer compounds/mixtures that melt or Sub the presence of other forms of carbon and the voids/porosities lime at temperatures above 1800° C. and in some cases are present within the fibers. These voids/porosities lower the among the highest melting point materials known (exceeding strength and toughness of the fibers.
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