US 3404061: "FLEXIBLE GRAPHITE MATERIAL OF EXPANDED PARTICLES COMPRESSED TOGETHER (OCR)"



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Patent Overview

Patent Title: FLEXIBLE GRAPHITE MATERIAL OF EXPANDED PARTICLES COMPRESSED TOGETHER (OCR)
Patent Number: 3404061 Filing Date: Apr 01, 0015
Application Number: Issue Date: Oct 01, 1968
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Referenced By:

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Patent Number Issue Date Title Author
4234638 Nov 18, 1980 Composite graphite sheets Yamazoe, Hiroshi; Sugiura, Isao
4244934 Jan 13, 1981 Process for producing flexible graphite product Kondo, Teruhisa; Ishiguro, Jiro; Watanabe, Nobuatsu
5765838 Jun 16, 1998 Sealing gasket made of expanded graphite, with opened thin-leaf surface structure Ueda, Takahisa; Fujiwara, Masaru; Yamamoto, Terumasa
7892514 Feb 22, 2011 Method of producing nano-scaled graphene and inorganic platelets and their nanocomposites Jang, Bor Z.; Zhamu, Aruna
5164130 Nov 17, 1992 Method of sintering ceramic materials Holcombe, Cressie E.; Dykes, Norman L.
4534922 Aug 13, 1985 Gaskets Atkinson, Alan W.; Dearden, Katryna J.; Lancaster, Janet M.
4547434 Oct 15, 1985 Heat-resistant shift member Sumiyoshi, Kikuo; Sato, Eiji; Kojima, Masamitsu; Izumi, Masayoshi; Miyasaka, Kingo
4620358 Nov 04, 1986 Method of securing equipment parts to a trackway supporting structure Miller, Luitpold; Raschbichler, Hans G.
4776602 Oct 11, 1988 Thermally conductive composite gasket Gallo, Paul E.
4614554 Sep 30, 1986 Method of making a gasket Bate, Cecil A.; Robinson, Kay
6582846 Jun 24, 2003 Method for preparing fuel cell component substrate of flexible graphite material having improved catalytic properties Reynolds, III, Robert Anderson; Mercuri, Robert Angelo; Greinke, Ronald Alfred
6620506 Sep 16, 2003 Fluid permeable flexible graphite article with enhanced electrical and thermal conductivity Mercuri, Robert Angelo; Weber, Thomas William; Warddrip, Michael Lee
6777086 Aug 17, 2004 Laminates prepared from impregnated flexible graphite sheets Norley, Julian; Brady, John Joseph; Getz, George; Klug, Jeremy
6841250 Jan 11, 2005 Thermal management system Tzeng, Jing-Wen
7182898 Feb 27, 2007 Process for complex shape formation using flexible graphite sheets Klug, Jeremy H.
4888242 Dec 19, 1989 Graphite sheet material Matsuo, Koichiro; Maekawa, Kazuhiro; Kondo, Teruhisa
6757154 Jun 29, 2004 Double-layer capacitor components and method for preparing them Reynolds, III, Robert Anderson; Norley, Julian
5895058 Apr 20, 1999 Laminated gasket Sanders, Gary G.
4752518 Jun 21, 1988 Flexible surface deformation-resistant graphite foil Lohrke, James L.; Sterry, Janet M.; Lyons, Michael D.
7206330 Apr 17, 2007 End-face seal for graphite electrodes Bowman, Brian; Weber, Thomas William; Wells, Terrence Patrick; Pavlisin, James J.; Varela, William
6960402 Nov 01, 2005 Perforated cylindrical fuel cells Yazici, Mehmet Suha; Mercuri, Robert Angelo; Reynolds, III, Robert Anderson
6746626 Jun 08, 2004 Graphite polymers and methods of use Hayward, Tommie P.; Roemmler, Mike G.
6143218 Nov 07, 2000 Method of forming a flexible graphite composite sheet Mercuri, Robert Angelo
6927250 Aug 09, 2005 Graphite composites and methods of making such composites Kaschak, David M.; Reynolds, III, Robert A.; Krassowski, Daniel W.
4296806 Oct 27, 1981 High temperature well packer Taylor, Donald F.; Bostock, James H.
6479182 Nov 12, 2002 Fuel cell electrode assembly with selective catalyst loading Mercuri, Robert Angelo
6460310 Oct 08, 2002 Composite I-beam having improved properties Ford, Brian McNeil; Krassowski, Daniel Witold
5683778 Nov 04, 1997 Braided graphite-foil and method of production Crosier, Robert A.
4872914 Oct 10, 1989 High purity, high temperature pipe thread sealant paste Howard, Ronald A.
5149518 Sep 22, 1992 Ultra-thin pure flexible graphite calendered sheet and method of manufacture Mercuri, Robert A.; Getz, George; Greinke, Ronald A.; Howard, Ronald A.
5376450 Dec 27, 1994 Low surface acid intercalated graphite and method Greinke, Ronald A.; Bretz, Richard I.
5494506 Feb 27, 1996 Gas filtering device for air bag gas generator Ford, Brian M.; Wetula, John J.
4162078 Jul 24, 1979 Injectable packing formulation containing flexible graphite Cox, Carl V.
7378178 May 27, 2008 Catalyst support material for fuel cell Mercuri, Robert Angelo
6330986 Dec 18, 2001 Aircraft de-icing system Rutherford, Robert B.; Dudman, Richard L.
7666270 Feb 23, 2010 Heat spreader for display panel Smalc, Martin David; Norley, Julian; Capp, Joseph Paul; Clovesko, Timothy
7863522 Jan 04, 2011 Semi-conducting polymer compositions for the preparation of wire and cable Han, Suh Joon; Wasserman, Scott H.; Paquette, Mike S.; Pawlowski, David; Cieslinski, Robert C.
7881042 Feb 01, 2011 Cell assembly for an energy storage device with activated carbon electrodes Buiel, Edward R.; Eshkenazi, Victor; Rabinovich, Leonid; Sun, Wei; Vichnyakov, Vladimir; Swiecki, Adam J.; Cole, Joseph E.
8023310 Sep 20, 2011 Nonvolatile memory cell including carbon storage element formed on a silicide layer Fu, Chu-Chen; Kumar, Tanmay; Ping, Er-Xuan; Xu, Huiwan
8048474 Nov 01, 2011 Method of making nonvolatile memory cell containing carbon resistivity switching as a storage element by low temperature processing Kumar, Tanmay; Ping, Er-Xuan; Ilkbahar, Alper
7889502 Feb 15, 2011 Heat spreading circuit assembly Reis, Bradley E.; Cartiglia, James R.
6387462 May 14, 2002 Thermal insulating device for high temperature reactors and furnaces which utilize highly active chemical gases Blain, David Paul; Mercuri, Robert Angelo
6287694 Sep 11, 2001 Method for expanding lamellar forms of graphite and resultant product Zaleski, Peter L.; Derwin, David J.; Girkant, Richard J.
6468686 Oct 22, 2002 Fluid permeable flexible graphite fuel cell electrode with enhanced electrical and thermal conductivity Mercuri, Robert Angelo; Weber, Thomas William; Warddrip, Michael Lee
5902762 May 11, 1999 Flexible graphite composite Mercuri, Robert Angelo; Capp, Joseph Paul; Gough, Jeffrey John
4175022 Nov 20, 1979 Electrolytic cell bottom barrier formed from expanded graphite Vadla, Jostein J.; Wilder, Harold J.
4668554 May 26, 1987 Composite refractory product Thornton, James M.
6503626 Jan 07, 2003 Graphite-based heat sink Norley, Julian; Tzeng, Jing-Wen; Klug, Jeremy
7150914 Dec 19, 2006 Heat spreader for emissive display device Clovesko, Timothy; Norley, Julian; Smalc, Martin David; Capp, Joseph Paul
6237874 May 29, 2001 Zoned aircraft de-icing system and method Rutherford, Robert B.; Dudman, Richard L.
5593166 Jan 14, 1997 Low friction packing Lovell, Michel K.; Jackson, Randall S.; Brestel, Ronald R.
6982874 Jan 03, 2006 Thermal solution for electronic devices Smalc, Martin David; Shives, Gary D.; Reynolds, III, Robert Anderson
6702970 Mar 09, 2004 Process to reduce sticking during surface treatment of graphite articles Klug, Jeremy H.
4516782 May 14, 1985 Method of producing high temperature composite seal Usher, Peter P.
6087034 Jul 11, 2000 Flexible graphite composite Mercuri, Robert Angelo
7420810 Sep 02, 2008 Base heat spreader with fins Reis, Bradley E.; Skandakumaran, Prathib; Smalc, Martin David; Shives, Gary D.; Kostyak, Gary Stephen; Norley, Julian
6037074 Mar 14, 2000 Flexible graphite composite for use in the form of a fuel cell flow field plate Mercuri, Robert Angelo; Gough, Jeffrey John
5785322 Jul 28, 1998 Gasket for flange connections Suggs, Steven M.; Meyer, Reid M.
5797982 Mar 19, 1996 Apparatus for manufacturing a seamless packing material Suggs, Steven M.; Meyer, Reid M.
6228914 May 08, 2001 Intumescent composition and method Ford, Brian M.; Hutchings, David A.; Foucht, Mel E.; Qureshi, Shahid P.; Garvey, Chad E.; Krassowski, Daniel W.
8308106 Nov 13, 2012 Hydrogen powered aircraft MacCready, Paul B.; Hibbs, Bart D.; Curtin, Robert F.
4146401 Mar 27, 1979 Graphite material having compressibility and recovering property and method for manufacturing the same Yamada, Kazuo; Nakano, Yasuo; Fujii, Yoshikatsu
RE031933 Oct 27, 1981 High temperature well packer Taylor, Donald F.; Bostock, James H.
4915925 Apr 10, 1990 Exfoliated graphite fibers and associated method Chung, Deborah D. L.
4934657 Jun 19, 1990 Graphite spiral packing for stuffing box and method for manufacturing the same Dodson, Garry W.
5065493 Nov 19, 1991 Method of making a spherical sealing body used for exhaust pipe joint Ozora, Kazuo
5370405 Dec 06, 1994 Packing Ueda, Takahisa
7550529 Jun 23, 2009 Expanded graphite and products produced therefrom Drzal, Lawrence T.; Fukushima, Hiroyuki
8114373 Feb 14, 2012 Method of producing nano-scaled graphene and inorganic platelets and their nanocomposites Jang, Bor Z.; Zhamu, Aruna
5097769 Mar 24, 1992 Structure for supporting trackway of a track following transportation system, in particular, a magnetic suspension railroad Raschbichler, Hans G.; Miller, Luitpold
5127949 Jul 07, 1992 Wet friction material Nakazawa, Shiro; Fujiwara, Mikio
4559249 Dec 17, 1985 Sliding member and a method for manufacturing the same Arigaya, Hideto; Katsui, Yoshihiro; Sumiyoshi, Kikuo; Sato, Eiji; Miyasaka, Kingo
7235301 Jun 26, 2007 Latent heat storage material, latent heat storage unit containing the material, processes for producing the material and the unit and processes for using the material Bacher, Jürgen; Öttinger, Oswin; Christ, Martin
6106961 Aug 22, 2000 Sliding sheet material for high-temperature use and packing Ozaki, Kouki; Inoue, Masatoshi; Kawai, Shigehiro; Yamada, Yutaka; Matsumura, Hideyumi; Shibayama, Takayuki
4551393 Nov 05, 1985 Heat-resistant shift member Sumiyoshi, Kikuo; Sato, Eiji; Hirai, Kazuo; Miyasaka, Kingo; Izumi, Masayoshi
4781389 Nov 01, 1988 Flat sealing gasket having graphite-filled armor Beyer, Horst; Maus, Karl-Heinz; Lachnit, Detlev; Lonne, Klaus; Majewski, Klaus-Peter; Zerfass, Hans-Rainer
6673289 Jan 06, 2004 Manufacture of materials from graphite particles Reynolds, III, Robert Anderson; Norley, Julian; Greinke, Ronald Alfred
6770161 Aug 03, 2004 Method of making thermal insulating device by winding Blain, David Paul; Mercuri, Robert Angelo
6886249 May 03, 2005 Method for making finned heat sink assemblies Smalc, Martin D.
6902841 Jun 07, 2005 Hydrophobic fuel cell electrode Mercuri, Robert Angelo; Weber, Thomas William
7186309 Mar 06, 2007 Method for preparing composite flexible graphite material Mercuri, Robert Angelo; Klug, Jeremy; Getz, Matthew George; Weber, Thomas William
7232601 Jun 19, 2007 Method for preparing composite flexible graphite material Mercuri, Robert Angelo; Klug, Jeremy; Getz, Matthew George; Weber, Thomas William
7241409 Jul 10, 2007 Gas permeable flexible graphite sheet material and process therefor Calarco, Paul; Mercuri, Robert Angelo; Getz, Matthew George; Jones, Lawrence K.; Weber, Thomas William; Yazici, Mehmet Suha; Klug, Jeremy H.
4667969 May 26, 1987 Packing materials for shaft seals Suggs, III, James W.
6886233 May 03, 2005 Method for decreasing the thickness of flexible expanded graphite sheet Rutherford, Robert B.; Dudman, Richard L.
6884745 Apr 26, 2005 Perforated cylindrical fuel cells Yazici, Mehmet Suha; Mercuri, Robert Angelo; Reynolds, III, Robert Anderson; Calarco, Paul
7108917 Sep 19, 2006 Variably impregnated flexible graphite material and method Klug, Jeremy
7324577 Jan 29, 2008 End-face seal for male-female electrode joints Bowman, Brian; Wells, Terrence Patrick; Weber, Thomas William; Pavlisin, James J.
6413601 Jul 02, 2002 Thermal insulating device Blain, David Paul; Mercuri, Robert Angelo
5830809 Nov 03, 1998 Laminated reinforced flexible graphic article Howard, Ronald Albert; Mercuri, Robert Angelo
6017633 Jan 25, 2000 Flexible graphite composite sheet and method Mercuri, Robert Angelo
6254993 Jul 03, 2001 Flexible graphite sheet with decreased anisotropy Mercuri, Robert Angelo
5228701 Jul 20, 1993 Flexible graphite articles with an amorphous carbon phase at the surface Greinke, Ronald A.; Howard, Ronald A.
5192605 Mar 09, 1993 Epoxy resin bonded flexible graphite laminate and method Mercuri, Robert A.; Ohneth, Edwin J.; Lewis, Richard T.
6669205 Dec 30, 2003 Retainer gasket with pressure relief vents Schenk, Douglas C.
7292441 Nov 06, 2007 Thermal solution for portable electronic devices Smalc, Martin David; Shives, Gary D.; Reynolds, III, Robert Anderson
7303005 Dec 04, 2007 Heat spreaders with vias Reis, Bradley E.; Smalc, Martin David; Laser, Brian J.; Kostyak, Gary Stephen; Skandakumaran, Prathib; Getz, Matthew G.; Frastaci, Michael
6695357 Feb 24, 2004 Threaded pipe connection having a retainer gasket with pressure relief vents Schenk, Douglas C.; Mannella, Eugene J.
7520953 Apr 21, 2009 Process for producing moldings of expanded graphite, process for conducting, exchanging or storing heat using moldings and process for producing a heat storage device Guckert, Werner; Kienberger, Wolfgang
7573717 Aug 11, 2009 Cycling LED heat spreader Reis, Bradley E.; Smalc, Martin David; Laser, Brian J.; Kostyak, Gary Stephen; Skandakumaran, Prathib; Getz, Matthew G.; Frastaci, Michael
6194685 Feb 27, 2001 De-ice and anti-ice system and method for aircraft surfaces Rutherford, Robert B.
5934617 Aug 10, 1999 De-ice and anti-ice system and method for aircraft surfaces Rutherford, Robert B.
7704405 Apr 27, 2010 Material mixtures for heat storage systems and production method Öttinger, Oswin; Bacher, Jürgen
7799309 Sep 21, 2010 Area weight uniformity flexible graphite sheet material Reynolds, III, Robert Anderson; Greinke, Ronald Alfred
6835453 Dec 28, 2004 Clean release, phase change thermal interface Greenwood, Alfred W.; Bunyan, Michael H.; Young, Kent M.; Wright, Deanna J.
4895713 Jan 23, 1990 Intercalation of graphite Greinke, Ronald A.; Mercuri, Robert A.; Beck, Edgar J.
7206189 Apr 17, 2007 Composite electrode and current collectors and processes for making the same Reynolds, III, Robert A.
4068853 Jan 17, 1978 Stuffing box seal Schnitzler, Danny Louis
4256317 Mar 17, 1981 High-temperature, high-pressure valve packing system Havens, Marvin R.; Fields, Donald R.; Miller, Douglas J.
4829509 May 09, 1989 Optical recording medium, its preparation and its use as a read only memory information carrier Schrott, Wolfgang; Neumann, Peter; Hauser, Peter; Wagenblast, Gerhard
4471837 Sep 18, 1984 Graphite heat-sink mountings Larson, Ralph I.
6984117 Jan 10, 2006 Apparatus and method for manufacturing gaskets Suggs, Steven M.; Meyer, Reid M.
6926285 Aug 09, 2005 Jacketed spiral wound gasket Suggs, Steven; Kolb, Kris; Fulmer, Ken
6521369 Feb 18, 2003 Flooding-reducing fuel cell electrode Mercuri, Robert Angelo; Krassowski, Daniel Witold
5509993 Apr 23, 1996 Process for the preparation of a metal and graphite laminate Hirschvogel, Alfred
7132629 Nov 07, 2006 Heat-conducting plate of expanded graphite, composite and method for production Guckert, Werner; Neuert, Richard; Kienberger, Wolfgang; Kipfelsberger, Christian
6079277 Jun 27, 2000 Methods and sensors for detecting strain and stress Chung, Deborah D. L.
6604457 Aug 12, 2003 Process and apparatus for embossing graphite articles Klug, Jeremy H.
6781817 Aug 24, 2004 Fringe-field capacitor electrode for electrochemical device Andelman, Marc D.
6060189 May 09, 2000 Electrically conductive seal for fuel cell elements Mercuri, Robert Angelo; Gough, Jeffrey John
4417733 Nov 29, 1983 Method of producing high temperature composite seal Usher, Peter P.
7276273 Oct 02, 2007 Heat spreader for display device Clovesko, Timothy; Norley, Julian; Smalc, Martin David; Capp, Joseph Paul
6861481 Mar 01, 2005 Ionomeric nanocomposites and articles therefrom Ding, Rui-dong; Newell, Clint
7138029 Nov 21, 2006 Heat spreader for plasma display panel Norley, Julian; Smalc, Martin David; Capp, Joseph Paul; Clovesko, Timothy
8235077 Aug 07, 2012 Device for refilling a fuel cartridge for a fuel cell Curello, Andrew J.; Fairbanks, Floyd; Curello, Michael; Gray, David
7220485 May 22, 2007 Bulk high thermal conductivity feedstock and method of making thereof Sayir, Haluk; Mariner, John Thomas
4102960 Jul 25, 1978 Process for making high strength flexible graphite foil Borkowski, John W.
4199628 Apr 22, 1980 Vermicular expanded graphite composite material Caines, Ronald S.
4265952 May 05, 1981 Vermicular expanded graphite composite material Caines, Ronald S.
4277532 Jul 07, 1981 Thermally expandable sealants Czepel, Hubert; Jilek, Franz; Zochbauer, Heinz
4279952 Jul 21, 1981 Multilayer insulating material and process for production thereof Kodama, Fumio; Ohyama, Noboru
4299332 Nov 10, 1981 Pressure vessel seal Pechacek, Raymond E.
4351412 Sep 28, 1982 Diaphragm for acoustic instruments and method of manufacturing the same Yamamuro, Isao; Tsukagoshi, Tsunehiro
RE033760 Oct 10, 1989 High purity, high temperature pipe thread sealant paste Howard, Ronald A.
5804316 Sep 08, 1998 Baked packing for sealing shafts and valve stems Suggs, Steven M.; Hawkins, John; Meyer, Reid M.
7998616 Aug 16, 2011 Negative electrode for hybrid energy storage device Buiel, Edward; Eshkenazi, Victor; Rabinovich, Leonid; Sun, Wei; Vichnyakov, Vladimir; Swiecki, Adam; Cole, Joseph
7147960 Dec 12, 2006 Conductive composite material and electrode for fuel cell using said material formed by thermo-compression Baurens, Pierre; Bourgeoisat, Eric; Jousse, Franck; Salas, Jean-Félix
4559248 Dec 17, 1985 Sliding member Sumiyoshi, Kikuo; Miyasaka, Kingo
4591520 May 27, 1986 Pressure relief disc Brodie, George W.
7401404 Jul 22, 2008 Retainer gasket construction Yetter, William P.; Schenk, Douglas C.; Rall, Darrell W.
6503584 Jan 07, 2003 Compact fluid storage system McAlister, Roy E.
4812212 Mar 14, 1989 Apparatus for cathodically protecting reinforcing members and method for installing same Dimond, James; Swackhammer, William
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6503652 Jan 07, 2003 Fuel cell assembly method with selective catalyst loading Reynolds, III, Robert Anderson; Mercuri, Robert Angelo
6548156 Apr 15, 2003 Fluid permeable flexible graphite article with enhanced electrical and thermal conductivity Mercuri, Robert Angelo; Weber, Thomas William; Warddrip, Michael Lee
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6746768 Jun 08, 2004 Thermal interface material Greinke, Ronald A.; Krassowski, Daniel W.
6385956 May 14, 2002 Packing yarn made of graphite foil and metal foil and method of manufacturing a packing yarn Öttinger, Oswin; Schellenberger, Bernd
5201532 Apr 13, 1993 Flexible non-planar graphite sealing ring Salesky, William J.; Lacquement, Harold A.
6841248 Jan 11, 2005 Graphite article comprising a compressed mass of impregnated graphite particles and a reactive lubricant Klug, Jeremy H.
7324576 Jan 29, 2008 Joint strengthening ring for graphite electrodes Bowman, Brian; Wells, Terrence Patrick
6645456 Nov 11, 2003 Method for producing expandable graphite intercalation compounds using phosphoric acids, and graphite foil Öttinger, Oswin; Malik, Hubert
6667100 Dec 23, 2003 Ultra-thin flexible expanded graphite heating element Rutherford, Robert B.; Dudman, Richard L.
7105108 Sep 12, 2006 Graphite intercalation and exfoliation process Kaschak, David M.; Reynolds, III, Robert A.; Krassowski, Daniel W.; Ford, Brian M.
6406612 Jun 18, 2002 Expandable graphite and method Greinke, Ronald Alfred
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4601476 Jul 22, 1986 Squeak free seal for exhaust couplings Usher, Peter P.; Gavaletz, Eugene J.
5885728 Mar 23, 1999 Flexible graphite composite Mercuri, Robert Angelo; Capp, Joseph Paul; Gough, Jeffrey John
5981072 Nov 09, 1999 Oxidation and corrosion resistant flexible graphite composite sheet and method Mercuri, Robert Angelo; Blain, David Paul; McGlamery, Joe Tom
6149972 Nov 21, 2000 Expandable graphite and method Greinke, Ronald Alfred
6245400 Jun 12, 2001 Flexible graphite with non-carrier pressure sensitive adhesive backing and release liner Tzeng, Jing-Wen; Getz, Jr., George; Weber, Thomas William
5167868 Dec 01, 1992 Conductive expandable carbonaceous paste material Willey, Harvey E.; Clark, William R.; King, Harold L.
4946892 Aug 07, 1990 Composites of in-situ exfoliated graphite Chung, Deborah D. L.
5085700 Feb 04, 1992 High purity, high temperature pipe thread sealant paste Howard, Ronald A.
4911972 Mar 27, 1990 Insulating composite gasket Mercuri, Robert A.
5451064 Sep 19, 1995 Exhaust seal ring Mercuri, Robert A.; Weber, Thomas W.
5628520 May 13, 1997 Sealing material made of expanded graphite having opened thin-leaf surface structure Ueda, Takahisa; Fujiwara, Masaru; Yamamoto, Terumasa
7470468 Dec 30, 2008 Flexible graphite article and method of manufacture Mercuri, Robert Angelo; Capp, Joseph Paul; Warddrip, Michael Lee; Weber, Thomas William
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6279856 Aug 28, 2001 Aircraft de-icing system Rutherford, Robert B.; Dudman, Richard L.
7754332 Jul 13, 2010 Thermal insulation structures comprising layers of expanded graphite particles compressed to different densities and thermal insulation elements made from these structures Potier, Alexandre; Berger, Dominique; Bommier, Christophe; Raymond, Olivier; De Wasch, Jerome
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5698088 Dec 16, 1997 Formic acid-graphite intercalation compound Kang, Feiyu; Leng, Yang; Zhang, Tong-Yi
5266764 Nov 30, 1993 Flexible heating head for induction heating Fox, Robert L.; Johnson, Samuel D.; Coultrip, Robert H.; Phillips, W. Morris
6432336 Aug 13, 2002 Flexible graphite article and method of manufacture Mercuri, Robert Angelo; Capp, Joseph Paul; Warddrip, Michael Lee; Weber, Thomas William
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6399204 Jun 04, 2002 Flexible multi-layer gasketing product Shekleton, Laura E.; Hill, Kenneth L.; Hurley, Timothy J.
4086380 Apr 25, 1978 Granular disc joints for lengthwise graphitization Juel, Leslie Harrisville; Joo', Louis Arpad; Tucker, Kenneth Wayne
6540852 Apr 01, 2003 Apparatus and method for manufacturing gaskets Suggs, Steven M.; Meyer, Reid M.
6241256 Jun 05, 2001 Gasket for heat exchanger and method and apparatus for manufacturing same Suggs, Steven M.; Meyer, Reid M.
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6555223 Apr 29, 2003 Graphite structure with increased flexibility Kubo, Akira
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7182887 Feb 27, 2007 Conductive composite material and fuel cell electrode using same Jousse, Franck; Salas, Jean-Felix; Marsacq, Didier; Mazabraud, Philippe
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4607851 Aug 26, 1986 Method of making composite wire mesh seal Usher, Peter P.
5499827 Mar 19, 1996 Seal for shafts and valve stems Suggs, Steven M.; Meyer, Reid M.
4333975 Jun 08, 1982 Flat gasket laminate of expanded graphite foil and metallic reinforcement layer Booth, Geoffrey
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4363847 Dec 14, 1982 Flexible sheet material Hargreaves, Brian; Cousens, Alan K.
4676515 Jun 30, 1987 Composite embossed sandwich gasket with graphite layer Cobb, David A.
6092811 Jul 25, 2000 Hybrid gasket Bojarczuk, Raphael M.; Paulson, Roger Dean
4811959 Mar 14, 1989 Seal assembly for well locking mandrel Bullard, Roy P.; Bayh, III, Russell I.
7744811 Jun 29, 2010 Furnace expansion joint with compressible graphite joint filler and manufacturing method Mittag, Jörg; Öttinger, Oswin
6395199 May 28, 2002 Process for providing increased conductivity to a material Krassowski, Daniel Witold; Tzeng, Jing-Wen; Ford, Brian McNeil
6413663 Jul 02, 2002 Fluid permeable flexible graphite fuel cell electrode Mercuri, Robert Angelo
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4794043 Dec 27, 1988 Carbon product comprising carbonaceous materials joined together, said carbon product for electrode substrate of fuel cells and process for production thereof Kaji, Hisatsugu; Saitoh, Kuniyuki
5990027 Nov 23, 1999 Flexible graphite composite Mercuri, Robert Angelo; Capp, Joseph Paul; Gough, Jeffrey John
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5582811 Dec 10, 1996 Stable blister free flexible graphite and method Greinke, Ronald A.; Bretz, Richard I.
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Description

(click to expand)

Ai-@ 9 It u4 9vo I .13 Oct. 1, 1968 J. H. SHANE ET AL 3,404,061 FLEXIBLE GRAPHITE MATERIAL OF EXPANDED PARTICLES COMPRESSED TOGETHER Filed April 15, 1963 3 Sheets-5heet 1 F- z Lu OZ 2 I<- F-- Enz (O co- 0tt COz C\i 2 LLj LiJ o uj LLI C) -J LO 111- 03 -J U') w < LDJ c -J x LL (D C\i L r ) 00 co r c ) z a (D w Cf) 0 WW U) Z - (O C< W L iL m < a- w M < 2 (D a- a U) -Oo cn cn' L.L LLJW W w LLJ cro 8 o 1< W3: z@-00 a< CL - < 0 ZCLL)V- ZXX < W C ) M @ - a- I X < l w w c o O A II 0 L U 0 Z 0 UJ W 0 @- L- W 0 Un ;q L@@ -J z J w x CL P: v Q- x CJ x QC) w LL 0 LL 0 Q: w 0 w cn < (n Z W ww -J c t 0 0 < CCL - OX< 7 U) (D a- i@ w t w (D 0 L) Liu=) @- Z Z 0 \@ a@z r 10 < < w z t@.J - 5 + clj -1 W O:D 1* u- ocr INVENTORG x E) 0 @0- :.@: (D 0 U) 0 (L w N 0 M < w cr LLi a- 0 T EcisseiL W 2m CIC 0 yvov z, 4 --e@acwltf4w Q<- (D uj 2@@, - f amAApo ge@@ ATTOR NEYS


Oct. 1, 1968 J. H. SHANE ET AL 3,404,061 FLEXIBLE GRAPHITE MATERIAL OF EXPANDTD PARTICLES COMPRESSED TOGETHER Filed April 15, 1963 3 5heetS-5heet 2 26 68 74 ,-84 60 70 64 62 Ei 80 2 @-28 32 30 38 F 1 G.3 F I G. 4 42 92 114 104 i9o 100 106 118 LIQUID--,, 1 1 2 'ITROGEN-/ F 1G. 5 102--/ 110 1 1 8 1 6 124 F 1 G. 6 122 120 FIG. 7 INVENTOR9 / / 5 ; @ , q t v r ATTORNEYS


Oct. 1, 1968 J. H. SHANE ET AL 3,404,061 FLEXIBLE GRAPHITE MATERIAL OF EXPANDED PARTICLES COMPRESSED TOGETHER Filed April 1963 3 Sheets-Sheet 3 132 142 146 134 143 136 130 F I G. 8 140 FIG-9 148 144 152 182 154 17 184 150 1 8 0 160 172 158 FIG. iO FIG. I I FIG. 12 190 204 19 9 0 192 2 0 2 FIG. 13 200 212 210 214 LA F I G. 14 FIG. 15 I N V E N T O R .4 @ @ 7 , F I G. 1.6 AT TO RN E'Y S


lw u %to &,%mod States Patent Office 3,404,061 P a t e n t e d O c t . 1 , 1 9 6 8 3,404,061 FLEXIBLE GRAPHITE MATERIAL OF EXPANDED PARTICLES COMPRESSED TOGETHER James H. Shane, Acton, Robert J. Russell, Framingham, 5 and:Raymond A. Bochman, North Reading, Mass., as- signors, by mesne assignments, to Union Carbide Cor- poration, a corporation of New York Filed Apr. 15, 1963, Ser. No. 273,245 15 Claims. (Cf. 161-125) 10 This invention relates to graphite and more particularly to a novel form of graphite and to a process for pro- ducing the same. A principal object of the invention is to provide flexible sheet material which consists essentially of graphite and 1,5 which is essentially free of any binding or bonding material. Another object of the invention is to provide flexible graphite sheet material which possesses aniso- tropic or highly directional properties. Another object of the invention is to provide biiider- 20 less, flexible graphite sheet, paper, strip, tape, or the like which can have a density within the range of from about 5 pounds per cubic foot to about 137 pounds per cubic foot. Another object of the invention is to provide flexible 25 gta-phite sheet material from graphite particles which have been first appreciably expanded or intumesced and then compressed or compacted together, Still another object of the invention is to provide flexi- ble graphite sheet material from voluminously - expanded 30 graphite particles which have a c direction dimension which is at least 80 times and preferably at least 200 times that of the original particles from which they are formed. Still another object of the invention is to provide - flexi- 35 ble graphite sheet material from vermiform - graphite masses and an impregnant or additive. A still further object of the invention is to provide flexible graphite products of the above types which have been physically modified. 40 Still another object of the invention is to provide flexi- ble graphite sheet material having at least one - embossed surface. Still another object of the invention is to provide flexi- ble graphite sheet material having at least one surface 45 or side coated with an adhesive or cement or the like, or a metallic material such as aluminum, tantalum - carbide, or the like. Still another object of the invention is to provide lami- nate or composite structures comprising pliable - graphite 50 sheet material. A still further object of the invention is to provide solid and hollow articles or products formed by wrapping. rolling, or otherwise working flexible graphite - products of the above types. 55 . Still another object of the invention is to provide fab- rics or cloths formed from flexible graphite strips, yarns, strands, threads or the like. Still another object of the invention is to provide a process for producing flexible graphite sheet - material from voluminously expanded graphite particles. 60 Other objects of the invention will in part be obvious and will in part appear hereinafter. The invention accordingly comprises the produc-s possessing the features and properties and the process in- 65 volving the several steps and the relation and the order of one or more <)f such steps with respect to each of the others which are exemplified in the following - detailed disclosure, and the scope of the application of which will be indicated in the claims. For a fuller understanding of the nature and objects 70 of the invention, reference should be had to the following 2 detailed description taken in connection with the draw- ings wherein- FIG. I is a flow sheet illustrating a series of steps embodying the present invention. FIGS. 2 and 3 are diagrammatic views illustrating m 9 eans for formin flexible sheet material such as web, paper, strip, tape or the like from expanded or intumeseed graphite particles; FIG. 4 is a sectional view also illustrating means for forming flexible sheet material from expanded or intuniesced graphite particles; FIG. 5 is a perspective view of a flexible graphite sheet material e.g. paper, having an embossed surface; FIG. 6 is a diagrammatic, schematic view illustrating a cryogenic container utilizing flexible graphite sheet material, e.g. sheet having one surface emboss6d and orie surface coated with a reflective coating, e.g. aluminum as the. insulating material; FIG. 7 is an enlarged cross-sectional view of a composite or laminate structure employing flexible graphite sheet material, e.g. strip or web; FIGS. 8 and 9 are perspective views of other. laminate structures employing flexible graphite sheet material. FIG. 10 is a view illustrating one embodiment fbr fabricating hollow or cylindrical structures from flexible graphite strip or tape; FIGS@ 11 and 12 are cross-sectional views of hollow articles or products formed from flexible grap@ite strip or tape; FIG. 13 represents a flexible graphite strip from which threads strands, or yams can be prepared; FIG@. 14 and 15 illustrate a portion of a strand of flexible graphite material formed by suitably twisting the strip of FIG. 13; and FIG. 16 illustrates a portion of a fabric formed by weaving strips, threads, or strands of flexible . graphite material. Graphites are made up of layer planes of hexagonal arrdys or networks of carbon atoms. These layer . anes of PI hexagonally arranged carbon atoms are substanti-@lly flat and are oriented or ordered so as to be substantially parallel and equidistant to one another. The substantially flat, parallel equidistant sheets or layers of carbon atoms, usually referred to as basal planes, are linked or bonded together and groups thereof are arranged in crystallites. Highly ordered graphites consist of crystallites of considerable size; the crystallites being highly aligned or oriented,with respect to each other and having well ordered carbon layers. In other words, highly ordered graphites have a high degree of preferred crystallite orientation. it should be noted that graphites possess anisotropic structures and thus exhibit or possess many properties which are highly directional. Briefly, graphites may be characterized. as laminated structures of carbon, that is, structures consisting of superposed layers or laminae of carbarl atoms joined together by weak van der Waals forces. In c6nsidering the graphite structure, two axes or directions are usually noted, t6 wit, the c axis or direction and t@e a axes or directions. For simplicity, the c axis or direction may be considered as the direction perpendicular to the carbon layers. The a axes or directions -may be considered as the directions parallel to the carbon layers or the directions perpendicular to the c direction. Among the graphites which may exhibit or possess a high degree of orientation, mention may be made of natural graphites, Kish graphite and synthetic graphites such as for example, pyrolytic graphites. Natural graphites are generally found ot, obtained in the form of small, soft flakes or powder. Kish graphite is the excess carbon which crystallizes out in the course of smelting iron. The graphite separates as fine flakes and is very similar to flake natural graphite. Synthetic graphites are prodiiced by the pyrolysis


3 or thermal decomposition of a carbonaceous gas on a suitable substrate or mandrel heated at an elevated temperature. The graphite usually in the form of a massive, coherent deposit can be separated from the substrate in the form coherent masses or bodies. If desired, the graphite masses can be pulverized, comminuted, shaved, or the like to produce synthetic graphite particles, e.g. powder, chip, flake, or the like of any desired size. Synthetic graphites having a high degree of orientation and which are of particular interest are the so called pyrolytic graphites produced at temperatures between about 1500' C. and 3000' C. Pyrolytic graphites are essentially highly oriented polycrystalline graphites produced by high temperature pyrolysis techniques. Briefly, the pyrolytic deposition process may be carried out on a furnace wherein, at a suitable pressure, a hydrocarbon gas such as methane, natural ga@, benzene, acetylene or the like is therinally decomposed at the surface of a substrate of suitable shape, size, and material, e.g. graphite, heated for instance, by appropriate induction or resistance means, to a temperature between about 1500' C. and 3000' C. and preferably between about 1900' C. and 2500' C. The pyrolysis is continued until pyrolytic graphite of the desired tbickness is obtained. The substrate, if desired, may then be removed or separated from the pyrolytic graphite. Pyrolytic grapbite material formed in the above manner is spectroscopically pure carbon, approaches theoretical density, and possesses a bigh degree of anisotropy. Pyrolytic graphites prepared in the above manner only approach the true or ideal graphite structure. Although pyrolytic graphites bave a bigh degree of preferred crystallite orientation, they do exhibit or display substantial disorder or random orientation between the carbdn hexagon networks whic@ lie parallel to one another. For example, pyrolytic graphites may exhibit interlayer disorder such as layer stacking defects or they may exhibit some rotational disorder. Pyrolytic graphites can be made or treated to reduce or eliminate defects such as those referred to above so as to form more or less ideal graphites. For instance, pyrolytic graphites having a high degree of preferred orientation can be produced by utilizing very high deposition temperatures. Likewise, disordered pyrolytic graphites can be converted or transformed to more perfect graphite structures by heat treating or annealing for a sufficient time above the deposition temperature. Moreover, graphitization of pyrolytic graphites can be achieved by the application of tensile strain in the basal plane direction while heating the same. The graphitization of pyrolytic graphites produce crystallites having a three dimensional order which more closely resembles the structure or lattice of ideal graphite. As noted above, the bonding forces holding the parallel layers of carbon atoms together are only weak van der Waals forces. It has been found that graphites having a high degree of orientation such as, for example, natural graphites, Kish graphite and synthetic graphites, for instance, heat treated pyrolytic graphites can be treated so that the spacing between the superposed carbon layers or laminae can be appreciably opened up so as to provide a marked expansion in the direction perpendicular to the layers, that is, in the c direction and thus form an expanded or intumesced graphite structure in which the laminar character is substantially retained. In U.S. Patents 1,137,373 and 1,191,383, natural graphite in the form of flake or powder of a size too great to pass through a 200 mesh screen is expanded by first subjecting the graphite particles for a suitable period of time to an oxidizing environment or medium maintained at a suitable temperature. Upon completion of the oxidizing treatment, the soggy graphite particles or masses are washed with water and then heated to between about 350' C. and 600' C. to more fully expand the graphite particles in the c direction. The oxidizing mediums disclosed are mixtures of sulfuric and nitric acids and mixtures of nitric acid and potassium chlorate. By the above treatment, expansions of the natural 3@4047061 4 graphite particles of up to about 25 times the original bulk were obtained. There is also disclosed that the expanded natural graphite can be compounded with a binder, e.9. a phenolic resin and the resultant composition compres@ed or molded into various forms, such as discs, rings, rods, sheets, etc, It has been found that particulate graphite whether it be a natural flake or powder graphite, Kish flake graphite, or a synthetic graphite such as, for example, heat treated 10 pyrolytic graphite in the form of chip, powder, flake, or the like which has been greatly expanded and more particularly expanded so as to have a final thickness or C direction dimension which is at least 80 or rnore times the original c direction dimension can be formed wi I thout 15 the -use of a binder or agglutinant into cohesive or- integrated sheets, e.g. webs, papers, strips, tapes, or the li ke. The formation of graphite particles which have been expanded to have a final thickness or c dimension which is at least 80 times and prefelrably at least 200 times the 20 original c direction dimensioii into integrated sheets without the use of any binding material is believed to be possible due to the excellent mechanical interlocking, or cohesion which is achieved between the voluminously ex-. panded grapbite particles. Graphite particles which have 25 been expanded to a degree somewhat less than 80 times the original thickness or c direction dimension do n6t exhibit the excellent mechanical interlocking properties required to form well integrate-d graphite sheet material which is free of any binder or bonding agent. in such 30 cases, formation of graphite sheet material or the like can only be achieved through the use of binders. As noted in U.S. Patents 1,137,373 and 1,191,383, it was necessary that the natural graphite flakes and powders with eipansions up to about 25 times the original bulk be com- 35 pounded with a binder such as a phenolic resin in order to form sheets, rods, etc. The sheet material formed from graphite particles having the desired degree of expansion also possesse@ substantial flexibility or pliability and can be made to have a 40 density within the range of from about 5 pounds per cubic foot to a density approaching theoretical, that is, about 147 pounds per cubic foot. In addition to the unique advantage of flexibility, the sheet material has also been found to possess an appre- 45 ciable degree of anisotropy. Sheet material can. be pr6duced which has excellent flexibility, good strength and a high degree of orientati<)n. Such highly oriented m@terial possesses the excellent anisotropy or highly directional properties of pyrolytic graphite. 50 Briefly, the process of producing flexible, binderless graphite sheet material, e.g. web, paper, strip, tape, foil, mat or the like comprises compressing or compacting under a predetermined load and in the absence of a biiider, expanded graphite particles which have a c direction, 55 dimension which is at least 80 times and preferably 200 times that of the original particles so as to form a substantially flat, flexible,- integrated graphite sheet. It should be noted that the expanded graphite particles which generally are worm- like or vermiform in appearance once 6o compressed will maintain the compression set. The density and thickness of the sheet material can be varied by controlling the degree of compression. The density of the sheet material can be within the range of from about 5 pounds per cubic foot to about 137 pounds per cubic 65 fOOt. The flexible graphite sheet material exhibits an appreciable degree of anisotropy; the degree of anisotropy increasing with increasing density. In other words, the greater the density, the greater the degree of anisotropy possessed by the flexible graphite sheet material. 70 In such anisotropic sbeet material, the thickness, i.e. the direction perpendicular to the sheet surface comprises the c direction and the directions ranging all ng the length and width, i.e. alo 0 ng or parallel to the Sur- faces comprises the a directions. 75 'I'he flexible graphite sheet material produced in the


354041061. above manner can be modified in many ways. For example, in the formation thereof, impregnants or additives such as metal powde-rs, clay, organic polymeric materials and the like can be incorporated or mixed with the expanded graphite and the composition compressed to 5 form the desired sheet material. Likewise, one or both sides or surfaces of the soft, flexible graphite sbeet material can be embossed, quilted, or otherwise provided witb a pattern. One or both surfaces of the flexible graph- ite sheet material can be coated with a suitable material 10 to provide reflectivity, oxidation resistance, wear re- sistance, additional strength or the like. For instance, the flexible sheet material can be provided with a thin coating of metal such as aluminum, gold, silver, or cop- per to provide a high reflectivity, low thermal conductivi- 15 ty material for cryogenic applications. The flexible graphite sheet material can also be em- ployed to form various laminate or composite structures. For example, at leasf one surface of the sheet material can be provided with an adhesive or with a suitable back- 20 ing or carrier material to provide additional strength thereto. Additionally, the flexible graphite sheet material can be cut or slit int6 narrow strips which can be used to form woven or braided graphite fabric or cloth or the 25 narrow strips can be formed into threads or strands sheet having a density on the order of about 10 pounds per cubic foot. The long, self- supporting sheet was then passed through another pair of superposed rolls; the spacing provided therebetween being adjusted to -further compress the vermiform masses to the desired density and thickness. In this run, the sizing rollers were adjusted to provide a graphite sheet baving a thickness of about 5 mils and a density of about 70 pounds per cubic foot. The thin, long, integrated graphite sheet formed was very flexible, of good strength, and possessed a bigh de.-ree of anisotropy. The surfaces were smooth and bad a metallic lustre. Example II A series of runs were made similar to that of Example 1. However, in these runs, various sizes of suitable pyrolytic graphite particles were treated so as to produce vermiform pyrolytic graphite masses. Expanded graphite ma@ses, having c direction dimensions greater than about 80 times that of the original particle dimension were fou,nd to be capable of being pressed or rolled into integrated flexible sheet of various thicknesses and densities without the use of a binding or bonding agent. The conditions of various runs and the expansions obtained are set forth below: Particle Size Bath Composition Bath Temperature, Bath Tiine Expansion . C. (minutes) Finer than 40 mesh ----- 90% by volume H2SO4 (66' B6.) Room temperature 5 100- 300 X 10% by volume HN03 (36' B6.). 3040 mesh -------------- Same as above ------------------ -------- do --------------- 15 100-300 X 20-30 mesb ------------------- do -------------- --------------- ----- do --------------- 15 100-M x Coarser than 20 mesh -------- do ----------------------------- ----- do --------------- 60-180 100-200 X Do ------------------ 75% by voluine H2SO4 (66' Bd.) 105 -- ---------------- 10 80-100 x 25% by volume HN03 (36' B6.). which then can be us@d in the formation of graphite cloth Example III or fabric. Furthermore, the flexible graphite sheet ma- terial as well as the graphite cloth or fabric can be suit- abiy rolled or wound or otherwise worked to form solid or hollow structures. 40 More detailed descriptions of producing the flexible graphite products of the present invention are -ei,@en in the following non-limiting examples which are set forth only for the purpose of illustration. Example 1 45 A pyrolytic graphite mass produced at a deposition temperature of abo-ut 2100' C. was heat treated or an- nealed at a temperature of about 2800' C. for about 4 hours to provide a bi.-her degree of preferred orienta- 50 tion or, in other words, to provide a well-ordered grapbitic structure. The pyrolytic graphite mass was pulverized to form particles havin-g a size between about one eigbth .of an inch and about one half of an ineb. The graphite -particles were immersed in an oxidizing 55 bath comprising 90 peicent by volu@me of concentrated sulfuric acid (95-98% ) and 10 percent by volume of con- centrated nitric acid (36' B6.) heated to about 100' C. The particles were maintained in the hot bath until they became soggy which was on the order of about 30 min- 60 utes. Upon removal from the bath, the soggy graphite particles were thoroughly rinsed with water and then subjected to a temperature of about 1000' C. to effect an al-most instantaneous c direction expansion thereof. In this -run, the c direction dimension of the expanded 65 particles ranged from about 100 to about 300 times that of the original dimension. The expanded graphite masses which were still unitary structures were vermi- for,m in appearance. A predetermined height or thickness of the vermiform 70 graphite masses was continuously deposited onto a travel- ling surface of substantial width and passed through a pair of superposed rolls; the spacing provided therebe- tween being sufficient to compress or compact the vermi- TABLEI Natural graphite particles of a size sufficient to pass through a 200 mesh screen were immersed in an oxidizin,a bath comprising 90 percent by volume of concentrated sulfuric acid (95-98%) and 10 percent by volume of concentrated nitric acid (36' B6.) maintained at room temperature. The particles were maintained in the bath for about 5 minutes. Upon removal from the bath, the soggy natural graphite particles were thoroughly washed or rinsed with water and subjected to a temperature of about 1000' C. to effect a substantially, instantaneous c direction expansion thereof. In this run, the c direction dimension of the expanded natural grapbite particles ranged from about 100 to about 300 times that of the ori-inal dimension. The expanded natural graphite masses which were still unitary structures were ver- miform in appearance. A predetermined height or thickness of the vermiforin natural graphite masses was continuously deposited onto a tra-velling surface or belt of substantial width and passed through a pair of super_posed rolls predeterminedly spaced apart so as to compress the vermiform masses into a coherent self-supporting long flat sheet having a density on the order of gbout 10 pounds per cubic foot. The lorig, self-supporting sheet was then passed through a pair of superposed sizing rolls wherein the sheet was compressed and rolled to the desired thickness. In this run, th@- sizing rollers -were adjusted to provide a graphite sheet having a thickness of about 10 mils and a density about 60 pounds per cubic foot. The long, integrated of graphite sheet possessed excellent flexibility and strength and a bigh degree of anisotropy. The surfaces were very smooth and had a metallic lustre. E x a m p l e 1 7 V A series of runs were -made similar to that of Example 111. However, in these runs various grades or types of natural graphite flakes or powders (e.g. Ceylon form masses into a coherent, self-sustaining long flat 7r) graphite, Madagascar graphite, etc.), having sizes 'be-


37404)061 7 tween about 10 and about 40 mesh were treated so as to produce vermifom natural graphite masses. In these runs, expansions ranging from about 100 to about 500 and generally between about 200 to about 300 times that of the original c direction dimension were obtained. These expanded graphite masses were found to be capable of being compressed or compacted into integrated flexible sheets of various thicknesses and densities without the use of any binding material. Flexible sheets of excellent quality were obtained from graphite masses having c direction expansions greater than about 200 times. Example V A phenolic resin was blended @with vermiform natural graphite masses having c direction di-mensions which were about 200 to about 300 times that of the original dimension. The quantity of phenolic resin used was about 30 percent by weight of the graphite masses. The composition or mixture was then compr@ssed to produce a flexible "green" sheet having a thickness of about 10 mils and a density of about 100 pounds per cubic foot. A summary of some of the properties of the flexible graphite sheet material of the present invention is set forth in the following table: TABLEII Al BI cl D 2 Physical Data: Density, lbs./ft.-'---- 4G-60 60-80 100- 120 60-100 Purity, percent ----- 99.9+ 99. 9+ 99.9 - ------------ Ash content -------- 0.06 0.06 0.003 ------------ Gas penneability --------------- (1) (1) ------------ Thermal Data: Thermal conductivity ("c" direction) B.t.u.-ft./ hr.-ft.2-' F. at 1,000' F ----------- 0. 2-0.8 0.3- 0.6 0.15-0.5 0.8-1.5 Therinal shock resistance --------- Excellent Excellent Excellent -----------Subliination point, 'F --------- 6, 600 6, 600 6,600 -----------Mechanical data (room temperatui,e): Ultimate tensfle, p.s.i ----------- 450-600 800--1,200 1,700-3,200 500-700 Elastic modulus tension, p.s.i. xi(r -------------------------- 0.194 0.550 -----------Electrical data (room temperature: Resistivity (microhm- cm.) "a" direction ---------------- 1,000 ------------------------- I No impregnant or bonding material present. 2 Impregnated with about 30% by weight of a phenolic resiii. 3 Impermeable to helium at 10-5 mm. Hg. Although only a limited number of examples are given above illustrating the expansion of graphite particles and the compression thereof to form flexible sheet material or the like, it should be pointed out that runs were carried out using wider ranges of expanding and compressing conditions. In general, in the chemical treatment of natural gra,pbite and beat treated pyrolytic graphite particles, particles of a wide range of sizes were subjected for periods of time ranging from about one minute to about 120 hourr. or more to a variety of oxidizing oT intercalating solutions maintained at temperatures ranging from about room temperature to about 125' C. The graphite pa-rticles utilized can range in size from a dust or fine powder smar enough to pass through a 325 mesh screen to a size such that no dimension is greater than about one inch. The concentrations of the various compounds or materials employed, e.g. H2SO4, HN03, KMnO4, FeCI3, etc. ranged from about 0.1 normal to concentrated strengths. Ratios of H2SO4 to HN03 were also varied from about 9 to I to about I to 1. Interlayer attack of graphite particles is preferably achieved by subjecting the grapbite particles to oxidizing conditions. Various oxidizing agents dnd oxidizing mixtures may be employed to effect controlled interlayer attack. For example, there may be utilized nitric acid, potassium chlorate, chromic acid, potassium permanganate, potassium chromate, potassium dicbromate, perchloric acid and the like, or mixtures such as, for instance, con- 8 centrated nitric acid and potassium chlorate, chromic acid and phosphoric acid, sulfuric acid and nitric acid, etc., or mixtures of or strong organic acid, e.g. trifluoroacetic acid and a strong oxidizing agent soluble in the organic acid used. A wide range of oxidizing agent concentrations can be utilized. Oxidizing agent solutions having concentrations ranging from 0.1 normal to concentrated strengths may be effectively employed to bring about interlayer attack. The acids or the like utilized with the oxidizing 10 agents to form suitable oxidizing mediums or mixtures can also be employed in conceritrations ranging from about 0.1 normal to concentrated strengths. In one embodiment, the oxidizing medium comprises sulfuric acid and an oxidizing agent such as nitric acid, 15 perchloric acid, chromic acid, potassium permanganate, iodic or periodic acids or the like. One preferred oxidizing medium comprises sulfuric and nitric acids. The ratio of sulfuric acid to oxidizing agent, and more particularly, nitric acid can range from about 9 to I or higher to 20 about 1 to 1. Likewise, various sulfuric and nitric acid concentrations can be employed, e.g. 0.1 N, 1.0 N 10 N and the like. Generally, the concentrations of the sulfuric acid and nitric acid which can be effectively utilized range from about 0.1 normal to concentrated strengths. 25 The treatment of graphite particles with oxidizing agents or oxidizing mixtures such as mentioned above is prefer- ably carried out at a temperature between about room temperature and about 125' C. and for periods of time sufficient to produce a high degree of interlayer attack. 30 The treatment time will depend upon such factors as the temperature of the oxidizing medium, grade or type of graphite treated, graphite particle size, amount of ex- pansion desired and strength of the oxidizing medium. It should also be briefly mentioned that the'opening 3,5 uP or spreading apart of carbon layers can also be achieved by chemically treating graphite particles with an intercalating solution or medium so as to insert or intercalate a suitable additive between the carbon hexagon net- works and thus form an addition or intercalation com- 40 pound of grapbite. For example, the additive can be a halogen such as bromine or a metal halide such as ferric chloride, aluminum chloride, or the like. A halogen, particularly bromine, may be intercalated by contacting the graphite particles with bromine vapors or with a solution of bromine in sulfuric acid or with bromine dissolved 45 in a suitable organic solvent. Metal halides can be- intercalated by contacting the graphite particles with a suitable metal halide solution. For example, ferric chloride can be intercalated by contacting graphite particles with a suitable aqueous solution of ferric chloride or with a 50 mixture comprising ferric cbloride and sulfuric acid. Temperature, times, and concentrations of reactants similar to those mentioned heretofore can also be employed for the above intercalation processes. Upon completion of the treatment directed to promot- 55 ing interlayer attack, the thoroughly wetted or soggy graphite particles can be subjected to conditions for bring- ing about the expansion thereof. Preferably, however, the treated grarpbite particles are rinsed with an aqueous solution. The rinsing or washing of the treated graphite 60 particles with aqueous solutions may serve several functions. For instance, the rinsing or leaching removes barinful materials, e.g. acid, from the graphite particles so that it can be safely handled. Moreover, it may decompose or remove intercalated material. Furthermore, it can 65 also serve as the source of the blowing or expanding agent which is to be incorporated between layers. For example, it can serve as the source of water if such is to be utilized as the blowing or expanding agent. The c direction expansion is brought about by acti- 70 vating a material sucb as, for example, a suitable foaming or blowing agent which has been incorporated between layers of parallel carbon networks, the incorporation tak- ing place either during the interlayer attack treatment or thereafter. The incorporated foaming or blowing agent 75 upon activation such as by chemical interaction or by


394042061 9 heat generates a fluid pressure which is effective to cause c direction expansion or intumescence of the graphite particles. Preferably, a foaming or blowing agent is utilized which when activated forms an expanding -as or vapor which exerts sufficient pressure to cause expansion. A wide variety of well-known foaming and blowing agents can be employed. For example, there can be utilized expanding agents such as water, volatile liquids, e.g., liquid nitrogen and the like which change their physical state during the expansion operation. When an expanding agent of the above type is employed, the expansion of the treated graphite particles is preferably achieved by subjecting the treated graphite particles to a temperature sufficient to produce a gas pressure which is effective to bring about an almost instantaneous and maximum expansion of the particles. For instance, when the expanding agent is believed to be water, the graphite particles having water incorporated in the structure are preferably rapidly heated or subjected to a temperature above 100' C. so as to effect a substantially instantaneous and full expansion of the graphite particles. If such particles to be expanded are slowly heated to a temperature above 100' C., substantial water will be lost by vaporization from the str-ucture resulting in a drying of the structure so that little or no expansion wifl be achieved. Preferably, the substantially complete and full expansion of the graphite particles is accomplished within a time of from about a fraction of a second to about 10 seconds. In addition to physical expanding methods such as described above, the expanding gas can be generated in situ, that is, between layers of carbon networks by the interaction of suitable chemical compounds or by the use of a suitable heat sensitive additive or chemical blowing agent. I As indicated previously, the graphite particles are sO treated with a suitable oxidizing medium and unrestrietedly expanded that there is preferably produced expanded graphite masses having expansion ratios of at least 80 to I or higher. In other words, the expanded graphit@ particles have a thickness or c direction dimension which is at least 80 times that of the original c direction dimension. The expanded graphite particles are unitary, laminar structures having a vermiform appearance. The vermiform masses are pure, lightweight, anisotropic graphite. Additionally, the expanded or vermiform graphite masses are chemically inert to mo-st reagents, have excellent dimensional stability, and very low thermal expansion. One very important characteristic exhibited by such masses is that they are easily compressed under load and will maintain the compression set. In addition to graphite particles, other materials having a high degree of orientation and anisotropy can also be expanded. For example, particles of alloys of graphite, boron nitride and alloys thereof can also be expanded and flexible sheet material formed therefrom. Graphite allo@ particles and more particularly, pyrolytic graphite allo@ particles can be treated, expanded, and compressed in substantially the same manner as heretofore described for substantially pure graphite- particles. Boron nitride has a crystal structure simiiar to that of graphite. To attack the bonding forces between the layers so as to form openings, holes, or spaces for the introduction of a suitable expanding agent, e.g. water, the boron nitride can be initially treated with a solution of, for example, ferric chloride, aluminum chloride, antimony trichloride, arsenous chloride, or cuprous cbloride. Subsequent to such treatment, the boron nitride can be processed and expanded and then recompressed in manners similar to those described above for graphite. The formation of flexible graphite sheet, strip, paper, tape or the like from expanded graphite particles and modifications of such will be more fully set forth in connection with the descriptioii of the drawings. Referring now to FIGURE 1, there is illustrated a flow 10 sheet which sets forth one method of forming flcxible graphite sheet material from graphite p@xticles and modifications which may be made to such flexibl6 graphite sheet material. As shown, graphite particles in the form of fl6ke, powder, chip, granules or the like having a bigh degr@e of preferred orientation are subjected to interlayer attack to form openings between the layers of carbon networks. The interlayer attack is preferably achieved by subjecting the graphite particles to an oxidizing medium 1( such as a mixture comprising sulfuric acid and nitric acid. After the graphite particles have become thoroughly wetted and preferably quite soggy, they are removed from the oxidizing medium, and then rapidly heated or subjected to a temperature above 100' C. so as to substantial- 15 ly instantaneously effect a full c direction expansion of the graphite particles. If desired, the soggy particles, after removal from the oxidizing medium, can be thoroughly leached or rinsed with water and then expanded. Predetermined quantities of the expanded or worm4ike 20 graphite masses having the desired degree of expansion are then compressed or compact@d together, in the absence of any binder, so as to form a flexible, integrated graphite sheet,material having a desired thickness and density. If desired, the expanded graphite particles before being com- 25 pressed can be mixed or blended with a stiitable impregnant or additive so as to modify the nature or structure of the flexible graphite sheet material. The flexible graphite sheet material thus formed can be used as such as it can be further treated or worked, e.@. coated, embossed, lam- 30 inated, etc. so as to impart additional properties or 6haracteristics thereto. The modifications and uses of the flexible graphite sheet material will be discussed hereinafter in more detail. Referring now to FIGURE 2, there is shown one mea@ns 35 fo@r@continuously forming a flexible graphite sheet material fr6m expanded or vermiform graphite masses. The apparatus shown comprises a conveyor 10 consisting of an endless belt 12 of a suitable material, e.g. hard rubber, nie,tal, or the like and a pair of spaced rolls or rollers 40 14 and 16 in horizontal axial alignment around which belt 12 moves or travels. The conveyor is also provided w@ith side walls, only one side 18 being shown. Predeterminedly spaced above and in vertical axial alignment with roll 16 is roll 20. 45 The vermiform graphite masses 22 -having a c direction diiiiension or thickness which is at least 80 times and preferably at least 200 times that of the particles from which they were formed are fed or deposited at a predetermined rate onto the surface of the traveling belt 12 50 by means of an electrically controlled vibrating feeder 24 which is located below and in connection with storage hopper or bin 26. The expanded graphite particles 22 deposited onto the traveling belt surface which is moved @t a predetermined rate can all be of substantially the 55 -same size or of different sizes. Likewise, the graphite masses fed onto the belt can all have substantially the same degree of expansion, e.g. all with expansion ratios on the order of about 300 to I or have different expansions, e.g. the feed can comprise a mixture of graphite 60 masses having expansion ratios of 100 to 1, 300 to 1, and 500 to 1 or the like. It should also be noted that the @ feed 22 may also consist of a mixture or composition comprising, for example, expanded grapbite particles mixed or blended with an impregnant, e.g. a phenolic resin, or 135 other organic material; or an additive such as clay- particles, metal powder, or other suitable inorganic material. As conveyor means 10 travels at a desired rate in the direction shown, predetermined quantities of the expanded graphite particles or masses 22 are continuously depiosited 70 onto the traveling belt 12,,between the confining side walls and settle thereon to a thickness according to the speed of travel of belt 12. The slower the speed, the greater the thickness or deposit. The resultant continuous thick" bed of expanded particles 22 is passed or carried between 7r, pressure rolls 16 and 20. The spacing between roll 20


11 and the belt 12 at this point is controlled or adjusted such that the expanded particles are sufficiently compacted or compressed as to form a self-supporting sheet 28 having a thickness which is somewhat greater and a density which is somewhat less than that ultimately desired. Of course, the above spacing can be such that the expanded particles are compressed to the thickness and density desired for the sheet material. Preferably, however, two or more compression steps or stages are utilized to compact and bond the expanded particles together -and to form a sheet material having the desired thickness and density. The coherent, self-supporting sheet material 28, is then passed between at least one pair of predeterminedly spaced superposed pressure or sizing rolls. As shown, two pairs of sizing rolls are provided. Sizing rolls 30 and 32 and sizing rolls 34 and 36 are both provided with the same spacing therebetween so as to finally compress or reduce sheet material 28 to a sheet material 38 having the desired thickness and density. A plurality of pairs of sizing rolls is preferably employed so as to produce a smoother sheet of more uniform thickness and density. In order to further insure the production of a smooth sheet of uniform thickness and density, the sheet material, after being pressed or molded to the desired thickness and density, can be subjected to a suitable elevated temperature so as to remove residual fluid in the sheet and to cause re-expansion of compressed particles such as those not previously fully expanded, and the heat treated sheet then recompressed or sized. As shown in FIGURE 2, suitable heating means 40 illustrated in dotted lines is provided between the pairs of sizing rolls. Sheet 38 after passing through sizing rolls 30 and 32 is subjected to an elevated temperature, e.g. 1000' C. so as to cause re-expansion of compressed particies which were not previously completely expanded or which contain residual fluid, e.g. moisture. The heat treated sheet which may be somewhat puffed is then re-rolled to the desired thickness and density by sizing rolls 34 and 36. If desired, the sheet material can be subjected to more than one heat treatment and rerolling operation. The finished integrated sheet 38 after passing through sizing rolls 34 and 36 can then be taken upon a suitable reel or spool 42. The various rolls utilized are suitably driven by means which are not sho,@n. Means (not shown) for controlling the speed of conveyor 10 and the feed of expanded graphite particles to the traveling surface are also provided so that sheet material of a wide range of thicknesscs and densities and with a high degree of thickness and density uniformity can be produced. It should be noted that instead of utilizing roll 20 in- conjunction with conveyor 10, an endless belt means may be used instead. For instance, such a belt may be positioned above conveyor 10 and at an angle thereto such that the expanded graphite particles carried therebetween are progressively or gradually comj@ressed together. Likewise, the expanded graphite particles may be compressed by suitable step pressing means. Additional pairs of pressure or compressing rolls having varying spacings therebetween may precede sizing rolls 30 and 32 so that sheet 28 comprising partially compressed expanded particles may be gradually or stepwise reduced or compressed. Although the use of two pairs of sizing rolls is iilustrated, it should be pointed out that only one such pair may be employed or more than two pairs may be utilized. If desi'red, sheet modifying means may be included in i the sheet'production line. For eiample, one or both s-arfaces of sheet 38 can be embossed or otherwise markcd or deformed by utilizing one or two embossing rolls as the case may be as the final compressing or sizing rolls or by positioning one or more embossing rolls after the siziig rolls as shown by the dotted rolls 44 and 46 in FIGURE 2. For instance, if it is desired to emboss only the top or 3.,404.,061 12 with a smooth surface while roll 44 will be provided with the pattern or marking to emboss the top surface. Laminated structures or composites may be obtained by combining sheet 38 with a suitable sheet material 48. As shown in dotted lines in FIGURE 2, a suitable sheet material 48, for example, adhesively backed paper may be supplied from a supply reel or spool 50 and is bonded over the sheet 38 as the superposed sheets pass between guide and pressure rolls 52 and 54. Obviously, if it is 1( desired only to providd an adhesive coating to one or both surfaces of sheet 38, sbitable adhesive coating means, e.g. roll coaters or the like may be provided. It should also be mentioned that the sheet material 38, whether it be smooth surfaced, embossed, provided with 15 an adhesive coating or laminated or bonded to other suitable materials can be slit or cut by knife or slitting means 56 shown in dotted lines to forni strips, ribbons, tapes, strands, or the like of any desired width and length. Referring now to FIGURE 3 wherein like numbers 20 refer to like elements or parts of FIGURE 2, there is shown a pair of belt conveyors 60 and 62 having a Vshaped arrangement. Belt conveyor 60 comprises an endless belt 64 which travels around spaced rolls 66 and 68. Belt conveyor 62 comprises an endless belt 70 which 25 travels around spaced rolls 72 and 74. Sides (not shown) are provided between the conveyors so as to confine the expanded particles therebetween. In this case, the expanded graphite particles 22 from storage hopper 26 are fed between the moving belts 64 30 and 70 and are gradually or progressively pressed or compacted together as they are moved downwardly between the conveying belts. The spacing between the belts at the lower ends thereof is adjusted or controiled s'o that the expanded particles are compressed so as to form a co- 35 herent, self-supporting sheet 28 having the desired thickness and density or preferably having a thickness which is somewht greater and a density which is somewhat less than that ultimately desired. This sheet can then be ftirther worked or treated in any one or more of the ways de- 40 scribed in FIGURE 2. FIGURE 4 illustrates a simple means for forming sheet material. In this embodiment, a female die 80 is charged with a predetermined quantity of expanded p@rticles 82 e.g. graphite having the desired expansion and punch 84 45 is forced downwardly to compress the expanded particles in the die cavity to the desired thickness or degree. The expanded graphite particles heretofore described are lightweight, anisotropic, vermiform masses -which are easily compressed under load and which maintain the 50 compressioii set. As describedabove, graphite particles having a c direction dimension expansion of at least 80 times and preferably 200 times or more can be compressed in.io flexible thoroughly cohesive integrated sheet material without the 55 use of any binder or bonding agent. In the formation of binderless, flexible graphite sheet material, the compres- sing operation flattens the voluminously expanded graphite particles causing them into inter-engagement with each other. The strong mechanical bond formed b@'the inter- 60 locking or inter-engagement of an enormous number of carbon layers and the effective natural cohesive forces or adhesive properties of the graphite make it possibie to ob- tain a flexible, integrated graphite sheet materi'al of good strength. It has been found that sheet material having. 65 excellent strength and a very high degree of flexibility can be formed from graphite particles having a c direction dimension expansion of at least 200 ti mes. It can be gen- erally stated that the greater the deg@ree of expansion in the masses used to form the sheet material, the better the 70 quality of the sheet material. Moreover, the preferred expanded particles are flattened or squeezed in such a manner upon compression that the sheet material possesses an -appreciable degree of crystallite orientationand aniso- tropic properties. The flexible graphite sheet material of upper surface of sheet 38, then roll 46 will be provided 7,5 the invention has been found to possess or exhibit an


13 appreciable degree of anisotropy; the degree of anisotropy increasing with increasing density. In the anisotropic, flexible graphite sheet material, the c direction is the direction perpendicular to the surface plane, that is, the thickness direction and the a directions are the directions along the surface plane, that is, the width and length directions. The pliant, graphite sheet material possesses chemical inertness, thermal,stability, high purity, and non-wettability. It can also be made to possess fluid impermeability. It possesses either low or high thermal conductivity, ,dependent upon the orientation. Ilreliminary measurements of the graphite sheet material have indicated c direction thermal conductivities of less than about 1.0 B.t.u .-ft./hr.-ft.2-' F. at 1000' F. which is lower than th-at of pyrolytic graphite or any otber available high temperature insulation, Thus, the graphite material of the present invention possesses the unique advantage of fl6xibility, in addition to excellent 'thermal insulating properties from the cryogenic range up to 6700' F. A very effective insulating bar-rier is thus available in a very smafl s pace. The a direction thermal conductivity of the graphite sheet,material is in the range of 140-150 B.t.u.ft./hr.'-ft.2-' F. at 1000' F. which is approximately equal to pyrolytic graphite. In addition to anisotropic thermal- propetties, 'the sheet material also possesses anisotrOPic electrical properties. The sttength of the flexible graphite material depeiids upon several factors. However, generally it can be stated that flexible graphite material having room temperature tensile strengths ranging from about 250 to about 3200 p.s.i. and higher can be produced. Graphite sheet material of indefinite and commercial lengths and of a wide range of widths, thicknesses, and densities, can be continuously produced. The supple graphite sheet material can be provided with a uniform thickness in the range of from about 0.0001 inch (0.1 mil) to about 0.500 inch (500 mits). The densities of the gfaphite materials can range from about 5 pounds per cubic foot to about 137 pounds per cubic foot. Flexible graphite sheet materials having a density within the range of from about 40 to about 100 pounds per cubic foot have been found to possess very desirable flexibilities, stren.-ths, and anisotropies. The flexible graphite materials of the present invention find a wide range of uses. For example, the graphite material can be used as an insulating material and/or as a therinal conductive material. It can also be used to form graphite fabrics or cloth or to fabricate various shapes or structures such as for instance, bricks, blocks, plates, tubes, or the like. High temperature, chemically inert gaskets, rupture discs, or the like can be made by cutting out the desired shape from a suitable thickness of flat stock material. It can also be used as resistance heating elements and as radiation shields. The flexible graphite sheet material can be modified to provide many- adidtional useful applications. While the flexible sheet material can be pure graphite free of any binders or additives, suitable organic and inorganic materials can be incorporated therein so as to modify the nature or properties thereof. For example, the expanded graphite particles can be impregnated with various amounts of a polymeric material and the composition compressed to form the desired flexible material. Thus, it can be impregnated with a thermoplastic resin such as cellulose or cellulose acetate or with a thermosetting resin such as an epoxy resin or a phenolic as phenol-formaldehyde. When a heat-curable impregnant or binder, e.g. a phenolic resin is utilized, the binder can be cured or hardened by suitably heating the compressed product. . When an organic impregnant or binder is present with the graphite in the compressed product, if desired, such productcan be subjected to a suitable elevated temperature so as to effect carbonization of the organic impregnant and thus form a- substantially all carbon product. It should be noted that with the use of an impregnant or additive, flexible graphite sheet materials hav- 3)404,061, 14 ing appreciably high densities can be obtained. Thus', it is possible to produce graphite sheets having densities above about 137 pounds per cubic foot. In addition to organic materials suitable inorganic mati terials can also be incorporated or mixed with the ex- panded graphite particles and the composition then compressed to the desired product. For example, the compressed product may have incorprated therein particulate or fibrous materials such as a metal powder or filaments, 10 fibrous reinforcing materials, e.g. fiber glass' clays, or the like. The inclusion of suchmaterials may be to reinforce or strengthen the compressed product or to otherwise modify the properties thereof, for example, make the sheet magnetic, increase the electrical conductivity, 35 or the like. The flexible graphite sheet material of the present invention can be treated so as to deform one or both surfaces thereof. For example, the soft material can be easily embossed or otherwise marked or deformed by well known 20 means. As shown in FIGURE 5, one surface of material. 90 is smooth while the other surface is provided with a pluraiity of protuberances 92. In addition, the flexible products of the invention can be suitably coated. For example, a suitable adhesive coat- 25 ing e.g. a pressure sensitive adhesive can be provided on at least one face or surface, of say, a flexible graphite sheet which then can be slit into narrow strips to pro- vide a flexible, adhesive thermal insulating tape, or a flexible adhesive tape for use in the fabrication of shapes 30 such as tubular articles or the like. Likewise, coatings of metallic materials, for example, metals, carbides, oxides, or the like can also be applied by well known techniques to provide reflectivity, additional strength, oxidation resistance, wear resistance, or 35 the like. For instance, flexible graphite strands can -be coated with tantalum carbide and used as filaments in incandescent lamps of the type disclosed, for instance, in U.S. Patents 3,022,438 and 3,022,439. Tbe flexibl& graphite sheets can be provided with a thin, highly re- 40 flective metal coating such as aluminum, gold, silver, or copper to provide a highly reflective, low thermal conductivity, material for cryogenic applications such as shown in FIGURE 6. In FIGURE 6, there is shown a portion of a vessel 100 43 for carrying a cryogenic fluid 102 such as, for example, liquid nitrogen. This vessel comprises an inner container 104, for carrying the cryogenic fluid in a space 106. Only one wall of inner container 104 is shown for simplicity of illustration. If the cryogenic fluid is liquid nitrogen, 50 then the fluid 102 will be at a temperature of 77' K. and at atmospheric pressure due to a suitable vent (not shown). An otiter container 110 encloses the inner container 104 and defines therewith a space 112 which may be evacuated through a suitable outlet (not shown) to a 55 pressure of less than about I micron Hg abs., when the temperature of the wall of the inner container 104 is les8@, than about 100' K. A plurality of layers of flexibl6 graphite sheet material 114 are provided in space 112 so that. the c direction thereof is normal to the wall's of 60 containers 104 and 110. The graphite layers can be suitably wound about the wall of the inner container. One surface of each of the flexible graphite sheets 114 is provided with a metal coating 116 such as aluminum. The other surface of each of the flexible graphite sheets 114 65 is embossed to provide a plurality of protuberances 118 thereon so that only point contact wiH be provided from one layer to the other. In other words, the protuberances .118 prevent the grapbite layers from having extensive areas of planar contact and eliminate the :necessity of 70 spacer elements. In view of the very low thermal conductivity in the c direction of each of the graphite layers, and the use of a highly reflective metal coating, the layers 114 serve as very effective radiant heat barriers. The flexible grapbite sheet material can also be em- 75 ployed to form various laminate or composite structures.


is For instance, utilizing FIGURE 7 to illustrate various embodiments, there can be provided a laminated structure comprising two flexible graphite sheets 120 and 124 adhered together by a suitable binder or adhesive 122. The sheets can be bonded together by a binding or b(ynding agent such as tar, pitch, a carbon cement, or suitable thermosetting synthetic resin adhesive, e.g., a phenolic resin or the like so that, if desired, the agent can be carbonized so as to form a substantially all carbon product. Instead of sheet 124 being similar to sheet 120, it can be of a dissimilar material. For instance, it can be of a flexible, fibrous or dissimilar non-fibrous material such as paper, cloth, or fabric, synthetic polymeric material or the like. For example, graphite sheet 120 can be bonded by means of a thin adhesive layer 122 to a suitable backing material such as cloth, e.g., fiber glass or the like to provide- additional strength to the graphite sheet. Likewise, graphite sheet 120 may be combined with a carrier sheet or tape, e.g., paper having an adhesive which is more adhesive, than cohesive so that upon removal or stripping of, th,e paper therefrom, the adhesive material transfers from the paper and adheres to the graphite sheet 120 thus producing an- adhesively backed flexible gra- phite sheet. The strength of a flexible graphite sheet or strip can be increased by providing a laminate comprising two superposed flexible graphite layers bonded together and having therebetween suitable strengthening means such as strings, threads, sheet4ike material or the like. FIGURE 8 represents a composite or laminated structure comprising two flexible graphite sheets 130 and 132. These sheets are bonded together by a suitable adhesive 136 in which is embedded a series or plurality of longitudi-, nally disposed filaments 134 extending side by side in approximate parallelism. The filaments or strands may be of metal, glass, flexible graphite, or the like. FIGURE 9 represents another two-ply composite structure- comprising two sheets 140 and 142 of flexible graphite material. These sheets are laminated together by a suitable adhesive 143 in which there is embedded a -material 144 which comprises transverse threads 146 and longitudinal threads 148. The material 144 may comprise woven metal threads or filaments, woven glass fabric, woven flexible graphite strands or thread or the like. The flexible graphite sheet material and flexible graphite cloth or fabric can be rolled, wrapped, pressed or otherwise worked or formed to any shape desired. Thus, it is possible to provide structural shapes of any desired thickness, rigidity, and density. Suitable organic and inorganic binders can be utilized in the building of such shapes or structures. For example, a thick graphite sheet or plate of say, a thickness of one inch and of a low density can be formed or built-up by suitably laminating together a desired number of superimposed layers of low density flexible graphite sheet material. Solid articles or objects can be made from such a laminated structure by utilizing well-known machining techniques or the like. Laminated hollow or tubular structures can be provided by winding flexible graphite sheet material in the form of strip, tape, or the like around a suitable mandrel or substrate or by otherwise conforming the material to a desired form. As shown in FIGURE 10, two overlying tapes or strips 150 and 152 of flexible graphite material are spirally wound about mandrel 154. Obviously, if a thicker wall is desired for the tubular structure, more than two overlying graphite plies or strips are wound about mandrel 154. The strips may be wound without the use of any adhesive to secure them together and after winding coated with a suitable material so as to adhesively unite the strips and to provide a coherent, self-supporting rigid structure. Likewise, the strips may be adhesively backed so that the strips are bonded together as they are wound.about the mandrel. The wound tube 156 issuing from the mandrel 154 may then be cut into the desired lengths 158 by knife means 160. Tubes comprisin,,, a 39404@061 16 spirally wound tubular body member formed from a plurality of overlying plies or strips of flexible graphite material find many uses. For example, such tubes can be used as piping for confining or conveying molten metals or other materials or for confining hot gases or the like. FIGURE 11 shows a cross-section of a tube 170 produced in the manner of FIGURE 10 so as to be provided with a slight flare 172 at one end thereof. Such a tube of a low density and hence of light weight finds particular 1( 'use -as a blast tube in space vehicles. The overlying strips or tapes are spirally wound so that the junctions or seams in the lower layers are covered. FIGURE 12 ill@ustrates another manner in which tubu- lar members may be constructed. In this embodiment there 15 is shown a tubular elbow 180 having an inner layer 182 comprising flexible graphite strip or tape material which runs longitudinally of the elbow. An outer layer 184 is spirally wound or wrapped around layer 182. Thin, flat, flexible graphite sheet material can be cut 20 or slit into very narrow strands or strips which can be woven, braided, or otherwise formed into a graphite fabric or cloth. Likewise, a strip of suitable width can be cut from thin, flexible graphite sheet material and twisted or otherwise spun about its longitudinal axis or about an 25 axis lying at an angle to the longitudinal axis of the strips to form a compact flexible thread, yarn or strand of substantially cylindrical cross section. Threads or yarns thus formed can be woven, braided or otherwise worked into a fabric or the like or two or more of such threads can 30 be plaited or twisted with each other or with other materials to iorm a strand or filament of larger cross section. FIGURE 13 designates a strip of flat, thin, flexible graphite material 190 which can be twisted about itself or a suitable core to form a strand or thread. The longi- 35 tudinal axis of the strip is designated by the dotted line 192. In FIGURE 14, there is shown a strand 200 formed by suitably folding strip 190 along the line 192, doubling each of the folded portions back upon itself and then twisting the resulting strip on a line lying at an angle to 40 the longitudinal axis. A somewhat similar strand can be formed by twisting the resulting strip around its longitudinal axis. In FIGURE 15, a strand 202 is prepared by twisting strip 190 around a core of extraneous material 204. The core 204 may be stiff material or it may be 45 flexible. For example, core 204 may be a metallic wire or strand, glass fiber, a textile -material such as a twine of cotton, jute, or the like, The core material 204 is laid along the line 192 of strip 190 and the strip is twisted about the material, or it may be placed in other positions 50 upon the strip and the strip wrapped therearound as a tape. There are many other ways of utilizing strip 190 to form strands or threads. For instance, a strand may be formed by merely twisting grat)hite strip 190 across its 55 breadth so that the line of twist follows the longitudinal axis of the strip or strip 190 may be twisted along an axis lying at an angle to the line 192. Likewise, strip 190 can be rolled or convolved upon itself starting with either longitudinal edge and the strand then twisted. 60 The threads or strands of graphite material formed in any of the above described ways can be woven into light- weight, -pliable grapbite fabric or cloth. A portion of such a fabric 210 is illustrated in FIGURE 16. In this figure, the warp 212 and the weft 214 are both formed of strands 65 of flexible graphite material. However, it should be pointed oiit that a fa@bric can be formed byusing either a warp or weft of graphite -material in combination with a wara or weft of extraneous material such as a textile material, e.g., cotton, twine, etc. -metal wire, or the like. Additionafly, it 70 should be noted that a braided fabric or cloth can be formed from warp strands of graphite material and suit- able braiding strands. The warp and braiding strands can both be graphite material, or one can be of extraneous material as mentioned above. The woven cir braided 75 araphite fabric or cloth can be used to form structures of


3y4O4,061 17 various shapes, e.g. tubular structures or the like, or they can be used as lightweight, pliable microwave shielding materials. As used in the specification and claims, the terminology "graphite sheet" is intended to include within its meaning graphite in the form of flexible we@bs, strips, papersi'tapes, foils, films, mats or the like. The term "graphite sheet" thus includes within its meaning sttbstantially flat, flexible, graphite material or stock of any length and width, Since cer-tain changes may be made in the above, prod- ucts and processes without departing from the sco e of ,P the invention herein involved, it is intended that all i@atter contained in the above description should be interpreted as illustrative and not in a limiting sense. What is claimed is: 1. A grap4ite material comprising a mass of expanded graphite particles compressed together in the absence of a binder, said expanded graphite particles prior to compression having a c direction dimension which is at least 80 times that of the graphite particles from v@hich said expanded graphite particles are formed. 2. A graph ite material according to claim I wher&in at least one surface is embossed. 3. A graphite material according to claim I w-herein at least one surface is coated with an adhesive. , 4. A graphite material according to claim I wherein at least one surface is coated with a metallic material. S. A graphite sheet material comprising a m@ss of expanded graphite particles compressed togetber ih the absence of a binder, said expanded graphite particles, prior to compression having a c direction dimension which is at least 200 times that of the graphite particles from which said expanded graphite particles are formed. 6. A graphite sheet material produced by compressing in the absence of a binder a mixture comprising expanded graphite particles and an additive, said expanded graphite particles prior to compression having a c direction dimension which is at least 80 times that of the gra@hite particles from which said- expanded,graphi'e par-ticles are formed. 7. A laminate structure comprising a plurality of si@perposed layers of graphite sheet material bonded togdther, said graphite sheet material comprising expanded graphite particles compressed together in the absence of a b@nder, said expanded graphite particles prior to compression having a c direction dimension which is at least 80 times that of the graphite particles from which said expanded graphite particles are forined. S. A laminate according -to claim 7 wherein a plurality of strands are provided between said superpos--d layers. 9. A composite structure comprising a layer of grapbite sheet material and a layer of another material in superpose.d relation, said- superposed layers being bonded together, said graphite sbeet material comprising expanded graphi'e particles compressed together in the absence of . a binder, said expanded grapbite particles prior to compression having a c direction dimension which is at least 80 times that of the graphite particles from wbich said expanded graphite particles are formed. 10. A composite structure comprising a layer of graphite sheet material and a layer of paper in superposed relation, said superposed layers bein releasably ,9 bonded together, said graphite sheet material comprising expanded graphi@te particles compressed together in the 18 absence of a binder, said expanded graphite particles prior to compressi6n having a c direction dimerision which is at least 80 times that of graphite particles irom which said expanded graphite particles are formed. 5 11. The graphite material of claim I wherein said particles prior to compression are of a size such as -to be able to pass tbrough a 200 mesh screen. 12. The graphite material of claim I wherein said material has a density within the range 6f from about 5 10 pounds per cubic foot to about 137 pounds per cubic foo,. 13. The process of producing a graphite product from graphite particles, said particles having layers of carbon networks therein which comprises (a) contacting said 15 graphite particles with an oxidizing agent which is capa ble of exfoliating said layers for a time sufficient for said oxidizing agent to permeate said graphite particles, (b) rapidly heating said part'icles to a temperature of at least 100' C. whereby said oxidizing agent ig expanded so as 20 to exert pressure on said layers to expand said graphite, (c) continuing said heblting until an,expansion of at least 80 times the original C dimension of said graphite particles is achieved and (d) compreesing said expanded graphite in the absence of a binder to form said graphite 25 produc,. 14. The process of claim 13 wherein said particles prior to expansion are of a size such as to be able to pass through a 200 mesh screen. 15. The process of producing a gra@hite product from 30 graphite particles having layers of . carbon networks therein which comprises (a) contacting said graphite particles with an oxidizing agent which @is capable of exfoliati@ig said layers until said oxidizing agent permeates said graphite whereby said layers are exfoliated, (b) con- 35 tacting said graphite particles with water which decom- poses upon heating to form at least one decomposition product, said contact being maintained until the water permeates said graphite. to thereby lie.-between the layers of carbon networks, (c) heating said interposed water 40 to its decomposition tdmperature thireby liberating a gaseous product such that a pressure is exerted on said layers of carbon networks sufficient' to expand said graphite in the C direction, (d) maintaining said heating until said graphite is exp@nded at least 80 times its orig- 45 inal C dimension, and @';(e) compressing said expanded graphite in the absence 6f a binder to form said graphite product. References Cited,, UNITED STATES PATENTS 50 1,137,373 4/1915 Aylsworth ---------- 252-378 1,191,383 7/1916 Aylsworth --------- 252-378 3,138,434 6/1964 Diefendorf -------- 23-209.1 3,174,895 3/1965 Gibson et al. 55 1,285,465 11/1918 Tewksbury ---------- 161-85 3,072,558 1/1963 Myers et al. 3,107,152 10/1963 Ford et al. 3,160,550 12/1964 Novak ef al - -------- 156-151 OTHER REFERENCES 60 Fuel: A Journal of Fuel Science, vol. 24, No. 1, published 1945 "The Lamellar Compounds of Carbon" by H. L. Riley, pp. 52 and 54 (TP 315 F85). 65 MORRIS SUSSMAN, Pi-itnary Examiner.


Disclaimer 3,404,061.-James H. Shane, Actoi-i, Ptobert J. Ptussell, Framingham, aiid Raymond A. Boohman, North Reading, Mtss. FLEXIBLE GRAPH- ITE MATERIAL OF EXPANDED PARTICLES COMPRESSED TOGETHER. Patent dated Oct. 1, 1968. Disclaimer filed Oct. 1211972, by the,,issignee, Union Carb;de Co),Z)oratioiL. Hereby enters this disclaimer to claims 1-4 and 11-15 of said patent. [Offloial Octzette Jaqiqiary 30,1973.]

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