United States Patent (19) 11 Patent Number: 5,366,526 Ellison-Hayashi Et Al
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US005366526A United States Patent (19) 11 Patent Number: 5,366,526 Ellison-Hayashi et al. 45 Date of Patent: Nov. 22, 1994 54 METHOD OF ABRADING WITH BORON tals:', Stanford Research Institute, Menlo Park, Calif., SUBOXIDE (BXO) AND THE BORON Jan., 1963. SUBOXIDE (BXO) ARTICLES AND H. Tracy Hall and Lane A. Compton, "Group IV Ana COMPOST ONUSED logs and High Pressure, High Temperature Synthesis of 75 Inventors: Cristan Ellison-Hayashi, Salt Lake B2O’, Inorg. Chem. 4 (1965) 1213. City, Utah; George T. Emond, W. C. Simmons, "Progress and Planning Report on Southington, Conn.; Shih Y. Kuo, Boron Suboxide B60', Air Force Materials Labora Salt Lake City, Utah tory, Mar., 1968. H. Wrerheit, P. Runow, and H. G. Leis, "On 73) Assignee: Norton Company, Worcester, Mass. Boron-Suboxide Surface Layers and Surface States of 21 Appl. No.: 51,114 B-Rhombohedral Boron:”, Phys. Stat. Sol. (a) 2, K125 (1970). 22 Filed: Apr. 21, 1993 E. V. Zubova, K. P. Burdina, "Synthesis of B6O Under Pressure', Dokl. Akad. Nauk. SSR, 197 (5) (1971) Related U.S. Application Data 1055-1056. 63 Continuation-in-part of Ser. No. 920,357, Jul. 28, 1992, which is a continuation-in-part of Ser. No. 729,467, Jul. (List continued on next page.) 12, 1991, Pat. No. 5,135,892. 51) int. Cl. ................................................ C09K3/14 Primary Examiner-Wayne Langel 52 U.S. C. ......................................... 51/307; 51/309 Attorney, Agent, or Firm-Brian M. Kolkowski 58 Field of Search ............................ 423/278; 501/1; 51/281 R, 307, 309 57 ABSTRACT 56 References Cited A method of removing material from a surface compris U.S. PATENT DOCUMENTS ing abrading a surface comprising the step of abrading a 1,105,388 7/1914 Weintraub ........................... 423/278 surface with an abrasive tool or an abrasive powder 3,660,031 5/1972 Holcombe, Jr. et al. ... 423/278 comprising a boron suboxide (BxO) composition, 3,816,586 6/1974 Goosey ..................... ... 264/332 wherein during the abrading step the boron suboxide 5,135,892 8/1992 Ellison-Hayashi ...................... 501/1 (BxO) composition is maintained at low temperatures. The abrasive which is from the boron suboxide (BxO) FOREIGN PATENT DOCUMENTS family of compounds exhibits an unexpectedly high 574609 4/1959 Canada ................................ 423/278 quality of abrading comparable with the highest quality OTHER PUBLICATIONS particulate natural and synthetic diamond, which has a R. R. Pasternak, "Crystallographic Evidence for the hardness about double that of the boron suboxide (BxO) Existence of B7O, Acta Cryst.” 12 (1959), 612. of the present invention. S. LaPlaca, B. Post, "The Boron Carbide Structure Further, the invention includes a lapping and polishing Type', Planseeberichte Fur Pulvermetallurgie, Bd. 9, powder and lapping slurry wherein the powder is made 1961. from a dense, finely crystalline boron suboxide material H. F. Rizzo, W. C. Simmons, and H. O. Bielstein, "The with a Knoop hardness KHN100 of at least about 2800 Existence and Formation of the Solid B6O, Journal of kg/mm2 and preferably at least 3800 kg/mm2. the Electrochemical Society,” Jan. 1963. F. A. Halden, R. Sedlacek, “Growth and Evaluation of Boron Suboxide and Zirconium Dioxide Single Crys 18 Claims, 14 Drawing Sheets O5 DAMOND O3 BORON SUBOXIDE O.2 O. BORON CARBIDE 3s 3. 3.6 4. 4.6 5. 5.6 6. 6.6 7. HARDNESS x IOOO(kg/mm *2) 5,366,526 Page 2 OTHER PUBLICATIONS V. S. Makarov and Ya. A. Ugai, "Thermochemical C. E. Holcombe, Jr., and O.J. Horne, Jr., “Preparation Study of Boron Suboxide B6O”, Journal of the Less of Boron Suboxide, B60', Journal of the American Common Metals, 117 (1986), 277-281. Ceramic Society-Discussions and Notes, vol. 55, No. 2 C. Brodhag and F. Thevenot, "Hot Pressing of Boron (1971) 106. Suboxide B1202', Journal of the Less Common Metals, D. R. Petrak, R. Ruh, B. F. Goosey, "Preparation and 117 (1986), 1-6. Characterization of Boron Suboxide', National Bureau of Standards Special Publication 364, Solid State Chem Tadashi Endo, Tsugio Sato, Masahiko Shimada, "High istry, Proceedings of 5th Materials Research Sympo pressure synthesis of B2O with diamond-like struc siums, issued Jul. 1972. ture”, Journal of Materials Science Letters 6(1987), W. H. Rhodes, A. J. DeLai, “Research on Develop 683-685. ment and Fabrication of Boron Suboxide Specimens', David Emin, “Icosahedra Boron-Rich Solids', Physics AVCO Corp., prepared for Air Force Materials Labo Today, Jan., 1987. ratory, Aug., 1972. R. R. Petrak, Robert Ruh, and G. R. Atkins, “Mechani Andrzej Badzian, "Superhard Material Comparable in cal Properties of Hot-Pressed Boron Suboxide and Hardness to Diamond'', Appl. Phys. Lett. 53(25), 19 Boron”, Ceramic Bulletin, vol. 53, No. 8 (1974), Dec. 1988. 569-573. W. E. Moddeman, A. R. Burke, W. C. Bowling and D. P. M. Bills and D. Lewis, "Non-stoichiometry of Boron S. Foose, “Surface Oxides of Boron and B12O2 as Deter Suboxide (B6O)', Journal of the Less Common Metals, mined by XPS' Surface and Interface Analysis, v. 14 45 (1976) 343-345. n5, May, 1989, pp. 224-232. U.S. Patent Nov. 22, 1994 Sheet 1 of 14 5,366,526 F G. U.S. Patent Nov. 22, 1994 Sheet 2 of 14 5,366,526 O5 DAMOND O4 O3 BORON SUBOXDE O.2 O. BORON CARBIDE 3s 3. 3.6 4. 4.6 5. 5.6 6. 6.6 7. HARDNESS x IOOO(kg/mm *2) F G. 2 O8 BORON O7 sk SUBOXIDE DAMOND O4CARBDEBORON O 2.6 3. 3.6 4. 4.6 5. 5.6 6. 6.6 7. HARDNESS x IOOO (kg/mm2) F. G. 3 U.S. Patent Nov. 22, 1994 Sheet 3 of 14 5,366,526 2. (f) (f) C 1.5 BORON DAMOND s SUBOXDE S9 | k O5 BORON CARBIDE O 2.6 3. 3.6 4. 4.6 5. 5.6 6. 6.6 7. HARDNESS x IOOO (kg/mm2) 2.5 k BORON 2 SUBOXIDE (f)5 .5 DAMOND 9 s SSK O.5 O 2.6 3. 36 4. 4.6 5. 5.6 6. 6.6 7. HARDNESS x IOOO(kg/mm2) F. G. 5 U.S. Patent Nov. 22, 1994 Sheet 4 of 14 5,366,526 3 2.5 DAMOND (f)f5 2 C 5 SUBOXIDE s se* O.5 BORON CARBDE O 2.6 3. 3.6 4. 4.6 5. 5.6 6. 6.6 7. HARDNESS x IOOO (kg/mm *2) 5 BORON 4. * SUBOXIDE 2 C 3 s DIAMOND e BORON CARBIDE k O 2.6 3. 3.6 4. 46 5. 5.6 6. 6.6 7. HARDNESS x IOOO (kg/mm2) F. G. 7 U.S. Patent Nov. 22, 1994 Sheet 5 of 14 5,366,526 U.S. Patent Nov. 22, 1994 Sheet 7 of 14 5,366,526 U.S. Patent ov. 22, 1994 Sheet 10 of 14 5,366,526 U.S. Patent Nov. 22, 1994 Sheet 11 of 14 5,366,526 O'OL). Ok (Sdo) ALISN3N U.S. Patent Nov. 22, 1994 Sheet 3 of 14 5,366,526 5,366,526 1. 2 under a 100 gram load (VHN100) of 3,820 kg/mm2 and METHOD OF ABRADING WITH BORON a density of 2.60 grams/cc. The material is described as SUBOXIDE (BXO) AND THE BORON SUBOXIDE highly refractory, and suitable for use on surfaces sub (BXO) ARTICLES AND COMPOSITION USED ject to abrasion, e.g., grinding wheels, drill bits, ma 5 chine tools, etc., and in structures employed in high CROSS-REFERENCE TO RELATED temperature applications. APPLICATIONS In U.S. Pat. No. 3,816,586, a method of fabricating This Application is a continuation-in-part of applica boron suboxide products is disclosed. According to this tion Ser. No. 07/920,357 filed Jul. 28, 1992, pending, patent, a mixture of elemental boron and boron oxide is which is a continuation-in-part of Ser. No. 07/729,467 O cold pressed in a tantalum lined metal die. After the filed Jul. 12, 1991, now U.S. Pat. No. 5,135,892 both of pressure on the compacted mixture is released, it is which are hereby incorporated by reference. coated with a mixture of boron nitride and boron oxide, and is subjected to a second pressing step while heating BACKGROUND OF THE INVENTION at a temperature sufficient to melt the boron oxide in the 1. Field of the Invention 15 compacted mixture. This is followed by a cooling step The invention relates to a method of removing mate rial from a surface using an abrasive tool or powder and another hot pressing step. The boron suboxide comprising a boron suboxide (BxO) composition. The product made by this method is reported as being a invention further includes the boron suboxide (BxO) smooth, sound boron suboxide article, free of flaws and composition and articles made from the boron suboxide 20 contaminants, and suitable for a variety of applications. (BxO) composition used in lapping and polishing, hon Upon analysis, the boron suboxide product gave 80.1 wt ing, bonded abrasives, coated abrasives, wire sawing, % boron and 19.9 wt % oxygen which corresponds to abrasive flow machining, abrasive jet machining, abra the stoichiometry of B6O. It was also reported as having sive waterjet machining and fixed abrasive lapping. The a density of 2.60 grams/cc and a Knoop hardness under invention further relates to a novel boron suboxide 25 a 100 gram load (KHN100) of 3000 kg/mm2. (BxO) material and to a method for its preparation. Other reports on methods of preparing boron subox 2. Technology Review ide and the properties of this material are the following: A great deal of research has been devoted to develop 1.