Skip to main content

Methods of Preparation of Amorphous Boron

  • Chapter
Boron and Refractory Borides

Abstract

Preparation of pure elemental boron presents certain difficulties. The conditions necessary for its preparation must be carefully main tained because boron reacts strongly with many substances at high temperatures required for reduction of its compounds. Any by-products formed during the reduction are difficult to separate.

This is a preview of subscription content, log in via an institution to check access.

Access this chapter

Chapter
USD 29.95
Price excludes VAT (USA)
  • Available as PDF
  • Read on any device
  • Instant download
  • Own it forever
eBook
USD 84.99
Price excludes VAT (USA)
  • Available as PDF
  • Read on any device
  • Instant download
  • Own it forever
Softcover Book
USD 109.99
Price excludes VAT (USA)
  • Compact, lightweight edition
  • Dispatched in 3 to 5 business days
  • Free shipping worldwide - see info

Tax calculation will be finalised at checkout

Purchases are for personal use only

Institutional subscriptions

Preview

Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.

References

  • AMBERGER, E., DIETZE, W.: Formation of α-rhombohedral red boron. Z. Anorg. Allg. Chem. 332, 131 (1964)

    Article  CAS  Google Scholar 

  • ANDRIEUX, L.: New process for the preparation of boron. C.R. Acad. Sci. (Paris) 185, 119–20 (1927)

    CAS  Google Scholar 

  • ANDRIEUX, L.: The electrolysis of metallic oxides dissolved in fused boric anhydride or borates. New methods for preparation of amorphous boron, borides and some metals. Ann. Chem. Phys. 12, 432–507 (1929)

    Google Scholar 

  • ANDRIEUX, L.: Making of metallic powders by electrolysis of fused salts. Rev. Metallurg. 45, 49–59 (1948)

    CAS  Google Scholar 

  • ANDRIEUX, L., DEISS, W.J.: Obtaining boron by electrolysis of melts. Bull. Soc. Chim. 838, (1955)

    Google Scholar 

  • ARKEL, A.E.: Production of high melting metals by thermal decomposition of their compounds. Metallwirtschaft 13, 405–8 (1934).

    Google Scholar 

  • APKER, L., TAFT, E., DICKEY, J.: Photoelectric emission and contact potentials of semiconductors. Phys. Rev. 74, 1462–74 (1948)

    Article  CAS  Google Scholar 

  • ARMINGTON, A.F., DILLON, G.F., MITCHELL, R.F.: Preparation of high purity boron via the iodide. Trans. Metallurg. Soc. AIME 230, N 2, 350 (1964)

    CAS  Google Scholar 

  • BELYAEV, A.I., ZHEMCHUZHINA, E.A., FIRSANOVA, L.A.: Metallurgiya chistych metallov i elementarnych poluprovodnikov (Metallurgy of pure metals and elemental semicon ductors), Chapt.15, Moskow: Metallurgiya 1969

    Google Scholar 

  • BOWER, J.G.: Progress in Boron Chemistry. Vol. II, pp. 231–271. Oxford: Pergamon Press 1970

    Google Scholar 

  • COOPER, H.S.: BC13, US Patent 2369212 (1945)

    Google Scholar 

  • COOPER, H.S.: Electrolytic production of boron. US Pat. 2572248 (1951a)

    Google Scholar 

  • COOPER, H.S.: Electrolytic production of boron. US Pat. 2572249 (1951b)

    Google Scholar 

  • COOPER, H.S., SCHAEFER, C.: Production of boron by fused salt-bath electrolysis. US Pat. 2,918,417 (1959)

    Google Scholar 

  • CUEILLERON, J.: Purification of elemental boron. Ann. Chim. 19, 459 (1944)

    CAS  Google Scholar 

  • CUEILLERON, J., PICHAT, P.: Manufacture of pure boron. C.R. Acad. Sci. (Paris) 260, 190 (1965)

    CAS  Google Scholar 

  • CUEILLERON, J., CRUIZAT, B.: Reduction of copper borate by hydrogen. Bull. Soc. Chim. France, 1207 (1973)

    Google Scholar 

  • CUEILLERON, J., CRUIZAT, B.: Preparation of high purity boron by reduction of boron chloride with hydrogen in an argon induction plazma. In: Boron, Preparation, Structure and Properties, p. 15–17 (F.N. Tavadze, Ed.) Moscow: Nauka 1974

    Google Scholar 

  • DEB, S.K., KHUNDKAR, M.H.: Boridation of metallic powder by B chloride. J. Indian Chem. Soc. 23, 555 (1958)

    Google Scholar 

  • DEISS, W.J., ANDRIEUX, L.: The boridation of metallic powders by boron chloride. Bull. Soc. Chim. France, 178–82 (1959)

    Google Scholar 

  • DEVYATYKH, G.G.: In: Poluchenie i analiz veshchestv osoboi chistoty (Preparation and Analysis of Super Pure Substances), p. 15, Moskow: Nauka 1966

    Google Scholar 

  • EFREMKIN, V.V.: Trudy Ural Nauch-Issledovatel. Chimi.Inst. (Trans Ural’s Sci. Res. Inst. Chem.), Vol. V, p. 152, Moskow: Goschimizdat 1957

    Google Scholar 

  • EFREMKIN, V.V., MIKULINSKII, A.S.: Mechanism of the reduction of boric anhydride with magnesium. Trans. Ural’s Sci. Res. Inst. Chem. Vol. V, p. 211, Moskow: Goschimizdat 1957

    Google Scholar 

  • EFREMKIN, V.V., SHEVELEVA, S.S.: Preparation of amorphous boron. Trans. Ural’s Sci. Res. Inst. Chem. Vol. V, p. 232, Moskow: Goschimizdat 1957

    Google Scholar 

  • EPELBAUM, V.A., STAROSTINA, M.T.: In: Bor. Trudy konferencii po chimii Bora i ego soedinenii (Trans. Conf. Boron and its Compounds Chemistry) p. 97, Moskow: Goschimizdat 1958

    Google Scholar 

  • FEDOROV, T.F., SHAMRAI, F.I., NISELSON, L.A., PETRUSEVICH, I.V.: Preparation of elemental boron. Zhurnal neorganicheskoi Chimii (Inorg. Chem.) 5, 226 (1960)

    CAS  Google Scholar 

  • FETTERLY, G.H.: In: Boron (Ed. G.K. Gaulé), Vol. I, p. 15, New York: Plenum Press 1960

    Google Scholar 

  • GMELIN’S Handbuch der anorganischen Chemie. 8, Vol. XIII Bor. Weinheim: Chemie Verlag (1926) Supplementary Vol. (1954)

    Google Scholar 

  • HAAG, H.: High purity boron. US Pat. 2794708 (1957)

    Google Scholar 

  • HACKSPILL, L., STIEBER, A., HOCART, R.: Crystallized boron. C.R. Acad. Sci. (Paris) 193, 776–8 (1931)

    CAS  Google Scholar 

  • HAGENMULLER, P., PAPE, R. DE: Reduction of B-trifluoride by Ca-hydride. C.R. Acad. Sci. (Paris) 249, 114 (1959)

    CAS  Google Scholar 

  • HAMBLYN, S.M.L., REUBEN, B.G., THOMPSON, B.: Hydrogen reduction of boron trichloride to boron in an R.F. plasma. Spec. Ceram. N 5, 147 (1973)

    Google Scholar 

  • HIGASHI, KEI: Preparation of B by reducing BC13 with Zn. (ii) Preparation end purification of BCl3. (iii) Factors affecting the deposition of B. Kyushu Kozan Gakkai-Shi 29, 209, 368 (1961)

    CAS  Google Scholar 

  • HINZ, I., WIRTH, H.: Purity of B produced by the decomposition of diboran and sub sequent zone melting. In: Boron (Ed. G.K. Gaulé), Vol. II, p. 9, New York: Plenum Press 1965

    Google Scholar 

  • HOBBS, D.Z., CAMPBELL, I.T., BLOCHE, F.E.: Methods used in preparing boron. Rep. Invest. Bur. Mines US Dept. Int. N 6456 (1964)

    Google Scholar 

  • HUG, A.K., DEB, S.K., KHUNDKAR, M.H.: Separation of heavy metals ions from mixtures with H3BO3. Indian J. Appl. Chem. 21, 81 (1958)

    Google Scholar 

  • ITO, HISASHI, YANAGASE TSUTOMU, HIGASHI, KEI: Purity and crystallinity of boron by reduction of BC13 with Zn. Nippon Kogyo Kaishi 78, 667 (1962)

    CAS  Google Scholar 

  • ITO, HISASHI, HIGASHI, KEI, MARUTA, KENJI: On preparation of boron by reducing boron trichloride with zinc. IV. Reduction reaction under low pressure. Kyushu Kozan Gakkai-Shi 31, 390 (1963a)

    CAS  Google Scholar 

  • ITO, HISASHI, AJUMA, KEI, MARUTA, KENJI: Nippon Kogyo Kaishi 79, 886 (1963b)

    Google Scholar 

  • ITO, HISASHI, YANAGASE, TSUTOMU, HIGASHI, KEI: Preparation of boron by reducing BCl3 with zinc. Trans. Japan Inst. Metals, 4, 205 (1963c)

    CAS  Google Scholar 

  • ITO, HISASHI, HIGASHI, KEI, MARUTA, KENJI: The preparation of boron by reducing boron trichloride with hydrogen. Kyushu Kozan Gakkai-Shi 32, 128 (1964)

    CAS  Google Scholar 

  • JAHAN, R., KHUNDKAR, M.H.: Reduction of cobalt borate by hydrogen. J. Indian Chem. Soc. 38, 7 (1961)

    CAS  Google Scholar 

  • JOHNSTON, H.L., HERSH, H.N., KERR, E.C.: Low temperature heat capacities of inorganic solids, V.J. Am. Chem. Soc. 73, 1112–7 (1951)

    Article  CAS  Google Scholar 

  • KAHLENBERG, H.H.: Boron and boron suboxide. Trans. Am. Electrochem. Soc. 47, 23 (1925)

    Google Scholar 

  • KEMENAR, B.: Preparation of elemental boron. Z. Anorg. Allg. Chem. 342, 108 (1962)

    Article  Google Scholar 

  • KIESSLING, R.: Preparing boron of high purity. Acta Chem. Scand. 2, 707–12 (1948)

    Article  CAS  Google Scholar 

  • KOREF, F.: Further growth of metal crystals by separation from the gaseous phase. Z. Electrochem. 28, 511–7 (1922)

    CAS  Google Scholar 

  • KRENEV, V.A., SAVEľEV, B.A., EVDOKIMOV, V.I.: In: Termodinamika i kinetika processov vosstanovleniya metallov (Thermodynamics and Kinetics of Metal Reduction Pro-cessess), p. 122, Moskow: Nauka 1972

    Google Scholar 

  • KROLL, W.: Preparation of amorphous boron. Z. Anorg. Chem. 101, 1–33 (1918)

    Google Scholar 

  • LAGRENAUDIE, J.: Semiconducting properties of boron. J. Chem. Phys. 50, 629 (1953)

    CAS  Google Scholar 

  • LAUBENGAYER, A.W., HURD, D.T., NEWKIRK, A.E., HOARD, H.: Preparation and properties of pure crystalline boron. J. Am. Chem. Soc. 65, 1924 (1943)

    Article  CAS  Google Scholar 

  • MCCARTY, L.V., CARPENTER, D.R.: Preparation of crystal modifications of boron -Synthesis of B-tri-iodide. J. Electrochem. Soc. 107, 38 (1960)

    CAS  Google Scholar 

  • MARCHESINI, L.: Reduction of boric anhydride with magnesium. Techn. Ital. 33, 139 (1968)

    CAS  Google Scholar 

  • MARKOVSKII, L.Ya.: Chemistry of magnesiothermal preparation of boron. Electron. Technol. 3, 95 (1970)

    CAS  Google Scholar 

  • MARKOVSKII, L.Ya., BELOV, M.P.: Chemical reactions occuring in the reduction of boric anhydride and magnesium. Zhur. Prik. Chim. (J. Appl. Chem.) 37, 1658 (1964)

    CAS  Google Scholar 

  • MARKOVSKII, L.Ya., BELOV, M.P.: Source of oxygen in amorphous boron, prepared by magnesium thermal method. Zhur. Prik. Chim. (J.Appl.Chem.) 40, 727 (1967)

    CAS  Google Scholar 

  • MARKOVSKII, L.Ya., KAPUTOVSKAYA, G.V.: Properties of Mg borides and their role in the preparation of boron by the Mg thermal method. Zhur. prikladnoi chimii (J. Appl. Chem.) 35, 723 (1962)

    Google Scholar 

  • MARKOVSKII, L.Ya., KONDRASHEV, Ju.D.: Composition and properties of the borides of Groups I and II of the periodic system. Zhur. Neorg. Chim. (J. Inorg. Chem.) 2, 34 (1957)

    CAS  Google Scholar 

  • MARKOVSKII, L.Ya., KONDRASHEV, Ju.D., KAPUTOVSKAYA, G.V.: Zhurnal obshchei chimii. (J. Gen. Chem.) 25, 433 (1955)

    CAS  Google Scholar 

  • MARON, F.S., VAL’SHCHIKOV, V.I.: Tezisy dokladov konferencii po Boru, ego Soedineniyam i splavam (Proc. Conf. Boron, its Alloys and Compounds) p. 12, Kiev 1962

    Google Scholar 

  • MAZZA, H., SAWYER, D.L., BAIER, R.W.: Amorphous high-purity Boron. US Pat. 2866688 (1958)

    Google Scholar 

  • MEERSON, G.A., SMIRNOV, M.P.: Mechanism of electrolytic preparation of borides of difficultly fusible metals. Chemistry of rare elements (Chimiya redkich elementov), Acad. Nauk S.S.S.R., 2, 130 (1955)

    Google Scholar 

  • MELLOR, J.W.: Comprehensive Treatise on Inorganic and Theoretical Chemistry, Vol. V, p. 1–147, London: Longmans Green 1924

    Google Scholar 

  • MEYER, F., ZAPPNER, R.: The preparation of boron by the dissociation of boron bromide. Ber. 54 B, 550–5 (1921)

    Google Scholar 

  • MIKHEEVA, V.I., MARKINA, V.Yu.: Physical chemical analysis for the reaction of magnesium with boric anhydride. Zhur. Neorg. Chim. (J. Inorg. Chem.) 2, 1232 (1957)

    CAS  Google Scholar 

  • MIKULINSKII, A.S., EFREMKIN, V.V., SHEVELEVA, S.S., SACHKO, A.P.: Preparation of amorphous B by magnesium thermal method. Trudy Ural. Nauch. Issledovatel Chimi. Inst. (Trans. Ural’s Sci. Res. Inst. Chem.) Vol. V, 5, 166 (1957a)

    Google Scholar 

  • MIKULINSKII, A.S., YAKUNCHIKOV, V.N., VAL’SHCHIKOV, V.I., EFREMKIN, V.V.: Refining of amorphous B by oxidative roasting in a fluidized bed. Trudy Ural. Nauch. Issledovatal. Chim. Inst. 5, 206 (1957b)

    Google Scholar 

  • MILLER, G.T.: Electrolytic production of boron. J. Electrochem. Soc. 106, 815–9 (1959)

    Article  CAS  Google Scholar 

  • MILLER, G.T.: Production of boron. J. Electrochem. Soc. 107, 817 (1960)

    Article  Google Scholar 

  • MIľMAN, D.N., BOBKOV, V.H.: Tezisy dokladov konferencii po boru, ego soedineniyam i splavam. (Proc. Conf. Boron, its Compounds and Alloys) p. 15, Kiev: 1962

    Google Scholar 

  • MOISSAN, H.: Preparation du bor amorphe. C.R. Acad. Sci. (Paris) 114, 392 (1892)

    Google Scholar 

  • MONIER, R., TISSOT, P., PEARSON, R.: Preparation of boron by electrolysis of boron sesquioxide solution in cryolite. Helv. Chem, Acta 49 (1), 67–72 (1965)

    Article  Google Scholar 

  • NEWKIRK, A.E.: Preparation and chemistry of elementary boron. Adv. Chem. Series 32, 27–41 (1961)

    Google Scholar 

  • NIEMYSKI, T., OLEMPSKA, Z.: High grade boron. Polish Pat. 46818 (1963a)

    Google Scholar 

  • NIEMYSKI, T., OLEMPSKA, Z.: High grade boron. Polish Pat. 46819 (1963b)

    Google Scholar 

  • NIES, N.P., FAJANS, E.W., THOMAS, L.L., HILBERT, L.E., MORGAN, N.: Electrolytic production of boron. US Pat. 2832730 (1958)

    Google Scholar 

  • NISEL’SON, L.A., PETRUSEVICH, I.V., SHAMRAI, F.I., FEDOROV, G.V.: In: Vysokotempera-turnye neorganicheskie soedineniya (High Temperature Inorganic Compounds) p. 362, Kiev: Naukova Dumka 1965

    Google Scholar 

  • OLEMPSKA, Z.: Current problems of the chemistry and technology of boron. Wiadom. Chem. 21, 169 (1967)

    CAS  Google Scholar 

  • PERMINOV, V.P., NERONOV, V.A.: Magnesiothermic furnace-less production of boron from boric oxide. Poroshkovaya metallurgiya (Powder Metallurgy) 15 (1969)

    Google Scholar 

  • PICHAT, P.: β-Rhombohedral from of boron. C.R. Acad. Sci. (Paris) C 264, 1121 (1967)

    Google Scholar 

  • PICHAT, P., FOREST, D.: Preparation of powdered boron. Bull. Soc. Chim. 10, 3825 (1967)

    Google Scholar 

  • POLYAK, A.M., SHEVELEVA, S.S., USPENSKAYA, Z.P.: Substitution of sulfuric acid by hydrochloric acid in the production of elemental B. Trudy Uralskogo Nauchno-Issledovatelskogo Chimicheskogo Instituta (Trans. Ural’s Sci. Res. Inst. Chem.), Vol. 5, p. 222, Moskow: Goschimizdat (1957)

    Google Scholar 

  • POWELL, C.F., ISH, C. J., BLOCHER, J.M.: Preparation of high purity boron. In: Boron (Ed. G.K. Gaulé), Vol. I, p. 7, New York: Plenum Press 1960

    Google Scholar 

  • RAY, R.C.: Magnesium boride and amorphous boron. J. Chem. Soc. (London) 105, 2162–8 (1914)

    CAS  Google Scholar 

  • SAMSONOV, G.V., OBOLONCHIK, V.A., KULICHKINA, G.N.: MP diagram of the KBF4 — KCl system. Chimicheskaya Nauka i promyshlennost (Chemical Science and Industry) 4, 804 (1959)

    CAS  Google Scholar 

  • SAMSONOV, G.V., OBOLONCHIK, V.A., KULICHKINA, G.N.: Electrolytic production of boron. Zhurnal prikladnoi chimii (J. Appl. Chem.) 33, 1365 (1960a)

    CAS  Google Scholar 

  • SAMSONOV, G.V., VALYASHKO, M.G., MARKOVSKII, L.YA., ZHIGACH, A.F.: Bor, ego splavy i soedineniya (Boron, its Alloys and Compounds) Kiev: Naukova Dumka 1960b

    Google Scholar 

  • SCHAEFFER, J.C., SCHMIDT, E.C.: Purifying Boron. Brit. Pat. 1064093 (1967)

    Google Scholar 

  • Fr. Pat. 1388928 (1965)

    Google Scholar 

  • US Pat. 3137647 (1964)

    Google Scholar 

  • US Pat. 2528514 (1950)

    Google Scholar 

  • SCHOTT, S., HANSLEY, T.: Boron. US Pat. 3086847 (1964)

    Google Scholar 

  • SCHRANGLE, W., DIETZE, W.: Boron Coating of Metal Fibers by Vacuum Pyrolytic deposition from Boron Compounds. Ger. Pat. 1521199 (1972)

    Google Scholar 

  • SEREBRENNIKOVA, M.A.: Tezisy dokladov konferencii po boru, ego splavam i soedineniyam (Proc. Conf. Rep. Boron, its Alloys and Compounds), p. 14, Moskow: Goschimizdat: Naukova Dumka 1962

    Google Scholar 

  • SHAMRAI, F.I., MIKHEEVA, V.I.: Refining of Amorphous Boron. Zhurn. Neorg. Khim. (J. Inorg. Chem.) 2, 1242 (1957)

    CAS  Google Scholar 

  • STERN, D.R., In: Boron (Ed. G.K. Gaulé), Vol. I, p. 27, New York: Plenum Press 1960a

    Google Scholar 

  • STERN, D.R.: Preparation of boron from boron carbide. J. Electrochen Soc. 107, 441 (1960b)

    Article  CAS  Google Scholar 

  • STERN, D.R., LYNDS, L.J.: Pure crystalline boron. J. Electrochen Soc. 105, 676 (1958)

    Article  CAS  Google Scholar 

  • SWIFT, R.M., WHITE, D.: Low temperature heat capacities of magnesium diboride (MgB2) and magnesium tetraboride (MgB4). J. Amer. Chem. Soc. 79, 3641–4 (1957)

    Article  CAS  Google Scholar 

  • TALLEY, C.P., LINE, L.E., OVERMAN, O.D.: Preparation and Properties of massive amorphous elemental boron. In: Boron (Ed. G.K. Gaulé), Vol. I, p. 94, New York: Plenum Press 1960

    Google Scholar 

  • TODD, B.J., MILLER, R.R.: Heat of formation of B2O3. J. Am. Chem. Soc. 68, 530 (1946)

    Article  CAS  Google Scholar 

  • UNO, R.: Electric properties of boron. J. Phys. Soc. Japan 13, 667 (1958)

    Article  CAS  Google Scholar 

  • WEINTRAUB, F.: Boron. Trans. Am. Electrochem. Soc. 14, 167 (1907)

    Google Scholar 

  • WEINTRAUB, F.: Preparation and properties of pure boron. Trans. Am. Electrochem. Soc. 16, 165 (1909)

    Google Scholar 

  • WEINTRAUB, F.: The properties and preparation of the element boron. Ind. Eng. Chem, 3, 2 (1911);

    Article  Google Scholar 

  • WEINTRAUB, F.: The properties and preparation of the element boron. Ind. Eng. Chem, 5, 106 (1913)

    Article  CAS  Google Scholar 

  • WIEBERG, E., AMBERGER, E., DIETZE, W.: Process for the preparation of boron with an α-rhombohedral crystal structure. Ger. Pat. 1231221 (1966)

    Google Scholar 

  • WIRTH, H., DIETZE, W.: High purity boron. Ger. Pat. 1174750 (1964)

    Google Scholar 

  • WOHLER, F., SAINT CLAIR DEVILLE, H.: Ãœber das Bor. Ann. Chim. Phys. 100, 635 (1857)

    Google Scholar 

  • YANNACAKIS, J., NIES, N.P.: Preparation of crystalline boron. In: Boron (Ed. G.K. Gaulé), Vol. I, p. 38, New York: Plenum Press 1960

    Google Scholar 

  • YANO; TOMASABURO; KOMATSU; AKITOSHI: Electrolytic preparation of boron. Japan. Pat. 3856 (1961)

    Google Scholar 

  • Electrolytic preparation of high purity metallic boron; Japan. Pat. 7005 (1961), 6109 (1961), 6110 (1961)

    Google Scholar 

  • Electrolysis of boron, Japan. Pat. 12503 (1962)

    Google Scholar 

  • ZHIGACH, A.F., STASINEVICH, D.S.: Chimiya gidridov (Hydride Chemistry), Leningrad: Chimiya 1968

    Google Scholar 

  • ZINTL, E., MORAWITZ, W., GASTINGER, E.: Boron monoxide. Z. Anorg. Allg. Chem. 245, 8 (1940)

    Article  CAS  Google Scholar 

Download references

Authors

Editor information

Editors and Affiliations

Rights and permissions

Reprints and permissions

Copyright information

© 1977 Springer-Verlag Berlin Heidelberg

About this chapter

Cite this chapter

Zhigach, A.F., Stasinevich, D.C. (1977). Methods of Preparation of Amorphous Boron. In: Matkovich, V.I. (eds) Boron and Refractory Borides. Springer, Berlin, Heidelberg. https://doi.org/10.1007/978-3-642-66620-9_13

Download citation

  • DOI: https://doi.org/10.1007/978-3-642-66620-9_13

  • Publisher Name: Springer, Berlin, Heidelberg

  • Print ISBN: 978-3-642-66622-3

  • Online ISBN: 978-3-642-66620-9

  • eBook Packages: Springer Book Archive

Publish with us

Policies and ethics