US3917462A - Method of producing sodium beta-alumina single crystals - Google Patents

Method of producing sodium beta-alumina single crystals Download PDF

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Publication number
US3917462A
US3917462A US492279A US49227974A US3917462A US 3917462 A US3917462 A US 3917462A US 492279 A US492279 A US 492279A US 49227974 A US49227974 A US 49227974A US 3917462 A US3917462 A US 3917462A
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US
United States
Prior art keywords
alumina
melt
sodium beta
single crystals
pressure
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US492279A
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English (en)
Inventor
Paul J Yancey
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Union Carbide Corp
Original Assignee
Union Carbide Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Union Carbide Corp filed Critical Union Carbide Corp
Priority to US492279A priority Critical patent/US3917462A/en
Priority to DE19752532653 priority patent/DE2532653C3/de
Priority to CA232,155A priority patent/CA1055816A/en
Priority to FR7523318A priority patent/FR2279461A1/fr
Priority to JP50090348A priority patent/JPS5137900A/ja
Priority to GB31141/75A priority patent/GB1516327A/en
Application granted granted Critical
Publication of US3917462A publication Critical patent/US3917462A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/906—Special atmosphere other than vacuum or inert

Definitions

  • the present invention relates to the production of single crystals of sodium beta-alumina, Na O.5Al O to Na O.l lAl O More particularly the present invention is directed to a method for growing single crystals of sodium beta-alumina by the well known Czochralski crystal growth technique.
  • the Czochralski technique for crystal growth involves heating raw material having a chemical composition corresponding to that of the desired crystal in a refractory metal crucible to the melting point to provide a melt having a chemical composition corresponding to that of the desired single crystal.
  • a single crystal seed crystal of composition similar to the desired crystal is dipped into the melt surface and slowly withdrawn upward. This is done in such a way that a meniscus of the melt attaches itself to the seed and is pulled up slightly by its upward motion.
  • the liquid being just at the melting point, even a relatively small temperature decrease can cause solidification of melt on the seed crystal.
  • the liquid which is raised above the surface is cooled slightly and crystallizes out on the tip of the seed forming as a single crystal corresponding to the seed crystal.
  • Sodium beta-alumina has composition in the range of Na O.5Al O to Na O.1 lAl O (1:5 to 1:11 soda to alumina).
  • Basic to the Czochralski technique described above is the preparation of the melt by the melting of the raw materials, e.g. Na O and A1 in proportions of 1:5 and 1:1 1.
  • a method in accordance with the present invention for producing single crystals of sodium beta'alumina comprises:
  • melt having a composition of Na O.- Al O to Na OJ lAl O in a gaseous environment at a pressure of 760 mm 1' 50% pressure and containing oxygen in an amount of between about 5000 to 15,000 parts per million;
  • a crucible 10 suitably made of iridium is supported on a mount 12, suitably made of ceramic, such as alumina.
  • Induction heating coil 14 provides heat energy to raise the charge materials (i.e. Na O and Al o lplaced in crucible -10 to the melting point to provide a melt 16 having a chemical composition corresponding to sodium beta-alumina, i.e. Na O.- 5Al O to Na O.1lAl O
  • A' seed crystal 18 of sodium beta-alumina is placed in contact with melt 16 and raised to pull an elongate single crystal mass 20 of sodium beta-alumina.
  • the aforementionedarrangement is enclosed within a vessel 22, suitably formed of glass and a gaseous environment is provided by way of inlet 24.
  • the gaseous environment contains from about 5,000 to 15,000 parts per million (0 by volume), preferably about 10,000 ppm.
  • the remainder of the gaseous environment can be nitrogen, the noble gases or other gases non-reactive with the melt.
  • the gaseous environment exits at outlet 26 and the total pressure within vessel 22 is substantially atmospheric pressure and can range from 760 mm i 50%.
  • a mixture of Na O and A1 0 e.g.
  • oxygen is in an amount of about 10,000 parts per million.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Secondary Cells (AREA)
US492279A 1974-07-26 1974-07-26 Method of producing sodium beta-alumina single crystals Expired - Lifetime US3917462A (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
US492279A US3917462A (en) 1974-07-26 1974-07-26 Method of producing sodium beta-alumina single crystals
DE19752532653 DE2532653C3 (de) 1974-07-26 1975-07-22 Verfahren zur Herstellung von Natriumoxid-ß-Aluminiumoxid Einkristallen
CA232,155A CA1055816A (en) 1974-07-26 1975-07-24 Method of producing sodium beta-alumina single crystals
FR7523318A FR2279461A1 (fr) 1974-07-26 1975-07-25 Procede pour produire des mono-cristaux de beta-alumine sodique
JP50090348A JPS5137900A (en) 1974-07-26 1975-07-25 Natoriumubeeta aruminatanketsushono seizoho
GB31141/75A GB1516327A (en) 1974-07-26 1975-07-25 Method of producing sodium beta-alumina single crystals

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US492279A US3917462A (en) 1974-07-26 1974-07-26 Method of producing sodium beta-alumina single crystals

Publications (1)

Publication Number Publication Date
US3917462A true US3917462A (en) 1975-11-04

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Family Applications (1)

Application Number Title Priority Date Filing Date
US492279A Expired - Lifetime US3917462A (en) 1974-07-26 1974-07-26 Method of producing sodium beta-alumina single crystals

Country Status (5)

Country Link
US (1) US3917462A (enExample)
JP (1) JPS5137900A (enExample)
CA (1) CA1055816A (enExample)
FR (1) FR2279461A1 (enExample)
GB (1) GB1516327A (enExample)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4286025A (en) * 1979-03-12 1981-08-25 Grant Zigurd A Detector for thermoluminescence dosimetry
US4792377A (en) * 1987-02-09 1988-12-20 The Regents Of The University Of California Flux growth of sodium beta" alumina
US4797269A (en) * 1988-02-08 1989-01-10 Norton Company Production of beta alumina by seeding and beta alumina produced thereby
US5415127A (en) * 1993-07-07 1995-05-16 Ontario Centre For Materials Research Method of forming a single crystal film of sodium-beta "-alumina

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3595803A (en) * 1969-09-04 1971-07-27 Cortland O Dugger Method for growing oxide single crystals
US3608050A (en) * 1969-09-12 1971-09-21 Union Carbide Corp Production of single crystal sapphire by carefully controlled cooling from a melt of alumina
US3625868A (en) * 1968-06-20 1971-12-07 Siemens Ag Thin semiconductor growth layer on alumina deficient, crucible-pulled magnesium aluminum spinel monocrystal as well as the method for producing the layer and producing the monocrystals
US3715194A (en) * 1970-10-29 1973-02-06 Union Carbide Corp Melt grown alumina crystals and process therefor
US3795723A (en) * 1972-03-29 1974-03-05 Shell Oil Co Beta alumina production
US3859427A (en) * 1969-11-10 1975-01-07 Aluminum Co Of America Production of beta alumina

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3625868A (en) * 1968-06-20 1971-12-07 Siemens Ag Thin semiconductor growth layer on alumina deficient, crucible-pulled magnesium aluminum spinel monocrystal as well as the method for producing the layer and producing the monocrystals
US3595803A (en) * 1969-09-04 1971-07-27 Cortland O Dugger Method for growing oxide single crystals
US3608050A (en) * 1969-09-12 1971-09-21 Union Carbide Corp Production of single crystal sapphire by carefully controlled cooling from a melt of alumina
US3859427A (en) * 1969-11-10 1975-01-07 Aluminum Co Of America Production of beta alumina
US3715194A (en) * 1970-10-29 1973-02-06 Union Carbide Corp Melt grown alumina crystals and process therefor
US3795723A (en) * 1972-03-29 1974-03-05 Shell Oil Co Beta alumina production

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4286025A (en) * 1979-03-12 1981-08-25 Grant Zigurd A Detector for thermoluminescence dosimetry
US4792377A (en) * 1987-02-09 1988-12-20 The Regents Of The University Of California Flux growth of sodium beta" alumina
US4797269A (en) * 1988-02-08 1989-01-10 Norton Company Production of beta alumina by seeding and beta alumina produced thereby
US5415127A (en) * 1993-07-07 1995-05-16 Ontario Centre For Materials Research Method of forming a single crystal film of sodium-beta "-alumina

Also Published As

Publication number Publication date
DE2532653B2 (de) 1977-03-10
JPS5137900A (en) 1976-03-30
JPS5735159B2 (enExample) 1982-07-27
GB1516327A (en) 1978-07-05
FR2279461A1 (fr) 1976-02-20
DE2532653A1 (de) 1976-02-05
CA1055816A (en) 1979-06-05
FR2279461B1 (enExample) 1978-09-22

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Owner name: MORGAN GUARANTY TRUST COMPANY OF NEW YORK, AND MOR

Free format text: MORTGAGE;ASSIGNORS:UNION CARBIDE CORPORATION, A CORP.,;STP CORPORATION, A CORP. OF DE.,;UNION CARBIDE AGRICULTURAL PRODUCTS CO., INC., A CORP. OF PA.,;AND OTHERS;REEL/FRAME:004547/0001

Effective date: 19860106

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Free format text: RELEASED BY SECURED PARTY;ASSIGNOR:MORGAN BANK (DELAWARE) AS COLLATERAL AGENT;REEL/FRAME:004665/0131

Effective date: 19860925