# US 5,343,827 A · Method for crystal growth of beta barium boratean > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,343,827 A - Document ID: US5343827A - Status: Granted - Kind: A - Application number: 07/838,628 - Filed: 1992-02-19 - Granted: 1994-09-06 - Earliest claimed: 1992-02-19 - Assignees: Crystal Technology, Inc. - Inventors: Peter F. Bordui; George D. Calvert - Web page: https://patentgrep.com/patent/US5343827A ## CPC - C30B 9/00: Single-crystal growth from melt solutions using molten solvents (by normal or gradient freezing C30B11/00; by zone-melting C30B13/00; by crystal pulling C30B15/00; on immersed seed crystal C30B17/00; by liquid phase epitaxial growth C30B19/00; under a protective fluid C30B27/00) - C30B 29/10: Inorganic compounds or compositions - C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR ## Abstract A method of growing optical quality beta barium borate; crystals from a pure NaCl fluxed melt. The method comprises maintaining particular thermal field conditions throughout the melt and slowly cooling the melt to cause beta barium borate to crystallize from the melt. The rate of cooling may be at a rate of not greater than 3.degree. C. per day. The method may utilize a seed crystal, suspended into the melt, so that the beta barium borate may crystallize on the seed crystal. ## Claims ### Claim 1 A method of growing a crystal of .beta.-BaB.sub.2 O.sub.4 from solution, comprising the steps of: a. preparing a mixture of a BaB.sub.2 O.sub.4 solution and a pure NaCl solvent; b. heating said mixture to produce a melt thereof; c. suspending a seed crystal of BaB.sub.2 O.sub.4 in said melt; d. maintaining particular thermal field conditions throughout said melt; and e. decreasing the temperature of said melt to thereby cause .beta.-BaB.sub.2 O.sub.4 to crystalize from said melt on said seed crystal. ### Claim 2 (depends on 1) The method of claim 1, wherein said melt comprises a molar ratio of NaCl/melt from about 0.6 to about 0.85. ### Claim 3 (depends on 1) The method of claim 1, wherein the step of suspending a seed crystal of BaB.sub.2 O.sub.4 in said melt further comprises rotating the seed crystal in said melt. ### Claim 4 (depends on 1) The method of claim 1, wherein the step of decreasing the temperature of said melt comprises decreasing the temperature of said melt at a rate not greater than about 3.degree. C. per day. ### Claim 5 (depends on 1) The method of claim 1, wherein the step of slowly decreasing the temperature of said melt comprises decreasing the temperature of said melt from an initial temperature chosen to correspond to the solubility of BaB.sub.2 O.sub.4 in NaCl. ### Claim 6 (depends on 1) The method of claim 1, wherein said melt comprises a molar ratio of NaCl/melt from about 0.6 to about 0.85 and the step of decreasing the temperature of said melt comprises decreasing the temperature of said melt from an initial temperature from about 870.degree. C. to about 770.degree. C. corresponding with the molar ratio of NaCl/melt. ### Claim 7 A method of growing crystalline .beta.-BaB.sub.2 O.sub.4 from a NaCl fluxed melt, comprising the steps of: a. maintaining particular thermal field conditions throughout said melt; and b. slowly cooling said melt to cause .beta.-BaB.sub.2 O.sub.4 to crystallize from said melt. ### Claim 8 (depends on 7) The method of claim 7, wherein the step of slowly cooling comprises cooling said fluxed melt at a rate of not greater than 3.degree. C. per day. ### Claim 9 (depends on 7) The method of claim 7, further comprising the step of suspending a seed crystal of BaB.sub.2 O.sub.4 in said fluxed melt to cause .beta.-BaB.sub.2 O.sub.4 to crystallize from said melt on said seed crystal. ### Claim 10 (depends on 7) The method of claim 7, wherein the step of slowly cooling comprises cooling the fluxed melt from an initial temperature chosen to correspond to the solubility of BaB.sub.2 O.sub.4 in NaCl. ### Claim 11 (depends on 7) The method of claim 7, wherein said fluxed melt comprises a molar ratio of NaCl/fluxed melt from about 0.6 to about 0.85. ### Claim 12 (depends on 11) The method of claim 11, wherein said fluxed melt comprises a molar ratio of NaCl/fluxed melt from about 0.6 to about 0.85 and the initial temperature ranges from about 870.degree. C. to about 770.degree. C. corresponding with the molar ratio of NaCl/melt. ### Claim 13 A method of growing a single crystal boule of .beta.-BaB.sub.2 O.sub.4, comprising the steps of: preparing a mixture of BaB.sub.2 O.sub.4 and a flux comprising pure NaCl; b. heating said mixture in a crucible enclosed within a furnace so as to raise the temperature of the mixture to a first temperature to form a melt of said mixture and to maintain particular thermal spatial conditions throughout the melt; c. homogenizing the melt; d. immersing a seed crystal of .beta.-BaB.sub.2 O.sub.4 mounted on the end of a seed crystal holder into the melt; e. rotating the seed crystal holder and the seed crystal within the melt; and f. decreasing the temperature of the melt while continuing to rotate the seed crystal holder and the seed crystal to cause .beta.-BaB.sub.2 O.sub.4 to crystallize from the melt onto said seed crystal to form the boule. ### Claim 14 (depends on 13) The method of claim 13, wherein the step of homogenizing the melt comprises: a. stirring the melt while maintaining the temperature of the melt at the first temperature; and b. discontinuing the stirring and, thereupon, reducing the temperature of the melt to a second temperature lower than the first temperature. ### Claim 15 (depends on 13) The method of claim 13, wherein the step of rotating comprises rotating the seed crystal holder and the seed crystal with regular reversals of direction within the melt. ### Claim 16 (depends on 13) The method of claim 13, further comprising the steps of: a. moving the seed crystal holder relative to the crucible so as to remove the newly grown boule from the melt but retain the newly grown boule in the furnace; and b. decreasing the temperature of the furnace to ambient temperature and retaining the seed crystal holder and the newly grown boule in the furnace until the newly grown boule has thermally stabilized. ### Claim 17 (depends on 13) The method of claim 13, wherein the melt comprises the molar ratio of NaCl:melt in the range of about 0.6 to about 0.85. ### Claim 18 (depends on 13) The method of claim 13, further comprising the step of cooling the homogenized melt so as to decrease the temperature of the melt from an initial temperature chosen to correspond to the solubility of BaB.sub.2 O.sub.4 in NaCl. ### Claim 19 (depends on 13) The method of claim 13, wherein the melt comprises the molar ratio of NaCl:melt in the range of about 0.6 to about 0.85 and further comprising the step of cooling the homogenized melt so as to decrease the temperature of the melt from about 870.degree. C. to about 770.degree. C. corresponding with the molar ratio of NaCl:melt. ### Claim 20 (depends on 13) The method of claim 13, wherein the step of slowly decreasing the temperature of the melt comprises decreasing the temperature of the melt at a rate of no greater than 3.degree. C. per day.