US2657122A - Method for continuous preparation of crystals - Google Patents

Method for continuous preparation of crystals Download PDF

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Publication number
US2657122A
US2657122A US129021A US12902149A US2657122A US 2657122 A US2657122 A US 2657122A US 129021 A US129021 A US 129021A US 12902149 A US12902149 A US 12902149A US 2657122 A US2657122 A US 2657122A
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Prior art keywords
solution
mother
substance
crystals
allowing
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US129021A
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Chaudoye Noelle
Fourdeux Angeline
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Compagnie des Freins et Signaux Westinghouse SA
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Compagnie des Freins et Signaux Westinghouse SA
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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
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
    • C30B7/04—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent using aqueous solvents
    • 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
    • C30B19/00—Liquid-phase epitaxial-layer growth
    • C30B19/06—Reaction chambers; Boats for supporting the melt; Substrate holders
    • C30B19/061—Tipping system, e.g. by rotation
    • 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
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y10T117/1024—Apparatus for crystallization from liquid or supercritical state

Definitions

  • the ⁇ process is a discontinuous one.
  • This invention has for its object to provide anew methodof crystal manufacture which is free of this drawback and which enables production to becarried out continuously.
  • the method of the invention is essentially characterized by the fact that it comprises the pro- Vision, at a point of the crystallising apparatus above the mother-solution, of a cold condensation surface the temperature of which is lower than the condensation point of the vapor from the mother-solution, and that the condensed liquid is caused to flow down onto a certain amount of the substance from which it is desired to produce crystals, the resulting solution being allowed to fall into the mother-solution.
  • the invention further comprises an apparatus for carrying the above-dened method into effect, said apparatus being characterized by the fact that in one of the walls of an isothermal enclosure containing the mother-solution, a recessed member is mounted above said solution, a cooling conduct extends through said recessed member, said member carrying a perforate container containing a predetermined amount of the substance from which crystals are to be produced.
  • the mother-solution I of the substance to be crystallised is contained in a container 2 maintained at a constant temperature by means of a jacket 3 through which a flow of fluid adapted to maintain a constant temperature within the container I may be circulated.
  • the container 2 is sealed with a cover 4 throughwhich extends a thermostat thermometer 5 retained in the cover by means of a suitably luted or cemented plug 6.
  • the thermostat is adapted to restore automatically the heating circuit of the container 2 whenever the temperature drops beneath a predetermined value and to cut off said circuit when said value is slightly exceeded.
  • the cover 4 is also traversed by an agitator rod 1 the spider-like bottom part 8 of which carries the seed crystals 9 from and around which the desired crystals are to develop.
  • the agitator I extends through the cover 4 by means of a hy- 134,3Serial No. 129,021 ember 18, ⁇ 19,48
  • the. cover caglass tube I2 is further cemented, and in .said tube extendsacoohngcoil ⁇ lapthroilsh which cold ⁇ water is circulated.
  • the cooling coil I3 is retained in place by means of a plug I4 sealing the top of the tube I2.
  • the bottom end of said tube is provided with projecting hooks I5 from which is suspended a perforate container such as a wire basket containing a predetermined amount of the substance I'I from which the desired crystals are to be produced.
  • vapour from the mother-solution I will thus be allowed to condense over the cold wall of the tube I2 and the condensed liquid will now down onto the mother-substance I'I dissolving a portion thereof; the resulting solution, after being ltered through the bottom of the basket, flows down into the mother-solution I, enriching it and thereby maintaining a constant concentration therein.
  • Insertion of the mother-substance is very easily eiected merely by unstopping the glass tube I2.
  • the frequency at which the basket I 6 is replenished makes it possible to regulate the rate of crystallisation.
  • Method of continuous crystal production from a mother solution of a substance to be crystallized containing a seed crystal which comprises agitating said mother solution with said seed crystal while maintaining said solution at constant temperature, condensing vapor from said solution at a point directly above said solution at a temperature below said constant temperature, allowing the resulting condensed liquid to ow by gravity onto a supply of said substance to dissolve a portion thereof, and allowing the resulting solution to fall dropwise directly into said first-mentioned mother solution, therebyV to maintain a substantially constant concentration therein,
  • Method of continuous crystal preparation from a mother solution of a substance vto be crystallized containing a seed crystal within an enclosure which comprises maintaining said mother solution in said enclosure at a constant temperature and agitating said mother solution with said seed crystal maintaining an area of ,said enclosure directly above said mother solution at a condensation temperature below said constant temperature to cause vapor from said mother solution to condense on contact with said area, allowing the resulting liquid to ow by gravity onto a supply of said substance in said enclosure to dissolve a portion thereof, and allowing the resulting solution to reflux dropwise directly back into said mst-mentioned mother solution, and regulating said condensation temperature to provide a rate of reux effective to maintain a substantially constant concentration within said solution.

Description

Oct. 27, 1953 N. cHAUDoYE ETAL 2,657,122
METHOD FOR CONTINUOUS PREPARATION OF CRYSTALS Filed Nov. 25, 1949 :lllflll i'llllhllllllii Patented Oct. 27, 1953 METHOD FOR CONTINUOUS PREPARATION F CRYSTALS Nolle Chaudoye, Paris, and Angeline Fourdeuir, Puteaux, France, assignors to 'Compagnie des Freins & Signaux Westinghouse, Paris, France,
Societe Anonyme Application November 23 In France `Dec V3 Claims. l
In ,currently Vused apparatus for the industrial production of synthetic crystals in an aqueous medium involving agitation of the solution, the `process is a discontinuous one. This invention has for its object to provide anew methodof crystal manufacture which is free of this drawback and which enables production to becarried out continuously.
The method of the invention is essentially characterized by the fact that it comprises the pro- Vision, at a point of the crystallising apparatus above the mother-solution, of a cold condensation surface the temperature of which is lower than the condensation point of the vapor from the mother-solution, and that the condensed liquid is caused to flow down onto a certain amount of the substance from which it is desired to produce crystals, the resulting solution being allowed to fall into the mother-solution.
The invention further comprises an apparatus for carrying the above-dened method into effect, said apparatus being characterized by the fact that in one of the walls of an isothermal enclosure containing the mother-solution, a recessed member is mounted above said solution, a cooling conduct extends through said recessed member, said member carrying a perforate container containing a predetermined amount of the substance from which crystals are to be produced.
Further characteristic features and the advantages of the invention will appear from the ensuing description and the accompanying diagrammatic drawings which illustrate by Way of indication and not of limitation, one embodiment of the invention.
As shown in the drawing, the mother-solution I of the substance to be crystallised is contained in a container 2 maintained at a constant temperature by means of a jacket 3 through which a flow of fluid adapted to maintain a constant temperature within the container I may be circulated. The container 2 is sealed with a cover 4 throughwhich extends a thermostat thermometer 5 retained in the cover by means of a suitably luted or cemented plug 6. The thermostat is adapted to restore automatically the heating circuit of the container 2 whenever the temperature drops beneath a predetermined value and to cut off said circuit when said value is slightly exceeded.
The cover 4 is also traversed by an agitator rod 1 the spider-like bottom part 8 of which carries the seed crystals 9 from and around which the desired crystals are to develop. The agitator I extends through the cover 4 by means of a hy- 134,3Serial No. 129,021 ember 18, `19,48
(Cl. 2li-301) -draulic seal I0 containing paramn oil or the like, said seal Abeinghermetically mounted in a :plug y.I I cemented fin the coverA. `Said agitator may .have `a vertical up and down :motion imparted to it, Vbut `a rotaryagitator `may also be used,
AQCOrdingto theinventiomin the. cover caglass tube I2 is further cemented, and in .said tube extendsacoohngcoil `lapthroilsh which cold `water is circulated. The cooling coil I3 is retained in place by means of a plug I4 sealing the top of the tube I2. The bottom end of said tube is provided with projecting hooks I5 from which is suspended a perforate container such as a wire basket containing a predetermined amount of the substance I'I from which the desired crystals are to be produced. Y
The vapour from the mother-solution I will thus be allowed to condense over the cold wall of the tube I2 and the condensed liquid will now down onto the mother-substance I'I dissolving a portion thereof; the resulting solution, after being ltered through the bottom of the basket, flows down into the mother-solution I, enriching it and thereby maintaining a constant concentration therein.
By suitably selecting the dimensions of the cooling coil, the rate of flow and the temperature of the cooling fluid flowing therethrough, it is possible suitably to adjust the rate of dissolution of the mother-substance I'I.
Insertion of the mother-substance is very easily eiected merely by unstopping the glass tube I2.
The frequency at which the basket I 6 is replenished makes it possible to regulate the rate of crystallisation.
It will thus be seen that there will be no discontinuity in the process of crystal-production, since the-concentration of the mother-solution is automatically restored in a continuous manner and there are no sudden variations in this concentration.
It may also be seen that aside from actuating the agitator 1, the only operation required during the process is replenishing the basket or container I6 with the mother-material at regular predetermined intervals.
It will be distinctly understood that alterations may be made in the details of the apparatus described without departing from the spirit of the invention.
We claim:
l. Method of continuous crystal production from a mother solution of a substance to be crystallized containing a seed crystal, which comprises agitating said mother solution with said seed crystal while maintaining said solution at constant temperature, condensing vapor from said solution at a point directly above said solution at a temperature below said constant temperature, allowing the resulting condensed liquid to ow by gravity onto a supply of said substance to dissolve a portion thereof, and allowing the resulting solution to fall dropwise directly into said first-mentioned mother solution, therebyV to maintain a substantially constant concentration therein,
2. Method of continuous crystal preparation from a mother solution of a substance vto be crystallized containing a seed crystal within an enclosure, which comprises maintaining said mother solution in said enclosure at a constant temperature and agitating said mother solution with said seed crystal maintaining an area of ,said enclosure directly above said mother solution at a condensation temperature below said constant temperature to cause vapor from said mother solution to condense on contact with said area, allowing the resulting liquid to ow by gravity onto a supply of said substance in said enclosure to dissolve a portion thereof, and allowing the resulting solution to reflux dropwise directly back into said mst-mentioned mother solution, and regulating said condensation temperature to provide a rate of reux effective to maintain a substantially constant concentration within said solution.
3. In the method of claim 2, the step of ltering said reflux solution in its downward flow from said supply to said mother solution.
NOLLE CHAUDOYE. ANGE'LINE FOURDEUX.
References Cited Vin the file of this patent UNITED STATES PATENTS Number Name Date 984,645 Bock Feb. 21, 1911 1,751,740 Jeremiassen Mar. 25, 1930 2,204,180 Gerlach June 11, 1940 2,347,073 Beekhuis Apr. 18, 1944 2,424,273 Haas July 22, 1947 2,452,576 Kjellgren Nov. 2, 1948 2,459,869 Christensen et al. Jan. 25, 1949 OTHER REFERENCES Chappelle, Jean: Comptes Rendus, July 4, 1949, 229, pages 61-63.
Laboratory Apparatus and Reagents, Fisher Scientific Co. catalog, Pittsburgh, Pa. (1925), page 326, Fig. 9-605.

Claims (1)

1. METHOD OF CONTINUOUS CRYSTAL PRODUCTION FROM A MOTHER SOLUTION OF A SUBSTANCE TO BE CRYSTALLIZED CONTAINING A SEED CRYSTAL, WHICH COMPRISES AGITATING SAID MOTHER SOLUTION WITH SAID SEED CRYSTAL WHILE MAINTAINING SAID SOLUTION AT CONSTANT TEMPERATURE, CONDENSING VAPOR FROM SAID SOLUTION AT A POINT DIRECTLY ABOVE SAID SOLUTION AT A TEMPERATURE BELOW SAID CONSTANT TEMPERATURE, ALLOWING THE RESULTING CONDENSED LIQUID TO FLOW BY GRAVITY ONTO A SUPPLY OF SAID SUBSTANCE TO DISSOLVE A PORTION THEREOF, AND ALLOWING THE RESULTING SOLUTION TO FALL DROPWISE DIRECTLY INTO SAID FIRST-MENTIONED MOTHER SOLUTION, THEREBY TO MAINTAIN A SUBSTANTIALLY CONSTANT CONCENTRATION THEREIN.
US129021A 1948-12-18 1949-11-23 Method for continuous preparation of crystals Expired - Lifetime US2657122A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2766105A (en) * 1952-05-09 1956-10-09 Washken Edward Method of growing nepheline crystals
US2793103A (en) * 1954-02-24 1957-05-21 Siemens Ag Method for producing rod-shaped bodies of crystalline material
US2827366A (en) * 1954-03-04 1958-03-18 Olin Mathieson Crystallization apparatus
US2893847A (en) * 1954-02-23 1959-07-07 Siemens Ag Apparatus for preparing rod-shaped, crystalline bodies, particularly semiconductor bodies
US3050407A (en) * 1959-08-25 1962-08-21 Bell Telephone Labor Inc Single crystal garnets
US3101259A (en) * 1959-03-27 1963-08-20 Sawyer Res Products Inc Method of controlling deposition of crystalline material from solution on a seed by use of a temperature profile curve
US3230051A (en) * 1964-09-22 1966-01-18 John L Sampson Closed-system evaporation crystallizer
US3519399A (en) * 1967-05-22 1970-07-07 Hughes Aircraft Co Method for growing single crystals of semiconductors
US4931133A (en) * 1988-01-29 1990-06-05 Allied-Signal Inc. High temperature solution growth of barium borate (β-BaB2 O4)
US20090223439A1 (en) * 2008-03-07 2009-09-10 Tufts University Apparatuses and Methods for Growing Single Crystals

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US984645A (en) * 1908-05-13 1911-02-21 Johannes Bock Process for producing large well-formed crystals from solutions of different kinds.
US1751740A (en) * 1925-01-12 1930-03-25 Krystal As Process of separately recovering soluble substances in alpha coarse granular condition
US2204180A (en) * 1936-07-14 1940-06-11 Telefunken Gmbh Apparatus for cultivating crystals
US2347073A (en) * 1941-06-06 1944-04-18 Solvay Process Co Process for recovering solids from solution
US2424273A (en) * 1945-04-13 1947-07-22 Western Electric Co Crystal growing apparatus
US2452576A (en) * 1945-11-10 1948-11-02 Bengt R F Kjellgren Method of growing crystals
US2459869A (en) * 1946-08-10 1949-01-25 Bell Telephone Labor Inc Crystal growing apparatus

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US984645A (en) * 1908-05-13 1911-02-21 Johannes Bock Process for producing large well-formed crystals from solutions of different kinds.
US1751740A (en) * 1925-01-12 1930-03-25 Krystal As Process of separately recovering soluble substances in alpha coarse granular condition
US2204180A (en) * 1936-07-14 1940-06-11 Telefunken Gmbh Apparatus for cultivating crystals
US2347073A (en) * 1941-06-06 1944-04-18 Solvay Process Co Process for recovering solids from solution
US2424273A (en) * 1945-04-13 1947-07-22 Western Electric Co Crystal growing apparatus
US2452576A (en) * 1945-11-10 1948-11-02 Bengt R F Kjellgren Method of growing crystals
US2459869A (en) * 1946-08-10 1949-01-25 Bell Telephone Labor Inc Crystal growing apparatus

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2766105A (en) * 1952-05-09 1956-10-09 Washken Edward Method of growing nepheline crystals
US2893847A (en) * 1954-02-23 1959-07-07 Siemens Ag Apparatus for preparing rod-shaped, crystalline bodies, particularly semiconductor bodies
US2793103A (en) * 1954-02-24 1957-05-21 Siemens Ag Method for producing rod-shaped bodies of crystalline material
US2827366A (en) * 1954-03-04 1958-03-18 Olin Mathieson Crystallization apparatus
US3101259A (en) * 1959-03-27 1963-08-20 Sawyer Res Products Inc Method of controlling deposition of crystalline material from solution on a seed by use of a temperature profile curve
US3050407A (en) * 1959-08-25 1962-08-21 Bell Telephone Labor Inc Single crystal garnets
US3230051A (en) * 1964-09-22 1966-01-18 John L Sampson Closed-system evaporation crystallizer
US3519399A (en) * 1967-05-22 1970-07-07 Hughes Aircraft Co Method for growing single crystals of semiconductors
US4931133A (en) * 1988-01-29 1990-06-05 Allied-Signal Inc. High temperature solution growth of barium borate (β-BaB2 O4)
US20090223439A1 (en) * 2008-03-07 2009-09-10 Tufts University Apparatuses and Methods for Growing Single Crystals

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