Method and apparatus for growing crystals

• US 5,997,636 A
• Filed: 05/01/1998
• Issued: 12/07/1999
• Est. Priority Date: 05/01/1998
• Status: Expired due to Fees

• Current Assignee: Instrumentation Technology Associates Incorporated
• Original Assignee: Instrumentation Technology Associates Incorporated
• Inventors: Gamarnik, Moisey Y., Alvarado, Ulises R.
• Primary Examiner(s): Hiteshew, Felisa
• Assistant Examiner(s): CHAMPAGNE, DONALD
• Application Number:
  US09/071,546
• Time in Patent Office: 585 Days
• Field of Search: 117/70, 117/206, 117/901, 422/245.1
• US Class Current: 117/70
• CPC Class Codes: B01D 9/0018 Evaporation of components of the mixture to be separated
• CPC Class Codes: B01D 9/0072 Crystallisation in microfluidic devices
• CPC Class Codes: B01D 9/0077 Screening for crystallisation conditions or for crystal forms
• CPC Class Codes: B01L 2300/0838 Capillaries
• CPC Class Codes: B01L 3/06 Crystallising dishes
• CPC Class Codes: C30B 29/58 Macromolecular compounds
• CPC Class Codes: C30B 7/00 Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions from molten solvents C30B9/00; by normal or gradient freezing C30B11/00; under a protective fluid C30B27/00
• CPC Class Codes: C30B 7/02 by evaporation of the solvent
• CPC Class Codes: Y10S 117/901 Levitation, reduced gravity, microgravity, space
• CPC Class Codes: Y10T 117/1032 Seed pulling

Abstract

For growing crystals, either in ground testing or in space, a capillary tube is used, which contains the solution of the substance to be crystallized, a layer of absorbent and a layer of air or other gas separating the solution from the absorbent. Two absorbent layers may be used on opposite sides of the solution, each separated from the solution by a gaseous layer. To delay the onset of crystallization, the absorbent on each side may be separated from the solution by two gaseous layers, with a charge of absorbable liquid between them. An absorbent may be removed or modified by removing or perforating an end cap used to seal the absorbent within the capillary tube.

Claims

1. A method for growing crystals comprising the steps of:

establishing a column of layers within a capillary tube, the column comprising a solution of a substance to be crystallized and a solvent, an absorbent, and a gaseous layer separating the solution and the absorbent from each other; and

increasing the concentration of said substance in the solution by gradually evaporating the solvent and absorbing at least a part of the evaporated solvent in the absorbent, thereby causing crystallization of said substance to take place.

2. The method of claim 1 in which the solution of the substance to be crystallized is located at an intermediate position along the length of the capillary tube, in which the gaseous layer is located on one side of the solution, in which the column of layers includes a second absorbent and a second gaseous layer separating the solution and the second absorbent from each other, and in which, in the evaporating step, another part of the evaporated solvent is absorbed in the second absorbent.

3. The method of claim 1 in which the absorbent has a first rate of absorption, in which the solution of the substance to be crystallized is located at an intermediate position along the length of the capillary tube, in which the gaseous layer is located on one side of the solution, in which the column of layers includes a second absorbent having a rate of absorption different from said first rate, and a second gaseous layer separating the solution and the second absorbent from each other, and in which, in the evaporating step, another part of the evaporated solvent is absorbed in the second absorbent.

4. The method of claim 1 in which the absorbent has a first rate of absorption, in which the solution of the substance to be crystallized is located at an intermediate position along the length of the capillary tube, in which the gaseous layer is located on one side of the solution, in which the column of layers includes a second absorbent having a rate of absorption less than said first rate, and a second gaseous layer separating the solution and the second absorbent from each other, in which, in the evaporating step, another part of the evaporated solvent is absorbed in the second absorbent, and in which the amount of the absorbent having the first rate is limited to an amount such that absorption of solvent takes place initially at a rapid rate primarily into the absorbent having the first rate of absorption, and thereafter takes place at a slower rate primarily into the second absorbent.

5. The method of claim 1 in which the solution of the substance to be crystallized is located at an intermediate position along the length of the capillary tube, in which the absorbent is a first absorbent and the gaseous layer is a first gaseous layer located on one side of the solution, in which the column of layers includes a second absorbent and a second gaseous layer separating the solution and the second absorbent from each other, in which the length of the first gaseous layer is less than the length of the second gaseous layer, in which, in the evaporating step, another part of the evaporated solvent is absorbed in the second absorbent, and in which the amount of the first absorbent is such that absorption of solvent takes place initially at a rapid rate primarily into the first absorbent and thereafter takes place at a slower rate primarily into the second absorbent.

6. The method of claim 1 in which the solution of the substance to be crystallized is located at an intermediate position along the length of the capillary tube, in which the absorbent is a first absorbent and the gaseous layer is a first gaseous layer located on one side of the solution, in which the column of layers includes a second absorbent and a second gaseous layer separating the solution and the second absorbent from each other, in which the length of the first gaseous layer is less than the length of the second gaseous layer, in which the rate of absorption of the first absorbent is greater than the rate of absorption of the second absorbent, in which, in the evaporating step, another part of the evaporated solvent is absorbed in the second absorbent, and in which the amount of the first absorbent is such that absorption of solvent takes place initially at a rapid rate primarily into the first absorbent and thereafter takes place at a slower rate primarily into the second absorbent.

7. The method of claim 1 in which, in the step of establishing a column of layers within the capillary tube, the solution and absorbent are separated by the gaseous layer, a layer of liquid capable of being absorbed by the absorbent, and another gaseous layer, the layer of liquid being located between the gaseous layers, and in which the layer of liquid is first absorbed in the absorbent and thereafter at least part of the evaporated solvent is absorbed in the absorbent, whereby the crystallization of the substance to be crystallized is delayed.

8. The method of claim 1 in which said absorbent is a first absorbent, said gaseous layer is a first gaseous layer located on one side of the solution and in contact with the solution, in which, on said one side of the solution, the column of layers includes a second gaseous layer in contact with the first absorbent and a first layer of liquid, capable of being absorbed by the first absorbent, located between the first and second gaseous layers, and in which the column of layers comprises a second absorbent, a third gaseous layer in contact with the solution on the side thereof opposite to said one side, a fourth gaseous layer in contact with the second absorbent, and a second layer of liquid, capable of being absorbed by the second absorbent, located between the third and fourth gaseous layers, in which the first layer of liquid is absorbed in the first absorbent before at least a part of the solution is absorbed in the first absorbent, in which a part of the solution is absorbed in the second absorbent, and in which the second layer of liquid is absorbed in the second absorbent before a part of the solution is absorbed in the second absorbent, whereby the crystallization of the substance to be crystallized is delayed.

9. The method of claim 1 in which, after absorbing a part of the evaporated solvent in the absorbent, at least a part of the absorbent is removed from the capillary tube.

10. The method of claim 1 in which, after absorbing a part of the evaporated solvent in the absorbent, at least a part of the absorbent is removed from the capillary tube and replaced by a different absorbent.

11. The method of claim 1 in which, after absorbing a part of the evaporated solvent in the absorbent, at least a part of the absorbent is diluted.

12. The method of claim 1 in which, in the step of establishing a column of layers within a capillary tube, the capillary tube is sealed at opposing ends.

13. Apparatus for growing crystals comprising a capillary tube, a column of layers within the capillary tube, the column comprising a solution of a substance to be crystallized in a solvent, an absorbent, and a gaseous layer separating the solution and the absorbent from each other, in which the absorbent is a first absorbent and the gaseous layer is a first gaseous layer, in which the first gaseous layer is in contact with the solution on one side thereof, and having a second absorbent on the opposite side of the solution and a second gaseous layer in contact with the solution and located between the solution and the second absorbent.

14. The apparatus of claim 13, in which the second absorbent has a rate of absorption different from the rate of absorption of the first absorbent layer.

15. The apparatus of claim 13, in which the length of the first gaseous layer is less than the length of the second gaseous layer.

16. Apparatus for growing crystals comprising a capillary tube, a column of layers within the capillary tube, the column comprising a solution of a substance to be crystallized in a solvent, an absorbent, and a gaseous layer separating the solution and the absorbent from each other, in which the gaseous layer is a first gaseous layer in contact with the solution, and including a second gaseous layer in contact with the absorbent and a layer of liquid capable of being absorbed by the absorbent, the layer of liquid being located between the first and second gaseous layers.

17. The apparatus of claim 16, in which the column of layers comprises a second absorbent on the side of the solution opposite to said one side, a third gaseous layer in contact with the solution on the side thereof opposite to said one side, a fourth gaseous layer in contact with the second absorbent, and a second layer of liquid, capable of being absorbed by the absorbent, located between the third and fourth gaseous layers.