IP Library Granted Patent US 11,591,710
Granted Patent B2
US 11,591,710 · App. 17/060,585 · Granted Feb 28, 2023

Crystallization of amorphous multicomponent ionic compounds

Inventors: Paul Gregory Evans (Madison, WI); Thomas Francis Kuech (Madison, WI); Susan Elizabeth Babcock (Madison, WI); Mohammed Humed Yusuf (Madison, WI); Yajin Chen (Madison, WI)
Assignee: Wisconsin Alumni Research Foundation
C30B1/023C30B29/22C30B29/32H01L21/02197H01L21/02266H01L21/02356H01L29/40111H01L29/6684
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Quick Facts
Patent No.
US 11,591,710
App. No.
17/060,585
Granted
Feb 28, 2023
Kind
B2
Abstract

A method for crystallizing an amorphous multicomponent ionic compound comprises applying an external stimulus to a layer of an amorphous multicomponent ionic compound, the layer in contact with an amorphous surface of a deposition substrate at a first interface and optionally, the layer in contact with a crystalline surface at a second interface, wherein the external stimulus induces an amorphous-to-crystalline phase transformation, thereby crystallizing the layer to provide a crystalline multicomponent ionic compound, wherein the external stimulus and the crystallization are carried out at a temperature below the melting temperature of the amorphous multicomponent ionic compound. If the layer is in contact with the crystalline surface at the second interface, the temperature is further selected to achieve crystallization from the crystalline surface via solid phase epitaxial (SPE) growth without nucleation.

Claims (24)

1. A method for crystallizing an amorphous multicomponent ionic compound, the method comprising:

(a) determining a largest distance to be crystallized via solid phase epitaxy (SPE) growth without nucleation in a layer of the amorphous multicomponent ionic compound,

wherein the layer contacts an amorphous surface of a deposition substrate at a first interface and contacts a crystalline surface of the deposition substrate at a second interface, and

wherein the largest distance is measured from the second interface along an SPE crystallization pathway through the layer to a surface of the layer that is furthest from the second interface;

(b) selecting a temperature for heating the layer from a calibration curve of maximum crystallization distance without nucleation L C versus temperature, such that the L C at the temperature is greater than or equal to the largest distance; and

(c) heating the layer at the temperature to convert the layer to a layer of a crystalline multicomponent ionic compound via SPE growth without nucleation.

2. The method of claim 1 , further comprising measuring L C as a function of temperature to provide the calibration curve.

3. The method of claim 2 , wherein L C =vt* , wherein v is a velocity for crystallization of the layer of the amorphous multicomponent ionic compound via SPE growth from the crystalline surface and t* is a nucleation time of the layer of the amorphous multicomponent ionic compound, and wherein measuring L C as a function of temperature comprises measuring v as a function of temperature and measuring t* as a function of temperature.

4. The method of claim 1 , wherein the temperature is no greater than 550° C.

5. The method of claim 1 , wherein the temperature is no greater than 450° C.

6. The method of claim 1 , further comprising depositing the layer of the amorphous multicomponent ionic compound on the deposition substrate.

7. The method of claim 6 , wherein depositing the layer of the amorphous multicomponent ionic compound is carried out at 300° C. or less.

8. The method of claim 6 , wherein depositing the layer of the amorphous multicomponent ionic compound is carried out at room temperature.

9. The method of claim 6 , wherein step (c) provides a single-crystalline multicomponent ionic compound.

10. The method of claim 1 , wherein the amorphous multicomponent ionic compound is an amorphous multicomponent oxide.

11. The method of claim 10 , wherein the amorphous multicomponent oxide is selected from the group consisting of perovskites, spinels, pyrochlores, and ferrites.

12. The method of claim 1 , wherein the amorphous surface is provided by a plastic, silica, or glass.

13. The method of claim 1 , wherein the deposition substrate is non-planar and three-dimensional such that the layer of the amorphous multicomponent ionic compound is characterized by a complementary three-dimensional morphology and step (c) provides the crystalline multicomponent ionic compound also characterized by the complementary three-dimensional morphology.

14. A method for crystallizing an amorphous multicomponent ionic compound, the method comprising:

(a) depositing a layer of an amorphous multicomponent ionic compound on a deposition substrate, wherein the layer contacts an amorphous surface of the deposition substrate at a first interface and contacts a crystalline surface of the deposition substrate at a second interface;

(b) selecting a temperature for heating the layer from a calibration curve of maximum crystallization distance without nucleation L C versus temperature; and

(c) heating the layer at the temperature to convert the layer to a layer of a crystalline multicomponent ionic compound via solid phase epitaxy (SPE) growth without nucleation.

15. The method of claim 14 , further comprising measuring L C as a function of temperature to provide the calibration curve.

16. The method of claim 15 , wherein L C =vt*, wherein v is a velocity for crystallization of the layer of the amorphous multicomponent ionic compound via SPE growth from the crystalline surface and t* is a nucleation time of the layer of the amorphous multicomponent ionic compound, and wherein measuring L C as a function of temperature comprises measuring v as a function of temperature and measuring t* as a function of temperature.

Assignments (3)
CONFIRMATORY LICENSE Recorded May 23, 2023
From: WISCONSIN ALUMNI RESEARCH FOUNDATION
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 063730/0180 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 13, 2023
From: EVANS, PAUL; BABCOCK, SUSAN; KUECH, THOMAS; CHEN, YAJIN; YUSUF, MOHAMMED
To: WISCONSIN ALUMNI RESEARCH FOUNDATION
Reel/Frame 063310/0814 →
CONFIRMATORY LICENSE Recorded Jan 15, 2021
From: UNIVERSITY OF WISCONSIN, MADISON
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 055013/0966 →
Continuity (2)
Continuation 15728595 · Oct 10, 2017
Related Publication 20210025074A1 · Jan 28, 2021