Seeded growth process for preparing aluminum nitride single crystals
View Patent ↗A method of growing bulk single crystals of an AlN on a single crystal seed is provided, wherein an AlN source material is placed within a crucible chamber in spacial relationship to a seed fused to the cap of the crucible. The crucible is heated in a manner sufficient to establish a temperature gradient between the source material and the seed with the seed at a higher temperature than the source material such that the outer layer of the seed is evaporated, thereby cleaning the seed of contaminants and removing any damage to the seed incurred during seed preparation. Thereafter, the temperature gradient between the source material and the seed is inverted so that the source material is sublimed and deposited on the seed, thereby growing a bulk single crystal of AlN.
1. A method of securing a single crystal seed to a crucible for use in a crystal growth process, the method comprising:
providing a crucible comprising a crucible body defining an open-ended chamber and a removable cap adapted for closing the open end of the chamber;
placing an AlN source material within the crucible chamber;
subliming the AlN source material within the crucible for a time and at a temperature sufficient to deposit a condensed polycrystalline mass of the AlN source material on an internal surface of the crucible chamber;
placing a single crystal seed on a surface of the removable cap facing the interior of the crucible chamber following said subliming step;
closing the open end of the crucible chamber with the removable cap carrying the seed; and
heating the crucible chamber containing the condensed polycrystalline mass of AlN source material to a temperature sufficient to fuse the seed to the crucible cap.
2. The method of claim 1 , wherein the single crystal seed is an AlN seed.
3. The method of claim 1 , wherein said subliming step comprises heating the crucible in a manner sufficient to establish an axial temperature gradient between the AlN source material and the internal surface upon which the condensed polycrystalline mass is to be deposited, the AlN source material being maintained at a higher temperature than the deposition surface.
4. The method of claim 3 , wherein said subliming step comprises maintaining a temperature gradient of about 1° C./cm to about 100° C./cm between the AlN source material and the deposition surface.
5. The method of claim 4 , wherein said subliming step comprises maintaining a temperature gradient of at least about 30° C./cm between the AlN source material and the deposition surface.
6. The method of claim 1 , wherein said heating step comprises heating the crucible chamber approximately isothermally.
7. The method of claim 1 , wherein the AlN source material is selected from the group consisting of AlN, AlN alloys, and AlN or AlN alloys including one or more dopants.
8. A method of securing a single crystal seed to a crucible for use in a crystal growth process, the method comprising:
providing a crucible comprising a crucible body defining an open-ended chamber and a removable cap adapted for closing the open end of the chamber;
placing an AlN source material within the crucible chamber;
subliming the AlN source material within the crucible, said subliming step comprising heating the crucible chamber in a manner sufficient to establish an axial temperature gradient between the AlN source material and an internal surface upon which a condensed polycrystalline mass of the AlN source material is to be deposited, the AlN source material being maintained at a higher temperature than the deposition surface, said heating step causing the deposition of a condensed polycrystalline mass of the AlN source material on the internal surface of the crucible chamber;
placing a single crystal AlN seed on a surface of the removable cap facing the interior of the crucible chamber following said subliming step;
closing the open end of the crucible chamber with the removable cap carrying the seed; and
heating the crucible chamber containing the condensed polycrystalline mass of AlN source material approximately isothermally to a temperature sufficient to fuse the seed to the crucible cap.
9. The method of claim 8 , wherein said subliming step comprises heating the crucible to a temperature of about 2000 to about 2300° C., the temperature gradient being about 1° C./cm to about 100° C./cm between the AlN source material and the deposition surface.
10. The method of claim 8 , wherein said step of heating the crucible chamber approximately isothermally comprises heating the crucible chamber to a temperature of about 1800 to about 2400° C.
11. A method of securing a single crystal seed to a crucible for use in a crystal growth process, the method comprising:
providing a crucible comprising a crucible body defining an open-ended chamber and a removable cap adapted for closing the open end of the chamber;
placing an AlN source material on the cap of the crucible with the crucible in an inverted position;
while maintaining the crucible in an inverted position, subliming the AlN source material within the crucible for a time and at a temperature sufficient to deposit a condensed polycrystalline mass of the AlN source material on an internal surface of the crucible chamber;
placing a single crystal seed on a surface of the removable cap facing the interior of the crucible chamber with the crucible in an inverted position, the polycrystalline mass of AlN source material being positioned above the seed; and
while maintaining the crucible in an inverted position, heating the crucible chamber containing the condensed polycrystalline mass of AlN source material to a temperature sufficient to fuse the seed to the crucible cap.