Silicon carbide single crystals with low boron content
View Patent ↗In a crystal growth method, an enclosed growth crucible is provided inside of a growth chamber. The growth crucible has polycrystalline source material and a seed crystal disposed in spaced relation therein. The interior of the growth crucible is heated whereupon a temperature gradient forms between the source material and the seed crystal. The temperature gradient is sufficient to cause the source material to sublimate and be transported to the seed crystal where it precipitates on the seed crystal. A gas mixture is caused to flow into the growth crucible and between the polycrystalline source material and an interior surface of the growth crucible. The gas mixture reacts with an unwanted element in the body of the growth crucible to form a gaseous byproduct which then flows through the body of the growth crucible to the exterior of the growth crucible.
1. A crystal growth method comprising:
(a) providing an enclosed growth crucible inside of a growth chamber with a thermal insulation disposed therebetween, the growth crucible having polycrystalline source material and a seed crystal disposed in spaced relation therein;
(b) heating the interior of the growth crucible such that a temperature gradient forms between the source material and the seed crystal, the source material is heated to a sublimation temperature and the temperature gradient is sufficient to cause sublimated source material to be transported to the seed crystal where the sublimated source material precipitates on the seed crystal; and
(c) causing a gas mixture to flow directly into the growth crucible and into a gap between the polycrystalline source material in the growth crucible and an interior surface of the growth crucible, whereupon the gas mixture reacts with an unwanted element in the body of the growth crucible to form a gaseous byproduct which, under the influence of the gas mixture flowing directly into the growth crucible, flows through a body of the growth crucible to the exterior of the growth crucible, which is formed of a material that is permeable to the gas mixture and the gaseous byproduct, under the influence of the flow of the gas mixture into the growth crucible, wherein the unwanted element is boron and the gas mixture comprises the combination of (a) halosilane gas and (b) an inert gas.
2. The method of claim 1 , wherein the inert gas is either argon or helium.
3. The method of claim 1 , wherein the halosilane gas is tetrahalosilane in a concentration in the gas mixture between either 0.1% and 10% by volume, or between 1% and 5% by volume.
4. The method of claim 1 , wherein the gas mixture further comprises hydrogen.
5. The method of claim 4 , wherein the concentration of hydrogen in the gas mixture is between 0.1% and 3% by volume.
6. The method of claim 1 , wherein:
the polycrystalline source material is disposed in a source crucible which is disposed inside the growth crucible; and
the gap is defined between an exterior surface of the source crucible and an interior surface of the growth crucible.
7. The method of claim 6 , wherein the gap includes:
a first gap between an exterior of a base of the source crucible disposed in spaced relation to an interior of a floor of the growth crucible; and
a second gap between an exterior of a wall of the source crucible disposed in spaced relation to an interior of a wall of the growth crucible, wherein the gas mixture flows in the first and second gaps.
8. The method of claim 1 , wherein the flow of the gas mixture is between 20 standard cubic centimeters per minute (sccm) and 200 sccm.
9. The method of claim 1 , wherein the wall(s) of the growth crucible have a thickness that is between either 4 mm and 20 mm, or between 8 mm and 16 mm.
10. The method of claim 1 , wherein:
the growth crucible is made from graphite;
the growth chamber is made from fused silica; and
the thermal insulation is made from a porous graphite.
11. The method of claim 1 , wherein the source material and the seed crystal are both made from SiC.
12. A crystal growth method comprising:
(a) providing a seed crystal and a source material in spaced relation inside of a growth crucible, wherein a body of the growth crucible-is made from a material that is at least in-part gas permeable and which includes an element that is not wanted in a crystal grown in the growth crucible;
(b) heating the growth crucible whereupon the source material sublimates and is transported via a temperature gradient in the growth crucible to the seed crystal where the sublimated source material precipitates; and
(c) concurrent with step (b), causing a gas mixture to flow directly into the interior of the growth crucible in a manner whereupon the unwanted element in the body of the growth crucible reacts with the gas mixture and is transported, under the influence of the gas mixture flowing directly into the growth crucible, to the exterior of the growth crucible via the at-least gas permeable part of the body of the growth crucible.
13. The method of claim 12 , wherein the gas mixture is caused to flow through the growth crucible at a rate between 20 sccm and 200 sccm.
14. The method of claim 12 , wherein the source material is disposed in a source crucible that is positioned inside the growth crucible.
15. The method of claim 14 , wherein an exterior wall of the source crucible is spaced from an interior wall of the growth crucible defining a gap between the source crucible and the growth crucible where the gas mixture flows.
16. The method of claim 15 , wherein the gap is between 4 mm and 7 mm.
17. The method of claim 12 , wherein at least one of:
the unwanted element is boron; and
the gas mixture is the combination of (a) halosilane gas and (b) an inert gas.
18. The method of claim 12 , wherein the growth crucible is comprised of graphite.
19. The method of claim 12 , wherein the source material and the seed crystal comprise SiC.
20. A crystal growth method comprising:
introducing a polycrystalline source material and a seed crystal into a physical vapor transport (PVT) growth system;
PVT growing sublimated source material on the seed crystal in the PVT growth system; and
promoting PVT growth of the sublimated source material on the seed crystal by introducing halosilane gas into the PVT growth system during said PVT growth.
21. The method of claim 20 , wherein the source material and the seed crystal are both made from SiC.
22. A crystal growth method comprising:
introducing a polycrystalline source material and a seed crystal into a PVT growth system; and
in the PVT growth system, PVT growing a single crystal on the seed crystal via precipitation of sublimated source material on the seed crystal in the presence of a flow of halosilane gas that reacts with and removes an unwanted element from the PVT growth system during said PVT growth.
23. The method of claim 22 , wherein the unwanted element is boron.
24. The method of claim 22 , wherein the single crystal is PVT grown in the presence of a flow of a gas mixture that includes the halosilane gas in a concentration between either 0.1% and 10% by volume, or between 1% and 5% by volume of the gas mixture.