Methods and apparatus for solid source refill
Various embodiments of the present technology may provide a first vessel to contain a slurry of a solid precursor powder and an inert liquid, a second vessel to receive the slurry, evaporate the inert liquid, and sublimate the solid precursor powder a first time to form a vapor, a third vessel to recondense the vapor back into a solid state and sublimate the solid precursor a second time to form a vapor, and a reaction chamber to receive the vapor from the third vessel.
1 . An apparatus for refill of a solid source precursor, comprising:
a first vessel configured to contain a liquid slurry, wherein the first vessel comprises a first vessel heating element and is configured to maintain the liquid slurry at a first temperature, wherein the slurry comprises a solid precursor powder and an inert liquid;
a first conduit fluidly connected to the first vessel, wherein the apparatus comprises at least one first conduit pump along a flow path of the first conduit, and wherein the first conduit is configured to flow the liquid slurry through the first conduit;
a second vessel fluidly connected to the first vessel via a first conduit, wherein the second vessel is connected to a sublimator configured to provide heat to the second vessel, and
wherein the second vessel is configured to:
receive the liquid slurry via the first conduit while the second vessel is at a second temperature, and
wherein the sublimator is configured to:
provide heat to the second vessel to a third temperature greater than the first temperature and the second temperature, wherein the liquid slurry thereby sublimates the solid precursor powder from the liquid slurry at the third temperature that is greater than the first temperature and the second temperature to form a vapor;
a second conduit fluidly connected to the second vessel, wherein the apparatus comprises at least one second conduit pump along a flow path of the second conduit, and wherein the second conduit is configured to flow the vapor;
a vacuum source, connected to the second vessel via a fourth conduit, configured to evaporate the inert fluid out of the second vessel;
a third vessel connected to the second vessel via a second conduit configured to flow the vapor from the second vessel to the third vessel, wherein the third vessel comprises a third vessel heating element and is configured to operate at a fourth temperature and a fifth temperature; and
a reactor connected to the third vessel via a third conduit.
2 . The apparatus according to claim 1 , wherein the first temperature is in a range of 20 to 25 degrees Celsius, and the first conduit comprises a first conduit heating element and is maintained at the first temperature.
3 . The apparatus according to claim 1 , wherein:
the second temperature is greater than the first temperature;
the fourth temperature is 15-20 degrees Celsius less than the fifth temperature; and
the third temperature is 15-20 degrees Celsius less than the fourth temperature.
4 . The apparatus according to claim 1 , wherein the second conduit comprises a second conduit heating element, wherein the third conduit comprises a third conduit heating element, and wherein the second and third conduits are heated to the third temperature.
5 . The apparatus according to claim 1 , wherein the first vessel contains a volume of the liquid slurry and wherein the first conduit comprises an inlet pipe extending into the volume of liquid slurry.
6 . The apparatus according to claim 1 , further comprising a second vessel heating element in direct contact with at least one wall of the second vessel, wherein the second vessel heating element heats the second vessel and a second volume of liquid slurry contained within the second vessel.
7 . The apparatus according to claim 1 , wherein the third vessel comprises a third vessel sublimator.
8 . The apparatus according to claim 1 , wherein the first vessel contains a first volume of liquid slurry and the second vessel contains a second volume of liquid slurry.
9 . The apparatus according to claim 1 , further comprising a cooling element in direct contact with the second vessel, wherein the cooling element operates to decrease the third temperature to the second temperature.
10 . The apparatus according to claim 1 , wherein the solid precursor powder comprises:
a transition metal element and a halide ligand, or
a transition metal element and an organic ligand.