Claims
- 1. A method, comprising:
preparing a growth melt of a solid crystal to be formed, inserting a seed crystal into a liquid comprising the growth melt, forming the solid crystal from the liquid; and temperature annealing the solid crystal in a predetermined high temperature crucible to produce a high resistivity solid-state radiation detector material.
- 2. The method of claim 1, wherein the step of forming comprises forming from a process selected from the group consisting of a Chzochralski, a Bridgman, and a Traveling Heat Method.
- 3. The method of claim 1, wherein the temperature annealing step further comprises heating to a temperature from about 700° C. to about 1050° C.
- 4. The method of claim 1, wherein the solid crystal is a single crystal.
- 5. The method of claim 1, wherein the solid crystal is a III-V compound.
- 6. The method of claim 1, wherein the detector material includes an energy band-gap greater than about 1.40 eV, an electron and a hole mobility greater than about 100 cm2/Vs, a free carrier recombination time (τ) greater than about 10−6 s, the resistivity greater than about 107 Ω-cm, and at least one of the elements has an atomic number (Z) greater than about 40.
- 7. The method of claim 1, wherein the crucible further comprises an outer graphite crucible having a first open end, a first lid, and a first bottom adapted to receive an inner alumina crucible, the inner crucible having a second open end, a second lid, and a second bottom adapted to receive the solid crystal and a first and second two-phase mixture, the second lid adapted to enclose the second open end of the inner alumina crucible, wherein the inner alumina crucible is removably inserted into the first bottom portion, a sealing means positioned therebetween the open end of the outer graphite crucible and the first lid; and a means of pressure sealing the first lid and the sealing means to the first bottom of the outer graphite crucible.
- 8. The method of claim 1, wherein the solid crystal is capable of being adapted as an ambient gamma ray detector.
- 9. The method of claim 1, wherein the solid crystal is capable of being adapted as an ambient X-ray detector.
- 10. The method of claim 1, wherein the solid crystal is capable of being adapted as an ambient AlSb gamma ray or X-ray camera.
- 11. The method of claim 1, wherein the temperature annealing step further comprises: combining a heated first mixture of a two-phase material comprising a first solid III-V compound and a first liquid III-V compound, the first mixture having a majority of III material, and a heated second mixture of a two phase material comprising a second solid III-V compound and a second liquid III-V compound, the second mixture having a majority of V material, placing the solid crystal in the presence of the first and said second two phase mixtures; and annealing the solid crystal and the first and second mixtures under a constant temperature and a constant volume within the crucible, to produce a predetermined stoichiometric crystal material.
- 12. The method of claim 1, wherein the temperature annealing step further comprises: combining a heated first mixture of a two-phase material comprising a first solid AlSb and a first liquid Al—Sb, the first mixture having a majority of Sb atoms, and a heated second mixture of a two phase material comprising a second solid AlSb and a second liquid Al—Sb, the second mixture having a majority of Al atoms, placing the solid crystal in the presence of the first and said second two phase mixtures; and annealing the solid crystal and the first and second mixtures under a constant temperature and a constant volume within the crucible to produce a predetermined stoichiometric crystal material.
- 13. The method of claim 1, wherein the preparing growth melt step further comprises: weighing out a substantially pure Al material and a substantially pure Sb material in a predetermined proportion to form an AlSb compound, acid etching the Al material and an Sb ingot formed from the Sb material to substantially remove an oxide slag, pre-firing a preparing crucible at about 1200° C. to remove a moisture content and to ensure a complete outgassing of the preparing crucible, placing the Al material in the preparing crucible, placing the Sb ingot in a Tantalum cage having one or more wires adapted to hold the Sb ingot, the cage being removably attached to a stainless steel rod mounted through a port on a chamber lid, generating a vacuum inside a crystal grower, heating the preparing crucible to about 1000° C., introducing an Argon gas into the grower when a pressure within an enclosing chamber is at about one atmosphere, raising a temperature of the preparing crucible above a melting temperature of AlSb, moving the stainless steel rod with the Sb ingot over a heat zone; and lowering the Sb ingot into the preparing crucible until it melts, wherein a resultant melt surface is substantially slag free.
- 14. The method of claim 1, wherein the preparing growth melt step further comprises: placing a proportional amount of Al and a proportional amount of Sb into a preparing crucible without an acid etching step, creating a vacuum within an enclosing chamber, introducing an Argon gas at a pressure of one atmosphere, heating the Al and the Sb to a liquid state to produce an AlSb compound, inserting one or more alumina-mixing rods removably attached to a stainless steel rod that is mounted through a port on a chamber lid while the preparing crucible is rotating, mixing with the one or more alumina-mixing rods for a predetermined mixing time range, lowering the temperature to about a melting temperature of a solid AlSb for a predetermined time period to stabilize the AlSb, further lowering the temperature such that a dendritic crystal growth occurs from the one or more alumina-mixing rods, allowing the dendritic growth to continue until the growth substantially approaches a wall of the preparing crucible; and removing the one or more alumina-mixing rods having a solid lid of dendritic AlSb from a melt to produce the melt substantially free of a slag.
- 15. A method of producing an ambient solid state gamma ray or X-ray detector, comprising:
preparing a growth melt of a solid crystal to be formed including weighing out a substantially pure Al material and a substantially pure Sb material in a predetermined proportion to form an AlSb compound, acid etching the Al material and an Sb ingot formed from the Sb material to substantially remove an oxide slag, pre-firing a preparing crucible at about 1200° C. to remove a moisture content and to ensure a complete outgassing of the preparing crucible, placing the Al material in the preparing crucible, placing the Sb ingot in a Tantalum cage having one or more wires adapted to hold the Sb ingot, the cage being removably attached to a stainless steel rod mounted through a port on a chamber lid, generating a vacuum inside a crystal grower, heating the preparing crucible to about 1000° C., introducing an Argon gas into the grower at a pressure within an enclosing chamber of about one atmosphere, raising a temperature of the preparing crucible above a melting temperature of AlSb, moving the stainless steel rod with the Sb ingot over a heat zone; and lowering the Sb ingot into the preparing crucible until it melts, wherein a resultant melt surface is substantially slag free, rotating the preparing crucible, inserting a seed crystal into a liquid comprising the growth melt, forming the solid crystal from the liquid; and temperature annealing subsequent to forming the solid crystal in an annealing crucible, wherein the temperature annealing step further comprises: combining a heated first mixture of a two-phase material comprising a first solid AlSb and a first liquid Al—Sb, the first mixture having a majority of Sb atoms, and a heated second mixture of a two phase material comprising a second solid AlSb and a second liquid Al—Sb, the second mixture having a majority of Al atoms, placing the solid crystal in the presence of the first and the second two phase mixtures; and annealing the solid crystal and the first and second mixtures under a constant temperature and a constant volume within the annealing crucible to produce a stoichiometric AlSb crystal material that is capable of detecting gamma radiation, the AlSb crystal having an energy band-gap greater than about 1.40 eV, an electron and a hole mobility greater than about 100 cm2/Vs, a free carrier recombination time (τ) greater than about 10−6 s, and a resistivity greater than about 107 Ω-cm.
- 16. A method of producing an ambient solid state gamma ray or X-ray detector, comprising:
preparing a growth melt of a solid crystal to be formed, wherein the preparing growth melt step further comprises: placing a proportional amount of Al and a proportional amount of Sb into a preparing crucible without an acid etching step, creating a vacuum within an enclosing chamber, introducing an Argon gas at a pressure of one atmosphere, heating at a predetermined temperature the Al and the Sb to a liquid state Al—Sb, inserting one or more alumina-mixing rods removably attached to a stainless steel rod that is mounted through a port on a chamber lid while the preparing crucible is rotating, mixing with the one or more alumina-mixing rods for a predetermined mixing time range, lowering the temperature to about the melting temperature of a solid AlSb for a predetermined time period to stabilize the liquid Al—Sb, further lowering the temperature such that a dendritic crystal growth occurs from the one or more alumina-mixing rods, allowing the dendritic growth to continue until the growth substantially approaches a wall of the preparing crucible; and removing the one or more alumina-mixing rods having a solid lid of dendritic AlSb from a melt to produce the melt substantially free of a slag, inserting a seed crystal into a liquid comprising the growth melt, forming the solid crystal from the liquid; and temperature annealing subsequent to forming the solid crystal in an annealing crucible, wherein the temperature annealing step further comprises: combining a heated first mixture of a two-phase material comprising a first solid AlSb and a first liquid Al—Sb, the first mixture having a majority of Sb atoms, and a heated second mixture of a two phase material comprising a second solid AlSb and a second liquid AlSb, the second mixture having a majority of Al atoms, placing the solid crystal in the presence of the first and the second two phase mixtures; and annealing the solid crystal and the first and second mixtures under a constant temperature and a constant volume within the annealing crucible to produce a stoichiometric AlSb crystal material that is capable of detecting gamma radiation, the AlSb crystal having an energy band-gap greater than about 1.40 eV, an electron and a hole mobility greater than about 100 cm2/Vs, a free carrier recombination time (τ) greater than about 10−6 s, and a resistivity greater than about 107 Ω-cm.
- 17. A material for detecting gamma rays or x-rays comprising: an energy bandgap greater than about 1.40 eV, an electron and a hole mobility greater than about 100 cm2/Vs, a free carrier recombination time (τ) greater than about 10−6 s, a resistivity greater than about 107 Ω-cm; and at least one of the elements has an atomic number (Z) greater than about 40.
- 18. The material of claim 17, wherein the material is a III-V compound.
- 19. The method of claim 15, wherein the preparing crucible is a material selected from alumina and zirconia.
- 20. The method of claim 16, wherein the preparing crucible is a material selected from alumina and zirconia.
- 21. A high temperature annealing crucible to control solid state crystal stoichiometry, comprising:
an outer crucible having a first lid and a bottom with an open end, the bottom adapted to receive an inner crucible, the inner crucible adapted to receive a solid crystal and a first and second two-phase mixture, the inner crucible having a second lid to enclose the inner crucible, wherein the inner crucible is removably inserted into the bottom of the outer crucible, a sealing means positioned therebetween the first open end and the first lid of the outer crucible; and a means of pressure sealing the first lid and the sealing means to the bottom portion of the outer crucible.
- 22. The annealing crucible of claim 21, wherein the outer crucible and the sealing means is E+50/IM35 graphite material.
- 23. The annealing crucible of claim 21, wherein the inner crucible is a material selected from alumina and zirconia.
- 24. The annealing crucible of claim 21, wherein the sealing means is a graphite material with a thickness between about 0.010″ and about 0.050″.
- 25. The annealing crucible of claim 21, wherein the inner crucible is further adapted to hold a heated first mixture of a two-phase material comprising a first solid AlSb and a first liquid Al—Sb, the first mixture having a majority of Sb atoms, and a heated second mixture of a two phase material comprising a second solid AlSb and a second liquid Al—Sb, the second mixture having a majority of Al atoms, and further adapted to hold a solid crystal to be annealed.
- 26. The annealing crucible of claim 21, wherein the means of pressure sealing the first lid and the sealing means to the open end of the first bottom further comprises: a plurality of high-temperature functioning bolts fixedly attached to the first open end of the outer crucible, a plurality of washers; and a plurality of nuts, wherein the first lid having a plurality of through holes is adapted to receive the bolts, the bolts having a distal end capable of receiving the washers and threaded to receive the nuts, wherein an enclosing steel chamber capable of holding a vacuum and adapted to receive the annealing crucible includes a pressure sealing lid adapted to allow access to the plurality of nuts such that the nuts are capable of being torqued to pressure seal the first lid and the sealing means to the first open end of the outer crucible while under a vacuum in the enclosing chamber.
- 27. The annealing crucible of claim 21, wherein the nuts and the bolts are high-temperature alloy TZM materials having a coefficient of thermal expansion of about 5.3×10−6/K°.
- 28. The annealing crucible of claim 21, wherein the means of pressure sealing the first lid and the sealing means to the open end of the first bottom further comprises the first lid having an inner diameter thread capable of receiving an outer diameter thread of the open end of the bottom of the outer crucible; and an annular projection interposed between an inner diameter of the open end of the bottom of the outer crucible and the threaded outer diameter of the open end of the bottom of the outer crucible, wherein an enclosing steel chamber capable of holding a vacuum and adapted to removably receive the annealing crucible includes a pressure sealing lid adapted to allow access to a rotation means removably attached to the first lid to apply torque to the first lid such that the first lid is threaded onto the bottom to pressure seal the first lid and the sealing means to the annular projection while under a vacuum in the enclosing chamber.
- 29. The annealing crucible of claim 28, wherein the annular projection has a radius of curvature between about 0.0625 and about 2.0 inches.
- 30. The annealing crucible of claim 28, wherein the inner diameter thread of the first lid and the outer diameter thread of the open end of the bottom is between about a 4 pitch and about a 32 pitch thread.
- 31. A detector, comprising:
a high resistivity AlSb crystal having a bottom surface and a top surface, intended for operation at an operationally created e-field by a detector voltage applied thereto, the crystal generating a charge as a result of interacting electromagnetic radiation, a first ohmic contact operationally connected to the top surface of the crystal; and a second ohmic contact operationally connected to the bottom surface of the crystal, wherein the e-field produces a sufficient charge collection to produce a representative signal in an operationally connected circuitry that indicates an energy spectrum of the electromagnetic radiation.
- 32. The detector of claim 31, wherein the detector is capable of being operated at a room temperature greater than −196° C. to about 45° C.
- 33. The detector of claim 31, wherein the detector is capable of being operated at a room temperature between about 20° C. and about 25° C.
- 34. The detector of claim 31, wherein the crystal further comprises a III-V compound.
- 35. The detector of claim 31, wherein the first and the second ohmic contact is a metal selected from Au, Ag, and Al.
- 36. The detector of claim 31, wherein the first and the second ohmic contact is an alloy.
- 37. The detector of claim 31, wherein the first ohmic contact further comprises an interposed doped semiconductor operationally connected to the top surface of said crystal and the second ohmic contacts further comprises an interposed oppositely doped semiconductor operationally connected to the bottom surface of said crystal.
- 38. The detector of claim 31, wherein the electromagnetic radiation is a high-energy ray selected from Gamma rays or X-rays.
Government Interests
[0001] The United States Government has rights in this invention pursuant to Contract No. W-7405-ENG-48 between the United States Department of Energy and the University of California for the operation of Lawrence Livermore National Laboratory.