Hydrothermal growth of hexagonal beryllium borate crystals for use in laser non-linear optical and birefringent applications and devices
Single, acentric, hexagonal, beryllium borate crystals having the formula Sr 2 Be 2 B 2 O 7 and of a size sufficient for use in a variety of laser and non-optical applications are formed by a hydrothermal method. Alternate structures are formed by partially substituting the strontium ion with at least one other divalent metal ion.
1. A method for making hexagonal beryllium borate crystals having the formula Sr 2 Be 2 B 2 O 7 (SBBO), comprising the steps of:
providing microcrystalline Sr 2 Be 2 B 2 O 7 powder; and
recrystallizing the microcrystalline Sr 2 Be 2 B 2 O 7 in an aqueous solution at a temperature of from about 350° C. to about 600° C. and at a pressure of from about 4 kpsi to about 30 kpsi. the aqueous solution comprising mineralizer ions at a concentration of from about 1×10 −6 to about 5 molarity.
2. The method set forth in claim 1 wherein the step of providing microcrystalline Sr 2 Be 2 B 2 O 7 powder comprises reacting a Sr 2 + salt, BeG, and a borate selected from H 3 BO 3 and B 2 O 3 in an air atmosphere at a temperature of at least about 850° C. for at least about 8 hours.
3. The method set forth in claim 1 wherein the mineralizer ions are selected from the group consisting of NaCI, NaOH, and KOH.
4. The method set forth in claim 3 wherein the step of recrystallizing the microcrystalline Sr 2 Be 2 B 2 O 7 occurs in an aqueous solution containing mineralizer ions comprising NaOH and wherein the NaOH is present at a concentration of from about 0.25 to about 1 molarity.
5. The method set forth in claim 1 wherein the step of recrystallizing the microcrystalline Sr 2 Be 2 B 2 O 7 occurs in an aqueous solution at a temperature of from about 450° C. to about 550° C.
6. The method set forth in claim 1 wherein the step of recrystallizing the microcrystalline Sr 2 Be 2 B 2 O 7 occurs in an aqueous solution at a pressure of from about 12 kpsi to about 18 kpsi.
7. A method for making hexagonal beryllium borate crystals having the formula Sr 2 Be 2 B 2 O 7 (SBBO), comprising the steps of:
reacting a St 2 + salt, BeO, and a borate selected from B 2 O 3 and H 3 BO 3 in an aqueous solution at a temperature of from about 350° C. to about 600° C. and at a pressure of from about 8 kpsi to about 40 kpsi, the aqueous solution further containing mineralizer ions at a concentration of from about 1×10 −6 to about 5 molarity.
8. The method set forth in claim 7 wherein the mineralizer ions are selected from the group consisting of hydroxide, carbonate, bicarbonate, chloride, and bromide.
9. The method set forth in claim 8 wherein the mineralizer ions comprise hydroxide ions and wherein the hydroxide ions are present in the aqueous solution at a concentration of from about 0.25 to about 1 molarity.
10. The method set forth in claim 7 wherein the temperature ranges from about 475° C. to about 550° C.
11. The method set forth in claim 7 wherein the pressure ranges from about 12 kpsi to about 18 kpsi.
12. A method for making hexagonal beryllium borate crystals having the formula Sr 2 Be 2 B 2 O 7 (SBBO), comprising the steps of:
providing a pressure vessel having a growth region and a nutrient region;
providing a seed crystal having the formula Sr 2 Be 2 B 2 O 7 ;
positioning the seed crystal in the growth region of the pressure vessel;
providing a medium comprising a nutrient and a mineralizer in the nutrient region, the nutrient comprising powdered or microcrystalline Sr 2 Be 2 B 2 O 7 , the mineralizer comprising an anion selected from the group consisting of hydroxide ions, carbonate ions, bicarbonate ions, chloride ions, and bromide ions; and
heating and pressurizing the vessel such that a growth temperature is produced in the growth region, a nutrient temperature is produced in the nutrient region, and a temperature gradient is produced between the growth region and the nutrient region, whereby growth of the crystal is initiated, the growth temperature ranging from about 350° C. to about 450° C. , the nutrient temperature ranging from about 450° C. to about 600° C. , the nutrient temperature being higher than the growth temperature and the pressure ranging from about 8 kpsi to about 40 kpsi.
13. The method set forth in claim 12 wherein the mineralizer comprises hydroxide ions and wherein the hydroxide ions are present in the medium at a concentration of from about 1×10 −6 to about 2 molarity.
14. The method set forth in claim 12 wherein the growth temperature ranges from about 400° C. to about 450° C.
15. The method set forth in claim 12 wherein the nutrient temperature ranges from about 470° C. to about 520° C.
16. The method set forth in claim 12 wherein the pressure ranges from about 12 kpsi to about 18 kpsi.