PATENT CLAIM ANALYSIS

Application Number: 16306902
Application Type: Utility
Filing Date: 2018-12
Publication Date: 2019-05
Patent Classification: ["359", "328000"]

Abstract:
A compound of cesium fluorooxoborate, a nonlinear optical crystal of cesium fluorooxoborate, and a method of preparation and use thereof. The compound has a chemical formula of CsB 4 O 6 F and a molecular weight of 291.15. It has a crystal structure, which is prepared by a solid-state synthesis method or a vacuum encapsulation method. The crystal has a chemical formula of CsB 4 O 6 F and a molecular weight of 291.15. It belongs to an orthorhombic crystal system, with a space group of Pna2 1 , crystal cell parameters of a=7.9241 Å, b=11.3996 Å, c=6.6638 Å, and α=β=γ=90°, and a unit cell volume of 601.95 Å 3 . A melt method, high temperature solution method, vacuum encapsulation method, hydrothermal method or room temperature solution method is used to grow the crystal of CsB 4 O 6 F.

Claim (Index 4):
A method for preparing the nonlinear optical crystal of cesium fluorooxoborate of  claim 3 , wherein the nonlinear optical crystal is grown by a melt method, a high temperature solution method, a vacuum encapsulation method, a hydrothermal method or a room temperature solution method; wherein\n the melt method for growing the nonlinear optical crystal of cesium fluorooxoborate comprises following steps: a) mixing a Cs-containing compound, a B-containing compound and an F-containing compound homogeneously at a molar ratio of 0.5-2:3-5:0.5-2 to obtain a third mixture; filling the third mixture into a platinum crucible; then placing the platinum crucible in a muffle furnace, and increasing a third temperature to 350-600\u00b0 C. for 3-96 hours, to obtain a polycrystal powder of the compound of CsB 4 O 6 F; wherein the Cs-containing compound is Cs 2 CO 3 , CsNO 3 , CsHCO 3 , CsF or CsBF 4 ; the F-containing compound is CsF or CsBF 4 ; and the B-containing compound is H 3 BO 3 , B 2 O 3  or CsBF 4 ; b) filling the polycrystal powder of the compound of CsB 4 O 6 F into a clean platinum crucible; placing the clean platinum crucible in a muffle furnace, and increasing a fourth temperature to 400-700\u00b0 C. at a rate of 20-40\u00b0 C./h for 7-15 hours, to obtain a melt; wherein the Cs-containing compound is Cs 2 CO 3 , CsNO 3 , CsHCO 3 , CsF or CsBF 4 ; the F-containing compound is CsF or CsBF 4 ; and the B-containing compound is H 3 BO 3 , B 2 O 3  or CsBF 4 ; c) decreasing a fifth temperature of the melt from step b) to 400-590\u00b0 C. at a rate of 0.1-5\u00b0 C./h, to 300-440\u00b0 C. at a rate of 0.2-2\u00b0 C./h, and further to 30\u00b0 C. at a rate of 3-15\u00b0 C./h, to obtain a seed crystal of CsB 4 O 6 F; and d) growing the seed crystal in the melt of the compound by a Czochralski method, comprising fixing the seed crystal obtained from step c) onto a seed crystal rod; lowering the seed crystal to 1 mm above a liquid surface from a top of a crystal growing furnace for the melt prepared in step b), and preheating the seed crystal for 5-60 minutes; then immersing the seed crystal in a liquid at 1-5 mm below the liquid surface; rotating the seed crystal at 2-30 rpm by a crystal growth controller and controlling a sixth temperature to saturate the melt; lifting the seed crystal at a rate of 1-3 mm/day while keeping the sixth temperature constant; upon completion of a crystal growth, pulling a crystal on the seed crystal rod, and decreasing the sixth temperature to 300-440\u00b0 C. at a rate of 0.2-2\u00b0 C./h, and further to 30\u00b0 C. at a rate of 3-15\u00b0 C./h, to obtain the nonlinear optical crystal of CsB 4 O 6 F; or growing the seed crystal in the melt of the compound by a Kyropoulos method, comprising fixing the seed crystal obtained from step c) onto a seed crystal rod; lowering the seed crystal to 1 mm above a liquid surface from a top of a crystal growing furnace for the melt prepared in step b), and preheating the seed crystal for 5-60 minutes; then immersing the seed crystal in a liquid at 1-5 mm below the liquid surface; decreasing a seventh temperature at a rate of 0.1-0.7\u00b0 C./h; 3-10 hours later, lifting the seed crystal by 1-2 mm, and further decreasing the seventh temperature at a rate of 0.1-0.7\u00b0 C./h; upon completion of a crystal growth, pulling a crystal on the seed crystal rod, and decreasing the seventh temperature to 300-440\u00b0 C. at a rate of 0.2-2\u00b0 C./h, and further to 30\u00b0 C. at a rate of 3-15\u00b0 C./h, to obtain the nonlinear optical crystal of CsB 4 O 6 F; or growing the crystal in the melt of the compound by a Bridgeman-Stockbarger method, comprising placing the seed crystal prepared in step c) at a bottom of a platinum crucible, then adding the polycrystal powder of the compound of CsB 4 O 6 F prepared in step a) to the platinum crucible; sealing the platinum crucible, and increasing a eighth temperature of the growing furnace to 500-700\u00b0 C. for 7-15 hours; adjusting a position of the platinum crucible such that a seeding temperature is 500-625\u00b0 C.; then lowering the platinum crucible at a rate of 1-10 mm/day while keeping a growth temperature constant; upon completion of a growth, decreasing the growth temperature to 300-440\u00b0 C. at a rate of 0.2-2\u00b0 C./h, and further to 30\u00b0 C. at a rate of 3-15\u00b0 C./h; and removing the platinum crucible, to obtain the nonlinear optical crystal of CsB 4 O 6 F; the high temperature solution method for growing the nonlinear optical crystal of cesium fluorooxoborate comprises following steps: a) mixing a Cs-containing compound, a B-containing compound and an F-containing compound homogeneously at a molar ratio of 0.5-2:3-5:0.5-2 to obtain a fourth mixture; filling the fourth mixture into a platinum crucible; then placing the platinum crucible in a muffle furnace, and increasing a ninth temperature to 350-600\u00b0 C. for 3-96 hours, to obtain a polycrystal powder of the compound of CsB 4 O 6 F; wherein the Cs-containing compound is Cs 2 CO 3 , CsNO 3 , CsHCO 3 , CsF or CsBF 4 ; the F-containing compound is CsF or CsBF 4 ; and the B-containing compound is H 3 BO 3 , B 2 O 3  or CsBF 4 ; b) mixing the polycrystal powder of the compound of CsB 4 O 6 F obtained from step a) homogeneously with a fluxing agent at a molar ratio of 1:0.1-0.5 to obtain a fifth mixture; then filling the fifth mixture into a clean platinum crucible, and increasing a tenth temperature to 400-700\u00b0 C. at a rate of 35-45\u00b0 C./h for 7-15 hours, to obtain a first mixed solution; wherein the Cs-containing compound is Cs 2 CO 3 , CsNO 3 , CsHCO 3 , CsF or CsBF 4 ; the F-containing compound is CsF or CsBF 4 ; the B-containing compound is H 3 BO 3 , B 2 O 3  or CsBF 4 ; and the fluxing agent is CsF, H 3 BO 3 , B 2 O 3 , PbO or PbF 2 ; c) preparation of a seed crystal: placing the first mixed solution prepared in step b) into a single crystal furnace, and then decreasing a eleventh temperature to 350-610\u00b0 C. at a rate of 0.1-5\u00b0 C./h, to 300-385\u00b0 C. at a rate of 0.2-0.6\u00b0 C./h, and further to 30\u00b0 C. at a rate of 3-10\u00b0 C./h, to obtain a seed crystal of CsB 4 O 6 F; and d) growth of a crystal: fixing the seed crystal of CsB 4 O 6 F onto a seed crystal rod; lowering the seed crystal to 1 mm above a liquid surface from a top of a crystal growing furnace for the first mixed solution prepared in step b), and preheating the seed crystal for 10-25 minutes; contacting the seed crystal with the liquid surface, and decreasing a twelfth temperature at a rate of 0.1-2\u00b0 C./h; upon completion of a crystal growth, pulling a crystal away from the surface of the first mixed solution, and then decreasing the twelfth temperature to 30\u00b0 C. at a rate of 3-10\u00b0 C./h, to obtain the nonlinear optical crystal of CsB 4 O 6 F; the vacuum encapsulation method for growing the nonlinear optical crystal of cesium fluorooxoborate comprises following steps: a) mixing a Cs-containing compound, a B-containing compound and an F-containing compound homogeneously at a molar ratio of 0.5-2:3-5:0.5-2 to a sixth mixture; filling the sixth mixture into a platinum crucible; then placing the platinum crucible in a muffle furnace, and increasing a thirteenth temperature to 350-600\u00b0 C. at a rate of 10-50\u00b0 C. for 3-96 hours, to obtain a polycrystal powder of the compound of CsB 4 O 6 F; wherein the Cs-containing compound is Cs 2 CO 3 , CsNO 3 , CsHCO 3 , CsF or CsBF 4 ; the F-containing compound is CsF or CsBF 4 ; and the B-containing compound is H 3 BO 3 , B 2 O 3  or CsBF 4 ; and b) mixing the polycrystal powder of the compound of CsB 4 O 6 F obtained from step a) homogeneously with a fluxing agent at a molar ratio of 1:0.1-1 to obtain a seventh mixture; then filling the seventh mixture into a quartz tube, and increasing a fourteenth temperature to 400-700\u00b0 C. at a rate of 10-50\u00b0 C./h for 3-96 hours; then decreasing the fourteenth temperature to 330-450\u00b0 C. at a rate of 0.5-1.5\u00b0 C./day, and further to 30\u00b0 C. at a rate of 2-5\u00b0 C./h; and cutting the quartz tube to obtain the nonlinear optical crystal of CsB 4 O 6 F; wherein the Cs-containing compound is Cs 2 CO 3 , CsNO 3 , CsHCO 3 , CsF or CsBF 4 ; the F-containing compound is CsF, CsBF4 or HF; the B-containing compound is H 3 BO 3 , B 2 O 3  or CsBF 4 ; and the fluxing agent is CsF, H 3 BO 3 , B 2 O 3 , PbO or PbF 2 ; the hydrothermal method for growing the nonlinear optical crystal of cesium fluorooxoborate comprises following steps: a) mixing a Cs-containing compound, a B-containing compound and an F-containing compound homogeneously at a molar ratio of 0.5-2:3-5:0.5-2 to obtain a eighth mixture; filling the eighth mixture into a platinum crucible; then placing the platinum crucible in a muffle furnace, and increasing a fifteenth temperature to 350-600\u00b0 C. for 3-96 hours, to obtain a polycrystal powder product of CsB 4 O 6 F; wherein the Cs-containing compound is Cs 2 CO 3 , CsNO 3 , CsHCO 3 , CsF or CH 3 COOCs; the F-containing compound is CsF or HF; and the B-containing compound is H 3 BO 3  or B 2 O 3 ; b) dissolving the polycrystal powder of the compound of CsB 4 O 6 F obtained from step a) in 5-30 mL of deionized water to obtain a incompletely dissolved mixture, and sonicating the incompletely dissolved mixture at a sixteenth temperature of 20-50\u00b0 C. for 5-30 minutes to allow for sufficient mixing and dissolution to obtain a second mixed solution; c) transferring the second mixed solution obtained from step b) into a lining of a clean, pollution-free high pressure reactor with a volume of 100 mL, and tightening and sealing the clean, pollution-free high pressure reactor; and d) placing the clean, pollution-free high pressure reactor in a thermostat, increasing a seventeenth temperature to 150-350\u00b0 C. at a rate of 5-50\u00b0 C./h for 3-15 days, and then decreasing the seventeenth temperature to room temperature at a rate of 5-30\u00b0 C./day, to obtain the nonlinear optical crystal of CsB 4 O 6 F; and the room temperature solution method for growing the nonlinear optical crystal of cesium fluorooxoborate comprises following steps: a) mixing a Cs-containing compound, a B-containing compound and an F-containing compound homogeneously at a molar ratio of 0.5-2:3-5:0.5-2 to obtain a ninth mixture; filling the ninth mixture into a platinum crucible; then placing the platinum crucible in a muffle furnace, and increasing a eighteenth temperature to 350-600\u00b0 C. for 3-96 hours, to obtain a polycrystal powder product of CsB 4 O 6 F; wherein the Cs-containing compound is Cs 2 CO 3 , CsNO 3 , CsHCO 3 , CsF or CH 3 COOCs; the F-containing compound is CsF or HF; and the B-containing compound is H 3 BO 3  or B 2 O 3 ; b) placing the polycrystal powder of the compound of CsB 4 O 6 F obtained from step a) in a clean glass container, 20-100 mL of deionized water is added to the clean glass container to obtain a solution, followed by ultrasonication for 5-60 minutes to allow for sufficient mixing and dissolution, and then adjusting a pH of the solution to 8-11 by addition of HF or CsOH; c) sealing the clean glass container containing the solution in step b) with weighing paper to have a seal, and placing the clean glass container in a static environment without shaking, pollution and air convection; controlling a evaporation rate at 0.2-2 mL/day by piercing the seal; and setting the clean glass container aside for 5-20 days at room temperature; d) obtaining a seed crystal upon completion of a growth when a size of crystal particles grown at a bottom of the clean glass container from the solution in step c) is no longer changed significantly; and e) filtering a remaining solution through qualitative filter paper to filter out grains and other impurities from the remaining solution to obtain a filtered solution; selecting seed crystal of better quality, fixing the seed crystal with a platinum wire and suspending the seed crystal in the filtered solution; controlling the evaporation rate at 0.2-2 mL/day by piercing the seal, and setting the seed crystal aside for growth for 5-20 days at room temperature, to obtain the nonlinear optical crystal of CsB 4 O 6 F.

Metadata:
- Claim Count in Document: 9.0
- Percentile: 98.0
- Lexical Diversity: 2.26087
- Patent Class: 359.0
- Transitional Phrase Type: open
- Component Type: 1
- Foreign Priority: True
- Related Applications: ['14426094', '11159143', '16070286', '16061670', '13383797']

Analysis Scores:
- 35 USC 101 Eligibility (BERT): 0.7896791158912635
- 35 USC 102 Novelty (BERT): 0.5185380251661826
- Combined Prediction Score: 0.7625650068187555
- Mean Citation Score: 279.447918
- Max Citation Score: 345.0713
- Similarity Product: 276.6371192508221

Labels:
- Claim Label 101: 1
- Claim Label 102: 1
- Claim Label 103: 1
- Claim Label 112: 1
- Combined Label: 1
- Label 101 Adjusted: 1

Dataset: test