Compound yttrium lead rubidium borate and yttrium lead rubidium borate nonlinear optical crystal and preparation method and use thereof

Abstract

The present invention provides a compound yttrium lead rubidium borate and a yttrium lead rubidium borate nonlinear optical crystal and a preparation method and use thereof. The chemical formula of the compound is Rb7PbY2B 15 O 30 , molecular weight is 1625.45, it is prepared by solid phase synthesis or vacuum packaging method, the crystal chemical formula is Rb7PbY2B 15 O 30 , molecular weight is 1625.45, belongs to the trigonal system, and the space group is R 32, the unit cell parameters are a =13.4642(3)Å, b =13.4642(3)Å, c =15.2917(8)Å, α =90°, β =90°, c =120°, the unit cell volume is 2400.18 Å 3 , using melt method, high temperature melt method or vacuum packaging method to grow crystals, the Rb7PbY2B obtained by this method 15 O 30 Nonlinear optical crystal, the powder frequency-doubled effect of the crystal is about 1.3 times that of KH2PO4 (KDP), the ultraviolet cutoff edge is lower than 300 nm, and the physical and chemical properties are stable. It can be used as a short-wavelength ultraviolet nonlinear optical crystal in all-solid-state lasers.

Description

Technical Field

[0001] The present invention relates to a compound yttrium lead rubidium borate and a yttrium lead rubidium borate nonlinear optical crystal as well as a preparation method and application thereof. Background Art

[0002] Ultraviolet nonlinear optical crystals can utilize their frequency conversion properties to convert near-infrared and visible lasers into ultraviolet lasers, offering significant applications in fields such as medicine, communications, and scientific research. Currently available ultraviolet and even deep-ultraviolet nonlinear optical crystals include KBe2BO3F2 (KBBF), BaB2O4 (BBO), and LiB3O5 (LBO), all developed by Chinese scientists. However, these crystals suffer from limitations, such as the difficulty of growing large crystals, which limits their application. Therefore, the preparation and synthesis of novel ultraviolet nonlinear optical crystal materials with superior comprehensive performance is of great significance and practical value. Summary of the Invention

[0003] The present invention aims to provide a compound of yttrium lead rubidium borate, the chemical formula of which is Rb7PbY2B 15 O 30 , molecular weight is 1625.45, and it is prepared by solid phase synthesis or vacuum encapsulation method.

[0004] Another object of the present invention is to provide yttrium lead rubidium borate Rb7PbY2B 15 O 30 Nonlinear optical crystal, the chemical formula of the crystal is Rb7PbY2B 15 O 30 , molecular weight is 1625.45. It belongs to the trigonal crystal system, space group is R32, unit cell parameters are α=90°,β=90°,γ=120°,the unit cell volume is

[0005] Another object of the present invention is to provide a method for preparing yttrium lead rubidium borate nonlinear optical crystals, which adopts a melt method, a high-temperature melt method or a vacuum packaging method to grow the crystals.

[0006] Another object of the present invention is to provide yttrium lead rubidium borate Rb7PbY2B 15 O 30 Applications of nonlinear optical crystals.

[0007] The compound of the present invention, yttrium lead rubidium borate, has the chemical formula Rb7PbY2B 15 O 30 , molecular weight is 1625.45, and it is prepared by solid phase synthesis or vacuum packaging method.

[0008] The preparation method of the compound yttrium lead rubidium borate adopts a solid phase synthesis method or a vacuum packaging method, and the specific operation is carried out according to the following steps:

[0009] The solid phase synthesis method is used to prepare the compound yttrium lead rubidium borate:

[0010] The Rb-containing compound, the Pb-containing compound, the Y-containing compound and the B-containing compound are mixed uniformly in a molar ratio of Rb:Pb:Y:B=7-14:1-2:2-4:15-30, put into a platinum crucible, placed in a muffle furnace, heated to 700-750°C, and kept at this temperature for 48-120 hours to obtain the compound Rb7PbY2B 15 O 30 , the Rb-containing compound is RbF, RbCl, Rb2CO3, RbNO3 or RbBF4; the Pb-containing compound is PbF2, PbCl2, Pb2O3, PbCO3 or Pb(BF4)2; the Y-containing compound is YF3, YCl3 or Y2O3; the B-containing compound is H3BO3, B2O3, RbBF4 or Pb(BF4)2;

[0011] The vacuum packaging method is used to prepare the compound yttrium lead rubidium borate:

[0012] The Rb-containing compound, the Pb-containing compound, the Y-containing compound and the B-containing compound are mixed uniformly in a molar ratio of Rb:Pb:Y:B=7-14:1-2:2-4:15-30, and the mixture is placed in a quartz tube. The quartz tube is evacuated to a vacuum degree of 1×10 -3 Pa, sealed at high temperature, placed in a muffle furnace, heated to 700-750°C at a rate of 5-10°C / h, and kept at this temperature for 24-120 hours to obtain the compound Rb7PbY2B 15 O 30 The Rb-containing compound is RbF, RbCl, Rb2CO3, RbNO3 or RbBF4; the Pb-containing compound is PbF2, PbCl2, Pb2O3, PbCO3 or Pb(BF4)2; the Y-containing compound is YF3, YCl3 or Y2O3; and the B-containing compound is H3BO3, B2O3, RbBF4 or Pb(BF4)2.

[0013] A yttrium lead rubidium borate nonlinear optical crystal, the chemical formula of the crystal is Rb7PbY2B 15 O 30 , molecular weight is 1625.45, belongs to the trigonal crystal system, space group is R32, unit cell parameters are α=90°,β=90°,γ=120°,the unit cell volume is

[0014] The method for preparing the yttrium lead rubidium borate nonlinear optical crystal adopts a melt method, a high-temperature melt method or a vacuum packaging method to grow the crystal;

[0015] The specific operation of growing the yttrium lead rubidium borate nonlinear optical crystal by the melt method is carried out in the following steps:

[0016] a. Mix the Rb-containing compound, the Pb-containing compound, the Y-containing compound and the B-containing compound in a molar ratio of Rb:Pb:Y:B=7-14:1-2:2-4:15-30, put them into a platinum crucible, place them in a muffle furnace, heat them to 700-750°C, and keep them at this temperature for 48-120 hours to obtain the compound Rb7PbY2B 15 O 30 Polycrystalline powder, wherein the Rb-containing compound is RbF, RbCl, Rb2CO3, RbNO3 or RbBF4; the Pb-containing compound is PbF2, PbCl2, Pb2O3, PbCO3 or Pb(BF4)2; the Y-containing compound is YF3, YCl3 or Y2O3; the B-containing compound is H3BO3, B2O3, RbBF4 or Pb(BF4)2;

[0017] b. Compound Rb7PbY2B prepared in step a 15 O 30 The polycrystalline powder is loaded into a platinum crucible, placed in a muffle furnace, heated to 800-950°C, and kept at this temperature for 10-120 hours to obtain a mixed melt;

[0018] c. Slowly cool the mixed melt obtained in step b to 350°C at a rate of 0.1-2°C / h, and then quickly cool it to room temperature at a rate of 5-10°C / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0019] d. Growing crystals in the compound melt by the Czochralski method: Fix the seed crystal obtained in step c on a seed crystal rod, place the seed crystal from the top of the mixed melt obtained in step b, apply a crystal rotation of 2-20 rpm through a crystal growth controller, pull the seed crystal at a speed of 1-10 mm / day, and cool it at a rate of 0.1-10 ° C / h. After the crystal growth stops, Rb7PbY2B is obtained. 15 O 30 Nonlinear optical crystals;

[0020] Alternatively, the crystals can be grown in the compound melt using the pyrolysis method: the seed crystal obtained in step c is fixed on a seed crystal rod, and the seed crystal is placed from above the melt obtained in step b. The temperature is lowered at a rate of 0.1°C / h, and the crystal is allowed to grow for 5-15 hours. The crystal is slowly lifted but does not leave the liquid surface to continue growing. This process is repeated until the crystal growth stops, and Rb7PbY2B is obtained. 15 O30 Nonlinear optical crystals;

[0021] Or use the crucible descent method to grow crystals in the compound melt: place the seed crystal prepared in step c at the bottom of the crucible, and then add the compound Rb7PbY2B prepared in step a 15 O 30 The polycrystal is placed in a crucible, which is then sealed with a platinum crucible. The growth furnace is heated to 800-900°C and kept at this temperature for 10-120 hours. The crucible position is adjusted to allow the seed crystal to melt slightly, and the crucible is then lowered at a rate of 1-10 mm / day. At the same time, the growth temperature is maintained constant, or the temperature is lowered to 350°C at a maximum cooling rate of 3°C / h. After the growth is completed, the temperature is rapidly lowered to room temperature at a rate of 10°C / h to obtain Rb7PbY2B. 15 O 30 Nonlinear optical crystals;

[0022] The specific operation of growing the yttrium lead rubidium borate nonlinear optical crystal by the high-temperature melt method is carried out in the following steps:

[0023] a. Mix the Rb-containing compound, the Pb-containing compound, the Y-containing compound and the B-containing compound in a molar ratio of Rb:Pb:Y:B=7-14:1-2:2-4:15-30, put them into a platinum crucible, place them in a muffle furnace, heat them to 700-750°C, and keep them at this temperature for 48-120 hours to obtain the compound Rb7PbY2B 15 O 30 Polycrystalline powder, wherein the Rb-containing compound is RbF, RbCl, Rb2CO3, RbNO3 or RbBF4; the Pb-containing compound is PbF2, PbCl2, Pb2O3, PbCO3 or Pb(BF4)2; the Y-containing compound is YF3, YCl3 or Y2O3; the B-containing compound is H3BO3, B2O3, RbBF4 or Pb(BF4)2;

[0024] b. Compound Rb7PbY2B obtained in step a 15 O 30 The polycrystalline powder and the flux are mixed uniformly in a molar ratio of 1:0.1-3, and then placed in a platinum crucible, heated to 800-850°C, and kept at this temperature for 5-120 hours to obtain a mixed melt; the flux is B2O3, PbO or PbF2;

[0025] c. Preparation of seed crystals: Place the mixed melt obtained in step b in a single crystal furnace, slowly cool it down to 350°C at a rate of 0.1-1°C / h, and then quickly cool it down to room temperature at a rate of 5°C / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0026] d. Growing crystals: The seed crystals obtained in step c are fixed on a seed crystal rod, and the seed crystals are placed from above the mixed melt obtained in step b. The crystals are rotated at 2-20 rpm using a crystal growth controller, and the temperature is lowered at a rate of 0.1-3°C / h. When the crystal growth stops, Rb7PbY2B is obtained. 15 O 30 Nonlinear optical crystals;

[0027] The specific operation of growing the yttrium lead rubidium borate nonlinear optical crystal by the vacuum packaging method is carried out in the following steps:

[0028] a. Mix the Rb-containing compound, the Pb-containing compound, the Y-containing compound and the B-containing compound in a molar ratio of Rb:Pb:Y:B=7-14:1-2:2-4:15-30, put them into a platinum crucible, place them in a muffle furnace, heat them to 700-750°C, and keep them at this temperature for 48-120 hours to obtain the compound Rb7PbY2B 15 O 30 Polycrystalline powder, wherein the Rb-containing compound is RbF, RbCl, Rb2CO3, RbNO3 or RbBF4; the Pb-containing compound is PbF2, PbCl2, Pb2O3, PbCO3 or Pb(BF4)2; the Y-containing compound is YF3, YCl3 or Y2O3; the B-containing compound is H3BO3, B2O3, RbBF4 or Pb(BF4)2;

[0029] b. Compound Rb7PbY2B obtained in step a 15 O 30 The polycrystalline powder is placed in a quartz tube, sealed at high temperature, and placed in a muffle furnace. The temperature is raised to 830-900°C, kept constant for 10-120 hours, then lowered to 350°C at a rate of 0.1-1°C / h, and then rapidly lowered to room temperature at a rate of 5-10°C / h to obtain Rb7PbY2B 15 O 30 Nonlinear optical crystals.

[0030] The yttrium lead rubidium borate nonlinear optical crystal is used in preparing multi-band frequency doubling devices or optical elements.

[0031] The yttrium lead rubidium borate nonlinear optical crystal is used in preparing a harmonic light output for frequency doubling of the fundamental frequency light of 1064 nm output by an Nd:YAG laser.

[0032] The yttrium lead rubidium borate nonlinear optical crystal is used in preparing a frequency doubling generator, an up or down frequency converter or an optical parametric oscillator.

[0033] The preparation method of the yttrium lead rubidium borate nonlinear optical crystal of the present invention comprises the following containers used in the preparation process: a platinum crucible, a ceramic crucible, a quartz tube, a conical flask, and a beaker; when the container is a quartz tube, vacuuming is required before sealing to prevent the volatilization of raw materials during the reaction and the explosion of the quartz tube.

[0034] In the preparation method of the yttrium lead rubidium borate nonlinear optical crystal of the present invention, the resistance furnace used in the preparation process is a muffle furnace or a drying box.

[0035] The preparation method of the yttrium lead rubidium borate nonlinear optical crystal of the present invention is used to obtain Rb7PbY2B 15 O 30 Nonlinear optical crystals have no obvious layered growth habits. By using large-sized containers and extending the crystal growth cycle, correspondingly large-sized nonlinear optical crystals Rb7PbY2B can be obtained. 15 O 30 , in the Rb7PbY2B 15 O 30 During the growth of nonlinear optical crystals, the crystals are easy to grow and become transparent without wrapping, and have the advantages of fast growth rate, low cost, and easy acquisition of large-sized crystals. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 The compound of the present invention is Rb7PbY2B 15 O 30 The powder XRD spectrum of the compound Rb7PbY2B is consistent with the theoretical XRD spectrum. 15 O 30 existence;

[0037] Figure 2 Rb7PbY2B of the present invention 15 O 30 A diagram of the crystal structure;

[0038] Figure 3 Rb7PbY2B of the present invention 15 O 30 The working principle diagram of the nonlinear optical device made of crystal, where 1 is the laser, 2 is the emitted light beam, and 3 is Rb7PbY2B 15 O 30 Crystal, 4 is the outgoing beam, and 5 is the filter. DETAILED DESCRIPTION

[0039] The present invention is further described below with reference to the following examples. It should be noted that the following examples are not intended to limit the scope of the present invention, and any improvements made based on the present invention do not violate the spirit of the present invention. Unless otherwise specified, the raw materials and equipment used in the present invention are commercially available.

[0040] Example 1

[0041] Preparation of compounds:

[0042] According to the reaction formula: 7RbF+PbF2+2YF3+10B2O3→Rb7PbY2B 15 O 30 +5BF3, using solid phase reaction method to synthesize compound Rb7PbY2B 15 O 30 :

[0043] RbF, PbF2, YF3, and B2O3 were mixed uniformly in a molar ratio of 7:1:2:10, placed in a platinum crucible, and placed in a muffle furnace. The temperature was raised to 700°C and kept constant for 48 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0044] Example 2

[0045] Preparation of compounds:

[0046] According to the reaction formula: 7Rb2CO3+2PbCO3+2Y2O3+15B2O3→2Rb7PbY2B 15 O 30 +9CO2, using solid phase reaction method to synthesize compound Rb7PbY2B 15 O 30 :

[0047] Rb2CO3, PbCO3, Y2O3, and B2O3 were mixed uniformly in a molar ratio of 7:2:2:15, placed in a platinum crucible, and placed in a muffle furnace. The temperature was raised to 750°C and kept constant for 120 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0048] Example 3

[0049] Preparation of compounds:

[0050] According to the reaction formula: 14RbNO3+2PbO+2Y2O3+15B2O3→2Rb7PbY2B 15 O 30 +7N2O5, using solid phase reaction method to synthesize compound Rb7PbY2B 15 O 30 :

[0051] RbNO3, PbO, Y2O3, and B2O3 were mixed evenly in a molar ratio of 14:2:2:15, placed in a platinum crucible, and placed in a muffle furnace. The temperature was raised to 750°C and kept constant for 120 hours to obtain the compound Rb7PbY2B15 O 30 of polycrystalline powder.

[0052] Example 4

[0053] Preparation of compounds:

[0054] According to the reaction formula: 7RbBF4+Pb(BF4)2+2YF3+10B2O3→Rb7PbY2B 15 O 30 +14BF3, using solid phase reaction method to synthesize compound Rb7PbY2B 15 O 30 :

[0055] RbBF4, Pb(BF4)2, YF3, and B2O3 were mixed uniformly in a molar ratio of 7:1:2:10, placed in a platinum crucible, and placed in a muffle furnace. The temperature was raised to 720°C and kept constant for 48 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0056] Example 5

[0057] Preparation of compounds:

[0058] According to the reaction formula: 7RbF+PbF2+2YF3+15H3BO3→Rb7PbY2B 15 O 30 +15H2O+15HF, using solid phase reaction method to synthesize compound Rb7PbY2B 15 O 30 :

[0059] RbF, PbF2, YF3, and H3BO3 were mixed uniformly in a molar ratio of 7:1:2:15, placed in a platinum crucible, and placed in a muffle furnace. The temperature was raised to 700°C and kept constant for 48 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0060] Example 6

[0061] Preparation of compounds:

[0062] According to the reaction formula: 7Rb2CO3+2PbCO3+2Y2O3+30H3BO3→2Rb7PbY2B 15 O 30 +45H2O+9CO2, using solid phase reaction method to synthesize compound Rb7PbY2B 15 O 30 :

[0063] Rb2CO3, PbCO3, Y2O3, H3BO3 were mixed uniformly in a molar ratio of 7:2:2:30, placed in a platinum crucible, placed in a muffle furnace and heated to 700℃, kept at this temperature for 120 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0064] Example 7

[0065] Preparation of compounds:

[0066] According to the reaction formula: 14RbNO3+2PbO+2Y2O3+30H3BO3→2Rb7PbY2B 15 O 30 +45H2O+7N2O5, using solid phase reaction method to synthesize compound Rb7PbY2B 15 O 30 :

[0067] RbNO3, PbO, Y2O3, and H3BO3 were mixed uniformly in a molar ratio of 14:2:2:30, placed in a platinum crucible, and placed in a muffle furnace. The temperature was raised to 700°C and kept constant for 48 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0068] Example 8

[0069] Preparation of compounds:

[0070] According to the reaction formula: 7RbCl+PbCl2+2YCl3+10B2O3→Rb7PbY2B 15 O 30 +5BCl3, using solid phase reaction method to synthesize compound Rb7PbY2B 15 O 30 :

[0071] RbCl, PbCl2, YCl3, and B2O3 were mixed uniformly in a molar ratio of 7:1:2:10, placed in a platinum crucible, and placed in a muffle furnace. The temperature was raised to 700°C and kept constant for 48 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0072] Example 9

[0073] Preparation of compounds:

[0074] According to the reaction formula: 7RbF+PbF2+2YF3+10B2O3→Rb7PbY2B 15 O 30 +5BF3, using vacuum packaging method to synthesize compound Rb7PbY2B15 O 30 :

[0075] RbF, PbF2, YF3, and B2O3 were mixed evenly in a molar ratio of 7:1:2:10, and placed in a Φ40 mm quartz tube. The quartz tube was evacuated to a vacuum degree of 1×10 -3 Pa, sealed at high temperature, placed in a muffle furnace, heated to 700°C at a rate of 10°C / h, and kept at this temperature for 24 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0076] Example 10

[0077] Preparation of compounds:

[0078] According to the reaction formula: 7Rb2CO3+2PbCO3+2Y2O3+15B2O3→2Rb7PbY2B 15 O 30 +2CO2, using vacuum encapsulation method to synthesize compound Rb7PbY2B 15 O 30 :

[0079] Rb2CO3, PbCO3, Y2O3, and B2O3 were mixed evenly in a molar ratio of 7:2:2:15, and placed in a Φ40 mm quartz tube. The quartz tube was evacuated to a vacuum degree of 1×10 -3 Pa, sealed at high temperature, placed in a muffle furnace, heated to 750°C at a rate of 10°C / h, and kept at this temperature for 120 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0080] Example 11

[0081] Preparation of compounds:

[0082] According to the reaction formula: 14RbNO3+2PbO+2Y2O3+15B2O3→2Rb7PbY2B 15 O 30 +7N2O5, using vacuum encapsulation method to synthesize the compound Rb7PbY2B 15 O 30 :

[0083] RbNO3, PbO, Y2O3, and B2O3 were mixed evenly in a molar ratio of 14:2:2:15, and placed in a Φ40 mm quartz tube. The quartz tube was evacuated to a vacuum degree of 1×10 -3 Pa, sealed at high temperature, placed in a muffle furnace, heated to 750°C at a rate of 5°C / h, and kept at this temperature for 120 hours to obtain the compound Rb7PbY2B15 O 30 of polycrystalline powder.

[0084] Example 12

[0085] Preparation of compounds:

[0086] According to the reaction formula: 7RbBF4+Pb(BF4)2+2YF3+10B2O3→Rb7PbY2B 15 O 30 +14BF3, using vacuum encapsulation method to synthesize compound Rb7PbY2B 15 O 30 :

[0087] RbBF4, Pb(BF4)2, YF3, and B2O3 were mixed evenly in a molar ratio of 7:1:2:10, and placed in a Φ40 mm quartz tube. The quartz tube was evacuated to a vacuum degree of 1×10 -3 Pa, sealed at high temperature, placed in a muffle furnace, heated to 720°C at a rate of 10°C / h, and kept at this temperature for 24 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0088] Example 13

[0089] Preparation of compounds:

[0090] According to the reaction formula: 7RbF+PbF2+2YF3+15H3BO3→Rb7PbY2B 15 O 30 +15H2O+15HF, using vacuum packaging method to synthesize compound Rb7PbY2B 15 O 30 :

[0091] RbF, PbF2, YF3, and H3BO3 were mixed evenly in a molar ratio of 7:1:2:15, and placed in a Φ40 mm quartz tube. The quartz tube was evacuated to a vacuum degree of 1×10 -3 Pa, sealed at high temperature, placed in a muffle furnace, heated to 700°C at a rate of 10°C / h, and kept at this temperature for 24 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0092] Example 14

[0093] Preparation of compounds:

[0094] According to the reaction formula: 7Rb2CO3+2PbCO3+2Y2O3+30H3BO3→2Rb7PbY2B 15 O30 +45H2O+9CO2, the compound Rb7PbY2B was synthesized by vacuum packaging method 15 O 30 :

[0095] Rb2CO3, PbCO3, Y2O3, and H3BO3 were mixed evenly in a molar ratio of 7:2:2:30, and placed in a Φ40 mm quartz tube. The quartz tube was evacuated to a vacuum degree of 1×10 -3 Pa, sealed at high temperature, placed in a muffle furnace, heated to 700°C at a rate of 10°C / h, and kept at this temperature for 24 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0096] Example 15

[0097] Preparation of compounds:

[0098] According to the reaction formula: 14RbNO3+2PbO+2Y2O3+30H3BO3→2Rb7PbY2B 15 O 30 +45H2O+7N2O5, the compound Rb7PbY2B was synthesized by vacuum encapsulation method 15 O 30 :

[0099] RbNO3, PbO, Y2O3, and H3BO3 were mixed evenly in a molar ratio of 14:2:2:30, and placed in a Φ40 mm quartz tube. The quartz tube was evacuated to a vacuum degree of 1×10 -3 Pa, sealed at high temperature, placed in a muffle furnace, heated to 700°C at a rate of 5°C / h, and kept at this temperature for 24 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0100] Example 16

[0101] Preparation of compounds:

[0102] According to the reaction formula: 7RbCl+PbCl2+2YCl3+10B2O3→Rb7PbY2B 15 O 30 +5BCl3, using vacuum encapsulation method to synthesize compound Rb7PbY2B 15 O 30 :

[0103] RbCl, PbCl2, YCl3, and B2O3 were mixed evenly in a molar ratio of 7:1:2:10, and placed in a Φ40 mm quartz tube. The quartz tube was evacuated to a vacuum degree of 1×10 -3Pa, sealed at high temperature, placed in a muffle furnace, heated to 700°C at a rate of 5°C / h, and kept at this temperature for 24 hours to obtain the compound Rb7PbY2B 15 O 30 of polycrystalline powder.

[0104] Example 17

[0105] Melt-grown Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0106] Compound Rb7PbY2B prepared according to Example 1 15 O 30 The polycrystalline powder was loaded into a platinum crucible, placed in a muffle furnace, heated to 900°C, and kept at this temperature for 10 hours to obtain a mixed melt;

[0107] The mixed melt was slowly cooled to 350°C at a rate of 0.1°C / h, and then rapidly cooled to room temperature at a rate of 5°C / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0108] The crystal was grown by the Czochralski method: the obtained seed crystal was fixed on the seed crystal rod, and the seed crystal was placed from the top of the mixed melt. The crystal was rotated at 2 rpm by the crystal growth controller, and the seed crystal was pulled at a speed of 1 mm / day. The temperature was lowered at a rate of 0.1 °C / h. After the crystal growth stopped, Rb7PbY2B with a size of 10 mm × 12 mm × 9 mm was obtained. 15 O 30 Nonlinear optical crystals.

[0109] Example 18

[0110] Melt-grown Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0111] Compound Rb7PbY2B prepared according to Example 2 15 O 30 The polycrystalline powder was loaded into a platinum crucible, placed in a muffle furnace, heated to 950°C, and kept at this temperature for 120 hours to obtain a mixed melt;

[0112] The mixed melt was slowly cooled to 350°C at a rate of 2°C / h, and then rapidly cooled to room temperature at a rate of 10°C / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0113] The crystal was grown by the Czochralski method: the obtained seed crystal was fixed on the seed crystal rod, and the seed crystal was placed from above the mixed melt. The crystal was rotated at 20 rpm by the crystal growth controller, and the seed crystal was pulled at a speed of 10 mm / day. The temperature was lowered at a rate of 10 ° C / h. After the crystal growth stopped, Rb7PbY2B with a size of 10 mm × 10 mm × 8 mm was obtained. 15 O 30 Nonlinear optical crystals.

[0114] Example 19

[0115] Melt-grown Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0116] Compound Rb7PbY2B prepared according to Example 3 15 O 30 The polycrystalline powder was loaded into a platinum crucible, placed in a muffle furnace, heated to 950°C, and kept at this temperature for 100 hours to obtain a mixed melt;

[0117] The obtained mixed melt was slowly cooled to 350°C at a rate of 1.5°C / h, and then quickly cooled to room temperature at a rate of 8°C / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0118] The crystal was grown by the kyropoulos method: the obtained seed crystal was fixed on the seed crystal rod, and the seed crystal was placed from the top of the mixed melt. The temperature was lowered at a rate of 0.1℃ / h, and the crystal was grown for 15 hours. The crystal was slowly lifted but not out of the liquid surface, and continued to grow. This was repeated 3 times to obtain Rb7PbY2B with a size of 11mm×10mm×10mm. 15 O 30 Nonlinear optical crystals.

[0119] Example 20

[0120] Melt-grown Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0121] Compound Rb7PbY2B prepared according to Example 4 15 O 30 The polycrystalline powder was loaded into a platinum crucible, placed in a muffle furnace, heated to 920°C, and kept at this temperature for 100 hours to obtain a mixed melt;

[0122] The obtained mixed melt was slowly cooled to 350°C at a rate of 1.5°C / h, and then quickly cooled to room temperature at a rate of 8°C / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0123] The crystal was grown by the kyropoulos method: the obtained seed crystal was fixed on the seed crystal rod, and the seed crystal was placed from the top of the mixed melt. The temperature was lowered at a rate of 0.1℃ / h, and the crystal was grown for 10 hours. The crystal was slowly lifted but not out of the liquid surface, and continued to grow. This was repeated 3 times to obtain Rb7PbY2B with a size of 12mm×10mm×9mm. 15 O 30 Nonlinear optical crystals.

[0124] Example 21

[0125] Melt-grown Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0126] Compound Rb7PbY2B prepared according to Example 5 15 O 30 The polycrystalline powder was placed in a platinum crucible, heated to 800°C, and kept at this temperature for 10 hours to obtain a mixed melt;

[0127] The obtained mixed melt was slowly cooled to 400℃ at a rate of 2℃ / h, and then quickly cooled to room temperature at a rate of 5℃ / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0128] The crystal was grown in the compound melt by the crucible descending method: the seed crystal was placed at the bottom of the crucible, and the compound Rb7PbY2B prepared in Example 5 was added. 15 O 30 The polycrystalline powder was placed in a crucible, which was then sealed with a platinum crucible. The growth furnace temperature was raised to 800°C and kept constant for 10 hours. The crucible position was adjusted to allow the seed crystal to melt slightly. The crucible was then lowered at a rate of 1 mm / day and cooled to 350°C at a rate of 3°C / h. After the growth was completed, the crucible was quickly cooled to room temperature at a rate of 10°C / h. This resulted in Rb7PbY2B with a size of 13 mm × 11 mm × 10 mm. 15 O 30 Nonlinear optical crystals.

[0129] Example 22

[0130] Melt-grown Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0131] Compound Rb7PbY2B prepared according to Example 6 15 O 30 The polycrystalline powder was placed in a platinum crucible, heated to 900°C, and kept at this temperature for 60 hours to obtain a mixed melt;

[0132] The obtained mixed melt was slowly cooled to 350°C at a rate of 1.5°C / h, and then rapidly cooled to room temperature at a rate of 5°C / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0133] The crystal was grown in the compound melt by the crucible descending method: the seed crystal was placed at the bottom of the crucible, and the compound Rb7PbY2B prepared in Example 6 was added. 15 O 30 The polycrystalline powder was placed in a crucible, which was then sealed with platinum. The growth furnace temperature was raised to 900°C and kept constant for 120 hours. The crucible position was adjusted to allow the seed crystal to melt slightly. The crucible was then lowered at a rate of 10 mm / day while the growth temperature was kept constant. After the growth was completed, the crucible was quickly lowered to room temperature at a rate of 10°C / h to obtain Rb7PbY2B with a size of 11 mm × 10 mm × 9 mm. 15 O 30 Nonlinear optical crystals.

[0134] Example 23

[0135] Melt-grown Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0136] Compound Rb7PbY2B prepared according to Example 7 15 O 30 The polycrystalline powder was loaded into a platinum crucible, placed in a muffle furnace, heated to 900°C, and kept at this temperature for 100 hours to obtain a mixed melt;

[0137] The obtained mixed melt was slowly cooled to 350°C at a rate of 1.5°C / h, and then quickly cooled to room temperature at a rate of 8°C / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0138] The crystal was grown by the kyropoulos method: the obtained seed crystal was fixed on the seed crystal rod, and the seed crystal was placed from the top of the mixed melt. The temperature was lowered at a rate of 0.1℃ / h, and the crystal was grown for 5 hours. The crystal was slowly lifted but not out of the liquid surface, and continued to grow. This was repeated 3 times to obtain Rb7PbY2B with a size of 11mm×10mm×9mm. 15 O 30 Nonlinear optical crystals.

[0139] Example 24

[0140] Melt-grown Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0141] Compound Rb7PbY2B prepared according to Example 8 15 O 30 The polycrystalline powder was placed in a platinum crucible, heated to 900°C, and kept at this temperature for 10 hours to obtain a mixed melt;

[0142] The obtained mixed melt was slowly cooled to 900℃ at a rate of 2℃ / h, and then quickly cooled to room temperature at a rate of 5℃ / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0143] The crystal was grown in the compound melt by the crucible descending method: the seed crystal was placed at the bottom of the crucible, and the compound Rb7PbY2B prepared in Example 8 was added. 15 O 30 The polycrystalline powder was placed in a crucible, which was then sealed with a platinum crucible. The growth furnace temperature was raised to 900°C and kept constant for 10 hours. The crucible position was adjusted to allow the seed crystal to melt slightly. The crucible was then lowered at a rate of 1 mm / day and cooled to 350°C at a rate of 3°C / h. After the growth was completed, the crucible was quickly cooled to room temperature at a rate of 10°C / h. This resulted in Rb7PbY2B with a size of 13 mm × 11 mm × 9 mm. 15 O 30 Nonlinear optical crystals.

[0144] Example 25

[0145] High-temperature melt growth of Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0146] Compound Rb7PbY2B prepared according to Example 1 15 O 30 The polycrystalline powder and flux B2O3 were mixed uniformly in a molar ratio of 1:0.1, placed in a platinum crucible, heated to 850°C, and kept at this temperature for 5 hours to obtain a mixed melt;

[0147] Preparation of seed crystal: The obtained mixed melt was placed in a single crystal furnace, slowly cooled to 350℃ at a rate of 0.1℃ / h, and then quickly cooled to room temperature at a rate of 5℃ / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0148] Growing crystals: The obtained seed crystals were fixed on the seed crystal rods, and the seed crystals were placed from above the prepared mixed melt. The crystals were rotated at 2 rpm by the crystal growth controller and cooled at a rate of 0.1 °C / h. After the crystal growth stopped, Rb7PbY2B with a size of 12 mm × 10 mm × 8 mm was obtained. 15 O 30 Nonlinear optical crystals.

[0149] Example 26

[0150] High-temperature melt growth of Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0151] Compound Rb7PbY2B prepared according to Example 2 15 O 30 The polycrystalline powder and flux B2O3 were mixed uniformly in a molar ratio of 1:0.1, placed in a platinum crucible, heated to 800°C, and kept at this temperature for 20 hours to obtain a mixed melt;

[0152] Preparation of seed crystal: The obtained mixed melt was placed in a single crystal furnace, slowly cooled to 350℃ at a rate of 0.1℃ / h, and then quickly cooled to room temperature at a rate of 5℃ / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0153] Growing crystals: The obtained seed crystals were fixed on the seed crystal rods, and the seed crystals were placed from above the prepared mixed melt. The crystals were rotated at 20 rpm by a crystal growth controller and cooled at a rate of 0.1 °C / h. After the crystal growth stopped, Rb7PbY2B with a size of 11 mm × 10 mm × 9 mm was obtained. 15 O 30 Nonlinear optical crystals.

[0154] Example 27

[0155] High-temperature melt growth of Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0156] Compound Rb7PbY2B prepared according to Example 3 15 O 30 The polycrystalline powder and flux B2O3 were mixed uniformly in a molar ratio of 1:0.1, placed in a platinum crucible, heated to 800°C, and kept at this temperature for 60 hours to obtain a mixed melt;

[0157] Preparation of seed crystal: The obtained mixed melt was placed in a single crystal furnace, slowly cooled to 350℃ at a rate of 0.5℃ / h, and then quickly cooled to room temperature at a rate of 5℃ / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0158] Growing crystals: The obtained seed crystals were fixed on the seed crystal rods, and the seed crystals were placed from above the prepared mixed melt. The crystals were rotated at 10 rpm by a crystal growth controller and cooled at a rate of 1 °C / h. After the crystal growth stopped, Rb7PbY2B with a size of 9 mm × 9 mm × 7 mm was obtained. 15 O 30 Nonlinear optical crystals.

[0159] Example 28

[0160] High-temperature melt growth of Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0161] Compound Rb7PbY2B prepared according to Example 4 15 O 30 The polycrystalline powder and flux B2O3 were mixed uniformly in a molar ratio of 1:0.1, placed in a platinum crucible, heated to 820°C, and kept at this temperature for 30 hours to obtain a mixed melt;

[0162] Preparation of seed crystal: The obtained mixed melt was placed in a single crystal furnace, slowly cooled to 350℃ at a rate of 0.2℃ / h, and then quickly cooled to room temperature at a rate of 5℃ / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0163] Growing crystals: The obtained seed crystals were fixed on the seed crystal rods, and the seed crystals were placed from above the prepared mixed melt. The crystals were rotated at 2 rpm by the crystal growth controller and cooled at a rate of 0.1 °C / h. After the crystal growth stopped, Rb7PbY2B with a size of 10 mm × 9 mm × 7 mm was obtained. 15 O 30 Nonlinear optical crystals.

[0164] Example 29

[0165] High-temperature melt growth of Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0166] Compound Rb7PbY2B prepared according to Example 5 15 O 30 The polycrystalline powder and flux B2O3 were mixed uniformly in a molar ratio of 1:0.1, placed in a platinum crucible, heated to 850°C, and kept at this temperature for 100 hours to obtain a mixed melt;

[0167] Preparation of seed crystal: The obtained mixed melt was placed in a single crystal furnace, slowly cooled to 350℃ at a rate of 1℃ / h, and then rapidly cooled to room temperature at a rate of 5℃ / h to obtain Rb7PbY2B 15 O30 seed crystal;

[0168] Growing crystals: The obtained seed crystals were fixed on the seed crystal rods, and the seed crystals were placed from above the prepared mixed melt. The crystals were rotated at 15 rpm by a crystal growth controller and cooled at a rate of 3 °C / h. After the crystal growth stopped, Rb7PbY2B with a size of 14 mm × 11 mm × 10 mm was obtained. 15 O 30 Nonlinear optical crystals.

[0169] Example 30

[0170] High-temperature melt growth of Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0171] Compound Rb7PbY2B prepared according to Example 6 15 O 30 The polycrystalline powder and flux B2O3 were mixed uniformly in a molar ratio of 1:0.1, placed in a platinum crucible, heated to 830°C, and kept at this temperature for 20 hours to obtain a mixed melt;

[0172] Preparation of seed crystal: The obtained mixed melt was placed in a single crystal furnace, slowly cooled to 350℃ at a rate of 0.1℃ / h, and then rapidly cooled to room temperature at a rate of 5℃ / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0173] Growing crystals: The obtained seed crystals were fixed on the seed crystal rods, and the seed crystals were placed from above the prepared mixed melt. The crystals were rotated at 5 rpm by a crystal growth controller and cooled at a rate of 3 °C / h. After the crystal growth stopped, Rb7PbY2B with a size of 12 mm × 10 mm × 9 mm was obtained. 15 O 30 Nonlinear optical crystals.

[0174] Example 31

[0175] High-temperature melt growth of Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0176] Compound Rb7PbY2B prepared according to Example 3 15 O 30 The polycrystalline powder and flux PbO were mixed uniformly in a molar ratio of 1:3, placed in a platinum crucible, heated to 800°C, and kept at this temperature for 120 hours to obtain a mixed melt;

[0177] Preparation of seed crystal: The obtained mixed melt was placed in a single crystal furnace, slowly cooled to 350℃ at a rate of 0.5℃ / h, and then quickly cooled to room temperature at a rate of 5℃ / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0178] Growing crystals: The obtained seed crystals were fixed on the seed crystal rods, and the seed crystals were placed from above the prepared mixed melt. The crystals were rotated at 2 rpm by the crystal growth controller and cooled at a rate of 0.1 °C / h. After the crystal growth stopped, Rb7PbY2B with a size of 14 mm × 11 mm × 9 mm was obtained. 15 O 30 Nonlinear optical crystals.

[0179] Example 32

[0180] High-temperature melt growth of Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0181] Compound Rb7PbY2B prepared according to Example 7 15 O 30 The polycrystalline powder and flux PbO were mixed uniformly in a molar ratio of 1:3, placed in a platinum crucible, heated to 800°C, and kept at this temperature for 100 hours to obtain a mixed melt;

[0182] Preparation of seed crystal: The obtained mixed melt was placed in a single crystal furnace, slowly cooled to 350℃ at a rate of 0.1℃ / h, and then quickly cooled to room temperature at a rate of 5℃ / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0183] Growing crystals: The obtained seed crystals were fixed on the seed crystal rods, and the seed crystals were placed from above the mixed melt. The crystals were rotated at 2 rpm by a crystal growth controller, and the temperature was lowered at a rate of 0.1 °C / h. After the crystal growth stopped, Rb7PbY2B with a size of 11 mm × 11 mm × 9 mm was obtained. 15 O 30 Nonlinear optical crystals.

[0184] Example 33

[0185] High-temperature melt growth of Rb7PbY2B 15 O 30 Nonlinear optical crystals:

[0186] Compound Rb7PbY2B prepared according to Example 5 15 O 30The polycrystalline powder and flux PbF2 were mixed uniformly in a molar ratio of 1:3, placed in a platinum crucible, heated to 810°C, and kept at this temperature for 60 hours to obtain a mixed melt;

[0187] Preparation of seed crystal: The obtained mixed melt was placed in a single crystal furnace, slowly cooled to 350℃ at a rate of 0.1℃ / h, and then quickly cooled to room temperature at a rate of 5℃ / h to obtain Rb7PbY2B 15 O 30 seed crystal;

[0188] Growing crystals: The obtained seed crystals were fixed on the seed crystal rods, and the seed crystals were placed from above the prepared mixed melt. The crystals were rotated at 10 rpm by a crystal growth controller and cooled at a rate of 1 °C / h. After the crystal growth stopped, Rb7PbY2B with a size of 13 mm × 10 mm × 9 mm was obtained. 15 O 30 Nonlinear optical crystals.

[0189] Example 34

[0190] Growth of Rb7PbY2B by vacuum encapsulation 15 O 30 Nonlinear optical crystals:

[0191] The compound Rb7PbY2B prepared in Example 8 15 O 30 The polycrystalline powder was placed in a Φ40 mm quartz tube, and the tube was evacuated to a vacuum degree of 1×10 -3 Pa, sealed at high temperature, placed in a muffle furnace, heated to 850 ° C, kept constant for 120 hours, then cooled to 350 ° C at a rate of 0.5 ° C / h, and then quickly cooled to room temperature at a rate of 8 ° C / h to obtain Rb7PbY2B with a size of 3mm × 3mm × 2mm 15 O 30 Nonlinear optical crystals.

[0192] Example 35

[0193] Growth of Rb7PbY2B by vacuum encapsulation 15 O 30 Nonlinear optical crystals:

[0194] The compound Rb7PbY2B prepared in Example 5 15 O 30 The polycrystalline powder was placed in a Φ40 mm quartz tube, and the tube was evacuated to a vacuum degree of 1×10 -3Pa, sealed at high temperature, placed in a muffle furnace, heated to 900 ° C, kept constant for 10 hours, then cooled to 350 ° C at a rate of 0.1 ° C / h, and then quickly cooled to room temperature at a rate of 5 ° C / h to obtain Rb7PbY2B with a size of 4mm × 3mm × 2mm 15 O 30 Nonlinear optical crystals.

[0195] Example 36

[0196] Growth of Rb7PbY2B by vacuum encapsulation 15 O 30 Nonlinear optical crystals:

[0197] The compound Rb7PbY2B prepared in Example 3 15 O 30 The polycrystalline powder was placed in a Φ40 mm quartz tube, and the tube was evacuated to a vacuum degree of 1×10 -3 Pa, sealed at high temperature, placed in a muffle furnace, heated to 870 ° C, kept constant for 60 hours, then cooled to 350 ° C at a rate of 0.1 ° C / h, and then quickly cooled to room temperature at a rate of 8 ° C / h to obtain Rb7PbY2B with a size of 4mm × 2mm × 2mm 15 O 30 Nonlinear optical crystals.

[0198] Example 37

[0199] Growth of Rb7PbY2B by vacuum encapsulation 15 O 30 Nonlinear optical crystals:

[0200] The compound Rb7PbY2B prepared in Example 6 15 O 30 The polycrystalline powder was placed in a Φ40 mm quartz tube, and the tube was evacuated to a vacuum degree of 1×10 -3 Pa, sealed at high temperature, placed in a muffle furnace, heated to 830 ° C, kept constant for 100 hours, then cooled to 350 ° C at a rate of 1 ° C / h, and then quickly cooled to room temperature at a rate of 10 ° C / h to obtain Rb7PbY2B with a size of 3mm × 2mm × 2mm 15 O 30 Nonlinear optical crystals.

[0201] Example 38

[0202] Growth of Rb7PbY2B by vacuum encapsulation 15 O 30 Nonlinear optical crystals:

[0203] The compound Rb7PbY2B prepared in Example 4 15O 30 The polycrystalline powder was placed in a Φ40 mm quartz tube, and the tube was evacuated to a vacuum degree of 1×10 -3 Pa, sealed at high temperature, placed in a muffle furnace, heated to 900 ° C, kept constant for 50 hours, then cooled to 350 ° C at a rate of 0.2 ° C / h, and then quickly cooled to room temperature at a rate of 8 ° C / h, thus obtaining Rb7PbY2B with a size of 2mm × 2mm × 1mm. 15 O 30 Nonlinear optical crystals.

[0204] Example 39

[0205] Any Rb7PbY2B obtained in Examples 17-38 15 O 30 Nonlinear optical crystals are processed in matching directions and attached Figure 3 As shown in the figure, it is placed at position 3. At room temperature, a Q-switched Nd:YAG laser is used as the light source. The incident wavelength is 1064nm. The infrared beam 2 with a wavelength of 1064nm emitted by the Q-switched Nd:YAG laser 1 is incident on the Rb7PbY2B 15 O 30 Single crystal 3 produces green frequency-doubled light with a wavelength of 532nm, and the output intensity is about 1.3 times that of KDP under the same conditions.

Claims

1. A yttrium lead rubidium borate nonlinear optical crystal, characterized in that The chemical formula of the crystal is Rb7PbY2B 15 O 30 , molecular weight is 1625.45, belongs to the trigonal system, and the space group is R 32, the unit cell parameters are a = 13.4642(3) Å, b = 13.4642(3) Å, c = 15.2917(8) Å, α = 90°, β = 90°, γ = 120°, the unit cell volume is 2400.18 Å 3 .

2. A method for preparing the yttrium lead rubidium borate nonlinear optical crystal according to claim 1, characterized in that Crystals are grown using melt method, high temperature melt method or vacuum packaging method; The specific operation of growing the yttrium lead rubidium borate nonlinear optical crystal by the melt method is carried out in the following steps: a. Mix the Rb-containing compound, the Pb-containing compound, the Y-containing compound and the B-containing compound in a molar ratio of Rb:Pb:Y:B=7-14:1-2:2-4:15-30, put them into a platinum crucible, place them in a muffle furnace, heat them to 700-750°C, and keep them at this temperature for 48-120 hours to obtain the compound Rb7PbY2B 15 O 30 Polycrystalline powder, wherein the Rb-containing compound is RbF, RbCl, Rb2CO3, RbNO3 or RbBF4; The Pb-containing compound is PbF2, PbCl2, Pb2O3, PbCO3 or Pb(BF4)2; the Y-containing compound is YF3, YCl3 or Y2O3; the B-containing compound is H3BO3, B2O3, RbBF4 or Pb(BF4)2; b. Compound Rb7PbY2B prepared in step a 15 O 30 The polycrystalline powder is loaded into a platinum crucible, placed in a muffle furnace, heated to 800-950°C, and kept at this temperature for 10-120 hours to obtain a mixed melt; c. The mixed melt obtained in step b was slowly cooled to 350°C at a rate of 0.1-2°C / h, and then rapidly cooled to room temperature at a rate of 5-10°C / h to obtain Rb7PbY2B 15 O 30 seed crystal; d. Growing crystals in the compound melt by the Czochralski method: Fix the seed crystal obtained in step c on a seed crystal rod, place the seed crystal from the top of the mixed melt obtained in step b, apply a crystal rotation of 2-20 rpm using a crystal growth controller, pull the seed crystal at a rate of 1-10 mm / day, and simultaneously cool it at a rate of 0.1-10 °C / h. After the crystal growth stops, Rb7PbY2B is obtained. 15 O 30 Nonlinear optical crystals; Alternatively, the crystals can be grown in the compound melt using the pyrolysis method: the seed crystal obtained in step c is fixed on a seed crystal rod, and the seed crystal is placed from above the melt obtained in step b. The temperature is lowered at a rate of 0.1°C / h, and the crystal is allowed to grow for 5-15 hours. The crystal is slowly lifted but does not leave the liquid surface to continue growing. This process is repeated until the crystal growth stops, and Rb7PbY2B is obtained. 15 O 30 Nonlinear optical crystals; Or use the crucible descent method to grow crystals in the compound melt: place the seed crystal prepared in step c at the bottom of the crucible, and then add the compound Rb7PbY2B prepared in step a 15 O 30 The polycrystal is placed in a crucible, which is then sealed with a platinum crucible. The growth furnace is heated to 800-900°C and kept at this temperature for 10-120 hours. The crucible position is adjusted to allow the seed crystal to melt slightly, and the crucible is then lowered at a rate of 1-10 mm / day. At the same time, the growth temperature is kept constant, or the temperature is lowered to 350°C at a maximum cooling rate of 3°C / h. After the growth is completed, the temperature is rapidly lowered to room temperature at a rate of 10°C / h to obtain Rb7PbY2B. 15 O 30 Nonlinear optical crystals; The specific operation of growing yttrium lead rubidium borate nonlinear optical crystal by high temperature melt method is carried out in the following steps: The Rb-containing compound, the Pb-containing compound, the Y-containing compound and the B-containing compound are mixed uniformly in a molar ratio of Rb:Pb:Y:B=7-14:1-2:2-4:15-30, placed in a platinum crucible, placed in a muffle furnace, heated to 700-750 ° C, and kept at this temperature for 48-120 hours to obtain the compound Rb7PbY2B 15 O 30 Polycrystalline powder, wherein the Rb-containing compound is RbF, RbCl, Rb2CO3, RbNO3 or RbBF4; The Pb-containing compound is PbF2, PbCl2, Pb2O3, PbCO3 or Pb(BF4)2; the Y-containing compound is YF3, YCl3 or Y2O3; the B-containing compound is H3BO3, B2O3, RbBF4 or Pb(BF4)2; b. Compound Rb7PbY2B obtained in step a 15 O 30 The polycrystalline powder and the flux are mixed uniformly in a molar ratio of 1:0.1-3, and then placed in a platinum crucible, heated to 800-850° C., and kept at this temperature for 5-120 hours to obtain a mixed melt; the flux is B2O3, PbO or PbF2; c. Preparation of seed crystal: Place the mixed melt obtained in step b in a single crystal furnace, slowly cool it down to 350°C at a rate of 0.1-1°C / h, and then quickly cool it down to room temperature at a rate of 5°C / h to obtain Rb7PbY2B 15 O 30 seed crystal; d. Growing crystals: The seed crystals obtained in step c are fixed on a seed crystal rod, and the seed crystals are placed from above the mixed melt obtained in step b. The crystals are rotated at 2-20 rpm using a crystal growth controller, and the temperature is lowered at a rate of 0.1-3 °C / h. When the crystal growth stops, Rb7PbY2B is obtained. 15 O 30 Nonlinear optical crystals; The specific operation of growing the yttrium lead rubidium borate nonlinear optical crystal by the vacuum packaging method is carried out in the following steps: a. Mix the Rb-containing compound, the Pb-containing compound, the Y-containing compound and the B-containing compound in a molar ratio of Rb:Pb:Y:B=7-14:1-2:2-4:15-30, put them into a platinum crucible, place them in a muffle furnace, heat them to 700-750°C, and keep them at this temperature for 48-120 hours to obtain the compound Rb7PbY2B 15 O 30 Polycrystalline powder, wherein the Rb-containing compound is RbF, RbCl, Rb2CO3, RbNO3 or RbBF4; The Pb-containing compound is PbF2, PbCl2, Pb2O3, PbCO3 or Pb(BF4)2; the Y-containing compound is YF3, YCl3 or Y2O3; the B-containing compound is H3BO3, B2O3, RbBF4 or Pb(BF4)2; b. Compound Rb7PbY2B obtained in step a 15 O 30 The polycrystalline powder is placed in a quartz tube, sealed at high temperature, and placed in a muffle furnace. The temperature is raised to 830-900°C, kept constant for 10-120 hours, then lowered to 350°C at a rate of 0.1-1°C / h, and then rapidly lowered to room temperature at a rate of 5-10°C / h to obtain Rb7PbY2B 15 O 30 Nonlinear optical crystals.

3. Use of the yttrium lead rubidium borate nonlinear optical crystal according to claim 1 in preparing a multi-band frequency doubling device or optical element.

4. Use of the yttrium lead rubidium borate nonlinear optical crystal according to claim 1 in preparing a harmonic light output of the 1064 nm fundamental frequency light output by an Nd:YAG laser for frequency doubling.

5. Use of the yttrium lead rubidium borate nonlinear optical crystal according to claim 1 in preparing a frequency doubling generator, an up- or down-frequency converter or an optical parametric oscillator.

Images