A high optical quality K3B6O 10 Fluxes and methods for Br crystal growth

Abstract

The application provides a high-optical-quality K3B6O 10 Br crystal growth flux and crystal growth method. The K3B6O 10 The use of the K3B6O 10 Br crystal growth flux can effectively reduce the growth temperature of the K3B6O 10 Br crystal to a temperature range of 650-700 DEG C. The viscosity of the solution can be obviously reduced, the solute transmission is facilitated, the crystal growth is easy, and the generation of inclusions is obviously reduced. The volatility of the system can be effectively reduced, the stability of the growth system is improved, the formation of floating crystals is prevented, the crystal growth speed is improved, and the repeatability of the crystal growth is improved. Due to the reduction of impurities in the crystal, the absorption in the 200-300 nm wave band is effectively solved, and the transmittance in the wave band is greatly improved.

Description

Technical Field

[0001] This invention relates to the field of crystal technology, specifically to a high optical quality K3B6O 10 Fluxes for Br crystal growth and crystal growth methods. Background Technology

[0002] K3B6O 10 Br compounds (KBB) were first synthesized by Belokoneva et al. in 2006 via a hydrothermal method. KBB crystals belong to the trigonal crystal system, space group R3m, with cell parameters a = 1.01153(8) nm, c = 0.88592(14) nm, Z = 3, V = 0.78502(15) nm. 3 KBB is an excellent nonlinear optical crystal material with many advantages, including high second harmonic conversion efficiency, wide light transmission range, phase matching over a large range, non-hygroscopicity, chemical stability, moderate hardness, and ease of machining.

[0003] Currently, centimeter-scale single crystals can be grown using a high-temperature solution method with a PbO co-solvent system. These crystals have an ultraviolet cutoff wavelength of 182 nm and exhibit high transmittance (>80%) in the 300-2500 nm wavelength range, with transmittance exceeding 50% in the 200-260 nm ultraviolet band. The shortest harmonic doubling wavelength of this crystal is 292.4 nm, making it suitable for harmonic and third-harmonic output in Nd:YAG lasers (wavelength 1064 nm). The individual nonlinear optical coefficients d are precisely measured using the Mark fringe method. 22 d 33 and d 31 d was measured 22 =1.23±0.01pm / V and d 33 = 0.43±0.01pm / V. Basic nonlinear optical parameters of the KBB crystal include the effective frequency doubling factor (0.92pm / V), acceptance angle (1.2mrad·cm), and temperature bandwidth (17.1℃·cm). Using an Nd:YAG laser with a pulse width of 10ns and a repetition rate of 10kHz, the uncoated size of the laser was... 3 A KBB crystal achieved a high power output of 45.5W with a conversion efficiency of 36.5%. The crystal's power stability at 43.8W and 24.8W outputs within 1 hour was 1.5% and 1.46%, respectively. Under the same experimental conditions, the KBB crystal slightly outperformed the LBO crystal, currently the preferred choice for high-power laser frequency doubling. A 4×4×13.3mm crystal was used. 3A phase-matched third-harmonic generation device achieved a high-power output of 19.3W from a 355nm ultraviolet laser, with a maximum conversion efficiency of 18.3%. Overall, KBB crystals possess a short ultraviolet cutoff edge (182nm), a large nonlinear optical coefficient (1.23pm / V), are non-hygroscopic, and have good machinability, making them a novel and potential crystal material for frequency doubling and third harmonic generation.

[0004] Currently, KBB crystals are heterogeneous molten compounds, and their growth mainly employs high-temperature solution methods and top-seeded Czochralski methods, with PbO and KF as the primary flux systems. However, the system using H3BO3 as a solvent has a very high viscosity, posing numerous challenges to crystal growth: a thick growth boundary layer, poor solute transport, and difficulties in heat dissipation and impurity removal. Traditionally, introducing PbO as a flux results in KBB crystals exhibiting significant absorption peaks in the 200-280 nm range, affecting crystal quality and subsequent applications. KF, being relatively light, easily causes melt stratification and also exhibits significant volatility, impacting crystal growth stability. Therefore, it is necessary to find new and suitable fluxes for growing high-quality KBB crystals. Summary of the Invention

[0005] To overcome the shortcomings of existing technologies, the purpose of this invention is to provide a high optical quality K3B6O 10 The present invention relates to a flux for Br crystal growth and a crystal growth method thereof. The use of the flux can reduce the viscosity and volatility of the crystal growth system, improve the stability of the crystal growth system, eliminate the absorption of the crystal in the low wavelength range (200-300nm) of the transmission spectrum, and obtain larger-sized, high-quality KBB crystals.

[0006] The objective of this invention is achieved through the following technical solution:

[0007] A K3B6O 10 Br crystal growth flux, wherein the flux is a K2CO3-MoO3 and / or Li2MoO4-LiF system, wherein the K2CO3-MoO3 and / or Li2MoO4-LiF system includes K2CO3, MoO3 and / or Li2MoO4, LiF.

[0008] According to an embodiment of the present invention, the flux is a K2CO3-MoO3-LiF system (including K2CO3, MoO3, and LiF), a K2CO3-Li2MoO4-LiF system (including K2CO3, Li2MoO4, and LiF), or a K2CO3-MoO3-Li2MoO4-LiF system (including K2CO3, MoO3, Li2MoO4, and LiF).

[0009] According to embodiments of the present invention, the molar ratio of K2CO3, MoO3 and / or Li2MoO4, LiF is (1.6-2):(0.8-1.2):(0.6-1.0), for example (1.6, 1.7, 1.8, 1.9 or 2):(0.8, 0.9, 1, 1.1 or 1.2):(0.6, 0.7, 0.8, 0.9 or 1.0), exemplary ratios are 1.6:0.8:0.6, 2:0.8:0.7, 2:0.8:0.8, 2:0.8:0.9, 2:0.8:1.0, 2:0. 9:0.6, 2:0.9:0.7, 2:0.9:0.8, 2:0.9:0.9, 2:0.9:1.0, 2:1.0:0.6, 2:1.0:0.7, 2:1.0:0.8, 2:1.0:0.9, 2:1.0:1.0, 2:1.1:0.6, 2:1.1:0.7, 2:1.1:0.8, 2:1.1:0.9, 2:1.1:1.0, 2:1.2:0.6, 2:1.2:0.7, 2:1.2:0.8, 2:1.2:0.9 or 2:1.2:1.0.

[0010] According to embodiments of the present invention, MoO3 and / or Li2MoO4 are excellent fluxes. The introduction of MoO3 can disrupt the B–O network structure in the growth system, weaken the interaction between B–O bonds, and thus reduce the viscosity of the growth system.

[0011] The present invention also provides the above-mentioned K3B6O 10 A method for preparing a flux for Br crystal growth, the method comprising the following steps:

[0012] The K3B6O was prepared by mixing K2CO3, MoO3 and / or Li2MoO4 and LiF. 10 Br crystal growth flux.

[0013] The present invention also provides the above-mentioned K3B6O 10 The use of Br crystal growth flux, as a K3B6O 10 Flux for Br crystal growth.

[0014] The present invention also provides a K3B6O 10 A method for growing Br crystals, the method comprising the following steps:

[0015] Using the above K3B6O 10 Br crystal growth flux, K3B6O was prepared using a high-temperature solution method. 10 Br crystal.

[0016] According to an embodiment of the present invention, the method includes the following steps:

[0017] 1) Ingredients and pretreatment: Potassium source, bromine source, boron source and K3B6O 10 The Br crystal growth flux is mixed and placed in a crystal growth furnace, heated to 750-850℃ to melt, and kept at the temperature for 12-24 hours to obtain the growth raw material.

[0018] 2) Seed crystal placement: Cool the growth material from step 1) to 650-700℃, determine the saturation temperature of the growth material, and introduce the seed crystal fixed on the seed crystal rod into the melt at 0.5-2℃ above the saturation temperature. Maintain the temperature for 5-30 minutes, and then cool down to the saturation temperature.

[0019] 3) Crystal growth: Starting from the saturation temperature, the temperature is reduced at a rate of 0.1-1℃ / day, while the crystal is rotated at a rate of 20-60 rpm to make the crystal grow continuously.

[0020] 4) Unloading: After the crystal has grown to the required size, the seed crystal rod is raised to remove the crystal from the liquid surface, and the temperature is lowered to room temperature at a rate of 5-10℃ / h to obtain the K3B6O. 10 Br crystal.

[0021] According to an embodiment of the present invention, in step 1), the boron source is selected from H3BO3 and / or B2O3.

[0022] According to an embodiment of the present invention, in step 1), the bromine source is selected from KBr.

[0023] According to an embodiment of the present invention, in step 1), the ingredients are prepared according to the molar ratio of K2CO3:H3BO3 and / or B2O3:KBr:MoO3 and / or Li2MoO4:LiF of (1.6-2):6:1:(0.8-1.2):(0.6-1.0).

[0024] According to an embodiment of the present invention, in step 1), the mixing is performed by grinding and mixing in an agate grinder.

[0025] According to an embodiment of the present invention, in step 1), a platinum crucible is used to hold the mixed ingredients.

[0026] According to an embodiment of the present invention, in step 1), the temperature is increased to 750-850℃ at a heating rate of 10-50℃ / h and held at the temperature for 12-24h; for example, the temperature is increased to 750℃, 760℃, 770℃, 780℃, 790℃, 800℃, 810℃, 820℃, 830℃, 840℃ or 850℃; and held at the temperature for 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h, 23h or 24h.

[0027] According to an embodiment of the present invention, in step 2), the saturation temperature of the growth raw material is determined by the trial seed crystal method.

[0028] According to an embodiment of the present invention, in step 2), the seed crystal can be fixed on the seed crystal rod using methods commonly used in the art.

[0029] According to an embodiment of the present invention, in step 2), the direction of the seed crystal can be any seed crystal direction.

[0030] According to an embodiment of the present invention, in step 3), the direction of crystal rotation is unidirectional or bidirectional. If the direction of crystal rotation is bidirectional, it rotates according to the following rotation cycle: in the first direction, it sequentially accelerates (e.g., from 0 to 60 rpm), rotates at a constant speed, decelerates (e.g., from 60 to 0 rpm), and stops rotating, and then in the second direction opposite to the first direction, it sequentially accelerates, rotates at a constant speed, decelerates, and stops rotating.

[0031] According to an embodiment of the present invention, in step 3), the center of the liquid surface in the crucible is defined as 0 cm, and the vertical temperature gradient of the solution from the center of the liquid surface downwards is 0.1-0.3℃ / cm.

[0032] According to an embodiment of the present invention, in step 4), the size of the crystal growth is determined by both the growth condition of the crystal and the size of the crucible. If the crystal growth condition is good, the crystal is allowed to grow continuously until its size is about 2-3 cm smaller than the crucible size to prevent it from colliding with the crucible; if the crystal growth condition is poor, growth should be stopped immediately and the crystal removed.

[0033] The present invention also provides a K3B6O 10 Br crystal, K3B6O 10 Br crystals were prepared using the method described above.

[0034] According to an embodiment of the present invention, the K3B6O 10 The size of the Br crystal is (20-80)×(20-80)×(13-70)mm 3 For example, 30×40×50mm 3 .

[0035] Beneficial effects:

[0036] This invention provides a high optical quality K3B6O 10 Flux for Br crystal growth and crystal growth method. The K3B6O... 10 The use of flux for Br crystal growth can effectively reduce K3B6O 10The growth temperature of Br crystals is set within the range of 650-700℃. This significantly reduces the viscosity of the solution, facilitating solute transport, promoting crystal growth, and significantly reducing inclusion formation. It effectively reduces system volatility, improves the stability of the growth system, prevents the formation of drift crystals, and increases crystal growth rate and repeatability. Due to the reduction of impurities in the crystal, absorption in the 200-300nm wavelength band is effectively resolved, and transmittance in this band is greatly improved. Furthermore, KBB crystals grown using the flux system of this application exhibit transmittance exceeding 75% across the entire wavelength band (compared to a minimum transmittance of around 50% for KBB crystals grown using the PbO flux system). In addition, the transmittance in the 300-400nm wavelength band is also superior to that of PbO flux, which is beneficial for the application of crystals in low-band frequency conversion. Large-size, high-optical-quality K3B6O crystals can be stably grown. 10 Br single crystal. Attached Figure Description

[0037] Figure 1 An optical photograph of the high optical quality, large-size KBB crystal (one grid on the substrate is one centimeter) grown according to this invention.

[0038] Figure 2 The transmission spectra of the KBB crystals grown in Example 1 and Comparative Example 1 of this invention are shown in the 200-700 nm wavelength range. Detailed Implementation

[0039] The preparation method of the present invention will be further described in detail below with reference to specific embodiments. It should be understood that the following embodiments are merely illustrative and explanatory of the present invention and should not be construed as limiting the scope of protection of the present invention. All technologies implemented based on the above content of the present invention are covered within the scope of protection intended by the present invention.

[0040] Unless otherwise specified, the experimental methods used in the following examples are conventional methods; unless otherwise specified, the reagents and materials used in the following examples are commercially available.

[0041] Example 1:

[0042] 442.2 g (3.2 mol) of analytical grade K₂CO₃, 1001.4 g (12 mol) of H₃BO₃, 238 g (2.0 mol) of KBr, 230.2 g (1.6 mol) of MoO₃, and 41.4 g (1.6 mol) of LiF were ground uniformly in an agate grinder and placed into an open platinum crucible. The crucible was then placed in a vertical resistance wire crystal growth furnace, and the furnace top was sealed with an insulating lid. A small hole was left in the center of the lid, corresponding to the center of the crucible, for the seed crystal rod to enter and exit. The temperature was increased to 750 °C at a rate of 30 °C / h to completely melt the raw materials and obtain a high-temperature solution. The solution was then stirred at this temperature for 24 hours using a platinum sheet stirrer. After stirring, the temperature was slowly reduced to 680 °C, approximately 10 °C above the saturation temperature. The precise saturation temperature was then determined using a trial-and-error seed crystal method. The cut seed crystal was then fixed to the end of the seed crystal rod with platinum wire and slowly introduced into the growth furnace through a small hole at the top, positioning the seed crystal approximately 5 mm below the solution surface to begin crystal growth. The seed crystal was rotated at 40 rpm, and the cooling rate was 0.1-0.5℃ per day. Once the crystal reached the desired size, growth was stopped, and the crystal was lifted 20 mm above the liquid surface and cooled to room temperature at a rate of 20℃ / h. The final crystal size was 55 × 42 × 27 mm. 3 KBB single crystal.

[0043] Example 2:

[0044] Analytical grade 221.1 g (1.6 mol) K₂CO₃, 500.7 g (6 mol) H₃BO₃, 119.0 g (1.0 mol) KBr, 129.5 g (0.9 mol) MoO₃, and 18.2 g (0.7 mol) LiF were ground uniformly in an agate grinder and placed into an open platinum crucible. The crucible was then placed in a vertical resistance wire crystal growth furnace, and the furnace top was sealed with an insulating lid. A small hole was left in the center of the lid, corresponding to the center of the crucible, for the seed crystal rod to enter and exit. The temperature was increased to 750 °C at a rate of 30 °C / h to completely melt the raw materials and obtain a high-temperature solution. The solution was then stirred at this temperature for 24 hours using a platinum sheet stirrer. After stirring, the temperature was slowly reduced to 685 °C, approximately 10 °C above the saturation temperature. The precise saturation temperature was then determined using a trial-and-error seed crystal method. The cut seed crystal was then fixed to the end of the seed crystal rod with platinum wire and slowly introduced into the growth furnace through a small hole at the top, positioning the seed crystal approximately 5 mm below the solution surface to begin crystal growth. The seed crystal was rotated at 40 rpm, and the cooling rate was 0.1-0.5℃ per day. Once the crystal reached the desired size, growth was stopped, and the crystal was lifted 25 mm above the liquid surface and cooled to room temperature at a rate of 30℃ / h, ultimately yielding a crystal measuring 35 × 18 × 14 mm. 3 KBB single crystal.

[0045] Example 3:

[0046] 221.1 g (1.6 mol) of analytical grade K₂CO₃, 500.7 g (6 mol) of H₃BO₃, 119.0 g (1.0 mol) of KBr, 143.9 g (1.0 mol) of MoO₃, and 16.58 g (0.64 mol) of LiF were ground uniformly in an agate grinder and placed into an open platinum crucible. The crucible was then placed in a vertical resistance wire crystal growth furnace, and the furnace top was sealed with an insulating lid. A small hole was left in the center of the lid, corresponding to the center of the crucible, for the seed crystal rod to enter and exit. The temperature was increased to 750 °C at a rate of 50 °C / h to completely melt the raw materials and obtain a high-temperature solution. The solution was then stirred at this temperature for 24 hours using a platinum sheet stirrer. After removing the stirrer, the temperature was slowly lowered to 690 °C, approximately 10 °C above the saturation temperature. The precise saturation temperature was then determined using a trial-and-error seed crystal method. The cut seed crystal was then fixed to the end of the seed crystal rod with platinum wire and slowly introduced into the growth furnace through a small hole at the top, positioning the seed crystal approximately 5 mm below the solution surface to begin crystal growth. The seed crystal was rotated at 30 rpm, and the cooling rate was 0.1-0.5℃ per day. Once the crystal reached the desired size, growth was stopped, and the crystal was lifted 25 mm above the liquid surface and cooled to room temperature at a rate of 25℃ / h, ultimately yielding a crystal measuring 33×18×16 mm. 3 KBB single crystal.

[0047] Example 4:

[0048] Analytical grade 221.1 g (1.6 mol) K₂CO₃, 500.7 g (6 mol) H₃BO₃, 119.0 g (1.0 mol) KBr, 172.7 g (1.2 mol) MoO₃, and 20.7 g (0.8 mol) LiF were ground uniformly in an agate grinder and placed into an open platinum crucible. The crucible was then placed in a vertical resistance wire crystal growth furnace, and the furnace top was sealed with an insulating lid. A small hole was left in the center of the lid, corresponding to the center of the crucible, for the seed crystal rod to enter and exit. The temperature was increased to 750 °C at a rate of 30 °C / h to completely melt the raw materials and obtain a high-temperature solution. The solution was then stirred at this temperature for 24 hours using a platinum sheet stirrer. After removing the stirrer, the temperature was slowly lowered to 665 °C, approximately 10 °C above the saturation temperature. The precise saturation temperature was then determined using a trial-and-error seed crystal method. The cut seed crystal is then fixed to the end of the seed crystal rod with platinum wire and slowly introduced into the growth furnace through a small hole at the top, positioning the seed crystal approximately 5 mm below the melt surface to begin crystal growth. The seed crystal rotates at 30 rpm, and the cooling rate is 0.1-0.5℃ per day. Once the crystal reaches the desired size, growth is stopped, and the crystal is lifted 20 mm above the liquid surface and cooled to room temperature at a rate of 30℃ / h, ultimately yielding a size of 42×20×18 mm. 3 KBB single crystal.

[0049] Example 5:

[0050] Analytical grade 221.1 g (1.6 mol) K₂CO₃, 500.7 g (6 mol) H₃BO₃, 119.0 g (1.0 mol) KBr, 138.14 g (0.96 mol) MoO₃, and 16.58 g (0.64 mol) LiF were ground uniformly in an agate grinder and placed into an open platinum crucible. The crucible was then placed in a vertical resistance wire crystal growth furnace, and the furnace top was sealed with an insulating lid. A small hole was left in the center of the lid, corresponding to the center of the crucible, for the seed crystal rod to enter and exit. The temperature was increased to 750 °C at a rate of 50 °C / h to completely melt the raw materials and obtain a high-temperature solution. The solution was then stirred at this temperature for 24 hours using a platinum sheet stirrer. After stirring, the temperature was slowly reduced to 675 °C, approximately 10 °C above the saturation temperature. The precise saturation temperature was then determined using a trial-and-error seed crystal method. The cut seed crystal is then fixed to the end of the seed crystal rod with platinum wire and slowly introduced into the growth furnace through a small hole at the top, positioning the seed crystal approximately 5 mm below the melt surface to begin crystal growth. The seed crystal rotates at 30 rpm, and the cooling rate is 0.1-0.5℃ per day. Once the crystal reaches the desired size, growth is stopped, and the crystal is lifted 20 mm above the liquid surface and cooled to room temperature at a rate of 20℃ / h, ultimately yielding a size of 40×16×13 mm. 3 KBB single crystal.

[0051] Example 6:

[0052] 248.8 g (1.8 mol) of analytical grade K₂CO₃, 500.7 g (6 mol) of H₃BO₃, 119.0 g (1.0 mol) of KBr, 173.8 g (1.0 mol) of Li₂MoO₄, and 20.8 g (0.8 mol) of LiF were ground uniformly in an agate grinder and placed into an open platinum crucible. The crucible was then placed in a vertical resistance wire crystal growth furnace, and the furnace top was sealed with an insulating lid. A small hole was left in the center of the lid, corresponding to the center of the crucible, for the seed crystal rod to enter and exit. The temperature was increased to 750 °C at a rate of 30 °C / h to completely melt the raw materials and obtain a high-temperature solution. The solution was then stirred at this temperature for 24 hours using a platinum sheet stirrer. After stirring, the temperature was slowly reduced to 680 °C, approximately 10 °C above the saturation temperature. The precise saturation temperature was then determined using a trial-and-error seed crystal method. The cut seed crystal was then fixed to the end of the seed crystal rod with platinum wire and slowly introduced into the growth furnace through a small hole at the top, positioning the seed crystal approximately 5 mm below the solution surface to begin crystal growth. The seed crystal was rotated at 40 rpm, and the cooling rate was 0.1-0.5℃ per day. Once the crystal reached the desired size, growth was stopped, and the crystal was lifted 20 mm above the liquid surface and cooled to room temperature at a rate of 20℃ / h, ultimately yielding a crystal measuring 35×24×20 mm. 3 KBB single crystal.

[0053] Comparative Example 1:

[0054] 276.4 g (2.0 mol) of analytical grade K₂CO₃, 174.3 g (3.0 mol) of KF, 494.6 g (8 mol) of H₃BO₃, 238.1 g (2.0 mol) of KBr, and 223.2 g (1.0 mol) of PbO were ground uniformly in an agate grinder and placed into an open platinum crucible. The crucible was then placed in a vertical resistance wire crystal growth furnace, and the furnace top was sealed with an insulating lid. A small hole was left in the center of the lid, corresponding to the center of the crucible, for the seed crystal rod to enter and exit. The temperature was increased to 780 °C at a rate of 25 °C / h to completely melt the raw materials and obtain a high-temperature solution. The solution was then stirred at this temperature for 24 hours using a platinum sheet stirrer. After stirring, the temperature was slowly reduced to 700 °C, approximately 10 °C above the saturation temperature. The precise saturation temperature was then determined using a trial-and-error seed crystal method. The cut seed crystal is then fixed to the end of the seed crystal rod with platinum wire and slowly introduced into the growth furnace through a small hole at the top, positioning the seed crystal approximately 2 mm below the melt surface to begin crystal growth. The seed crystal rotates at 15 rpm, and the cooling rate is 0.1-0.5℃ per day. Once the crystal reaches the desired size, growth is stopped, and the crystal is lifted 20 mm above the liquid surface and cooled to room temperature at a rate of 30℃ / h, finally yielding a size of 32×18×15 mm. 3 KBB single crystal.

[0055] Test Example 1:

[0056] Transmission spectroscopy tests were performed on the KBB single crystals of Example 1 and Comparative Example 1, and the results are as follows: Figure 2 As shown, from Figure 2 As can be seen from the results, the KBB single crystal prepared in Example 1 effectively solved the absorption problem of the crystal in the 200-300nm wavelength band and greatly improved the transmittance in this band. Moreover, the transmittance of the KBB single crystal prepared in Example 1 exceeded 75% in the entire wavelength band, while the lowest transmittance of the KBB crystal grown in the PbO flux system of Comparative Example 1 was about 50% in the entire wavelength band. In addition, the transmittance of the KBB single crystal prepared in Example 1 in the 300-400nm wavelength band was also better than that of Comparative Example 1, indicating that the flux and growth method of the present invention produce KBB crystals with higher optical quality.

[0057] The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiments. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A K3B6O 10 Br crystal growth flux, of which, The flux is a K2CO3-MoO3-LiF system, which includes K2CO3, MoO3, and LiF; or, the flux is a K2CO3-Li2MoO4-LiF system, which includes K2CO3, Li2MoO4, and LiF; or, the flux is a K2CO3-MoO3-Li2MoO4-LiF system, which includes K2CO3, MoO3, Li2MoO4, and LiF. The molar ratio of K2CO3, MoO3 and / or Li2MoO4, LiF is (1.6-2):(0.8-1.2):(0.6-1.0).

2. The use of the flux according to claim 1, as K3B6O 10 Flux for Br crystal growth.

3. A K3B6O 10 Br crystal growth methods, among which, The method includes the following steps: Using the K3B6O as described in claim 1 10 Br crystal growth flux, K3B6O was prepared using a high-temperature solution method. 10 Br crystal.

4. The K3B6O according to claim 3 10 Br crystal growth methods, among which, The method includes the following steps: 1) Ingredients and pretreatment: Potassium source, bromine source, boron source and K3B6O 10 The Br crystal growth flux is mixed and placed in a crystal growth furnace, heated to 750-850℃ to melt, and kept at the temperature for 12-24 hours to obtain the growth raw material. 2) Seed crystal placement: Cool the growth material from step 1) to 650-700℃, determine the saturation temperature of the growth material, and introduce the seed crystal fixed on the seed crystal rod into the melt at 0.5-2℃ above the saturation temperature. Maintain the temperature for 5-30 minutes, and then cool down to the saturation temperature. 3) Crystal growth: Starting from the saturation temperature, the temperature is reduced at a rate of 0.1-1℃ / day, while the crystal is rotated at a rate of 20-60 rpm to make the crystal grow continuously. 4) Unloading: After the crystal has grown to the required size, the seed crystal rod is raised to remove the crystal from the liquid surface, and the temperature is lowered to room temperature at a rate of 5-10℃ / h to obtain the K3B6O. 10 Br crystal.

5. The K3B6O according to claim 4 10 Br crystal growth methods, among which, In step 1), the boron source is selected from H3BO3 and / or B2O3; In step 1), the bromine source is selected from KBr.

6. The K3B6O according to claim 5 10 Br crystal growth methods, among which, In step 1), the ingredients are prepared according to the molar ratio of K2CO3:H3BO3 and / or B2O3:KBr:MoO3 and / or Li2MoO4:LiF as (1.6-2):6:1:(0.8-1.2):(0.6-1.0).

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