CN111206282A - Production method of 8-inch lithium niobate crystal - Google Patents
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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Abstract
The invention relates to the technical field of photoelectron materials, and discloses a production method of 8-inch lithium niobate crystals, which comprises the following steps: (1) preparing a polycrystalline raw material: mixing and sintering lithium carbonate and niobium oxide raw materials, and then briquetting and crushing to obtain a polycrystalline raw material; (2) and (3) crystal growth: putting the polycrystalline raw material into a platinum crucible in a multilayer thermal field, performing crystal growth by adopting a pulling method, and performing seeding, necking, shouldering, isodiametric growth and pulling-off to obtain a multi-domain crystal; (3) annealing and polarization of the crystal: and embedding the multi-domain crystal into a polycrystalline raw material, and annealing and polarizing to obtain the 8-inch lithium niobate crystal. In the crystal growth process, a multilayer temperature field is adopted, so that the temperature field is uniform and free of mutation, crystal polycrystal and cracking are avoided, and the crystal growth is easier to control; the crystal is not easy to crack by adopting the powder embedding method for annealing polarization; and the materials are mixed and fired for many times when the polycrystalline raw material is prepared, so that the Curie temperature of the crystal can be ensured to be stable.
Description
Technical Field
The invention relates to the technical field of photoelectron materials, in particular to a production method of 8-inch lithium niobate crystals.
Background
Lithium niobate single crystal is an excellent multifunctional artificial crystal, is a ferroelectric with the highest known curie temperature and the highest spontaneous polarization, shows the characteristics of integration of electricity melting, light, nonlinearity and the like, is an rare artificial crystal with wide application, has good piezoelectric property, nonlinear optical property, electrooptical and photorefractive property and the like, and can be used for manufacturing various devices with different functions, such as: the device comprises a surface acoustic wave device, an infrared detector, a laser modulator, an optical switch, an optical parametric oscillator, an integrated optical element, a high-frequency broadband filter, a high-frequency high-temperature transducer, a micro-acoustic device, a laser frequency multiplier, a self-frequency doubling laser, a photorefractive device and the like. Because of the wide application range and large dosage of lithium niobate crystals, the production of lithium niobate in the world has a large scale, and the annual output is hundreds of tons. The manufacturing method has the advantages that the yield is the largest, the application range is the widest, namely the manufacturing of Surface Acoustic Waves (SAW) and bulk acoustic wave devices (BAW), and the manufacturing method is an indispensable functional material for the development of novel electronic devices in the IT industry.
Most of common lithium niobate crystals are 3-6 inch crystal bars, and with the further integration of the semiconductor planar process of IT devices and the further improvement of the device frequency, wafers are required to flow on large-size high-precision planar process equipment, so that higher requirements are immediately provided for the diameter of the lithium niobate crystal bar, and compared with the common conventional crystal bar, the eight-inch surface acoustic wave single crystal bar has larger size and can better meet the latest requirements of the international market.
In the prior art, a crystal of lithium niobate is generally prepared by a pulling method, for example, a method for preparing a lithium niobate crystal doped with Zr, Ru, Fe, three times disclosed in chinese patent literature, which is disclosed in publication No. CN101892523A, the method is as follows: weighing ZrO2、RuO2、Fe2O3、Nb2O5And Li2CO3Then mixing to obtain a mixture; and (2) drying the mixture, putting the mixture into a platinum crucible, calcining the mixture at 750 ℃ for 3 hours, sintering the mixture at 1150 ℃ for 4 hours, putting the platinum crucible into an intermediate frequency furnace, and pulling the platinum crucible under the conditions that the pulling speed is 0.5-1.8 mm/h, the axial temperature gradient is 40-50 ℃/cm, and the rotating speed is 15-25 r/min to obtain the Zr, Ru and Fe tri-doped lithium niobate crystal.
However, the method in the prior art is only suitable for preparing 3-6 inch crystals, when 8 inch crystals are produced by the method, the crystal diameter is increased, the crystallization amount is too large in the crystal growth process, the weight of a melt is changed too fast, the temperature gradient change of the whole crystal growth is also caused too fast, and the crystal polycrystal and the cracking are easily caused; meanwhile, because the original lithium niobate crystal with the same composition is in a multi-domain structure, the crystal needs to be subjected to single domain formation near the Curie temperature, and because the diameter of the crystal is increased, the temperature difference of each part of the crystal is increased, the annealing polarization difficulty is increased, the phenomenon of uneven polarization is easy to occur, and the cracking phenomenon can occur if the current is too large. Therefore, in order to meet the market demand, a novel 8-inch lithium niobate crystal processing technology which can process in batches and ensure the precision is urgently needed to be researched and developed by production enterprises to realize the controllability and easy control of the product quality.
Disclosure of Invention
The invention aims to overcome the defects that when 8-inch lithium niobate crystals are produced by using the method in the prior art, the crystal diameter is increased, the crystal quantity in the crystal growth process is overlarge, the weight change of a melt is too fast, the temperature gradient change of the whole crystal growth is too fast, and the crystal polycrystal and the cracking are easily caused; meanwhile, due to the fact that the diameter of the crystal is increased, the temperature difference of each part of the crystal is increased, annealing polarization difficulty is increased, the phenomenon of uneven polarization is easy to occur, and if the current is too large, the problem of cracking is also likely to occur.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production method of 8-inch lithium niobate crystals comprises the following steps:
(1) preparing a polycrystalline raw material: mixing and sintering lithium carbonate and niobium oxide raw materials, and then briquetting and crushing to obtain a polycrystalline raw material;
(2) and (3) crystal growth: putting the polycrystalline raw material into a platinum crucible in a multilayer thermal field, performing crystal growth by adopting a pulling method, and performing seeding, necking, shouldering, isodiametric growth and pulling-off to obtain a multi-domain crystal;
(3) annealing and polarization of the crystal: and embedding the multi-domain crystal into a polycrystalline raw material, and annealing and polarizing to obtain the 8-inch lithium niobate crystal.
In the step (2), the 8-inch lithium niobate crystal is prepared by adopting a pulling method, and the platinum crucible is placed in a multilayer temperature field, so that the temperature field is uniform and has no mutation in the whole growth process, and the polycrystalline and cracking of the crystal caused by the over-quick temperature gradient change of the whole crystal growth are avoided; and (3) annealing polarization is carried out by adopting a powder embedding method, the multi-domain crystal is embedded into the polycrystalline raw material, the whole crystal bar is completely covered by the polycrystalline raw material, the crystal is single-domain at the temperature near the Curie temperature, the phenomenon that the polarization is uneven because the temperature difference of each part of the crystal is large due to overlarge diameter can be avoided, the crystal is effectively prevented from cracking, and the continuous, stable, low-defect and high-quality production of the eight-inch lithium niobate crystal is realized.
Preferably, the mixed sintering process in the step (1) is as follows:
A) pre-burning: pre-burning the raw materials for 2-4 h at 740-760 ℃;
B) reinforced mixing: mixing the pre-sintered raw materials in a mixer for 20-30 h;
C) and (3) secondary material burning: heating the raw materials after the reinforced mixing to 1225-1235 ℃, and preserving the heat for 2-4 h.
In the preparation of the polycrystalline raw material, the lithium carbonate and the niobium oxide are presintered, and then subjected to moisture removal and oxidation treatment; then after the materials are mixed in a strengthening way, secondary material burning from low temperature to high temperature is carried out, the chemical reaction speed of niobium oxide and lithium carbonate is accurately controlled, the high-purity polycrystalline raw material which has uniform components and is suitable for the growth of lithium niobate is prepared, the Curie temperature of the crystal is ensured to be stable, and the Curie temperature of the head and the tail are both in the range of the requirement (1142 +/-3 ℃).
Preferably, the mass ratio of the lithium carbonate to the niobium oxide is (58-59): (41-42). By adopting the proportion, the lithium niobate crystal with near stoichiometric ratio can be effectively prepared.
Preferably, the multilayer thermal field in the step (2) sequentially comprises a ceramic crucible, heat insulation cotton and a corundum crucible from outside to inside, the bottom in the ceramic crucible is provided with a high-alumina brick, the corundum crucible is arranged on the high-alumina brick, the heat insulation cotton is filled between the inner wall of the ceramic crucible and the outer wall of the corundum crucible, and the platinum crucible is arranged in the corundum crucible. The invention adopts the multilayer thermal field sequentially comprising the ceramic crucible, the heat preservation cotton and the corundum crucible from outside to inside, can effectively ensure that the thermal field is uniform and has no mutation in the crystal growth process, and avoids the crystal polycrystal and the crystal cracking caused by the too fast temperature gradient change of the whole crystal growth due to the too large crystallization amount and the too fast weight change of a melt in the crystal growth process.
Preferably, the heat preservation cotton is polycrystalline mullite cotton. The polycrystalline mullite cotton can obviously improve the thermal efficiency of equipment, greatly save energy, improve the production efficiency and improve the product quality.
Preferably, the platinum crucible has a diameter of 310 to 350 mm. The invention designs the platinum crucible with the size within the range by adopting a computer simulation mode according to the required diameter and weight of the single crystal and combining the conditions of melt density and the like, and can grow the high-quality crystal.
Preferably, in the step (2), the pulling rate of the pulling method is 0.5-1.5 mm/h, the axial temperature gradient is 35-45 ℃/cm, and the rotating speed is 15-25 r/min. The process can realize the growth of the eight-inch lithium niobate crystal with continuous stability, low defect and high quality.
Preferably, the annealing process in step (3) is: the temperature rise time is 170-190 min at 30-200 ℃, 1070-1090 min at 200-1100 ℃, the temperature rise time is 390-410 min at 1100-1230 +/-5 ℃, the heat preservation time is 550-650 min, the temperature is lowered to 1170 +/-10 ℃ at 170-190 min, the temperature is preserved for 230-250 min, the temperature is lowered to 950 ℃ at 1650-1750 min, and the temperature is lowered to 600 ℃ at 410-430 min. By adopting the process to carry out powder embedding annealing, the residual stress in the crystal can be effectively eliminated, the component uniformity of the crystal is improved, and the crystal is not easy to crack.
Preferably, the electric polarization is conducted for 25-35 min at 1230 +/-5 ℃ in the annealing process of the step (3). The polarization is carried out at high temperature, the crystal polarization is more complete under the same electric field, and the crystal is not easy to crack.
Preferably, in step (3), the polarization current of the Z-axis crystals is 1.9625 crystal diameter (cm) mA; the polarization current for the Y, X axis crystal was 1.9625 crystal diameter (cm) crystal length (cm) mA. The polarized current is accurately controlled, and the crystal is not easy to crack.
Therefore, the invention has the following beneficial effects:
(1) the materials are mixed and fired for many times when the polycrystalline raw material is prepared, so that the Curie temperature of the crystal can be ensured to be stable;
(2) in the crystal growth process, a multilayer temperature field is adopted, so that the temperature field is uniform and free of mutation, crystal polycrystal and cracking are avoided, and the crystal growth is easier to control;
(3) the crystal is not easy to crack by adopting the powder embedding method for annealing polarization;
(4) the crystal is polarized at high temperature, and the crystal is more completely polarized under the same electric field and is not easy to crack.
Drawings
FIG. 1 is a schematic structural view of a multi-layer thermal field according to the present invention.
In the figure: 1 ceramic crucible, 2 heat preservation cotton, 3 corundum crucible, 4 platinum crucible and 5 high-alumina brick.
Detailed Description
The invention is further described with reference to the following detailed description and accompanying drawings.
As shown in figure 1, the multilayer thermal field in the crystal growth process of the invention sequentially comprises a ceramic crucible 1, heat-insulating cotton 2 and a corundum crucible 3 from outside to inside, wherein the bottom in the ceramic crucible is provided with a high-alumina brick 5, the corundum crucible is arranged on the high-alumina brick, the heat-insulating cotton is filled between the inner wall of the ceramic crucible and the outer wall of the corundum crucible, and the platinum crucible is arranged in the corundum crucible.
Example 1:
a production method of 8-inch lithium niobate crystals comprises the following steps:
(1) preparing a polycrystalline raw material:
A) pre-burning: pre-burning lithium carbonate and niobium oxide raw materials with the mass ratio of 58.5:41.5 at 750 ℃ for 3 h;
B) reinforced mixing: mixing the preburned raw materials in a mixer for 24 hours;
C) and (3) secondary material burning: heating the reinforced mixed raw materials to 1230 ℃, preserving the heat for 3 hours, and then briquetting and crushing to obtain a polycrystalline raw material;
(2) and (3) crystal growth: putting a polycrystalline raw material into a platinum crucible with the diameter of 330mm in a multilayer thermal field, performing crystal growth by adopting a pulling method, and performing seeding, necking, shouldering, isodiametric growth and pulling-off to obtain a multi-domain crystal, wherein the pulling speed is 1.0mm/h, the axial temperature gradient is 40 ℃/cm, and the rotating speed is 20 r/min;
(3) annealing and polarization of the crystal: embedding the multi-domain crystal into a polycrystalline raw material, and annealing and polarizing, wherein the annealing process comprises the following steps: heating up to 30-200 ℃ for 180min, heating up to 200-1100 ℃ for 1080min, heating up to 1100-1230 ℃ for 400min, keeping the temperature for 600min, cooling to 1170 ℃ for 180min, keeping the temperature for 240min, cooling to 950 ℃ for 1700min, and cooling to 600 ℃ for 420min to obtain 8-inch lithium niobate crystals, electrifying and polarizing for 30min at 1230 ℃ in the annealing process, wherein the polarization current is 1.9625 multiplied by the diameter (cm) of the crystals and the length (cm) mA of the crystals.
Example 2:
a production method of 8-inch lithium niobate crystals comprises the following steps:
(1) preparing a polycrystalline raw material:
A) pre-burning: pre-burning lithium carbonate and niobium oxide raw materials with the mass ratio of 58:42 at 740 ℃ for 4 h;
B) reinforced mixing: mixing the preburning raw materials in a mixer for 20 hours;
C) and (3) secondary material burning: heating the reinforced mixed raw materials to 1225 ℃, preserving heat for 4 hours, and then briquetting and crushing to obtain a polycrystalline raw material;
(2) and (3) crystal growth: putting a polycrystalline raw material into a platinum crucible with the diameter of 310mm in a multilayer thermal field, performing crystal growth by adopting a pulling method, and performing seeding, necking, shouldering, isodiametric growth and pulling-off to obtain a multi-domain crystal, wherein the pulling speed is 0.5mm/h, the axial temperature gradient is 35 ℃/cm, and the rotating speed is 15 r/min;
(3) annealing and polarization of the crystal: embedding the multi-domain crystal into a polycrystalline raw material, and annealing and polarizing, wherein the annealing process comprises the following steps: heating up to 170min at 30-200 ℃, 1070min at 200-1100 ℃, 390min at 1100-1225 ℃, 550min at the temperature of heat preservation, 1180 ℃ at 170min, 230min at the temperature of heat preservation, 1650min at 950 ℃, and 600 ℃ at 410min to obtain 8-inch lithium niobate crystals, electrifying and polarizing for 25min at 1225 ℃ in the annealing process, wherein the polarization current is 1.9625 mA multiplied by the crystal diameter (cm) and the crystal length (cm).
Example 3:
a production method of 8-inch lithium niobate crystals comprises the following steps:
(1) preparing a polycrystalline raw material:
A) pre-burning: pre-burning lithium carbonate and niobium oxide raw materials with the mass ratio of 59:41 at 760 ℃ for 2 h;
B) reinforced mixing: mixing the preburning raw materials in a mixer for 30 hours;
C) and (3) secondary material burning: heating the reinforced mixed raw materials to 1235 ℃, preserving heat for 2 hours, and then briquetting and crushing to obtain a polycrystalline raw material;
(2) and (3) crystal growth: putting a polycrystalline raw material into a platinum crucible with the diameter of 350mm in a multilayer thermal field, performing crystal growth by adopting a pulling method, and performing seeding, necking, shouldering, isodiametric growth and pulling-off to obtain a multi-domain crystal, wherein the pulling speed is 1.5mm/h, the axial temperature gradient is 45 ℃/cm, and the rotating speed is 25 r/min;
(3) annealing and polarization of the crystal: embedding the multi-domain crystal into a polycrystalline raw material, and annealing and polarizing, wherein the annealing process comprises the following steps: heating up to 190min at 30-200 ℃, 1090min at 200-1100 ℃, 410min at 1100-1235 ℃, 650min at the temperature, 1160 ℃ at 190min, 250min at the temperature, 1750min at the temperature, 430min at 600 ℃ to obtain 8-inch lithium niobate crystals, electrifying and polarizing at 1235 ℃ for 35min in the annealing process, wherein the polarizing current is 1.9625 (cm) of the diameter of the crystals (cm) mA.
Comparative example 1:
comparative example 1 is different from example 1 in that the polycrystalline raw material in comparative example 1 is prepared by the following method: and sintering the lithium carbonate and niobium oxide raw materials in a mass ratio of 58.5:41.5 at 1230 ℃ for 3h, and crushing a pressed block to obtain the polycrystalline raw material. The rest is the same as in example 1.
Comparative example 2:
comparative example 2 is different from example 1 in that the platinum crucible is not placed in the multi-layer temperature field during the growth of the crystal in step (2); and (3) during annealing and polarization, the multi-domain crystal is not embedded into the polycrystalline raw material. The rest is the same as in example 1.
The growth and polarization results of the 8-inch lithium niobate crystals in the above examples and comparative examples are shown in table 1.
Table 1: growth and polarization results for 8 inch lithium niobate crystals.
| Numbering | Head-to-tail Curie temperature Difference (. degree. C.) | Whether or not to crack |
| Example 1 | 0.5 | Whether or not |
| Example 2 | 0.7 | Whether or not |
| Example 3 | 0.8 | Whether or not |
| Comparative example 1 | 1.9 | Whether or not |
| Comparative example 2 | 1.1 | Is that |
As can be seen from Table 1, in examples 1 to 3, by the method of the present invention, it was possible to obtain fully polarized 8-inch lithium niobate crystals without causing cracking. In contrast, in the comparative example 1, the polycrystalline raw material is not sintered for the second time, and the prepared crystal has incomplete polarization; in comparative example 2, the multi-layer thermal field of the present invention was not used in the growth process, and polycrystalline material was not used to cover the ingot in the annealing and polarization processes, so that the prepared crystal was not polarized completely and cracked. The method of the invention can realize the production of the eight-inch lithium niobate crystal with continuous stability, low defect and high quality.
Claims (10)
1. A production method of 8-inch lithium niobate crystals is characterized by comprising the following steps:
(1) preparing a polycrystalline raw material: mixing and sintering lithium carbonate and niobium oxide raw materials, and then briquetting and crushing to obtain a polycrystalline raw material;
(2) and (3) crystal growth: putting the polycrystalline raw material into a platinum crucible in a multilayer thermal field, performing crystal growth by adopting a pulling method, and performing seeding, necking, shouldering, isodiametric growth and pulling-off to obtain a multi-domain crystal;
(3) annealing and polarization of the crystal: and embedding the multi-domain crystal into a polycrystalline raw material, and annealing and polarizing to obtain the 8-inch lithium niobate crystal.
2. The method for producing an 8-inch lithium niobate crystal according to claim 1, wherein the mixed sintering process in the step (1) is:
A) pre-burning: pre-burning the raw materials for 2-4 h at 740-760 ℃;
B) reinforced mixing: mixing the pre-sintered raw materials in a mixer for 20-30 h;
C) and (3) secondary material burning: heating the raw materials after the reinforced mixing to 1225-1235 ℃, and preserving the heat for 2-4 h.
3. The method for producing an 8-inch lithium niobate crystal according to claim 1 or 2, wherein the mass ratio of the lithium carbonate to the niobium oxide is (58-59): (41-42).
4. The method for producing an 8-inch lithium niobate crystal according to claim 1, wherein the multilayer thermal field in the step (2) comprises a ceramic crucible, heat-insulating cotton and a corundum crucible in sequence from outside to inside, the bottom in the ceramic crucible is provided with a high alumina brick, the corundum crucible is placed on the high alumina brick, the heat-insulating cotton is filled between the inner wall of the ceramic crucible and the outer wall of the corundum crucible, and the platinum crucible is placed in the corundum crucible.
5. The method for producing an 8-inch lithium niobate crystal according to claim 4, wherein the heat-insulating cotton is polycrystalline mullite cotton.
6. The method for producing an 8-inch lithium niobate crystal according to claim 1, 4 or 5, wherein the platinum crucible has a diameter of 310 to 350 mm.
7. The method for producing an 8-inch lithium niobate crystal according to claim 1, 4 or 5, wherein the pulling method in the step (2) has a pulling rate of 0.5 to 1.5mm/h, an axial temperature gradient of 35 to 45 ℃/cm, and a rotation speed of 15 to 25 r/min.
8. The method for producing an 8-inch lithium niobate crystal according to claim 1, wherein the annealing process in the step (3) is: the temperature rise time is 170-190 min at 30-200 ℃, 1070-1090 min at 200-1100 ℃, the temperature rise time is 390-410 min at 1100-1230 +/-5 ℃, the heat preservation time is 550-650 min, the temperature is lowered to 1170 +/-10 ℃ at 170-190 min, the temperature is preserved for 230-250 min, the temperature is lowered to 950 ℃ at 1650-1750 min, and the temperature is lowered to 600 ℃ at 410-430 min.
9. The method for producing an 8-inch lithium niobate crystal according to claim 8, wherein the electric polarization is conducted for 25-35 min at 1230 ℃ ± 5 ℃ during the annealing in the step (3).
10. The method for producing an 8-inch lithium niobate crystal according to claim 1 or 9, wherein in the step (3), the polarization current of the Z-axis crystal is =1.9625 crystal diameter (cm) mA; polarization current for Y, X axis crystals =1.9625 crystal diameter (cm) crystal length (cm) mA.
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| CN112376114A (en) * | 2020-10-15 | 2021-02-19 | 天通控股股份有限公司 | Single-domain method for large-size lithium tantalate crystals |
| CN113913937A (en) * | 2021-09-01 | 2022-01-11 | 中国科学院深圳先进技术研究院 | Lithium niobate crystal and preparation method thereof |
| CN116200828A (en) * | 2023-05-06 | 2023-06-02 | 天通控股股份有限公司 | Preparation method of large-size lithium niobate crystal |
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| CN112376114A (en) * | 2020-10-15 | 2021-02-19 | 天通控股股份有限公司 | Single-domain method for large-size lithium tantalate crystals |
| WO2022077546A1 (en) * | 2020-10-15 | 2022-04-21 | 天通控股股份有限公司 | Large-size lithium tantalate crystal single domain method |
| CN113913937A (en) * | 2021-09-01 | 2022-01-11 | 中国科学院深圳先进技术研究院 | Lithium niobate crystal and preparation method thereof |
| WO2023029288A1 (en) * | 2021-09-01 | 2023-03-09 | 中国科学院深圳先进技术研究院 | Lithium niobate crystal and preparation method therefor |
| CN116200828A (en) * | 2023-05-06 | 2023-06-02 | 天通控股股份有限公司 | Preparation method of large-size lithium niobate crystal |
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Application publication date: 20200529 |