CN113529170B - Method for growing oversized lithium niobate monocrystal - Google Patents
Method for growing oversized lithium niobate monocrystal Download PDFInfo
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- CN113529170B CN113529170B CN202110768733.XA CN202110768733A CN113529170B CN 113529170 B CN113529170 B CN 113529170B CN 202110768733 A CN202110768733 A CN 202110768733A CN 113529170 B CN113529170 B CN 113529170B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/30—Niobates; Vanadates; Tantalates
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/36—Single-crystal growth by pulling from a melt, e.g. Czochralski method characterised by the seed, e.g. its crystallographic orientation
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Abstract
The invention discloses a method for growing an oversized lithium niobate single crystal, which comprises the following steps: (1) preparing small-sized crystals by a Czochralski method; pulling a section of thin neck after the growth of the small-size crystal is finished; after the pulling of the thin neck is finished, the steps of shoulder expansion, constant diameter and ending are carried out, and the growth of the oversized lithium niobate monocrystal is completed; (2) And after the growth of the oversized lithium niobate single crystal is finished, cooling, and separating the oversized lithium niobate single crystal from the thin neck to obtain the oversized lithium niobate single crystal. The invention solves the problem of sinking caused by unfavorable convection of central heat when the pulling method is used for preparing the oversized lithium niobate monocrystal during shoulder expansion, and can remarkably meet the requirement of the new generation of large-scale mass production of the most urgent strategic large-size crystal materials.
Description
Technical Field
The invention relates to the technical field of preparation of lithium niobate crystals, in particular to a method for growing oversized lithium niobate single crystals.
Background
The fifth generation mobile communication technology (5G) system is accelerating the advent of the fourth industrial revolution era, leading to systematic revolution worldwide. The chinese part 5G core technology is already in the first echelon of the global industry, but some key core devices still rely heavily on importation. The radio frequency filter is the largest sub-industry in the radio frequency front end acoustic chip, and the common SAW uses a lithium niobate wafer as a substrate, so that the temperature drift is larger, and the loss of a high-frequency wave band above 3.5GHz is large. In recent years, the acoustic application potential of the lithium niobate single crystal film material gradually gets widespread international attention, TC-SAW with low temperature coefficient, IHP-SAW with high Q value and high frequency Xbar can be realized, and the film has the advantages of integration and miniaturization, and can meet all performance requirements of a new generation communication system on a radio frequency filter. The lithium niobate thin film is peeled from the lithium niobate wafer and depends on the bonding technology of the lithium niobate wafer and the silicon wafer; chip micromachining relies on semiconductor micromachining lines, currently the semiconductor main flow line is 8 inches; therefore, the 8-inch lithium niobate crystal conforming to the semiconductor production line is a strategic crystal material for mass production of the new generation of acoustic chips.
In addition, specifically, lithium niobate crystals are mainly grown by a Czochralski (Czochralski) pulling method, which comprises the steps of putting a sintered lithium niobate raw material into a platinum crucible, heating and melting, completing seeding by a seed crystal rotation pulling method, and further performing necking, shouldering, isodiametric and ending processes to complete the growth of lithium niobate single crystals. When the pulling method is used for preparing the lithium niobate single crystal, the situation that the shoulder is wide and the waist is thin often exists, which is very unfavorable for large-scale growth of the lithium niobate single crystal, and the problems of great waste and the like exist when the crystal reaches the crystal rod, although the phenomenon can slow down the shoulder expanding speed by operating the instrument and the parameters of crystal growth, thereby slowing down the shoulder width to a certain extent. However, for the growth of oversized (8 inch, 10 inch, 12 inch) lithium niobate single crystals closely related to the process in the semiconductor industry, the situation is firstly transformed into a shoulder expanding process under the influence of the large size, namely, the center heat is unfavorable in convection during shoulder expanding, so that a very serious concave phenomenon exists in the center of the crystal, the shape of the crystal is similar to that of a pot cover, and the phenomenon causes the crystal to stop growing. This is extremely disadvantageous for oversized lithium niobate crystal growth, further limiting further applications.
Disclosure of Invention
In view of the above prior art, an object of the present invention is to provide a method for growing an oversized lithium niobate single crystal. The invention solves the problem of sinking caused by unfavorable convection of central heat when the pulling method is used for preparing the oversized lithium niobate monocrystal during shoulder expansion, and can remarkably meet the requirement of the new generation of large-scale mass production of the most urgent strategic large-size crystal materials.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for growing an oversized lithium niobate single crystal, comprising the steps of:
(1) Firstly, preparing small-size crystals by adopting a pulling method; pulling a section of thin neck after the growth of the small-size crystal is finished; then entering the shoulder expansion, constant diameter and ending stage to finish the growth of the oversized lithium niobate monocrystal;
(2) And after the growth of the oversized lithium niobate single crystal is finished, cooling, and separating the oversized lithium niobate single crystal from the thin neck to obtain the oversized lithium niobate single crystal.
Preferably, in the step (1), the ratio of the small-size crystal diameter to the oversized lithium niobate single crystal diameter is (20 to 40): (200-300).
More preferably, in the step (1), the small-sized crystals have a diameter of 20 to 30mm and a length of 8 to 9mm.
Preferably, in the step (1), the length of the thin neck is 6-10mm, and the diameter of the thin neck is 6-8mm.
Preferably, in step (1), the pulling method for preparing small-sized crystals comprises: batching, mixing, sintering, melting, seeding, necking, shouldering, isodiametric and ending.
More preferably, the batching is carried out by taking lithium carbonate and niobium pentoxide as raw materials according to the molar ratio of the lithium to the niobium of 48.38/51.62.
Preferably, in the step (2), the oversized lithium niobate single crystal is separated from the neck at 3 to 5mm of the neck.
Preferably, in the step (2), the diameter of the oversized lithium niobate single crystal is 200-300mm.
The invention has the beneficial effects that:
according to the method, the oversized lithium niobate crystal is continuously grown at the tail end of the small crystal, so that the heat dissipation in the central axial direction is increased. The heat dissipation and upward transmission of the center of the oversized lithium niobate single crystal without small crystal direct growth mainly depend on seed crystals, and the seed crystals are too small relative to the oversized lithium niobate single crystal, and the diameter ratio of the seed crystals is more than 40 times, so that the axial heat dissipation capability is not outstanding, and the grown crystal is sunken. The invention adopts a method of pulling small crystals first, thereby solving the problem of central liquid level depression when directly growing large-size crystals, and simultaneously increasing the utilization rate of the small crystals by cutting off the large-size crystals after the growth of the oversized crystals is finished, thereby reducing the growth period; or returning the small crystals to the furnace for treatment, thereby more fully improving the utilization rate of the raw materials. Meanwhile, for the growth habit of the shoulder width and waist fineness of the crystal, the invention accelerates the quality change of the crystal in the shoulder expanding process through accelerating the heat dissipation in the central axial direction, thereby entering the constant diameter stage more quickly, shortening the shoulder placing and constant diameter rotating time on the basis of improving the equipment parameters, further optimizing and solving the defect of the shoulder width, and further better utilizing the raw materials and realizing industrialized preparation.
Drawings
FIG. 1 is a schematic diagram of a small-sized crystal structure grown first in accordance with the present invention;
FIG. 2 is a schematic diagram of an 8-size crystal structure obtained after growing small-size crystals according to the present invention;
FIG. 3 is a schematic diagram of a small-sized crystal structure for reuse after cutting in the present invention.
Fig. 4 is a photograph of an 8-inch lithium niobate crystal prepared in example 1 of the present invention.
FIG. 5 is a growth-stopping "pot-cover" type primary crystal prepared in comparative example 1 of the present invention; in the figure, A and B are respectively the front side and the back side of the pot cover type primary crystal.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the present application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
As described in the background section, oversized (8 inch, 10 inch, 12 inch) lithium niobate single crystals are the most demanding strategic crystal materials for mass production of new generation acoustic chips. In the prior art, lithium niobate crystals are mainly grown by a (Czochralski) pulling method. When an oversized lithium niobate single crystal is prepared by using a Czochralski method, there is often a case that the shoulder is wide and the waist is thin, affecting the quality of the single crystal, and this is very disadvantageous for large-scale growth of lithium niobate single crystals; furthermore, latent heat released during crystal growth must be conducted away from the vicinity of the interface, so that the crystal will remain stably grown, and for the growth of oversized lithium niobate crystals, this condition will first be transformed into a shoulder expansion process under the influence of large size, and during shoulder expansion, there is a very serious dishing phenomenon in the center of the crystal due to the adverse convection of central heat, which is similar to a pot cover in shape, and this phenomenon will cause the crystal to stop growing.
Therefore, it is very difficult to grow an oversized lithium niobate single crystal by the existing Czochralski method.
Based on the above, the invention aims to provide a method for growing oversized lithium niobate crystals, which aims to accurately solve the problem of center depression in the shoulder expanding process of the oversized crystals so as to meet the growth requirement of the oversized crystals. The main inventive concept of the present invention is as follows: before the oversized lithium niobate crystal grows, a small crystal is pulled, so that the axial heat dissipation of the oversized lithium niobate crystal growth can be increased through the small crystal, and the problem that the central depression of the oversized lithium niobate crystal growth causes termination of the growth is effectively solved through the acceleration of the central axial heat dissipation.
In one embodiment of the present invention, a method for growing oversized lithium niobate crystals is provided, comprising the steps of:
(1) The raw material proportion is selected for proportioning, and the molar ratio of lithium to niobium is 48.38/51.62;
(2) Briquetting the prepared material, and then placing the briquetted material into a muffle furnace for high-temperature sintering;
(3) Placing the sintered raw materials into a platinum crucible container for compacting, and then placing the raw materials into a pulling furnace for melting;
(4) Slowly lowering the seed crystal to the position of 20mm of the liquid level, and baking the crystal;
(5) Immersing seed crystal into the liquid level, melting part of the seed crystal at a proper point of seeding temperature, and then lifting;
(6) After seeding, pulling up by 1mm, and necking, wherein the width of the necking is smaller than that of the seed crystal;
(7) After the 1mm pulling of the necking is finished, carrying out a small crystal growth shoulder-expanding stage, and entering program automatic control to complete the isodiameter and ending stage of the small crystal when the shoulder-expanding degree is larger than the width of the seed crystal (figure 1);
(8) At the end of the small crystal ending phase, a thin neck is pulled, and in the case of the set crystal form, the oversized crystal is then passed into the oversized crystal growth shoulder phase, followed by completion of the isodiametric and ending phases (fig. 2).
After the oversized crystal is grown, the oversized crystal is cut from the 3-5mm position of the thin neck, the oversized crystal and the small crystal are separated to obtain the oversized crystal and the small crystal (figure 3), and the separated small crystal can be directly utilized or returned to the furnace for treatment, so that the utilization rate of the raw materials is more fully improved.
In order to enable those skilled in the art to more clearly understand the technical solutions of the present application, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples and comparative examples of the present invention are conventional in the art and are commercially available.
Example 1:
the preparation method of the oversized lithium niobate crystal comprises the following steps:
s1, firstly, drying a lithium niobate growing raw material of 5N-grade lithium carbonate and 5N niobium pentoxide to remove moisture in air, and selecting a molar ratio of lithium to niobium to 48.38/51.62 for proportioning;
s2, putting the prepared lithium niobate raw materials into a mixer for mixing, wherein the mixing time is 24 hours;
s3, carrying out briquetting treatment on the mixed materials, and then placing the materials into a muffle furnace for sintering at 1200 ℃ for 14 hours;
s4, after the raw materials are sintered, placing the raw materials into a platinum crucible, melting and stabilizing, and then, lowering seed crystals with the size of 6-50 mm to a position 20mm away from the position above the liquid level, wherein the seed crystals keep rotating at the rotating speed of 7 revolutions per minute;
s41, after the temperature of the melt is stabilized, enabling the seed crystal to enter a liquid level for 1mm, stabilizing for 10min after entering the liquid level for 1mm, starting lifting and necking, wherein the lifting speed during necking is 2mm/h, the heating speed is 2 ℃/h, the necking width is 4mm, and the lifting height is 10mm;
s43, after necking, slowly cooling, entering a shoulder expansion stage at a cooling rate of 10 ℃/h, reducing the pulling speed to 1mm/h, and expanding the crystal diameter to 20mm; then, the temperature is slowly raised, the temperature raising rate is 5 ℃/h, then, the small crystal is in an equal diameter stage, the temperature is constant, the equal diameter pulling speed is 1mm/h, after the equal diameter height reaches 9mm, the temperature raising rate is 10 ℃/h, the small crystal is in a tail-in stage, after the crystal diameter is reduced to 8mm, the temperature is kept stable, a section of thin neck is pulled at the pulling speed of 2mm/h, the length of the thin neck is 8mm, and the diameter of the thin neck is 6mm.
S5, then entering an 8-inch lithium niobate crystal growth stage, and completing the growth of the oversized lithium niobate crystal through shoulder expansion, isodiametric and ending stages;
s51, related parameters of shoulder expanding stage: the cooling rate is 10 ℃/h, the pulling speed is 1mm/h, the crystal diameter is enlarged to 205mm, and then the heating rate is 8 ℃/h, and the diameter is changed to be equal;
s52, parameters related to the constant diameter stage: the cooling rate is 5 ℃/h, the lifting speed is 0.9mm/h, and the constant diameter is 70mm high.
S53, relevant parameters of ending stage: heating rate of 8 ℃/h, lifting speed of 1mm/h, maintaining for 1 hour, and separating the crystal from the melt at a pull rate of 200 mm/h.
And S6, finally, cooling the room temperature at a cooling speed of 50 ℃/h.
S7, cutting the 8-inch lithium niobate crystal obtained by growth from the 3-5mm position of the thin neck, and separating to obtain the 8-inch lithium niobate crystal (figure 4).
Comparative example 1:
s1, firstly, drying a lithium niobate growing raw material of 5N-grade lithium carbonate and 5N niobium pentoxide to remove moisture in air, and selecting a molar ratio of lithium to niobium to 48.38/51.62 for proportioning;
s2, putting the prepared lithium niobate raw materials into a mixer for mixing, wherein the mixing time is 24 hours;
s3, carrying out briquetting treatment on the mixed materials, and then placing the materials into a muffle furnace for sintering at 1200 ℃ for 14 hours;
s4, after the raw materials are sintered, placing the raw materials into a platinum crucible, and after melting and stabilizing, lowering the seed crystal to a position 20mm away from the position above the liquid level;
s41, after the temperature of the melt is stabilized, enabling the seed crystal to enter a liquid level for 1mm, stabilizing for 10min after entering the liquid level for 1mm, starting lifting and necking, wherein the lifting speed during necking is 2mm/h, the heating speed is 2 ℃/h, the necking width is 4mm, and the lifting height is 10mm;
s42, after necking, slowly cooling, entering a shoulder expansion stage at a cooling rate of 10 ℃/h, reducing the pulling speed to 1mm/h, and expanding the crystal diameter to 205mm; then the temperature is slowly raised, the temperature raising rate is 5 ℃/h, the constant temperature is carried over to the constant diameter stage, the constant diameter pulling rate is 1mm/h, at the moment, the concave interface is easy to appear on the growth interface, and the growth is interrupted under severe conditions. The crystal takes the shape of a "pot lid" (fig. 5, A, B).
Comparative example 2:
the diameter of the small-sized crystal prepared in step S43 of example 1 was adjusted to 15mm, the isodiametric height was adjusted to 6mm, and the rest of the operation was unchanged.
Comparative example 3:
the length of the neck pulled up in step S43 of example 1 was adjusted to 12mm, the diameter of the neck was adjusted to 10mm, and the rest of the operation was unchanged.
Comparative example 4:
the length of the neck pulled up in step S43 of example 1 was adjusted to 4mm, the diameter of the neck was adjusted to 4mm, and the rest of the operation was unchanged.
The procedure of example 1, comparative example 1-comparative example 4 was repeated 20 times to prepare 8-inch lithium niobate crystals, and the number of times of occurrence of "pot lid" shaped crystals during the preparation was recorded, and the results are shown in table 1:
table 1:
| group of | Number of times of appearance of "pot lid" shaped crystals |
| Example 1 | 0 |
| Comparative example 1 | 18 |
| Comparative example 2 | 4 |
| Comparative example 3 | 1 |
| Comparative example 4 | 2 |
The above results indicate that: the method can remarkably improve the preparation success rate of the oversized lithium niobate crystal, is beneficial to realizing the large-scale production of the oversized lithium niobate crystal, and avoids the problem of stopping growth caused by the central depression of the oversized lithium niobate crystal growth.
The foregoing description is only of the preferred embodiments of the present application and is not intended to limit the same, but rather, various modifications and variations may be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (3)
1. A method for growing an oversized lithium niobate single crystal, comprising the steps of:
(1) Firstly, preparing small-size crystals by adopting a pulling method; pulling a section of thin neck after the growth of the small-size crystal is finished; then entering the shoulder expansion, constant diameter and ending stage to finish the growth of the oversized lithium niobate monocrystal;
(2) After the growth of the oversized lithium niobate single crystal is finished, cooling, and separating the oversized lithium niobate single crystal from the thin neck to obtain the oversized lithium niobate single crystal;
in the step (1), the ratio of the small-size crystal diameter to the oversized lithium niobate single crystal diameter is (20-40): (200-300);
in the step (1), the diameter of the small-size crystal is 20-30mm, and the length is 8-9mm;
in the step (1), the length of the thin neck is 6-10mm, and the diameter of the thin neck is 6-8mm;
in step (1), the pulling method for preparing small-sized crystals comprises: batching, mixing, sintering, melting, seeding, necking, shoulder expanding, isodiametric and ending;
the batching is carried out by taking lithium carbonate and niobium pentoxide as raw materials and according to the molar ratio of the lithium to the niobium of 48.38/51.62.
2. The growing method according to claim 1, wherein in the step (2), the oversized lithium niobate single crystal is separated from the thin neck at 3-5mm of the thin neck.
3. The growing method according to claim 1, wherein in the step (2), the diameter of the oversized lithium niobate single crystal is 200 to 300mm.
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