CN112813493A - Growth device and growth method for YCOB crystal growth - Google Patents
Growth device and growth method for YCOB crystal growth Download PDFInfo
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- CN112813493A CN112813493A CN202110154587.1A CN202110154587A CN112813493A CN 112813493 A CN112813493 A CN 112813493A CN 202110154587 A CN202110154587 A CN 202110154587A CN 112813493 A CN112813493 A CN 112813493A
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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
- C30B15/34—Edge-defined film-fed crystal-growth using dies or slits
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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
Abstract
The present invention relates to a growth apparatus and a growth method for YCOB crystal growth, the growth apparatus comprising: a crucible (6); a crystal growth mold (7); a seed rod (1); the crystal growth mould (7) is arranged in the crucible (6); the seed rod (1) is arranged above the growth mould (7) in a way of moving up and down, the lower part of the seed rod (1) is provided with a seed crystal (4) for pulling the crystal to grow, and the crucible (6) is externally sleeved with an induction coil (12) for heating the crucible (6) in an induction way. The growth method comprises the following steps: (1) pretreating raw materials; (2) charging; (3) melting crystal; (4) seeding; (5) shouldering; (6) a stage of equal-diameter growth; (7) and (5) cooling and annealing. Compared with the prior art, the method adopts a mode-guiding method to carry out crystal growth, has the advantages of small crystal growth solid-liquid interface, high crystallization speed, high crystal quality, capability of shaping and directional growth and the like, and becomes one of the mainstream growth modes of the oversized crystal.
Description
Technical Field
The invention relates to the field of crystal material preparation, in particular to a growth device and a growth method for YCOB crystal growth.
Background
The ultra-strong and ultra-fast laser technology is one of the main directions of laser technology development, and how to improve the peak power of the laser and shorten the pulse width of the laser is always the research subject in the technical field of the laser. The main technical methods for realizing the output of the ultra-strong and ultra-fast laser at present comprise: the laser amplification system comprises a Q-switched technology, a mode locking technology, a Chirped Pulse Amplification (CPA) technology, an Optical Parametric Chirped Pulse Amplification (OPCPA) technology and a quasi-parametric chirped pulse amplification (QPCPA) technology, wherein the OPCPA technology has the advantages of high gain, large bandwidth, good beam quality and the like, can further improve the laser peak power in a cascading mode, a beam combining mode and other modes, and is a main way for realizing ultrahigh peak power and ultrashort pulse laser amplification. But either technique is limited by the damage threshold of the laser amplification medium. Therefore, the key to further increase the peak power of the laser is to improve the performance of the laser amplification medium and the effective use area thereof.
The development of the large-caliber nonlinear optical crystal is the key for further improving the peak power of the OPCPA laser system. Yttrium calcium oxide triborate (YCa)4O(BO3)3For short: YCOB) crystal is a novel nonlinear optical crystal, has the advantages of large effective nonlinear coefficient, wide tolerance temperature range, good thermal property, high bearable thermal limit power, no deliquescence, high growth speed and the like, and compared with the traditional nonlinear optical crystal: KDP, LBO, BBO and the like, and YCOB crystals have incomparable advantages in the technical field of ultra-strong and ultra-fast laser. The traditional YCOB crystal growth mode is as follows: the method comprises a cosolvent method, a pulling method and a Bridgman method, wherein the cosolvent method has the defects of complex system, small crystal growth size, polycrystal and the like, so that the poor crystal quality cannot meet the application requirement in the optical field; although the CYCOB crystal of high quality can be grown by the Czochralski method and the Bridgman-Stockbarge method, the Czochralski method has the problem of spiral growth, and defects such as polycrystal, dissociation crack and inclusion exist in the two growth methods. Therefore, the development of techniques for growing YCOB crystals has important research and practical significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a growth device and a growth method for YCOB crystal growth, which have the advantages of small crystal growth solid-liquid interface, high crystallization speed, high crystal quality and capability of shaping and oriented growth.
The purpose of the invention can be realized by the following technical scheme:
the invention adopts a die-guiding method, namely an Edge-defined Film-fed Growth (EFG) technology, which is one of the methods for artificially preparing single crystal materials from a melt, is mainly used for growing crystals with specific shapes, and actually is a deformation of a pulling method. The working principle of the mold guiding method is that raw materials are put into a crucible to be heated and melted, a melt rises to the top end of a mold under the capillary action along the mold, a seed crystal is connected to the liquid level at the top of the mold to pull the melt, and a single crystal with the same shape as the edge of the mold is grown after gradual solidification along with temperature reduction. The crystal growth method by the mode-guiding method has the advantages of small solid-liquid interface, high crystallization speed, high crystal quality and capability of shaping and directional growth, and becomes one of the mainstream growth modes of the crystal with the super-large size, and the specific scheme is as follows:
a growth apparatus for growing a YCOB crystal, the apparatus comprising:
the crucible is used for containing raw material melt for crystal growth;
the crystal growth mould is used for guiding the flow direction of the raw material melt;
a seed rod for guiding crystal growth;
the crystal growth mould is arranged in a crucible and is fixed by a mould clamping sleeve, after raw materials in the crucible are melted, the raw material melt rises to the upper surface of the growth mould from a mould slot through the siphon action, and crystal growth is carried out through seed crystal traction; the seed rod is arranged above the growth mould in a vertically movable mode, seed crystals used for pulling crystals to grow are arranged on the lower portion of the seed rod, and an induction coil used for enabling the crucible to be inductively heated is arranged outside the crucible.
Furthermore, the crystal growth die is made of iridium alloy, is formed by combining and welding a plurality of iridium alloy plates and is isolated by iridium strips, the middle gap corresponds to a die gap for crystal growth, and the top end of the die is provided with a V-shaped opening. The thickness of the grown crystal is limited by the width of the V-shaped opening, and the width of the crystal is limited by the width of the iridium plate; the crucible and the seed rod are both made of iridium; the width of the die slot is 0.3-0.5mm, and the angle of the opening is 100-150 degrees.
Furthermore, the device also comprises a heat-insulating container for avoiding heat dissipation in the crystal growth process; the crucible is arranged in a heat-insulating container.
Furthermore, zirconia balls for further heat preservation are stacked between the heat preservation container and the crucible; the material of the heat preservation container is zirconia ceramics.
Furthermore, a crucible cover is arranged on the crucible.
Further, the heat preservation container including the heat preservation upper cover plate, the last heat preservation cover that splice each other, side heat preservation section of thick bamboo and bottom insulating brick, the heat preservation upper cover plate be located the crucible top, side heat preservation section of thick bamboo be located crucible side, bottom insulating brick be located the crucible bottom.
Furthermore, the seed crystal is a YCOB single crystal bar, the growth direction is b to [010], the side surface is a YCOB dissociation surface direction [ -201], and the large surface direction of the YCOB crystal plate grown according to the direction is [ -201 ]. Can effectively avoid the growth direction from dissociating and cracking.
A YCOB crystal growth method using the growth apparatus as described above, the method comprising the steps of:
(1) pretreating raw materials, and synthesizing a YCOB raw material by adopting a secondary solid phase method;
(2) charging: filling YCOB raw materials into a crucible in a dry and clean environment, adjusting the distance between seed crystals and a die opening of a crystal growth die, and placing YCOB crushed grains as melting point reference materials at the die opening of the crystal growth die;
(3) and (3) crystal melting: vacuumizing, filling protective gas, heating until the material block is observed to be melted to obtain a raw material melt, and observing a mold seam, namely a feeding seam at the bottom of a V-shaped opening at the top end of the crystal growth mold and a bright melt liquid level line in the bottom; the protective gas is selected from Ar and N2Etc.;
(4) seeding: descending the seed crystal to enable the seed crystal to contact a V-shaped opening on a die opening of a crystal growth die until the lower end of the seed crystal contacts the molten liquid level at the bottom end of the seed crystal, then reducing the temperature, and pulling a seed crystal rod to enable the raw material melt to condense and grow on the seed crystal;
(5) shouldering: after the crystal seeding is finished, reducing the power, entering a shouldering stage, keeping the seed rod pulling rate in the stage, simultaneously reducing the heating power, and gradually thickening and widening the crystal along with the upward pulling process until the width of the crystal reaches the width of a corresponding crystal growth mold;
(6) and (3) an equal-diameter growth stage: after shouldering is finished, the crystal grows in a constant width, namely the design width of the mold, along with pulling of the seed crystal rod; the growth rate is constant in the stage, the high pulling rate is increased until the raw material melt in the crucible is exhausted, the crystal automatically separates from the crystal growth mould, and the crystal growth is finished;
(7) cooling and annealing: and after the crystal growth is finished, cooling and annealing to room temperature.
If a plurality of YCOB crystals are grown by a die-guiding method, the crystal growth die is designed into a multi-slit structure formed by combining a plurality of iridium golden plates, and the YCOB seed crystals are designed into sheet seed crystals which can cover all feeding slits of the die.
Further, the specific steps of the step (1) are as follows:
(1-1) selecting Y with the purity of 99.99%2O3、CaCO3、H3BO3Powder is used as a raw material; firstly, Y is put in2O3、CaCO3Baking the powder at 200-300 ℃ for 8-12h to remove the water adsorbed in the raw material;
(1-2) weighing 3 raw materials, mixing the weighed raw materials for 16-32 hours by a mixer, and pressing into a pressed powder with the diameter of 40-60 mm;
weighing according to the solid phase reaction equation:
0.5Y2O3+4CaCO3+3H3BO3→YCa4O(BO3)3+4.5H2O↑+4CO2↑
in which H is taken into account3BO3Easy volatilization of H3BO3Excess 1-5 at%;
(1-3) placing the powder cake in a crucible, and sintering for 20-30 hours at 1200-1400 ℃ by using a muffle furnace;
(1-4) the sintered compact is reground and pulverized again, and is pressed into a compact again, and then sintering is repeated at 1200-1400 ℃ for 20-30 hours, at which time the solid phase reaction of the raw materials is sufficient, and a phase of YCOB is formed.
Further, the temperature rise rate in the step (3) is 60-100 ℃/h; the pulling rate in the step (4) is 3-5 mm/h; the temperature reduction slope of the heating power reduction in the step (5) is 30-50W/h; the pulling rate in the step (5) is 5-8 mm/h; and (4) the cooling rate of the cooling annealing in the step (7) is 40-60 ℃/h.
Compared with the prior art, the method adopts a mode-guiding method to carry out crystal growth, and the rapid crystallization is carried out in a large-gradient temperature thermal field, so that the rapid growth of the YCOB crystal is realized. The crystal growth has small solid-liquid interface, high crystallization speed and high crystal quality, can carry out shaping and directional growth, and becomes one of the mainstream growth modes of the crystal with the super-large size.
Drawings
FIG. 1 is a schematic view of a crystal growth apparatus according to example 1;
FIG. 2 is an XRD pattern of YCOB crystals grown by the guided mode method in example 1;
the reference numbers in the figures indicate: 1-seed crystal rod, 2-heat preservation upper cover plate, 3-upper heat preservation cover, 4-seed crystal, 5-crucible cover, 6-crucible, 7-crystal growth mold, 8-raw material melt, 9-first side heat preservation cylinder, 10-zirconia ball, 11-second side heat preservation cylinder, 12-induction coil, and 13-bottom heat preservation brick.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
A growth apparatus for growing a YCOB crystal, as shown in fig. 1, the apparatus comprising: a crucible 6 for holding a raw material melt 8 for crystal growth; a crystal growth mould 7 for guiding the flow direction of the raw material melt 8; a seed rod 1 for guiding crystal growth;
the crystal growth mould 7 is arranged in the crucible 6 and is fixed by a mould clamping sleeve, after the raw material in the crucible 6 is melted, the raw material melt 8 rises to the upper surface of the growth mould 7 from the mould slot through the siphon action, and the crystal growth is carried out through the traction of the seed crystal 4; the seed rod 1 is arranged above the growth mould 7 in a way of moving up and down, the lower part of the seed rod 1 is provided with a seed crystal 4 for pulling crystals to grow, and the crucible 6 is externally sleeved with an induction coil 12 for heating the crucible 6 by induction. The device also comprises a heat-insulating container for preventing heat dissipation in the crystal growth process; the crucible 6 is arranged in a heat-insulating container. Zirconia balls 10 for further heat preservation are stacked between the heat preservation container and the crucible 6; the material of the heat preservation container is zirconia ceramics. The crucible 6 is provided with a crucible cover 5.
The crystal growth mold 7 is made of iridium alloy, is formed by combining and welding a plurality of iridium alloy plates and is isolated by iridium strips, the middle gap corresponds to a mold gap for crystal growth, and the top end is provided with a V-shaped opening. The thickness of the grown crystal is limited by the width of the V-shaped opening, and the width of the crystal is limited by the width of the iridium plate; the crucible 6 and the seed rod 1 are both made of iridium; the width of the die slot is 0.3-0.5mm, and the angle of the opening is 100-150 degrees.
The heat preservation container includes heat preservation upper cover plate 2, the last heat preservation cover 3, the side heat preservation section of thick bamboo 9, 11 and the bottom insulating brick 13 of splicing each other, heat preservation upper cover plate 2 be located 6 tops of crucible, first side heat preservation section of thick bamboo 9 and second side heat preservation section of thick bamboo 11 be located 6 sides of crucible, bottom insulating brick 13 be located 6 bottoms of crucible.
The seed crystal 4 is a YCOB single crystal bar, the growth direction is b direction [010], the side surface is YCOB dissociation surface direction [ -201], and the major surface direction of the YCOB crystal plate grown according to the direction is [ -201 ]. Can effectively avoid the growth direction from dissociating and cracking.
The device is used for a chip YCOB die-guiding method crystal growth method, and the method specifically comprises the following steps:
pretreating raw materials in the step (1):
using a secondary solid-phase synthesis method to contract YCOB raw materials, and selecting Y with the purity of 99.99 percent2O3、CaCO3、H3BO3Powder is used as a raw material; firstly, Y is put in2O3、CaCO3The powder is baked for 10 hours at 250 ℃,removing the adsorbed water in the raw material; then according to the solid phase reaction equation: 0.5Y2O3+4CaCO3+3H3BO3→YCa4O(BO3)3+4.5H2O↑+4CO2×) 3 kinds of raw materials were weighed while taking into account H3BO3Easy volatilization of H3BO3An excess of 1-5 at%. Mixing the weighed raw materials for 24 hours by a mixer, and pressing into pressed powder with the diameter of about 50 mm; the pressed powder is placed in an alumina crucible and sintered for 20-30 hours at 1300 ℃ by a muffle furnace.
And (3) regrinding and crushing the sintered compact, pressing the reground compact into a compact, and then repeating the sintering at 1300 ℃ for 20-30 hours, wherein the solid-phase reaction of the raw materials is sufficient, and the phase of the YCOB is basically synthesized.
Step (2) charging: under a dry and clean environment, filling the raw materials into a crucible 6, adjusting the distance between a seed crystal 4 and a die opening of a crystal growth die 7, and placing YCOB crushed crystal grains as melting point reference materials at the die opening;
vacuumizing and filling protective gas, and heating at the speed of 60-100 ℃/h until a material block is observed to be molten, wherein a mold seam can be observed, namely a feeding seam at the bottom of a V-shaped opening at the top end of the mold and a bright molten liquid surface line at the bottom;
seeding in step (4): descending the seed crystal 4 to enable the seed crystal 4 to contact the V-shaped feeding seam on the die opening of the growth die 7 until the lower end of the seed crystal contacts the molten liquid level at the bottom end of the V-shaped feeding seam, then reducing the temperature, pulling the seed crystal rod 1, controlling the pulling speed to be 3-5mm/h, and enabling the raw material to condense and grow on the seed crystal 4;
step (5), shoulder setting: after the crystal seeding is finished, reducing the power, entering a shouldering stage, keeping a low pulling rate in the stage, and simultaneously properly reducing the heating power, wherein the cooling slope is generally 30-50W/h, and the crystal gradually becomes thicker and wider along with the upward pulling process until the width of the wafer reaches the width of the corresponding crystal growth mold 7;
step (6) equal-diameter growth stage: after shouldering is finished, the wafer grows in a constant width, namely the design width of the die, along with the lifting of the seed crystal rod 1; the growth rate at this stage is constant, the high pulling rate is kept, generally 5-8mm/h, until the raw material in the crucible 6 is exhausted, the wafer is automatically separated from the die, and the crystal growth is finished;
step (7), cooling and annealing: and after the crystal growth is finished, cooling annealing is started, wherein the cooling rate is 40-60 ℃/h.
The XRD pattern of the YCOB crystal grown by the guided mode method in this example is shown in FIG. 2, wherein (a) the curve is the XRD pattern of the measured sample, and (b) the curve is the YCOB standard XRD card (number: PDF # 50-0403).
In addition, the long crystal solid-liquid interface in the embodiment is small, and only the area of the die opening is provided; the crystallization speed is high, because the pulling speed is more than 5 mm/h; the crystal quality is high, and the width of the half-height peak of the twin-crystal rocking curve is less than 35%; can be shaped and directionally grown, and can be used for growing sheet, rod and tubular crystals.
In the scope of the invention, a plurality of YCOB crystals are grown by a die-guided growth method, a die is designed into a multi-slit structure formed by combining a plurality of iridium golden plates, and the YCOB seed crystals are designed into sheet seed crystals capable of covering all feeding slits of the die.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. A growth apparatus for growing a YCOB crystal, the apparatus comprising:
a crucible (6) for holding a raw material melt (8) for crystal growth;
a crystal growth mould (7) for guiding the flow direction of the raw material melt (8);
a seed rod (1) for guiding crystal growth;
the crystal growth mould (7) is arranged in the crucible (6); the seed rod (1) is arranged above the growth mould (7) in a vertically movable manner, a seed crystal (4) for pulling the crystal to grow is arranged at the lower part of the seed rod (1), and an induction coil (12) for heating the crucible (6) in an induction manner is sleeved outside the crucible (6).
2. A growth apparatus for YCOB crystal growth according to claim 1, wherein said crystal growth die (7) is made of iridium, and is made of a plurality of pieces of iridium plates welded together and isolated by iridium strips, the middle gap corresponds to the die gap for crystal growth, and the top end is V-shaped and open; the crucible (6) and the seed rod (1) are both made of iridium; the width of the die slot is 0.3-0.5mm, and the angle of the opening is 100-150 degrees.
3. A growth apparatus for growing a YCOB crystal according to claim 1, further comprising a thermal container for avoiding heat dissipation during the crystal growth process; the crucible (6) is arranged in a heat-insulating container.
4. A growth apparatus for YCOB crystal growth according to claim 3, wherein zirconia balls (10) for further keeping temperature are stacked between said heat-keeping container and said crucible (6); the material of the heat preservation container is zirconia ceramics.
5. A growth apparatus for growing YCOB crystals as in claim 1, wherein said crucible (6) is provided with a crucible cover (5).
6. A growth apparatus for YCOB crystal growth according to claim 1, wherein said thermal container comprises a thermal upper cover plate (2), an upper thermal cover (3), side thermal cylinders (9, 11) and bottom thermal bricks (13) which are spliced with each other, said thermal upper cover plate (2) is located above the crucible (6), said side thermal cylinders (9, 11) are located at the side of the crucible (6), said bottom thermal bricks (13) are located at the bottom of the crucible (6).
7. A YCOB crystal growth apparatus according to claim 1, characterized in that said seed crystal (4) is a YCOB single crystal ingot with a growth direction b to [010] and a side in a direction of YCOB dissociation plane [ -201], and the plate of YCOB crystal grown in this direction has a large plane direction of [ -201 ].
8. A YCOB crystal growth method using the growth apparatus of any one of claims 1-7, comprising the steps of:
(1) pretreating raw materials, and synthesizing a YCOB raw material by adopting a secondary solid phase method;
(2) charging: filling YCOB raw materials into a crucible (6) in a dry and clean environment, and adjusting the distance between a seed crystal (4) and a die opening of a crystal growth die (7);
(3) and (3) crystal melting: vacuumizing and filling protective gas, and heating until the material block is observed to be melted to obtain a raw material melt (8);
(4) seeding: descending the seed crystal (4), enabling the seed crystal (4) to be in contact with a V-shaped opening on a die opening of a crystal growth die (7) until the lower end of the seed crystal (4) is in contact with the molten liquid level at the bottom end of the seed crystal (4), then reducing the temperature, and pulling a seed crystal rod (1) to enable a raw material melt (8) to condense and grow on the seed crystal (4);
(5) shouldering: after the crystal seeding is finished, the pulling rate of the seed rod (1) is kept, and meanwhile, the heating power is reduced until the width of the crystal reaches the width of the corresponding crystal growth mold (7);
(6) and (3) an equal-diameter growth stage: after the shouldering is finished, increasing the high pulling rate until the raw material melt (8) in the crucible (6) is exhausted, automatically separating the crystal from the crystal growth mould (7), and finishing the crystal growth;
(7) cooling and annealing: and after the crystal growth is finished, cooling and annealing to room temperature.
9. A YCOB crystal growth apparatus according to claim 8, wherein the specific steps of step (1) are:
(1-1) first, Y2O3、CaCO3Baking the powder at 200-300 ℃ for 8-12h to remove the water adsorbed in the raw material;
(1-2) weighing 3 raw materials, mixing the weighed raw materials for 16-32 hours by a mixer, and pressing into a pressed powder with the diameter of 40-60 mm;
(1-3) placing the powder cake in a crucible, and sintering for 20-30 hours at 1200-1400 ℃ by using a muffle furnace;
(1-4) the sintered compact is reground and pulverized again, and is pressed into a compact again, and then sintering is repeated at 1200-1400 ℃ for 20-30 hours, at which time the solid phase reaction of the raw materials is sufficient, and a phase of YCOB is formed.
10. A growth apparatus for YCOB crystal growth according to claim 8 or 9, wherein said temperature rise rate in step (3) is 60-100 ℃/h; the pulling rate in the step (4) is 3-5 mm/h; the temperature reduction slope of the heating power reduction in the step (5) is 30-50W/h; the pulling rate in the step (5) is 5-8 mm/h; and (4) the cooling rate of the cooling annealing in the step (7) is 40-60 ℃/h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115287744A (en) * | 2022-08-09 | 2022-11-04 | 中国工程物理研究院流体物理研究所 | Preparation method, detection method, calibration experimental device and method of piezoelectric single crystal |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115287744A (en) * | 2022-08-09 | 2022-11-04 | 中国工程物理研究院流体物理研究所 | Preparation method, detection method, calibration experimental device and method of piezoelectric single crystal |
| CN115287744B (en) * | 2022-08-09 | 2023-11-21 | 中国工程物理研究院流体物理研究所 | Preparation method, detection method, calibration experiment device and method of piezoelectric monocrystal |
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