CN110230099B - Preparation method of potassium tantalate niobate crystal with high dielectric constant - Google Patents

Preparation method of potassium tantalate niobate crystal with high dielectric constant Download PDF

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CN110230099B
CN110230099B CN201910348502.6A CN201910348502A CN110230099B CN 110230099 B CN110230099 B CN 110230099B CN 201910348502 A CN201910348502 A CN 201910348502A CN 110230099 B CN110230099 B CN 110230099B
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邱程程
王旭平
刘冰
户延延
禹化健
马玲
张琮
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New Material Institute of Shandong Academy of Sciences
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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
    • 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
    • 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
    • C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor

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Abstract

The invention relates to a high-dielectric-constant potassium tantalate-niobate crystalAnd a preparation method thereof, belonging to the technical field of functional crystal material preparation. The chemical formula of the crystal is as follows: na, Fe: KTa1‑xNbxO3Wherein the Nb content in the crystal component is not more than 0.36xThe invention introduces sodium and iron elements as doping ions, prepares large-size high-quality crystals by determining doping amount, selecting optimal proportion and matching with a special preparation method, has no bubble and cracking phenomenon in the crystals, has good uniformity and greatly improves the crystal quality.

Description

Preparation method of potassium tantalate niobate crystal with high dielectric constant
Technical Field
The invention relates to a preparation method of a potassium tantalate niobate crystal with a high dielectric constant, belonging to the technical field of preparation of functional crystal materials.
Background
Potassium tantalate niobate (KTN) crystal is a famous multifunctional nonlinear optical crystal, and has excellent electrooptical effect and photorefractive effect. The KTN crystal has excellent secondary electro-optic (Kerr) effect, and the Kerr coefficient of the KTN crystal can reach 10-14m2/V2In order of magnitude, the crystal shows more excellent performance in laser modulation than the linear electro-optic crystal which is widely applied at present. The electro-optical modulation device based on the secondary electro-optical effect of the KTN crystal has more advantages in the aspects of reducing the driving voltage and the size of the device, and can meet the requirements of miniaturization and integration development of future laser devices. In general, the higher the dielectric constant of a material, the greater the specific capacitance of the capacitor. Therefore, in order to meet the requirement that the miniaturization and integration of KTN electronic devices are important factors for promoting the development of the electronic industry, the preparation of KTN crystals with high dielectric constants is imperative.
Disclosure of Invention
The invention provides a preparation method of a potassium tantalate niobate crystal with a high dielectric constant, aiming at the requirements of miniaturization and integration of electronic devices. The crystal electro-optic effect is enhanced, the high dielectric constant is compounded, and the requirements of miniaturization and integration of KTN electronic devices are met.
The technical scheme of the invention is as follows:
na, Fe: KTa1-xNbxO3Crystal
The potassium tantalate niobate crystal with high dielectric constant is a sodium and iron co-doped potassium tantalate niobate crystal, and the chemical formula of the crystal is as follows: na, Fe: KTa1-xNbxO3Wherein the Nb content in the crystal component is not more than 0.36xNot more than 0.39, and Curie point at-241-90°CThe crystal above the Curie point is cubic phase, and m3m points are clustered; below the Curie point, the phase changed to tetragonal phase, 4mm point group.
The Na is+The doping concentration of (A) is 2.2-2.8at%, and the Fe3+The doping concentration is 3.1-3.7at%, and the Na+/Fe3+The doping concentration ratio is 0.59-0.90.
II, Na, Fe: KTa1-xNbxO3Method for growing and preparing crystal
The Na, Fe: KTa1-xNbxO3The preparation method of the crystal takes high-purity K2CO3, Nb2O5 and Ta2O5 as raw materials and high-purity Na2O and Fe2O3For doping ions, a pulling method is adopted for growth, a growth device is an induction heating pulling type single crystal furnace, and the crystal growth steps are as follows:
(1) KTa according to the required Na and Fe1-xNbxO3Crystal component, selecting main material K according to KT-KN phase diagram analysis2CO3、Ta2O5、Nb2O5Proportioning, uniformly mixing the raw materials, compacting into blocks, putting the blocks into a Pt crucible, and sintering for 10 hours at 1000 ℃ to obtain a crystal polycrystal material A; taking out the crystal polycrystalline material A, grinding the crystal polycrystalline material A into powder with the granularity of 100nm-120nm, and adding Na according to the doping elements and the doping proportion2O and Fe2O3Compacting again, sintering for 5 hours at 1100 ℃ for secondary sintering to obtain a crystal polycrystal material; taking out the crystal polycrystalline material B, grinding the crystal polycrystalline material B again to powder with the granularity of 150nm-180-nm, compacting again, and sintering at 900 ℃ for 3h to obtain a blocky polycrystalline material C.
(2) In thatAnd growing the crystal in a single crystal pulling furnace. The heating body is a platinum crucible, and the growth atmosphere is oxygen atmosphere. Placing the blocky polycrystalline material C in a platinum crucible, charging, heating to 1000-1100 ℃ to melt the raw material, overheating for 1 hour, then adding seed crystals, and performing processes of seeding, neck closing, shoulder putting, neck growing and the like to obtain Na and Fe: KTa1-xNbxO3According to different crystal components, the crystal growth temperature is 980-1040 ℃, the pulling speed in the equal neck growth process is 0.52-0.57 mm/h, the crystal rotation speed in the equal diameter growth process is 12-16 r/min, and the growth period is 3-4.5 days.
(3) After the crystal growth process is finished, quickly lifting the crystal away from the liquid level of the melt, keeping the temperature for 4-5 hours, and treating Na +/Fe3+Doping Na and Fe with concentration ratio of 0.59-0.728 to KTa1-xNbxO3The temperature can be reduced to room temperature according to the cooling rate of 8-13 ℃/h; for Na+/Fe3+Doping Na and Fe with concentration ratio of 0.729-0.9: KTa1-xNbxO3And cooling to room temperature at a cooling rate of 22-27 ℃ per hour, and taking out the crystal.
In the above preparation method, the grinding particle size of the polycrystalline material A in the step (1) is preferably 110 nm; the grinding particle size of the polycrystalline material A in the step (1) is preferably 170 nm; in the step (2), a cylindrical platinum crucible is preferred, the height of the crucible is preferably 5-7mm higher than the C plane of the blocky polycrystalline material, and the wall thickness of the crucible is preferably 2.5-2.7 mm; in the step (2), a KTN single crystal rod in the c direction is preferably selected as a seed crystal; the pulling speed in the medium neck growth process in the step (2) is preferably 0.55mm/h, and the crystal rotating speed in the constant diameter growth process is preferably 14 r/min.
According to the invention, sodium and iron elements are introduced as doping ions, the doping amount is determined, the optimal proportion is selected, and a special preparation method is matched, so that the large-size high-quality crystal is prepared, no bubble or cracking phenomenon exists in the crystal, the uniformity is good, and the crystal quality is greatly improved; the transmittance of the crystal is high, and the transmission range can cover the wave bands of ultraviolet light, visible light and the like; the dielectric constant of the crystal is greatly improved at room temperature, the requirements of miniaturization and integration of KTN electronic devices are met, and the practicability is high; the preparation method has the advantages of simple operation and low energy consumption, shortens the crystal growth period and greatly improves the production efficiency.
Drawings
FIG. 1, crystal prepared in example 1.
Fig. 2, a transmittance profile of the crystal prepared in example 2.
FIG. 3 shows a plot of the dielectric constant of the crystal prepared in example 4.
Detailed Description
Example 1: na, Fe: KTa0.64Nb0.36O3Crystal
The sodium-iron co-doped potassium tantalate niobate crystal described in this example is Na, Fe: KTa0.64Nb0.36O3Crystals of said Na+The doping concentration of (2.8 at%), the Fe3+The doping concentration was 3.1 at%.
II, Na, Fe: KTa0.64Nb0.36O3Method for growing and preparing crystal
In this example, high-purity K2CO3, Nb2O5 and Ta2O5 were used as raw materials, and high-purity Na was used2O and Fe2O3For doping ions, a pulling method is adopted for growth, a growth device is an induction heating pulling type single crystal furnace, and the crystal growth steps are as follows:
(1) selecting raw materials K according to the proportion2CO3、Ta2O5、Nb2O5Uniformly mixing the raw materials, compacting into blocks, putting the blocks into a Pt crucible, and sintering for 10 hours at 1000 ℃ to obtain a crystal polycrystal material A; taking out the crystal polycrystalline material A, grinding the crystal polycrystalline material A into powder with the granularity of 100nm again, adding Na according to the doping proportion2O and Fe2O3Compacting again, sintering for 5 hours at 1100 ℃ for secondary sintering to obtain a crystal polycrystal material B; taking out the crystal polycrystalline material B, grinding the crystal polycrystalline material B again to powder with the granularity of 180nm, re-compacting, and sintering at 900 ℃ for 3h to obtain a crystal polycrystalline material C.
(2) The crystal growth is carried out in a single crystal pulling furnace. The heating body is a platinum crucible, and the growth atmosphere is oxygen atmosphere. Placing the blocky polycrystalline material C in a platinum crucible, charging, heating to 1100 ℃ to melt the raw material, overheating for 1 hour, adding seed crystals, and seedingNeck-on-shoulder-isocontour growth, to obtain Na, Fe: KTa0.64Nb0.36O3A crystal; the crystal growth temperature is 1040 ℃, the pulling speed in the equal neck growth process is 0.52mm/h, the crystal rotation speed in the equal diameter growth process is 16r/min, and the growth period is 3 days. In the step, a KTN single crystal rod in the c direction is used as a seed crystal.
(3) And (3) after the crystal growth process is finished, quickly lifting the crystal away from the liquid level of the melt, keeping the temperature for 4 hours, cooling to room temperature according to the cooling rate of 27 ℃ per hour, taking out the crystal, cooling to room temperature after the crystal growth is finished, and discharging.
In the preparation method, the cylindrical platinum crucible is selected in the step (2), the height of the crucible is 5mm higher than the C plane of the crystal polycrystalline material, and the wall thickness of the crucible is 2.7 mm.
Example 2:
na, Fe: KTa0.62Nb0.38O3Crystal
The sodium-iron co-doped potassium tantalate niobate crystal described in this example is Na, Fe: KTa0.62Nb0.38O3Crystals of said Na+The doping concentration of (2.6 at%), the Fe3+The doping concentration was 3.7 at%.
II, Na, Fe: KTa0.62Nb0.38O3Method for growing and preparing crystal
In this example, high-purity K2CO3, Nb2O5 and Ta2O5 were used as raw materials, and high-purity Na was used2O and Fe2O3For doping ions, a pulling method is adopted for growth, a growth device is an induction heating pulling type single crystal furnace, and the crystal growth steps are as follows:
(1) selecting raw materials K according to the proportion2CO3、Ta2O5、Nb2O5Uniformly mixing the raw materials, compacting into blocks, putting the blocks into a Pt crucible, and sintering for 10 hours at 1000 ℃ to obtain a crystal polycrystal material A; taking out the crystal polycrystalline material A, grinding the crystal polycrystalline material A into powder with the granularity of 120nm again, adding Na according to the doping proportion2O and Fe2O3Compacting again, sintering for 5 hours at 1100 ℃ for secondary sintering to obtain a crystal polycrystal material B; taking out the crystal polycrystalline material B and grinding the crystal polycrystalline material B into powder with the granularity of150nm, recompacted and sintered for 3h at 900 ℃ to obtain the crystal polycrystal material C.
(2) The crystal growth is carried out in a single crystal pulling furnace. The heating body is a platinum crucible, and the growth atmosphere is oxygen atmosphere. Placing the blocky polycrystalline material C in a platinum crucible, charging, heating to 1000 ℃ to melt the raw material, overheating for 1 hour, then putting seed crystals, and obtaining Na and Fe through the processes of seeding, neck closing, shoulder putting, neck growing and the like: KTa0.62Nb0.38O3A crystal; the crystal growth temperature is 1000 ℃, the pulling speed in the constant neck growth process is 0.57mm/h, the crystal rotation speed in the constant diameter growth process is 12r/min, and the growth period is 4.5 days. In the step, a KTN single crystal rod in the c direction is used as a seed crystal.
(3) And (5) after the crystal growth process is finished, quickly lifting the crystal away from the liquid level of the melt, keeping the temperature for 5 hours, cooling the crystal to room temperature according to the cooling rate of 13 ℃/h, and discharging the crystal out of the furnace.
In the preparation method, a cylindrical platinum crucible is selected in the step (2), the height of the crucible is 6mm higher than the C plane of the crystal polycrystalline material, and the wall thickness of the crucible is 2.5 mm;
example 3:
na, Fe: KTa0.61Nb0.39O3Crystal
The sodium-iron co-doped potassium tantalate niobate crystal described in this example is Na, Fe: KTa0.61Nb0.39O3Crystals of said Na+The doping concentration of (2.4 at%), the Fe3+The doping concentration was 3.5 at%.
II, Na, Fe: KTa0.61Nb0.39O3Method for growing and preparing crystal
In this example, high-purity K2CO3, Nb2O5 and Ta2O5 were used as raw materials, and high-purity Na was used2O and Fe2O3For doping ions, a pulling method is adopted for growth, a growth device is an induction heating pulling type single crystal furnace, and the crystal growth steps are as follows:
(1) selecting raw materials K according to the proportion2CO3、Ta2O5、Nb2O5Mixing the raw materials uniformly, compacting into blocks, putting the blocks into a Pt crucible, and sintering for 10 hours at 1000 DEG CThen obtaining a crystal polycrystal material A; taking out the crystal polycrystalline material A, grinding the crystal polycrystalline material A into powder with the granularity of 110nm again, adding Na according to the doping proportion2O and Fe2O3Compacting again, sintering for 5 hours at 1100 ℃ for secondary sintering to obtain a crystal polycrystal material B; taking out the crystal polycrystalline material B, grinding the crystal polycrystalline material B again to powder with the granularity of 170nm, compacting again, and sintering at 900 ℃ for 3h to obtain a crystal polycrystalline material C.
(2) The crystal growth is carried out in a single crystal pulling furnace. The heating body is a platinum crucible, and the growth atmosphere is oxygen atmosphere. Placing the blocky polycrystalline material C in a platinum crucible, charging, heating to 1050 ℃ to melt the raw material, overheating for 1 hour, then putting seed crystals, and obtaining Na and Fe through the processes of seeding, neck closing, shoulder putting, neck growing and the like: KTa0.61Nb0.39O3A crystal; the crystal growth temperature is 980 ℃, the pulling speed in the constant neck growth process is 0.55mm/h, the crystal rotation speed in the constant diameter growth process is 14r/min, and the growth cycle is 4 days. In the step, a KTN single crystal rod in the c direction is used as a seed crystal.
(3) And (3) after the crystal growth process is finished, quickly lifting the crystal away from the liquid level of the melt, keeping the temperature for 5 hours, cooling the crystal to room temperature according to the cooling rate of 8 ℃ per hour, and discharging the crystal out of the furnace.
In the preparation method, the cylindrical platinum crucible is selected in the step (2), the height of the crucible is 7mm higher than the C plane of the crystal polycrystalline material, and the wall thickness of the crucible is 2.6 mm.
Example 4:
na, Fe: KTa0.63Nb0.37O3Crystal
The sodium-iron co-doped potassium tantalate niobate crystal described in this example is Na, Fe: KTa0.63Nb0.37O3Crystals of said Na+The doping concentration of (2.7 at%), the Fe3+The doping concentration was 3.2 at%.
II, Na, Fe: KTa0.63Nb0.37O3Method for growing and preparing crystal
In this example, high-purity K2CO3, Nb2O5 and Ta2O5 were used as raw materials, and high-purity Na was used2O and Fe2O3For doping ions, the crystal is grown by Czochralski method with induction as growth deviceThe crystal growth steps of the heating and pulling type single crystal furnace are as follows:
(1) selecting raw materials K according to the proportion2CO3、Ta2O5、Nb2O5Uniformly mixing the raw materials, compacting into blocks, putting the blocks into a Pt crucible, and sintering for 10 hours at 1000 ℃ to obtain a crystal polycrystal material A; taking out the crystal polycrystalline material A, grinding the crystal polycrystalline material A into powder with the granularity of 110nm again, adding Na according to the doping proportion2O and Fe2O3Compacting again, sintering for 5 hours at 1100 ℃ for secondary sintering to obtain a crystal polycrystal material B; taking out the crystal polycrystalline material B, grinding the crystal polycrystalline material B again to powder with the granularity of 160nm, compacting again, and sintering at 900 ℃ for 3h to obtain a crystal polycrystalline material C.
(2) The crystal growth is carried out in a single crystal pulling furnace. The heating body is a platinum crucible, and the growth atmosphere is oxygen atmosphere. Placing the blocky polycrystalline material C in a platinum crucible, charging, heating to 1050 ℃ to melt the raw material, overheating for 1 hour, then putting seed crystals, and obtaining Na and Fe through the processes of seeding, neck closing, shoulder putting, neck growing and the like: KTa0.63Nb0.37O3A crystal; the crystal growth temperature is 980 ℃, the pulling speed in the constant neck growth process is 0.54mm/h, the crystal rotation speed in the constant diameter growth process is 13r/min, and the growth cycle is 3 days. In the step, a KTN single crystal rod in the c direction is used as a seed crystal.
(3) And (3) after the crystal growth process is finished, quickly lifting the crystal away from the liquid level of the melt, keeping the temperature for 5 hours, cooling the crystal to room temperature according to the cooling rate of 24 ℃/h, and discharging the crystal out of the furnace.
In the preparation method, the cylindrical platinum crucible is selected in the step (2), the height of the crucible is 7mm higher than the C plane of the crystal polycrystalline material, and the wall thickness of the crucible is 2.6 mm.

Claims (4)

1. A high dielectric constant potassium tantalate niobate crystal is characterized in that: the chemical formula of the crystal is as follows: na, Fe: KTa1- xNbxO3Wherein x is more than or equal to 0.36 and less than or equal to 0.38 in the crystal component, the Curie point is between-241 and 90 ℃, the crystal above the Curie point is a cubic phase, and m3m points are clustered; below the Curie point, the phase changes into a tetragonal phase, and the point group is 4 mm; the Na is+The doping concentration of (A) is 2.2-2.8at%, and the Fe3+The doping concentration is 3.1-3.7at%, and the Na+/Fe3+The doping concentration ratio is 0.59-0.90.
2. A method for producing the potassium tantalate niobate crystal of claim 1, comprising: the preparation method of the potassium tantalate niobate crystal adopts high-purity K2CO3、Nb2O5、Ta2O5As raw material, high-purity Na2O and Fe2O3For doping ions, a pulling method is adopted for growth, a growth device is an induction heating pulling type single crystal furnace, and the crystal growth steps are as follows:
(1) according to the required Na, Fe: KTa1-xNbxO3Crystal component, selecting main material K according to KT-KN phase diagram analysis2CO3、Ta2O5、Nb2O5Proportioning, uniformly mixing the raw materials, compacting into blocks, putting the blocks into a Pt crucible, and sintering for 10 hours at 1000 ℃ to obtain a crystal polycrystal material A; taking out the crystal polycrystalline material A, grinding the crystal polycrystalline material A into powder with the granularity of 100nm-120nm, and adding Na according to the doping elements and the doping proportion2O and Fe2O3Compacting again, sintering for 5 hours at 1100 ℃ for secondary sintering to obtain a crystal polycrystal material B; taking out the crystal polycrystalline material B, grinding the crystal polycrystalline material B again to powder with the granularity of 150nm-180nm, compacting again, and sintering at 900 ℃ for 3h to obtain a blocky polycrystalline material C;
(2) growing crystals in a single crystal pulling furnace, wherein a heating body is a platinum crucible, and the growing atmosphere is oxygen atmosphere; placing the blocky polycrystalline material C in a platinum crucible, charging, heating to 1000-1100 ℃ to melt the raw material, overheating for 1 hour, then adding seed crystals, and performing processes of seeding, neck closing, shoulder putting, neck growing and the like to obtain Na and Fe: KTa1-xNbxO3According to different crystal components, the crystal growth temperature is 980-1040 ℃, the pulling speed in the equal neck growth process is 0.52-0.57 mm/h, the crystal rotation speed in the equal diameter growth process is 12-16 r/min, and the growth cycle is 3-4.5 days;
(3) after the crystal growth process is finished, the crystal is quickly lifted away from the liquid level of the melt,keeping the temperature for 4-5 hours for Na+/Fe3+A doping concentration ratio of 0.59 to 0.728 of Na, Fe: KTa1-xNbxO3The temperature can be reduced to room temperature according to the cooling rate of 8-13 ℃/h; and for Na+/Fe3+Doping concentration ratio of 0.729-0.9 of Na, Fe: KTa1-xNbxO3And cooling to room temperature at a cooling rate of 22-27 ℃/h, and taking out the crystal.
3. The method of claim 2, wherein: the grinding granularity of the polycrystalline material A in the step (1) is 110nm, and the grinding granularity of the polycrystalline material B in the step (1) is 170 nm.
4. The production method according to claim 3, characterized in that: the step (2) is a cylindrical platinum crucible, the height of the crucible is 5-7mm higher than the C plane of the blocky polycrystalline material, and the wall of the crucible is 2.5-2.7 mm; taking a KTN single crystal rod in the c direction as a seed crystal in the step (2); in the step (2), the pulling speed in the medium neck growth process is 0.55mm/h, and the crystal rotating speed in the constant diameter growth process is 14 r/min.
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