CN110230099A - A kind of high dielectric constant potassium tantalate-niobate crystal preparation method - Google Patents
A kind of high dielectric constant potassium tantalate-niobate crystal preparation method Download PDFInfo
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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
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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
- 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
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- C30B29/30—Niobates; Vanadates; Tantalates
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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 present invention relates to a kind of high dielectric constant potassium tantalate-niobate crystal and preparation method thereof, belong to functional crystal material preparation technical field.The chemical formula of the crystal are as follows: Na, Fe:KTa1‑xNbxO3, wherein in crystal composition Nb content be 0.36≤x≤ 0.39, the present invention is by introducing sodium, ferro element as Doped ions, by determining doping, optimum ratio is selected, cooperates dedicated preparation method, is prepared for large-size high-quality crystal, bubble-free and cracking phenomena in crystal, uniformity is good, substantially improves crystal quality.
Description
Technical field
The present invention relates to a kind of high dielectric constant potassium tantalate-niobate crystal preparation methods, belong to functional crystal material technology of preparing
Field.
Background technique
Potassium tantalate-niobate (KTN) crystal is a kind of famous multi-functional nonlinear optical crystal, is imitated with excellent electric light
Should and photorefractive effect.KTN crystal has excellent secondary electric light (Kerr) effect, and Kerr coefficient is up to 10-14m2/V2Amount
Grade, the crystal show performance more more excellent than the linear electrooptic crystal being widely used at present in terms of Laser Modulation.It is based on
The electro-optical modulation device of KTN crystal quadratic electro-optical effect has more advantage in terms of reducing driving voltage, reducing device size, more can
Meet the needs of the following laser device miniaturization, integrated development.In general, the dielectric constant of material is higher, capacitor
Specific capacitance is bigger.Therefore in order to meet KTN electronic device miniaturization, it is integrated be push electronic industry development it is important because
Element, preparing has the KTN crystal of high dielectric constant imperative.
Summary of the invention
The present invention is directed to electronics miniaturization, integrated demand, provides a kind of high dielectric constant potassium tantalate-niobate crystal
Preparation method.The enhancing of crystal electrooptic effect of the present invention and high dielectric constant it is compound, meet the small-sized of KTN electronic device
Change, integrated requirement.
Technical scheme is as follows:
One, Na, Fe:KTa1-xNbxO3Crystal
High dielectric constant potassium tantalate-niobate crystal of the present invention is sodium, iron is co-doped with potassium tantalate-niobate crystal, the change of the crystal
Formula are as follows: Na, Fe:KTa1-xNbxO3, wherein in crystal composition Nb content be 0.36≤x≤ 0.39, curie point is located at -241 ~ 90° CBetween, it is cubic phase, m3m point group in the above crystal of curie point；Become tetragonal phase, 4mm point group below curie point.
The Na+Doping concentration be 2.2-2.8at%, the Fe3+Doping concentration is 3.1-3.7at%, the Na+/Fe3+Doping concentration ratio 0.59-0.90.
Two, Na, Fe:KTa1-xNbxO3The growth and preparation method of crystal
Na of the present invention, Fe:KTa1-xNbxO3The preparation method of crystal is original with high-purity K2CO3, Nb2O5, Ta2O5
Material, with high-purity N a2O and Fe2O3For Doped ions, using Czochralski grown, grower is induction heating pull-type monocrystalline
Furnace, crystal growth step are as follows:
(1) according to required Na, Fe:KTa1-xNbxO3Crystal composition selects main material K according to KT-KN Phase Diagram Analysis2CO3、
Ta2O5、Nb2O5Raw material is uniformly mixed and is compacted blocking, is put into Pt crucible by proportion, 1000 DEG C sintering 10 hours, obtain crystalline substance
Body polycrystal material A；Taking out crystalline polymorphic material A and re-grinding into powder size is 100nm-120nm, according to doped chemical and doping ratio
Na is added in example2O and Fe2O3, it is compacted again, in 1100 DEG C of sintering, 5 hours progress double sinterings, obtains crystalline polymorphic material；It takes
It is 150nm-180-nm that crystalline polymorphic material B, which re-grinds into powder size, out, is compacted again, in 900 DEG C of sintering 3h, obtains bulk
Polycrystal material C.
(2) crystal growth is carried out in single crystal pulling furnace.Calandria is platinum crucible, and growth atmosphere is oxygen atmosphere.It will
Bulk polycrystal material C is placed in platinum crucible, and after shove charge, being warming up to 1000 ~ 1100 DEG C melts raw material, tripping in after overheat 1 hour
Seed crystal, neck-shouldering-of being sowed-received wait the processes such as necks growth, obtain Na, Fe:KTa1-xNbxO3Crystal, not according to crystal composition
Together, for crystal growth temperature between 980 ~ 1040 DEG C, waiting pull rate when necks growth course is 0.52 ~ 0.57mm/h, etc.
Diameter growth process crystal rotation be 12 ~ 16r/min, growth cycle 3-4.5 days.
(3) crystal growing process terminates, quickly by crystal lift-off melt liquid level, constant temperature 4 ~ 5 hours, and for Na+/Fe3+
Doping concentration is than the Na for 0.59-0.728, Fe:KTa1-xNbxO3, room can be down to always according to the rate of temperature fall of 8 ~ 13 °C/h
Temperature；And for for Na+/Fe3+Doping concentration is than the Na for 0.729-0.9, Fe:KTa1-xNbxO3, can be according to 22 ~ 27 °C/h
Rate of temperature fall be down to room temperature always, take out crystal afterwards.
In above-mentioned preparation method, the preferred 110nm of grind size of polycrystal material A in step (1)；Polycrystal material A in step (1)
The preferred 170nm of grind size；Preferred tubular platinum crucible in step (2), the crucible is highly preferred to be higher than bulk polycrystal material C
Plane 5-7mm, the preferred 2.5-2.7mm of crucible wall thickness；The preferred direction c KTN monocrystal rod is as seed crystal in step (2)；Step
Suddenly pull rate when (2) medium neck growth course is preferably 0.55mm/h, and isodiametric growth process crystal rotation is preferably 14r/
min。
The present invention selects optimum ratio, cooperation by determining doping by introducing sodium, ferro element as Doped ions
Dedicated preparation method is prepared for large-size high-quality crystal, and bubble-free and cracking phenomena in crystal, uniformity is good, changes significantly
It has been apt to crystal quality；The transmitance of crystal is higher, can cover the wave bands such as ultraviolet, visible light through range；At room temperature, crystalline dielectric
Constant increases substantially, and meets miniaturization, the integrated requirement of KTN electronic device, practical；The operation of this preparation method
Simply, low energy consumption, shortens crystal growth cycles, substantially increases production efficiency.
Detailed description of the invention
Crystal prepared by Fig. 1, the present embodiment 1.
The transmitance map of crystal prepared by Fig. 2, the present embodiment 2.
Jie's temperature constant map of crystal prepared by Fig. 3, the present embodiment 4.
Specific embodiment
Embodiment 1: one, Na, Fe:KTa0.64Nb0.36O3Crystal
It is Na, Fe:KTa that sodium described in the present embodiment, iron, which are co-doped with potassium tantalate-niobate crystal,0.64Nb0.36O3Crystal, the Na+Doping
Concentration is 2.8at%, the Fe3+Doping concentration is 3.1at%.
Two, Na, Fe:KTa0.64Nb0.36O3The growth and preparation method of crystal
The present embodiment is using high-purity K2CO3, Nb2O5, Ta2O5 as raw material, with high-purity N a2O and Fe2O3For Doped ions, adopt
With Czochralski grown, grower is induction heating pull-type single crystal growing furnace, and crystal growth step is as follows:
(1) raw material K is selected in proportion2CO3、Ta2O5、Nb2O5, raw material is uniformly mixed and is compacted blocking, is put into Pt crucible,
1000 DEG C are sintered 10 hours, obtain crystalline polymorphic material A；Taking out crystalline polymorphic material A and re-grinding into powder size is 100nm, is pressed
Na is added according to doping ratio2O and Fe2O3, it is compacted again, in 1100 DEG C of sintering, 5 hours progress double sinterings, it is more obtains crystal
Crystalline substance material B；Taking out crystalline polymorphic material B and re-grinding into powder size is 180nm, is compacted again, in 900 DEG C of sintering 3h, obtains crystalline substance
Body polycrystal material C.
(2) crystal growth is carried out in single crystal pulling furnace.Calandria is platinum crucible, and growth atmosphere is oxygen atmosphere.It will
Bulk polycrystal material C is placed in platinum crucible, and after shove charge, being warming up to 1100 DEG C melts raw material, tripping in seed crystal after overheat 1 hour,
Neck-shouldering-of being sowed-received waits the processes such as necks growth, obtains Na, Fe:KTa0.64Nb0.36O3Crystal；Crystal growth temperature is
1040 DEG C, waiting pull rate when necks growth course is 0.52mm/h, and isodiametric growth process crystal rotation is 16r/min, growth
Period 3 days.Using the direction c KTN monocrystal rod as seed crystal in this step.
(3) crystal growing process terminates, quickly by crystal lift-off melt liquid level, constant temperature 4 hours, and according to 27 °C/h's
Rate of temperature fall is down to always room temperature, takes out crystal afterwards, and crystal growth, which finishes, is cooled to room temperature, comes out of the stove.
In above-mentioned preparation method, step (2) selects tubular platinum crucible, and the crucible height is higher than crystalline polymorphic material C
Plane 5mm, the crucible wall thickness 2.7mm.
Embodiment 2:
One, Na, Fe:KTa0.62Nb0.38O3Crystal
It is Na, Fe:KTa that sodium described in the present embodiment, iron, which are co-doped with potassium tantalate-niobate crystal,0.62Nb0.38O3Crystal, the Na+Doping
Concentration is 2.6at%, the Fe3+Doping concentration is 3.7at%.
Two, Na, Fe:KTa0.62Nb0.38O3The growth and preparation method of crystal
The present embodiment is using high-purity K2CO3, Nb2O5, Ta2O5 as raw material, with high-purity N a2O and Fe2O3For Doped ions, adopt
With Czochralski grown, grower is induction heating pull-type single crystal growing furnace, and crystal growth step is as follows:
(1) raw material K is selected in proportion2CO3、Ta2O5、Nb2O5, raw material is uniformly mixed and is compacted blocking, is put into Pt crucible,
1000 DEG C are sintered 10 hours, obtain crystalline polymorphic material A；Taking out crystalline polymorphic material A and re-grinding into powder size is 120nm, is pressed
Na is added according to doping ratio2O and Fe2O3, it is compacted again, in 1100 DEG C of sintering, 5 hours progress double sinterings, it is more obtains crystal
Crystalline substance material B；Taking out crystalline polymorphic material B and re-grinding into powder size is 150nm, is compacted again, in 900 DEG C of sintering 3h, obtains crystalline substance
Body polycrystal material C.
(2) crystal growth is carried out in single crystal pulling furnace.Calandria is platinum crucible, and growth atmosphere is oxygen atmosphere.It will
Bulk polycrystal material C is placed in platinum crucible, and after shove charge, being warming up to 1000 DEG C melts raw material, tripping in seed crystal after overheat 1 hour,
Neck-shouldering-of being sowed-received waits the processes such as necks growth, obtains Na, Fe:KTa0.62Nb0.38O3Crystal；Crystal growth temperature is
1000 DEG C, waiting pull rate when necks growth course is 0.57mm/h, and isodiametric growth process crystal rotation is 12r/min, growth
Period 4.5 days.Using the direction c KTN monocrystal rod as seed crystal in this step.
(3) crystal growing process terminates, quickly by crystal lift-off melt liquid level, constant temperature 5 hours, and according to 13 °C/h's
Rate of temperature fall is down to always room temperature, comes out of the stove.
In above-mentioned preparation method, step (2) selects tubular platinum crucible, and the crucible height is higher than crystalline polymorphic material C
Plane 6mm, the crucible wall thickness 2.5mm；
Embodiment 3:
One, Na, Fe:KTa0.61Nb0.39O3Crystal
It is Na, Fe:KTa that sodium described in the present embodiment, iron, which are co-doped with potassium tantalate-niobate crystal,0.61Nb0.39O3Crystal, the Na+Doping
Concentration is 2.4at%, the Fe3+Doping concentration is 3.5at%.
Two, Na, Fe:KTa0.61Nb0.39O3The growth and preparation method of crystal
The present embodiment is using high-purity K2CO3, Nb2O5, Ta2O5 as raw material, with high-purity N a2O and Fe2O3For Doped ions, adopt
With Czochralski grown, grower is induction heating pull-type single crystal growing furnace, and crystal growth step is as follows:
(1) raw material K is selected in proportion2CO3、Ta2O5、Nb2O5, raw material is uniformly mixed and is compacted blocking, is put into Pt crucible,
1000 DEG C are sintered 10 hours, obtain crystalline polymorphic material A；Taking out crystalline polymorphic material A and re-grinding into powder size is 110nm, is pressed
Na is added according to doping ratio2O and Fe2O3, it is compacted again, in 1100 DEG C of sintering, 5 hours progress double sinterings, it is more obtains crystal
Crystalline substance material B；Taking out crystalline polymorphic material B and re-grinding into powder size is 170nm, is compacted again, in 900 DEG C of sintering 3h, obtains crystalline substance
Body polycrystal material C.
(2) crystal growth is carried out in single crystal pulling furnace.Calandria is platinum crucible, and growth atmosphere is oxygen atmosphere.It will
Bulk polycrystal material C is placed in platinum crucible, and after shove charge, being warming up to 1050 DEG C melts raw material, tripping in seed crystal after overheat 1 hour,
Neck-shouldering-of being sowed-received waits the processes such as necks growth, obtains Na, Fe:KTa0.61Nb0.39O3Crystal；Crystal growth temperature is
980 DEG C, waiting pull rate when necks growth course is 0.55mm/h, and isodiametric growth process crystal rotation is 14r/min, growth
Period 4 days.Using the direction c KTN monocrystal rod as seed crystal in this step.
(3) crystal growing process terminates, quickly by crystal lift-off melt liquid level, constant temperature 5 hours, and according to 8 °C/h's
Rate of temperature fall is down to always room temperature, comes out of the stove.
In above-mentioned preparation method, step (2) selects tubular platinum crucible, and the crucible height is higher than crystalline polymorphic material C
Plane 7mm, the crucible wall thickness 2.6mm.
Embodiment 4:
One, Na, Fe:KTa0.63Nb0.37O3Crystal
It is Na, Fe:KTa that sodium described in the present embodiment, iron, which are co-doped with potassium tantalate-niobate crystal,0.63Nb0.37O3Crystal, the Na+Doping
Concentration is 2.7at%, the Fe3+Doping concentration is 3.2at%.
Two, Na, Fe:KTa0.63Nb0.37O3The growth and preparation method of crystal
The present embodiment is using high-purity K2CO3, Nb2O5, Ta2O5 as raw material, with high-purity N a2O and Fe2O3For Doped ions, adopt
With Czochralski grown, grower is induction heating pull-type single crystal growing furnace, and crystal growth step is as follows:
(1) raw material K is selected in proportion2CO3、Ta2O5、Nb2O5, raw material is uniformly mixed and is compacted blocking, is put into Pt crucible,
1000 DEG C are sintered 10 hours, obtain crystalline polymorphic material A；Taking out crystalline polymorphic material A and re-grinding into powder size is 110nm, is pressed
Na is added according to doping ratio2O and Fe2O3, it is compacted again, in 1100 DEG C of sintering, 5 hours progress double sinterings, it is more obtains crystal
Crystalline substance material B；Taking out crystalline polymorphic material B and re-grinding into powder size is 160nm, is compacted again, in 900 DEG C of sintering 3h, obtains crystalline substance
Body polycrystal material C.
(2) crystal growth is carried out in single crystal pulling furnace.Calandria is platinum crucible, and growth atmosphere is oxygen atmosphere.It will
Bulk polycrystal material C is placed in platinum crucible, and after shove charge, being warming up to 1050 DEG C melts raw material, tripping in seed crystal after overheat 1 hour,
Neck-shouldering-of being sowed-received waits the processes such as necks growth, obtains Na, Fe:KTa0.63Nb0.37O3Crystal；Crystal growth temperature is
980 DEG C, waiting pull rate when necks growth course is 0.54mm/h, and isodiametric growth process crystal rotation is 13r/min, growth
Period 3 days.Using the direction c KTN monocrystal rod as seed crystal in this step.
(3) crystal growing process terminates, quickly by crystal lift-off melt liquid level, constant temperature 5 hours, and according to 24 °C/h's
Rate of temperature fall is down to always room temperature, comes out of the stove.
In above-mentioned preparation method, step (2) selects tubular platinum crucible, and the crucible height is higher than crystalline polymorphic material C
Plane 7mm, the crucible wall thickness 2.6mm.
Claims (4)
1. a kind of high dielectric constant potassium tantalate-niobate crystal, it is characterised in that: the chemical formula of the crystal are as follows: Na, Fe:KTa1- xNbxO3, wherein in crystal composition Nb content be 0.36≤x≤ 0.39, curie point is located at -241 ~ 90°CBetween, curie point with
Upper crystal is cubic phase, m3m point group；Become tetragonal phase, 4mm point group below curie point；The Na+Doping concentration be 2.2-
2.8at%, the Fe3+Doping concentration is 3.1-3.7at%, the Na+/Fe3+Doping concentration ratio 0.59-0.90.
2. a kind of method for preparing potassium tantalate-niobate crystal described in claim 1, it is characterised in that: the potassium tantalate-niobate crystal
Preparation method, using high-purity K2CO3, Nb2O5, Ta2O5 as raw material, with high-purity N a2O and Fe2O3For Doped ions, use
Czochralski grown, grower are induction heating pull-type single crystal growing furnace, and crystal growth step is as follows:
(1) according to required Na, Fe:KTa1-xNbxO3Crystal composition selects main material K according to KT-KN Phase Diagram Analysis2CO3、
Ta2O5、Nb2O5Raw material is uniformly mixed and is compacted blocking, is put into Pt crucible by proportion, 1000 DEG C sintering 10 hours, obtain crystalline substance
Body polycrystal material A；Taking out crystalline polymorphic material A and re-grinding into powder size is 100nm-120nm, according to doped chemical and doping ratio
Na is added in example2O and Fe2O3, it is compacted again, in 1100 DEG C of sintering, 5 hours progress double sinterings, obtains crystalline polymorphic material；It takes
It is 150nm-180-nm that crystalline polymorphic material B, which re-grinds into powder size, out, is compacted again, in 900 DEG C of sintering 3h, obtains bulk
Polycrystal material C；
(2) crystal growth is carried out in single crystal pulling furnace；Calandria is platinum crucible, and growth atmosphere is oxygen atmosphere；It will be blocky
Polycrystal material C is placed in platinum crucible, and after shove charge, being warming up to 1000 ~ 1100 DEG C melts raw material, tripping in seed after overheat 1 hour
Crystalline substance, neck-shouldering-of being sowed-received wait the processes such as necks growth, obtain Na, Fe:KTa1-xNbxO3Crystal, it is different according to crystal composition,
For crystal growth temperature between 980 ~ 1040 DEG C, waiting pull rate when necks growth course is 0.52 ~ 0.57mm/h, isometrical life
Growth process crystal rotation be 12 ~ 16r/min, growth cycle 3-4.5 days；
(3) crystal growing process terminates, quickly by crystal lift-off melt liquid level, constant temperature 4 ~ 5 hours, and for Na+/Fe3+Doping
Concentration is than the Na for 0.59-0.728, Fe:KTa1-xNbxO3, room temperature can be down to always according to the rate of temperature fall of 8 ~ 13 °C/h；
And for for Na+/Fe3+Doping concentration is than the Na for 0.729-0.9, Fe:KTa1-xNbxO3, can be according to 22 ~ 27 °C/h's
Rate of temperature fall is down to always room temperature, takes out crystal afterwards.
3. preparation method according to claim 2, it is characterised in that: the grind size of polycrystal material A in the step (1)
For 110nm；The grind size 170nm of polycrystal material B in step (1).
4. preparation method according to claim 3, it is characterised in that: crucible is tubular platinum crucible in step (2), described
Crucible height be higher than bulk polycrystal material C plane 5-7mm, the crucible wall thickness be 2.5-2.7mm；The side c is used in step (2)
To KTN monocrystal rod as seed crystal；Pull rate when the medium neck growth course of step (2) is 0.55mm/h, isodiametric growth process
Crystal rotation is 14r/min.
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| CN114280136A (en) * | 2021-12-28 | 2022-04-05 | 江西理工大学 | Preparation method of scheelite main trace element micro-area analysis quantitative correction standard substance |
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