CN110241456A - The method that flux method grows uniform near-stoichiometric lithium tantalate crystals - Google Patents
The method that flux method grows uniform near-stoichiometric lithium tantalate crystals Download PDFInfo
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- CN110241456A CN110241456A CN201910626550.7A CN201910626550A CN110241456A CN 110241456 A CN110241456 A CN 110241456A CN 201910626550 A CN201910626550 A CN 201910626550A CN 110241456 A CN110241456 A CN 110241456A
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- lithium tantalate
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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
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
- C30B9/12—Salt solvents, e.g. flux growth
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- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A kind of method that flux method grows uniform near-stoichiometric lithium tantalate crystals includes the following steps: Li in molar ratio2CO ︰ Ta2O5︰ K2CO3Ratio for 48.75 ︰, 51.25 ︰ 13 is made into base-material, and above-mentioned base-material ground and mixed is then reheated mixture, so that CO at mixture2It decomposites and, then calcine the mixture again, obtain lithium tantalate polycrystal material, finally lithium tantalate polycrystal material is compacted, and is fitted into crucible, molten condition is heated to, after held for some time, near-stoichiometric lithium tantalate crystals are made with czochralski method, use Li in the present invention2CO3、Ta2O5With cosolvent K2CO3Molar ratio is the ratio of 48.75 ︰, 51.25 ︰ 13, and the head of the LT crystal of preparation and the Curie temperature difference of tail portion are mutated, touch the bottom, and obtains uniform near stoichiometric proportion L T crystal up and down.
Description
Technical field
The present invention relates to lithium tantalate preparation technical field, in particular to uniformly nearly chemistry is counted for a kind of flux method growth
Measure the method than lithium tantalate.
Background technique
Lithium tantalate (LiTaO3, abbreviation LT) and crystal and lithium niobate (LiNbO3, abbreviation LN) and isostructural.LT crystal is a kind of
The important crystalline material with multifunction piezoelectric actuator, ferroelectricity and electric light, acousto-optic, non-linear, Preset grating and laser active,
It is the artificial lens that a kind of optical property is more, overall target is good.Similar with LN crystal, LT crystal is also a kind of non-stoichiometric
Oxide, with the raising of [Li] in crystal/[Ta] ratio, the performance of crystal is improved.But due to the fusing point of LT crystal compared with
High (1600 °C), growth ratio LN are difficult.
Flux growth metrhod is the growth more common method of LT and LN crystal, the growth of near stoichiometric proportion LT and LN crystal
Cheng Zhong, it in crystal melt by being added a certain amount of fluxing agent (K of certain mol proportion2O it) adjusts its fusing point and obtains closeization
Metering is learned than LT and LN crystal.Its advantage is that growth technique is close with congruent crystal is grown, technology difficulty is small, but the disadvantage is that by
In K2O does not enter crystal substantially, and the ratio of fluxing agent gradually rises, and the component of melt constantly changes with the growth of crystal, therefore
It is difficult to obtain uniform near stoichiometric proportion LT and LN crystal up and down.
Summary of the invention
In view of this, in view of the above deficiencies, it is necessary to it is brilliant to propose that a kind of energy obtains uniform near stoichiometric proportion LT up and down
The method that the flux method of body grows uniform near-stoichiometric lithium tantalate crystals.
A kind of method that flux method grows uniform near-stoichiometric lithium tantalate crystals, includes the following steps:
Step 1: Li in molar ratio2CO ︰ Ta2O5︰ K2CO3Ratio for 48.75 ︰, 51.25 ︰ 13 is made into base-material；
Step 2: by above-mentioned base-material ground and mixed at mixture；
Step 3: heating mixture, so that CO2It decomposites and, then calcine the mixture again, obtain lithium tantalate polycrystal material；
Step 4: lithium tantalate polycrystal material being compacted, and is fitted into crucible, is heated to molten condition, after held for some time, with mentioning
Near-stoichiometric lithium tantalate crystals are made in daraf(reciprocal of farad).
Preferably, before step 1, the Li2CO3Powder, Ta2O5Powder and K2CO3Powder will also be by the step of drying
Suddenly.
Preferably, the Li2CO3Powder, Ta2O5Powder and K2CO3Powder purity is 99.999%.
Li is used in the present invention2CO3、Ta2O5With cosolvent K2CO3Molar ratio is the ratio of 48.75 ︰, 51.25 ︰ 13, preparation
The head of LT crystal and the Curie temperature difference of tail portion be mutated, touch the bottom, obtain uniform nearly chemistry meter up and down
Amount is than L T crystal.
Detailed description of the invention
Fig. 1 is doping different mol ratio cosolvent K2CO3The Curie temperature on the LT crystal head and tail portion that measure is poor.
Specific embodiment
The present invention provides a kind of flux method growth that can obtain uniform near stoichiometric proportion LT crystal up and down is uniform
The method of near-stoichiometric lithium tantalate crystals.
A kind of method that flux method grows uniform near-stoichiometric lithium tantalate crystals, includes the following steps:
Step S301: Li in molar ratio2CO ︰ Ta2O5︰ K2CO3Ratio for 48.75 ︰, 51.25 ︰ 13 is made into base-material；
Step S302: by above-mentioned base-material ground and mixed at mixture；
Step S303: heating mixture, so that CO2It decomposites and, then calcine the mixture again, obtain lithium tantalate polycrystal material；
Step S304: lithium tantalate polycrystal material being compacted, and is fitted into crucible, is heated to molten condition, after held for some time, is used
Near-stoichiometric lithium tantalate crystals are made in czochralski method.
Further, before step 1, the Li2CO3Powder, Ta2O5Powder and K2CO3Powder will also be by the step of drying
Suddenly.
Further, the Li2CO3Powder, Ta2O5Powder and K2CO3Powder purity is 99.999%.
The present invention is exactly to select K in flux method growth LT crystallization process2CO3As cosolvent, rubbed by adulterating difference
The cosolvent of your concentration, to adjust the fusing point of melt, the Curie temperature (Tc) of the LT crystal of acquisition is consistent end to end, to grow
Uniform near stoichiometric proportion LT crystal up and down out.
Li is used in the present invention2CO3、Ta2O5With cosolvent K2CO3Molar ratio is the ratio of 48.75 ︰, 51.25 ︰ 13, preparation
The head of LT crystal and the Curie temperature difference of tail portion be mutated, touch the bottom, obtain uniform nearly chemistry meter up and down
Amount is than L T crystal.
Further illustrate that the present invention, the following examples are only intended to that this is described in detail with comparative example by the following examples
Invention, does not limit the protection scope of invention in any way.
Embodiment 1: Li in molar ratio2CO ︰ Ta2O5︰ K2CO3Ratio for 48.75 ︰, 51.25 ︰ 6 is made into base-material, by above-mentioned base
Abrasive lapping is mixed into mixture, mixture is heated, so that CO2It decomposites and, then calcine the mixture again, obtain lithium tantalate
Lithium tantalate polycrystal material is compacted, and is fitted into crucible by polycrystal material, is heated to molten condition, after held for some time, uses czochralski method
Near-stoichiometric lithium tantalate crystals are made, obtained LT crystal takes head and tail portion after cutting process, then using poor
It is respectively 656 C and 660 C that formula scanning calorimetry (DSC), which tests Curie temperature (Tc), is illustrated under the proportion, the nearly chemistry of growth
Metering is non-uniform than LT crystal composition.
Embodiment 2: Li in molar ratio2CO ︰ Ta2O5︰ K2CO3Ratio for 48.75 ︰, 51.25 ︰ 8 is made into base-material, by above-mentioned base
Abrasive lapping is mixed into mixture, mixture is heated, so that CO2It decomposites and, then calcine the mixture again, obtain lithium tantalate
Lithium tantalate polycrystal material is compacted, and is fitted into crucible by polycrystal material, is heated to molten condition, after held for some time, uses czochralski method
Near-stoichiometric lithium tantalate crystals are made, obtained LT crystal takes head and tail portion after cutting process, then using poor
It is respectively 663 C and 670 C that formula scanning calorimetry (DSC), which tests Curie temperature (Tc), is illustrated under the proportion, the nearly chemistry of growth
Metering is non-uniform than LT crystal composition.
Embodiment 3: Li in molar ratio2CO ︰ Ta2O5︰ K2CO3Ratio for 48.75 ︰, 51.25 ︰ 13 is made into base-material, will be above-mentioned
Base-material ground and mixed heats mixture, so that CO at mixture2It decomposites and, then calcine the mixture again, obtain tantalic acid
Lithium tantalate polycrystal material is compacted, and is fitted into crucible by lithium polycrystal material, is heated to molten condition, after held for some time, with lifting
Legal system obtains near-stoichiometric lithium tantalate crystals, and obtained LT crystal takes head and tail portion, then use after cutting process
It is respectively 675 C and 675 C that differential scanning calorimetry (DSC), which tests Curie temperature (Tc), is illustrated under the proportion, closeization of growth
It is uniform that metering, which is learned, than LT crystal composition.
Embodiment 4: Li in molar ratio2CO ︰ Ta2O5︰ K2CO3Ratio for 48.75 ︰, 51.25 ︰ 17 is made into base-material, will be above-mentioned
Base-material ground and mixed heats mixture, so that CO at mixture2It decomposites and, then calcine the mixture again, obtain tantalic acid
Lithium tantalate polycrystal material is compacted, and is fitted into crucible by lithium polycrystal material, is heated to molten condition, after held for some time, with lifting
Legal system obtains near-stoichiometric lithium tantalate crystals, and obtained LT crystal takes head and tail portion, then use after cutting process
It is respectively 676 C and 680 C that differential scanning calorimetry (DSC), which tests Curie temperature (Tc), is illustrated under the proportion, closeization of growth
It is non-uniform that metering, which is learned, than LT crystal composition.
Embodiment 5: Li in molar ratio2CO ︰ Ta2O5︰ K2CO3Ratio for 48.75 ︰, 51.25 ︰ 21 is made into base-material, will be above-mentioned
Base-material ground and mixed heats mixture, so that CO at mixture2It decomposites and, then calcine the mixture again, obtain tantalic acid
Lithium tantalate polycrystal material is compacted, and is fitted into crucible by lithium polycrystal material, is heated to molten condition, after held for some time, with lifting
Legal system obtains near-stoichiometric lithium tantalate crystals, and obtained LT crystal takes head and tail portion, then use after cutting process
It is respectively 682 C and 685 C that differential scanning calorimetry (DSC), which tests Curie temperature (Tc), is illustrated under the proportion, closeization of growth
It is non-uniform that metering, which is learned, than LT crystal composition.
As can be seen from FIG. 1, Li2CO3、Ta2O5With cosolvent K2CO3Range of the molar ratio in 48.75 ︰, 51.25 ︰ (6~8)
Interior, the head of made LT crystal and the Curie temperature difference of tail portion are all larger than 4, and present with cosolvent K2CO3The increasing of molar ratio
Add, the trend of the Curie temperature difference rising on the head and tail portion of made LT crystal, Li2CO3、Ta2O5With cosolvent K2CO3It rubs
In the range of (17~21) 51.25 ︰ 48.75 ︰, the head of made LT crystal and the Curie temperature difference of tail portion are all larger than that ratio
4, and present with cosolvent K2CO3The increase of molar ratio, the Curie temperature difference decline on the head and tail portion of made LT crystal
Trend.According to above-mentioned Li2CO3、Ta2O5With cosolvent K2CO3Molar ratio in 48.75 ︰ 51.25 ︰ (6~8) range, and mole
Than in 48.75 ︰ 51.25 ︰ (17~21) range, the Curie temperature difference variation tendency on the head and tail portion of made LT crystal
Analysis, it may be speculated that in Li2CO3、Ta2O5With cosolvent K2CO3In the range of molar ratio is 48.75 ︰, 51.25 ︰ (8~17), institute
The head of the LT crystal of system and the Curie temperature difference of tail portion are not in 0 point, and in a specific embodiment of the invention,
Li2CO3、Ta2O5With cosolvent K2CO3When molar ratio is 48.75 51.25 ︰ 13 of ︰, the head of prepared LT crystal and tail portion
Curie temperature difference is mutated instead, and Curie temperature difference is 0, is touched the bottom, is illustrated under the proportion, the near-stoichiometric of growth
It is uniformly, to have exceeded the effect of expectation than LT crystal composition.
The steps in the embodiment of the present invention can be sequentially adjusted, merged and deleted according to actual needs.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, those skilled in the art can understand all or part of the processes for realizing the above embodiment, and wants according to right of the present invention
Made equivalent variations is sought, is still belonged to the scope covered by the invention.
Claims (3)
1. a kind of method that flux method grows uniform near-stoichiometric lithium tantalate crystals, it is characterised in that including walking as follows
It is rapid:
Step 1: Li in molar ratio2CO3︰ Ta2O5︰ K2CO3Ratio for 48.75 ︰, 51.25 ︰ 13 is made into base-material；
Step 2: by above-mentioned base-material ground and mixed at mixture；
Step 3: heating mixture, so that CO2It decomposites and, then calcine the mixture again, obtain lithium tantalate polycrystal material；
Step 4: lithium tantalate polycrystal material being compacted, and is fitted into crucible, is heated to molten condition, after held for some time, with mentioning
Near-stoichiometric lithium tantalate crystals are made in daraf(reciprocal of farad).
2. the method that flux method as described in claim 1 grows uniform near-stoichiometric lithium tantalate crystals, feature exist
In: before step 1, the Li2CO3Powder, Ta2O5Powder and K2CO3The step of powder will also be by drying.
3. the method that flux method as described in claim 1 grows uniform near-stoichiometric lithium tantalate crystals, feature exist
In: the Li2CO3Powder, Ta2O5Powder and K2CO3Powder purity is 99.999%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5515939A (en) * | 1978-07-18 | 1980-02-04 | Toshiba Corp | Production of single crystal |
| CN1818151A (en) * | 2005-12-31 | 2006-08-16 | 国内贸易部物资再生利用研究所 | Method for growing tantalic acid lithium in diameter of 5-inch single crystal |
| CN101225545A (en) * | 2007-10-25 | 2008-07-23 | 宁夏东方钽业股份有限公司 | Method for preparing near-stoichiometric lithium tantalate crystals |
| CN102689928A (en) * | 2012-06-19 | 2012-09-26 | 南开大学 | Preparation method of near-stoichiometric lithium tantalate crystals |
| CN104163454A (en) * | 2014-09-01 | 2014-11-26 | 中山大学 | Preparing method of lithium tantalate crystal |
-
2019
- 2019-07-11 CN CN201910626550.7A patent/CN110241456A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5515939A (en) * | 1978-07-18 | 1980-02-04 | Toshiba Corp | Production of single crystal |
| CN1818151A (en) * | 2005-12-31 | 2006-08-16 | 国内贸易部物资再生利用研究所 | Method for growing tantalic acid lithium in diameter of 5-inch single crystal |
| CN101225545A (en) * | 2007-10-25 | 2008-07-23 | 宁夏东方钽业股份有限公司 | Method for preparing near-stoichiometric lithium tantalate crystals |
| CN102689928A (en) * | 2012-06-19 | 2012-09-26 | 南开大学 | Preparation method of near-stoichiometric lithium tantalate crystals |
| CN104163454A (en) * | 2014-09-01 | 2014-11-26 | 中山大学 | Preparing method of lithium tantalate crystal |
Non-Patent Citations (1)
| Title |
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| 贾宝申: "基于化学计量比钽酸锂中红外光参量振荡器研究", 《中国博士学位论文全文数据库 信息科技辑》 * |
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Application publication date: 20190917 |