CN112267146A - A method for growing yttrium iron garnet crystal using composite flux - Google Patents
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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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- 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
- C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
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Abstract
The invention discloses a method for growing an yttrium iron garnet crystal by adopting a composite fluxing agent. Yttrium iron garnet (Y)3Fe5O12YIG crystal is an important magneto-optical material, and the preparation steps are as follows: accurately weighing, mixing, grinding and sintering to obtain polycrystal materials, crushing the polycrystal materials, adding a composite fluxing agent, carrying out ball milling to obtain mixed materials, putting the mixed materials into a crucible, putting the crucible filled with the materials into a growth furnace for heating, heating to a set temperature and keeping the temperature to obtain a high-temperature molten crystal solution, then slowly cooling until the solution in the crucible is completely cooled and crystallized, and finally cooling to room temperature to obtain crystal ingots. And removing the fluxing agent by adopting a mechanical stripping and chemical corrosion method to finally obtain the crystal. The invention greatly reduces the pollution of lead element to the environment and the corrosion to the platinum crucible by the lead-free composite fluxing agent, effectively reduces the growth temperature of the crystal, and can obtain a body with larger sizeA bulk single crystal.
Description
Technical Field
The invention relates to the technical field of crystal growth, in particular to a method for growing an yttrium iron garnet crystal by adopting a composite fluxing agent.
Background
The yttrium iron garnet crystal is a functional material with excellent garnet structure of microwave, magneto-optic and magnetic properties, and the theoretical density is 5.171g/cm3The material is in a full transparent state under infrared radiation, is widely researched and applied to various optical devices, magneto-optical devices and microwave devices, and is a key material in the field of optical communication. The optical isolator made of Yttrium Iron Garnet (YIG) can well solve the problem of interference of reflected light on optical fiber transmission, and has important application in the fields of optical fiber communication and the like. With the needs of modern military and the rapid development of information society, the fields of 5G communication, electronic countermeasure and the like put higher requirements on the yttrium iron garnet crystal and the doping modification thereof.
Oxide raw material Y for growing yttrium iron garnet single crystal due to its high melting point2O3Has a melting point of 2410 ℃ and Fe2O3The melting point of (a) is 1538 ℃, and the grown yttrium iron garnet crystal has high-temperature phase change, and peritectic reaction and eutectic reaction occur in the growth process, so that certain difficulty exists in growing large-size yttrium iron garnet single crystals. Conventional methods for producing crystals, such as the czochralski method, are not suitable for such non-uniformly molten materials; the YIG crystal obtained by the zone melting method has smaller size and is difficult to meet the application of large-size devices; the liquid phase epitaxy method can grow a thin film and is not suitable for growing large-size bulk single crystals. The invention adopts the composite fluxing agent method to grow the large-size blocky single crystal, is beneficial to solving the problems and is suitable for growing the large-size blocky single crystal.
Disclosure of Invention
In view of the above, the present invention provides a method for growing an yttrium iron garnet crystal by using a composite flux without lead, which solves the problems of environmental pollution, high melting point of the crystal and the bottleneck of difficult growth of large-size massive yttrium iron garnet in the existing growth process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for growing yttrium iron garnet crystals by adopting a composite fluxing agent comprises the following steps:
(1) of raw materialsPreparation: according to Y3Fe5O12According to formula Y: fe: accurately weighing Y at a molar ratio of O =3:5:122O3And Fe2O3Powder raw materials are put into an agate mortar and are fully ground for 4 to 5 hours, and mixed raw materials are obtained;
(2) preparing a polycrystalline material: and (2) putting the mixed raw materials into a crucible, putting the crucible into a muffle furnace, pre-burning for 10-16 hours at 1050-1400 ℃ to obtain an yttrium iron garnet polycrystalline material block, and determining that the synthesized substance is YIG polycrystalline material through XRD test, wherein the result is shown in figure 1. Crushing the polycrystalline material block, adding a composite fluxing agent, and performing ball milling for 4 hours to obtain a polycrystalline material;
(3) seed crystal treatment: sequentially using deionized water, acetone and absolute ethyl alcohol to ultrasonically heat and clean cylindrical YIG seed crystals with the diameter of 3mm for 40 minutes, then boiling in a mixed solution of concentrated nitric acid and water in a ratio of 1:2 for 1 hour, and finally cleaning with deionized water; filling the treated seed crystal into the bottom of a crucible, filling a polycrystal material into the crucible, and then sealing the crucible;
(4) crystal growth pretreatment: firstly, raising the temperature in a crystal growth furnace to 1150-1500 ℃, placing a sealed crucible on a lifting platform in the crystal growth furnace, adjusting the crucible to the vertical position of a temperature field in the furnace, vertically raising an area of the crucible filled with materials to a high-temperature area in the furnace, preserving heat for 24-36 hours at 1150-1500 ℃ to fully melt the materials, slowly raising a seed crystal area in the crucible to the high-temperature area to melt the top of the seed crystal, and preserving heat for 3-5 hours;
(5) and (3) crystal growth: after the step (4) is finished, enabling the crucible to gradually leave the high-temperature area of the temperature field and move to the low-temperature area at the moving speed of 0.05-1mm/h until the crucible is completely separated from the high-temperature area to the low-temperature area, slowly cooling the high-temperature solution and separating out garnet crystals, and naturally cooling to room temperature after the growth is finished; taking out and stripping the crucible to obtain a crystal ingot;
(6) post-treatment of the crystals: and (5) cleaning the crystal ingot obtained in the step (5) through mechanical stripping or concentrated nitric acid corrosion, and removing externally wrapped fluxing agent to obtain the yttrium iron garnet crystal. The yttrium iron garnet crystal obtained by the experiment is shown in figure 2.
Preferably, the raw materials have a purity of more than or equal to 99.99 percent.
Preferably, the composite fluxing agent is Bi2O3+B2O3The addition amount of the polycrystalline material is 50-95% of the total weight of the polycrystalline material.
Preferably, the orientation of the seed crystal is <111>, <110>, <100>, or <001 >.
Preferably, the thickness of the crucible is 0.2 to 0.7 mm.
Preferably, the concentrated nitric acid solution in the step (6) is prepared by mixing concentrated nitric acid with the concentration of 69% according to the volume ratio of 1:2 and heating and corroding and cleaning the mixture in a water bath kettle at 60-80 ℃.
The invention has the beneficial effects that: the melting point of the material is effectively reduced by adding the composite fluxing agent, a driving force is provided for crystal growth in the vertical direction by a vertical moving method, the growth and the growth of the crystal are promoted, the growth difficulty and the energy consumption cost are reduced, the limitation of the existing yttrium iron garnet crystal preparation method on the crystal growth is overcome, the bulk yttrium iron garnet crystal is prepared, the crystal is smooth and has no cracking phenomenon, the crystal size can reach 20 multiplied by 30mm, and the bulk yttrium iron garnet crystal can be used as a magneto-optical material; the use requirement of a magneto-optical device which needs a block magneto-optical crystal material is met, and the development of industrialization is promoted.
Drawings
FIG. 1 is an XRD pattern of a synthesized YIG polycrystalline material;
FIG. 2 is a diagram of the YIG crystal obtained at the end of the experiment.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
a method for growing yttrium iron garnet crystals by adopting a composite fluxing agent comprises the following steps:
(1) preparation of raw materials: the raw material used in the experiment is Y with the purity of more than or equal to 99.99 percent2O3And Fe2O3According to Y3Fe5O12According to formula (ii) as Y: fe: o =3:5: the molar ratio of 12 was weighed. Adding the weighed raw materials into an agate mortar for fully grinding for 4 hours to obtain a mixed raw material;
(2) preparing a polycrystalline material: loading the mixed raw materials into a crucible, putting the crucible into a muffle furnace, pre-burning the crucible for 16 hours at 1050 ℃ to obtain an yttrium iron garnet polycrystalline material block, crushing the polycrystalline material block, and adding Bi2O3And B2O3The purity of the raw materials of the fluxing agent is 99.99 percent and accounts for 60 percent of the mixed materials, and the mixed materials are physically and fully ball-milled for 6 hours to obtain polycrystal materials; the XRD pattern is shown in FIG. 1 in comparison with the standard card, and the two patterns are consistent with each other, which indicates that the experiment successfully synthesizes YIG polycrystal materials.
(3) Seed crystal treatment: adopting YIG seed crystal for growth, adopting 3mm YIG seed crystal with the orientation of <000> and the circular section, ultrasonically heating and cleaning the seed crystal for 40 minutes by using deionized water, acetone and absolute ethyl alcohol in sequence, then boiling in a mixed solution of concentrated nitric acid and water in a ratio of 1:2 for 1 hour, and cleaning by using deionized water; filling the treated seed crystal into the bottom of a crucible, filling a polycrystal material into the crucible, and then sealing the crucible;
(4) crystal growth pretreatment: firstly, raising the temperature in a crystal growth furnace to 1150 ℃, placing a sealed crucible on a lifting platform of the crystal growth furnace, adjusting the crucible to the vertical position of a temperature field in the furnace, slowly and vertically raising a region of the crucible filled with materials to a high-temperature region in the furnace, preserving heat for 36 hours at 1150 ℃ to fully melt the materials, slowly raising a seed crystal region in part of the crucible to the high-temperature region to melt the top of the seed crystal, and preserving heat for 3 hours;
(5) and (3) crystal growth: after the step (4) is completed, the crystal growth furnace can be descended, so that the crucible is gradually descended to leave the high-temperature area of the temperature field and move to the low-temperature area, the moving speed is 0.05mm/h until the crucible is completely departed from the high-temperature area to reach the low-temperature area, the high-temperature solution is slowly cooled to be completely crystallized, and the crystal ingot is obtained after the temperature is cooled to the room temperature;
(6) post-treatment of the crystals: and (5) mechanically stripping and carrying out corrosion cleaning on the crystal ingot obtained in the step (5) by concentrated nitric acid, and removing flux impurities wrapped outside to obtain the yttrium iron garnet crystal.
Example 2:
a method for growing yttrium iron garnet crystals by adopting a composite fluxing agent comprises the following steps:
(1) preparation of raw materials: the raw material used in the experiment is Y with the purity of more than or equal to 99.99 percent2O3And Fe2O3According to Y3Fe5O12According to formula (ii) as Y: fe: o =3:5: the molar ratio of 12 was weighed. Adding the weighed raw materials into an agate mortar for fully grinding for 5 hours to obtain a mixed raw material;
(2) preparing a polycrystalline material: loading the mixed raw materials into a crucible, putting the crucible into a muffle furnace, pre-burning the crucible for 10 hours at 1400 ℃ to obtain yttrium iron garnet polycrystalline material blocks, crushing the polycrystalline material blocks, and adding Bi2O3And B2O3The purity of the raw materials of the fluxing agent is 99.99 percent and accounts for 50 percent of the mixed materials, and the mixed materials are physically and fully ball-milled for 6 hours to obtain polycrystal materials;
(3) seed crystal treatment: adopting YIG seed crystal for growth, adopting 3mm YIG seed crystal with the orientation of <000> and the circular section, ultrasonically heating and cleaning the seed crystal for 40 minutes by using deionized water, acetone and absolute ethyl alcohol in sequence, then boiling in a mixed solution of concentrated nitric acid and water in a ratio of 1:2 for 1 hour, and cleaning by using deionized water; filling the treated seed crystal into the bottom of a crucible, filling a polycrystal material into the crucible, and then sealing the crucible;
(4) crystal growth pretreatment: firstly, raising the temperature in a crystal growth furnace to 1500 ℃, placing a sealed crucible on a lifting platform of the crystal growth furnace, adjusting the crucible to the vertical position of a temperature field in the furnace, slowly and vertically lifting a region of the crucible filled with materials to a high-temperature region in the furnace, preserving heat for 24 hours at 1500 ℃ to fully melt the materials, slowly lifting a part of seed crystal regions in the crucible to the high-temperature region to melt the tops of the seed crystals, and preserving heat for 5 hours;
(5) and (3) crystal growth: and (4) after the step (4) is completed, the crystal growth furnace can be descended, so that the crucible is gradually descended to leave the high-temperature area of the temperature field and move to the low-temperature area at the moving speed of 1mm/h until the crucible is completely departed from the high-temperature area to reach the low-temperature area, the high-temperature solution is slowly cooled to be completely crystallized, and the crystal ingot is obtained after the high-temperature solution is cooled to the room temperature.
(6) Post-treatment of the crystals: and (5) mechanically stripping and carrying out corrosion cleaning on the crystal ingot obtained in the step (5) by concentrated nitric acid, and removing flux impurities wrapped outside to obtain the yttrium iron garnet crystal.
Example 3
A method for growing yttrium iron garnet crystals by adopting a composite fluxing agent comprises the following steps:
(1) preparation of raw materials: the raw material used in the experiment is Y with the purity of more than or equal to 99.99 percent2O3And Fe2O3According to Y3Fe5O12According to formula (ii) as Y: fe: o =3:5: the molar ratio of 12 was weighed. Adding the weighed raw materials into an agate mortar for fully grinding for 4.5 hours to obtain a mixed raw material;
(2) preparing a polycrystalline material: loading the mixed raw materials into a crucible, putting the crucible into a muffle furnace, pre-burning for 12 hours at 1250 ℃ to obtain yttrium iron garnet polycrystalline material blocks, crushing the polycrystalline material blocks, and adding Bi2O3And B2O3The purity of the raw materials of the fluxing agent is 99.99 percent and accounts for 60 percent of the mixed materials, and the mixed materials are physically and fully ball-milled for 6 hours to obtain polycrystal materials;
(3) seed crystal treatment: adopting YIG seed crystal for growth, adopting 3mm YIG seed crystal with the orientation of <000> and the circular section, ultrasonically heating and cleaning the seed crystal for 40 minutes by using deionized water, acetone and absolute ethyl alcohol in sequence, then boiling in a mixed solution of concentrated nitric acid and water in a ratio of 1:2 for 1 hour, and cleaning by using deionized water; filling the treated seed crystal into the bottom of a crucible, filling a polycrystal material into the crucible, and then sealing the crucible;
(4) crystal growth pretreatment: firstly, raising the temperature in a crystal growth furnace to 1350 ℃, placing a sealed crucible on a lifting platform of the crystal growth furnace, adjusting the crucible to the vertical position of a temperature field in the furnace, slowly and vertically lifting an area of the crucible filled with materials to a high-temperature area in the furnace, preserving heat for 30 hours at 1350 ℃ to fully melt the materials, slowly lifting a part of seed crystal areas in the crucible to the high-temperature area to melt the tops of the seed crystals, and preserving heat for 4 hours;
(5) and (3) crystal growth: and (4) after the step (4) is completed, the crystal growth furnace can be descended, so that the crucible is gradually descended to leave the high-temperature area of the temperature field and move to the low-temperature area at the moving speed of 0.08mm/h until the crucible is completely departed from the high-temperature area to reach the low-temperature area, the high-temperature solution is slowly cooled to be completely crystallized, and the crystal ingot is obtained after the temperature is cooled to the room temperature.
(6) Post-treatment of the crystals: and (5) mechanically stripping and carrying out corrosion cleaning on the crystal ingot obtained in the step (5) by concentrated nitric acid, and removing flux impurities wrapped outside to obtain the yttrium iron garnet crystal.
As can be seen from FIG. 2, the crystal size can reach 20X 30mm, the crystal has obvious growth stripes and cleaned edges and corners, and the crystal quality of the crystal is good.
Finally, the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solutions of the present invention by those of ordinary skill in the art should be covered within the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. A method for growing yttrium iron garnet crystals by adopting a composite fluxing agent is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing raw materials: according to Y3Fe5O12According to formula Y: fe: accurately weighing Y at a molar ratio of O =3:5:122O3And Fe2O3Powder raw materials are put into an agate mortar and are fully ground for 4 to 5 hours, and mixed raw materials are obtained;
(2) preparing a polycrystalline material: putting the mixed raw materials into a crucible, putting the crucible into a muffle furnace, pre-burning the crucible for 10 to 16 hours at 1050 to 1400 ℃ to obtain yttrium iron garnet polycrystalline material blocks, crushing the polycrystalline material blocks, adding a composite fluxing agent, and ball-milling the mixture for 4 hours to obtain a polycrystalline material;
(3) seed crystal treatment: sequentially using deionized water, acetone and absolute ethyl alcohol to ultrasonically heat and clean cylindrical YIG seed crystals with the diameter of 3mm for 40 minutes, then boiling in a mixed solution of concentrated nitric acid and water in a ratio of 1:2 for 1 hour, and finally cleaning with deionized water; filling the treated seed crystal into the bottom of a crucible, filling a polycrystal material into the crucible, and then sealing the crucible;
(4) crystal growth pretreatment: firstly, raising the temperature in a crystal growth furnace to 1150-1500 ℃, placing a sealed crucible on a lifting platform in the crystal growth furnace, adjusting the crucible to the vertical position of a temperature field in the furnace, vertically raising an area of the crucible filled with materials to a high-temperature area in the furnace, preserving heat for 24-36 hours at 1150-1500 ℃ to fully melt the materials, slowly raising a seed crystal area in the crucible to the high-temperature area to melt the top of the seed crystal, and preserving heat for 3-5 hours;
(5) and (3) crystal growth: after the step (4) is finished, enabling the crucible to gradually leave the high-temperature area of the temperature field and move to the low-temperature area at the moving speed of 0.05-1mm/h until the crucible is completely separated from the high-temperature area to the low-temperature area, slowly cooling the high-temperature solution and separating out garnet crystals, and naturally cooling to room temperature after the growth is finished; taking out and stripping the crucible to obtain a crystal ingot;
(6) post-treatment of the crystals: and (5) mechanically stripping or cleaning the crystal ingot obtained in the step (5) by concentrated nitric acid corrosion, and removing the flux coated outside to obtain the bismuth-doped yttrium iron garnet crystal.
2. The method for growing yttrium iron garnet crystal by using a composite flux as claimed in claim 1, wherein the raw materials are all of a purity of 99.99% or more.
3. The method for growing yttrium iron garnet crystal by using composite flux as claimed in claim 1, wherein the composite flux is Bi2O3+B2O3The addition amount of the polycrystalline material is 50-95% of the total weight of the polycrystalline material.
4. The method of growing an yttrium-iron-garnet crystal with a composite flux according to claim 1, wherein the seed crystal has an orientation of <111>, <110>, <100> or <001 >.
5. The method of growing an yttrium iron garnet crystal using a composite flux according to claim 1, wherein the thickness of the crucible is 0.2 to 0.7 mm.
6. The method for growing an yttrium iron garnet crystal using a composite flux as claimed in claim 1, wherein the concentrated nitric acid solution in the step (6) is prepared from a concentrated nitric acid solution having a concentration of 69% in a volume ratio of 1:2 and heating and corroding and cleaning the mixture in a water bath kettle at 60-80 ℃.
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| CN114150365A (en) * | 2021-10-29 | 2022-03-08 | 中国科学院福建物质结构研究所 | Preparation method of large-size yttrium iron garnet single crystal |
| CN114318535A (en) * | 2021-12-29 | 2022-04-12 | 上海应用技术大学 | Method for rapidly growing yttrium iron garnet crystal |
| CN115491748A (en) * | 2022-11-01 | 2022-12-20 | 安徽科瑞思创晶体材料有限责任公司 | Bismuth yttrium-doped iron garnet, crystal growth method and application thereof |
| CN118028979A (en) * | 2024-04-02 | 2024-05-14 | 山东大学 | Synthesis method of gadolinium gallium garnet single crystal |
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