CN114686983A - Preparation method of garnet-phase-doped magneto-optical and nonlinear optical material - Google Patents
Preparation method of garnet-phase-doped magneto-optical and nonlinear optical material Download PDFInfo
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- CN114686983A CN114686983A CN202111481399.6A CN202111481399A CN114686983A CN 114686983 A CN114686983 A CN 114686983A CN 202111481399 A CN202111481399 A CN 202111481399A CN 114686983 A CN114686983 A CN 114686983A
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- 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
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- 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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- C30B19/00—Liquid-phase epitaxial-layer growth
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- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/12—Liquid-phase epitaxial-layer growth characterised by the substrate
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Abstract
The invention relates to the technical field of new materials, in particular to a preparation method of a garnet-phase-doped magneto-optical and nonlinear optical material, wherein the interaction between light and a substance is influenced by the magnetic state of a medium and the electronic structure of the material, the interaction between electromagnetic radiation and a magnetic polarization material causes a 'magneto-optical' effect, the magneto-optical effect plays an important role in the early history of electromagnetism, and experimental support is provided for the electromagnetic theory of light, the classical and quantum theory of substances such as electron spin motion, spin orbit coupling and the like.
Description
The technical field is as follows:
the invention relates to the technical field of new materials, in particular to a preparation method of a garnet-phase-doped magneto-optical and nonlinear optical material.
Background art:
the interaction between light and a substance is influenced by the magnetic state of a medium and the electronic structure of the material, the interaction between electromagnetic radiation and a magnetic polarization material causes a magneto-optical effect, the magneto-optical effect plays an important role in the early history of electromagnetism, and experimental support is provided for the electromagnetic theory of light and the classical and quantum theory of substances such as electron spin motion, spin orbit coupling and the like, in 1845, Michel-Faraday discovers that the polarization direction of linearly polarized light rotates when the linearly polarized light propagates through the medium because the medium is placed in a magnetic field parallel to the propagation direction, the experiment is one of the first experiments showing that the magnetic field is closely related to the light, the intensity or polarization of a light beam can be rapidly operated through an external field, so that a subject research of crossing the optical and the material is developed, and in the invention, the frequency of the light generating the magneto-optical effect is reduced to a terahertz wave band, the Terahertz (Terahertz, THz) wave is an electromagnetic wave with the frequency within the range of 0.1THz to 10THz, the wavelength is between 3mm and 30um, and the Terahertz (THz) wave has great application potential in the fields of information communication and the like, and in 2019, the Terahertz wave band within the range of 0.275 to 0.45THz is already determined as the next generation communication technical frequency band, but the research on the magneto-optical crystal and the nonlinear optical crystal in the Terahertz wave band is a blank at present, and the preparation technology of the invention is hopeful to fill the blank.
The invention content is as follows:
the invention aims to solve the existing problems and provides a preparation method of a garnet-phase-doped magneto-optical and nonlinear optical material.
The technical solution of the invention is as follows:
a method for preparing a garnet-phase-doped magneto-optical and nonlinear optical material comprises the steps of growing on [111] crystal-oriented gadolinium-crop garnet by adopting a liquid phase epitaxy method, doping V ions and Ti ions in a yttrium-iron garnet structure, and growing a garnet-phase-doped magneto-optical and nonlinear optical film by taking high-quality single-crystal gadolinium-crop garnet as a substrate, wherein the method comprises the following specific steps:
step 1: thoroughly cleaning a gadolinium-crop garnet substrate before starting growth, wherein the cleaning step comprises the steps of sequentially carrying out trichloroethylene at 80 ℃, deionized water at 80 ℃, a potassium dichromate solution at 80 ℃, deionized water at 80 ℃, an alkali solution at 80 ℃, deionized water at 80 ℃, an ammonia water solution at room temperature and deionized water at room temperature, and finally carrying out steam distillation by using isopropanol;
step 2: accurately weighing high-purity oxide raw materials according to preset components, grinding the raw materials into powder in an agate mortar, adding the powder into a platinum crucible, heating the crucible to 1000 ℃, standing the crucible for 24 hours, and cooling the crucible to the growth temperature of 805 ℃ to wait for growth after the melt is uniformly welded;
and 3, step 3: fixing a cleaned gadolinium-crop garnet substrate on a bracket by using a platinum wire, keeping an included angle of 8 degrees between the gadolinium-crop garnet substrate and a melt, and slowly putting the gadolinium-crop garnet substrate and the melt into the melt to prepare epitaxial growth;
and 4, step 4: setting growth time and rotation speed of the gadolinium-crop garnet substrate in an automatic control system, and starting an automatic growth process;
and 5: after the preset growth time is reached, the clamp automatically conveys the film out to the position above the melt for staying; increasing the rotating speed of the gadolinium-crop garnet substrate, throwing off residual melt on the film, taking the gadolinium-crop garnet substrate out of the epitaxial furnace, taking down the film, and putting the film into glacial acetic acid for cleaning.
Step 6: the film was washed in hot nitric acid to remove residual co-solvent.
Preferably, the gadolinium gallium garnet has a thickness of 500 um.
As a preferred technical scheme, the working range is 0.1THz-1.0 THz.
Preferably, the temperature is raised to 1000 ℃ in the step 2, the temperature is kept for 12 hours, after the temperature is kept, a clean platinum stirrer is slowly placed into the melt, the melt is stirred at a preset rotating speed, the stirring direction is changed every 1 hour, and the stirring is continued for 12 hours, so that the melt is uniformly melted.
As a preferable technical scheme, in the step 3, the substrate of the gadolinium-gallium-garnet is slowly put into the melt for 15 minutes, so that the temperature of the substrate of the gadolinium-gallium-garnet is consistent with the temperature of the melt.
As a preferable technical scheme, the growth time in the step 4 is 500-834 minutes, and the rotation speed of the gadolinium gallium garnet substrate is 60-80 r/min.
As a preferred technical scheme, the thickness of the film prepared in the step 5 is 300-500 um.
The invention has the beneficial effects that:
(1) the yttrium iron garnet is used as a typical magnetic material, has good permeability in a microwave band, but has an unobvious magneto-optical effect, the yttrium iron garnet crystal is modified by using a doping means, in the yttrium iron garnet structure, oxygen ions form three structures, namely a dodecahedron structure, an octahedron structure and a tetrahedron structure, because the radius of Y ions is large, the dodecahedron structure is generally occupied, and iron ions occupy gaps between the octahedron and the tetrahedron, and the magnetic moments in the octahedron and the tetrahedron are opposite;
(2) v and Ti ions replace Y ions in the yttrium iron garnet, the formed polyhedron distortion is large, magneto-optical and nonlinear optical effects are strong, the V and Ti doped yttrium iron garnet crystal has a preparation method with excellent magneto-optical and nonlinear effects, and the preparation method is simple and feasible, and the prepared doped yttrium iron garnet film has obvious magneto-optical effects and nonlinear optical effects in a terahertz waveband;
(3) liquid phase epitaxy is a standard technology for growing single crystal garnet films, gadolinium-gallium-garnet single crystals are used as substrates, lattice mismatch with yttrium-iron garnet is very small, the liquid phase technology process is mature, high-temperature melt epitaxy is adopted, special requirements on doped ions are not required, and the prepared epitaxial film is large in epitaxial thickness.
Description of the drawings:
FIG. 1 is an X-ray diffraction test chart of the doped yttrium iron garnet film of the invention
FIG. 2 is a diagram of a calculated band structure for the structure of the present invention
FIG. 3 shows the magneto-optical effect rotation angle of the present invention
FIG. 4 is an atomic structure diagram of a doped yttrium iron garnet film of the invention
The specific implementation mode is as follows:
the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: a method for preparing a garnet-phase-doped magneto-optical and nonlinear optical material comprises the steps of growing on gadolinium-crop garnet in a [111] crystal direction by adopting a liquid phase epitaxy method, doping V ions and Ti ions in an yttrium-iron garnet structure, and growing a garnet-phase-doped magneto-optical and nonlinear optical film by using high-quality single-crystal gadolinium-crop garnet as a substrate.
Further, the thickness of gadolinium gallium garnet is 500 um.
Further, the working range is 0.1THz-1.0 THz.
The method comprises the following specific steps:
step 1: thoroughly cleaning a gadolinium-crop garnet substrate before starting growth, wherein the cleaning step comprises the steps of sequentially carrying out trichloroethylene at 80 ℃, deionized water at 80 ℃, a potassium dichromate solution at 80 ℃, deionized water at 80 ℃, an alkali solution at 80 ℃, deionized water at 80 ℃, an ammonia water solution at room temperature and deionized water at room temperature, and finally carrying out steam distillation by using isopropanol;
step 2: accurately weighing high-purity oxide raw materials according to preset components, grinding the raw materials into powder in an agate mortar, adding the powder into a platinum crucible, heating the crucible to 1000 ℃, standing the crucible for 24 hours, keeping the temperature for 12 hours after the temperature is raised to 1000 ℃, slowly putting a cleaned platinum stirrer into a melt after the temperature is kept, stirring the melt at a preset rotating speed, changing the stirring direction once every 1 hour, continuously stirring the melt for 12 hours, and cooling the melt to the growth temperature of 805 ℃ to wait for growth after the melt is uniformly welded;
and step 3: fixing the cleaned gadolinium-crop garnet substrate on a bracket by using a platinum wire, keeping an included angle of 8 degrees between the gadolinium-crop garnet substrate and a melt, slowly placing the gadolinium-crop garnet substrate into the melt for staying for 15 minutes, and enabling the temperature of the gadolinium-crop garnet substrate to be consistent with the temperature of the melt for preparing epitaxial growth;
and 4, step 4: setting the growth time to be 500 minutes and the rotating speed of 60 revolutions per minute in an automatic control system, and starting the automatic growth process;
and 5: after the preset growth time is reached, the clamp automatically conveys the film out to the position above the melt for staying; increasing the rotating speed of the gadolinium-crop garnet substrate, throwing off residual melt on the film, taking the gadolinium-crop garnet substrate out of the epitaxial furnace, taking down the film, putting the film into glacial acetic acid for cleaning, and taking down the prepared yttrium-iron-garnet-doped film with the thickness of 300um after 1 hour.
Step 6: the film was washed in hot nitric acid to remove residual co-solvent.
Example 2: a method for preparing garnet-doped magneto-optical and nonlinear optical materials comprises the steps of growing gadolinium-gallium-garnet in a [111] crystal direction by a liquid phase epitaxy method, doping V ions and Ti ions in a yttrium-iron-garnet structure, and growing a garnet-doped magneto-optical and nonlinear optical film by taking high-quality single-crystal gadolinium-gallium-garnet as a substrate.
Further, the thickness of gadolinium gallium garnet is 500 um.
Further, the working range is 0.1THz-1.0 THz.
The method comprises the following specific steps:
step 1: thoroughly cleaning a gadolinium-crop garnet substrate before starting growth, wherein the cleaning step comprises the steps of sequentially carrying out trichloroethylene at 80 ℃, deionized water at 80 ℃, a potassium dichromate solution at 80 ℃, deionized water at 80 ℃, an alkali solution at 80 ℃, deionized water at 80 ℃, an ammonia water solution at room temperature and deionized water at room temperature, and finally carrying out steam distillation by using isopropanol;
step 2: accurately weighing high-purity oxide raw materials according to preset components, grinding the raw materials into powder in an agate mortar, adding the powder into a platinum crucible, heating the crucible to 1000 ℃, standing the crucible for 24 hours, keeping the temperature for 12 hours after the temperature is raised to 1000 ℃, slowly putting a cleaned platinum stirrer into a melt after the temperature is kept, stirring the melt at a preset rotating speed, changing the stirring direction once every 1 hour, continuously stirring the melt for 12 hours, and cooling the melt to the growth temperature of 805 ℃ to wait for growth after the melt is uniformly welded;
and step 3: fixing the cleaned gadolinium-crop garnet substrate on a bracket by using a platinum wire, keeping an included angle of 8 degrees between the gadolinium-crop garnet substrate and a melt, slowly placing the gadolinium-crop garnet substrate into the melt for staying for 15 minutes, and enabling the temperature of the gadolinium-crop garnet substrate to be consistent with the temperature of the melt for preparing epitaxial growth;
and 4, step 4: setting the growth time 834 minutes and the rotation speed of 80 revolutions per minute in an automatic control system, and starting the automatic growth process;
and 5: after the preset growth time is reached, the clamp automatically conveys the film out to the upper part of the melt for staying; increasing the rotating speed of the gadolinium-crop garnet substrate, throwing off residual melt on the film, lifting the gadolinium-crop garnet substrate from the epitaxial furnace, taking down the film, cleaning the film in glacial acetic acid, and taking down the prepared doped yttrium iron garnet film with the thickness of 500um after 1 hour.
Step 6: the film was washed in hot nitric acid to remove residual co-solvent.
The diffraction peak of the substrate and the prepared film is similar to that of the substrate, which shows that the garnet structure is not changed, and the Faraday rotation angles are all around 12 degrees and the energy band width is 2.05eV at 0.1-1.0THz, so that the application significance exists.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (7)
1. A method for preparing a garnet phase doped magneto-optical and nonlinear optical material, which comprises the step of growing on gadolinium-gallium-garnet with a [111] crystal orientation by adopting a liquid phase epitaxy method, and is characterized in that: v ions and Ti ions are doped in an yttrium iron garnet structure, and a garnet-phase-doped magneto-optical and nonlinear optical film grows by taking high-quality single crystal gadolinium-gallium-garnet as a substrate, and the method comprises the following specific steps:
step 1: thoroughly cleaning a gadolinium-crop garnet substrate before starting growth, wherein the cleaning step comprises the steps of sequentially carrying out trichloroethylene at 80 ℃, deionized water at 80 ℃, a potassium dichromate solution at 80 ℃, deionized water at 80 ℃, an alkali solution at 80 ℃, deionized water at 80 ℃, an ammonia water solution at room temperature and deionized water at room temperature, and finally carrying out steam distillation by using isopropanol;
step 2: accurately weighing high-purity oxide raw materials according to preset components, grinding the raw materials into powder in an agate mortar, adding the powder into a platinum crucible, heating the crucible to 1000 ℃, standing the crucible for 24 hours, and cooling the crucible to the growth temperature of 805 ℃ to wait for growth after the melt is uniformly welded;
and step 3: fixing a cleaned gadolinium-crop garnet substrate on a bracket by a platinum wire, keeping an included angle of 8 degrees between the gadolinium-crop garnet substrate and a fused mass, and slowly putting the gadolinium-crop garnet substrate into the fused mass to prepare epitaxial growth;
and 4, step 4: setting growth time and rotation speed of a gadolinium-crop garnet substrate in an automatic control system, and starting an automatic growth process;
and 5: after the preset growth time is reached, the clamp automatically conveys the film out to the upper part of the melt for staying; increasing the rotating speed of the gadolinium-crop garnet substrate, throwing off residual melt on the film, taking the gadolinium-crop garnet substrate out of the epitaxial furnace, taking down the film, and putting the film into glacial acetic acid for cleaning.
Step 6: the film was washed in hot nitric acid to remove residual co-solvent.
2. A method of making a garnet-phase doped magneto-optical and nonlinear optical material as claimed in claim 1, wherein the method comprises the steps of: the thickness of the gadolinium gallium garnet is 500 um.
3. A method of making a garnet-phase doped magneto-optical and nonlinear optical material as claimed in claim 1, wherein the method comprises the steps of: the working range is 0.1THz-1.0 THz.
4. A method of making a garnet-phase doped magneto-optical and nonlinear optical material as claimed in claim 1, wherein the method comprises the steps of: and (3) in the step (2), after the temperature is raised to 1000 ℃, keeping the temperature for 12 hours, after the temperature is kept, slowly putting a clean platinum stirrer into the melt, stirring the melt at a preset rotation speed, changing the stirring direction every 1 hour, and continuously stirring for 12 hours to uniformly melt the melt.
5. A method of making a garnet-phase doped magneto-optical and nonlinear optical material as claimed in claim 1, wherein the method comprises the steps of: in the step 3, the gadolinium-gallium-garnet substrate is slowly put into the melt and stays for 15 minutes, so that the temperature of the gadolinium-gallium-garnet substrate is consistent with that of the melt.
6. A method of making a garnet-phase doped magneto-optical and nonlinear optical material as claimed in claim 1, wherein the method comprises the steps of: the growth time in the step 4 is 500-834 minutes, and the rotation speed of the gadolinium gallium garnet substrate is 60-80 r/min.
7. A method of manufacturing a garnet-doped magneto-optical and nonlinear optical material as claimed in claim 1, wherein: the thickness of the film prepared in the step 5 is 300-500 um.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4269651A (en) * | 1978-06-22 | 1981-05-26 | Rockwell International Corporation | Process for preparing temperature-stabilized low-loss ferrite films |
| CN104818518A (en) * | 2015-04-17 | 2015-08-05 | 电子科技大学 | Preparation method of in-plane anisotropy Bi-substituted garnet magneto-optic single crystal thin film |
| CN105714379A (en) * | 2016-02-26 | 2016-06-29 | 电子科技大学 | Preparation method for directly growing highly-doped yttrium iron garnet film on silicon |
| CN107146761A (en) * | 2017-05-05 | 2017-09-08 | 电子科技大学 | The yttrium iron garnet of a kind of large magneto-optical effect/bismuth heterofilm and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4269651A (en) * | 1978-06-22 | 1981-05-26 | Rockwell International Corporation | Process for preparing temperature-stabilized low-loss ferrite films |
| CN104818518A (en) * | 2015-04-17 | 2015-08-05 | 电子科技大学 | Preparation method of in-plane anisotropy Bi-substituted garnet magneto-optic single crystal thin film |
| CN105714379A (en) * | 2016-02-26 | 2016-06-29 | 电子科技大学 | Preparation method for directly growing highly-doped yttrium iron garnet film on silicon |
| CN107146761A (en) * | 2017-05-05 | 2017-09-08 | 电子科技大学 | The yttrium iron garnet of a kind of large magneto-optical effect/bismuth heterofilm and preparation method thereof |
Non-Patent Citations (1)
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