CN116005260A - Faraday rotation sheet and preparation method thereof - Google Patents
Faraday rotation sheet and preparation method thereof Download PDFInfo
- Publication number
- CN116005260A CN116005260A CN202211314503.7A CN202211314503A CN116005260A CN 116005260 A CN116005260 A CN 116005260A CN 202211314503 A CN202211314503 A CN 202211314503A CN 116005260 A CN116005260 A CN 116005260A
- Authority
- CN
- China
- Prior art keywords
- substrate
- melt
- faraday
- temperature
- garnet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a Faraday rotary plate and a preparation method thereof, which relate to the technical field of optical materials and comprise the following steps: heating a mixture of a plurality of element oxides to a preset temperature to melt the element oxides into a melt; cooling the melt to a predetermined temperature to change the melt into supersaturated melt; completely immersing the substrate and the horizontal plane into the supersaturated molten liquid at a preset angle; rotating the substrate to generate a Bi garnet film; and removing the substrate. According to the invention, the substrate and the liquid level of the melt are kept at 45 degrees and are all immersed in the melt, so that the melt can be more uniform in the rotating process, and qualified Bi garnet films can be grown on both sides of the substrate, thereby improving the film growth efficiency and reducing the substrate consumption; through the addition of multiple element oxides, the lattice constant and the temperature coefficient of the Bi garnet are optimized, and the problem of film cracking is solved.
Description
Technical Field
The invention relates to the technical field of optical materials, in particular to a Faraday rotary plate and a preparation method thereof.
Background
The Faraday rotation plate is an important element for manufacturing nonreciprocal optical communication passive devices such as an optical isolator, an optical circulator and the like. The optical isolator is mainly applied to the field of 5G communication systems, such as: communication between the base station and the switching center, data centers, communication backbones, and autonomous lidar, etc.
An optical isolator is a two-port device that allows an optical signal to pass from a first port to a second port, while an optical signal from the second port to the first port is attenuated. Therefore, an optical isolator can be added behind the light source to prevent reflected light from entering the light source, and the stability of the light source is maintained. Laser radar or 10Gb/s high-speed optical communication requires an optical isolator for each laser source.
An optical circulator is a multi-port input-output nonreciprocal device that allows optical signals to be transmitted only along a prescribed port sequence, for example, light can pass through ports 1 to 2 and ports 2 to 3, while other path optical signals cannot pass through. The optical circulator is applied to the fields requiring optical fiber multiplexing such as OADM and sensing.
To achieve the nonreciprocity of light of the optical isolator and the optical circulator, faraday rotation plates are required, 1 plate is required for the optical isolator, and 4 plates are required for the optical circulator. Due to yttrium iron garnet YIG (Y 3 Fe 5 O 12 ) The monocrystal has small light absorption and larger nonreciprocal magneto-optical rotation in near infrared band, is mostly used for manufacturing Faraday rotary plates, bi ions are doped in YIG, bismuth garnet containing rare earth ions has larger Faraday rotary coefficient and lower light absorption coefficient in near infrared region, the rotary coefficient in the region is an order of magnitude larger than that of pure YIG, and self-bias magnet can be realized, namely, after the magneto-optical film is magnetized, the magnetization state can be kept under the condition of removing an external magnetic field, so that the bismuth garnet is an ideal material for manufacturing the Faraday rotary plates.
At present, a faraday rotator is generally grown by a top immersion liquid phase epitaxy method, the main equipment is a liquid phase epitaxy furnace, a plurality of metal oxides are mixed and then are filled into a platinum crucible, the crucible is heated to about 1000 ℃, the oxides are melted into high-temperature melt, then the temperature is reduced to supersaturated melt, then as shown in fig. 2, a substrate of garnet material is provided with a rotating rod, then as shown in fig. 3, the substrate is lowered to the surface of the supersaturated melt through the rotating rod and rotated, a Bi garnet film starts to grow on the lower surface of the substrate, when the Bi garnet film grows to a required thickness, the rotating rod is lifted, the substrate with the Bi garnet is taken down, the substrate is polished, and the rest part is the required faraday rotator.
However, if the substrate is placed horizontally, the substrate is immersed in the melt, and the melt near the upper and lower surfaces of the substrate has larger concentration and temperature difference, the films grown on the upper and lower surfaces are inconsistent, the generated stress can cause the cracking of the films, and the manufacturing qualification rate of the Faraday rotary sheet can be reduced, so that only one layer of Faraday rotary sheet can be grown on the surface of the melt, and the efficiency and the substrate utilization rate can be halved.
Disclosure of Invention
The invention aims to provide a Faraday rotary piece and a preparation method thereof, and the preparation method of the Faraday rotary piece reduces the concentration and temperature difference of accessories on the upper surface and the lower surface of a substrate and the stress of films growing on the upper surface and the lower surface of the substrate, avoids the problem of film cracking caused by overlarge stress, and effectively improves the manufacturing efficiency and the qualification rate of the Faraday rotary piece.
In order to achieve the above object, the present invention provides the following solutions:
a preparation method of a Faraday rotary plate comprises the following steps:
heating the oxide mixture to a first temperature for heat preservation to obtain an oxide melt;
cooling the oxide melt to a second temperature to obtain supersaturated melt;
immersing a substrate in the supersaturated solution; the plane of the substrate and the liquid level of the supersaturated molten liquid form an angle of 45 degrees;
rotating the substrate to generate a Bi garnet film;
and removing the substrate to obtain the Faraday rotation sheet.
Preferably, the oxide mixture comprises: tb (Tb) 2 O 3 、Gd 2 O 3 、B 2 O 3 、Fe 2 O 3 、PbO、Bi 2 O 3 And AI 2 O 3 。
Preferably, the Tb 2 O 3 、Gd 2 O 3 、B 2 O 3 、Fe 2 O 3 、PbO、Bi 2 O 3 And AI 2 O 3 The mass ratio of (2) is 1: (1.078 to 1.096): (7.456-7.476): (25.809-25.841): (212.571-212.771): (146.076-146.216): (0.796-0.806).
Preferably, the substrate is (CaGd) 3 (ZrMgGa) 5 O 12 。
Preferably, the first temperature is 1099-1101 ℃, and the heat preservation time is 34-36 min.
Preferably, the cooling rate is 99-101 ℃/hr, and the second temperature is 849-851 ℃.
Preferably, the substrate is rotated at a rate of 10rpm for the same time as the growth time of the Bi garnet film.
Preferably, the method for removing the substrate comprises the following steps: the substrate was cut into two pieces from the middle and the substrate was ground away. .
The invention also provides the Faraday rotary sheet prepared by the preparation method, and the Faraday rotary sheet comprises Bi 1.13 Gd 1.14 Tb 0.70 Pb 0.03 Fe 4.95 Pt 0.01 Al 0.04 O 12 。
Preferably, the rotation angle of the Faraday rotation plate is 45 degrees, the insertion loss is 0.05dB, and the Faraday rotation coefficient is 0.1115/um.
According to the specific embodiment provided by the invention, the following technical effects are disclosed:
the invention provides a Faraday rotary piece and a preparation method thereof, wherein the substrate and the liquid level of the melt are kept at 45 degrees and are all immersed in the melt, so that the concentration and temperature difference of the melt near the upper surface and the lower surface of the substrate are reduced, the melt can be more uniform in the rotation process, and qualified Bi garnet films can be grown on both sides of the substrate, thereby improving the film growth efficiency and reducing the substrate consumption; by adding multiple element oxides, the lattice constant and the temperature coefficient of the Bi garnet are optimized, the stress generated by the film is reduced, and the problem of film cracking is solved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the drawings that are needed in the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a flow chart of a method for improving qualification rate and efficiency of fabricating faraday rotator according to an embodiment of the present invention.
Fig. 2 is a schematic structural diagram of an apparatus for manufacturing a faraday rotator in the prior art.
Figure 3 is a schematic diagram of a prior art faraday rotator fabrication.
Fig. 4 is a schematic structural diagram of an apparatus for manufacturing a faraday rotator according to an embodiment of the present invention.
Fig. 5 is a schematic diagram of fabrication of a faraday rotator according to an embodiment of the present invention.
(1) -a substrate, (2) -a high temperature melt, (3) -a rotating rod
Detailed Description
The invention provides a preparation method of a Faraday rotary piece, which comprises the following steps:
s1: heating the oxide mixture to a first temperature for heat preservation to obtain an oxide solution;
s2: cooling the oxide solution to a second temperature to obtain a supersaturated solution;
s3: immersing a substrate in the supersaturated solution; the substrate plane forms an angle of 45 degrees with the supersaturated solution level;
s4: rotating the substrate to generate a Bi garnet film;
s5: and removing the substrate to obtain the Faraday rotation sheet.
The invention heats the oxide mixture to a first temperature for heat preservation to obtain an oxide solution.
In the present invention, the oxide mixture includes Tb 2 O 3 、Gd 2 O 3 、B 2 O 3 、Fe 2 O 3 、PbO、Bi 2 O 3 And AI 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The Tb is 2 O 3 、Gd 2 O 3 、B 2 O 3 、Fe 2 O 3 、PbO、Bi 2 O 3 And AI 2 O 3 The mass ratio of (2) is 1: (1.078 to 1.096): (7.456-7.476): (25.809-25.841): (212.571-212.771): (146.076-146.216): (0.796 to 0.806), more preferably 1: (1.082-1.092): (7.461-7.471): (25.819-25.831): (212.621-212.721): (146.116-146.176): (0.798 to 0.804), most preferably 1:1.087:7.466:25.825:212.671:146.146:0.801. according to the invention, through the addition of multiple element oxides, the lattice constant and the temperature coefficient of the Bi garnet are optimized, the stress generated by the film is reduced, and the problem of film cracking is solved.
In the present invention, the first temperature is preferably 1099 ℃ to 1101 ℃, more preferably 1100 ℃; the time for the heat preservation is preferably 34min to 36min, more preferably 35min.
In the present invention, the solution is preferably stirred after the incubation is completed. The stirring time is preferably 14 to 16 minutes, more preferably 15 minutes. The invention makes the solution more uniform by stirring.
The method comprises the steps of obtaining oxide melt, and cooling the oxide melt to a second temperature to obtain supersaturated melt.
In the present invention, the cooling rate is preferably 99 to 101 ℃ per hour, more preferably 100 ℃ per hour, and the second temperature is preferably 849 to 851 ℃, more preferably 850 ℃. The invention makes the oxide melt become supersaturated melt by cooling.
After obtaining the supersaturated solution, the invention immerses the substrate in the supersaturated solution.
In the invention, the plane of the substrate forms an angle of 45 degrees with the liquid level of the supersaturated molten solution; the substrate is preferably Gd 3 (ScGa) 5 O 12 、Sm 3 (ScGa) 5 O 12 、La 3 (ScGa) 5 O 12 Or (CaGd) 3 (ZrMgGa) 5 O 12 . More preferably (CaGd) 3 (ZrMgGa) 5 O 12 . In the present invention, the substrate is preferably preheated in a preheating zone, the preheating temperature is preferably 800 to 1000 ℃, more preferably 880 to 920 ℃, and the preheating time is preferably 5 to 30min, more preferably 10 to 20min, and most preferably 15min, before being immersed in the saturated melt.
According to the invention, the substrate and the liquid level of the molten liquid are kept at 45 degrees and are fully immersed in the molten liquid, so that the concentration and temperature difference of the molten liquid near the upper surface and the lower surface of the substrate are reduced, the molten liquid can be more uniform in the rotating process, and qualified Bi garnet films can be grown on both sides of the substrate, thereby improving the film growth efficiency and reducing the substrate consumption.
The substrate is immersed into the supersaturated molten liquid, and then the substrate is rotated to generate the Bi garnet film.
In the present invention, the substrate is rotated at a rate of preferably 1 to 100rpm, more preferably 5 to 20rpm, and most preferably 10rpm; the time for rotating the substrate is preferably 30 to 60 hours, more preferably 40 to 50 hours. The substrate rotation time is the same as the growth time of the Bi garnet film.
The Bi garnet film is obtained, and the substrate is removed to obtain the Faraday rotary plate.
In the present invention, the method of removing the substrate is preferably to cut the substrate into two pieces from the middle and grind away the substrate.
According to the invention, after the substrate is removed, two Bi garnet sheets are obtained, and the single Bi garnet sheet is ground until the Faraday rotation angle is 45 degrees.
Preferably, the method for removing the substrate comprises the following steps: the substrate was cut into two pieces from the middle and the substrate was ground away.
The invention also provides the Faraday rotary sheet prepared by the preparation method, and the Faraday rotary sheet comprises Bi 1.05～1.21 Gd 1.07～1.21 Tb 0.66～0.74 Pb 0.03 Fe 4.85～5.05 Pt 0.01 Al 0.03～0.05 O 12 Most preferably: bi (Bi) 1.13 Gd 1.1 4 Tb 0.70 Pb 0.03 Fe 4.95 Pt 0.01 Al 0.04 O 12 。
Preferably, the rotation angle of the Faraday rotator is 45 ℃, the insertion loss is 0.05dB, and the Faraday rotation coefficient is 0.115 DEG/um.
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention aims to provide a method capable of improving qualification rate and efficiency of manufacturing Faraday rotary plates, which solves the problems that in the prior art, because of concentration and temperature difference of molten liquid near the upper surface and the lower surface of a substrate caused by horizontal immersion of the substrate in the molten liquid, films growing on the upper surface and the lower surface are inconsistent, the films are cracked due to the generated stress, and the manufacturing qualification rate and efficiency of the Faraday rotary plates are reduced.
Based on the analysis of the prior art, the embodiment of the invention provides the following technical scheme:
example 1:
1. and (3) batching:
the following oxides were weighed using an analytical balance, 5.643gTb 2 O 3 ，6.134gGd 2 O 3 ，42.131gB 2 O 3 ，145.73gFe 2 O 3 ，1200.1gPbO，824.7gBi 2 O3，4.520gAl 2 O 3 。
2. And (2) charging:
the weighed oxides are poured into a platinum crucible in sequence of large quantity and small quantity.
3. And (3) feeding:
and placing the platinum crucible filled with the oxide into a liquid phase epitaxial furnace.
4. Heating:
starting a temperature-raising program of the liquid phase epitaxial furnace, heating the platinum crucible, and preserving heat for 35 minutes when the temperature is raised to 1100 ℃, so that the oxides are mixed and melted into a melt.
5. Stirring:
the rotary rod with the stirring clamp is put down, the molten liquid is stirred for 15 minutes, so that the molten liquid is more uniform, and after stirring is finished, the rotary rod is lifted to take down the stirring clamp.
6. And (3) cooling:
cooling to 850 ℃ at a rate of 100 ℃/hr, and forming stable supersaturated melt in the crucible.
7. And (3) loading a substrate:
as shown in FIG. 4, a 3 inch (CaGd) 3 (ZrMgGa) 5O12 substrate was mounted under the rotating rod so that the substrate was 45℃from the horizontal, and the rotating rod was lowered to preheat for 15 minutes in the preheating zone.
8. And (3) growing:
as shown in FIG. 5, the rotating rod was further lowered to completely immerse the substrate in the melt, and the substrate was rotated to initiate growth of the Bi garnet film, and after 30 hours, the film growth was completed. The rotating rod is lifted, and the substrate on which the Bi garnet grows is taken off after the substrate stays in the preheating zone for 30 minutes.
9. Grinding:
the substrate was cut from the middle into two pieces by wire cutting, and the substrate was ground away to obtain two 3-inch Bi garnet faraday rotator pieces. The thickness was measured to be 513 μm. Grinding of the monolithic Bi garnet was continued until its faraday rotation angle was 45 °.
10. Measurement:
the Bi garnet component is measured to be Bi by adopting an X-ray scanning electron microscope 1.13 Gd 1.14 Tb 0.70 Pb 0.03 Fe 4.95 Pt 0.01 Al 0.0 4 O 12 。
The insertion loss was measured to be 0.05dB using an optical measurement system, and the Faraday rotation coefficient was 0.115 DEG/μm. Basically meets the requirements of manufacturing the optical isolator.
The existing manufacturing method of the Faraday rotary plate can only grow one layer of Faraday rotary plate on the surface of the molten liquid, and the efficiency and the substrate utilization rate are reduced by half. The invention can grow Faraday rotation plates on both sides of the substrate, the efficiency is doubled, the utilization rate of the substrate is reduced by half, and the manufacturing cost of the Faraday rotation plates is reduced.
According to the invention, the addition of multiple element oxides is selected, so that the lattice constant and the temperature coefficient of the Bi garnet are optimized, the problem of film cracking is solved, and the qualification rate of Faraday rotary plate manufacturing is improved.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the system disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The principles and embodiments of the present invention have been described herein with reference to specific examples, the description of which is intended only to assist in understanding the methods of the present invention and the core ideas thereof; also, it is within the scope of the present invention to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the invention.
Claims (10)
1. The preparation method of the Faraday rotary piece is characterized by comprising the following steps of:
heating the oxide mixture to a first temperature for heat preservation to obtain an oxide melt;
cooling the oxide melt to a second temperature to obtain supersaturated melt;
immersing a substrate in the supersaturated solution; the plane of the substrate and the liquid level of the supersaturated molten liquid form an angle of 45 degrees;
rotating the substrate to generate a Bi garnet film;
and removing the substrate to obtain the Faraday rotation sheet.
2. The method of claim 1, wherein the oxide mixture comprises: tb (Tb) 2 O 3 、Gd 2 O 3 、B 2 O 3 、Fe 2 O 3 、PbO、Bi 2 O 3 And AI 2 O 3 。
3. The method according to claim 2, wherein the Tb 2 O 3 、Gd 2 O 3 、B 2 O 3 、Fe 2 O 3 、PbO、Bi 2 O 3 And AI 2 O 3 The mass ratio of (2) is 1: (1.078 to 1.096): (7.456-7.476): (25.809-25.841): (212.571-212.771): (146.076-146.216): (0.796-0.806).
4. The method of claim 1, wherein the substrate is Gd 3 (ScGa) 5 O 12 、Sm 3 (ScGa) 5 O 12 、La 3 (ScGa) 5 O 12 Or (CaGd) 3 (ZrMgGa) 5 O 12 。
5. The method according to claim 1, wherein the first temperature is 1099 to 1101 ℃, and the time for heat preservation is 34 to 36 minutes.
6. The method according to claim 1, wherein the rate of cooling is 99 to 101 ℃/hr and the second temperature is 849 ℃ to 851 ℃.
7. The method of claim 1, wherein the substrate is rotated at a rate of 10rpm for the same time as the growth time of the Bi garnet film.
8. The method of claim 1, wherein the method of removing the substrate comprises: the substrate was cut into two pieces from the middle and the substrate was ground away.
9. A faraday rotator prepared by the preparation method according to any one of claims 1 to 8, wherein the faraday rotator comprises Bi 1.05～1.21 Gd 1.07～1.21 Tb 0.66～0.74 Pb 0.03 Fe 4.85～ 5.05 Pt 0.01 Al 0.03～0.05 O 12 。
10. A faraday rotator according to claim 9, characterized in that the angle of rotation of the faraday rotator is 45 ℃, the insertion loss is 0.05dB, and the faraday rotation factor is 0.115 °/um.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211314503.7A CN116005260A (en) | 2022-10-25 | 2022-10-25 | Faraday rotation sheet and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211314503.7A CN116005260A (en) | 2022-10-25 | 2022-10-25 | Faraday rotation sheet and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116005260A true CN116005260A (en) | 2023-04-25 |
Family
ID=86032373
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211314503.7A Pending CN116005260A (en) | 2022-10-25 | 2022-10-25 | Faraday rotation sheet and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116005260A (en) |
-
2022
- 2022-10-25 CN CN202211314503.7A patent/CN116005260A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7333261B2 (en) | Magnetic garnet material, faraday rotator, optical device, bismuth-substituted rare earth-iron-garnet single-crystal film and method for producing the same crucible for producing the same | |
| CN104775160A (en) | Preparation method of monocrystalline garnet thick film | |
| CN104775153A (en) | Novel magneto-optic single crystal material growing method | |
| JPH0354198A (en) | Oxide garnet single crystal | |
| CN104818518A (en) | Preparation method of in-plane anisotropy Bi-substituted garnet magneto-optic single crystal thin film | |
| CN111910252A (en) | Large-size doped YIG single crystal thin film material and preparation method thereof | |
| US6059878A (en) | Method of manufacturing a bismuth-substituted rare-earth iron garnet single crystal film | |
| Damen et al. | Calcium gallium germanium garnet as a substrate for magnetic bubble application | |
| CN114318536B (en) | Bismuth-doped rare earth iron garnet single crystal film, preparation method thereof and optical device | |
| CN116005260A (en) | Faraday rotation sheet and preparation method thereof | |
| CN110629286A (en) | Dysprosium vanadate-doped magneto-optical crystal, growth method and application thereof | |
| JP3816591B2 (en) | Method for producing bismuth-substituted rare earth iron garnet single crystal film | |
| JPH09202697A (en) | Production of bismuth-substituted type garnet | |
| JPH05117095A (en) | Production of bismuth-substituted rare earth iron garnet | |
| Laudise | Single crystals for bubble domain memories | |
| JP4874921B2 (en) | Magneto-optical element, manufacturing method thereof, and optical device manufactured using the same | |
| JP2756273B2 (en) | Oxide garnet single crystal and method for producing the same | |
| CN113463196B (en) | Super-thick garnet single crystal film prepared by liquid phase epitaxy method and preparation method thereof | |
| JP2018095486A (en) | Bismuth-substituted type rare earth iron garnet crystal film, production method thereof, and optical isolator | |
| JPS62138396A (en) | Magnetic garnet material for magneto-optical element | |
| Gualtieri | Liquid phase epitaxy of yttrium aluminum garnet: Reduction of growth rate by germanium oxide | |
| JPH1192290A (en) | Bismuth substituted type garnet thick film material and its production | |
| JPH10139596A (en) | Single crystal substrate | |
| JPH11116396A (en) | Bismuth-substituted type garnet material and its production | |
| JPH1192292A (en) | Bismuth substituted type garnet single crystal thick film material and its production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |