CN115161776B - Method for etching YIG film by laser-induced chemical vapor phase - Google Patents
Method for etching YIG film by laser-induced chemical vapor phase Download PDFInfo
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- CN115161776B CN115161776B CN202210616876.3A CN202210616876A CN115161776B CN 115161776 B CN115161776 B CN 115161776B CN 202210616876 A CN202210616876 A CN 202210616876A CN 115161776 B CN115161776 B CN 115161776B
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- 238000005530 etching Methods 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000000126 substance Substances 0.000 title claims abstract description 12
- 239000012808 vapor phase Substances 0.000 title description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000010931 gold Substances 0.000 claims abstract description 22
- 229910052737 gold Inorganic materials 0.000 claims abstract description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052802 copper Inorganic materials 0.000 claims abstract description 20
- 239000010949 copper Substances 0.000 claims abstract description 20
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 238000004528 spin coating Methods 0.000 claims abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- UEJQQMLXZQUJHF-UHFFFAOYSA-L [K+].[I+].[I-].[I-] Chemical compound [K+].[I+].[I-].[I-] UEJQQMLXZQUJHF-UHFFFAOYSA-L 0.000 claims description 4
- 238000013461 design Methods 0.000 claims description 4
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000010408 film Substances 0.000 claims 8
- 238000001182 laser chemical vapour deposition Methods 0.000 claims 1
- 239000010409 thin film Substances 0.000 claims 1
- 238000003486 chemical etching Methods 0.000 abstract description 6
- 238000001312 dry etching Methods 0.000 abstract description 6
- 238000007747 plating Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000001259 photo etching Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000001039 wet etching Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- 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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/12—Etching in gas atmosphere or plasma
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Plasma & Fusion (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- ing And Chemical Polishing (AREA)
- Drying Of Semiconductors (AREA)
Abstract
The invention discloses a method for performing laser-induced chemical vapor etching on YIG film, which comprises the following steps: sequentially plating copper film and gold film on YIG film substrate as mask layer, spin-coating photoresist, exposing, developing to obtain pre-etched pattern, chemically etching YIG film etching window by using laser-induced HCl, HF, ar mixed gas, and sequentially stripping photoresist, copper film and gold film to obtain YIG film with preset pattern; according to the invention, the copper film and the gold film are used as mask layers, and the laser physical etching and the chemical etching of the HCl and HF mixed gas are organically combined to carry out dry etching on the YIG film, so that a non-etching window area is effectively protected, and the etching precision and speed are improved.
Description
Technical Field
The invention relates to the technical field of processing of microwave devices formed by ferrite YIG films, in particular to a method for forming a metal pattern on the surface of a YIG film by laser-induced chemical vapor etching.
Background
Etching patterns on the surface of YIG film is an important technical approach for realizing the development of microwave devices to miniaturization, chip type and integration. At present, the method for realizing YIG film etching comprises dry etching and wet etching, wherein the dry etching adopts ion beams to bombard the surface of the YIG film, so that part of material atoms are sputtered to realize the etching purpose, and the method has the advantages of high etching precision and good process stability, but the pure physical etching has the defects of low etching speed, large substrate damage and high etching cost; the wet etching is carried out by using hot concentrated phosphoric acid to dissolve YIG under the protection of mask materials, and has the advantages of high etching speed and low cost, but the chemical etching has the defects of serious lateral etching, low etching precision, reduced substrate performance and the like.
For the technical defects, chinese patent publication No. CN109811325B discloses a magnetic transducer of a magnonic crystal and a preparation method thereof, wherein a design pattern is formed on a YIG film by adopting a photoetching method, and a metallization pattern is obtained by plating platinum on the pattern by adopting a magnetron sputtering method. The pattern transfer technology is simple to operate, however, the etching efficiency and the precision are low, the depth-to-width ratio can not meet the design requirement of a device, uneven and discontinuous plating layers are easy to occur when the surface is metallized, the adhesion with a substrate is not firm, the inventor tries the method, as a result, YIG etching can not be realized, the manufactured device is easy to generate harmonic waves, and the insertion loss is larger.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for etching a YIG film by laser-induced chemical vapor phase with stable and rapid etching rate and high precision, and a controllable groove pattern is formed on the surface of the YIG film.
The invention provides a method for etching YIG film by laser-induced chemical vapor phase, which relates to the technical principle that: the plasma laser is utilized to bombard the surface of the YIG film, and the reactive particles at the collision interface are activated while physical etching is generated, so that the YIG film and the reactive etching gas are subjected to chemical etching, and the chemical etching rate is further accelerated due to the heat released by the etching point at the laser focusing position, so that the dry etching effect of organically combining the physical etching and the chemical etching is achieved.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method of laser-induced chemical vapor etching YIG films, comprising the steps of:
(1) Taking a YIG film as a substrate, and adopting a magnetron sputtering method to sequentially copper-plate the substrate to form a copper mask layer and gold-plate the substrate to form a gold mask layer;
(2) Spin-coating photoresist on the substrate prepared in the step (1), sequentially exposing and developing to form a design pattern, and then using Ar+ laser as a light source and Ar gas as a carrier to induce HCl and HF mixed gas to chemically etch a window;
in the step, ar gas is used as a carrier, and a YIG film is etched by adopting HCl and HF mixed gas with proper proportion, because the etching speed of single HCl or HF gas is slower, the laser radiation time is prolonged, and the substrate is damaged.
(3) And (3) separating and cleaning the YIG film from the photoresist, the copper mask layer and the gold mask layer in the step (2) to obtain the etched YIG film.
By using the copper film and the gold film as mask layers, the laser physical etching and the chemical etching of the HCl and HF mixed gas are organically combined to carry out dry etching on the YIG film, thereby effectively protecting a non-etching window area and improving etching precision and speed.
As a preferable technical scheme, in the step (1), the roughness of the YIG film surface is less than or equal to 50nm, the thickness is 50-300 mu m, the thickness of the sputtered copper mask layer is 20-60nm, and the thickness of the sputtered gold mask layer is 20-40nm. The thickness can realize the mask function, and is common, and excessive thickness and excessive thinness can cause cost increase.
As a preferable technical scheme, the photoresist in the step (2) is a positive photoresist, and the spin-coating thickness is 1-2 mu m.
As a preferable technical scheme, in the step (2), the power of the Ar+ laser source is 50-200W, the speed is 100-1000mm/s, the volume ratio of the etching mixed gas HCl, HF, ar is 6:1:1-1:1:1, the gas flow is 10-100 sccm, the pressure is 1-30Pa, and the etching depth is 0.5-100 mu m and the etching width is 10-100 mu m.
As an preferable technical scheme, in the separation method of the YIG film, the photoresist and the mask layer in the step (3), firstly, acetone is adopted to strip the photoresist, then a gold etching solution potassium iodide-iodine is used to etch the gold mask layer, the copper mask layer and the YIG film are not etched, and finally, dilute nitric acid or dilute sulfuric acid solution is used to etch the copper mask layer.
The method comprises the steps of removing a gold mask layer by utilizing chemical inertness of copper and YIG in a potassium iodide-iodine etching solution, and removing a copper mask layer by utilizing chemical inertness of YIG in a dilute nitric acid solution.
Compared with the prior art, the invention has the beneficial effects that:
the method realizes high-efficiency, high-precision and low-cost etching of the YIG film by combining laser induction with the mixed etching gas, and can realize etching rate control by adjusting laser power and etching mixed gas proportion so as to meet the requirements of actual etching depth and width, and has the advantages of simple operation, strong controllability and dry etching, thereby ensuring the accuracy of etching patterns.
Drawings
FIG. 1 is a process flow diagram of example 1 of the present invention;
FIG. 2 is a side view of YIG etched pattern obtained in example 1 of the present invention under an optical microscope;
FIG. 3 is a surface view of YIG etched pattern obtained in example 1 of the present invention under an optical microscope;
in the figure: 1. YIG single crystal film; 2. a copper mask layer; 3. a gold mask layer; 4. a photoresist; 5. a groove.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Example 1:
a method for laser-induced chemical vapor etching YIG film, as shown in FIG. 1, comprises the following steps:
(1) Taking a YIG single crystal film 1 with the thickness of 100 mu m as a substrate, adopting a magnetron sputtering method to sequentially sputter a copper film with the thickness of 40nm on the substrate as a copper mask layer 2, and sputtering a gold layer with the thickness of 30nm as a gold mask layer 3;
(2) Preparing PR1-1000A positive photoresist with the thickness of 1.8 mu m on a substrate by spin coating, sequentially exposing and developing a photoetching pattern, then taking Ar+ laser as a light source, selecting 150W power, setting the speed to be 500mm/s, selecting etching mixed gas HCl, HF, ar with the volume ratio of 3:1:1, setting the gas flow to be 60 sccm and setting the pressure to be 10Pa; after etching, YIG groove depth is 22 μm and width is 50 μm. According to an etching rate calculation formula er=Δt/T, wherein: ER represents etching rate in μm/min; Δt represents the etching amount, unit um or a; t represents etching time per unit min, so that the etching rate is calculated to be 0.6 mu m/min;
(3) In order to separate the YIG single crystal film 1 from the photoresist 4 and the mask layer in the step (2), the specific method comprises the following steps: firstly, stripping the photoresist 4 by using acetone, corroding a gold mask layer by using gold etching solution potassium iodide-iodine, checking the removal condition of the gold layer under a microscope, after the gold layer is completely removed, cleaning by using deionized water, corroding the copper mask layer by using dilute nitric acid solution until copper is completely removed, and finally washing by using deionized water and absolute ethyl alcohol in sequence, and airing to obtain the etched YIG film.
YIG etching patterns prepared by the laser-induced chemical vapor etching are shown in fig. 2 and 3, and the depth 22.003 μm and the width 51.471 μm of the etching groove are clear in outline, free of pattern distortion and good in processing effect.
Example 2
Based on example 1, the power in step (2) was changed to 50W only in this example, and the etching rate was 0.15 μm/min in the same manner as in example 1.
Example 3
Based on example 1, only the power in step (2) was changed to 200W in this example, and the etching rate was 0.8 μm/min in the same manner as in example 1.
Example 4
Based on example 1, only the volume ratio of the etching mixture gas HCl, HF, ar in step (2) was changed to 1:1:1 in this example, and the etching rate was 0.22 μm/min in the rest of the same as in example 1.
Example 5
Based on the embodiment 1, only the volume ratio of the etching mixed gas HCl, HF, ar in the step (2) is changed to 6:1:1, and the rest is the same as the embodiment 1, wherein the etching rate is 0.4 mu m/min.
Example 6
Based on example 1, only the gas flow rate in step (2) was changed to 10 sccm in this example, and the etching rate was 0.13 μm/min in the same manner as in example 1.
Example 7
Based on example 1, only the gas flow rate in step (2) was changed to 100sccm in this example, and the etching rate was 0.55 μm/min in the same manner as in example 1.
Example 8
Based on example 1, in this example, only the pressure was set to 1 Pa in step (2), and the etching rate was 0.2 μm/min in the same manner as in example 1.
Example 9
Based on example 1, in this example, only the pressure was set to 30Pa in step (2), and the etching rate was 0.6 μm/min in the same manner as in example 1.
Comparative example 1
Based on example 1, only the etching mixture gas in step (2) was changed to HCl and Ar in the volume ratio of 3:1 in this example, and the etching rate was 0.05 μm/min in the rest of the same as in example 1.
Comparative example 2
Based on example 1, in this example, only the etching mixture gas in step (2) was changed to HF, ar at a volume ratio of 1:1, and the remainder was the same as in example 1, with an etching rate of 0.08 μm/min.
The above embodiments are only some of the embodiments of the present invention, and are not intended to limit the present invention, but any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. A method for laser-induced chemical vapor etching YIG thin film, comprising the steps of:
(1) Taking a YIG film as a substrate, and adopting a magnetron sputtering method to sequentially copper-plate the substrate to form a copper mask layer and gold-plate the substrate to form a gold mask layer;
(2) Spin-coating photoresist on the substrate prepared in the step (1), sequentially exposing and developing to form a design pattern, and then using Ar+ laser as a light source and Ar gas as a carrier to induce HCl and HF mixed gas to chemically etch a window; the volume ratio of the etching mixed gas HCl, HF, ar is 6:1:1-1:1:1;
(3) And (3) separating and cleaning the YIG film from the photoresist, the copper mask layer and the gold mask layer in the step (2) to obtain the etched YIG film.
2. The method of claim 1, wherein in step (1), the roughness of the YIG film surface is less than or equal to 50nm, the thickness is 50-300 μm, the thickness of the copper mask layer is 20-60nm, and the thickness of the gold mask layer is 20-40nm.
3. The method of claim 1, wherein the photoresist in step (2) is a positive photoresist, and the spin-on thickness is 1-2 μm.
4. The method for etching YIG film according to claim 1, wherein in the step (2), the Ar+ laser source power is 50-200W, the rate is 100-1000mm/s, the gas flow is 10-100 sccm, the pressure is 1-30Pa, the etching depth is 0.5-100 μm, and the etching width is 10-100 μm.
5. The method for etching YIG film by laser-induced chemical vapor deposition according to claim 1, wherein in the step (3), the YIG film is separated from the photoresist and the mask layer by stripping the photoresist with acetone, etching the gold mask layer with gold etchant such as potassium iodide-iodine, and etching the copper mask layer and YIG film with dilute nitric acid or dilute sulfuric acid solution.
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CN202210616876.3A CN115161776B (en) | 2022-06-01 | 2022-06-01 | Method for etching YIG film by laser-induced chemical vapor phase |
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CN202210616876.3A CN115161776B (en) | 2022-06-01 | 2022-06-01 | Method for etching YIG film by laser-induced chemical vapor phase |
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CN115161776B true CN115161776B (en) | 2023-11-07 |
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH03150378A (en) * | 1989-11-07 | 1991-06-26 | Nippon Telegr & Teleph Corp <Ntt> | Method for etching garnet |
JPH08325756A (en) * | 1995-05-30 | 1996-12-10 | Sharp Corp | Method for processing ferrite |
US5874011A (en) * | 1996-08-01 | 1999-02-23 | Revise, Inc. | Laser-induced etching of multilayer materials |
CN104536262A (en) * | 2015-01-11 | 2015-04-22 | 南昌航空大学 | Method for manufacturing binary optical element with transparent ceramic as substrate material |
CN113337894A (en) * | 2021-05-21 | 2021-09-03 | 中国科学院上海光学精密机械研究所 | Cerium-doped yttrium aluminum garnet scintillation crystal surface moth eye type microstructure and preparation method thereof |
-
2022
- 2022-06-01 CN CN202210616876.3A patent/CN115161776B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH03150378A (en) * | 1989-11-07 | 1991-06-26 | Nippon Telegr & Teleph Corp <Ntt> | Method for etching garnet |
JPH08325756A (en) * | 1995-05-30 | 1996-12-10 | Sharp Corp | Method for processing ferrite |
US5874011A (en) * | 1996-08-01 | 1999-02-23 | Revise, Inc. | Laser-induced etching of multilayer materials |
CN104536262A (en) * | 2015-01-11 | 2015-04-22 | 南昌航空大学 | Method for manufacturing binary optical element with transparent ceramic as substrate material |
CN113337894A (en) * | 2021-05-21 | 2021-09-03 | 中国科学院上海光学精密机械研究所 | Cerium-doped yttrium aluminum garnet scintillation crystal surface moth eye type microstructure and preparation method thereof |
Non-Patent Citations (2)
Title |
---|
Preparation of two-dimensional yttrium iron garnet magnonic crystal on porous silicon substrate;H. Zheng;Materials Letters;第123卷;181-183 * |
厘米尺寸YIG晶体生长研究;马健;中国优秀硕士学位论文全文数据库工程科技Ⅰ辑(第2期);B014-3555 * |
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