CN112410885A - Lithium niobate single crystal film and manufacturing method thereof - Google Patents

Lithium niobate single crystal film and manufacturing method thereof Download PDF

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Publication number
CN112410885A
CN112410885A CN202011250278.6A CN202011250278A CN112410885A CN 112410885 A CN112410885 A CN 112410885A CN 202011250278 A CN202011250278 A CN 202011250278A CN 112410885 A CN112410885 A CN 112410885A
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lithium niobate
dielectric layer
layer
single crystal
wafer
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周赤
吉贵军
刘昆
张大鹏
王兴龙
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Zhuhai Guangku Technology Co ltd
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Zhuhai Guangku Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B31/00Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
    • C30B31/20Doping by irradiation with electromagnetic waves or by particle radiation
    • C30B31/22Doping by irradiation with electromagnetic waves or by particle radiation by ion-implantation
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/22Complex oxides
    • C30B29/30Niobates; Vanadates; Tantalates
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/68Crystals with laminate structure, e.g. "superlattices"
    • GPHYSICS
    • G02OPTICS
    • G02FOPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/03Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on ceramics or electro-optical crystals, e.g. exhibiting Pockels effect or Kerr effect
    • G02F1/035Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on ceramics or electro-optical crystals, e.g. exhibiting Pockels effect or Kerr effect in an optical waveguide structure

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Nonlinear Science (AREA)
  • Electromagnetism (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Optical Modulation, Optical Deflection, Nonlinear Optics, Optical Demodulation, Optical Logic Elements (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Optical Integrated Circuits (AREA)

Abstract

The invention provides a lithium niobate single crystal thin film and a manufacturing method thereof, wherein the manufacturing method comprises the following steps: preparing a dielectric layer on the optical-level surface of a raw material lithium niobate wafer; injecting ions towards the optical surface through the dielectric layer, forming an ion layer after the ions penetrate the optical surface, and forming a single crystal lithium niobate thin layer between the ion layer and the dielectric layer; bonding the carrier wafer with the dielectric layer; heating to a first preset temperature to separate the single crystal lithium niobate thin layer from the raw material lithium niobate wafer and keep the single crystal lithium niobate thin layer on the dielectric layer; heating to a second preset temperature, wherein the second preset temperature is higher than the first preset temperature. The single crystal lithium niobate thin layer is separated from the raw material lithium niobate wafer and is firmly positioned on the dielectric layer, so that stable optical waveguide can be realized.

Description

Lithium niobate single crystal film and manufacturing method thereof
Technical Field
The invention relates to the field of photoelectric semiconductor materials, in particular to a lithium niobate single crystal film and a manufacturing method thereof.
Background
The lithium niobate single crystal has excellent transmission performance, electro-optic performance, nonlinear optical performance and piezoelectric performance, and is widely applied to optical communication, data center optical interconnection and high-frequency filtering devices. The nanometer thin film lithium niobate single crystal on other material substrate has the excellent characteristics, and can be used for integrated devices, which is a novel hopeful integrated optical material. However, growing lithium niobate single crystal thin films on other substrate materials has proven difficult to achieve, whereas mechanical slicing techniques have difficulty in producing thin films of nanometer-scale thickness.
The lithium niobate single crystal film prepared by using Smart-Cut technology in recent years makes the mass production of thin film lithium niobate wafers possible. The method comprises the following general steps: firstly, polishing the surface of a raw material lithium niobate wafer to meet the requirements of wafer bonding, simultaneously preparing another carrier wafer, such as a silicon (Si) wafer, preparing a buffer layer, such as silicon dioxide (SiO2), on the carrier wafer, polishing to enable the buffer layer to meet the requirements of wafer bonding, then performing ion implantation with specific energy and specific measurement, such as helium ions (He +), on the polished surface of the raw material lithium niobate wafer, then bonding the polished surface of the raw material wafer and the polished surface of the carrier wafer, heating the two wafers after bonding to enable the implanted ions to be compounded into micro bubbles, separating the raw material lithium niobate wafer after expansion, and leaving a lithium niobate film on the carrier wafer.
In the method for preparing the lithium niobate thin film wafer, the most critical and difficult step is how to form a bond with sufficient strength between the lithium niobate wafer and the silicon dioxide film layer of the bearing wafer. Since the optical waveguide to be subsequently fabricated is based on this bonding interface, the optical waveguide structure may be damaged if the bonding strength is insufficient to cause cracking or peeling. Therefore, how to increase the bonding strength between the lithium niobate wafer and the silicon dioxide film on the surface of the carrier wafer is always a key factor influencing the yield of the production process.
Disclosure of Invention
The first purpose of the present invention is to provide a method for forming a firmly bonded lithium niobate single crystal thin film on a hetero wafer.
The second purpose of the invention is to provide a lithium niobate single crystal thin film which is firmly bonded on a heterogeneous wafer.
In order to achieve the first object of the present invention, the present invention provides a method for producing a lithium niobate single crystal thin film, comprising:
preparing a dielectric layer on the optical-level surface of a raw material lithium niobate wafer;
injecting ions towards the optical surface through the dielectric layer, forming an ion layer after the ions penetrate the optical surface, and forming a single crystal lithium niobate thin layer between the ion layer and the dielectric layer;
bonding the carrier wafer with the dielectric layer;
heating to a first preset temperature to separate the single crystal lithium niobate thin layer from the raw material lithium niobate wafer and keep the single crystal lithium niobate thin layer on the dielectric layer;
heating to a second preset temperature, wherein the second preset temperature is higher than the first preset temperature.
In a further aspect, after forming the thin lithium niobate monocrystal layer and before bonding the carrier wafer and the dielectric layer, the method further includes: and polishing the dielectric layer.
In a further aspect, after the dielectric layer is polished, the manufacturing method further includes: a cleaning process is performed.
In a further embodiment, the first predetermined temperature is 200 ℃ to 230 ℃.
In a further embodiment, the second predetermined temperature is 250 ℃ to 350 ℃.
In order to achieve the second object of the present invention, the present invention provides a lithium niobate single crystal thin film, which is produced by the above-mentioned production method; the lithium niobate single crystal film comprises a lithium niobate thin film layer, a dielectric layer and a carrier wafer which are sequentially arranged in a laminated manner, wherein the lithium niobate thin film layer is combined with a plated film of the dielectric layer, and the dielectric layer is bonded with the carrier wafer.
According to the scheme, through the lithium niobate single crystal thin film and the manufacturing method thereof, the firmly attached dielectric layer is formed on the raw material lithium niobate wafer in a film coating mode, then the wafer with the dielectric layer is subjected to ion implantation, is bonded with the bearing wafer, is heated to enable the ion implantation layer to be gasified, and the lithium niobate thin film layer, the dielectric layer and the bearing wafer are sequentially formed on the bearing wafer after being stripped. The single crystal lithium niobate thin layer is separated from the raw material lithium niobate wafer and firmly positioned on the dielectric layer, so that the firmness is much higher compared with an interface formed by direct bonding in other methods, and the stable optical waveguide can be realized by utilizing the key interfaces of the lithium niobate thin layer and the dielectric layer.
Drawings
FIG. 1 is a flowchart of an embodiment of the method for producing a lithium niobate single crystal thin film of the present invention.
FIG. 2 is a schematic structural diagram of a raw material lithium niobate wafer in an embodiment of the method for manufacturing a lithium niobate single crystal thin film of the present invention.
FIG. 3 is a schematic structural diagram of a raw material lithium niobate wafer and a dielectric layer in an embodiment of the method for manufacturing a lithium niobate single crystal thin film of the present invention.
FIG. 4 is a schematic structural view of a lithium niobate single crystal thin film forming method of the present invention in which an ion implanted layer is formed.
FIG. 5 is a graph showing the relationship between the implantation depth and the ion energy in the example of the method for producing a lithium niobate single crystal thin film of the present invention.
FIG. 6 is a schematic structural diagram of a bonded carrier wafer in an embodiment of the method for producing a lithium niobate single crystal thin film according to the present invention.
FIG. 7 is a schematic structural diagram of an embodiment of a lithium niobate single crystal thin film of the present invention.
The invention is further explained with reference to the drawings and the embodiments.
Detailed Description
Referring to fig. 1 and 2, when the method for manufacturing a lithium niobate single crystal thin film is performed, step S11 is performed first to provide a raw material lithium niobate wafer 100, which is made of single crystal lithium niobate and has an optical-grade surface 101 formed on a lower surface thereof by grinding, and then step S12 is performed, referring to fig. 3, a dielectric layer 400 is prepared on the optical-grade surface of the raw material lithium niobate wafer by using a plating method, the dielectric layer may be formed by using various commercial plating techniques, and the dielectric layer 400 has a surface 401 on a side opposite to the wafer.
Then, step S13 is executed, referring to fig. 4, ions are implanted from one side of the surface 401 through the dielectric layer 400 toward the optical-level surface of the raw material lithium niobate wafer 100, the ions may be implanted by helium ions (He +), and the ions penetrate the optical-level surface and stay at a predetermined depth on the wafer surface, so as to form an ion layer 200, and form a single-crystal lithium niobate thin layer 300 with a predetermined thickness between the ion layer and the dielectric layer. Specifically, the sum of the thicknesses of the dielectric layer 400 and the single-crystal lithium niobate thin layer 300 can be calculated according to the energy of ions, the collision cross section of ions in the target medium, and the properties of the target medium, and the result of the calculation of the penetration depth of helium ions (He +) into a single lithium niobate crystal coated with 1 micrometer (1 μm) thick silicon dioxide (SiO2) can be obtained with reference to fig. 5.
Then, step S14 is executed, after ion implantation is completed, the dielectric layer 400 is polished to meet the requirements of the smoothness and flatness of wafer bonding, and then step S15 is executed to perform cleaning, specifically, the polished dielectric layer 400 and the raw material lithium niobate wafer 100 are cleaned, organic contamination, particles, metal and other contamination on the wafer surface can be respectively removed by using a standard semiconductor wafer cleaning solution, such as RCA, and then are cleaned and dried by deionized water, spin-dried or heated and dried.
Subsequently, step S16 is performed to prepare another carrier wafer 500, where the carrier wafer 500 may be a silicon (Si) wafer having an optical-grade surface, and bond the carrier wafer 500 with the polished surface 401 of the dielectric layer 400, so as to form a single-crystal lithium niobate thin layer 300 as shown in fig. 6, where the carrier wafer 500 includes the raw lithium niobate wafer 100, the dielectric layer 400, and the carrier wafer 500, which are sequentially stacked, the raw lithium niobate wafer 100 is formed with the ionic layer 200 on a side close to the dielectric layer, and the ionic layer 200 and the dielectric layer 400 are formed therebetween. Then, step S17 is executed, the bonded wafer is slowly heated to a first preset temperature, which may be 200 to 230 ℃, so that ions in the ionic layer are polymerized into micro-bubbles, the ionic layer is separated at the raw material lithium niobate wafer 100 under the action of the bubbles, the lithium niobate single crystal thin film layer 300 with a specific thickness remains on the dielectric layer 400 bonded on the carrier wafer, and the lithium niobate thin film layer is combined with the dielectric layer coating film.
And finally, executing a step S18, slowly heating the lithium niobate single crystal film with the lithium niobate thin film layer 300, the dielectric layer 400 and the carrier wafer 500 to a second preset temperature, wherein the second preset temperature can be 250-350 ℃, and the second preset temperature is higher than the first preset temperature, repairing the internal damage of the crystal possibly caused by ion implantation, releasing stress, further improving the bonding strength of the wafer, and obtaining the final lithium niobate thin film wafer.
In view of the separation of the raw material lithium niobate wafer 100, the lithium niobate single crystal thin film shown in fig. 7 is formed, and comprises a lithium niobate thin film layer 300, a dielectric layer 400 and a carrier wafer 500 which are sequentially stacked, wherein the lithium niobate thin film layer is combined with a plated film of the dielectric layer, the dielectric layer is bonded with the carrier wafer, and the lithium niobate thin film layer 300 can realize stable optical waveguide.
According to the lithium niobate single crystal thin film and the manufacturing method thereof, the firmly attached dielectric layer is formed on the raw material lithium niobate wafer in a film coating mode, then the wafer with the dielectric layer is subjected to ion implantation, is bonded with the bearing wafer, is heated to gasify the ion implantation layer, and forms the structures of the lithium niobate thin film layer, the dielectric layer and the bearing wafer on the bearing wafer in sequence after being stripped. The single crystal lithium niobate thin layer is separated from the raw material lithium niobate wafer and firmly positioned on the dielectric layer, so that the firmness is much higher compared with an interface formed by direct bonding in other methods, and the stable optical waveguide can be realized by utilizing the key interfaces of the lithium niobate thin layer and the dielectric layer.

Claims (6)

1. The method for producing a lithium niobate single crystal thin film is characterized by comprising:
preparing a dielectric layer on the optical-level surface of a raw material lithium niobate wafer;
injecting ions towards the optical-grade surface through the dielectric layer, forming an ion layer after the ions penetrate through the optical-grade surface, and forming a single-crystal lithium niobate thin layer between the ion layer and the dielectric layer;
bonding a carrier wafer with the dielectric layer;
heating to a first preset temperature to separate the single crystal lithium niobate thin layer from the raw material lithium niobate wafer and keep the single crystal lithium niobate thin layer on the dielectric layer;
heating to a second preset temperature, wherein the second preset temperature is higher than the first preset temperature.
2. The method of manufacturing according to claim 1, wherein:
after the ion implantation and before the bonding of the carrier wafer and the dielectric layer, the manufacturing method further comprises:
and polishing the dielectric layer.
3. The method of manufacturing according to claim 2, wherein:
after the dielectric layer is polished, the manufacturing method further comprises the following steps:
a cleaning process is performed.
4. The production method according to any one of claims 1 to 3, characterized in that:
the first preset temperature is 200 ℃ to 230 ℃.
5. The production method according to any one of claims 1 to 3, characterized in that:
the second preset temperature is 250 ℃ to 350 ℃.
6. A lithium niobate single crystal thin film produced by the production method according to any one of claims 1 to 5;
the lithium niobate single crystal film comprises a lithium niobate thin film layer, a dielectric layer and a carrier wafer which are sequentially arranged in a laminated manner, wherein the lithium niobate thin film layer is combined with the dielectric layer through coating, and the dielectric layer is bonded with the carrier wafer.
CN202011250278.6A 2020-11-10 2020-11-10 Lithium niobate single crystal film and manufacturing method thereof Pending CN112410885A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06256093A (en) * 1993-03-01 1994-09-13 Ibiden Co Ltd Single crystal thin film of lithium niobate
CN104752308A (en) * 2013-12-26 2015-07-01 中国科学院上海微系统与信息技术研究所 Method of preparing on-insulator material based on hybrid heating
CN104862784A (en) * 2014-06-09 2015-08-26 济南晶正电子科技有限公司 Method for manufacturing monocrystalline film with near stoichiometric ratio
CN110010755A (en) * 2019-03-13 2019-07-12 电子科技大学 Preparation method, monocrystal thin films and the resonator of monocrystal thin films with buffer layer

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06256093A (en) * 1993-03-01 1994-09-13 Ibiden Co Ltd Single crystal thin film of lithium niobate
CN104752308A (en) * 2013-12-26 2015-07-01 中国科学院上海微系统与信息技术研究所 Method of preparing on-insulator material based on hybrid heating
CN104862784A (en) * 2014-06-09 2015-08-26 济南晶正电子科技有限公司 Method for manufacturing monocrystalline film with near stoichiometric ratio
CN110010755A (en) * 2019-03-13 2019-07-12 电子科技大学 Preparation method, monocrystal thin films and the resonator of monocrystal thin films with buffer layer

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Application publication date: 20210226