CN111850692A - Lithium niobate self-supporting film and preparation method thereof - Google Patents
Lithium niobate self-supporting film and preparation method thereof Download PDFInfo
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- CN111850692A CN111850692A CN202010645070.8A CN202010645070A CN111850692A CN 111850692 A CN111850692 A CN 111850692A CN 202010645070 A CN202010645070 A CN 202010645070A CN 111850692 A CN111850692 A CN 111850692A
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL 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
- G02F1/00—Devices 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
- G02F1/35—Non-linear optics
- G02F1/355—Non-linear optics characterised by the materials used
- G02F1/3551—Crystals
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/30—Niobates; Vanadates; Tantalates
Abstract
The invention discloses a preparation method of a lithium niobate self-supporting film, which comprises the following steps: obtaining a lithium niobate single crystal wafer with a polished surface; obtaining a high-resistance substrate, and depositing a dielectric layer on the high-resistance substrate; etching a groove on the surface of the dielectric layer; bonding the polished surface of the lithium niobate single crystal wafer and the surface of the dielectric layer with the groove to form a first composite structure; thinning the first composite structure to obtain a second composite structure; carrying out surface treatment on the second composite structure to obtain a third composite structure; and putting the third composite structure into a treatment liquid for corrosion to obtain the lithium niobate self-supporting film. The quality of the lithium niobate self-supporting film obtained by the method is the same as that of a lithium niobate single crystal wafer, so that the problem of film defects caused by the ion beam effect in the prior art for preparing the lithium niobate film is solved.
Description
Technical Field
The invention relates to the technical field of semiconductor materials, in particular to a lithium niobate self-supporting film and a preparation method thereof.
Background
The lithium niobate crystal is a multifunctional material integrating the performances of piezoelectricity, ferroelectricity, pyroelectricity, nonlinearity, electro-light, photorefractivity and the like, and has good thermal stability and chemical stability; due to their large size and low preparation cost, lithium niobate crystals have gradually become important functional new materials in the field of materials. At present, lithium niobate crystals have been widely and practically applied in infrared detectors, laser modulators, optical communication modulators, optical switches, optical parametric oscillators, integrated optical elements, high-frequency broadband filters, narrow-band filters, high-frequency high-temperature transducers, micro-acoustic devices, laser frequency multipliers, self-frequency doubling lasers, photorefractive devices (such as high-resolution holographic storage), optical waveguide substrates, optical isolators and the like, and are known as one of the main candidate substitute materials for optical silicon in the optical electronics era. Periodic polarization (periodically poled LiNbO3, PPLN) based on the lithium niobate crystal quasi-phase matching technology can utilize the effective nonlinear coefficient to the maximum extent, is widely applied to optical processes such as frequency doubling, sum frequency/difference frequency, optical parametric oscillation and the like, has wide application prospect in the fields of laser display and optical communication, and becomes a very popular nonlinear optical material.
However, since the device manufacturing process of lithium niobate crystal is costly, the etching process is difficult, and the current most popular Complementary Metal Oxide Semiconductor (CMOS) process cannot be compatible, the chip integration on the system is difficult to realize, so that the lithium niobate crystal is prevented from exerting the optimal material characteristics. In order to solve the problem, the lithium niobate thin film (LNOI) prepared by the ion beam cutting and layer transfer technology provides a good solution, but due to the damage effect of the ion beam on the crystal, a large number of defects still exist even after the crystal performance is recovered, and the performance of the lithium niobate thin film as an optical device is limited.
Disclosure of Invention
The invention aims to solve the problem of film defects caused by the damage effect of ion beams on crystals when a lithium niobate film is prepared based on ion beam cutting and layer transfer technologies.
In order to solve the technical problem, the embodiment of the invention discloses a preparation method of a lithium niobate self-supporting film, which comprises the following steps:
obtaining a lithium niobate single crystal wafer with a polished surface; obtaining a high-resistance substrate, and depositing a dielectric layer on the high-resistance substrate; etching a groove on the surface of the dielectric layer; bonding the polished surface of the lithium niobate single crystal wafer and the surface of the dielectric layer with the groove to form a first composite structure; thinning the first composite structure to obtain a second composite structure; carrying out surface treatment on the second composite structure to obtain a third composite structure; and putting the third composite structure into a treatment liquid for corrosion to obtain the lithium niobate self-supporting film.
Further, the thickness of the lithium niobate single crystal wafer is 200 micrometers to 500 micrometers; the surface roughness of the polished surface of the lithium niobate single crystal wafer is less than 1 nanometer; the size of the lithium niobate single crystal wafer is 2 inches to 6 inches.
Further, the high-resistance substrate is a silicon wafer, silicon carbide or gallium nitride; the dielectric layer is a tantalum oxide layer, a titanium dioxide layer, a barium titanate layer, a zirconium dioxide layer, a hafnium dioxide layer, an aluminum oxide layer or a silicon oxide layer.
Further, the thickness of the dielectric layer is 5 to 500 nanometers; the surface roughness of the dielectric layer is less than 1 nanometer.
Further, the number of the grooves is multiple, and each groove has the same size; the length of the groove is 10-500 micrometers, the depth is 50-200 nanometers, and the width is 1-50 micrometers; the distance between every two adjacent grooves is 20 micrometers to 100 micrometers.
Further, the surface bonding mode of the polished surface of the lithium niobate single crystal wafer and the dielectric layer with the groove is a surface activation bonding mode, a metal bonding mode or an anodic bonding mode; the conditions of the bonding mode are as follows: vacuum 1E-7 Pa, pressure 16 MPa and temperature 25-200 deg.C.
Further, the thinning treatment method is a grinding method or a wet etching method.
Further, the surface treatment method is a chemical mechanical polishing method, a plasma etching method, an ion sputtering method or a chemical etching method.
Further, the treatment liquid is aqueous hydrogen fluoride or aqueous sodium hydroxide; the ratio of hydrogen fluoride to water in the hydrogen fluoride aqueous solution is 1: 10 to 1: 100, respectively; the ratio of sodium hydroxide to water in the sodium hydroxide aqueous solution is 1: 1 to 1: 100, respectively; and the treatment time for putting the third composite structure into the treatment liquid for corrosion is 1 second to 24 hours.
The embodiment of the invention also discloses a lithium niobate self-supporting film, which is prepared by adopting the preparation method of any scheme.
By adopting the technical scheme, the preparation method of the lithium niobate self-supporting film and the lithium niobate self-supporting film provided by the embodiment of the invention have the following beneficial effects: the invention obtains the lithium niobate self-supporting film by the following steps: 1. obtaining a lithium niobate single crystal wafer with a polished surface; 2. obtaining a high-resistance substrate, and depositing a dielectric layer on the high-resistance substrate; 3. etching a groove on the surface of the dielectric layer; 4. bonding the polished surface of the lithium niobate single crystal wafer and the surface of the dielectric layer with the groove to form a first composite structure; 5. thinning the first composite structure to obtain a second composite structure; 6, carrying out surface treatment on the second composite structure to obtain a third composite structure; and 7, putting the third composite structure into a treatment liquid for corrosion to obtain the lithium niobate self-supporting film. The obtained lithium niobate self-supporting film has the same quality as a lithium niobate single crystal wafer, thereby solving the problem of film defects caused by the ion beam effect in the prior art for preparing the lithium niobate film. Meanwhile, the lithium niobate self-supporting film obtained by the preparation method of the lithium niobate self-supporting film can be combined with the most common and CMOS compatible silicon substrate at present and can also be integrated with a high-heat-conductivity carborundum (SiC) substrate, so that the available degree of freedom of the film is greatly improved, and the film can fully exert excellent material characteristics.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a process for preparing a lithium niobate self-supporting thin film according to an embodiment of the present invention;
fig. 2 is an operation flowchart of a method for preparing a lithium niobate self-supporting thin film according to an embodiment of the present invention.
The reference numbers in the figures are: 1-lithium niobate single crystal wafer, 11-polished surface, 2-high resistance substrate, 3-dielectric layer and 4-groove.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
Reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic may be included in at least one implementation of the invention. In the description of the embodiments of the present invention, it should be understood that the terms "upper", "lower", "top", "bottom", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only used for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. Moreover, the terms "first," "second," and the like are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein.
As shown in fig. 1 to 2: the embodiment of the invention discloses a preparation method of a lithium niobate self-supporting film, which specifically comprises the following steps:
s1, obtaining a lithium niobate single crystal wafer 1 having a polished surface 11 (the bottom surface is not visible in FIG. 1);
s2, obtaining a high-resistance substrate 2, and depositing a dielectric layer 3 on the high-resistance substrate 2;
s3, etching a groove 4 on the surface of the dielectric layer 3;
s4, bonding the polished surface 11 of the lithium niobate single crystal wafer 1 and the surface of the dielectric layer 3 with the grooves 4 to form a first composite structure;
s5, thinning the first composite structure to obtain a second composite structure;
s6, performing surface treatment on the second composite structure to obtain a third composite structure;
and S7, putting the third composite structure into a treatment liquid for corrosion to obtain the lithium niobate self-supporting film.
The quality of the lithium niobate self-supporting film obtained by the preparation method of the lithium niobate self-supporting film disclosed by the embodiment of the invention is the same as that of the lithium niobate single crystal wafer 1, so that the problem of film defects caused by the ion beam effect in the process of preparing the lithium niobate film in the prior art is solved. Meanwhile, the lithium niobate self-supporting film obtained by the preparation method of the lithium niobate self-supporting film can be combined with the most common and CMOS compatible silicon substrate at present and can also be integrated with a high-heat-conductivity carborundum (SiC) substrate, so that the available degree of freedom of the film is greatly improved, and the film can fully exert excellent material characteristics.
In another embodiment of the present invention, the thickness of the lithium niobate single crystal wafer 1 in step S1 is 200 micrometers to 500 micrometers; the surface roughness of the polished surface 11 of the lithium niobate single crystal wafer 1 is less than 1 nanometer; the size of the lithium niobate single crystal wafer 1 is 2 inches to 6 inches.
In another embodiment of the present invention, the high-resistance substrate 2 in step S2 may be a silicon wafer, silicon carbide or gallium nitride; the dielectric layer 3 can be a tantalum oxide layer, a titanium dioxide layer, a barium titanate layer, a zirconium dioxide layer, a hafnium dioxide layer, an aluminum oxide layer or a silicon oxide layer; the thickness of the dielectric layer 3 is 5 to 500 nanometers; the surface roughness of the dielectric layer 3 is less than 1 nanometer.
In another embodiment of the present invention, the number of the grooves 4 in step S3 is multiple, and each of the grooves 4 has the same size; the length of the groove 4 is 10 micrometers to 500 micrometers, the depth can be 50 nanometers to 200 nanometers, and the width can be 1 micrometer to 50 micrometers; the distance between every two adjacent grooves 4 can be 20 micrometers to 100 micrometers.
In another embodiment of the present invention, the surface bonding method of the polished surface 11 of the lithium niobate single crystal wafer 1 and the dielectric layer 3 having the groove 4 in step S4 may be a surface activation bonding method, a metal bonding method, or an anodic bonding method; the conditions of the bonding mode can be as follows: vacuum 1E-7 Pa, pressure 16 MPa and temperature 25-200 deg.C.
In another embodiment of the present invention, the thinning process in step S5 may be performed by a grinding method or a wet etching method; specifically, the lithium niobate single crystal wafer 1 is thinned, and the thickness of the thinned lithium niobate single crystal wafer 1 is 5 micrometers to 50 micrometers.
In another embodiment of the present invention, the surface treatment method in step S6 may be a chemical mechanical polishing method, a plasma etching method, an ion sputtering method, or a chemical etching method.
In another embodiment of the present invention, the processing liquid in step S7 may be an aqueous hydrogen fluoride solution or an aqueous sodium hydroxide solution; the ratio of hydrogen fluoride to water in the hydrogen fluoride aqueous solution is 1: 10 to 1: 100, respectively; the ratio of sodium hydroxide to water in the sodium hydroxide aqueous solution is 1: 1 to 1: 100, respectively; and the treatment time for putting the third composite structure into the treatment liquid for corrosion is 1 second to 24 hours.
The present invention will be described in more detail below in two specific embodiments in conjunction with the above-mentioned embodiments.
The first embodiment is as follows:
with reference to FIG. 2, the procedure was as follows, namely, obtaining a lithium niobate single crystal wafer having a polished surface, a size of 4 inches, a thickness of 300um (micrometers), and a surface roughness of 0.5nm (nanometers); the method comprises the steps of obtaining a high-resistance silicon substrate with the size of 4 inches, the thickness of 500um and the surface roughness of 0.4nm, depositing a dielectric layer with the thickness of 30nm and the surface roughness of 0.4nm and the component of alumina on the high-resistance silicon, and then forming a plurality of grooves with the length of 50um, the width of 5um and the depth of 100nm on the surface of the dielectric layer by utilizing a photoetching method, wherein the distance between every two adjacent grooves is 25 um. Then, bonding the polished surface of the lithium niobate single crystal wafer and the surface of the dielectric layer with the groove to form a first composite structure; thinning the lithium niobate single crystal wafer from the outer side until the thickness of the lithium niobate single crystal wafer is 20um, and forming a second composite structure after thinning treatment; then carrying out surface polishing treatment on the lithium niobate single crystal wafer with the second composite structure until the roughness is reduced to 0.5nm to obtain a third composite structure; and finally, putting the third composite structure into the treatment liquid for corrosion for 10 minutes, and enabling the dielectric layer to fall off to obtain the lithium niobate single crystal film with the thickness of 20 microns, namely the lithium niobate self-supporting single crystal film.
The first embodiment is as follows:
with reference to FIG. 2, the method comprises the steps of obtaining a lithium niobate single crystal wafer having a polished surface, a size of 6inch, a thickness of 500 μm, and a surface roughness of 0.8 nm; the method comprises the steps of obtaining a high-resistance silicon carbide substrate with the size of 6 inches, the thickness of 300 microns and the surface roughness of 0.4nm, depositing a dielectric layer with the thickness of 10nm and the component of alumina on the high-resistance silicon carbide substrate, and then forming a plurality of grooves with the length of 50 microns, the width of 5 microns and the depth of 200nm on the surface of the dielectric layer by utilizing a photoetching method, wherein the distance between every two adjacent grooves is 20 microns. Then, bonding the polished surface of the lithium niobate single crystal wafer and the surface of the dielectric layer with the groove to form a first composite structure; thinning the lithium niobate single crystal wafer from the outer side until the thickness of the lithium niobate single crystal wafer is 10um, and forming a second composite structure after thinning treatment; then carrying out surface polishing treatment on the lithium niobate single crystal wafer with the second composite structure until the roughness is reduced to 0.5nm to obtain a third composite structure; and finally, putting the third composite structure into the treatment liquid for corrosion for 10 minutes, and enabling the dielectric layer to fall off to obtain a lithium niobate single crystal film with the thickness of 10 microns, namely the 6-inch lithium niobate self-supporting single crystal film.
The embodiment of the invention also provides a lithium niobate self-supporting film obtained by adopting the preparation method related to any one of the embodiments and the implementation modes.
The present invention is not limited to the above preferred embodiments and examples, and any modifications, equivalent replacements, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a lithium niobate self-supporting film is characterized by comprising the following steps:
obtaining a lithium niobate single crystal wafer with a polished surface;
obtaining a high-resistance substrate, and depositing a dielectric layer on the high-resistance substrate;
etching a groove on the surface of the dielectric layer;
bonding the polished surface of the lithium niobate single crystal wafer and the surface of the dielectric layer with the groove to form a first composite structure;
thinning the first composite structure to obtain a second composite structure;
carrying out surface treatment on the second composite structure to obtain a third composite structure;
and putting the third composite structure into a treatment liquid for corrosion to obtain the lithium niobate self-supporting film.
2. The method for producing a lithium niobate self-supporting thin film according to claim 1, characterized in that:
The thickness of the lithium niobate single crystal wafer is 200-500 microns;
the surface roughness of the polished surface of the lithium niobate single crystal wafer is less than 1 nanometer;
the size of the lithium niobate single crystal wafer is 2 inches to 6 inches.
3. The method for producing a lithium niobate self-supporting thin film according to claim 1, characterized in that:
the high-resistance substrate is a silicon wafer, silicon carbide or gallium nitride;
the dielectric layer is a tantalum oxide layer, a titanium dioxide layer, a barium titanate layer, a zirconium dioxide layer, a hafnium dioxide layer, an aluminum oxide layer or a silicon oxide layer.
4. The method for producing a lithium niobate self-supporting thin film according to claim 3, characterized in that:
the thickness of the dielectric layer is 5 to 500 nanometers;
the surface roughness of the dielectric layer is less than 1 nanometer.
5. The method for producing a lithium niobate self-supporting thin film according to claim 1, characterized in that:
the number of the grooves is multiple, and each groove has the same size;
the length of the groove is 10-500 micrometers, the depth is 50-200 nanometers, and the width is 1-50 micrometers;
the distance between every two adjacent grooves is 20 micrometers to 100 micrometers.
6. The method for producing a lithium niobate self-supporting thin film according to claim 1, characterized in that:
The surface bonding mode of the polished surface of the lithium niobate single crystal wafer and the dielectric layer with the groove is a surface activation bonding mode, a metal bonding mode or an anode bonding mode;
the conditions of the bonding mode are as follows: the vacuum degree is 1E-7 Pa, the pressure is 16 MPa and the temperature is 25-200 ℃.
7. The method for producing a lithium niobate self-supporting thin film according to claim 1, characterized in that:
the thinning treatment method is a grinding method or a wet etching method.
8. The method for producing a lithium niobate self-supporting thin film according to claim 1, characterized in that:
the surface treatment method is a chemical mechanical polishing method, a plasma etching method, an ion sputtering method or a chemical etching method.
9. The method for producing a lithium niobate self-supporting thin film according to claim 1, characterized in that:
the treatment liquid is hydrogen fluoride aqueous solution or sodium hydroxide aqueous solution;
the ratio of hydrogen fluoride to water in the hydrogen fluoride aqueous solution is 1: 10 to 1: 100, respectively;
the ratio of sodium hydroxide to water in the sodium hydroxide aqueous solution is 1: 1 to 1: 100, respectively;
and the treatment time for putting the third composite structure into the treatment liquid for corrosion is 1 second to 24 hours.
10. A lithium niobate self-supporting film produced by the production method according to any one of claims 1 to 9.
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CN114460685A (en) * | 2022-01-30 | 2022-05-10 | 上海图灵智算量子科技有限公司 | Optical unit, chip and method for manufacturing the same |
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