CN112490349B - Electro-optic crystal film, preparation method and electronic component - Google Patents
Electro-optic crystal film, preparation method and electronic component Download PDFInfo
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- CN112490349B CN112490349B CN202011348841.3A CN202011348841A CN112490349B CN 112490349 B CN112490349 B CN 112490349B CN 202011348841 A CN202011348841 A CN 202011348841A CN 112490349 B CN112490349 B CN 112490349B
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- 238000002360 preparation method Methods 0.000 title abstract description 12
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- 239000010408 film Substances 0.000 claims abstract description 170
- 239000010409 thin film Substances 0.000 claims abstract description 159
- 239000000758 substrate Substances 0.000 claims abstract description 153
- 238000000034 method Methods 0.000 claims abstract description 72
- 238000005468 ion implantation Methods 0.000 claims abstract description 20
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000005498 polishing Methods 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 70
- 239000000463 material Substances 0.000 claims description 53
- 235000012239 silicon dioxide Nutrition 0.000 claims description 49
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 claims description 40
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 claims description 30
- 239000010453 quartz Substances 0.000 claims description 28
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims description 24
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 24
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 24
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 24
- 239000000377 silicon dioxide Substances 0.000 claims description 21
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 20
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 20
- 239000010703 silicon Substances 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 125000006850 spacer group Chemical group 0.000 claims description 11
- 239000011159 matrix material Substances 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
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- 239000010452 phosphate Substances 0.000 claims description 5
- WYOHGPUPVHHUGO-UHFFFAOYSA-K potassium;oxygen(2-);titanium(4+);phosphate Chemical compound [O-2].[K+].[Ti+4].[O-]P([O-])([O-])=O WYOHGPUPVHHUGO-UHFFFAOYSA-K 0.000 claims description 5
- 229910052701 rubidium Inorganic materials 0.000 claims description 5
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims description 5
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- 239000010980 sapphire Substances 0.000 description 19
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 18
- 239000010432 diamond Substances 0.000 description 15
- 229910003460 diamond Inorganic materials 0.000 description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 13
- 239000002210 silicon-based material Substances 0.000 description 11
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/853—Ceramic compositions
- H10N30/8542—Alkali metal based oxides, e.g. lithium, sodium or potassium niobates
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/07—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base
- H10N30/072—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base by laminating or bonding of piezoelectric or electrostrictive bodies
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Abstract
The application discloses an electro-optic crystal film, a preparation method and an electronic component, which comprise the following steps: preparing an isolation layer on the substrate layer; preparing a functional thin film layer on the isolation layer by using an ion implantation method and a bonding method, or by using a bonding method and a grinding and polishing method; after the isolation layer and the film substrate are bonded by a bonding method, compressive stress is formed in the film substrate, tensile stress is formed in the isolation layer, and further, the compressive stress and the tensile stress which are mutually contained are formed in the isolation layer and the film substrate by applying mechanical compressive stress or mechanical tensile stress to the film substrate and the isolation layer or by utilizing the thermal expansion coefficients of the isolation layer and the film substrate and controlling the temperature before and after bonding, so that the purpose of improving the refractive index difference between the isolation layer and the film substrate is realized.
Description
Technical Field
The application belongs to the field of semiconductor element preparation, and particularly relates to an electro-optic crystal film, a preparation method and an electronic component.
Background
Electro-optic crystals, such as lithium niobate and lithium tantalate crystals, have been widely used in the electronics industry due to their various characteristics, including piezoelectricity, electro-optic characteristics, photorefractive effect, and ferroelectricity. Particularly in the photoelectric direction, the material has a large electro-optic coefficient, a high refractive index, good thermal stability, and excellent nonlinear optical properties, and thus is one of the most important materials in the fields of electro-optic modulators, wavelength conversion devices, optical switches, and the like, and is known as a silicon material in the photoelectric direction.
The electro-optic crystal thin film disclosed in the prior art comprises a substrate layer, an isolation layer and a lithium niobate crystal thin film layer which are sequentially stacked, and the electro-optic crystal thin film replaces the traditional lithium niobate crystal, so that the manufactured electronic component is smaller in size, higher in integration level, lower in loss and higher in speed. The lithium niobate crystal thin film layer generally needs to be etched into a waveguide shape for transmitting optical signals, and the isolation layer generally adopts a material with a lower refractive index than the lithium niobate crystal thin film layer so as to limit the leakage of the optical signals from the lithium niobate crystal thin film layer to the substrate layer. In some special electronic components, the lithium niobate crystal thin film layer needs to turn to realize a specific function, the turning radius is limited by the refractive index difference between the lithium niobate crystal thin film layer and the isolation layer, and if the turning radius is too small due to insufficient refractive index difference, the phenomenon of transverse light leakage occurs. Therefore, in order to meet the preparation requirements of some special electronic components, the refractive index difference between the lithium niobate crystal thin film layer and the isolation layer needs to be further increased.
However, in the prior art, in order to obtain a better optical signal confinement effect by restricting the refractive index difference by the refractive indices of the lithium niobate crystal thin film layer and the spacer layer, it is necessary to dig two materials having a larger refractive index difference, which is a long and difficult problem, and it has not been possible to provide an electro-optical crystal thin film having a larger refractive index difference at present.
Disclosure of Invention
In order to solve the technical problems that in the prior art, the refractive index difference is restrained by the refractive indexes of a lithium niobate crystal thin film layer and an isolating layer, two materials with larger refractive index difference need to be excavated to obtain a better optical signal limiting effect, which is a long and difficult problem, and an electro-optic crystal thin film with larger refractive index difference cannot be provided at present, the electro-optic crystal thin film, the preparation method and the electronic component are provided.
In a first aspect, the present application provides a method for preparing an electro-optic crystal thin film, comprising: preparing an isolation layer on the substrate layer; preparing a functional thin film layer on the isolation layer by using an ion implantation method and a bonding method, or by using a bonding method and a grinding and polishing method; after the isolation layer is bonded with the film substrate by a bonding method, compressive stress is formed in the film substrate, tensile stress is formed in the isolation layer, and the film substrate is a base material for forming the functional film layer.
Further, the compressive stress formed within the film matrix is greater than 1 Mpa.
Further, after the isolation layer is bonded to the thin film substrate by using a bonding method, forming a compressive stress in the thin film substrate and forming a tensile stress in the isolation layer includes:
if the thermal expansion coefficient of the isolation layer is smaller than that of the film substrate, bonding the isolation layer and the film substrate by adopting a bonding method at a first temperature to obtain a bonded body;
and placing the bonding body at a second temperature, forming compressive stress in the film substrate, and forming tensile stress in the isolation layer, wherein the second temperature is higher than the first temperature.
Further, the functional thin film layer is a lithium niobate crystal, a lithium tantalate crystal or a quartz material, and the isolation layer is silicon dioxide, silicon nitride, aluminum oxide, diamond, sapphire, silicon carbide, gallium arsenide or a silicon material; or the isolating layer is made of silicon dioxide material, and the functional thin film layer is made of lithium niobate crystal, lithium tantalate crystal, quartz, silicon nitride, aluminum oxide, diamond, sapphire, silicon carbide, gallium arsenide or silicon material; or, the functional thin film layer is made of lithium niobate crystals or lithium tantalate crystals, and the isolation layer is made of quartz materials.
Further, after the isolation layer is bonded to the thin film substrate by using a bonding method, forming a compressive stress in the thin film substrate and forming a tensile stress in the isolation layer includes:
if the thermal expansion coefficient of the isolation layer is larger than that of the film base body, bonding the isolation layer and the film base body by adopting a bonding method at a first temperature to obtain a bonded body;
and placing the bonding body at the second temperature, forming compressive stress in the film substrate, and simultaneously forming tensile stress in the isolation layer, wherein the second temperature is lower than the first temperature.
Further, the functional thin film layer is made of silicon dioxide, silicon nitride, aluminum oxide, diamond, sapphire, silicon carbide, gallium arsenide or silicon materials, and the isolation layer can be made of lithium niobate crystals, lithium tantalate crystals or quartz materials; or the functional film layer is made of silicon or gallium arsenide material, and the isolation layer is made of aluminum oxide, sapphire or silicon carbide material; or the functional film layer is made of quartz material, and the isolating layer is made of lithium niobate crystal or lithium tantalate crystal material.
Further, after the isolation layer is bonded to the thin film substrate by using a bonding method, forming a compressive stress in the thin film substrate and forming a tensile stress in the isolation layer includes:
if the thermal expansion coefficient of the isolation layer is equal to that of the film base body, bonding the film base body with the third temperature and the isolation layer with the fourth temperature to obtain a bonding body, wherein the third temperature is lower than the fourth temperature;
placing the bonding body at the fifth temperature, forming a compressive stress in the film substrate, and forming a tensile stress in the isolation layer, wherein the fifth temperature is higher than the third temperature, and is lower than or equal to the fourth temperature; alternatively, the fifth temperature is greater than the third temperature and the fourth temperature.
Further, the isolation layer and the film substrate are made of the same material, and the isolation layer is made of lithium niobate crystals, lithium tantalate crystals, potassium titanyl phosphate crystals, rubidium titanyl phosphate crystals, silicon, gallium arsenide, quartz, silicon nitride, silicon carbide or silicon dioxide.
Further, after the isolation layer is bonded to the thin film substrate by using a bonding method, forming a compressive stress in the thin film substrate and forming a tensile stress in the isolation layer includes:
applying a mechanical compressive stress to the thin film substrate;
and bonding the film substrate with the compressive stress and the isolation layer by using a bonding method to obtain a bonded body, wherein the compressive stress is formed in the film substrate of the bonded body, and the tensile stress is formed in the isolation layer.
Further, after the isolation layer is bonded to the thin film substrate by using a bonding method, forming a compressive stress in the thin film substrate and forming a tensile stress in the isolation layer includes:
applying a mechanical tensile stress to the isolation layer;
and bonding the isolation layer with tensile stress and the film substrate by adopting a bonding method to obtain a bonded body, wherein the tensile stress is formed in the isolation layer of the bonded body, and the compressive stress is formed in the film substrate.
Further, after the isolation layer is bonded to the thin film substrate by using a bonding method, forming a compressive stress in the thin film substrate and forming a tensile stress in the isolation layer includes:
applying a mechanical compressive stress to the film substrate and applying a mechanical tensile stress to the isolation layer;
and bonding the isolation layer with the tensile stress and the film substrate with the compressive stress by adopting a bonding method to obtain a bonded body, wherein the compressive stress is formed in the film substrate of the bonded body, and the tensile stress is formed in the isolation layer of the bonded body.
In a second aspect, the present application also provides an electro-optic crystal film comprising: the substrate layer, the isolation layer and the functional thin film layer are sequentially stacked; the refractive index of the functional thin film layer is larger than that of the isolation layer, wherein the functional thin film layer has compressive stress therein, and the isolation layer has tensile stress therein.
Further, the compressive stress in the functional film layer is greater than 1 Mpa.
Further, if the functional thin film layer is a lithium niobate crystal, a lithium tantalate crystal, gallium arsenide, silicon, or a silicon carbide material, and the isolation layer is a silicon dioxide, quartz, silicon nitride, aluminum oxide, diamond, or sapphire material, the compressive stress in the functional thin film layer and the tensile stress in the isolation layer are formed by applying a mechanical compressive stress to the functional thin film layer, or by applying a mechanical tensile stress to the isolation layer, or by simultaneously applying a mechanical compressive stress to the thin film substrate, and by applying a mechanical tensile stress to the isolation layer.
Further, if the thermal expansion coefficient of the isolation layer is smaller than that of the functional thin film layer, the isolation layer and the functional thin film layer are bonded at a first temperature to form a bonded body, and the service temperature of the bonded body is a second temperature; wherein the first temperature is lower than the second temperature.
Further, the functional thin film layer is a lithium niobate crystal, a lithium tantalate crystal or a quartz material, and the isolation layer is silicon dioxide, silicon nitride, aluminum oxide, diamond, sapphire, silicon carbide, gallium arsenide or a silicon material; or the isolating layer is made of silicon dioxide material, and the functional thin film layer is made of lithium niobate crystal, lithium tantalate crystal, quartz, silicon nitride, aluminum oxide, diamond, sapphire, silicon carbide, gallium arsenide or silicon material; or, the functional thin film layer is made of lithium niobate crystals or lithium tantalate crystals, and the isolation layer is made of quartz materials.
Further, if the thermal expansion coefficient of the isolation layer is larger than that of the functional thin film layer, the isolation layer and the functional thin film layer are bonded at a first temperature to form a bonded body, and the service temperature of the bonded body is a second temperature; wherein the first temperature is higher than the second temperature.
Further, the functional thin film layer is made of silicon dioxide, silicon nitride, aluminum oxide, diamond, sapphire, silicon carbide, gallium arsenide or silicon materials, and the isolation layer can be made of lithium niobate crystals, lithium tantalate crystals or quartz materials; or the functional film layer is made of silicon or gallium arsenide material, and the isolation layer is made of aluminum oxide, sapphire or silicon carbide material; or the functional film layer is made of quartz material, and the isolating layer is made of lithium niobate crystal or lithium tantalate crystal material.
Further, if the isolation layer and the functional thin film layer are made of the same material or have the same expansion coefficient, when the isolation layer and the functional thin film layer are bonded to form a bonding body, the functional thin film layer is bonded under the conditions that the temperature of the functional thin film layer is the third temperature and the temperature of the isolation layer is the fourth temperature, and the service temperature of the bonding body is the fifth temperature; wherein the fifth temperature is greater than the third temperature and less than or equal to the fourth temperature; alternatively, the fifth temperature is greater than the third temperature and the fourth temperature, and the third temperature is less than the fourth temperature.
In a third aspect, the present application provides an electronic component comprising the electro-optic crystal film according to any one of the second aspects.
In a fourth aspect, the present application provides another method for preparing an electro-optic crystal film, comprising: preparing an isolation layer on the substrate layer; preparing a functional thin film layer on the isolation layer by using an ion implantation method and a bonding method, or by using a bonding method and a grinding and polishing method, wherein the refractive index of the functional thin film layer is greater than that of the isolation layer; in the step of bonding the isolation layer and the film substrate by adopting a bonding method, bonding the isolation layer with first compressive stress and the film substrate; after the isolation layer with the first compressive stress is bonded with the film substrate, a second compressive stress is formed in the film substrate, a third compressive stress is formed in the isolation layer, and the film substrate is a base material for forming the functional film layer.
Further, a second compressive stress is formed within the film matrix greater than 1 Mpa.
Further, the refractive index difference between the bonded film substrate and the isolation layer is larger than the refractive index difference between the bonded film substrate and the isolation layer before bonding.
In a fifth aspect, the present application provides an electro-optic crystal film comprising: the substrate layer, the isolation layer and the functional thin film layer are sequentially stacked; the refractive index of the functional thin film layer is larger than that of the isolation layer, wherein the functional thin film layer has a second compressive stress therein, and the isolation layer has a third compressive stress therein.
Further, the second compressive stress in the functional thin film layer is greater than 1 Mpa.
In a sixth aspect, the present application provides an electronic component comprising the electro-optic crystal film according to any one of the fifth aspects.
According to the electro-optic crystal film, the preparation method and the electronic component, the mechanical compression stress or the mechanical tensile stress is applied to the film substrate and the isolation layer, or the self thermal expansion coefficients of the isolation layer and the film substrate are utilized to control the temperature before and after bonding, so that the mutually-constrained compression stress and tensile stress are formed in the isolation layer and the film substrate, the purpose of improving the refractive index difference between the isolation layer and the film substrate is achieved, the preparation method is simple, two materials with larger refractive index difference do not need to be excavated, and only the conventional materials are used.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an electro-optic crystal film according to an embodiment of the present disclosure;
fig. 2 is a schematic structural diagram of another electro-optic crystal film provided in an embodiment of the present application.
Description of the reference numerals
110-substrate layer, 120-isolation layer, 130-functional thin film layer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
In order to solve the problem that in the prior art, the refractive index difference is restrained by the refractive indexes of the electro-optical crystal and the isolation layer, two materials with larger refractive index difference need to be excavated to obtain a better optical signal limiting effect, which is a long and difficult problem, the electro-optical crystal film with larger refractive index difference cannot be provided at present. The following is a detailed description of the method for preparing an electro-optic crystal film provided by the present application.
The preparation method of the electro-optic crystal film provided by the embodiment of the application comprises the following steps:
step 1, preparing an isolation layer 120 on a substrate layer 110.
The preparation method of step 1 is not limited in the present application, and for example, a deposition method may be adopted to deposit the isolation layer 120 with a target thickness on the substrate layer 110; for another example, if the substrate layer 110 is a silicon material and the isolation layer 120 is a silicon dioxide material, an oxidation method may be used to oxidize a silicon dioxide layer on the substrate layer 110 as the isolation layer 120.
It should be noted that, in the embodiment of the present application, the substrate layer may be a single-layer substrate or a composite substrate, which is not limited in the present application. The material of the substrate layer may be lithium niobate, lithium tantalate, quartz, silicon, sapphire, SOI, diamond, silicon carbide, silicon nitride, gallium arsenide, indium phosphide, or the like, which is not limited in the present application.
It should be noted that the isolation layer in the embodiment of the present application may also be a single-layer or multi-layer structure, which is not limited in the present application. If the spacer is a multilayer structure, the spacer described below refers to the spacer bonded to the film substrate.
Step 2, preparing a functional thin film layer 130 on the isolation layer 120 by using an ion implantation method and a bonding method, or by using a bonding method and a grinding and polishing method; after the isolation layer 120 is bonded to the thin film substrate by a bonding method, a compressive stress is formed in the thin film substrate, and a tensile stress is formed in the isolation layer, where the thin film substrate is a base material for forming the functional thin film layer.
The method of forming the functional thin film layer 130 on the isolation layer 120 is not limited in the present application, and for example, an ion implantation method and a bonding method may be used, and a bonding method and a polishing method may also be used, but whichever method is used to form the functional thin film layer is the key point of the present application, after the isolation layer is bonded to a thin film substrate by using the bonding method, a compressive stress is formed in the thin film substrate, and a tensile stress is formed in the isolation layer, where the thin film substrate in the present application refers to a base material for forming the functional thin film layer.
In one embodiment, the method for preparing the functional thin film layer on the isolation layer by adopting an ion implantation method and a bonding method comprises the following steps:
and 21, carrying out ion implantation in the film matrix, and sequentially dividing the film matrix into a functional film layer, a separation layer and a residual layer.
The film substrate in step 21 is a base material with a certain thickness for obtaining the functional film layer, that is, a wafer with a certain thickness. The thin film substrate may be an electro-optic crystal material such as lithium niobate or lithium tantalate, but is not limited in this application.
Ion implantation may be performed from one surface of the film substrate into the film substrate, thereby forming the functional thin film layer, the separation layer, and the residual layer on the film substrate.
The ion implantation method in the embodiment of the present application is not particularly limited, and any ion implantation method in the prior art may be used, and the implanted ions may be ions that can generate gas by heat treatment, for example: hydrogen ions or helium ions. When implanting hydrogen ions, the implantation dose can be 3 × 1016ions/cm2~8×1016ions/cm2The implantation energy can be 120 KeV-400 KeV; when implanting helium ions, the implantation dose can be 1 × 1016ions/cm2~1×1017ions/cm2The implantation energy may be 50KeV to 1000 KeV. For example, when implanting hydrogen ions, the implantation dose may be 4 × 1016ions/cm2The implantation energy may be 180 KeV; when implanting helium ions, implantingThe dosage is 4X 1016ions/cm2The implantation energy was 200 KeV.
In the embodiment of the application, the thickness of the functional thin film layer can be adjusted by adjusting the ion implantation depth, and specifically, the larger the ion implantation depth is, the larger the thickness of the prepared functional thin film layer is; conversely, the smaller the depth of ion implantation, the smaller the thickness of the functional thin film layer prepared.
And step 22, bonding the ion implantation surface of the film substrate with the isolation layer to obtain a bonded body.
In the embodiment of the present application, the bond is formed after a film substrate is bonded to an isolation layer, wherein the film substrate is not peeled off from the isolation layer, and the ion implantation surface is a surface that implants ions into the film substrate.
The method for bonding the thin film substrate and the isolation layer is not particularly limited, and any bonding method in the prior art may be adopted, for example, the bonding surface of the thin film substrate is subjected to surface activation, the bonding surface of the isolation layer is also subjected to surface activation, and then the two activated surfaces are bonded to obtain the bonded body.
The method for surface activation of the bonding surface of the thin film substrate is not particularly limited, and any method for surface activation of the thin film substrate in the prior art, such as plasma activation and chemical solution activation, may be used; similarly, the present application does not limit the bonding surface of the isolation layer in any way, and any method that can be used in the prior art for surface activation of the bonding surface of the isolation layer, such as plasma activation, can be used.
In the embodiment of the application, in order to form a compressive stress in the thin film substrate and a tensile stress in the isolation layer after the isolation layer is bonded with the thin film substrate, the bonding temperature of the thin film substrate and the isolation layer is adjusted by using the thermal expansion coefficients of the thin film substrate and the isolation layer, so that the compressive stress is formed in the bonded thin film substrate and the tensile stress is formed in the isolation layer; the other method is to form compressive stress in the bonded film substrate and form tensile stress in the isolation layer by applying mechanical compressive stress or mechanical tensile stress to the film substrate and the isolation layer.
In a first feasible mode, if the thermal expansion coefficient of the isolation layer is smaller than that of the film base body, bonding the isolation layer and the film base body by adopting a bonding method at a first temperature to obtain a bonded body; and placing the bonding body at a second temperature, forming compressive stress in the film substrate, and forming tensile stress in the isolation layer, wherein the second temperature is higher than the first temperature. In a specific example, the thin film substrate can be lithium niobate, lithium tantalate, or quartz material, and the isolation layer is silicon dioxide, silicon nitride, aluminum oxide, diamond, sapphire, silicon carbide, gallium arsenide, or silicon material; or the isolating layer is made of silicon dioxide material, and the film substrate can be made of lithium niobate, lithium tantalate, quartz, silicon nitride, aluminum oxide, diamond, sapphire, silicon carbide, gallium arsenide or silicon material; or, the film substrate can be made of lithium niobate or lithium tantalate, and the isolating layer is made of quartz material. Wherein the second temperature is generally the use temperature of the electro-optic crystal film prepared, for example, the use temperature is 15-30 ℃ at room temperature. In one example, if a temperature is used, i.e., the second temperature is 20 ℃, the first temperature may be a temperature less than 20 ℃, such as-25 ℃. When bonding is carried out at a first temperature, the isolation layer and the film substrate are in a stress-free state, when the first temperature is raised to a second temperature, because the film substrate has a large thermal expansion coefficient and a small thermal expansion coefficient, and the expansion degree of the film substrate is greater than that of the isolation layer, the film substrate is subjected to inward compressive stress and the isolation layer is subjected to outward tensile stress in the bonded state, so that the refractive index of the film substrate is increased (the refractive index of the corresponding generated functional film layer is increased), and the refractive index of the isolation layer is reduced.
If the thermal expansion coefficient of the isolation layer is larger than that of the film base body, bonding the isolation layer and the film base body by adopting a bonding method at a first temperature to obtain a bonded body; and placing the bonding body at the second temperature, forming compressive stress in the film substrate, and simultaneously forming tensile stress in the isolation layer, wherein the second temperature is lower than the first temperature. In a specific example, the thin film substrate can be silicon dioxide, silicon nitride, aluminum oxide, diamond, sapphire, silicon carbide, gallium arsenide or silicon material, and the isolation layer can be lithium niobate, lithium tantalate or quartz material; or the film substrate can be made of silicon or gallium arsenide materials, and the isolation layer is made of aluminum oxide, sapphire or silicon carbide materials; or the film substrate can be made of quartz material, and the isolating layer is made of lithium niobate or lithium tantalate material. Wherein the second temperature is generally the use temperature of the prepared electro-optic crystal film, for example, the use temperature is 15-30 ℃. In one example, if a temperature is used, i.e. the second temperature is 30 ℃, the first temperature may be a temperature greater than 30 ℃, such as 50 ℃. When bonding is carried out at a first temperature, the isolation layer and the film substrate are in a stress-free state, when the first temperature is reduced to a second temperature, because the film substrate has a small thermal expansion coefficient and a large thermal expansion coefficient, and the shrinkage degree of the film substrate is smaller than that of the isolation layer, the film substrate is subjected to inward compressive stress and the isolation layer is subjected to outward tensile stress in the bonded state, so that the refractive index of the film substrate is improved (the refractive index of the corresponding generated functional film layer is improved), and the refractive index of the isolation layer is reduced.
If the thermal expansion coefficient of the isolation layer is equal to that of the film base body, bonding the film base body with the third temperature and the isolation layer with the fourth temperature to obtain a bonding body, wherein the third temperature is lower than the fourth temperature; placing the bonding body at the fifth temperature, forming a compressive stress in the film substrate, and forming a tensile stress in the isolation layer, wherein the fifth temperature is higher than the third temperature, and is lower than or equal to the fourth temperature; alternatively, the fifth temperature is greater than the third temperature and the fourth temperature, and the third temperature is less than the fourth temperature. In a specific example, the isolation layer and the thin film substrate may be made of the same material, and both the isolation layer and the thin film substrate are made of lithium niobate crystal, lithium tantalate crystal, potassium titanyl phosphate crystal, rubidium titanyl phosphate crystal, silicon, gallium arsenide, quartz, silicon nitride, silicon carbide or silicon dioxide material. In this embodiment, before bonding, the film substrate is processed to a third temperature, the isolation layer is processed to a fourth temperature, then the film substrate having the third temperature and the isolation layer having the fourth temperature are bonded, and finally, the bonded body obtained after bonding is placed at the fifth temperature. Wherein the fifth temperature is generally the use temperature of the prepared electro-optic crystal film, for example, the use temperature is 15-30 ℃. In one example, if a temperature is used, i.e., the fifth temperature is 30 ℃, the third temperature may be a temperature less than 30 ℃, e.g., 10 ℃, and the fourth temperature is greater than 30 ℃, e.g., 100 ℃. Before bonding, when the film base body is at the third temperature and the isolation layer is at the fourth temperature, the film base body and the isolation layer are both in a stress-free state, when the bonding temperature is changed to the fifth temperature, the film base body expands, and the isolation layer contracts, so that the film base body is subjected to inward compressive stress and the isolation layer is subjected to outward tensile stress in the bonded state, the refractive index of the film base body is improved (the refractive index of the corresponding generated functional thin film layer is improved), and the refractive index of the isolation layer is reduced. In another example, if a temperature is used, i.e., the fifth temperature is 30 ℃, the third temperature may be a temperature less than 30 ℃, e.g., 10 ℃, and the fourth temperature is also less than 30 ℃, e.g., 20 ℃. Before bonding, when the film base body is at the third temperature and the isolation layer is at the fourth temperature, the film base body and the isolation layer are both in a stress-free state, and when the bonding temperature is changed to the fifth temperature, the expansion degree of the film base body is greater than that of the isolation layer, so that the film base body is subjected to inward compressive stress and the isolation layer is subjected to outward tensile stress in the bonded state, the refractive index of the film base body is improved (the refractive index of the corresponding generated functional thin film layer is improved), and the refractive index of the isolation layer is reduced.
In summary, in the first feasible manner, the thermal expansion coefficients of the isolation layer and the film substrate are utilized to control the temperatures before and after bonding, so that the mutually-constrained compressive stress and tensile stress are formed in the isolation layer and the film substrate, and the purpose of improving the refractive index difference between the isolation layer and the film substrate is realized.
In another first possible way, a mechanical compressive stress or a mechanical tensile stress is applied to the thin film substrate and the isolation layer, so that a compressive stress is formed in the bonded thin film substrate, and a tensile stress is formed in the isolation layer. In one embodiment, a mechanical compressive stress is applied to the thin film substrate; and bonding the film substrate with the compressive stress and the isolation layer by using a bonding method to obtain a bonded body, wherein the compressive stress is formed in the film substrate of the bonded body, and the tensile stress is formed in the isolation layer. In another specific example, a mechanical tensile stress is applied to the isolation layer; and bonding the isolation layer with tensile stress and the film substrate by adopting a bonding method to obtain a bonded body, wherein the tensile stress is formed in the isolation layer of the bonded body, and the compressive stress is formed in the film substrate. Applying a mechanical compressive stress to the film substrate and applying a mechanical tensile stress to the isolation layer; and bonding the isolation layer with tensile stress and the film substrate with compressive stress by using a bonding method to obtain a bonded body, wherein the compressive stress is formed in the film substrate of the bonded body, and the tensile stress is formed in the isolation layer of the bonded body.
Any one of the two possible ways may be adopted to form a compressive stress in the film substrate and a tensile stress in the isolation layer, which is not limited in the present application. And the compressive stress formed in the film matrix by adopting any feasible mode can achieve the technical effect of more than 1Mpa, so that the refractive index of the film matrix is greatly improved, and the film matrix can be applied to electronic components with higher refractive index requirements.
And 23, carrying out heat treatment on the bonding body to separate the residual layer from the functional thin film layer.
In an implementation mode, the bonded body is subjected to heat treatment, the temperature of the heat treatment is 100-600 ℃, bubbles are formed in the separation layer in the heat treatment process, for example, H ions form hydrogen, He ions form helium and the like, the bubbles in the separation layer are connected into one piece along with the progress of the heat treatment, finally, the separation layer is cracked, the residual layer is separated from the functional thin film layer, so that the residual layer is stripped from the bonded body, a functional thin film layer is formed on the surface of the separation layer, and then the functional thin film layer is polished and thinned to 50-3000nm (for example, 400nm, 500nm, 600nm, 800nm, 1000nm and the like) to obtain the functional thin film layer with the nanoscale thickness.
In the embodiment of the present application, an achievable heat treatment manner is to put the bonding body into a heating device, first raise the temperature to a preset temperature, and then keep the temperature at the preset temperature. Among them, preferably, the heat-preserving conditions include: the holding time may be 1 minute to 48 hours, for example, 3 hours, the holding temperature may be 100 ℃ to 600 ℃, for example, 400 ℃, and the holding atmosphere may be in a vacuum atmosphere or in a protective atmosphere of at least one of nitrogen and an inert gas. Through the heat treatment, the bonding force between the functional thin film layer and the isolation layer can be improved to be larger than 10MPa, and the damage of ion implantation to the functional thin film layer can be recovered, so that the properties of the obtained functional thin film layer and an electro-optic crystal material, namely a film substrate are close to each other.
In the embodiment of the present application, after the heat treatment, the obtained electro-optic crystal thin film is returned to the normal temperature (i.e., the temperature before the heat treatment), so that the compressive stress is formed in the thin film substrate and the tensile stress is formed in the spacer in step 22, and the refractive index of the functional thin film layer is increased and the refractive index of the spacer is decreased in the electro-optic crystal thin film obtained finally.
In one embodiment, the method for preparing the functional thin film layer on the isolation layer by adopting a bonding method and a grinding and polishing method comprises the following steps: firstly, bonding the prepared film substrate and the isolation layer to obtain a bonded body, wherein the manner of bonding the film substrate and the isolation layer can refer to the description of step 22, and is not described herein again. And then, carrying out heat treatment on the bonding body to improve the bonding force between the film substrate and the isolating layer. For example, the bonding body is placed in a heating device and is subjected to heat preservation at a high temperature, the heat preservation process is performed in a vacuum environment or in a protective atmosphere formed by at least one of nitrogen and inert gas, the heat preservation temperature can be 100 ℃ to 600 ℃, for example, the heat preservation time is 400 ℃, and the heat preservation time can be 1 minute to 48 hours, for example, the heat preservation time is 3 hours. And finally, mechanically grinding and polishing the film substrate on the bonding body, and thinning the film substrate to the thickness of the preset functional film layer. For example, if the thickness of the preset functional thin film layer is 20 μm, the electro-optic crystal material on the bonding body, i.e., the thin film substrate, may be first thinned to 22 μm by mechanical grinding, and then polished to 20 μm, so as to obtain the functional thin film layer. Wherein, the thickness of the functional film layer can be 400nm-100 μm.
In the present application, compressive stress refers to a stress formed by inward contraction of the wafer from the outer edge, and tensile stress refers to a stress formed by expansion of the wafer from the inner edge to the outer edge.
As shown in fig. 1, an embodiment of the present application further provides an electro-optic crystal film, which includes a substrate layer 110, an isolation layer 120, and a functional film layer 130, which are sequentially stacked; the refractive index of the functional thin film layer 130 is greater than the refractive index of the isolation layer 120, wherein the functional thin film layer 130 has a compressive stress therein, and the isolation layer 120 has a tensile stress therein. Wherein the compressive stress in the functional thin film layer 130 and the tensile stress in the isolation layer 130 can be measured by the prior art means. The compressive stress formed in the functional thin film layer 130 in the embodiment of the present application can achieve the technical effect of being greater than 1Mpa, so that the refractive index of the functional thin film layer 130 is greatly improved, and the application in electronic components with higher refractive indexes is satisfied.
Corresponding to the embodiment of preparing the electro-optic crystal film, if the functional thin film layer is lithium niobate, lithium tantalate, gallium arsenide, silicon or silicon carbide, and the isolation layer is silicon dioxide, quartz, silicon nitride, aluminum oxide, diamond or sapphire, the compressive stress in the functional thin film layer and the tensile stress in the isolation layer are formed by applying mechanical compressive stress to the functional thin film layer, or applying mechanical tensile stress to the isolation layer, or simultaneously applying mechanical compressive stress to the thin film substrate and applying mechanical tensile stress to the isolation layer.
If the thermal expansion coefficient of the isolation layer is smaller than that of the functional thin film layer, the isolation layer and the functional thin film layer are bonded at a first temperature to form a bonded body, and the service temperature of the bonded body is a second temperature; wherein the first temperature is lower than the second temperature. Correspondingly, the functional thin film layer is lithium niobate, lithium tantalate or quartz, and the isolating layer is silicon dioxide, silicon nitride, aluminum oxide, diamond, sapphire, silicon carbide, gallium arsenide or silicon; or the isolating layer is silicon dioxide, and the functional thin film layer is lithium niobate, lithium tantalate, quartz, silicon nitride, aluminum oxide, diamond, sapphire, silicon carbide, gallium arsenide or silicon; or the functional thin film layer is lithium niobate or lithium tantalate, and the isolating layer is quartz.
If the thermal expansion coefficient of the isolation layer is larger than that of the functional thin film layer, the isolation layer and the functional thin film layer are bonded at a first temperature to form a bonded body, and the service temperature of the bonded body is a second temperature; wherein the first temperature is higher than the second temperature. Correspondingly, the functional thin film layer is silicon dioxide, silicon nitride, aluminum oxide, diamond, sapphire, silicon carbide, gallium arsenide or silicon, and the isolating layer can be lithium niobate, lithium tantalate or quartz; or the functional thin film layer is silicon or gallium arsenide, and the isolation layer is aluminum oxide, sapphire or silicon carbide; or the functional thin film layer is made of quartz, and the isolating layer is made of lithium niobate or lithium tantalate.
If the isolation layer and the functional thin film layer are made of the same material or have the same expansion coefficient, when the isolation layer and the functional thin film layer are bonded to form a bonding body, the functional thin film layer is bonded under the conditions that the temperature of the functional thin film layer is third and the temperature of the isolation layer is fourth, and the service temperature of the bonding body is fifth; wherein the fifth temperature is greater than the third temperature and less than or equal to the fourth temperature; alternatively, the fifth temperature is greater than the third temperature and the fourth temperature, and the third temperature is less than the fourth temperature. Correspondingly, the functional thin film layer and the isolating layer are made of lithium niobate crystals, lithium tantalate crystals, potassium titanyl phosphate crystals, rubidium titanyl phosphate crystals, silicon, gallium arsenide, quartz, silicon nitride, silicon carbide or silicon dioxide materials.
The embodiment of the application also provides an electronic component which comprises the electro-optic crystal thin film shown in the figure 1.
In the above embodiments, the refractive indexes of the functional thin film layer and the isolation layer in the electro-optic crystal thin film are increased by forming a compressive stress in the thin film substrate and forming a tensile stress in the isolation layer. In addition, the optical signal can be limited in the functional thin film layer in a mode of improving the refractive index of the functional thin film layer by forming the second compressive stress in the thin film substrate and forming the third compressive stress in the isolation layer.
In the scheme of forming the second compressive stress in the film substrate and forming the third compressive stress in the isolation layer, the difference is similar to the scheme of forming the compressive stress in the film substrate and forming the tensile stress in the isolation layer, and the scheme is as follows: in this scheme, before bonding, a first compressive stress is formed in the isolation layer, which is mainly formed through interaction between the isolation layer and the substrate layer, where a forming manner of the first compressive stress in the isolation layer before bonding may refer to a principle of formation of compressive stress between the film base and the isolation layer in the above embodiments, and is not described herein again. Further, the isolation layer having the first compressive stress is bonded to the film base, and a tensile stress generated in the isolation layer after bonding and corresponding to the second compressive stress in the film base is smaller than the first compressive stress generated before bonding the isolation layer, so that a compressive stress, i.e., a third compressive stress, is still present in the isolation layer after bonding, where a manner of bonding the isolation layer to the film base may be referred to the description of step 22 in the above embodiment, and is not described herein again. In the scheme, the refractive index of the functional thin film layer in the formed electro-optic crystal thin film is improved, so that optical signals can be well limited in the functional thin film layer. Similarly, the second compressive stress formed in the film substrate in the embodiment can achieve the technical effect of being greater than 1Mpa, so that the refractive index of the film substrate is greatly improved, and the film substrate can be applied to electronic components with higher refractive indexes. Further, in order to better confine the optical signal in the functional thin film layer and increase the refractive index difference between the functional thin film layer and the spacer layer, it is preferable to control the refractive index difference between the thin film substrate and the spacer layer after bonding to be larger than the refractive index difference between the thin film substrate and the spacer layer before bonding.
As shown in fig. 2, the present embodiment further provides another electro-optic crystal film including: a substrate layer 110, an isolation layer 120 and a functional thin film layer 130 stacked in sequence; the refractive index of the functional thin film layer 130 is greater than the refractive index of the isolation layer 120, wherein the functional thin film layer 130 has a second compressive stress therein, and the isolation layer 120 has a third compressive stress. The second compressive stress that forms in the functional thin film layer 130 in the embodiment of the present application can all reach the technical effect that is greater than 1Mpa, so that the refractive index of the functional thin film layer 130 is greatly improved, and the application in electronic components with higher refractive index requirements is satisfied.
The embodiment of the application also provides an electronic component which comprises the electro-optic crystal film shown in the figure 2.
The same and similar parts among the various embodiments in the specification can be referred to each other, and especially the corresponding embodiments of the electro-optic crystal film can be referred to the preparation method part.
The present application has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to limit the application. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the presently disclosed embodiments and implementations thereof without departing from the spirit and scope of the present disclosure, and these fall within the scope of the present disclosure. The protection scope of this application is subject to the appended claims.
Claims (6)
1. A method for preparing an electro-optic crystal film, comprising:
preparing an isolation layer on the substrate layer;
preparing a functional thin film layer on the isolation layer by using an ion implantation method and a bonding method, or by using a bonding method and a grinding and polishing method; wherein the preparing the functional thin film layer on the isolation layer by using the ion implantation method and the bonding method comprises:
carrying out ion implantation in a film matrix, and sequentially dividing the film matrix into a functional film layer, a separation layer and a residual layer;
bonding the ion implantation surface of the film substrate with the isolation layer to obtain a bonded body;
carrying out heat treatment on the bonding body to separate the residual layer from the functional thin film layer;
the film substrate is a base material for forming the functional film layer;
the thermal expansion coefficient of the isolation layer is equal to that of the film base body, the film base body with the first temperature and the isolation layer with the second temperature are bonded to obtain a bonding body, and the first temperature is lower than the second temperature; placing the bonding body at a third temperature, forming a compressive stress in the film substrate, and forming a tensile stress in the isolation layer, wherein the third temperature is higher than the first temperature, and is lower than or equal to the second temperature; alternatively, the third temperature is greater than the first temperature and the second temperature.
2. The method according to claim 1, wherein the isolation layer is made of the same material as the thin film substrate, and the isolation layer is made of a lithium niobate crystal, a lithium tantalate crystal, a potassium titanyl phosphate crystal, a rubidium titanyl phosphate crystal, silicon, gallium arsenide, quartz, silicon nitride, silicon carbide, or silicon dioxide.
3. An electro-optic crystal film, wherein the electro-optic crystal film is prepared by the method for preparing an electro-optic crystal film according to claim 1.
4. The electro-optic crystal film of claim 3, wherein the spacer layer is made of the same material as the functional thin film layer, and the spacer layer is made of lithium niobate crystal, lithium tantalate crystal, potassium titanyl phosphate crystal, rubidium titanyl phosphate crystal, silicon, gallium arsenide, quartz, silicon nitride, silicon carbide, or silicon dioxide.
5. The electro-optic crystal film of claim 3, wherein the functional film layer in the electro-optic crystal film has a compressive stress greater than 1 Mpa.
6. An electronic component comprising the electro-optic crystal film according to any one of claims 3 to 5.
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