CN114420833A - Film preparation method based on staged heat treatment and composite film thereof - Google Patents

Film preparation method based on staged heat treatment and composite film thereof Download PDF

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CN114420833A
CN114420833A CN202210089179.7A CN202210089179A CN114420833A CN 114420833 A CN114420833 A CN 114420833A CN 202210089179 A CN202210089179 A CN 202210089179A CN 114420833 A CN114420833 A CN 114420833A
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heat treatment
layer
wafer
thin film
bonding
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胡文
胡卉
李真宇
张秀全
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Jinan Jingzheng Electronics Co Ltd
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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
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/01—Manufacture or treatment
    • H10N30/04—Treatments to modify a piezoelectric or electrostrictive property, e.g. polarisation characteristics, vibration characteristics or mode tuning
    • 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
    • H10N30/09—Forming piezoelectric or electrostrictive materials
    • H10N30/092—Forming composite materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/80—Constructional details
    • H10N30/85—Piezoelectric or electrostrictive active materials
    • H10N30/852—Composite materials, e.g. having 1-3 or 2-2 type connectivity

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Abstract

The application discloses a film preparation method based on staged heat treatment and a composite film thereof, wherein the method comprises the following steps: obtaining a single crystal wafer and a substrate wafer; implanting ions into a single crystal wafer by an ion implantation method, and dividing the single crystal wafer into a residual layer, a separation layer and a thin film layer in sequence; bonding the single crystal wafer and the substrate wafer to form a bonded body; and (3) putting the bonded body into an annealing furnace for heat treatment, and putting the bonded body into the annealing furnace for carrying out bonding force enhancing heat treatment, thin layer and residual material layer separation heat treatment and ion damage eliminating heat treatment in sequence by stages to obtain the composite film. According to the method, the bonding body is subjected to staged heat treatment, the bonding force is improved, the thin film layer and the excess material layer are separated to reduce the risk of film breakage, the damage caused by ion implantation is eliminated, the quality of the composite film is finally improved, and the yield of downstream devices is further improved.

Description

Film preparation method based on staged heat treatment and composite film thereof
Technical Field
The application belongs to the field of semiconductor element preparation, and particularly relates to a film preparation method based on staged heat treatment and a composite film thereof.
Background
The composite film can be used as a basic material for manufacturing high-frequency, high-broadband, high-integration, large-capacity and low-power-consumption optoelectronic devices and integrated optical paths due to excellent optical performance.
At present, methods for preparing a composite thin film mainly include an epitaxial growth method, an ion implantation and bonding separation method, an ion implantation and a polishing and grinding method. The ion implantation method is mainly characterized in that ions are implanted into a single crystal wafer to divide the single crystal wafer into a thin film layer, a separation layer and a residual layer, then the ion implantation surface of the single crystal wafer is bonded with a substrate layer to form a bonded body, and finally the bonded body is subjected to heat treatment to separate the residual layer from the thin film layer and keep the thin film layer on the substrate layer, so that the thin film layer with the performance close to that of the single crystal wafer is prepared.
However, in the process of preparing the composite film, since the bonding between the ion implantation surface of the single crystal wafer and the substrate layer is performed at room temperature, the bonding force is not strong, and the bonding surface may be broken in the subsequent heating separation process; meanwhile, when the annealing separation temperature is high, different wafers have the problem that the film is cracked due to the difference of thermal expansion coefficients; in addition, ion implantation also causes damage to the implantation surface. These several factors combine to reduce the quality of the overall composite film and also cause low yield of downstream devices.
Disclosure of Invention
The invention provides a film preparation method based on staged heat treatment, which aims to solve the problems of bonding surface fracture caused by weak bonding force, film fracture caused by high-temperature separation and thermal expansion coefficient difference and damage of an injection surface caused by ion implantation in the process of preparing a composite film in the prior art.
The present application aims to provide the following aspects:
in a first aspect, the present application provides a method for preparing a thin film based on a staged heat treatment, comprising the steps of:
obtaining a single crystal wafer and a substrate wafer;
implanting ions into a single crystal wafer by an ion implantation method, and dividing the single crystal wafer into a residual layer, a separation layer and a thin film layer in sequence;
bonding the single crystal wafer and the substrate wafer to form a bonded body;
and (3) putting the bonding body into an annealing furnace for staged heat treatment, and putting the bonding body into the annealing furnace for heat treatment for enhancing bonding force, heat treatment for separating the thin film layer from the residual material layer and heat treatment for eliminating ion damage in sequence to obtain the composite film.
Preferably, the temperature of the bonding force heat treatment is higher than the temperature of the separation heat treatment of the thin film layer and the residual material layer, and the time of the bonding force heat treatment is shorter than the time of the separation heat treatment of the thin film layer and the residual material layer.
Preferably, the temperature of the ion damage eliminating heat treatment is higher than the temperature of the separation heat treatment of the thin film layer and the residual material layer.
Preferably, the bonding force heat treatment is that the bonding body lasts for 0.2 to 1 hour at 220 to 300 ℃; the thin film layer and the residual material layer are separated and thermally treated, namely, the bonding body lasts for 3-6h at the temperature of 150-190 ℃; the heat treatment for eliminating the ion damage is that the bonding body lasts for 2-4h at 320-350 ℃.
Preferably, an insulating layer is manufactured on one surface of the substrate wafer or a dielectric layer is manufactured on one surface of the substrate wafer firstly and then the insulating layer is manufactured; and bonding the insulating layer on the substrate wafer and the monocrystalline wafer during bonding.
Preferably, the insulating layer is one of silicon dioxide, silicon oxynitride, and silicon nitride.
Preferably, the method for manufacturing the dielectric layer on one surface of the substrate wafer comprises the following steps: depositing polycrystalline silicon or amorphous silicon on the surface of a substrate wafer by a deposition method; or generating a corrosion damage layer on the surface of the substrate wafer by a corrosion method; or generating a corrosion damage layer on the surface of the substrate wafer by an etching method.
Preferably, the ions used in the ion implantation method are helium ions, hydrogen ions, nitrogen ions, oxygen ions, or argon ions.
Preferably, the method for bonding the single crystal wafer and the substrate wafer is any one of a direct bonding method, an anodic bonding method, a low-temperature bonding method, a vacuum bonding method, a plasma enhanced bonding method and an adhesive bonding method.
Preferably, the single crystal wafer is lithium niobate, lithium tantalate, quartz, ceramic, lithium tetraborate, potassium titanyl phosphate, rubidium titanyl phosphate, gallium arsenide or silicon; the substrate wafer is lithium niobate, lithium tantalate, a silicon wafer, a silicon carbide wafer, silicon nitride, quartz, sapphire or quartz glass.
In a second aspect, the present application provides a composite film comprising the composite film prepared by the method of any one of the first aspect.
Compared with the traditional scheme, the invention optimizes the process of the segmented heat treatment through three times of heat treatment, firstly, the bonding force is enhanced through enhancing the bonding force heat treatment so as to solve the problem of the fracture of the bonding surface caused by weak bonding force; then, reducing the temperature to carry out heat treatment for separating the thin film layer and the residual material layer so as to solve the problem of film cracking caused by high-temperature separation and difference of thermal expansion coefficients; and finally, raising the temperature to carry out ion damage elimination heat treatment so as to solve the problem of damage of an implanted surface caused by ion implantation. The quality of the composite film and the yield of downstream devices are improved by the film preparation method based on staged heat treatment.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a thin film based on staged thermal treatment according to an embodiment of the present disclosure;
FIG. 2 is a schematic diagram illustrating the formation of a composite film according to an embodiment of the present disclosure;
fig. 3 is a schematic diagram of another composite film according to an embodiment of the present disclosure.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying 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 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.
In the prior art, in the process for preparing the composite film, the ion implantation surface and the substrate layer of the single crystal wafer are bonded at room temperature, the bonding force is not strong, and the problem of bonding surface fracture may occur in the subsequent heating separation process; when the annealing separation temperature is high, different wafers have the problem that the film is cracked due to the difference of the thermal expansion coefficients; ion implantation can also cause damage to the implanted surfaces. In summary, these disadvantages reduce the quality of the overall composite film and also cause the problem of low yield of the downstream devices.
Therefore, to solve the above problems, embodiments of the present application provide a method for preparing a thin film based on a staged heat treatment.
Referring to fig. 1, a flow chart of a method for preparing a thin film based on a staged thermal treatment according to the present application is shown.
As can be seen, the present application provides a method for preparing a thin film based on a staged thermal process, the method comprising:
and S10, acquiring the single crystal wafer and the substrate wafer.
The single crystal wafer can be lithium niobate, lithium tantalate, quartz, ceramic, lithium tetraborate, potassium titanyl phosphate, rubidium titanyl phosphate, gallium arsenide or silicon; the invention is not limited. The substrate wafer may be lithium niobate, lithium tantalate, a silicon wafer, a silicon carbide wafer, silicon nitride, quartz, sapphire, or quartz glass. The invention is not limited.
And S20, implanting ions into the single crystal wafer by an ion implantation method, and sequentially dividing the single crystal wafer into a residual layer, a separation layer and a thin film layer.
By ion implantationThe ions of (b) may be helium ions, hydrogen ions, nitrogen ions, oxygen ions, or argon ions. 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 120KeV-400 KeV; when implanting helium ions, the implantation dose can be 1 × 1016ions/cm2-1×1017ions/cm2The implantation energy may be 50KeV-1000 KeV. The ion implantation depth can be arbitrarily selected, and the implantation energy depends on how many nanometers the implantation depth is.
In addition, the thickness of the thin film layer can be adjusted by adjusting the ion implantation depth, specifically, the greater the ion implantation depth, the greater the thickness of the prepared thin film layer; conversely, the smaller the depth of ion implantation, the smaller the thickness of the thin film layer produced.
One specific example of the ion-implanted single crystal wafer is to prepare a 6-inch lithium niobate wafer, fix the lithium niobate wafer on a porous ceramic chuck of a polishing apparatus, perform chemical mechanical polishing to obtain a smooth surface, and then perform semiconductor RCA cleaning on the wafer to obtain a clean surface. And implanting oxygen ions into the processed lithium niobate wafer by adopting a stripping ion implantation method, so that the lithium niobate wafer is sequentially divided into a residual material layer, a separation layer and a thin film layer, and the implanted oxygen ions are distributed in the separation layer to obtain a single crystal wafer implanted sheet. When oxygen ions are implanted by adopting a stripping ion implantation method, the implantation dosage parameters are as follows: the implantation dose is 3 × 1016ions/cm2, implant energy 380keV, implant depth 534 nm.
And S30, bonding the single crystal wafer and the substrate wafer to form a bonded body.
Specifically, the single crystal wafer and the substrate wafer may be bonded by any one of a direct bonding method, an anodic bonding method, a low-temperature bonding method, a vacuum bonding method, a plasma-enhanced bonding method, and an adhesive bonding method, and is not particularly limited.
And S40, putting the bonding body into an annealing furnace, and sequentially carrying out bonding force enhancing heat treatment, thin film layer and residual material layer separation heat treatment and ion damage eliminating heat treatment in stages to obtain the composite film.
The bonding force enhancing heat treatment aims at solving the problem that the bonding surface is broken due to weak bonding force; the heat treatment of the separation of the thin film layer and the residual material layer is used for solving the problem of the breakage of the thin film caused by the high-temperature separation and the difference of the thermal expansion coefficients; the ion damage heat treatment is eliminated to solve the problem of damage of the implantation surface caused by ion implantation.
The temperature of the bonding force heat treatment is higher than the temperature of the separation heat treatment of the thin film layer and the residual material layer, and the time of the bonding force heat treatment is shorter than the time of the separation heat treatment of the thin film layer and the residual material layer. The temperature of the heat treatment for eliminating the ion damage is higher than the temperature of the separation heat treatment of the thin film layer and the residual material layer.
The temperature of the bonding force heat treatment designed by the invention is higher than that of the separation heat treatment, so that the effect of stronger bonding force than that obtained by the heat treatment in the prior art can be achieved, the time of the bonding force heat treatment is not too long, and the range of the bonding force heat treatment in the invention is 0.2-1h, because the high-temperature heat treatment for a long time can cause the defect of film cracking due to the difference of thermal expansion coefficients of different wafers.
In this step, the bonding force can be enhanced by increasing the temperature in the bonding force heat treatment, but the problem of film cracking caused by the difference of the thermal expansion coefficients of the substrate wafer and the single crystal wafer also occurs, so the time for enhancing the bonding force heat treatment is not suitable to be too long.
The thin film layer and the residual material layer are separated through heat treatment, only the thin film layer is bonded on the substrate wafer after separation, and the nano-scale or micro-scale thin film is broken at high temperature due to the difference of thermal expansion coefficients, so that the temperature of the thin film layer and the residual material layer is not too high, and the separation time can be prolonged to achieve the separation purpose.
After the film is separated, the influence of the film cracking problem caused by the difference of the thermal expansion coefficients is reduced, so that the temperature can be increased to carry out the heat treatment for eliminating the ion damage, the quality of the whole composite film can be enhanced by utilizing the heat treatment for eliminating the ion damage caused by the ion implantation, and the quality of a finished product of a downstream device is also improved.
The bonded body may be subjected to heat treatment in a vacuum atmosphere or in a protective atmosphere of at least one of nitrogen and an inert gas. The specific temperature and duration relationships are shown in the following table.
Name of Heat treatment Temperature of Duration of time
Bond enhancing heat treatment 220℃-300℃ 0.2-1h
Thin film layer and remainder layer separation heat treatment 150℃-190℃ 3-6h
Thermal treatment for eliminating ion damage 320℃-350℃ 2-4h
For example, under a helium atmosphere, placing the bonding body into an annealing furnace, and performing first heat treatment on the bonding body at 240 ℃ for 0.5h, namely, heat treatment for enhancing bonding force; then, performing a second heat treatment process of keeping the temperature at 180 ℃ for 5 hours, namely separating and heat treating the thin film layer and the residual material layer to separate the thin film layer from the residual material layer; and after the thin film layer is separated from the residual material layer, continuously performing third heat treatment of heating annealing at 330 ℃ for 3h on the bonding body, namely removing ion damage heat treatment to obtain the composite film. Fig. 2 is a schematic diagram illustrating formation of a simple composite film according to the present application.
In an optimized embodiment, an insulating layer can be manufactured on one surface of a substrate wafer to obtain the insulating layer; and then, contacting the insulating layer on the substrate wafer with the thin film layer of the single crystal wafer to obtain the bonding body. Fig. 3 is a schematic diagram illustrating the formation of a composite film with a silicon dioxide insulating layer according to the present embodiment.
Furthermore, a dielectric layer can be manufactured on one surface of the substrate wafer, then an insulating layer is manufactured on the dielectric layer, and the insulating layer is bonded with the thin film layer of the single crystal wafer during bonding. The manufacturing method of the dielectric layer comprises the steps of depositing polycrystalline silicon or amorphous silicon by a deposition method, generating a corrosion damage layer on the surface of a substrate wafer by an etching method, and generating an injection damage layer by injecting the substrate wafer by an injection method; and then manufacturing an insulating layer on the dielectric layer, wherein the insulating layer is bonded with the thin film layer of the single crystal wafer during bonding.
The method for forming the insulating layer is not particularly limited, and a Deposition method and a thermal oxidation method may be used, in which the Deposition method uses an LPCVD (Low Pressure Chemical Vapor Deposition) method or a PECVD (Plasma Enhanced Chemical Vapor Deposition) method to form the insulating layer.
To further illustrate the technical solutions in the present application, the embodiments of the present application further disclose the following specific examples.
Example 1
1) Preparing a 6-inch silicon wafer and a 6-inch lithium niobate wafer, respectively fixing the silicon wafer and the lithium niobate wafer on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment to obtain a smooth surface, and then carrying out semiconductor RCA cleaning on the two wafers to obtain a clean surface.
2) Injecting He into the lithium niobate wafer processed in the step 1 by adopting a stripping ion injection method+Sequentially dividing the lithium niobate wafer into a remainder layer, a separation layer and a thin film layer, and injecting He+Distributing ions in the separation layer to obtain a single crystal wafer implantation piece;
implanting He by lift-off ion implantation+The implantation dose parameters were: the implantation dose is 2 × 1016ions/cm2The implantation energy is 40keV and the implantation depth is 220 nm.
3) And bonding the thin film layer of the lithium niobate wafer injection sheet with a silicon wafer, and obtaining a bonded body by adopting a direct bonding method.
4) Putting the bonding body into an annealing furnace in a nitrogen atmosphere, and performing first heat treatment on the bonding body at 300 ℃ for 0.2h, namely heat treatment for enhancing bonding force; then performing a second heat treatment process of keeping the temperature at 150 ℃ for 6h to separate the thin film layer from the residual material layer, namely separating and heat treating the thin film layer and the residual material layer; and after the thin film layer is separated from the residual material layer, continuously performing third heat treatment of heating annealing at 320 ℃ for 4 hours on the bonding body, namely removing ion damage heat treatment to obtain the composite film.
Example 2
1) Preparing a 6-inch silicon carbide wafer and a 6-inch lithium tantalate wafer, respectively fixing the silicon carbide wafer and the lithium tantalate wafer on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment to obtain a smooth surface, and then carrying out semiconductor RCA cleaning on the two wafers to obtain a clean surface.
2) Injecting nitrogen ions into the lithium tantalate wafer processed in the step 1 by adopting a stripping ion injection method, so that the lithium tantalate wafer is sequentially divided into a residual material layer, a separation layer and a thin film layer, and the injected nitrogen ions are distributed in the separation layer to obtain a single crystal wafer injection sheet;
when the stripping ion implantation method is adopted to implant nitrogen ions, the implantation dosage parameters are as follows: the implantation dose is 2 × 1016ions/cm2The implantation energy is 400keV and the implantation depth is 492 nm.
3) A silicon dioxide layer was formed on the cleaned silicon carbide wafer by LPCVD, followed by chemical mechanical polishing to obtain a smooth surface with a thickness of 10 μm, and RCA cleaning to obtain a clean surface.
4) And bonding the thin film layer of the lithium tantalate wafer injection piece with the silicon dioxide layer on the silicon carbide wafer, and obtaining a bonded body by adopting an anode bonding method.
5) Putting the bonding body into an annealing furnace in an argon atmosphere, and performing first heat treatment of preserving heat for 1h at 220 ℃ on the bonding body, namely heat treatment for enhancing bonding force; then, performing a second heat treatment process of heat preservation at 190 ℃ for 3 hours to separate the thin film layer from the residual material layer, namely separating and heat treating the thin film layer and the residual material layer; after the thin film layer and the residual material layer are separated, continuously carrying out third heat treatment of heating annealing at 350 ℃ for 2h on the bonding body, namely, heat treatment for eliminating ion damage to obtain a composite film;
6) and fixing the composite film on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment on the film layer, and then carrying out RCA cleaning to obtain a clean surface.
Example 3
1) Preparing a 6-inch silicon nitride wafer and a 6-inch lithium niobate wafer, respectively fixing the silicon nitride wafer or the lithium niobate wafer on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment to obtain a smooth surface, and then carrying out semiconductor RCA cleaning on the two wafers to obtain a clean surface.
2) And (3) implanting oxygen ions into the lithium niobate wafer processed in the step (1) by adopting a stripping ion implantation method, so that the lithium niobate wafer is sequentially divided into a residual material layer, a separation layer and a thin film layer, and the implanted oxygen ions are distributed in the separation layer to obtain a single crystal wafer implanted sheet. When oxygen ions are implanted by adopting a stripping ion implantation method, the implantation dosage parameters are as follows: the implantation dose is 3 × 1016ions/cm2The implantation energy is 380keV and the implantation depth is 534 nm.
3) And manufacturing polycrystalline silicon on the cleaned silicon nitride wafer by using a PECVD method, wherein the thickness of the polycrystalline silicon is 1 mu m, and the polycrystalline silicon is the dielectric layer.
4) And (3) manufacturing a silicon dioxide layer on the dielectric layer by a thermal oxidation method, then carrying out chemical mechanical polishing to obtain a smooth surface with the thickness of 1 mu m, and carrying out RCA cleaning to obtain a clean surface.
5) And bonding the lithium niobate wafer injection sheet with the silicon dioxide layer, and obtaining a bonded body by adopting a low-temperature bonding method.
6) Putting the bonding body into an annealing furnace in an argon atmosphere, and performing first heat treatment on the bonding body at 250 ℃ for 0.5h, namely heat treatment for enhancing bonding force; then, performing a second heat treatment process of keeping the temperature at 160 ℃ for 4 hours to separate the thin film layer from the residual material layer, namely, performing separation heat treatment on the thin film layer and the residual material layer; and after the thin film layer is separated from the residual material layer, continuously performing third heat treatment of heating annealing at 330 ℃ for 3h on the bonding body, namely removing ion damage heat treatment to obtain the composite film.
Example 4
1) Preparing a 6-inch silicon wafer and a 6-inch lithium tantalate wafer, respectively fixing the silicon wafer and the lithium tantalate wafer on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment to obtain a smooth surface, and then carrying out semiconductor RCA cleaning on the two wafers to obtain a clean surface.
2) Injecting argon ions into the lithium niobate wafer processed in the step 1 by adopting a stripping ion injection method, so that the lithium niobate wafer is sequentially divided into a residual material layer, a separation layer and a thin film layer, and the injected argon ions are distributed in the separation layer to obtain a single crystal wafer injection sheet;
when argon ions are implanted by adopting a stripping ion implantation method, the implantation dosage parameters are as follows: the implantation dose is 4X 1016ions/cm2The implantation energy is 400keV and the implantation depth is 285 nm.
3) And (3) manufacturing amorphous silicon on the cleaned silicon wafer by using a PVD method, wherein the thickness of the amorphous silicon is 500nm, and the amorphous silicon is a dielectric layer.
4) And (3) manufacturing a silicon dioxide layer on the dielectric layer by using a PECVD method, wherein the thickness is 5 mu m, then carrying out chemical mechanical polishing to obtain a smooth surface, and cleaning the RCA to obtain a clean surface.
5) And (3) contacting the lithium tantalate wafer injection sheet with the silicon dioxide layer, and obtaining a bonded body by adopting a vacuum bonding method.
6) Putting the bonding body into an annealing furnace under a helium atmosphere, and performing first heat treatment on the bonding body at 280 ℃ for 0.4h, namely heat treatment for enhancing bonding force; then, performing a second heat treatment process of keeping the temperature at 180 ℃ for 4 hours to separate the thin film layer from the residual material layer, namely, performing separation heat treatment on the thin film layer and the residual material layer; and after the thin film layer and the residual material layer are separated, continuously performing third heat treatment of heating annealing at 350 ℃ for 2h on the bonding body, namely removing ion damage heat treatment to obtain the composite film.
7) And fixing the composite film on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment on the film layer, and then carrying out RCA cleaning to obtain a clean surface.
Example 5
1) Preparing a 6-inch silicon carbide wafer and a 6-inch lithium niobate wafer, respectively fixing the silicon carbide wafer and the lithium niobate wafer on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment to obtain a smooth surface, and then carrying out semiconductor RCA cleaning on the two wafers to obtain a clean surface.
2) H is implanted into the lithium niobate wafer processed in the step 1 by adopting a stripping ion implantation method+Sequentially dividing the lithium niobate wafer into a remainder layer, a separation layer and a thin film layer, and injecting H+Distributing ions in the separation layer to obtain a single crystal wafer implantation piece;
implanting H by lift-off ion implantation+The implantation dose parameters were: the implantation dose is 4X 1016ions/cm2The implantation energy was 40keV and the implantation depth was 287 nm.
3) Injecting argon ions on the cleaned silicon carbide wafer by an ion injection method to manufacture a silicon carbide damage layer, namely a dielectric layer; the thickness was 5 μm.
4) And (3) preparing a silicon dioxide layer on the dielectric layer by using a PECVD method, then carrying out chemical mechanical polishing to obtain a smooth surface with the thickness of 500nm, and cleaning by RCA to obtain a clean surface.
5) And contacting the lithium niobate wafer injection sheet with the silicon dioxide layer, and obtaining a bonded body by adopting a plasma enhanced bonding method.
6) Putting the bonding body into an annealing furnace in a nitrogen atmosphere, and performing first heat treatment of preserving heat for 1h at 220 ℃ on the bonding body, namely heat treatment for enhancing bonding force; then, performing a second heat treatment process of keeping the temperature at 180 ℃ for 3 hours to separate the thin film layer from the residual material layer, namely, performing separation heat treatment on the thin film layer and the residual material layer; and after the thin film layer and the residual material layer are separated, continuously performing third heat treatment of heating annealing at 350 ℃ for 2h on the bonding body, namely removing ion damage heat treatment to obtain the composite film.
7) Fixing the single crystal piezoelectric composite film on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment on the film layer, and then carrying out RCA cleaning to obtain a clean surface.
Example 6
1) Preparing a 6-inch silicon carbide wafer and a 6-inch lithium niobate wafer, respectively fixing the silicon carbide wafer and the lithium niobate wafer on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment to obtain a smooth surface, and then carrying out semiconductor RCA cleaning on the two wafers to obtain a clean surface.
2) H is implanted into the lithium niobate wafer processed in the step 1 by adopting a stripping ion implantation method+Sequentially dividing the lithium niobate wafer into a remainder layer, a separation layer and a thin film layer, and injecting H+The ions are distributed in the separation layer to obtain a single crystal wafer implantation piece. Implanting H by lift-off ion implantation+The implantation dose parameters were: the implantation dose is 4X 1016ions/cm2The implantation energy was 40keV and the implantation depth was 287 nm.
3) Corroding a damaged layer on the cleaned silicon carbide wafer by using a wet method, wherein the damaged layer is a dielectric layer; the thickness was 5 μm.
4) And (3) preparing a silicon dioxide layer on the dielectric layer by using a PECVD method, then carrying out chemical mechanical polishing to obtain a smooth surface with the thickness of 500nm, and cleaning by RCA to obtain a clean surface.
5) And contacting the lithium niobate wafer injection sheet with the silicon dioxide layer, and obtaining a bonded body by adopting an adhesive bonding method.
6) Putting the bonding body into an annealing furnace in a nitrogen atmosphere, and performing first heat treatment of preserving heat for 1h at 220 ℃ on the bonding body, namely heat treatment for enhancing bonding force; then, performing a second heat treatment process of keeping the temperature at 180 ℃ for 3 hours to separate the thin film layer from the residual material layer, namely, performing separation heat treatment on the thin film layer and the residual material layer; and after the thin film layer and the residual material layer are separated, continuously performing third heat treatment of heating annealing at 350 ℃ for 2h on the bonding body, namely removing ion damage heat treatment to obtain the composite film.
7) Fixing the single crystal piezoelectric composite film on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment on the film layer, and then carrying out RCA cleaning to obtain a clean surface.
The above examples are for illustrating the method of laminating the thin film, and do not show the limitation of the thin film wafer method. The various steps or parameters in the foregoing embodiments may also be combined in other ways, and will not be described here. The technical solutions formed by the combination of the aforementioned steps or parameters are also within the scope of the present application.
The embodiment of the application provides a film preparation method based on staged heat treatment and a composite film thereof, wherein the method comprises the following steps: implanting ions into a single crystal wafer by an ion implantation method to form a thin film layer, a separation layer and a residual material layer in the single crystal wafer, wherein the thin film layer is positioned on the surface of the single crystal wafer, and the separation layer is positioned between the thin film layer and the residual material layer; contacting one side of the single crystal wafer after ion implantation with a substrate wafer; forming a bonding body; and putting the bonding body into an annealing furnace to carry out bonding force enhancing heat treatment, thin layer and residual material layer separation heat treatment and ion damage eliminating heat treatment in sequence to obtain the composite film.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.

Claims (10)

1. A method for preparing a thin film based on staged heat treatment is characterized by comprising the following steps:
obtaining a single crystal wafer and a substrate wafer;
implanting ions into a single crystal wafer by an ion implantation method, and dividing the single crystal wafer into a residual layer, a separation layer and a thin film layer in sequence;
bonding the single crystal wafer and the substrate wafer to form a bonded body;
and (3) putting the bonding body into an annealing furnace for staged heat treatment, and putting the bonding body into the annealing furnace for heat treatment for enhancing bonding force, heat treatment for separating the thin film layer from the residual material layer and heat treatment for eliminating ion damage in sequence to obtain the composite film.
2. The method of claim 1, wherein the temperature of the bond force heat treatment is greater than the temperature of the thin film layer and residue layer separation heat treatment, and the time of the bond force heat treatment is less than the time of the thin film layer and residue layer separation heat treatment.
3. The method of claim 1, wherein the temperature of the ion damage removal heat treatment is greater than the temperature of the thin film layer and the remainder layer separation heat treatment.
4. The method of claim 1, wherein the bond force heat treatment is at 220-300 ℃ for 0.2-1 h; the thin film layer and the residual material layer are separated and thermally treated, namely, the bonding body lasts for 3-6h at the temperature of 150-190 ℃; the heat treatment for eliminating the ion damage lasts for 2-4h at 320-350 ℃.
5. The method of claim 1, wherein an insulating layer is formed on one surface of the substrate wafer or a dielectric layer is formed on one surface of the substrate wafer before the insulating layer is formed; and bonding the insulating layer on the substrate wafer and the monocrystalline wafer during bonding.
6. The method of claim 5, wherein the insulating layer is one of silicon dioxide, silicon oxynitride, and silicon nitride.
7. The method of claim 5, wherein the method for forming the dielectric layer on one side of the substrate wafer comprises: depositing polycrystalline silicon or amorphous silicon on the surface of a substrate wafer by a deposition method; or generating a corrosion damage layer on the surface of the substrate wafer by a corrosion method; or generating a corrosion damage layer on the surface of the substrate wafer by an etching method.
8. The method according to claim 1, wherein the ions of the ion implantation method are helium ions, hydrogen ions, nitrogen ions, oxygen ions, or argon ions.
9. The method of claim 1, wherein the single crystal wafer is lithium niobate, lithium tantalate, quartz, ceramic, lithium tetraborate, potassium titanyl phosphate, rubidium titanyl phosphate, gallium arsenide, or silicon; the substrate wafer is lithium niobate, lithium tantalate, a silicon wafer, a silicon carbide wafer, silicon nitride, quartz, sapphire or quartz glass.
10. A composite film produced by the method according to any one of claims 1 to 9.
CN202210089179.7A 2022-01-25 2022-01-25 Film preparation method based on staged heat treatment and composite film thereof Pending CN114420833A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115867107A (en) * 2023-02-27 2023-03-28 青禾晶元(天津)半导体材料有限公司 Method for synchronously preparing two composite piezoelectric substrates by using bonding technology

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115867107A (en) * 2023-02-27 2023-03-28 青禾晶元(天津)半导体材料有限公司 Method for synchronously preparing two composite piezoelectric substrates by using bonding technology
CN115867107B (en) * 2023-02-27 2023-12-08 青禾晶元(天津)半导体材料有限公司 Method for synchronously preparing two composite piezoelectric substrates by using bonding technology

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