CN115867106B - Composite piezoelectric substrate and preparation method and application thereof - Google Patents
Composite piezoelectric substrate and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a composite piezoelectric substrate, a preparation method and application thereof, wherein the composite piezoelectric substrate comprises a piezoelectric layer, a bonding reaction layer and a supporting layer which are arranged in a laminated manner; the preparation method comprises the following steps: (1) Bonding a piezoelectric material and a virtual support substrate to obtain a piezoelectric donor; (2) Ion implantation is carried out on one side surface of the piezoelectric layer of the piezoelectric donor, namely, a damaged layer is formed on the surface of the piezoelectric layer; (3) Bonding the piezoelectric donor and the support substrate to obtain a bonded body; (4) And carrying out heat treatment on the bonding body to enable the bonding body to be broken along the damaged layer, so that the composite piezoelectric substrate and the rest of the piezoelectric donor are obtained, and the rest of the piezoelectric donor is recycled. The preparation method eliminates deformation caused by the difference of thermal expansion coefficients in the thermal annealing process, realizes the recycling of the piezoelectric material, simplifies the process flow and improves the product yield.
Description
Technical Field
The invention belongs to the technical field of piezoelectric substrate manufacturing, relates to a composite piezoelectric substrate, and particularly relates to a composite piezoelectric substrate, a preparation method and application thereof.
Background
The piezoelectric material has the function of conversion and inverse conversion between mechanical energy and electric energy due to the piezoelectric effect. The principle of the piezoelectric effect is: if pressure is applied to the piezoelectric material, it will generate a potential difference, known as the positive piezoelectric effect; conversely, application of a voltage produces mechanical stress, known as the inverse piezoelectric effect. If the pressure is a high frequency shock, the current generated is a high frequency current.
Lithium niobate and lithium tantalate are the most widely used novel electrodeless materials at present, belong to very excellent piezoelectric transduction materials, and lithium tantalate has excellent piezoelectric, ferroelectric, acousto-optic and electro-optic effects, and is widely applied to electronic communication devices such as resonators, filters, transducers and the like and high-frequency surface acoustic wave devices. The lithium niobate has good nonlinear optical property, and can be used as an optical waveguide material or used for manufacturing a middle-low frequency acoustic surface filter, a high-power high-temperature-resistant ultrasonic transducer and the like.
Compared with piezoelectric crystals, the piezoelectric substrate prepared from lithium niobate and lithium tantalate has the advantages of high frequency, good temperature compensation, good stability, low manufacturing cost and the like, and has the advantage of irreplaceability in the fields of RF (radio frequency), optical fiber communication, RF filters and the like. Typically the composite piezoelectric substrate consists of a thin film layer of piezoelectric material, an insulating layer and a substrate layer of semiconductor material.
However, since the difference between the thermal expansion coefficients of the piezoelectric material and the semiconductor material substrate is very large, significant deformation occurs during the peeling heat process after heterobonding, and thus quality problems such as bond fracture are caused. In the prior art, when the piezoelectric material film is prepared, the bonded body is thinned and then thermally annealed, so that the piezoelectric material cannot be reused, the processing steps and the cost are increased, and the yield of products is reduced.
The other technology uses UV ultraviolet curing optical cement to bond the semiconductor material with the piezoelectric material after the photoresist is uniformly coated on the semiconductor material, and uses UV light irradiation to bond the virtual semiconductor material with the piezoelectric material and then carries out subsequent processes, so that the deformation in the thermal annealing process after bonding is reduced, but the method has the risk of contamination of the organic UV optical cement, is very sensitive to temperature and has complex operation process.
CN 111919290a discloses a process for transferring a piezoelectric layer onto a carrier substrate, said process comprising: (1) Providing a donor substrate comprising a heterostructure including a piezoelectric substrate bonded to an handle substrate, and a polymerized adhesive layer located at an interface between the piezoelectric substrate and the handle substrate; (2) Forming a weakened region in the piezoelectric substrate, thereby defining a piezoelectric layer to be transferred; (3) providing a carrier substrate; (4) Forming a dielectric layer on a main surface of the carrier substrate and/or the piezoelectric substrate; (5) Bonding the donor substrate to the carrier substrate, the dielectric layer being located at the bonding interface; (6) The donor substrate is divided and separated along the weakened region at a temperature lower than or equal to 300 ℃. The process introduces the organic UV ultraviolet curing optical adhesive, the risk of contamination of the organic UV optical adhesive exists, and a large room for improvement is left.
Therefore, how to provide a composite piezoelectric substrate and a preparation method thereof, eliminate deformation caused by thermal expansion coefficient difference in the thermal annealing process, realize the recycling of piezoelectric materials, simplify the process flow, avoid the use of organic UV optical adhesive, reduce the processing cost and improve the product yield, and become the urgent problem to be solved by the current technicians in the field.
Disclosure of Invention
The invention aims to provide a composite piezoelectric substrate, a preparation method and application thereof, wherein the preparation method eliminates deformation caused by thermal expansion coefficient difference in the thermal annealing process, simultaneously realizes the recycling of piezoelectric materials, simplifies the process flow, avoids the use of organic UV optical cement, reduces the processing cost, improves the product yield, and is beneficial to large-scale popularization and application.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a composite piezoelectric substrate, the method comprising the steps of:
(1) Bonding a piezoelectric material and a virtual supporting substrate to obtain a piezoelectric donor containing a piezoelectric layer and a virtual supporting layer;
(2) Ion implantation is carried out on one side surface of the piezoelectric layer of the piezoelectric donor obtained in the step (1), namely, a damaged layer is formed on the surface of the piezoelectric layer;
(3) Bonding the piezoelectric layer of the piezoelectric donor obtained in the step (2) with a supporting substrate to obtain a bonded body;
(4) And (3) carrying out heat treatment on the bonding body obtained in the step (3) to disconnect the bonding body along the damaged layer, so as to obtain a composite piezoelectric substrate and a piezoelectric donor residual part, wherein the piezoelectric donor residual part is reused in the step (1).
According to the preparation method provided by the invention, the piezoelectric material and the virtual support substrate are bonded to form the piezoelectric donor, and then the piezoelectric donor and the support substrate are bonded to realize the transfer of the film, and the deformation caused by the difference of the thermal expansion coefficients in the thermal annealing process is eliminated by adjusting the product structure, so that the repeated utilization of the piezoelectric material is realized, the process flow is simplified, the use of organic UV optical cement is avoided, the processing cost is reduced, the product yield is improved, and the large-scale popularization and application are facilitated.
Preferably, the piezoelectric material and the virtual support substrate in step (1) are subjected to chemical cleaning and activation treatment, respectively and independently, in sequence, before bonding.
Preferably, the chemical cleaning is performed using the RCA standard cleaning method.
In the invention, the cleaning liquid adopted by the RCA standard cleaning method comprises any one of SPM, DHF, APM or HPM.
Specifically, the SPM is a mixed solution of sulfuric acid solution and hydrogen peroxide, and the cleaning temperature is 120-150 ℃; the DHF is hydrofluoric acid solution, and the cleaning temperature is 20-25 ℃; the APM is a mixed solution of ammonia water and hydrogen peroxide, and the cleaning temperature is 30-80 ℃; the HPM is a mixed solution of hydrochloric acid solution and hydrogen peroxide, and the cleaning temperature is 65-85 ℃.
Preferably, the chemical cleaning is performed until the surface of the piezoelectric material and the virtual support substrate respectively satisfies a roughness Ra of 0.05 to 0.5nm, and may be, for example, 0.05nm, 0.1nm, 0.15nm, 0.2nm, 0.25nm, 0.3nm, 0.35nm, 0.4nm, 0.45nm or 0.5nm, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the chemical cleaning is performed until the number of particles of the piezoelectric material and the surface of the virtual support substrate, respectively, satisfies a size of 0.3 μm or more, which is not limited to the recited values, but may be 5, 10, 15, 20, 25 or 30, for example.
In the invention, the surfaces of the piezoelectric material and the virtual support substrate subjected to chemical cleaning are smooth and clean enough, and intermolecular acting force can be generated under certain pressure to realize mutual bonding.
Preferably, the activation treatment includes bombarding the surfaces to be bonded of the piezoelectric material and the virtual support substrate, respectively, with Ar ions.
Preferably, the bonding in step (1) is performed in a vacuum environment and the absolute vacuum is less than or equal to 10 -3 Pa may be, for example, 5X 10 -5 Pa、10 -5 Pa、5×10 -4 Pa、10 -4 Pa、5×10 -3 Pa or 10 -3 Pa, but is not limited to the recited values, and other non-recited values within this range are equally applicable.
The bonding temperature in step (1) is preferably 20 to 40 ℃, and may be, for example, 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃, 30 ℃, 32 ℃, 34 ℃, 36 ℃, 38 ℃, or 40 ℃, but is not limited to the recited values, and other non-recited values within the range are equally applicable.
In the invention, the bonding is performed at normal temperature without a thermal annealing process to increase bonding force, thereby avoiding deformation caused by the difference of thermal expansion coefficients.
Preferably, the strength of the bond in step (1) is not less than 1.5J/cm 2 For example, it may be 1.5J/cm 2 、2J/cm 2 、2.5J/cm 2 、3J/cm 2 、3.5J/cm 2 、4J/cm 2 、4.5J/cm 2 Or 5J/cm 2 But are not limited to, the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the ion implantation in the step (2) further comprises grinding and polishing the piezoelectric layer of the piezoelectric donor, and the thickness of the piezoelectric layer after the polishing is 2-150 μm, for example, may be 2 μm, 5 μm, 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm, 110 μm, 120 μm, 130 μm, 140 μm or 150 μm, but is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Preferably, the ion implantation in step (2) is performed using hydrogen ions and/or helium ions.
Preferably, the depth of the ion implantation in step (2) is 0.2-2 μm, for example, 0.2 μm, 0.4 μm, 0.6 μm, 0.8 μm, 1 μm, 1.2 μm, 1.4 μm, 1.6 μm, 1.8 μm or 2 μm, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the difference in thermal expansion coefficient between the support substrate in step (3) and the virtual support substrate in step (1) is not more than 3%, for example, may be 0%, 0.5%, 1%, 1.5%, 2%, 2.5% or 3%, and more preferably 0%, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the support substrate of step (3) is further provided with an insulating layer on the surface to be bonded before bonding.
Preferably, the preparation method of the insulating layer includes a thermal oxidation method and/or a deposition method.
Preferably, in step (3), the piezoelectric donor and the support substrate are respectively and independently subjected to chemical cleaning and activation treatment in sequence before bonding.
In the present invention, the conditions of the chemical cleaning and activating treatment in the step (3) and the chemical cleaning and activating treatment in the step (1) are the same, so that the description thereof will not be repeated here.
Preferably, the chemical cleaning and the activating treatment further comprise in-situ deposition of a bonding reaction layer on the piezoelectric layer of the piezoelectric donor and/or the surface to be bonded of the support substrate in a vacuum environment.
Preferably, the in-situ deposition method of the bonding reaction layer comprises any one of electron beam evaporation, DC magnetron sputtering or radio frequency sputtering.
Preferably, the bonding in step (3) is performed in a vacuum environment and the absolute vacuum is less than or equal to 10 -3 Pa may be, for example, 5X 10 -5 Pa、10 -5 Pa、5×10 -4 Pa、10 -4 Pa、5×10 -3 Pa or 10 -3 Pa, but is not limited to the recited values, and other non-recited values within this range are equally applicable.
In the invention, the in-situ deposition and the subsequent bonding of the bonding reaction layer are carried out in a vacuum environment, namely, the deposition step is carried out in a high vacuum environment, and then the bonding step is carried out, so that an object to be bonded after the deposition step is not required to be moved out of the high vacuum environment, thereby ensuring the quality of the bonding reaction layer and the bonding connection strength to the greatest extent.
Preferably, the bonding temperature in step (3) is 20 to 40 ℃, and may be, for example, 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃, 30 ℃, 32 ℃, 34 ℃, 36 ℃, 38 ℃, or 40 ℃, but is not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the bonding strength in step (3) is not less than 1.5J/cm 2 For example, it may be 1.5J/cm 2 、2J/cm 2 、2.5J/cm 2 、3J/cm 2 、3.5J/cm 2 、4J/cm 2 、4.5J/cm 2 Or 5J/cm 2 But are not limited to, the recited values, and other non-recited values within the range of values are equally applicable.
The temperature of the heat treatment in the step (4) is preferably 100 to 300 ℃, and may be, for example, 100 ℃, 120 ℃, 140 ℃, 160 ℃, 180 ℃, 200 ℃, 220 ℃, 240 ℃, 260 ℃, 280 ℃ or 300 ℃, but is not limited to the values listed, and other values not listed in the range are equally applicable.
Preferably, the heat treatment in the step (4) is accompanied by a pressurizing treatment, and the pressurizing treatment has a pressure value of 0.1 to 20MPa, for example, 0.1MPa, 1MPa, 2MPa, 4MPa, 6MPa, 8MPa, 10MPa, 12MPa, 14MPa, 16MPa, 18MPa or 20MPa, but the present invention is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
In a second aspect, the present invention provides a composite piezoelectric substrate prepared by the preparation method according to the first aspect, the composite piezoelectric substrate comprising a piezoelectric layer, a bonding reaction layer and a support layer which are stacked.
Preferably, an insulating layer is further arranged between the bonding reaction layer and the supporting layer.
Preferably, the material of the piezoelectric layer includes any one of lithium niobate, lithium tantalate, and piezoelectric ceramic.
Preferably, the material of the bonding reaction layer includes any one or a combination of at least two of titanium dioxide, silicon monoxide, ferric oxide or ferric oxide, and typical but non-limiting combinations include a combination of titanium dioxide and silicon monoxide, a combination of silicon monoxide and ferric oxide, a combination of ferric oxide and ferric oxide, a combination of titanium dioxide, silicon monoxide and ferric oxide, or a combination of silicon monoxide, ferric oxide and ferric oxide.
Preferably, the bonding reaction layer contains Ar ion, and the content of Ar ion in the bonding reaction layer is less than or equal to 1wt%, for example, 0.1wt%, 0.2wt%, 0.3wt%, 0.4wt%, 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt% or 1wt%, but not limited to the recited values, and other non-recited values in the range of values are equally applicable.
Preferably, the material of the insulating layer includes any one or a combination of at least two of silicon oxide, polysilicon, amorphous silicon or silicon nitride, and typically, but not limited to, a combination of silicon oxide and polysilicon, a combination of polysilicon and amorphous silicon, a combination of amorphous silicon and silicon nitride, a combination of silicon oxide, polysilicon and amorphous silicon, or a combination of polysilicon, amorphous silicon and silicon nitride.
Preferably, the material of the supporting layer includes any one of monocrystalline silicon, sapphire, silicon carbide, spinel, quartz, glass, aluminum nitride or diamond.
The thickness of the piezoelectric layer is preferably 0.2 to 2 μm, and may be, for example, 0.2 μm, 0.4 μm, 0.6 μm, 0.8 μm, 1 μm, 1.2 μm, 1.4 μm, 1.6 μm, 1.8 μm or 2 μm, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
The thickness of the bonding reaction layer is preferably 0.5 to 15nm, and may be, for example, 0.5nm, 1nm, 2nm, 3nm, 4nm, 5nm, 6nm, 7nm, 8nm, 9nm, 10nm, 11nm, 12nm, 13nm, 14nm or 15nm, but is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
The thickness of the insulating layer is preferably 0.1 to 5 μm, and may be, for example, 0.1 μm, 0.5 μm, 1 μm, 1.5 μm, 2 μm, 2.5 μm, 3 μm, 3.5 μm, 4 μm, 4.5 μm or 5 μm, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
The thickness of the support layer is preferably 300 to 1000. Mu.m, for example 300 μm, 350 μm, 400 μm, 450 μm, 500 μm, 550 μm, 600 μm, 650 μm, 700 μm, 750 μm, 800 μm, 850 μm, 900 μm, 950 μm or 1000 μm, but is not limited to the values recited, and other values not recited in the range of values are equally applicable.
In a third aspect, the present invention provides the use of a composite piezoelectric substrate as described in the second aspect for the manufacture of a filter or modulator.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method provided by the invention, the piezoelectric material and the virtual support substrate are bonded to form the piezoelectric donor, and then the piezoelectric donor and the support substrate are bonded to realize the transfer of the film, and the deformation caused by the difference of the thermal expansion coefficients in the thermal annealing process is eliminated by adjusting the product structure, so that the repeated utilization of the piezoelectric material is realized, the process flow is simplified, the use of organic UV optical cement is avoided, the processing cost is reduced, the product yield is improved, and the large-scale popularization and application are facilitated.
Drawings
FIG. 1 is a schematic flow chart of a preparation method of a composite piezoelectric substrate provided by the invention.
Wherein: 10-a piezoelectric donor; 11-a piezoelectric layer; 12-a virtual support layer; 13-a damaged layer; 20-supporting a substrate; 21-an insulating layer; 22-a support layer; 30-a linker; 31-bonding reaction layer.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a composite piezoelectric substrate and a preparation method thereof, as shown in fig. 1, wherein the preparation method comprises the following steps:
(1) First pressThe electric material and the virtual support substrate are respectively and independently subjected to chemical cleaning and activation treatment in sequence, and then are subjected to chemical cleaning and activation treatment in a vacuum environment (the absolute vacuum degree is 10) -4 Pa) and bonding at 30 ℃ with bonding strength of 2J/cm 2 Obtaining a piezoelectric donor 10 including a piezoelectric layer 11 and a virtual support layer 12; the chemical cleaning is carried out by adopting an RCA standard cleaning method until the surfaces of the piezoelectric material and the virtual support substrate respectively meet the requirement that the roughness Ra is 0.25+/-0.05 nm and the number of particles with the size of more than 0.3 mu m is less than or equal to 20; the activation treatment is to bombard the surface to be bonded of the piezoelectric material and the virtual support substrate respectively by Ar ions;
(2) Polishing the piezoelectric layer 11 of the piezoelectric donor 10 obtained in the step (1) until the thickness of the piezoelectric layer 11 is 25 mu m, and then implanting hydrogen ions into one side surface of the piezoelectric layer 11 to an implantation depth of 1 mu m, namely forming a damaged layer 13 on the surface of the piezoelectric layer 11;
(3) Providing a support substrate 20, wherein the thermal expansion coefficients of the support substrate 20 and the virtual support substrate are consistent, and preparing an insulating layer 21 on the surface of the support substrate 20 by using a deposition method and a thermal oxidation method;
(4) The piezoelectric donor 10 obtained in the step (2) and the support substrate 20 obtained in the step (3) are respectively and independently subjected to chemical cleaning and activation treatment in turn, and then are subjected to a vacuum treatment (absolute vacuum degree is 10) -4 Pa) the bonding reaction layer 31 is deposited in situ on the piezoelectric layer 11 of the piezoelectric donor 10 by electron beam evaporation, and finally the piezoelectric layer 11 of the piezoelectric donor 10 and the insulating layer 21 of the support substrate 20 are deposited in a vacuum environment (absolute vacuum degree 10 -5 Pa) and bonding at 30 ℃ with bonding strength of 2J/cm 2 Obtaining a bonded body 30; the conditions of the chemical cleaning and the activation treatment are the same as those in the step (1), so that the description is omitted here;
(5) And (3) carrying out heat treatment on the bonding body 30 obtained in the step (4) at 200 ℃ and simultaneously carrying out pressurization treatment under 10MPa, so that the bonding body 30 is broken along the damaged layer 13 to obtain a composite piezoelectric substrate and a piezoelectric donor residual part, and the piezoelectric donor residual part is recycled in the step (1) for recycling.
As shown in fig. 1, the composite piezoelectric substrate obtained in this embodiment includes a piezoelectric layer 11, a bonding reaction layer 31, an insulating layer 21, and a support layer 22, which are stacked.
Specifically, the piezoelectric layer 11 is made of lithium niobate, and has a thickness of 1 μm; the bonding reaction layer 31 is made of titanium dioxide and has a thickness of 2nm; the bonding reaction layer 31 contains Ar ions, and the content of the Ar ions in the bonding reaction layer 31 is 0.8wt%; the insulating layer 21 is made of silicon oxide and has a thickness of 1 μm; the material of the supporting layer 22 is monocrystalline silicon, and the thickness is 500 μm.
Example 2
The embodiment provides a composite piezoelectric substrate and a preparation method thereof, as shown in fig. 1, wherein the preparation method comprises the following steps:
(1) The piezoelectric material and the virtual support substrate are respectively and independently subjected to chemical cleaning and activation treatment in sequence, and then are subjected to chemical cleaning and activation treatment in a vacuum environment (the absolute vacuum degree is 10) -4 Pa) and bonding at 20℃with a bonding strength of 1.5J/cm 2 Obtaining a piezoelectric donor 10 including a piezoelectric layer 11 and a virtual support layer 12; the chemical cleaning is carried out by adopting an RCA standard cleaning method until the surfaces of the piezoelectric material and the virtual support substrate respectively meet the requirement that the roughness Ra is 0.45+/-0.05 nm and the number of particles with the size of more than 0.3 mu m is less than or equal to 30; the activation treatment is to bombard the surface to be bonded of the piezoelectric material and the virtual support substrate respectively by Ar ions;
(2) Polishing the piezoelectric layer 11 of the piezoelectric donor 10 obtained in the step (1) until the thickness of the piezoelectric layer 11 is 50 mu m, and then implanting helium ions into one side surface of the piezoelectric layer 11 to an implantation depth of 1 mu m, namely forming a damaged layer 13 on the surface of the piezoelectric layer 11;
(3) Providing a support substrate 20, and preparing an insulating layer 21 on the surface of the support substrate 20 by a deposition method, wherein the difference of thermal expansion coefficients between the support substrate 20 and the virtual support substrate is 2%;
(4) The piezoelectric donor 10 obtained in the step (2) and the support substrate 20 obtained in the step (3) are respectively and independently carried out in sequenceChemical cleaning and activating treatment, and then in vacuum environment (absolute vacuum degree is 10 -3 Pa) the insulating layer 21 of the support substrate 20 is subjected to in-situ deposition of the bonding reaction layer 31 by DC magnetron sputtering, and finally the piezoelectric layer 11 of the piezoelectric donor 10 and the insulating layer 21 of the support substrate 20 are subjected to in-vacuum (absolute vacuum degree 10) -5 Pa) and bonding at 20℃with a bonding strength of 1.5J/cm 2 Obtaining a bonded body 30; the conditions of the chemical cleaning and the activation treatment are the same as those in the step (1), so that the description is omitted here;
(5) And (3) carrying out heat treatment on the bonding body 30 obtained in the step (4) at 100 ℃, and simultaneously carrying out pressurization treatment under 20MPa, so that the bonding body 30 is broken along the damaged layer 13 to obtain a composite piezoelectric substrate and a piezoelectric donor residual part, and the piezoelectric donor residual part is recycled in the step (1) for recycling.
As shown in fig. 1, the composite piezoelectric substrate obtained in this embodiment includes a piezoelectric layer 11, a bonding reaction layer 31, an insulating layer 21, and a support layer 22, which are stacked.
Specifically, the piezoelectric layer 11 is made of lithium tantalate, and has a thickness of 2 μm; the bonding reaction layer 31 is made of silicon monoxide and has a thickness of 10nm; the bonding reaction layer 31 contains Ar ions, and the content of the Ar ions in the bonding reaction layer 31 is 1wt%; the insulating layer 21 is made of silicon oxide and has a thickness of 2 μm; the material of the supporting layer 22 is monocrystalline silicon, and the thickness is 625 μm.
Example 3
The embodiment provides a composite piezoelectric substrate and a preparation method thereof, as shown in fig. 1, wherein the preparation method comprises the following steps:
(1) The piezoelectric material and the virtual support substrate are respectively and independently subjected to chemical cleaning and activation treatment in sequence, and then are subjected to chemical cleaning and activation treatment in a vacuum environment (the absolute vacuum degree is 5 multiplied by 10) -5 Pa) and bonding at 25℃with a bonding strength of 1.5J/cm 2 Obtaining a piezoelectric donor 10 including a piezoelectric layer 11 and a virtual support layer 12; the chemical cleaning is carried out by adopting an RCA standard cleaning method until piezoelectric materials and virtual materials are obtainedThe surface of the substrate to be supported respectively meets the requirements that the roughness Ra is 0.1 plus or minus 0.05nm, and the number of particles with the size of more than 0.3 mu m is less than or equal to 15; the activation treatment is to bombard the surface to be bonded of the piezoelectric material and the virtual support substrate respectively by Ar ions;
(2) Polishing the piezoelectric layer 11 of the piezoelectric donor 10 obtained in the step (1) until the thickness of the piezoelectric layer 11 is 2 mu m, and then implanting hydrogen ions into one side surface of the piezoelectric layer 11 to an implantation depth of 0.8 mu m, namely forming a damaged layer 13 on the surface of the piezoelectric layer 11;
(3) Providing a support substrate 20, and preparing an insulating layer 21 on the surface of the support substrate 20 by using a thermal oxidation method, wherein the difference of thermal expansion coefficients between the support substrate 20 and the virtual support substrate is 3%;
(4) The piezoelectric donor 10 obtained in the step (2) and the support substrate 20 obtained in the step (3) are respectively and independently subjected to chemical cleaning and activation treatment in turn, and then are subjected to a vacuum treatment (absolute vacuum degree is 5×10) -35 Pa) the bonding reaction layer 31 is deposited in situ on the piezoelectric layer 11 of the piezoelectric donor 10 by radio frequency sputtering, and finally the piezoelectric layer 11 of the piezoelectric donor 10 and the insulating layer 21 of the supporting substrate 20 are subjected to vacuum (absolute vacuum degree is 5×10) -5 Pa) and bonding at 25℃with a bonding strength of 2.0J/cm 2 Obtaining a bonded body 30; the conditions of the chemical cleaning and the activation treatment are the same as those in the step (1), so that the description is omitted here;
(5) And (3) carrying out heat treatment on the bonding body 30 obtained in the step (4) at 300 ℃, and simultaneously carrying out pressurization treatment under 1MPa, so that the bonding body 30 is broken along the damaged layer 13 to obtain a composite piezoelectric substrate and a piezoelectric donor residual part, and the piezoelectric donor residual part is recycled in the step (1) for recycling.
As shown in fig. 1, the composite piezoelectric substrate obtained in this embodiment includes a piezoelectric layer 11, a bonding reaction layer 31, an insulating layer 21, and a support layer 22, which are stacked.
Specifically, the piezoelectric layer 11 is made of piezoelectric ceramic, and has a thickness of 0.6 μm; the bonding reaction layer 31 is made of ferric oxide, and has a thickness of 0.5nm; the bonding reaction layer 31 contains Ar ions, and the content of the Ar ions in the bonding reaction layer 31 is 0.5wt%; the insulating layer 21 is made of silicon oxide and has a thickness of 0.1 μm; the material of the supporting layer 22 is monocrystalline silicon, and the thickness is 300 μm.
Example 4
The present embodiment provides a composite piezoelectric substrate and a method for preparing the same, and the method for preparing the same is not described herein, except that the in-situ deposition of the bonding reaction layer 31 in the step (4) is removed, and the other steps and conditions are the same as those in embodiment 1.
The composite piezoelectric substrate obtained in this embodiment includes the piezoelectric layer 11, the insulating layer 21, and the supporting layer 22, which are stacked.
Comparative example 1
The present comparative example provides a composite piezoelectric substrate and a method for manufacturing the same, which is performed with reference to the specific embodiment in CN 111919290a, and will not be described herein.
Compared with example 1, the comparative example introduces the organic UV-curable optical adhesive, which has the risk of contamination of the organic UV-curable optical adhesive, is very sensitive to temperature, and has complicated operation process.
Therefore, the preparation method provided by the invention firstly bonds the piezoelectric material and the virtual support substrate to form the piezoelectric donor, then bonds the piezoelectric donor and the support substrate to realize the transfer of the film, and by adjusting the product structure, the deformation caused by the difference of the thermal expansion coefficients in the thermal annealing process is eliminated, meanwhile, the repeated utilization of the piezoelectric material is realized, the process flow is simplified, the use of organic UV optical cement is avoided, the processing cost is reduced, the product yield is improved, and the large-scale popularization and application are facilitated.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (9)
1. A method for preparing a composite piezoelectric substrate, the method comprising the steps of:
(1) The piezoelectric material and the virtual supporting substrate are arranged in the absolute vacuum degree of less than or equal to 10 -3 Bonding is carried out in a vacuum environment of Pa, and a piezoelectric donor containing a piezoelectric layer and a virtual supporting layer is obtained; the piezoelectric material and the virtual support substrate are respectively and independently subjected to chemical cleaning and activating treatment in sequence before bonding, and the chemical cleaning is carried out until the surfaces of the piezoelectric material and the virtual support substrate respectively meet the requirement that the roughness Ra is 0.05-0.5nm, and the number of particles with the size of more than 0.3 mu m is less than or equal to 30; the activation treatment comprises the steps of bombarding the surfaces to be bonded of the piezoelectric material and the virtual support substrate respectively by Ar ions;
(2) Ion implantation is carried out on one side surface of the piezoelectric layer of the piezoelectric donor obtained in the step (1), namely, a damaged layer is formed on the surface of the piezoelectric layer;
(3) The absolute vacuum degree of the piezoelectric layer of the piezoelectric donor obtained in the step (2) and the supporting substrate is less than or equal to 10 -3 Bonding is carried out in a vacuum environment of Pa to obtain a bonding body; the piezoelectric donor and the support substrate are respectively and independently subjected to chemical cleaning and activating treatment in sequence before bonding, and an in-situ deposition bonding reaction layer is further arranged between the chemical cleaning and activating treatment and used for carrying out in-situ deposition bonding reaction on the piezoelectric layer of the piezoelectric donor and/or the surface to be bonded of the support substrate in a vacuum environment;
(4) Carrying out heat treatment on the bonding body obtained in the step (3), and carrying out pressurization treatment, wherein the pressure value of the pressurization treatment is 0.1-20MPa, so that the bonding body is disconnected along a damaged layer to obtain a composite piezoelectric substrate and a piezoelectric donor residual part, and the piezoelectric donor residual part is recycled in the step (1) for recycling;
wherein the bonding temperature in the step (1) and the step (3) is 20-40 ℃; the bonding strength is more than or equal to 1.5J/cm 2 。
2. The method of claim 1, wherein the chemical cleaning in step (1) is performed using RCA standard cleaning.
3. The method according to claim 1, wherein the ion implantation in step (2) is preceded by a lapping and polishing treatment of the piezoelectric layer of the piezoelectric donor, and the thickness of the piezoelectric layer after the polishing treatment is 2 to 150 μm;
the ion implantation in the step (2) is performed by adopting hydrogen ions and/or helium ions;
the depth of the ion implantation in the step (2) is 0.2-2 mu m;
the difference of the thermal expansion coefficients between the support substrate in the step (3) and the virtual support substrate in the step (1) is less than or equal to 3 percent;
step (3), preparing an insulating layer on the surface to be bonded of the support substrate before bonding;
the preparation method of the insulating layer comprises a thermal oxidation method and/or a deposition method.
4. The method of claim 1, wherein the in-situ deposition of the bonding reaction layer in step (3) comprises any one of electron beam evaporation, DC magnetron sputtering or radio frequency sputtering.
5. The method according to claim 1, wherein the temperature of the heat treatment in step (4) is 100 to 300 ℃.
6. A composite piezoelectric substrate produced by the production method according to any one of claims 1 to 5, wherein the composite piezoelectric substrate comprises a piezoelectric layer, a bonding reaction layer, and a support layer which are laminated.
7. The composite piezoelectric substrate according to claim 6, wherein an insulating layer is further provided between the bonding reaction layer and the support layer;
the piezoelectric layer is made of any one of lithium niobate, lithium tantalate or piezoelectric ceramic;
the bonding reaction layer is made of any one or a combination of at least two of titanium dioxide, silicon monoxide, ferric oxide or ferric oxide;
ar ions are contained in the bonding reaction layer, and the content of the Ar ions in the bonding reaction layer is less than or equal to 1wt%;
the insulating layer is made of any one or a combination of at least two of silicon oxide, polysilicon, amorphous silicon and silicon nitride;
the material of the supporting layer comprises any one of monocrystalline silicon, sapphire, silicon carbide, spinel, quartz, glass, aluminum nitride or diamond.
8. The composite piezoelectric substrate according to claim 7, wherein the piezoelectric layer has a thickness of 0.2-2 μm;
the thickness of the bonding reaction layer is 0.5-15nm;
the thickness of the insulating layer is 0.1-5 mu m;
the thickness of the supporting layer is 300-1000 mu m.
9. Use of a composite piezoelectric substrate according to any of claims 6-8 for the manufacture of a filter or modulator.
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