CN113764572A - Preparation method of heterogeneous single crystal film for acoustic filter - Google Patents
Preparation method of heterogeneous single crystal film for acoustic filter Download PDFInfo
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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
- H10N30/04—Treatments to modify a piezoelectric or electrostrictive property, e.g. polarisation characteristics, vibration characteristics or mode tuning
-
- H—ELECTRICITY
- H03—ELECTRONIC CIRCUITRY
- H03H—IMPEDANCE NETWORKS, e.g. RESONANT CIRCUITS; RESONATORS
- H03H3/00—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators
- H03H3/007—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators for the manufacture of electromechanical resonators or networks
- H03H3/02—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators for the manufacture of electromechanical resonators or networks for the manufacture of piezoelectric or electrostrictive resonators or networks
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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
- H03—ELECTRONIC CIRCUITRY
- H03H—IMPEDANCE NETWORKS, e.g. RESONANT CIRCUITS; RESONATORS
- H03H3/00—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators
- H03H3/007—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators for the manufacture of electromechanical resonators or networks
- H03H3/02—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators for the manufacture of electromechanical resonators or networks for the manufacture of piezoelectric or electrostrictive resonators or networks
- H03H2003/023—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators for the manufacture of electromechanical resonators or networks for the manufacture of piezoelectric or electrostrictive resonators or networks the resonators or networks being of the membrane type
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Abstract
The invention relates to the technical field of acoustic filters, in particular to a preparation method of a heterogeneous single crystal film for an acoustic filter. The preparation method of the heterogeneous single crystal film comprises the following steps: providing a heterogeneous thin film structure; the heterogeneous thin film structure comprises a piezoelectric thin film; performing post-annealing treatment on the heterogeneous thin film structure; the post-annealing temperature range is 300-800 ℃; the post-annealing atmosphere contains an element material corresponding to the piezoelectric thin film. Therefore, bonding strength can be improved, lattice defects can be recovered, the problem of external release of lithium elements, oxygen elements and the like in the piezoelectric film can be effectively solved, and the quality of the heterogeneous single crystal film is improved.
Description
Technical Field
The invention relates to the technical field of acoustic filters, in particular to a preparation method of a heterogeneous single crystal film for an acoustic filter.
Background
With the advent of the 5G era, frequencies in communication systems have increased, bandwidth has expanded, and the requirements of related high-performance filters have put higher demands on materials. In recent years, the rising of the piezoelectric film enables the size of related optical and acoustic devices to be greatly reduced, the working efficiency is improved, and a novel working mode is realized.
Currently, integrating piezoelectric material with silicon provides a material-level integrated wafer substrate that provides a material platform for the fabrication of monolithically integrated modules. In addition, the piezoelectric material is bonded with a foreign substrate, particularly a rigid substrate, namely a substrate with a large Young modulus, so that the center frequency and the bandwidth of a related filter can be effectively improved, and the power consumption can be reduced. Corresponding wafer materials can be provided by transferring the piezoelectric single crystals to the required substrate by using an ion beam stripping method, the thickness of the piezoelectric film is uniform, and the prepared device has good stability. However, the preparation of the piezoelectric thin film by ion implantation requires high-temperature annealing to recover lattice defects in the material introduced by ion implantation, so that the piezoelectric material has diffusion of lighter elements at high temperature, especially Li, O and other elements, and the material composition on the surface of the thin film changes, which makes it difficult to prepare high-quality piezoelectric single crystal thin films and large-bandwidth filters.
Disclosure of Invention
The invention aims to solve the technical problem that the preparation method in the prior art has the defects that the components of the piezoelectric single crystal film material are easy to change, so that the film quality is low.
In order to solve the technical problem, the application discloses a method for preparing a heterogeneous single crystal thin film for an acoustic filter, which comprises the following steps:
providing a heterogeneous thin film structure; the heterogeneous thin film structure comprises a piezoelectric thin film;
performing post-annealing treatment on the heterogeneous thin film structure; the post-annealing temperature range is 300-800 ℃; the post-annealing atmosphere contains an element material corresponding to the piezoelectric thin film.
Optionally, the providing a heterogeneous thin film structure comprises:
providing a support substrate and a piezoelectric film having a defect layer;
bonding the piezoelectric film with the defect layer and the support substrate to obtain a heterostructure to be stripped;
and carrying out annealing, peeling and transferring treatment on the heterostructure to be peeled to obtain the heterostructure.
Optionally, the material of the supporting substrate comprises at least one or a combination of more of silicon, silicon oxide, sapphire, diamond, aluminum nitride, gallium nitride, SOI and silicon carbide;
the material of the piezoelectric film comprises lithium-containing piezoelectric crystals.
Optionally, the bonding temperature range is 40-250 ℃;
the pressure range of the bonding is 1e-5Mbar-1000 mbar.
Optionally, the temperature range of the annealing, stripping and transferring is 100-300 ℃;
the time for annealing, peeling and transferring is 1-100 hours.
Optionally, the method for preparing the piezoelectric film with the defect layer includes:
providing a piezoelectric film; the piezoelectric film includes a first surface;
and performing ion implantation on the piezoelectric film from the first surface to form a defective layer in the piezoelectric film, thereby obtaining the piezoelectric film with the defective layer.
Optionally, the ion implantation method includes hydrogen ion implantation, helium ion implantation, neon ion implantation or hydrogen-helium ion co-implantation.
Optionally, the temperature of the implanted ions is 50-150 ℃;
the energy of the ion implantation is 1-2000 kilo electron volts;
the ion implantation dose is 1 × 1016～1.5×1017Per square centimeter.
Optionally, the support substrate comprises a second surface;
bonding the piezoelectric film with the defect layer and the supporting substrate to obtain a heterostructure to be stripped, comprising:
bonding the piezoelectric film with the defect layer and the supporting substrate through the first surface and the second surface to obtain a heterostructure to be stripped;
after the ion implantation is performed on the piezoelectric film from the first surface to form a defective layer in the piezoelectric film, the piezoelectric film with the defective layer is obtained, the method further includes:
performing surface treatment on the first surface and the second surface;
the surface treatment comprises a surface roughness treatment, and the method for performing the surface roughness treatment comprises at least one of chemical mechanical polishing, chemical etching and low-energy ion irradiation.
Optionally, the post-annealing time is in the range of 0.5 to 100 hours.
By adopting the technical scheme, the preparation method of the heterogeneous single crystal film has the following beneficial effects:
this application is through carrying out annealing processing after high temperature to the heterogeneous thin film structure after peeling off the transfer, can improve the bonding strength of piezoelectric film and substrate, resume the crystal defect who is introduced by ion implantation, this application sets up the atmosphere of annealing processing into containing piezoelectric film and leads to the component material through to the realization suppresses the outer problem of releasing of lithium element and oxygen element etc. in the piezoelectric film, improved film quality and relevant acoustic filter's use bandwidth, realized high performance heterogeneous single crystal film, the preparation of big bandwidth acoustic filter.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a flow chart of an alternative method for fabricating a heterogeneous single crystal thin film according to the present application;
FIG. 2 is a schematic structural view of an alternative heterogeneous thin film structure of the present application;
FIG. 3 illustrates a method for fabricating a hetero-single crystal thin film according to another alternative embodiment of the present application;
FIG. 4 is a schematic structural view of an alternative support substrate of the present application;
FIG. 5 is a schematic structural diagram of an alternative piezoelectric film having a defective layer according to the present application;
FIG. 6 is a schematic structural view of an alternative piezoelectric film of the present application;
FIG. 7 is a schematic structural view of an alternative heterostructure to be exfoliated according to the present application;
FIG. 8 is a schematic diagram of an alternative acoustic filter according to the present application;
fig. 9 is a test graph of an acoustic filter device prepared based on the heterogeneous thin film structure of the present application and an acoustic filter device of the prior art.
The following is a supplementary description of the drawings:
1-heterogeneous thin film structures; 2-a piezoelectric film; 21-a defect layer; 3-a piezoelectric film having a defective layer; 4-a support substrate; 5-a heterostructure to be stripped; 6-interdigital electrodes.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. It is to be understood that the embodiments described are only a few embodiments of the present application and not all 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 application.
Reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic may be included in at least one implementation of the present application. In the description of the present application, it is to be understood that the terms "upper", "lower", "top", "bottom", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present application and simplifying the description, and do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present application. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. Moreover, the terms "first," "second," and the like are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the application described herein are capable of operation in sequences other than those illustrated or described herein.
For purposes of the following detailed description, it is to be understood that the invention may assume various alternative variations and step sequences, except where expressly specified to the contrary. Moreover, other than in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contains certain errors necessarily resulting from the standard deviation found in their respective testing measurements.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein. For example, a stated range from "1 to 10" should be considered to include any and all subranges between the minimum value of 1 and the maximum value of 10. Exemplary subranges of the range 1 to 10 include, but are not limited to, 1 to 6.1, 3.5 to 7.8, 5.5 to 10, and the like.
Referring to fig. 1, fig. 1 is a flow chart of an alternative method for preparing a heterogeneous single crystal thin film according to the present application. The application discloses a preparation method of a heterogeneous single crystal film for an acoustic filter, which comprises the following steps:
s101: providing a heterogeneous thin film structure 1; the heterogeneous thin film structure 1 comprises a piezoelectric thin film 2, as shown in fig. 2, and fig. 2 is a schematic structural diagram of an alternative heterogeneous thin film structure 1 of the present application.
In an alternative embodiment, referring to FIG. 3, FIG. 3 illustrates a method for fabricating a heterogeneous single crystal thin film in accordance with another alternative embodiment of the present application. Step S101 may be specifically expressed as:
s1011: providing a support substrate 4 and a piezoelectric film 3 with a defect layer, referring to fig. 4-5, fig. 4 is a schematic structural view of an alternative support substrate 4 of the present application; fig. 5 is a schematic structural diagram of an alternative piezoelectric film 3 with a defective layer according to the present application.
In an alternative embodiment, the material of the support substrate 4 comprises at least one or a combination of silicon, silicon oxide, sapphire, diamond, aluminum nitride, gallium nitride, SOI, silicon carbide; the material of the piezoelectric film 2 includes a lithium-containing piezoelectric crystal; alternatively, the material of the piezoelectric film 2 may be one or a combination of lithium niobate, lithium tantalate and lithium borate.
S1012: the piezoelectric thin film 3 with the defective layer and the support substrate 4 are bonded, resulting in a heterostructure 5 to be exfoliated.
In an alternative embodiment, the bonding temperature is in the range of 40-250 degrees Celsius; the pressure range of the bonding is 1e-5Mbar-1000 mbar.
In an alternative embodiment, in step S1012, the method of manufacturing the piezoelectric thin film 3 having the defective layer includes: providing a piezoelectric film 2; the piezoelectric film 2 includes a first surface; performing ion implantation on the piezoelectric film 2 from the first surface to form a defect layer 21 in the piezoelectric film 2, and obtaining the piezoelectric film 3 with the defect layer, as shown in fig. 6, where fig. 6 is a schematic structural diagram of an alternative piezoelectric film 2 of the present application.
In an alternative embodiment, the ion implantation method includes hydrogen ion implantation, helium ion implantation, neon ion implantation, or hydrogen-helium ion co-implantation.
In an optional embodiment, the temperature of the implanted ions is between 50 and 150 ℃; the energy of the ion implantation is 1-2000 kilo electron volts; the ion implantation dose is 1 × 1016～1.5×1017Per square centimeter.
The depth of the ion implantation can be adjusted by adjusting the implantation energy, which is not limited herein.
S1013: and carrying out annealing, peeling and transferring treatment on the heterostructure 5 to be peeled to obtain the heterogeneous thin film structure 1.
In an alternative embodiment, the temperature range for the annealing, lift-off transfer is 100-; the time for annealing, peeling and transferring is 1-100 hours.
In an alternative embodiment, the support substrate 4 comprises a second surface; step S1013 may be specifically expressed as: the piezoelectric film 3 with the defect layer and the supporting substrate 4 are bonded through the first surface and the second surface to obtain a heterostructure 5 to be stripped; fig. 7 is a schematic structural diagram of an alternative heterostructure 5 to be exfoliated according to the present application, as shown in fig. 7.
In an optional embodiment, before step S1013, the preparation method further includes: the first surface and the second surface are subjected to surface treatment. Optionally, the surface treatment includes a surface roughness treatment, and the method of performing the surface roughness treatment includes at least one of chemical mechanical polishing, chemical etching, and low-energy ion irradiation to improve the bonding strength of the first surface and the second surface.
S102: carrying out post-annealing treatment on the heterogeneous thin film structure 1; the post-annealing temperature range is 300-800 ℃; the post-annealing atmosphere contains an element material corresponding to the piezoelectric thin film 2; in an optional embodiment, the material of the piezoelectric film 2 is lithium niobate, and the post-annealing atmosphere contains corresponding piezoelectric film 2 powder, i.e. lithium niobate powder, which has the advantage of high stability of post-annealing treatment, and optionally, the post-annealing time is in the range of 0.5 to 100 hours; the post-annealing temperature range is 300-800 ℃, and lithium niobate powder, namely lithium element and the like, is contained in the post-annealing atmosphere; alternatively, the mass of the lithium niobate powder is 80 to 120 grams, the size of the heterogeneous thin film structure 1 is 4 to 8 inches, and the support substrate 4 comprises a stacked silicon oxide and silicon substrate; the thickness range of the silicon oxide is 500-2000 nm; the thickness range of the silicon substrate is 400-600 nm, and the thickness of the piezoelectric film 2 is 400-600 nm; the mass range of the lithium niobate powder is not related to the thickness of the supporting substrate 4, but is related to the size of the heterogeneous thin film structure 1, i.e., the larger the size is, the more mass of the lithium niobate powder is needed, and the above parameters can be adjusted according to actual needs, and are not limited herein.
In another alternative embodiment, the post-annealing atmosphere contains lithium powder and niobium oxide powder.
Because the specific surface area of the powder sample is larger, the external release of elements is more than that of the thin film material, so that the powder sample can form an environment with more concentrated distribution concentration of elements such as lithium element and oxygen element in the annealing process, and the heterogeneous thin film structure 1 can realize dynamic balance of the external release of elements (such as lithium and oxygen) in the piezoelectric thin film material under the atmosphere of the same component material (lithium niobate powder), namely the external release elements and the elements in the atmosphere have the same diffusion rate into the piezoelectric thin film 2, and the piezoelectric thin film 2 without the problem of the external release of elements is obtained; thereby effectively inhibiting the release of lithium and other elements (such as oxygen) during the high temperature annealing process of the heterogeneous thin film structure 1.
According to the above description, the preparation method of the heterogeneous thin film structure provided by the application can improve the bonding strength, recover the crystal defects introduced by ion implantation, simultaneously completely inhibit the problem of external release of elements such as lithium element and oxygen element in the piezoelectric thin film, improve the quality of the thin film and the use bandwidth of the related acoustic filter, realize the preparation of the high-performance heterogeneous single crystal thin film and the large-bandwidth acoustic filter, and has great significance.
The element material corresponding to the piezoelectric thin film 2 in the post-annealing atmosphere means that the material elements contained in the post-annealing atmosphere correspond to the elements contained in the piezoelectric thin film 2, but the structure of the compound formed by the elements in the atmosphere is not limited to the compound in the piezoelectric thin film 2, as long as the same elements are ensured in both; when the non-piezoelectric film 2 powder is used to form the annealing atmosphere, a proper material powder needs to be selected to avoid the material deposition phenomenon. The post-annealing temperature range and the post-annealing time provided by the application are matched according to the corresponding material of the piezoelectric film 2, for example, when the piezoelectric film 2 selects a piezoelectric crystal film containing lithium, the problem of external release of lithium element and the like can occur when the post-annealing temperature is higher than 150 ℃, however, the post-annealing is generally high-temperature annealing, and in order to achieve the annealing effect, the lithium element can be released from the piezoelectric film 2 containing lithium, and the application of the improved preparation method can effectively inhibit the external release of the lithium element; of course, when the piezoelectric film 2 is other types of crystal films, the corresponding high temperature annealing temperature ranges may be different.
In an alternative embodiment, as shown in fig. 8, fig. 8 is a schematic structural diagram of an alternative acoustic filter according to the present application. And depositing a metal layer on the heterogeneous thin film structure 1 obtained in the above step, and performing patterning treatment on the metal layer to form an interdigital electrode 6 on the heterogeneous thin film structure 1. The filter obtained by the preparation is tested, and another reference filter device is prepared, wherein the difference between the reference filter device and the application lies in that after annealing is carried out, only common atmosphere is adopted for processing, the reference filter device is tested, the test result is shown in figure 9, and figure 9 is a test curve graph of the acoustic filter device prepared based on the heterogeneous thin film structure of the application and the acoustic filter device in the prior art. Wherein, curve a in fig. 9 corresponds to the acoustic filter device prepared based on the heterogeneous thin film structure of the present application, and curve b corresponds to the above-mentioned reference filter device, as can be seen from fig. 9, the bandwidth of the acoustic filter device of the present application at 3 db is 150 MHz; the reference filter device has a bandwidth of 120MHz in 3 dB, and obviously, the acoustic filter device prepared by the preparation method provided by the application has a large broadband, so that the application range of the acoustic filter device is widened.
The above description is only exemplary of the present application and should not be taken as limiting, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A method for preparing a heterogeneous single crystal thin film for an acoustic filter, comprising the steps of:
providing a heterogeneous thin film structure (1); the heterogeneous thin film structure (1) comprises a piezoelectric thin film (2);
carrying out post-annealing treatment on the heterogeneous thin film structure (1); the post-annealing temperature range is 300-800 ℃; the post-annealing atmosphere contains an element material corresponding to the piezoelectric film (2).
2. A method of preparing a hetero-single crystal thin film according to claim 1, wherein the providing a hetero-thin film structure (1) comprises:
providing a support substrate (4) and a piezoelectric film (3) with a defect layer;
bonding the piezoelectric film (3) with the defect layer and the support substrate (4) to obtain a heterostructure (5) to be stripped;
and carrying out annealing and stripping transfer treatment on the heterostructure (5) to be stripped to obtain the heterogeneous thin film structure (1).
3. The method for preparing a hetero-single crystal thin film according to claim 2, wherein the material of the support substrate (4) comprises at least one or a combination of silicon, silicon oxide, sapphire, diamond, aluminum nitride, gallium nitride, SOI, silicon carbide;
the material of the piezoelectric film (2) comprises lithium-containing piezoelectric crystals.
4. The method of claim 2, wherein the bonding temperature is in the range of 40-250 degrees celsius;
the pressure range of the bonding is 1e-5Mbar-1000 mbar.
5. The method as claimed in claim 2, wherein the temperature range of the annealing, peeling and transferring is 100-300 ℃;
the time for annealing, stripping and transferring is 1-100 hours.
6. The method for preparing a hetero-single crystal thin film according to claim 2, wherein the method for preparing the piezoelectric thin film (3) having a defective layer comprises:
providing a piezoelectric film (2); the piezoelectric film (2) comprises a first surface;
and performing ion implantation on the piezoelectric film (2) from the first surface to form a defect layer (21) in the piezoelectric film (2), thereby obtaining the piezoelectric film (3) with the defect layer.
7. The method of claim 6, wherein the ion implantation comprises hydrogen ion implantation, helium ion implantation, neon ion implantation or hydrogen-helium ion co-implantation.
8. The method for preparing a hetero-single crystal thin film according to claim 7, wherein the temperature of the implanted ions is 50 to 150 ℃;
the energy of the ion implantation is 1-2000 kilo electron volts;
the dosage of the ion implantation is 1 x 1016～1.5×1017Per square centimeter.
9. A method of preparing a hetero-single crystal thin film according to claim 6, wherein the support substrate (4) comprises a second surface;
bonding the piezoelectric film (3) with the defect layer and the support substrate (4) to obtain a heterostructure (5) to be stripped, comprising:
the piezoelectric film (3) with the defect layer and the supporting substrate (4) are bonded through the first surface and the second surface to obtain a heterostructure (5) to be stripped;
after the ion implantation is performed on the piezoelectric thin film (2) from the first surface to form a defect layer (21) in the piezoelectric thin film (2), and the piezoelectric thin film (3) with the defect layer is obtained, the method further comprises the following steps:
performing surface treatment on the first surface and the second surface;
the surface treatment comprises a surface roughness treatment, and the method for performing the surface roughness treatment comprises at least one of chemical mechanical polishing, chemical etching and low-energy ion irradiation.
10. A method of preparing a hetero-single crystal thin film according to claim 1, wherein the time of the post-annealing is in the range of 0.5 to 100 hours;
the temperature range of the post annealing is 300-800 ℃.
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