CN114122250A - Blackened single crystal piezoelectric composite film and preparation method thereof - Google Patents
Blackened single crystal piezoelectric composite film and preparation method thereof Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 17
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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
- 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
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/08—Shaping or machining of piezoelectric or electrostrictive bodies
- H10N30/085—Shaping or machining of piezoelectric or electrostrictive bodies by machining
- H10N30/086—Shaping or machining of piezoelectric or electrostrictive bodies by machining by polishing or grinding
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/853—Ceramic compositions
- H10N30/8542—Alkali metal based oxides, e.g. lithium, sodium or potassium niobates
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Ceramic Engineering (AREA)
- Surface Acoustic Wave Elements And Circuit Networks Thereof (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The application discloses a blackened single crystal piezoelectric composite film and a preparation method thereof, wherein the preparation method comprises the following steps: implanting ions into the first wafer through an ion implantation method, and bonding the first wafer and the substrate to obtain a bonded body; carrying out heat treatment on the bonding body to obtain a single crystal piezoelectric composite film; laying a second wafer or reduction paper on the film layer of the single crystal piezoelectric composite film to obtain a prefabricated body; burying the pre-prepared body in the blackening powder; carrying out blackening reduction heat treatment on the single crystal piezoelectric composite film buried in the blackening powder in a reducing furnace; and removing the second wafer or the reduction paper to obtain the blackened monocrystal piezoelectric composite film. According to the preparation method, the blackened single crystal piezoelectric composite film subjected to heat treatment is subjected to blackening reduction heat treatment, so that the blackened thin film layer in the finally prepared blackened single crystal piezoelectric composite film has a low pyroelectric coefficient and resistivity.
Description
Technical Field
The application belongs to the technical field of semiconductor preparation, and particularly relates to a blackened single crystal piezoelectric composite film and a preparation method thereof.
Background
Lithium niobate and lithium tantalate crystals have been widely used in various core electronic devices such as surface acoustic wave devices, film bulk acoustic resonators, and photoelectric sensors due to their excellent optical properties such as piezoelectricity, ferroelectricity, photoelectricity, photoelastic, pyroelectric, photorefractive, and nonlinearity.
Because the lithium niobate and lithium tantalate crystals are ferroelectric crystals, the pyroelectric coefficient and the resistivity of the lithium niobate and lithium tantalate crystals are higher. Therefore, when the lithium niobate and lithium tantalate wafers are used for preparing electronic components, a large amount of static charges are easily accumulated on the surfaces of the lithium niobate and lithium tantalate wafers, and the lithium niobate and lithium tantalate wafers are damaged by the release of the static charges, so that the service performance and the yield of the prepared electronic components are influenced.
In order to solve the problems, in one implementation mode, blackening treatment is performed on lithium niobate and lithium tantalate wafers in advance, wherein the blackening treatment refers to treatment of the lithium niobate and lithium tantalate wafers through a high-temperature chemical reduction method and the like so as to reduce the pyroelectric effect and the resistivity of the lithium niobate and lithium tantalate wafers, and the lithium niobate and lithium tantalate wafers after the blackening treatment can be changed into black brown from a colorless transparent state; furthermore, the electronic component is prepared by adopting the lithium niobate and lithium tantalate wafers after blackening treatment, so that the problem that the lithium niobate or lithium tantalate wafers are damaged due to the release of static charges can be solved.
However, the applicant found that, in the case of an electronic component using a piezoelectric composite thin film, although a previously blackened lithium niobate or lithium tantalate wafer is used, when the piezoelectric composite thin film obtained is applied to an electronic component, the electronic component is damaged by the discharge of electrostatic charges.
Disclosure of Invention
In order to solve the technical problems in the prior art, the application provides a blackened single crystal piezoelectric composite film and a preparation method thereof.
In a first aspect, the present application provides a method for preparing a blackened single-crystal piezoelectric composite film, comprising: .
Preparing a first wafer and a substrate base plate, wherein the first wafer is a lithium niobate wafer or a lithium tantalate wafer;
implanting ions into the first wafer through an ion implantation method, and sequentially dividing the first wafer into a residual layer, a separation layer and a thin film layer;
bonding the first wafer and the substrate base plate to obtain a bonded body;
carrying out heat treatment on the bonding body, and separating the residual layer from the thin film layer to obtain a single crystal piezoelectric composite film;
laying a second wafer or reduction paper on the film layer of the single crystal piezoelectric composite film to obtain a prefabricated body;
burying the pre-prepared body in blackening powder, wherein the blackening powder comprises reducing powder and lithium carbonate powder;
carrying out blackening reduction heat treatment on the single crystal piezoelectric composite film buried in the blackening powder in a reducing furnace;
and removing the second wafer or the reduction paper to obtain the blackened monocrystal piezoelectric composite film.
In one implementation, the second wafer is the same material as the first wafer.
In one implementation mode, the blackening powder comprises 1-10 parts of reducing powder and 90-99 parts of lithium carbonate powder by mass.
In one implementation mode, the blackening powder comprises 5-10 parts of reducing powder and 90-95 parts of lithium carbonate powder by mass.
In one implementation, the reducing powder includes any one or more of iron powder, aluminum powder, zinc powder, magnesium powder, silicon powder, and carbon powder.
In one implementation manner, the reducing powder includes a mixed powder of any one or more of iron powder, aluminum powder, zinc powder, magnesium powder, silicon powder and carbon powder and graphene.
In one implementation mode, the temperature of the blackening reduction heat treatment of the single crystal piezoelectric composite film buried in the blackening powder is 300-600 ℃ in a reduction furnace, and the heat preservation time is 1-100 hours.
In one implementation, the ions implanted into the first wafer by the ion implantation method are helium ions, hydrogen ions, nitrogen ions, oxygen ions or argon ions, and the implantation dose is 2 × 1016ions/cm2-4×1016ions/cm2(ii) a The implantation energy is 40-400 keV.
In one implementation, the preparation method further comprises: and polishing and cleaning the surface of the film layer in the blackened monocrystal piezoelectric composite film.
In one implementation, the substrate base plate is a single-layer substrate or a composite substrate.
In a second aspect, the present application provides a blackened single-crystal piezoelectric composite film, which is prepared by any one of the preparation methods of the blackened single-crystal piezoelectric composite film of the first aspect.
In a third aspect, the present application also provides an electronic component including the blackened single crystal piezoelectric composite film of the second aspect.
According to the blackened single-crystal piezoelectric composite film and the preparation method thereof, the blackened and reduced heat treatment is carried out on the single-crystal piezoelectric composite film after the heat treatment, so that the film layer prepared by the blackened and reduced first wafer can be subjected to blackened and reduced heat treatment and repair; for the thin film layer prepared by the first wafer which is not subjected to blackening reduction, the whitening of the thin film layer can be inhibited, so that the blackened thin film layer in the finally prepared blackened single crystal piezoelectric composite film has lower pyroelectric coefficient and resistivity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
Fig. 1 is a flowchart of a method for preparing a blackened single-crystal piezoelectric composite film according to an embodiment of the present disclosure.
Description of the reference numerals
100-first wafer, 110-residual layer, 120-separation layer, 130-thin film layer, 130A-blackened thin film layer, 200-substrate base plate, 300-bonding body, 400-second wafer, and 500-blackened powder.
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, and it is obvious that the described embodiments are only a part of the embodiments of the present application, 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 application.
As described in the background section, in order to solve the technical problem that a large amount of static charges are easily accumulated on the surfaces of lithium niobate and lithium tantalate wafers and the lithium niobate and lithium tantalate wafers are damaged by releasing the static charges, the lithium niobate and lithium tantalate wafers are usually subjected to blackening treatment in advance, and then the blackened lithium niobate and lithium tantalate wafers are used for preparing the piezoelectric composite film.
However, the applicant found that when the piezoelectric composite thin film is applied to an electronic component, the electronic component is still damaged by the discharge of static charge. Based on this, the applicant further studies and analyses to find that: in the process of preparing the piezoelectric composite film, after the lithium niobate or lithium tantalate film layer is separated from the residual layer, the bonded body of the film layer and the substrate wafer is annealed at high temperature so as to further enhance the bonding force and eliminate the lattice defects formed in the film layer in the ion implantation process, however, the applicant finds that the film layer which is supposed to be dark brown has the phenomenon of partial or complete whitening in the high-temperature annealing process, that is, the originally blackened film layer in the finally prepared composite film material recovers the characteristics of higher pyroelectric coefficient and resistivity, thereby influencing the service performance of electronic components applied by the composite film material.
Based on the above analysis, the embodiment of the application provides a method for preparing a blackened single-crystal piezoelectric composite film, which can solve the technical problem that the piezoelectric composite film prepared from the blackened lithium niobate or lithium tantalate wafer still has the phenomenon that electrostatic charges are released to damage electronic components.
The following is a detailed description of a method for preparing a blackened single crystal piezoelectric composite film provided in the embodiments of the present application.
As shown in fig. 1, a method for preparing a blackened single-crystal piezoelectric composite film according to an embodiment of the present application includes the following steps:
The first wafer 100 in the embodiment of the present application refers to a base material having a certain thickness for preparing a thin film layer. The first wafer may be a wafer that is not blackened, or a wafer that is blackened, which is not limited in this application. If the first wafer is a blackened wafer, the first wafer 100 can be obtained by direct purchase; alternatively, the first wafer 100 may be a lithium niobate wafer which is directly purchased and is not subjected to blackening treatment or a lithium tantalate wafer which is not subjected to blackening treatment, wherein any currently available blackening treatment method may be adopted as the blackening treatment method for the lithium niobate wafer or the lithium tantalate wafer, and the blackening treatment method is not limited in the present application.
In the embodiment of the present application, the substrate base 200 may be a single-layer substrate or a composite substrate, that is, the substrate base 200 includes at least one substrate layer. The material of each substrate layer may be the same or different, and the present application does not limit this. For example: the substrate layer material may be lithium niobate, lithium tantalate, quartz, silicon, sapphire, SOI, diamond, silicon carbide, silicon nitride, gallium arsenide, indium phosphide, or the like, which is not limited in this application.
The ion implantation method in the embodiments of the present application is not particularly limited, and any ion implantation method in the prior art may be used, and the implanted ions may be ions that can generate gas by heat treatment, for example: the implanted ions may be hydrogen ions, helium ions, nitrogen ions, oxygen ions, or argon ions. When implanting ions, the implantation dose can be 2 × 1016ions/cm2～4×1016ions/cm2The implantation energy may be 40KeV to 400KeV, for example, 50 KeV.
In the embodiment of the present application, the thickness of the thin film layer 130 may 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 130; conversely, the smaller the depth of ion implantation, the smaller the thickness of the thin film layer 130 is produced.
After bonding, the thin film layer 130 of the first wafer 100 is in contact with the substrate 200 and stacked on the substrate 200, such that the bonded body 300 has the remainder layer 110, the separation layer 120, the thin film layer 130, and the substrate 200 stacked in this order from top to bottom.
The bonding method is not particularly limited in the present application, and any bonding method in the prior art, for example, surface activation bonding, may be used to obtain a bonded body. The surface activation method is not limited in the present application, and for example, plasma activation or chemical solution activation may be used.
It should be noted that, the present application may further include a step of preparing an isolation layer on the substrate base 200 before step 300, for example, the substrate base 200 is a single-layer silicon substrate, silicon oxide may be prepared on the single-layer silicon substrate by a thermal oxidation method, and the generated silicon oxide layer serves as the isolation layer. In this way, in step 300, the first wafer 100 is bonded to the substrate 200 having the isolation layer, so as to obtain a bonded body.
It should be noted that the isolation layer prepared on the base substrate 200 may be a single layer or a plurality of layers, which is not limited in this application. For example, silicon oxide layers and silicon nitride layers are alternately stacked on the substrate base plate 200.
And (3) carrying out heat treatment on the bonded body 300, wherein the heat treatment process can be carried out at the temperature of 180-280 ℃ for 1-100 hours, bubbles are formed in the separation layer 120 in the heat treatment process, for example, H ions form hydrogen, He ions form helium and the like, the bubbles in the separation layer 120 are connected into one piece along with the progress of the heat treatment, finally, the separation layer 120 is cracked, and the residual layer 110 is separated from the thin film layer 130, so that the residual layer 110 is stripped from the bonded body 300, and the single crystal piezoelectric composite film is obtained, wherein the thin film layer 130 and the substrate 200 are sequentially laminated from top to bottom.
When the first wafer is a blackened lithium niobate wafer or lithium tantalate wafer, the applicant found that the thin film layer 130, which should be brown in color, in the single crystal piezoelectric composite thin film is partially or entirely whitened after the above step 400, and thus found that the originally blackened thin film layer 130 is partially or entirely oxidized after the heat treatment of the bonded body, and the following steps 500 to 800 are performed in order to change this phenomenon.
It should be noted that, when the first wafer is a lithium niobate wafer or a lithium tantalate wafer that has not been subjected to blackening treatment, the following steps 500 to 800 are also performed to blacken the thin film layer 130, so that it is possible to ensure that the thin film layer 130 in the finally prepared blackened single crystal piezoelectric composite film is completely blackened.
First, although the material of the second wafer 400 is not limited in the present application, the second wafer 400 is preferably made of the same material as the first wafer 100 in order to avoid introducing other unnecessary impurities into the thin film layer 130.
The second wafer 400 and the reduction paper can remove static electricity, and can isolate the thin film layer 130 from the blackening powder, so that particle impurities cannot be attached to the surface of the thin film layer 130 when the prefabricated body is buried in the blackening powder, and the cleanness of the thin film layer 130 can be guaranteed.
In addition, the reduction paper may also serve as a source of the reducing material with respect to the second wafer 400, and the reduction paper may be a tin foil paper.
Step 600, burying the pre-prepared body in the blackening powder 500, wherein the blackening powder 500 comprises reducing powder and lithium carbonate powder.
And 700, carrying out blackening reduction heat treatment on the monocrystalline piezoelectric composite film buried in the blackening powder in a reduction furnace.
And 800, removing the second wafer or the reduction paper to obtain the blackened monocrystal piezoelectric composite film.
After the blackened single-crystal piezoelectric composite film is prepared, the embodiment may further include polishing and cleaning the surface of the film layer in the blackened single-crystal piezoelectric composite film, so that the surface roughness of the blackened single-crystal piezoelectric composite film meets the requirement.
In the present application, the blackened powder 500 reacts in the reducing furnace to generate reducing gas carbon monoxide, and then the carbon monoxide performs a blackened reducing heat treatment on the thin film layer in the preform, thereby repairing the blackened thin film layer or suppressing the whitening of the thin film layer. Specifically, the reducing gas carbon monoxide can react with oxygen in the thin film layer to increase the concentration of oxygen vacancies in the thin film layer, thereby reducing the resistivity, and repairing the blackening or suppressing the whitening of the thin film layer.
In addition, if the blackening powder 500 is directly contacted with the surface of the thin film layer in the pre-fabricated body to perform the blackening-reduction heat treatment, the blackening powder 500 damages the thin film layer, and further, after the blackening reduction is completed, the thickness of the surface of the thin film layer from several um to several tens um needs to be removed by polishing to remove the damaged layer on the surface of the thin film layer, which is unacceptable for the thin film. Therefore, in contrast to the method of performing the blackening-reducing heat treatment by directly contacting the blackening powder 500 with the surface of the thin film layer in the preform, the present application can prevent the surface of the thin film layer after the blackening-reduction from being damaged by laying the second wafer 400 or the base paper on the thin film layer in the preform.
In the present invention, although the second wafer or the reduction paper is laid on the thin film layer of the single crystal piezoelectric composite film, carbon monoxide, which is a reducing gas generated in the reduction furnace, can diffuse to the surface of the thin film layer of the single crystal piezoelectric composite film to react with the thin film layer, and the blackened powder does not contact the surface of the thin film layer of the single crystal piezoelectric composite film.
The material of the reducing powder in the blackened powder 500 is not limited, and examples thereof include: the reducing powder can be any one or a mixture of iron powder, aluminum powder, zinc powder, magnesium powder, silicon powder and carbon powder. Wherein, the carbon powder can be all powders containing carbon elements, such as diamond, C60, C70, graphite powder, activated carbon, carbon black, charcoal and the like; the silicon powder can be elemental silicon powder. For another example, the reducing powder may be a mixed powder of graphene and any one or more of iron powder, aluminum powder, zinc powder, magnesium powder, silicon powder, and carbon powder, so that the graphene in the mixed powder can greatly enhance the reducing property of the reducing powder.
Before use, the reducing powder in the blackening powder 500 and the lithium carbonate powder are weighed according to a preset proportion, mechanically ground, and uniformly mixed to serve as a composite reducing agent to perform a blackening reduction reaction on the single crystal piezoelectric composite film, wherein the lithium carbonate powder can also play a role in improving the uniformity of reduction.
The blackening reduction heat treatment process for the single crystal piezoelectric composite film can be heat preservation at the temperature of 300-600 ℃ for 1-100 hours, and more preferably can be heat preservation at the temperature of 500-600 ℃ for 2-4 hours to complete the blackening reduction of the film layer. The blackened single crystal piezoelectric composite film includes a blackened thin film layer 130A and a base substrate 200.
In conclusion, the blacking reduction heat treatment is carried out on the single crystal piezoelectric composite film after the heat treatment, so that the blacking reduction heat treatment and repair can be carried out on the film layer prepared by the blacking reduction first wafer; for the thin film layer prepared by the first wafer which is not subjected to blackening reduction, the whitening of the thin film layer can be inhibited, so that the blackened thin film layer in the finally prepared blackened single crystal piezoelectric composite film has lower pyroelectric coefficient and resistivity. In addition, the second wafer 400 or the base paper is laid on the thin film layer in the preform, and the surface of the thin film layer after blackening and reduction can be prevented from being damaged.
The applicant found that the ratio of the reducing powder to the lithium carbonate powder in the blackened powder has a certain effect on the blackening-reducing effect of the thin film layer in the preform. According to research and comparison, the blackening powder is prepared according to the following proportion, and the blackening single crystal piezoelectric composite film prepared according to the proportion is optimal in blackening reduction effect, wherein the proportion comprises 5-10 parts of reducing powder and 90-95 parts of lithium carbonate powder in parts by weight. When the addition amount of the reducing powder is less than 5 parts, it is not enough to completely blacken the thin film layer; when the addition amount of the reducing powder is more than 10 parts, the carbon monoxide is wasted because the rate of the generated carbon monoxide is too high and part of the carbon monoxide does not reach the reduction and blackening film layer; when the blackening powder comprises 5-10 parts of reducing powder and 90-95 parts of lithium carbonate powder, the thin film layer can be completely blackened, and no redundant carbon monoxide is wasted.
The effect of the blackened single crystal piezoelectric composite film prepared by burying the pre-preparation body with the blackened powder and performing the blackening reduction heat treatment is explained by experimental data.
Experimental example 1
The blackening monocrystal piezoelectric composite film is prepared by the method provided by the embodiment of the application, wherein the first wafer is a lithium tantalate wafer with the thickness of 0.25mm, and the substrate base plate is a silicon wafer with the thickness of 0.25 mm; the method comprises the following steps of paving base paper (namely aluminum foil paper) on a film layer of a single crystal piezoelectric composite film, wherein blackening powder comprises iron powder and lithium carbonate powder, and the mass ratio of the iron powder to the lithium carbonate powder is 5: 95; in a reducing furnace, the temperature of blackening reduction heat treatment of the single crystal piezoelectric composite film buried in the blackening powder is 530 ℃, and the heat preservation time is 4 hours.
Experimental example two
The second experimental example is substantially the same as the first experimental example except that the mass ratio of the iron powder to the lithium carbonate powder is 10:90 in the second experimental example.
Experimental example III
The third experimental example is substantially the same as the first experimental example, except that the mass ratio of the iron powder to the lithium carbonate powder is 1:99 in the third experimental example.
Experimental example four
The fourth experimental example is substantially the same as the first experimental example, except that in the fourth experimental example, a lithium tantalate wafer is laid on the thin film layer of the single crystal piezoelectric composite film, and the blackening powder is iron powder and lithium carbonate powder, wherein the mass ratio of the iron powder to the lithium carbonate powder is 5: 95.
Experimental example five
Experimental example five is substantially the same as experimental example four described above, except that in experimental example five, the mass ratio of the iron powder to the lithium carbonate powder is 10: 90.
Experimental example six
Experimental example six is substantially the same as experimental example four described above, except that in experimental example six, the mass ratio of the iron powder to the lithium carbonate powder is 1: 99.
Experimental example seven
The method provided by the embodiment of the application is adopted to prepare the blackened single crystal piezoelectric composite film, wherein the first wafer is a lithium niobate wafer with the thickness of 0.25mm, and the substrate base plate is a silicon wafer with the thickness of 0.25 mm; laying a lithium niobate wafer on a film layer of the single crystal piezoelectric composite film, wherein the blackening powder is iron powder and lithium carbonate powder, and the mass ratio of the iron powder to the lithium carbonate powder is 5: 95; in a reducing furnace, the temperature of blackening reduction heat treatment of the single crystal piezoelectric composite film buried in the blackening powder is 530 ℃, and the heat preservation time is 4 hours.
Experimental example eight
Experimental example eight is substantially the same as experimental example seven described above, except that in experimental example eight, the mass ratio of the iron powder to the lithium carbonate powder is 10: 90.
Experimental example nine
Experimental example nine is substantially the same as experimental example seven above, except that in experimental example nine, the mass ratio of the iron powder to the lithium carbonate powder is 1: 99.
Comparative example 1
Comparative example one is substantially the same as experimental example one except that the prepared preform was directly placed in a reducing furnace and carbon monoxide gas was introduced to perform a blackening-reduction heat treatment, wherein the preform was neither laid down nor buried in the blackening powder.
Comparative example No. two
Comparative example two is substantially the same as experimental example one except that the comparative example two directly places a preform laid with a base paper in a reducing furnace and introduces carbon monoxide gas to perform a blackening-reduction heat treatment, wherein the preform is not buried in blackening powder.
Comparative example No. three
The third comparative example is substantially the same as the fourth experimental example except that the third comparative example directly places the preform on which the lithium tantalate wafer is laid in the reduction furnace, and introduces carbon monoxide gas to perform the blackening-reduction heat treatment, wherein the preform is not buried in the blackening powder.
Comparative example No. four
Comparative example four is substantially the same as experimental example seven except that in comparative example four, a preform on which a lithium niobate wafer is laid is directly placed in a reducing furnace, and carbon monoxide gas is introduced to perform a blackening-reduction heat treatment, wherein the preform is not buried in blackening powder.
The performance of the blackened single crystal piezoelectric composite film prepared in the experimental examples and the comparative examples was tested, wherein the performance of the blackened single crystal piezoelectric composite film was observed, and the appearance color of the film layer in the blackened single crystal piezoelectric composite film was observed, and the resistivity of the film layer in the blackened single crystal piezoelectric composite film was observed, which is specifically shown in table 1 below.
TABLE 1 comparison of the properties of the blackened single crystal piezoelectric composite films prepared in the Experimental examples and the comparative examples
The application also provides a blackened single-crystal piezoelectric composite film which is obtained by adopting the preparation method provided by the embodiment.
In one implementation, the application provides a blackened single-crystal piezoelectric composite film, which comprises a blackened thin film layer and a substrate base plate which are sequentially stacked, wherein the substrate base plate can be a single-layer substrate or a composite substrate.
In yet another implementation, the present application provides a blackened single crystal piezoelectric composite film, which may further include one or more isolation layers between the blackened film layer and the base substrate.
The application also provides an electronic component, and the electronic component adopts the blackening single crystal piezoelectric composite film provided by the embodiment of the application. The thin film layer in the blackened single crystal piezoelectric composite film provided by the embodiment of the application can be repaired through blackening reduction heat treatment, and the pyroelectric effect of the single crystal piezoelectric composite film can be effectively reduced, so that the use performance of electronic components cannot be influenced during use.
The preparation method provided by the present application is illustrated below by specific examples.
Example one
The preparation method of the blackened single-crystal piezoelectric composite film comprises the following steps:
1. preparing a 200-micron silicon wafer and a 200-micron lithium tantalate wafer, respectively fixing the silicon wafer or 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; the lithium tantalate wafer is subjected to blackening treatment.
2. Subjecting the lithium tantalate crystal treated in the step 1 to treatmentImplanting He into circle by stripping ion implantation+Separating the lithium tantalate wafer into a residual layer, a separation layer and a thin film layer in this order from the implantation surface, and implanting He+Distributed on the separation layer to obtain the single crystal lithium tantalate wafer implanted 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 (3) manufacturing a silicon dioxide layer on the cleaned silicon wafer by an LPCVD (low pressure chemical vapor deposition) method, then carrying out chemical mechanical polishing until the thickness is 100nm to obtain a smooth surface, and carrying out RCA (Rolling circle and circle) cleaning to obtain a clean surface.
4. And (3) contacting the thin film layer of the single-crystal lithium tantalate wafer injection piece with the silicon dioxide layer, and bonding by adopting a direct bonding method to obtain a bonded body.
5. And (3) putting the bonding body into an annealing furnace in a nitrogen atmosphere, preserving the heat for 2 hours at 180 ℃, and separating the bonding body at the separation layer to obtain the single crystal piezoelectric composite film.
6. Laying aluminum foil paper on the thin film layer of the single crystal piezoelectric composite film obtained after the treatment in the step 5, and burying the single crystal piezoelectric composite film with the laid aluminum foil paper in blackening powder (composite powder of aluminum powder and lithium carbonate), wherein the aluminum powder comprises the following components in percentage by mass: lithium carbonate powder 5: 95.
7. and (3) preserving the heat of the monocrystalline piezoelectric composite film buried in the blackening powder for 4 hours in a reduction furnace at 500 ℃ under the nitrogen atmosphere to carry out blackening reduction reaction, taking out the blackening powder after the blackening reduction reaction is finished, and removing the laid aluminum foil paper to obtain the blackening monocrystalline piezoelectric composite film.
8. Fixing the blackened single crystal piezoelectric composite film on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment on the film layer until reducing ions on the surface of the film layer are removed, and then carrying out RCA cleaning to obtain a clean surface.
The blackened monocrystal piezoelectric composite film sequentially comprises a blackened film layer, a silicon dioxide layer and a monocrystal silicon layer, wherein the film layer is made of monocrystal lithium tantalate.
Example two
The second embodiment provides a preparation method of a blackened single-crystal piezoelectric composite film, which comprises the following steps:
1. preparing a 500-micron silicon carbide wafer and a 500-micron lithium tantalate wafer, respectively fixing the silicon carbide wafer or the lithium tantalate wafer on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing to obtain a smooth surface, and then carrying out semiconductor RCA cleaning on the two wafers to obtain a clean surface, wherein the lithium tantalate wafer is a blackened lithium tantalate wafer.
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 layer, a separation layer and a thin film layer from an injection surface, and the injected nitrogen ions are distributed in the separation layer to obtain a single crystal lithium tantalate 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 50 keV.
3. An amorphous silicon layer with the thickness of 10 mu m is manufactured on the cleaned silicon carbide wafer by a PVD method;
4. and (2) manufacturing a silicon dioxide layer on the amorphous silicon layer by using a PVD method, then carrying out chemical mechanical polishing to obtain a smooth surface with the thickness of 10 mu m, and carrying out RCA cleaning to obtain a clean surface.
5. And (3) contacting the single-crystal lithium tantalate wafer injection sheet with the silicon dioxide layer, and bonding by adopting a direct bonding method to obtain a bonded body.
6. And putting the bonding body into an annealing furnace in a hydrogen atmosphere, preserving the heat at 280 ℃ for 4 hours, and separating the bonding body at a separation layer to obtain the single crystal piezoelectric composite film.
7. Laying a layer of lithium niobate single crystal wafer on the film of the single crystal piezoelectric composite film obtained after the treatment in the step 6, and burying the single crystal piezoelectric composite film obtained by laying the lithium niobate single crystal wafer in blackening powder (composite powder of iron powder and lithium carbonate), wherein the iron powder comprises the following components in percentage by mass: lithium carbonate powder ═ 8: 92.
8. and (3) preserving the temperature of the monocrystalline piezoelectric composite film buried in the blackened powder for 4 hours in a reducing furnace at 550 ℃ under hydrogen atmosphere to carry out blackening reduction reaction, taking out the blackened powder after the blackening reduction is finished, and removing the laid lithium niobate monocrystalline wafer to obtain the blackened monocrystalline piezoelectric composite film.
9. Fixing the blackened single crystal piezoelectric composite film on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment on the film layer until reducing ions on the surface of the film layer are removed, and then carrying out RCA cleaning to obtain a clean surface.
The blackened single-crystal piezoelectric composite film sequentially comprises a blackened film layer, a silicon dioxide layer, a polycrystalline silicon layer and a silicon carbide layer, wherein the film layer is made of single-crystal lithium tantalate.
Example three
The third embodiment provides a preparation method of a blackened single-crystal piezoelectric composite film, which comprises the following steps:
1. preparing a 200-micron silicon nitride wafer and a 250-micron 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, wherein the lithium niobate wafer is the lithium niobate wafer after blackening treatment.
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 layer, a separation layer and a thin film layer from an implantation surface, and the implanted oxygen ions are distributed in the separation layer to obtain a single crystal lithium niobate wafer implantation piece.
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 400 keV.
3. And (3) manufacturing a polycrystalline silicon layer on the cleaned silicon nitride wafer by using a PECVD method, wherein the thickness of the polycrystalline silicon layer is 1 mu m.
4. And (3) manufacturing a silicon dioxide layer on the polycrystalline silicon 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 contacting the single-crystal lithium niobate wafer injection sheet with the silicon dioxide layer, and bonding by adopting a direct bonding method to obtain a bonded body.
6. And (3) putting the bonding body into an annealing furnace in an argon atmosphere, preserving the heat for 2 hours at 200 ℃, and separating the bonding body at the separation layer to obtain the single crystal piezoelectric composite film.
7. Laying aluminum foil paper on the thin film layer of the single crystal piezoelectric composite film obtained after the treatment in the step 6, and burying the single crystal piezoelectric composite film with the laid aluminum foil paper in blackening powder (composite powder of zinc powder and lithium carbonate), wherein the zinc powder comprises the following components in percentage by mass: lithium carbonate powder 10: 90.
8. and (3) preserving the temperature of the monocrystalline piezoelectric composite film buried in the blackening powder for 100 hours in a reduction furnace at 300 ℃ under the argon atmosphere to carry out blackening reduction reaction, taking out the blackening powder after the blackening reduction reaction is finished, and removing the laid aluminum foil paper to obtain the blackening monocrystalline piezoelectric composite film.
9. Fixing the blackened single crystal piezoelectric composite film on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment on the film layer until reducing ions on the surface of the film layer are removed, and then carrying out RCA cleaning to obtain a clean surface.
The blackened monocrystal piezoelectric composite film sequentially comprises a blackened film layer, a silicon dioxide layer, a polycrystalline silicon layer and a silicon nitride layer, wherein the film layer is made of monocrystal lithium niobate.
Example four
Example four provides a method for preparing a blackened single crystal piezoelectric composite film, comprising the steps of:
1. preparing a 300-micron silicon wafer and a 400-micron lithium tantalate wafer, respectively fixing the silicon wafer or the lithium tantalate wafer on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing to obtain a smooth surface, and then carrying out semiconductor RCA cleaning on the two wafers to obtain a clean surface, wherein the lithium tantalate wafer is a blackened lithium tantalate wafer.
2. And (3) implanting argon 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 layer, a separation layer and a thin film layer from an implantation surface, and the implanted argon ions are distributed in the separation layer to obtain a single crystal lithium tantalate wafer implantation piece.
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 was 225 keV.
3. An amorphous silicon layer was formed on the cleaned silicon wafer by a PVD method, and the thickness of the amorphous silicon layer was 500 nm.
4. And (2) manufacturing a silicon dioxide layer on the amorphous silicon 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 single-crystal lithium tantalate wafer injection sheet with the silicon dioxide layer, and bonding by adopting a direct bonding method to obtain a bonded body.
6. And (3) putting the bonding body into an annealing furnace in a helium atmosphere, preserving the heat for 3 hours at 220 ℃, and separating the bonding body at the separation layer to obtain the single crystal piezoelectric composite film.
7. Laying a layer of lithium tantalate single crystal wafer on the single crystal piezoelectric composite film obtained after the treatment in the step 6, and burying the single crystal piezoelectric composite film on which the lithium tantalate single crystal wafer is laid in blackening powder (composite powder of magnesium powder and lithium carbonate), wherein the magnesium powder comprises the following components in percentage by mass: lithium carbonate powder ═ 1: 99.
8. and (3) preserving the heat of the monocrystalline piezoelectric composite film buried in the blackening powder for 1h in a reduction furnace at 600 ℃ under the atmosphere of helium, carrying out blackening reduction reaction, taking out the blackening powder after the blackening reduction reaction is finished, and removing the laid lithium tantalate monocrystalline wafer to obtain the blackening monocrystalline piezoelectric composite film.
9. Fixing the blackened single crystal piezoelectric composite film on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment on the film layer until reducing ions on the surface of the film layer are removed, and then carrying out RCA cleaning to obtain a clean surface.
The blackened monocrystal piezoelectric composite film sequentially comprises a blackened film layer, a silicon dioxide layer, a polycrystalline silicon layer and a monocrystal silicon layer, wherein the film layer is made of monocrystal lithium tantalate.
Example five
Example five provides a method for preparing a blackened single crystal piezoelectric composite film, comprising the steps of:
1. preparing a 410 mu m silicon carbide wafer and a 300 mu m lithium niobate wafer, respectively fixing the silicon carbide 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, wherein the lithium niobate wafer is the lithium niobate wafer after blackening treatment.
2. Injecting He into the lithium niobate wafer processed in the step 1 by adopting a stripping ion injection method+The lithium niobate wafer is divided into a residual layer, a separation layer and a thin film layer in this order from the implantation surface, and He is implanted+And distributing ions in the separation layer to obtain the single crystal lithium niobate wafer implantation piece.
Implanting He by lift-off ion implantation+The implantation dose parameters were: the implantation dose is 3 × 1016ions/cm2The implantation energy is 35 keV.
3. Argon ions were implanted into the cleaned silicon carbide wafer by ion implantation to form a damaged layer of single crystal silicon, which was 5 μm thick as a dielectric layer.
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 single-crystal lithium niobate wafer injection sheet with the silicon dioxide layer, and bonding by adopting a direct bonding method to obtain a bonded body.
6. And (3) putting the bonding body into an annealing furnace in a nitrogen atmosphere, preserving the heat for 2 hours at 240 ℃, and separating the bonding body at the separation layer to obtain the single crystal piezoelectric composite film.
7. Laying a layer of lithium niobate single crystal wafer on the thin film layer of the single crystal piezoelectric composite film obtained after the treatment in the step 6, and burying the single crystal piezoelectric composite film on which the lithium niobate single crystal wafer is laid in blackening powder (composite powder of iron powder, aluminum powder and lithium carbonate), wherein the iron powder comprises the following components in percentage by mass: aluminum powder: lithium carbonate powder 5: 5: 90.
8. and (3) preserving the temperature of the monocrystalline piezoelectric composite film buried in the blackening powder for 3 hours in a reduction furnace at 550 ℃ under the nitrogen atmosphere to carry out blackening reduction reaction, taking out the blackening powder after the blackening reduction reaction is finished, and removing the laid lithium tantalate monocrystalline wafer to obtain the blackening monocrystalline piezoelectric composite film.
9. Fixing the blackened single crystal piezoelectric composite film on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment on the film layer until reducing ions on the surface of the film layer are removed, and then carrying out RCA cleaning to obtain a clean surface.
The obtained blackened monocrystal piezoelectric composite film sequentially comprises a film layer, a silicon dioxide layer, a dielectric layer and a monocrystal silicon layer; wherein the material of the thin film layer is monocrystalline lithium niobate.
Example six
Example six provides a method for preparing a blackened single crystal piezoelectric composite film, comprising the steps of:
1. preparing a 300-micron silicon carbide wafer and a 300-micron lithium niobate wafer, respectively fixing the silicon carbide 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, wherein the lithium niobate wafer is the lithium niobate wafer after blackening treatment.
2. Injecting He into the lithium niobate wafer processed in the step 1 by adopting a stripping ion injection method+The lithium niobate wafer is divided into a residual layer, a separation layer and a thin film layer in this order from the implantation surface, and He is implanted+And distributing ions in the separation layer to obtain the single crystal lithium niobate wafer implantation piece.
Implanting He by lift-off ion implantation+The implantation dose parameters were: the implantation dose is 3 × 1016ions/cm2The implantation energy is 35 keV.
3. Argon ions were implanted into the cleaned silicon carbide wafer by ion implantation to form a damaged layer of single crystal silicon, which was 5 μm thick as a dielectric layer.
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 single-crystal lithium niobate wafer injection sheet with the silicon dioxide layer, and bonding by adopting a direct bonding method to obtain a bonded body.
6. And (3) putting the bonding body into an annealing furnace in a nitrogen atmosphere, preserving the heat for 2 hours at 240 ℃, and separating the bonding body at the separation layer to obtain the single crystal piezoelectric composite film.
7. Laying a layer of lithium niobate single crystal wafer on the thin film layer of the single crystal piezoelectric composite film obtained after the treatment in the step 6, and burying the single crystal piezoelectric composite film on which the lithium niobate single crystal wafer is laid in blackened powder (composite powder of silicon powder and lithium carbonate), wherein the silicon powder comprises the following components in percentage by mass: lithium carbonate powder 5: 95.
8. and (3) preserving the temperature of the monocrystalline piezoelectric composite film buried in the blackening powder for 3 hours in a reduction furnace at 550 ℃ under the nitrogen atmosphere to carry out blackening reduction reaction, taking out the blackening powder after the blackening reduction reaction is finished, and removing the laid lithium tantalate monocrystalline wafer to obtain the blackening monocrystalline piezoelectric composite film.
9. Fixing the blackened single crystal piezoelectric composite film on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment on the film layer until reducing ions on the surface of the film layer are removed, and then carrying out RCA cleaning to obtain a clean surface.
The obtained blackened monocrystal piezoelectric composite film sequentially comprises a film layer, a silicon dioxide layer, a dielectric layer and a monocrystal silicon layer; wherein the material of the thin film layer is monocrystalline lithium niobate.
Example seven
Example seven provides a method for preparing a blackened single crystal piezoelectric composite film, comprising the steps of:
1. preparing a 300-micron silicon carbide wafer and a 300-micron lithium tantalate wafer, respectively fixing the silicon carbide wafer or the lithium tantalate wafer on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing to obtain a smooth surface, and then carrying out semiconductor RCA cleaning on the two wafers to obtain a clean surface, wherein the lithium tantalate wafer is a blackened lithium tantalate wafer.
2. Injecting He into the lithium tantalate wafer processed in the step 1 by adopting a stripping ion implantation method+Separating the lithium tantalate wafer into a residual layer, a separation layer and a thin film layer in this order from the implantation surface, and implanting He+And distributing ions in the separation layer to obtain the single crystal lithium tantalate wafer implanted piece.
Implanting He by lift-off ion implantation+The implantation dose parameters were: the implantation dose is 3 × 1016ions/cm2The implantation energy is 35 keV.
3. Argon ions were implanted into the cleaned silicon carbide wafer by ion implantation to form a damaged layer of single crystal silicon, which was 5 μm thick as a dielectric layer.
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 (3) contacting the single-crystal lithium tantalate wafer injection sheet with the silicon dioxide layer, and bonding by adopting a direct bonding method to obtain a bonded body.
6. And (3) putting the bonding body into an annealing furnace in a nitrogen atmosphere, preserving the heat for 2 hours at 240 ℃, and separating the bonding body at the separation layer to obtain the single crystal piezoelectric composite film.
7. Laying a lithium tantalate single crystal wafer on the thin film layer of the single crystal piezoelectric composite film obtained after the treatment in the step 6, and burying the single crystal piezoelectric composite film on which the lithium tantalate single crystal wafer is laid in blackening powder (composite powder of diamond powder and lithium carbonate), wherein the diamond powder comprises the following components in percentage by mass: lithium carbonate powder 5: 95.
8. and (3) preserving the temperature of the monocrystalline piezoelectric composite film buried in the blackening powder for 3 hours in a reduction furnace at 550 ℃ under the nitrogen atmosphere to carry out blackening reduction reaction, taking out the blackening powder after the blackening reduction reaction is finished, and removing the laid lithium tantalate monocrystalline wafer to obtain the blackening monocrystalline piezoelectric composite film.
9. Fixing the blackened single crystal piezoelectric composite film on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment on the film layer until reducing ions on the surface of the film layer are removed, and then carrying out RCA cleaning to obtain a clean surface.
The obtained blackened monocrystal piezoelectric composite film sequentially comprises a film layer, a silicon dioxide layer, a dielectric layer and a monocrystal silicon layer; wherein the material of the thin film layer is monocrystalline lithium tantalate.
Example eight
Example eight provides a method for preparing a blackened single crystal piezoelectric composite film, comprising the steps of:
1. preparing a 400-micron silicon carbide wafer and a 300-micron lithium niobate wafer, respectively fixing the silicon carbide 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, wherein the lithium niobate wafer is the lithium niobate wafer after blackening treatment.
2. And (3) implanting He + 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 layer, a separation layer and a thin film layer from an implantation surface, and implanted He + ions are distributed in the separation layer to obtain a single crystal lithium niobate wafer implantation piece.
When the stripping ion implantation method is adopted to implant He +, the implantation dosage parameters are as follows: the implantation dose was 3X 1016ions/cm2 and the implantation energy was 35 keV.
3. Argon ions were implanted into the cleaned silicon carbide wafer by ion implantation to form a damaged layer of single crystal silicon, which was 5 μm thick as a dielectric layer.
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 single-crystal lithium niobate wafer injection sheet with the silicon dioxide layer, and bonding by adopting a direct bonding method to obtain a bonded body.
6. And (3) putting the bonding body into an annealing furnace in a nitrogen atmosphere, preserving the heat for 2 hours at 240 ℃, and separating the bonding body at the separation layer to obtain the single crystal piezoelectric composite film.
7. Laying a layer of lithium niobate single crystal wafer on the thin film layer of the single crystal piezoelectric composite film obtained after the treatment in the step 6, and burying the single crystal piezoelectric composite film on which the lithium niobate single crystal wafer is laid in blackening powder (composite powder of iron powder, graphene and lithium carbonate), wherein the iron powder comprises the following components in percentage by mass: graphene: lithium carbonate powder 5: 5: 90.
8. and (3) preserving the temperature of the monocrystalline piezoelectric composite film buried in the blackening powder for 3 hours in a reduction furnace at 550 ℃ under the nitrogen atmosphere to carry out blackening reduction reaction, taking out the blackening powder after the blackening reduction reaction is finished, and removing the laid lithium tantalate monocrystalline wafer to obtain the blackening monocrystalline piezoelectric composite film.
9. Fixing the blackened single crystal piezoelectric composite film on a porous ceramic sucker of polishing equipment, carrying out chemical mechanical polishing treatment on the film layer until reducing ions on the surface of the film layer are removed, and then carrying out RCA cleaning to obtain a clean surface.
The obtained blackened monocrystal piezoelectric composite film sequentially comprises a film layer, a silicon dioxide layer, a dielectric layer and a monocrystal silicon layer; wherein the material of the thin film layer is monocrystalline lithium niobate.
The same and similar parts among the various embodiments in the present specification may be referred to each other, and especially, the corresponding embodiment part of the blackened single crystal piezoelectric composite film may be referred to the preparation method part of the blackened single crystal piezoelectric composite film.
The present application has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to limit the application. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the presently disclosed embodiments and implementations thereof without departing from the spirit and scope of the present disclosure, and these fall within the scope of the present disclosure. The protection scope of this application is subject to the appended claims.
Claims (11)
1. A preparation method of a blackened single-crystal piezoelectric composite film is characterized by comprising the following steps:
preparing a first wafer and a substrate base plate, wherein the first wafer is a lithium niobate wafer or a lithium tantalate wafer;
implanting ions into the first wafer through an ion implantation method, and dividing the first wafer into a residual layer, a separation layer and a thin film layer in sequence;
bonding the first wafer and the substrate base plate to obtain a bonded body;
carrying out heat treatment on the bonding body, and separating the residual substance layer from the thin film layer to obtain a single crystal piezoelectric composite film;
laying a second wafer or reduction paper on the thin film layer of the single crystal piezoelectric composite film to obtain a prefabricated body;
burying the pre-prepared body in a blackening powder, wherein the blackening powder comprises a reducing powder and a lithium carbonate powder;
carrying out blackening reduction heat treatment on the single crystal piezoelectric composite film buried in the blackening powder in a reducing furnace;
and removing the second wafer or the base paper to obtain the blackened single crystal piezoelectric composite film.
2. The method of claim 1, wherein the second wafer is the same material as the first wafer.
3. The production method according to claim 1, wherein the blackening powder comprises 1 to 10 parts by mass of reducing powder and 90 to 99 parts by mass of lithium carbonate powder.
4. The production method according to claim 3, wherein the blackening powder comprises 5 to 10 parts by mass of reducing powder and 90 to 95 parts by mass of lithium carbonate powder.
5. The method according to claim 1, wherein the reducing powder comprises any one or more of iron powder, aluminum powder, zinc powder, magnesium powder, silicon powder, and carbon powder.
6. The preparation method according to claim 1, wherein the reducing powder comprises a mixed powder of graphene and any one or more of iron powder, aluminum powder, zinc powder, magnesium powder, silicon powder and carbon powder.
7. The method according to claim 1, wherein the temperature of the blackening reduction heat treatment of the single crystal piezoelectric composite film buried in the blackening powder is 300-600 ℃ and the holding time is 1-100 hours in a reduction furnace.
8. The method as claimed in claim 1, wherein the ions implanted into the first wafer by the ion implantation method are helium ions, hydrogen ions, nitrogen ions, oxygen ions or argon ions, and the implantation dose is 2 x 1016ions/cm2-4×1016ions/cm2(ii) a The implantation energy is 40-400 keV.
9. The method of manufacturing according to claim 1, further comprising:
and polishing and cleaning the surface of the film layer in the blackened monocrystal piezoelectric composite film.
10. The production method according to claim 1, wherein the substrate base plate is a single-layer substrate or a composite substrate.
11. A blackened single-crystal piezoelectric composite film, which is prepared by the method for preparing a blackened single-crystal piezoelectric composite film according to any one of claims 1 to 10.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115207206A (en) * | 2022-09-16 | 2022-10-18 | 济南晶正电子科技有限公司 | Near-stoichiometric composite film and preparation method thereof |
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