CN117604471A - Silicon-based aluminum nitride composite substrate and preparation method thereof - Google Patents
Silicon-based aluminum nitride composite substrate and preparation method thereof Download PDFInfo
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 338
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 154
- 239000010703 silicon Substances 0.000 title claims abstract description 154
- 239000000758 substrate Substances 0.000 title claims abstract description 148
- 239000002131 composite material Substances 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 35
- 239000013078 crystal Substances 0.000 claims abstract description 29
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- 230000008025 crystallization Effects 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 192
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 95
- 229910052786 argon Inorganic materials 0.000 claims description 60
- 238000004544 sputter deposition Methods 0.000 claims description 34
- PWKWDCOTNGQLID-UHFFFAOYSA-N [N].[Ar] Chemical compound [N].[Ar] PWKWDCOTNGQLID-UHFFFAOYSA-N 0.000 claims description 22
- 238000009832 plasma treatment Methods 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 6
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims 1
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- 238000012360 testing method Methods 0.000 description 11
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- 238000002441 X-ray diffraction Methods 0.000 description 8
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- 238000011065 in-situ storage Methods 0.000 description 6
- 229910017083 AlN Inorganic materials 0.000 description 5
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 5
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- 229910021641 deionized water Inorganic materials 0.000 description 4
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- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0617—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
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Abstract
The application provides a silicon-based aluminum nitride composite substrate and a preparation method thereof, and relates to the field of composite material preparation. The preparation method comprises the following steps: forming a first aluminum nitride film on the surface of the silicon substrate by adopting a reactive magnetron sputtering method, and continuously forming a second aluminum nitride film on the surface of the first aluminum nitride film by adopting the reactive magnetron sputtering method, wherein the second aluminum nitride film and the first aluminum nitride film are columnar crystals, and repeating the steps to obtain the aluminum nitride film which is formed by alternately and periodically changing the first aluminum nitride film and the second aluminum nitride film in sequence. By controlling the thickness and crystallization quality of the first aluminum nitride film and the second aluminum nitride film, the tensile stress of the sputtered aluminum nitride film on the silicon substrate is relaxed finally, and the silicon-based aluminum nitride composite substrate which has a low stress state and can be applied to back-end devices such as radio frequency filters and the like is finally obtained, so that the yield and repeatability of the back-end devices are improved.
Description
Technical Field
The application relates to the field of composite material preparation, in particular to a silicon-based aluminum nitride composite substrate and a preparation method thereof.
Background
With the development of the internet of things, the performance requirements of devices such as home appliances and the like on radio frequency filters capable of being used in the GHz frequency range are gradually improved, so that good communication effects among the devices of the internet of things are ensured. As a representative material of the GHz band radio frequency filter, the silicon-based aluminum nitride composite substrate has been successfully applied to the thin film bulk acoustic wave filter, and exhibits excellent filtering efficacy.
However, the technical threshold of the film bulk acoustic wave filter is still higher at present, so that strict requirements are put on the material quality of silicon-based aluminum nitride. Particularly, the stress state of the aluminum nitride film layer directly determines the yield and stability of the device when the device is manufactured subsequently, so that a brand new method is found to reduce the stress state of the silicon-based aluminum nitride, and the method has great significance for further improving the technical index of the aluminum nitride-based film bulk acoustic wave filter and reducing the manufacturing cost in the future.
Disclosure of Invention
The embodiment of the application aims to provide a silicon-based aluminum nitride composite substrate and a preparation method thereof, which can reduce the tensile stress of the silicon-based aluminum nitride composite substrate, thereby improving the yield and the stability in the subsequent preparation of devices.
In a first aspect, an embodiment of the present application provides a method for preparing a silicon-based aluminum nitride composite substrate, including the following steps:
and forming a first aluminum nitride film on the surface of the silicon substrate by adopting a reactive magnetron sputtering method in a first mixed atmosphere of nitrogen and argon.
Forming a second aluminum nitride film on the surface of the first aluminum nitride film by adopting a reactive magnetron sputtering method in a second mixed atmosphere of nitrogen and argon, wherein the second aluminum nitride film and the first aluminum nitride film are columnar crystals, the nitrogen-argon flow ratio in the first mixed atmosphere is 8-13.4, the nitrogen-argon flow ratio in the second mixed atmosphere is smaller than the nitrogen-argon flow ratio in the first mixed atmosphere, and the thickness of the second aluminum nitride film is smaller than the thickness of the first aluminum nitride film; or the ratio of the flow rates of nitrogen and argon in the second mixed atmosphere is 8-13.4, the ratio of the flow rates of nitrogen and argon in the second mixed atmosphere is larger than the ratio of the flow rates of nitrogen and argon in the first mixed atmosphere, and the thickness of the second aluminum nitride film is larger than that of the first aluminum nitride film.
Repeating the steps to obtain the aluminum nitride film which is formed by alternately and periodically changing the first aluminum nitride film and the second aluminum nitride film in sequence.
According to the method, the thickness and the crystallization quality of the first aluminum nitride film and the second aluminum nitride film are controlled in the preparation process, the tensile stress of the sputtered aluminum nitride film on the silicon substrate is finally relaxed, the silicon-based aluminum nitride composite substrate with a low stress state is finally obtained, and the silicon-based aluminum nitride composite substrate can be used in rear-end devices such as radio frequency filters and is beneficial to improving the yield and repeatability of the rear-end devices, and is particularly suitable for large-scale industrial production.
In a second aspect, an embodiment of the present application provides a silicon-based aluminum nitride composite substrate, which includes a silicon substrate and an aluminum nitride film formed on a surface of the silicon substrate, wherein the aluminum nitride film is composed of a first aluminum nitride film and a second aluminum nitride film which alternately and periodically change in sequence in a direction from a direction close to the silicon substrate to a direction far from the silicon substrate, and the first aluminum nitride film and the second aluminum nitride film are columnar crystals.
Wherein the thickness of the first aluminum nitride film is 50-100 nm, the thickness of the second aluminum nitride film is 20-50% of the thickness of the first aluminum nitride film, and the crystallization quality of the first aluminum nitride film is better than that of the second aluminum nitride film; alternatively, the thickness of the second aluminum nitride film is 50-100 nm, the thickness of the first aluminum nitride film is 20-50% of the thickness of the second aluminum nitride film, and the crystallization quality of the second aluminum nitride film is better than that of the first aluminum nitride film.
According to the silicon-based aluminum nitride composite substrate, the tensile stress of the sputtered aluminum nitride film on the silicon substrate is finally relaxed by controlling the thickness and the crystallization quality of the first aluminum nitride film and the second aluminum nitride film, the silicon-based aluminum nitride composite substrate with a low stress state is finally obtained, and the silicon-based aluminum nitride composite substrate can be used in rear-end devices such as radio frequency filters and the like, is favorable for improving the yield and repeatability of the rear-end devices, and is particularly suitable for large-scale industrialized production.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments of the present application will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of a silicon-based aluminum nitride composite substrate provided in embodiment 1;
FIG. 2 is an XRD pattern of the (002) crystal face of aluminum nitride in the silicon-based aluminum nitride composite substrate provided in example 1;
fig. 3 is a schematic structural diagram of a silicon-based aluminum nitride composite substrate provided in embodiment 4;
fig. 4 is a schematic structural diagram of a silicon-based aluminum nitride composite substrate provided in example 5;
fig. 5 is an XRD pattern of the (002) crystal face of aluminum nitride in the silicon-based aluminum nitride composite substrate provided in comparative example 2.
In the figure: a 100-silicon-based aluminum nitride composite substrate; 10-a silicon substrate; 20-aluminum nitride film; 21-a first aluminum nitride film; 22-a second aluminum nitride film.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions in the embodiments of the present application will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The silicon-based aluminum nitride composite substrate and the preparation method thereof in the embodiment of the application are specifically described below.
The preparation method of the silicon-based aluminum nitride composite substrate mainly comprises the following steps:
forming a first aluminum nitride film on the surface of the silicon substrate by adopting a reactive magnetron sputtering method in a first mixed atmosphere of nitrogen and argon;
forming a second aluminum nitride film on the surface of the first aluminum nitride film by adopting a reactive magnetron sputtering method in a second mixed atmosphere of nitrogen and argon, wherein the second aluminum nitride film and the first aluminum nitride film are columnar crystals, the nitrogen-argon flow ratio in the first mixed atmosphere is 8-13.4, the nitrogen-argon flow ratio in the second mixed atmosphere is smaller than the nitrogen-argon flow ratio in the first mixed atmosphere, and the thickness of the second aluminum nitride film is smaller than the thickness of the first aluminum nitride film; or the ratio of the flow rates of nitrogen and argon in the second mixed atmosphere is 8-13.4, the ratio of the flow rates of nitrogen and argon in the second mixed atmosphere is larger than the ratio of the flow rates of nitrogen and argon in the first mixed atmosphere, and the thickness of the second aluminum nitride film is larger than that of the first aluminum nitride film.
Repeating the steps to obtain the aluminum nitride film which is formed by alternately and periodically changing the first aluminum nitride film and the second aluminum nitride film in sequence.
It will be appreciated that the number of layers of the first aluminum nitride film and the second aluminum nitride film in the finally obtained aluminum nitride film in fig. 1 is merely an example, and the number of periodic changes may be selected according to the thickness of the actually required aluminum nitride film, which is not limited herein.
It can be understood that, because the parameters of the reactive magnetron sputtering method mainly include the sputtering temperature, the sputtering power, the nitrogen-argon flow ratio and the cavity vacuum degree, wherein the former three affect the crystallization quality and the crystal structure of the film, the cavity vacuum degree changes with the difference of the nitrogen-argon flow ratio, the reactive magnetron sputtering method is adopted in the first mixed atmosphere to form the first aluminum nitride film on the surface of the silicon substrate, and the reactive magnetron sputtering method is adopted in the second mixed atmosphere to form the second aluminum nitride film on the surface of the first aluminum nitride film, which means that: the sputtering power and the sputtering temperature of the reactive magnetron sputtering method adopted for forming the second aluminum nitride film are the same as those of the first aluminum nitride film, and the main difference between the two is that the ratio of the nitrogen to the argon flow of the first mixed atmosphere to that of the second mixed atmosphere are different. Through above-mentioned setting, be favorable to controlling second aluminium nitride film and first aluminium nitride film and be columnar crystal, and through controlling nitrogen argon flow ratio in order to obtain second aluminium nitride film and first aluminium nitride film of different crystallization quality, the crystallization quality in this application refers to lattice uniformity, and the higher crystallization quality of lattice uniformity is better the higher, and generally the higher stress of lattice quality is bigger.
When the flow ratio of nitrogen to argon is 8-13.4, a film with good crystallization quality can be prepared, and when the flow ratio of nitrogen to argon is less than 8-13.4, the crystallization quality of the obtained film is deteriorated, namely, when the flow ratio of nitrogen to argon in the second mixed atmosphere is 8-13.4, the flow ratio of nitrogen to argon in the second mixed atmosphere is greater than the flow ratio of nitrogen to argon in the first mixed atmosphere, the crystallization quality of the second aluminum nitride film in the prepared silicon-based aluminum nitride composite substrate is superior to that of the first aluminum nitride film; when the ratio of the flow rates of nitrogen and argon in the first mixed atmosphere is 8-13.4 and the ratio of the flow rates of nitrogen and argon in the second mixed atmosphere is smaller than the ratio of the flow rates of nitrogen and argon in the first mixed atmosphere, the crystallization quality of the first aluminum nitride film in the prepared silicon-based aluminum nitride composite substrate is better than that of the second aluminum nitride film.
That is, in either of the above embodiments, the thickness of the thin film having a high crystalline quality is larger than that of the thin film having a low crystalline quality, so that the thin film having a low crystalline quality can be advantageously used as a transition layer to release stress, and can be applied to a back-end device such as a radio frequency filter.
That is, the thickness and the crystallization quality of the first aluminum nitride film and the second aluminum nitride film are controlled, the tensile stress of the sputtered aluminum nitride film on the silicon substrate is finally relaxed, and the silicon-based aluminum nitride composite substrate with a low stress state is finally obtained.
In order to facilitate the subsequent description, the final product obtained by preparing in a setting mode that the nitrogen-argon flow ratio in the first mixed atmosphere is 8-13.4, the nitrogen-argon flow ratio in the second mixed atmosphere is smaller than the nitrogen-argon flow ratio in the first mixed atmosphere, and the thickness of the second aluminum nitride film is smaller than that of the first aluminum nitride film is used as the first silicon-based aluminum nitride composite substrate. And taking the final product prepared in a mode that the nitrogen-argon flow ratio in the second mixed atmosphere is 8-13.4, the nitrogen-argon flow ratio in the second mixed atmosphere is larger than the nitrogen-argon flow ratio in the first mixed atmosphere, and the thickness of the second aluminum nitride film is larger than that of the first aluminum nitride film as a second silicon-based aluminum nitride composite substrate.
Wherein, for a first silicon-based aluminum nitride composite substrate:
in some embodiments, the ratio of the flow rates of nitrogen and argon in the second mixed atmosphere is 0.49 to 0.51 times the ratio of the flow rates of nitrogen and argon in the first mixed atmosphere.
In the range, the tensile stress of the sputtered aluminum nitride film on the silicon substrate is relaxed finally, and the silicon-based aluminum nitride composite substrate with a low stress state is obtained.
Illustratively, the ratio of the flow rates of nitrogen and argon in the second mixed atmosphere is any one of or between any two of 0.49 times, 0.50 times, 0.51 times the ratio of the flow rates of nitrogen and argon in the first mixed atmosphere.
In some embodiments, the first aluminum nitride film has a thickness of 50-100 nm and the second aluminum nitride film has a thickness of 20-50% of the thickness of the first aluminum nitride film.
The thickness of the silicon substrate and the aluminum nitride film is controlled within the range, so that the tensile stress of the sputtered aluminum nitride film on the silicon substrate is relaxed finally, and the silicon-based aluminum nitride composite substrate with a low stress state is obtained.
Illustratively, the first aluminum nitride film has a thickness of any one of 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, 85nm, 90nm, 95nm, 100nm or between any two values, and the second aluminum nitride film has a thickness of any one of 20%, 30%, 40%, 50% or between any two values of the thickness of the first aluminum nitride film.
In the first silicon-based aluminum nitride composite substrate, one side of the aluminum nitride film, which is far away from the silicon substrate, can be a first aluminum nitride film or a second aluminum nitride film, and one side of the aluminum nitride film, which is far away from the silicon substrate, is the surface of aluminum nitride.
Since the first aluminum nitride film has better crystalline quality than the second aluminum nitride film in the first silicon-based aluminum nitride composite substrate, in order to improve the surface flatness of the finally prepared aluminum nitride film, in some embodiments, the first aluminum nitride film is located on the side of the aluminum nitride film facing away from the silicon substrate.
Wherein, for the second silicon-based aluminum nitride composite substrate:
in some embodiments, the ratio of the flow rates of nitrogen and argon in the first mixed atmosphere is 0.49 to 0.51 times the ratio of the flow rates of nitrogen and argon in the second mixed atmosphere.
In the range, the tensile stress of the sputtered aluminum nitride film on the silicon substrate is relaxed finally, and the silicon-based aluminum nitride composite substrate with a low stress state is obtained.
Illustratively, the ratio of the flow rates of nitrogen and argon in the first mixed atmosphere is any one of or between 0.49 times, 0.50 times, 0.51 times the ratio of the flow rates of nitrogen and argon in the second mixed atmosphere.
In some embodiments, the second aluminum nitride film has a thickness of 50-100 nm and the first aluminum nitride film has a thickness of 20-50% of the thickness of the second aluminum nitride film.
The thickness of the silicon substrate and the aluminum nitride film is controlled within the range, so that the tensile stress of the sputtered aluminum nitride film on the silicon substrate is relaxed finally, and the silicon-based aluminum nitride composite substrate with a low stress state is obtained.
Illustratively, the second aluminum nitride film has a thickness of any one of 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, 85nm, 90nm, 95nm, 100nm or between any two values, and the first aluminum nitride film has a thickness of any one of 20%, 30%, 40%, 50% or between any two values of the second aluminum nitride film.
In the second silicon-based aluminum nitride composite substrate, the side of the aluminum nitride film, which is away from the silicon substrate, can be the first aluminum nitride film or the second aluminum nitride film, and the side of the aluminum nitride film, which is away from the silicon substrate, refers to the surface of aluminum nitride.
Since the second aluminum nitride film has better crystalline quality than the first aluminum nitride film in the second silicon-based aluminum nitride composite substrate, in order to improve the surface flatness of the finally prepared aluminum nitride film, in some embodiments, the second aluminum nitride film is located on the side of the aluminum nitride film facing away from the silicon substrate.
The processing methods of the first silicon-based aluminum nitride composite substrate and the second silicon-based aluminum nitride composite substrate according to the preparation method are the same except for the difference in thickness, nitrogen-argon ratio, and the like, and the following detailed description is given below:
in some embodiments, the flow rate of argon in the first mixed atmosphere is the same as the flow rate of argon in the second mixed atmosphere.
The flow rate of the argon is the same, so that different nitrogen-argon ratios can be obtained only by adjusting the flow rate of the nitrogen, and the quality of the formed first aluminum nitride film and the quality of the formed second aluminum nitride film can be controlled.
Optionally, the argon flow is 30-50 sccm.
Illustratively, the argon flow is any one of 30sccm, 35sccm, 40sccm, 45sccm, 50sccm or between any two values.
Wherein, the target material used in the reaction magnetron sputtering method is an aluminum target with the purity of 99.9999 percent so as to avoid introducing impurities.
In some embodiments, the reactive magnetron sputtering method has a sputtering power of 3000-5000W, a sputtering temperature of 600-700 ℃ and a vacuum of 0.1-0.9 Pa.
Within the above parameter range, the aluminum nitride film with columnar crystal structure is obtained.
Illustratively, the sputtering power in the reactive magnetron sputtering method is any one value or any range between any two values of 3000W, 3250W, 3500W, 3750W, 4000W, 4250W, 4500W, 4750W, 5000W, the sputtering temperature is any one value or any range between any two values of 600 ℃, 630 ℃, 650 ℃, 670 ℃, 700 ℃, and the vacuum degree is any one value or any range between any two values of 0.1Pa, 0.3Pa, 0.5Pa, 0.7Pa, and 0.9Pa.
The kind of the silicon substrate is not limited, and it may be intrinsic silicon, p-type silicon or n-type silicon, and the crystal orientation of silicon may be [111], 110 or 100].
In some embodiments, the silicon substrate comprises cubic phase single crystal silicon having a crystal orientation of [111] or [110], and no bevel.
It will be appreciated that before the first aluminum nitride film is formed on the surface of the silicon substrate, the silicon substrate needs to be cleaned to avoid the introduction of impurities, wherein the cleaning is to sequentially ultrasonically clean the substrate by using acetone, ethanol and deionized water, and then blow-dry the surface liquid by using nitrogen, which is beneficial to keeping the surface of the silicon substrate clean.
In some embodiments, the method of making comprises:
after forming a first aluminum nitride film, performing nitrogen plasma treatment on the surface of the first aluminum nitride film, and then forming a second aluminum nitride film by adopting a reactive magnetron sputtering method;
and/or after forming the second aluminum nitride film, performing nitrogen plasma treatment on the surface of the second aluminum nitride film, and then forming a first aluminum nitride film by adopting a reactive magnetron sputtering method;
and/or, before forming the first aluminum nitride film on the surface of the silicon substrate, performing nitrogen plasma treatment on the surface of the silicon substrate.
That is, in either arrangement, the surface of the first aluminum nitride film or the second aluminum nitride film, which is the surface of the aluminum nitride film, is not subjected to plasma treatment.
The silicon substrate, the first aluminum nitride film and the second first aluminum nitride film in the preparation process are subjected to plasma treatment, so that the interface binding force of the first aluminum nitride film and the second first aluminum nitride film is improved, and the tensile stress of the sputtered aluminum nitride film on the silicon substrate is relaxed finally.
Optionally, the preparation method comprises the following steps: after forming a first aluminum nitride film, performing nitrogen plasma treatment on the surface of the first aluminum nitride film, and then forming a second aluminum nitride film by adopting a reactive magnetron sputtering method; after forming a second aluminum nitride film, performing nitrogen plasma treatment on the surface of the second aluminum nitride film, and then forming a first aluminum nitride film by adopting a reactive magnetron sputtering method; and performing nitrogen plasma treatment on the surface of the silicon substrate before forming the first aluminum nitride film on the surface of the silicon substrate.
In some embodiments, the nitrogen plasma treatment is performed in a chamber of a reactive magnetron sputter deposition apparatus, the step of nitrogen plasma treatment comprising: the background atmosphere is pure nitrogen, the power of nitrogen plasma is 100-200W, and the pressure of the cavity in the treatment process is 0.2-0.4 Pa.
Under the above conditions, the nitrogen plasma treatment effect is good.
Exemplary, the nitrogen plasma power is any one of 100W, 120W, 150W, 170W, 200W or between any two values, and the chamber pressure during processing is any one of 0.2Pa, 0.3Pa, 0.4Pa or between any two values
The application also provides a silicon-based aluminum nitride composite substrate prepared by the preparation method, which comprises a silicon substrate and an aluminum nitride film formed on the surface of the silicon substrate, wherein the aluminum nitride film is composed of a first aluminum nitride film and a second aluminum nitride film which are alternately periodically changed in sequence in the direction from the direction close to the silicon substrate to the direction far away from the silicon substrate, and the first aluminum nitride film and the second aluminum nitride film are columnar crystals.
Wherein the thickness of the first aluminum nitride film is 50-100 nm, the thickness of the second aluminum nitride film is 20-50% of the thickness of the first aluminum nitride film, and the crystallization quality of the first aluminum nitride film is better than that of the second aluminum nitride film; alternatively, the thickness of the second aluminum nitride film is 50-100 nm, the thickness of the first aluminum nitride film is 20-50% of the thickness of the second aluminum nitride film, and the crystallization quality of the second aluminum nitride film is better than that of the first aluminum nitride film.
The silicon-based aluminum nitride composite substrate can be used in rear-end devices such as radio frequency filters and the like, the yield and repeatability of the rear-end devices are improved, and the silicon-based aluminum nitride composite substrate is particularly suitable for large-scale industrialized production.
In some alternative embodiments, the aluminum nitride film has a thickness of 60nm to 1000nm.
Illustratively, the aluminum nitride film has a thickness of any one of 60nm, 100nm, 200nm, 500nm, 700nm, 1000nm or between any two values. The features and capabilities of the present application are described in further detail below in connection with the examples.
In each of the following examples and comparative examples, stress tests were conducted using a stress tester of model FST 5000.
Example 1
The present embodiment provides a silicon-based aluminum nitride composite substrate 100 with a structure shown in fig. 1, and the preparation steps thereof are as follows;
1) Selecting 4-inch tangent silicon with the crystal orientation of [111] as a silicon substrate 10, and sequentially adopting an acetone solution, an ethanol solution and deionized water to ultrasonically clean the surface of the silicon substrate, wherein the cleaning time of each solution is 10min; after the cleaning is completed, the silicon substrate 10 is fished out and the surface is dried with nitrogen gas.
2) The silicon substrate 10 is placed in a reaction magnetron sputtering cavity, and the surface is subjected to in-situ nitrogen plasma treatment by utilizing nitrogen plasma, wherein during the treatment process, the background atmosphere is high-purity nitrogen with the concentration of 99.999 percent, the power of the nitrogen plasma is 100W, and the pressure of the cavity during the treatment process is 0.4Pa, and the treatment is carried out for 5 minutes.
3) Surface of silicon substrate 10 after nitriding treatment by reactive magnetron sputteringGrowing a first aluminum nitride film 21, wherein the thickness of the first aluminum nitride film 21 is 100nm, sputtering gas is mixed gas of nitrogen and argon, the flow rate of the argon is 30sccm, the flow rate of the nitrogen is 200sccm, and the vacuum degree of a cavity is 8 multiplied by 10 -1 Pa, the sputtering power is 3000W, and the sputtering temperature is 650 ℃; the crystal structure of the first aluminum nitride film 21 is columnar crystal.
4) Performing in-situ nitrogen plasma treatment on the surface of the first aluminum nitride film 21 in a reaction magnetron sputtering cavity, wherein the background atmosphere is high-purity nitrogen with the concentration of 99.999%, the power of the nitrogen plasma is 100W, and the cavity pressure is 4 multiplied by 10 during the treatment -1 Pa, treatment for 5 minutes.
5) Growing a second aluminum nitride film 22 on the first aluminum nitride film 21 after nitriding treatment by utilizing reactive magnetron sputtering, wherein the thickness of the second aluminum nitride film 22 is 20nm, sputtering gas is mixed gas of nitrogen and argon, the flow rate of the argon is 30sccm, the flow rate of the nitrogen is 100sccm, and the vacuum degree of a cavity is 5 multiplied by 10 -1 Pa, the sputtering power is 3000W, and the sputtering temperature is 650 ℃; the crystal structure of the second aluminum nitride film 22 is columnar crystal.
6) Performing in-situ nitrogen plasma treatment on the surface of the second aluminum nitride film 22 in a reaction magnetron sputtering cavity, wherein the background atmosphere is high-purity nitrogen with the concentration of 99.999%, the power of the nitrogen plasma is 100W, and the cavity pressure is 4 multiplied by 10 in the treatment process -1 Pa, treating for 5 minutes;
7) The above steps 2-6) are continuously repeated for 4 cycles, for 5 cycles, and finally the aluminum nitride film 20 is 600nm thick on the silicon-based aluminum nitride composite substrate 100 shown in fig. 1.
The XRD pattern of the aluminum nitride film prepared in example 1 is shown in fig. 2, wherein the half-width of the X-ray diffraction rocking curve of the (002) crystal face of aluminum nitride is 1.4484 degrees, and the aluminum nitride film can be applied to back-end devices such as radio frequency filters.
The silicon-based aluminum nitride composite substrate was subjected to stress test, and the results are shown in table 1.
Table 1 results of stress test on silicon-based aluminum nitride composite substrate in example 1
Example 2
The present embodiment provides a silicon-based aluminum nitride composite substrate, which is different from embodiment 1 in the preparation steps only in that:
in the step 3), the thickness of the first aluminum nitride film is 150nm.
In step 5), the thickness of the second aluminum nitride film was 30nm. And
And in the step 7), continuously repeating the steps 2-6) for 4 periods, and 5 periods altogether, thereby finally obtaining the silicon-based aluminum nitride composite substrate with the aluminum nitride film thickness of 720 nm.
The silicon-based aluminum nitride composite substrate was subjected to stress test, and the results are shown in table 2.
Table 2 results of stress test on silicon-based aluminum nitride composite substrate in example 2
Example 3
The embodiment provides a silicon-based aluminum nitride composite substrate, which comprises the following preparation steps:
1) Selecting a 4 inch tangent silicon [111] substrate with a specific orientation, carrying out chemical cleaning on the substrate, sequentially carrying out ultrasonic cleaning by adopting an acetone solution, an ethanol solution and deionized water, respectively carrying out ultrasonic cleaning for 10 minutes, and drying by using nitrogen after fishing out to keep the surface clean;
2) The first aluminum nitride film grows on the surface of the silicon substrate by utilizing reactive magnetron sputtering, the thickness is 100nm, sputtering gas is mixed gas of nitrogen and argon, the flow rate of the argon is 30sccm, the flow rate of the nitrogen is 200sccm, and the vacuum degree of a cavity is 8 multiplied by 10 - 1 Pa, the sputtering power was 3000W, and the sputtering temperature was 650 ℃.
3) Growing a second aluminum nitride film on the surface of the first aluminum nitride film by utilizing reactive magnetron sputtering, wherein the thickness of the second aluminum nitride film is 20nm, sputtering gas is mixed gas of nitrogen and argon, the flow rate of the argon is 30sccm, the flow rate of the nitrogen is 200sccm, and the vacuum degree of a cavity is 8 multiplied by 10 -1 Pa, the sputtering power was 3000W, and the sputtering temperature was 650 ℃.
4) And continuously repeating the steps 2-3) for 4 periods, wherein the total period is 5, and obtaining the silicon-based AlN composite substrate with the thickness of 600nm, and finally obtaining the silicon-based aluminum nitride composite substrate with the average stress of 405MPa and the thickness of 600 nm.
The silicon-based aluminum nitride composite substrate was subjected to stress test, and the results are shown in table 3.
TABLE 3 stress test results for silicon-based aluminum nitride composite substrate in example 3
As can be seen from table 1 and table 3, the internal stress of the silicon-based aluminum nitride composite substrate can be significantly improved by treating the silicon substrate and the first and second aluminum nitride films during the preparation process with nitrogen plasma.
Example 4
As shown in fig. 3, this embodiment provides a silicon-based aluminum nitride composite substrate 100, which is prepared by the following steps:
1) Selecting 4-inch tangent silicon with the crystal orientation of [111] as a silicon substrate 10, and sequentially adopting an acetone solution, an ethanol solution and deionized water to ultrasonically clean the surface of the silicon substrate, wherein the cleaning time of each solution is 10min; after the cleaning is completed, the silicon substrate 10 is fished out and the surface is dried with nitrogen gas.
2) The silicon substrate 10 is placed in a reaction magnetron sputtering cavity, and the surface is subjected to in-situ nitrogen plasma treatment by utilizing nitrogen plasma, wherein during the treatment process, the background atmosphere is high-purity nitrogen with the concentration of 99.999 percent, the power of the nitrogen plasma is 100W, and the pressure of the cavity during the treatment process is 0.4Pa, and the treatment is carried out for 5 minutes.
3) A first aluminum nitride film 21 is grown on the surface of the silicon substrate 10 after nitriding treatment by utilizing a reactive magnetron sputtering method, the thickness of the first aluminum nitride film 21 is 20nm, sputtering gas is mixed gas of nitrogen and argon, the flow rate of the argon is 30sccm, the flow rate of the nitrogen is 100sccm, and the vacuum degree of a cavity is 5 multiplied by 10 -1 Pa, sputtering power of3000W, the sputtering temperature is 650 ℃; the crystal structure of the first aluminum nitride film 21 is columnar crystal.
4) The surface of the first aluminum nitride film 21 is subjected to in-situ nitrogen plasma treatment in a reaction magnetron sputtering chamber, the background atmosphere is high-purity nitrogen with the concentration of 99.999%, the power of the nitrogen plasma is 100W, and the pressure of the chamber is 4 multiplied by 10 during the treatment -1 Pa, treatment for 5 minutes.
5) Growing a second aluminum nitride film 22 on the first aluminum nitride film 21 after nitriding treatment by utilizing reactive magnetron sputtering, wherein the thickness of the second aluminum nitride film 22 is 100nm, sputtering gas is mixed gas of nitrogen and argon, the flow rate of the argon is 30sccm, the flow rate of the nitrogen is 200sccm, and the vacuum degree of a cavity is 8 multiplied by 10 -1 Pa, the sputtering power is 3000W, and the sputtering temperature is 650 ℃; the crystal structure of the second aluminum nitride film 22 is columnar crystal.
6) Performing in-situ nitrogen plasma treatment on the surface of the second aluminum nitride film 22 in a reaction magnetron sputtering cavity, wherein the background atmosphere is high-purity nitrogen with the concentration of 99.999%, the power of the nitrogen plasma is 100W, and the cavity pressure is 4 multiplied by 10 in the treatment process -1 Pa, treating for 5 minutes;
7) And repeating the steps 2-6) for 4 periods, and finally obtaining the silicon-based aluminum nitride composite substrate with the thickness of the aluminum nitride film 20 of 600nm as shown in figure 3.
The silicon-based aluminum nitride composite substrate was subjected to stress test, and the results are shown in table 4.
Table 4 results of stress test on silicon-based aluminum nitride composite substrate in example 4
Example 5
As shown in fig. 4, this embodiment provides a silicon-based aluminum nitride composite substrate 100, which is specifically different from embodiment 1 in the preparation steps:
7) After repeating the above steps 2-6) for 4 cycles, steps 2) -3) are repeated once, and finally the aluminum nitride film 20 is 700nm thick as the silicon-based aluminum nitride composite substrate 100 shown in fig. 4.
The silicon-based aluminum nitride composite substrate prepared in the embodiment has better surface flatness and crystallization quality than those of the silicon-based aluminum nitride composite substrate prepared in the embodiment 1, so that the electrode prepared in the subsequent MEMS device is better combined with the surface of aluminum nitride, and voltage is easier to apply.
Comparative example 1
This comparative example provides a silicon-based aluminum nitride composite substrate whose preparation steps differ from those of example 1 only in that:
in the step 2) and the step 5), the sputtering gas is the mixture of nitrogen and argon, the flow rate of the argon is 30sccm, the flow rate of the nitrogen is 200sccm, and the vacuum degree of the cavity is 5 multiplied by 10 -1 Pa, sputtering powers are 3000W, and sputtering temperatures are 650 ℃.
Finally, the silicon-based aluminum nitride composite substrate with the aluminum nitride film thickness of 600nm is obtained.
The silicon-based aluminum nitride composite substrate was subjected to stress test, and the results are shown in table 5.
Table 5 stress test results of silicon-based aluminum nitride composite substrate in comparative example 1
As can be seen from table 5, comparative example 1 was always under the preparation condition of high nitrogen-argon flow ratio, and the average stress of the obtained material was 841MPa, which was significantly increased compared with example 1.
Comparative example 2
This comparative example provides a silicon-based aluminum nitride composite substrate, which is prepared by the steps of comparison with example 2, differing only in that:
in the step 2) and the step 5), the sputtering gas is the mixture of nitrogen and argon, the flow rate of the argon is 30sccm, the flow rate of the nitrogen is 100sccm, and the vacuum degree of the cavity is 5 multiplied by 10 -1 Pa, sputtering powers are 3000W, and sputtering temperatures are 650 ℃.
Finally, the silicon-based aluminum nitride composite substrate with the aluminum nitride film thickness of 600nm is obtained.
The X-ray diffraction rocking curve of aluminum nitride (002) crystal face X-ray diffraction rocking curve of comparative example 2 is shown in fig. 5, and the half-height width of the X-ray diffraction rocking curve of aluminum nitride (002) crystal face is larger than 4 °, so that the aluminum nitride (002) crystal face X-ray diffraction rocking curve cannot be practically applied to back-end devices such as radio frequency filters, that is, the quality of the prepared material is obviously deteriorated when comparative example 2 is always under the preparation condition of low nitrogen-argon flow ratio.
In summary, the preparation method provided by the application relaxes the tensile stress of the sputtered aluminum nitride film on the silicon substrate by controlling the thickness and the crystallization quality of the first aluminum nitride film and the second aluminum nitride film, and finally obtains the silicon-based aluminum nitride composite substrate with a low stress state.
The above is only an example of the present application, and is not intended to limit the scope of the present application, and various modifications and variations will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (10)
1. The preparation method of the silicon-based aluminum nitride composite substrate is characterized by comprising the following steps of:
forming a first aluminum nitride film on the surface of the silicon substrate by adopting a reactive magnetron sputtering method in a first mixed atmosphere of nitrogen and argon;
forming a second aluminum nitride film on the surface of the first aluminum nitride film by adopting the reactive magnetron sputtering method continuously in a second mixed atmosphere of nitrogen and argon, wherein the second aluminum nitride film and the first aluminum nitride film are columnar crystals, the nitrogen-argon flow ratio in the first mixed atmosphere is 8-13.4, the nitrogen-argon flow ratio in the second mixed atmosphere is smaller than the nitrogen-argon flow ratio in the first mixed atmosphere, and the thickness of the second aluminum nitride film is smaller than the thickness of the first aluminum nitride film; or the ratio of the flow rates of nitrogen and argon in the second mixed atmosphere is 8-13.4, the ratio of the flow rates of nitrogen and argon in the second mixed atmosphere is larger than the ratio of the flow rates of nitrogen and argon in the first mixed atmosphere, and the thickness of the second aluminum nitride film is larger than that of the first aluminum nitride film;
repeating the steps to obtain the aluminum nitride film which is formed by alternately and periodically changing the first aluminum nitride film and the second aluminum nitride film in sequence.
2. The method for manufacturing a silicon-based aluminum nitride composite substrate according to claim 1, wherein the ratio of the flow rate of nitrogen to argon in the second mixed atmosphere is 0.49 to 0.51 times that of the flow rate of nitrogen to argon in the first mixed atmosphere;
optionally, the thickness of the first aluminum nitride film is 50-100 nm, and the thickness of the second aluminum nitride film is 20-50% of the thickness of the first aluminum nitride film;
optionally, the first aluminum nitride film is located on one side of the aluminum nitride film away from the silicon substrate.
3. The method for manufacturing a silicon-based aluminum nitride composite substrate according to claim 1, wherein the ratio of the flow rates of nitrogen and argon in the first mixed atmosphere is 0.49 to 0.51 times that of the flow rate of nitrogen and argon in the second mixed atmosphere;
optionally, the thickness of the second aluminum nitride film is 50-100 nm, and the thickness of the first aluminum nitride film is 20-50% of the thickness of the second aluminum nitride film;
optionally, the second aluminum nitride film is located on one side of the aluminum nitride film away from the silicon substrate.
4. The method for producing a silicon-based aluminum nitride composite substrate according to any one of claims 1 to 3, wherein the flow rate of the argon gas in the first mixed atmosphere is the same as the flow rate of the argon gas in the second mixed atmosphere;
optionally, the flow rate of the argon is 30-50 sccm.
5. A method of producing a silicon-based aluminum nitride composite substrate according to any one of claims 1 to 3, comprising:
after the first aluminum nitride film is formed, performing nitrogen plasma treatment on the surface of the first aluminum nitride film, and then forming the second aluminum nitride film by adopting the reactive magnetron sputtering method;
and/or the number of the groups of groups,
after the second aluminum nitride film is formed, performing nitrogen plasma treatment on the surface of the second aluminum nitride film, and then forming the first aluminum nitride film by adopting the reactive magnetron sputtering method;
and/or the number of the groups of groups,
and carrying out nitrogen plasma treatment on the surface of the silicon substrate before the first aluminum nitride film is formed on the surface of the silicon substrate.
6. The method of preparing a silicon-based aluminum nitride composite substrate according to claim 5, wherein the nitrogen plasma treatment is performed in a chamber of a reactive magnetron sputtering deposition apparatus, the step of nitrogen plasma treatment comprising: the background atmosphere is pure nitrogen, the power of nitrogen plasma is 100-200W, and the pressure of the cavity in the treatment process is 0.2-0.4 Pa.
7. The method for producing a silicon-based aluminum nitride composite substrate according to any one of claims 1 to 3, wherein the sputtering power in the reactive magnetron sputtering method is 3000 to 5000W, the sputtering temperature is 600 to 700 ℃, and the vacuum degree is 0.1 to 0.9Pa.
8. A method of producing a silicon-based aluminum nitride composite substrate according to any one of claims 1 to 3, wherein the silicon substrate comprises cubic phase single crystal silicon having a crystal orientation of [111] or [110], and no bevel.
9. The silicon-based aluminum nitride composite substrate is characterized by comprising a silicon substrate and an aluminum nitride film formed on the surface of the silicon substrate, wherein the aluminum nitride film is composed of a first aluminum nitride film and a second aluminum nitride film which are alternately periodically changed in sequence in the direction from the direction close to the silicon substrate to the direction far away from the silicon substrate, and the first aluminum nitride film and the second aluminum nitride film are columnar crystals;
the thickness of the first aluminum nitride film is 50-100 nm, the thickness of the second aluminum nitride film is 20-50% of the thickness of the first aluminum nitride film, and the crystallization quality of the first aluminum nitride film is better than that of the second aluminum nitride film;
or the thickness of the second aluminum nitride film is 50-100 nm, the thickness of the first aluminum nitride film is 20-50% of the thickness of the second aluminum nitride film, and the crystallization quality of the second aluminum nitride film is better than that of the first aluminum nitride film.
10. The silicon-based aluminum nitride composite substrate according to claim 9, wherein the thickness of the aluminum nitride film is 60nm to 1000nm.
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