CN114855280A - Method for preparing high-quality crack-free aluminum nitride film on silicon and application thereof - Google Patents
Method for preparing high-quality crack-free aluminum nitride film on silicon and application thereof Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 12
- 239000010703 silicon Substances 0.000 title claims abstract description 12
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title abstract description 34
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 239000010408 film Substances 0.000 claims description 15
- 239000010409 thin film Substances 0.000 claims description 14
- 238000005530 etching Methods 0.000 claims description 6
- 238000011065 in-situ storage Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 14
- 238000005336 cracking Methods 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000004891 communication Methods 0.000 description 4
- 230000010354 integration Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000010897 surface acoustic wave method Methods 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
- C30B29/406—Gallium nitride
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/12—Etching in gas atmosphere or plasma
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- H—ELECTRICITY
- H03—ELECTRONIC CIRCUITRY
- H03H—IMPEDANCE NETWORKS, e.g. RESONANT CIRCUITS; RESONATORS
- H03H9/00—Networks comprising electromechanical or electro-acoustic devices; Electromechanical resonators
- H03H9/02—Details
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Abstract
The invention discloses a method for preparing a high-quality crack-free aluminum nitride film on silicon and application thereof. According to the invention, AlN epitaxially grows on a Si substrate at high temperature through MOCVD, then the high temperature is maintained, a GaN cap layer is epitaxially grown on the AlN, compressive stress is applied to a film system by utilizing the lattice constant of the AlN smaller than that of GaN so as to compensate thermal tensile stress in the cooling process, and then the GaN cap layer is removed, so that a high-quality AlN film with a certain thickness and without cracking is obtained. The method is simple, convenient and effective, and the prepared AlN-based material is applied to the film bulk acoustic resonator, thereby being beneficial to improving the performance of the device.
Description
Technical Field
The invention belongs to the technical field of film bulk acoustic resonators, and particularly relates to a method for preparing a high-quality crack-free aluminum nitride film on silicon and application thereof.
Background
The filter is one of the components of the rf front end, and its main function is to selectively filter the transceiving signal of a specific frequency band, and reduce the influence of the interference signal, so that it directly determines the working frequency band and bandwidth of the communication device, and plays a very important role in the rf front end. With the development of information-oriented society and communication applications, higher requirements on filter performance are put forward for higher transmission rate and higher frequency. In particular, accompanying the extremely high data transmission capability of 5G communications is the need for high bandwidth of the filter. In addition, the number of filters required in modern smart phones is now multiplied by the support of various communication systems. Surface Acoustic Wave (SAW) filters and bulky dielectric filters have been unable to meet the requirements of mobile phone terminals, micro base stations and the like for high frequency and micro, while Film Bulk Acoustic Resonator (FBAR) filters have the advantages of small volume, low loss, integration capability, high quality factor, high out-of-band rejection, high operating frequency, high power bearing capacity and the like, thus becoming 5G radio frequency filters which can meet the requirements of 5G high frequency and can also meet the requirement of radio frequency front end modularization integration.
Aluminum nitride (AlN) is currently the piezoelectric material of choice for FBARs due to its excellent material properties such as high piezoelectric coefficient, stable chemistry, low temperature coefficient, etc. Since the FBAR adopts a cavity structure, the selection of the substrate material has little influence on its performance, and can function as a carrier, so that silicon (Si) and silicon dioxide (SiO) 2 ) Sapphire (Al) 2 O 3 ) Lithium niobate (LiNbO) 3 ) And some organic film materials, etc. can be used as the substrate material, but in consideration of cost, practicality, and integration with IC, Si is often used as the substrate material. In addition, FBAR is a bulk acoustic wave filter (BAW) in which an acoustic wave propagates longitudinally in the thickness direction, and thus it is required that AlN material has good (002) orientation. Therefore, in summary, the preparation of high-quality (002) preferentially oriented AlN film on Si substrate is one of the key technologies to obtain high-performance FBAR devices.
At present, materials for the AlN-based filter on Si are mostly prepared by adopting a radio frequency magnetron sputtering method, but the obtained film has generally larger full width at half maximum through the test of an X-ray rocking curve, and reflects the poorer crystal quality. By adopting Metal Organic Chemical Vapor Deposition (MOCVD), an AlN epitaxial film with higher quality can be prepared on a Si substrate, but the problem that the film is easy to crack after the film is larger than a certain thickness (such as 200nm) because of large tensile stress in the film caused by the difference of the thermal expansion coefficients between the substrate and the epitaxial layer in the cooling process after high-temperature epitaxial growth also exists. However, AlN-based materials for FBAR often have corresponding requirements for their thickness and surface condition (e.g. the thickness needs to be 500nm to 1.5 μm, and there is no crack on the surface), so a method for preparing an AlN film with a certain thickness and high quality without cracking while maintaining low cost is urgently needed, which is of great significance for improving the performance of FBAR devices and promoting them to enter the 5G end market with large volume.
Disclosure of Invention
The invention aims to provide a method for preparing a high-quality AlN thin film with a certain thickness and without cracking on silicon.
Specifically, the technical scheme provided by the invention is as follows:
a method for preparing high-quality crack-free AlN thin film with certain thickness on silicon, after epitaxially growing AlN on a Si substrate by MOCVD, a GaN cap layer is further epitaxially grown, and then the GaN cap layer is removed, specifically comprising the following steps:
1) putting the Si substrate into an MOCVD growth chamber, and carrying out high-temperature epitaxial growth on an AlN layer with the required thickness after heating and in-situ baking;
2) maintaining high temperature, and then epitaxially growing a GaN cap layer with a certain thickness on the AlN layer;
3) after cooling, removing the GaN cap layer by adopting a proper method including but not limited to etching, grinding, polishing and thinning and the like to obtain the AlN thin film on the silicon.
As described aboveIn the step 1), the baking temperature is preferably 900-1100 ℃, and the baking temperature is H under the pressure of 50-300 mbar 2 And carrying out in-situ baking on the Si substrate in the atmosphere, wherein the baking time is 5-20 minutes.
In the step 1), an AlN layer with a certain thickness is epitaxially grown under the conditions of a certain temperature, a certain reaction chamber pressure, a certain growth speed and V/III. Preferably, the epitaxial growth temperature is 800-1200 ℃, and more preferably 850-1100 ℃; the pressure of the reaction chamber is 50-200 mbar, and more preferably 50-100 mbar; the growth rate is 0.1-0.5 μm/h, more preferably 0.2-0.4 μm/h; V/III is 100 to 10000, and more preferably 2000 to 8000; and epitaxially growing an AlN layer with the thickness of 500-1500 nm.
And in the step 2), epitaxially growing a GaN layer with a certain thickness under the conditions of a certain temperature, reaction chamber pressure, growth speed and V/III. Preferably, the growth temperature is 900-1100 ℃, more preferably 950-1050 ℃; the pressure of the reaction chamber is 50-300 mbar, the growth speed is 0.5-3 μm/h, the V/III is 500-5000, and the GaN cap layer with the thickness of 50-300 nm (more preferably 100-250 nm) is epitaxially grown.
According to the method for preparing the high-quality crack-free AlN thin film with a certain thickness, provided by the invention, the compressive stress is provided for the thin film system through the growth of the GaN cap layer so as to compensate the thermal tensile stress generated in the cooling process, so that the AlN thin film with a certain thickness is prevented from cracking in the cooling process. The method is simple, convenient and effective, and plays an important role in improving the quality of the AlN-based material for the FBAR and the performance of the device.
Drawings
FIG. 1 is a schematic diagram of a high quality AlN thin film structure with a certain thickness and without cracking, grown on a Si substrate according to the present invention, wherein 1-Si substrate; 2-an AlN layer; 3-GaN cap layer.
Detailed Description
The invention will be further explained by the embodiments with reference to the drawings.
The method for preparing the high-quality crack-free AlN thin film with a certain thickness has the core that a GaN cap layer is epitaxially grown on AlN to prevent the thin film from cracking due to thermal tensile stress.
Example 1
Referring to fig. 1, an AlN thin film was prepared by the following steps:
A. selecting a Si substrate 1 and placing the Si substrate 1 into an MOCVD reaction chamber, wherein the resistance value of the Si substrate 1 is 0.02 ohm-cm (omega-cm), and the thickness is 975 mu m;
B. the reaction chamber was brought to 1000 ℃ at a reaction chamber pressure of 67mbar and H 2 In-situ baking the substrate for 5min under the atmosphere;
C. growing an AlN layer 2 with a thickness of 500nm at a growth rate of 0.27 μm/h and V/III of 4880 at a reaction chamber temperature of 1060 ℃ and a reaction chamber pressure of 53 mbar;
D. continuing to grow the GaN cap layer 3 at 735V/III and 0.65 mu m/h long speed at the reaction chamber temperature of 1000 ℃ and the reaction chamber pressure of 67mbar, wherein the thickness of the GaN cap layer is 200 nm;
E. and after cooling, etching the GaN cap layer 3 by adopting an Inductively Coupled Plasma (ICP) etching method, thereby obtaining the AlN material on Si for FBAR.
Example 2
Referring to fig. 1, an AlN thin film was prepared by the following steps:
A. selecting a Si substrate 1 and placing the Si substrate 1 into an MOCVD reaction chamber, wherein the resistance value of the Si substrate 1 is 0.02 ohm-cm (omega-cm), and the thickness is 975 mu m;
B. the reaction chamber was brought to 1000 ℃ at a reaction chamber pressure of 67mbar and H 2 Carrying out in-situ bake on the substrate for 5min under the atmosphere;
C. growing an AlN layer 2 with a thickness of 800nm at a growth rate of 2350V/III and 0.23 μm/h at a reaction chamber temperature of 1040 ℃ and a reaction chamber pressure of 53 mbar;
D. continuing to grow the GaN cap layer 3 with the thickness of 250nm at the growth speed of 735V/III and 0.65 mu m/h at the temperature of the reaction chamber of 1020 ℃ and the pressure of the reaction chamber of 67 mbar;
E. and after cooling, etching the GaN cap layer 3 by adopting an Inductively Coupled Plasma (ICP) etching method, thereby obtaining the AlN material on Si for FBAR.
The invention adopts a unique method for epitaxially growing the GaN cap layer on the AlN, and can effectively solve the cracking problem of the AlN film with a certain thickness, thereby being beneficial to obtaining high-quality AlN material and improving the performance of the FBAR filter.
Although the preferred embodiment of the present invention and the accompanying drawings have been disclosed for illustrative purposes, those skilled in the art will appreciate that various substitutions, alterations, and modifications are possible without departing from the scope of the invention and the appended claims, and the invention should not be limited to the disclosure of the preferred embodiment and the accompanying drawings. Therefore, the protection scope of the present invention is subject to the appended claims.
Claims (10)
1. A method of producing a crack-free AlN film on silicon, comprising the steps of:
1) putting the Si substrate into an MOCVD growth chamber, carrying out in-situ baking on the Si substrate, and carrying out high-temperature epitaxial growth on an AlN layer with the required thickness;
2) maintaining high temperature, and epitaxially growing a GaN cap layer on the AlN layer;
3) and removing the GaN cap layer after cooling to obtain the AlN thin film on the silicon.
2. The process according to claim 1, wherein in step 1) the temperature is initially raised to 900 ℃ to 1100 ℃ and H is applied at a pressure of 50 to 300mbar 2 And carrying out in-situ baking on the Si substrate in the atmosphere.
3. The method of claim 1, wherein the step 1) epitaxially grows the AlN layer under the conditions of a growth temperature of 800 ℃ to 1200 ℃, a pressure in the reaction chamber of 50 to 200mbar, a growth rate of 0.1 to 0.5 μm/h, and a V/III of 100 to 10000.
4. The method of claim 1, wherein the step 1) epitaxially grows an AlN layer with a thickness of 500 to 1500nm on the Si substrate.
5. The method of claim 1, wherein the GaN cap layer is epitaxially grown in the step 2) under the conditions of a growth temperature of 900 ℃ to 1100 ℃, a pressure in the reaction chamber of 50 mbar to 300mbar, a growth rate of 0.5 μm/h to 3 μm/h, and a V/III ratio of 500 to 5000.
6. The method according to claim 1, wherein the step 2) epitaxially grows a GaN cap layer with a thickness of 50-300 nm on the AlN layer.
7. The method of claim 6, wherein the thickness of the epitaxially grown GaN cap layer of step 2) is 100-250 nm.
8. The method of claim 1, wherein step 3) removes the GaN cap layer by etching, grinding and/or polishing for thinning.
9. A crack-free AlN thin film on silicon, prepared according to the method of any one of claims 1 to 8.
10. Use of the crack-free AlN film on silicon, according to claim 9, in a thin film bulk acoustic resonator.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116180233A (en) * | 2023-04-27 | 2023-05-30 | 北京中博芯半导体科技有限公司 | Preparation method and application of AlN film with high quality and low residual stress |
| CN116590687A (en) * | 2023-07-18 | 2023-08-15 | 广州市艾佛光通科技有限公司 | AlN thin film epitaxial wafer, preparation method and application of AlN thin film |
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| CN112680714A (en) * | 2020-12-04 | 2021-04-20 | 至芯半导体(杭州)有限公司 | Method for growing AlN thin film |
| CN113823557A (en) * | 2021-08-05 | 2021-12-21 | 乂馆信息科技(上海)有限公司 | HEMT device and preparation method thereof |
| CN114362703A (en) * | 2021-11-15 | 2022-04-15 | 奥趋光电技术(杭州)有限公司 | Preparation method of piezoelectric film template for acoustic wave device |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116180233A (en) * | 2023-04-27 | 2023-05-30 | 北京中博芯半导体科技有限公司 | Preparation method and application of AlN film with high quality and low residual stress |
| CN116590687A (en) * | 2023-07-18 | 2023-08-15 | 广州市艾佛光通科技有限公司 | AlN thin film epitaxial wafer, preparation method and application of AlN thin film |
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