CN113363133A - Aluminum nitride-silicon carbide composite film and manufacturing method thereof - Google Patents
Aluminum nitride-silicon carbide composite film and manufacturing method thereof Download PDFInfo
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- CN113363133A CN113363133A CN202010146465.3A CN202010146465A CN113363133A CN 113363133 A CN113363133 A CN 113363133A CN 202010146465 A CN202010146465 A CN 202010146465A CN 113363133 A CN113363133 A CN 113363133A
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- silicon carbide
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 61
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 45
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000758 substrate Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 24
- 230000008569 process Effects 0.000 claims abstract description 12
- 238000007788 roughening Methods 0.000 claims abstract description 12
- 239000011148 porous material Substances 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 56
- 229910052757 nitrogen Inorganic materials 0.000 claims description 28
- 238000004140 cleaning Methods 0.000 claims description 20
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 238000000861 blow drying Methods 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 claims description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 2
- 239000010408 film Substances 0.000 description 29
- 239000010409 thin film Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/02373—Group 14 semiconducting materials
- H01L21/02378—Silicon carbide
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02538—Group 13/15 materials
- H01L21/0254—Nitrides
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- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for manufacturing an aluminum nitride-silicon carbide composite film, which comprises the following steps: roughening the carbon surface of the silicon carbide substrate to form a roughened carbon surface; and forming an aluminum nitride film with a pore structure on the roughened carbon surface by utilizing an epitaxial growth process. The invention discloses an aluminum nitride-silicon carbide composite film manufactured by the manufacturing method. The invention solves the problem that when the aluminum nitride film grows on the silicon carbide substrate, tensile stress is generated between the silicon carbide substrate and the aluminum nitride film, so that cracks are generated on the aluminum nitride film.
Description
Technical Field
The invention relates to the technical field of semiconductor materials, in particular to an aluminum nitride-silicon carbide composite film and a manufacturing method thereof.
Background
Silicon carbide as a third-generation wide bandgap semiconductor material has excellent characteristics of good thermal conductivity, wide band gap, high breakdown electric field strength, high carrier saturation mobility and the like, so that the silicon carbide is widely applied to the manufacturing fields of high-temperature, high-frequency and high-power electronic devices and integrated circuits. Meanwhile, SiC has a good lattice match and a close thermal expansion coefficient to some semiconductor materials, so that a great number of researchers and technicians grow semiconductor single crystal thin films by using silicon carbide as a substrate. However, AlN is subjected to tensile stress when grown on a SiC substrate, and the AlN thin film starts to crack when the growth thickness of the AlN thin film exceeds 1 μm, thereby limiting the range of applications of the aluminum nitride-silicon carbide composite film.
Disclosure of Invention
In order to solve the defects in the prior art, the invention adopts the following technical scheme:
in one aspect of the present invention, a method for manufacturing an aluminum nitride-silicon carbide composite film is provided, including:
roughening the carbon surface of the silicon carbide substrate to form a roughened carbon surface;
and forming an aluminum nitride film with a pore structure on the roughened carbon surface by utilizing an epitaxial growth process.
Preferably, cleaning is required prior to roughening.
Preferably, roughening the carbon side of the silicon carbide substrate comprises: and coarsening the carbon surface of the silicon carbide substrate by using diamond polishing solution.
Preferably, the forming of the aluminum nitride thin film having a pore structure on the roughened carbon surface using an epitaxial growth process includes:
introducing ammonia gas for a preset time under a preset temperature environment;
introducing a nitrogen source and an aluminum source, and epitaxially growing the aluminum nitride film at a preset growth rate; wherein the flow rate of the nitrogen source is larger than that of the aluminum source.
Preferably, the step of introducing a nitrogen source and an aluminum source and epitaxially growing the aluminum nitride thin film at a predetermined growth rate comprises:
introducing ammonia gas for 3-10 minutes at the temperature of 1300-1350 ℃, then introducing a nitrogen source and an aluminum source according to the flow ratio of the nitrogen source to the aluminum source of more than 90:1, and epitaxially growing a first aluminum nitride film with the thickness of 10-50 nm at the growth rate of 50-200 nm/h;
introducing a nitrogen source and an aluminum source at the temperature of 1350-1400 ℃, wherein the flow ratio of the nitrogen source to the aluminum source is 60-90: 1, and a second sub aluminum nitride layer with the thickness of 500 nm-1000 nm is epitaxially grown on the first sub aluminum nitride layer at the growth rate of 200 nm/h-500 nm/h;
and introducing a nitrogen source and an aluminum source at the temperature of 1400-1450 ℃, wherein the flow ratio of the nitrogen source to the aluminum source is 35-60: 1, and extending a third sub-aluminum nitride layer with the thickness of 1000-10000 nm on the second sub-aluminum nitride layer at the growth rate of 500-2000 nm/h to form the aluminum nitride layer.
Preferably, the silicon carbide substrate is a 6H-SiC single crystal silicon carbide substrate.
Preferably, the roughened carbon surface has a surface roughness of 3 to 10 nm.
Preferably, cleaning is also required after roughening.
Preferably, the cleaning comprises:
putting the silicon carbide substrate into an HF or HCl solution for ultrasonic cleaning for 8-10 minutes to finish the first-stage cleaning;
putting the silicon carbide substrate cleaned in the first stage into an acetone solution for ultrasonic cleaning for 10-12 minutes to finish cleaning in the second stage;
putting the silicon carbide substrate cleaned in the second stage into an isopropanol solution for ultrasonic cleaning for 8-12 minutes to finish the cleaning in the third stage;
putting the silicon carbide substrate cleaned in the third stage into an ethanol solution for ultrasonic cleaning for 7-8 minutes to finish cleaning in a fourth stage;
and carrying out nitrogen blow-drying on the silicon carbide substrate cleaned in the fourth stage to finish cleaning.
In another aspect of the invention, the aluminum nitride-silicon carbide composite film formed by the manufacturing method is also provided.
The aluminum nitride film of the aluminum nitride-silicon carbide composite film manufactured by the manufacturing method has a structure with a plurality of holes. The purpose of roughening the carbon surface of the silicon carbide substrate in the manufacturing method of the invention is to improve the probability of forming a pore structure in the epitaxial growth process of the aluminum nitride film. The aluminum nitride film with the porous structure can relieve tensile stress generated during growth on the silicon carbide substrate and relieve cracks, so that the growth thickness of the aluminum nitride film can reach more than 3 microns, a sensor or an optical device based on the aluminum nitride-silicon carbide composite film can be manufactured, and the application range of the aluminum nitride-silicon carbide composite film is further improved.
Drawings
FIG. 1 is a flow chart of a method for manufacturing an aluminum nitride-silicon carbide composite film according to an embodiment of the present invention;
FIG. 2 is a morphology chart of porous aluminum nitride of the aluminum nitride-silicon carbide composite film according to the embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in detail below with reference to the accompanying drawings. Examples of these preferred embodiments are illustrated in the accompanying drawings. The embodiments of the invention shown in the drawings and described in accordance with the drawings are exemplary only, and the invention is not limited to these embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme according to the present invention are shown in the drawings, and other details not so relevant to the present invention are omitted.
The embodiment provides a method for manufacturing an aluminum nitride-silicon carbide composite film, which comprises the following steps:
step 1, providing a 6H-SiC monocrystal silicon carbide substrate, and putting the silicon carbide substrate into an HF solution or an HCl solution for ultrasonic cleaning for 8-10 minutes.
And 2, putting the silicon carbide substrate obtained in the step 1 into an acetone solution for ultrasonic cleaning for 10-12 minutes.
And 3, putting the silicon carbide substrate subjected to the step 2 into an isopropyl alcohol solution, and ultrasonically cleaning for 8-12 minutes.
And 4, putting the silicon carbide substrate subjected to the step 3 into an ethanol solution, and ultrasonically cleaning for 7-8 minutes.
And 5, carrying out nitrogen blow-drying on the silicon carbide substrate after the step 4 to finish cleaning.
And 6, roughening the carbon surface of the silicon carbide substrate by using a diamond polishing solution to form a roughened carbon surface, wherein the surface roughness of the roughened carbon surface is 3-10 nm (detected by a commercial atomic force microscope and fitted by self-contained software).
And 7, carrying out epitaxial growth of aluminum nitride on the roughened carbon surface, specifically:
introducing ammonia gas for 3-10 minutes at the temperature of 1300-1350 ℃, then introducing a nitrogen source and an aluminum source according to the flow ratio of the nitrogen source to the aluminum source of more than 90:1, and epitaxially growing a first aluminum nitride film with the thickness of 10-50 nm at the growth rate of 50-200 nm/h;
introducing a nitrogen source and an aluminum source at the temperature of 1350-1400 ℃, wherein the flow ratio of the nitrogen source to the aluminum source is 60-90: 1, and a second sub aluminum nitride layer with the thickness of 500 nm-1000 nm is epitaxially grown on the first sub aluminum nitride layer at the growth rate of 200 nm/h-500 nm/h;
and introducing a nitrogen source and an aluminum source at the temperature of 1400-1450 ℃, wherein the flow ratio of the nitrogen source to the aluminum source is 35-60: 1, and extending a third sub-aluminum nitride layer with the thickness of 1000-10000 nm on the second sub-aluminum nitride layer at the growth rate of 500-2000 nm/h to form the aluminum nitride layer with the pore structure. The specific surface topography is shown in fig. 2.
Wherein, the specific growth principle is as follows: the formation of porous aluminum nitride is a result of controlling the growth of aluminum nitride using growth kinetics. Initially, aluminum nitride non-uniformly nucleates on the carbon face of the roughened silicon carbide substrate, forming aluminum nitride islands. Then the small islands grow gradually and are connected with each other. At this time, at a specific V/III ratio (nitrogen source/aluminum source ratio, generally between 50 and 300), it is difficult for the aluminum nitride islands to be completely merged to form a continuous aluminum nitride film, and a large number of pores are thus formed and retained.
And 8, repeating the cleaning process from the step 1 to the step 5.
The aluminum nitride thin film of the aluminum nitride-silicon carbide composite film manufactured by the manufacturing method of the embodiment has a structure with a plurality of holes. The purpose of roughening the carbon surface of the silicon carbide substrate in the manufacturing method of the invention is to improve the probability of forming a pore structure in the epitaxial growth process of the aluminum nitride film. The aluminum nitride film with the porous structure can relieve tensile stress generated during growth on the silicon carbide substrate and relieve cracks, so that the growth thickness of the aluminum nitride film can reach more than 3 microns, a sensor or an optical device based on the aluminum nitride-silicon carbide composite film can be manufactured, and the application range of the aluminum nitride-silicon carbide composite film is further improved.
In addition, in the process of forming the third aluminum nitride layer in the step 7, the temperature is increased to 1450-1600 ℃, and when the growth rate of the aluminum nitride is increased to 3000-7000 nm/h, the aluminum nitride film with the cavity structure can be obtained, that is, the pore structure of the aluminum nitride film can be sealed by increasing the growth temperature and the growth rate of the aluminum nitride, so that the surface of the aluminum nitride-silicon carbide composite film is smoother, and the application range is further expanded.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A method for manufacturing an aluminum nitride-silicon carbide composite film is characterized by comprising the following steps:
roughening the carbon surface of the silicon carbide substrate to form a roughened carbon surface;
and forming an aluminum nitride film with a pore structure on the roughened carbon surface by utilizing an epitaxial growth process.
2. The method of claim 1, wherein the pre-roughening cleaning is performed.
3. The method of claim 1, wherein roughening the carbon side of the silicon carbide substrate comprises: and coarsening the carbon surface of the silicon carbide substrate by using diamond polishing solution.
4. The method of claim 1, wherein forming an aluminum nitride film having a pore structure on the roughened carbon surface using an epitaxial growth process comprises:
introducing ammonia gas for a preset time under a preset temperature environment;
introducing a nitrogen source and an aluminum source, and epitaxially growing the aluminum nitride film at a preset growth rate; wherein the flow rate of the nitrogen source is larger than that of the aluminum source.
5. The method of claim 4, wherein the step of introducing a source of nitrogen and a source of aluminum and epitaxially growing the aluminum nitride film at a predetermined growth rate comprises:
introducing ammonia gas for 3-10 minutes at the temperature of 1300-1350 ℃, then introducing a nitrogen source and an aluminum source according to the flow ratio of the nitrogen source to the aluminum source of more than 90:1, and epitaxially growing a first aluminum nitride film with the thickness of 10-50 nm at the growth rate of 50-200 nm/h;
introducing a nitrogen source and an aluminum source at the temperature of 1350-1400 ℃, wherein the flow ratio of the nitrogen source to the aluminum source is 60-90: 1, and a second sub aluminum nitride layer with the thickness of 500 nm-1000 nm is epitaxially grown on the first sub aluminum nitride layer at the growth rate of 200 nm/h-500 nm/h;
and introducing a nitrogen source and an aluminum source at the temperature of 1400-1450 ℃, wherein the flow ratio of the nitrogen source to the aluminum source is 35-60: 1, and extending a third sub-aluminum nitride layer with the thickness of 1000-10000 nm on the second sub-aluminum nitride layer at the growth rate of 500-2000 nm/h to form the aluminum nitride layer.
6. The production method according to claim 1, wherein the silicon carbide substrate is a 6H — SiC single crystal silicon carbide substrate.
7. The method of claim 1 or 3, wherein the roughened carbon surface has a surface roughness of 3 to 10 nm.
8. The method of claim 1, further comprising cleaning after roughening.
9. The method of manufacturing of claim 2 or 8, wherein the cleaning comprises:
putting the silicon carbide substrate into an HF or HCl solution for ultrasonic cleaning for 8-10 minutes to finish the first-stage cleaning;
putting the silicon carbide substrate cleaned in the first stage into an acetone solution for ultrasonic cleaning for 10-12 minutes to finish cleaning in the second stage;
putting the silicon carbide substrate cleaned in the second stage into an isopropanol solution for ultrasonic cleaning for 8-12 minutes to finish the cleaning in the third stage;
putting the silicon carbide substrate cleaned in the third stage into an ethanol solution for ultrasonic cleaning for 7-8 minutes to finish cleaning in a fourth stage;
and carrying out nitrogen blow-drying on the silicon carbide substrate cleaned in the fourth stage to finish cleaning.
10. An aluminum nitride-silicon carbide composite film produced by the production method according to any one of claims 1 to 9.
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CN117650053A (en) * | 2024-01-30 | 2024-03-05 | 天津正新光电科技有限公司 | Preparation method of silicon carbide packaging heat sink |
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2020
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CN117650053A (en) * | 2024-01-30 | 2024-03-05 | 天津正新光电科技有限公司 | Preparation method of silicon carbide packaging heat sink |
CN117650053B (en) * | 2024-01-30 | 2024-05-17 | 天津正新光电科技有限公司 | Preparation method of silicon carbide packaging heat sink |
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