CN106486339B - Preparation method of GaN film - Google Patents

Preparation method of GaN film Download PDF

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CN106486339B
CN106486339B CN201510532696.7A CN201510532696A CN106486339B CN 106486339 B CN106486339 B CN 106486339B CN 201510532696 A CN201510532696 A CN 201510532696A CN 106486339 B CN106486339 B CN 106486339B
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epitaxial
gan film
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CN106486339A (en
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彭昀鹏
王刚宁
戴执中
杨广立
王蛟
孙泓
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Semiconductor Manufacturing International Shanghai Corp
Semiconductor Manufacturing International Beijing Corp
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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
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/301—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C23C16/303—Nitrides
    • 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
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
    • H01L22/20—Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps
    • H01L22/26—Acting in response to an ongoing measurement without interruption of processing, e.g. endpoint detection, in-situ thickness measurement

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Abstract

The invention provides a preparation method of a GaN film, which comprises the following steps: providing a semiconductor substrate; putting the semiconductor substrate into an epitaxial cavity, introducing a gallium source and a nitrogen source into the epitaxial cavity, extending a GaN film on the surface of the semiconductor substrate, and monitoring the reflectivity of the film in the epitaxial process; when the reflectivity of the GaN film rises to a first preset value, stopping introducing a gallium source into the epitaxial cavity, introducing silane and a nitrogen source into the epitaxial cavity, and etching the GaN film by the silane; and when the reflectivity of the GaN film is reduced to a second preset value, stopping introducing the silane into the epitaxial cavity, introducing a gallium source and a nitrogen source into the epitaxial cavity, and continuing to epitaxially grow the GaN film on the semiconductor substrate. According to the invention, the GaN film is etched by adopting silane, so that dislocation defects generated during epitaxial growth of the GaN film can be effectively reduced, carrier capture traps in crystals are reduced, and the performance of the GaN film is improved.

Description

Preparation method of GaN film
Technical Field
The invention relates to the technical field of semiconductor manufacturing, in particular to a preparation method of a GaN film.
Background
The GaN material is a direct band gap wide band gap semiconductor material, has a continuously variable direct band gap between 1.9 and 6.2eV, and has excellent physical and chemical stability, high saturated electron drift velocity, high breakdown field strength, high thermal conductivity and other superior performances, so that the GaN material has important application in the preparation of short-wavelength semiconductor photoelectronic devices, high-frequency, high-voltage and high-temperature microelectronic devices and the like, and is used for manufacturing blue, purple and ultraviolet band light-emitting devices, detecting devices, high-temperature, high-frequency and high-field high-power devices, field emission devices, anti-radiation devices, piezoelectric devices and the like.
There are many methods for growing GaN materials, such as Metal Organic Chemical Vapor Deposition (MOCVD), high temperature and high pressure composite GaN single crystals, Molecular Beam Epitaxy (MBE), sublimation, and Hydride Vapor Phase Epitaxy (HVPE). The growth of GaN single crystals is very difficult due to the physical property limitations of GaN materials, and has not been put into practical use. GaN can only be grown on foreign substrates such as sapphire, silicon, etc.
In the epitaxial growth process, dislocation defects and the like exist in the GaN thin film due to lattice mismatch and thermal mismatch between the GaN thin film and a heterogeneous substrate, so that large stress exists in the GaN thin film, and the performance of a GaN-based device is difficult to improve. In addition, the huge stress causes the GaN thick film and the foreign substrate to be broken into pieces, and thus cannot be applied. Therefore, the defects in the GaN thick film are reduced or eliminated, and the method is an important solution for effectively exerting the potential of the GaN material.
Disclosure of Invention
The invention aims to provide a preparation method of a GaN film, which reduces defects in the GaN film and improves the performance of the GaN film.
In order to solve the above technical problems, the present invention provides a method for preparing a GaN thin film, comprising:
providing a semiconductor substrate;
putting the semiconductor substrate into an epitaxial cavity, introducing a gallium source and a nitrogen source into the epitaxial cavity, extending a GaN film on the surface of the semiconductor substrate, and monitoring the reflectivity of the film in the epitaxial process;
when the reflectivity of the GaN film rises to a first preset value, stopping introducing a gallium source into the epitaxial cavity, introducing silane and a nitrogen source into the epitaxial cavity, and etching the GaN film by the silane;
and when the reflectivity of the GaN film is reduced to a second preset value, stopping introducing the silane into the epitaxial cavity, introducing a gallium source and a nitrogen source into the epitaxial cavity, and continuing to epitaxially grow the GaN film on the semiconductor substrate.
Optionally, after the reflectivity of the GaN film is reduced to the second predetermined value and before the gallium source and the nitrogen source are introduced into the epitaxial cavity, an aluminum source, a gallium source and a nitrogen source are introduced into the epitaxial cavity, so as to form Al on the surface of the GaN filmxGa(1-x)And (6) N thin films.
Optionally, when said Al isxGa(1-x)And stopping introducing an aluminum source into the epitaxial cavity when the reflectivity of the N film rises to the first preset value, introducing a gallium source and a nitrogen source into the epitaxial cavity, and epitaxially growing a GaN film on the surface of the AlxGa (1-x) N film.
Optionally, the AlxGa(1-x)The thickness of the N thin film is 10nm-50 nm.
Alternatively, x is between 0 and 1.
Optionally, the second predetermined value is 1/3-1/2 of the first predetermined value.
Optionally, the first predetermined value is greater than or equal to 16.
Optionally, the flow rate of the silane introduced is 0.1sccm-1.0 sccm.
Optionally, the nitrogen source is ammonia gas.
Optionally, the temperature in the epitaxial chamber is 300 ℃ to 500 ℃.
In the preparation method of the GaN film, silane is introduced into the epitaxial cavity when the reflectivity of the GaN film rises to a first preset value in the epitaxial process, the silane etches the surface of the GaN film, so that the reflectivity of the GaN film is reduced, and dislocation defects and the like in the GaN film can be removed in the etching process. And then, when the reflectivity is reduced to a second preset value, continuing to extend the GaN film on the semiconductor substrate, wherein the damage of etching can be repaired in the extending process. According to the invention, dislocation defects generated during epitaxial growth of the GaN film can be effectively reduced, carrier capture traps in the crystal are reduced, and the performance of the GaN film is improved.
Drawings
FIG. 1 is a schematic view of a process for growing a GaN thin film in the prior art;
FIG. 2 is a flow chart of a GaN thin film fabrication method of the invention;
FIG. 3 is a schematic structural view of a first epitaxial GaN film performed in an embodiment of the method for preparing a GaN film according to the invention;
FIG. 4 is a schematic structural diagram of a silane-etched GaN film in an embodiment of the GaN film preparation method of the invention;
FIG. 5 shows Al growth in an embodiment of a method for fabricating a GaN thin film according to the inventionxGa(1-x)A schematic structural diagram of N;
FIG. 6 is a schematic structural view of a second epitaxial GaN film performed in one embodiment of the method for manufacturing a GaN film of the invention;
FIG. 7 is a reflectance curve during epitaxy in an embodiment of a method for fabricating a GaN thin film according to the invention.
Detailed Description
The inventor researches the growth process of the GaN material in the prior art to find that the reflectivity value of the GaN film is related to the lattice structure of the GaN film, and different lattice structures correspond to different reflectivity values. Referring to fig. 1, a GaN material is epitaxially grown on a foreign substrate 1, and a commonly adopted method is to grow a GaN buffer layer 2 on the substrate 1, perform high-temperature annealing on the buffer layer 2, epitaxially grow GaN by introducing a Ga source and an N source, obtain a 3D island-shaped GaN structure 3 first, and then grow a two-dimensional GaN film 4 sequentially, so as to obtain a GaN film 4 with a certain size on the foreign substrate 1 by epitaxy. The reflectance curve of the substrate surface during epitaxy in fig. 1, the reflectance value of the final GaN film, shows that GaN has formed a 2D film on the substrate, but the defect density and crystalline quality in GaN film 4 are not ideal. The inventors have conducted intensive studies to find that a high-performance GaN thin film can be obtained if dislocation defects of a GaN material during growth can be reduced.
The method for fabricating a GaN thin film according to the present invention will be described in more detail with reference to the schematic drawings, in which preferred embodiments of the present invention are shown, it being understood that those skilled in the art can modify the present invention described herein while still achieving the advantageous effects of the present invention. Accordingly, the following description should be construed as broadly as possible to those skilled in the art and not as limiting the invention.
The core idea of the invention is that a semiconductor substrate is placed in an epitaxial cavity to grow a GaN film, when the reflectivity of the GaN film rises to a first preset value, namely the GaN film grows to be a 2D material, the introduction of a gallium source into the epitaxial cavity is stopped, silane is introduced into the epitaxial cavity, the silane can etch the GaN film, so that the reflectivity of the GaN film is reduced, and dislocation defects and the like in the GaN film can be removed through the etching of the silane. And then, when the reflectivity of the GaN film is reduced to a second preset value, stopping etching. And then, continuously introducing a gallium source and a nitrogen source, and extending a GaN film on the semiconductor substrate, wherein the etching damage part can be repaired in the extending process. Therefore, the invention can effectively reduce dislocation defects generated during epitaxial growth of the GaN film, reduce carrier capture traps in the crystal and improve the performance of the GaN film.
A flowchart of a method for manufacturing a GaN thin film according to the present invention is shown with reference to fig. 2, and the steps of the method for manufacturing a GaN thin film will be described in detail below with reference to fig. 3 to 7.
Referring to fig. 2, the steps of the method for fabricating the GaN thin film include;
step S1 is performed, and referring to fig. 3, a semiconductor substrate 10 is provided, the semiconductor substrate 10 being a sapphire substrate, a silicon carbide substrate, or the like.
Step S2 is executed, and with continued reference to fig. 3, the semiconductor substrate 10 is placed in an epitaxial chamber, and the epitaxial chamber is subjected to pressure reduction and temperature rise operations, so as to raise the temperature of the epitaxial chamber to 300 ℃ -500 ℃. Generally, a buffer layer (not shown) is grown on the surface of the semiconductor substrate 10, and a high temperature annealing process is performed along with the buffer layer to weaken the lattice mismatch between the semiconductor substrate 10 and the buffer layer, thereby facilitating the growth of the GaN film. And then, introducing a gallium source and a nitrogen source into the epitaxial cavity, and performing a first epitaxial process of the GaN film to form a GaN film 20 on the surface of the semiconductor substrate. Wherein the nitrogen source is ammonia gas. The epitaxial chamber is provided with a laser fiber and a laser probe, and laser is applied to the surface of the semiconductor substrate 1, and the reflected light from the semiconductor substrate 10 is collected by the laser probe, and the reflectance on the surface of the semiconductor substrate 10 is obtained from the intensity relationship between the emitted light and the reflected light of the laser. In the epitaxial growth process on the semiconductor substrate 10, the reflectivity on the surface of the semiconductor substrate 10 is monitored in real time, so that the reflectivity of the grown material is obtained, and the reflectivity curve of the GaN in the epitaxial process is obtained, which can be used for monitoring the epitaxial growth condition. After the gallium source and the nitrogen source are introduced, a 3D island-shaped GaN crystal is firstly formed on the buffer layer structure, and then a 2D film GaN is formed. Referring correspondingly to fig. 7, after forming the buffer layer on the semiconductor substrate 10, the reflectivity of the surface of the semiconductor substrate 10 rises, indicating that a smoother buffer layer has been created. Then, a high temperature annealing process is performed, and the emissivity is reduced. After the gallium source and the nitrogen source are introduced, the reflectivity of the substrate 10 gradually rises, which shows that the GaN forms a 2D film through the 3D island-shaped structure.
Step S3 is performed, and referring to fig. 4, when the reflectivity of the GaN thin film 20 rises to a first predetermined value, as shown by R1 in fig. 7, it indicates that the GaN thin film has formed a thin film structure with better flatness on the semiconductor substrate 10. The first predetermined value R1 is a constant value of the GaN film, and is different according to the measured values of different devices, for example, the first predetermined value R1 is a constant of 16 or more. At this time, stopping introducing the gallium source into the epitaxial cavity, introducing silane and a nitrogen source into the epitaxial cavity, etching the GaN film 20 by the silane, forming a pit on the GaN film 20, and reducing the reflectivity of the GaN film 20. In the process of etching the GaN thin film 20 by using silane, dislocation defects and the like on the surface of the GaN thin film 20 can be removed, and carrier capture traps in the crystal are reduced. In this embodiment, the silane etching rate is positively correlated to the introduced flow rate, and when the silane flow rate is increased, the etching rate is too fast, so that the silane flow rate is 0.1sccm to 1.0sccm, preferably 0.1sccm, to avoid the over-etching phenomenon.
Referring to fig. 7, as the etching proceeds, the reflectivity of the GaN thin film 20 gradually decreases, and when the reflectivity of the GaN thin film 20 decreases to the second predetermined value R2, an aluminum source, a gallium source and a nitrogen source are introduced into the epitaxial cavity, so as to form Al on the surface of the GaN thin film 20xGa(1-x)N film 30, as shown with reference to fig. 5. The Al isxGa(1-x)The epitaxial growth of the N-film 30 can repair damage such as pits generated during the silane etching process. Generally, the second predetermined value R2 is set to 1/3-1/2 of the first predetermined value R1. In this example, the Al is formedxGa(1-x)The thickness of the N thin film is 10nm-50 nm. It should be noted that x is between 0 and 1, that is, when x is 0, the Al is presentxGa(1-x)The N film is a GaN film, that is, damage to the GaN film 20 may be repaired without introducing an aluminum source. However, the inventors have conducted trial and error to find that x>0, i.e. Al containing aluminumxGa(1-x)N film 30 ratio to Al without aluminumxGa(1-x)The N thin film 30 has better repair properties for GaN.
Step S4 is executed, referring to FIG. 7, the AlxGa(1-x)During the growth of the N film 30, the reflectivity of the surface of the semiconductor substrate 10 gradually rises when the AlxGa(1-x)And stopping introducing an aluminum source into the epitaxial cavity when the reflectivity of the N film 30 rises to the first preset value R1, introducing a gallium source and a nitrogen source into the epitaxial cavity, and performing the second GaN epitaxy process to epitaxially grow the GaN film 40 on the semiconductor substrate 10. It can be understood that, since there is an interface between the semiconductor substrate 10 and the buffer layer, and there is also an interface between the GaN thin film 40 and the buffer layer, during the reflectivity test of the GaN thin film 40, the laser light will form interference between the two interfaces, and the periodic occurrence of interference is constructive and destructive, so that the reflectivity has periodic oscillation as shown in fig. 7. Wherein the oscillation period is related to the thickness of the GaN thin film 40, so that the GaN thin film can be obtained according to the oscillation periodThe thickness of the film.
In the case of the GaN thin film 40 that is epitaxially grown for the second time, since the GaN thin film 20 having few dislocation defects is formed in the substrate to be grown, dislocations are not generated in the GaN thin film 40 during the second epitaxy process, and the performance of the formed GaN thin film 40 is improved. In addition, the flow rates of the nitrogen source introduced in the process of extending the GaN and the nitrogen source introduced in the process of etching the GaN film are kept unchanged, and the nitrogen source protects the GaN in the etching process so as to avoid the phenomenon of over-etching.
In conclusion, according to the preparation method of the GaN film, the GaN film is etched through the silane, so that dislocation defects generated during epitaxial growth of the GaN film can be effectively reduced, carrier capture traps in crystals are reduced, and the performance of the GaN film is improved.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims (7)

1. A method for preparing a GaN thin film is characterized by comprising the following steps:
providing a semiconductor substrate;
putting the semiconductor substrate into an epitaxial cavity, introducing a gallium source and a nitrogen source into the epitaxial cavity, extending a GaN film on the surface of the semiconductor substrate, and monitoring the reflectivity of the film in the epitaxial process;
when the reflectivity of the GaN film rises to a first preset value, stopping introducing a gallium source into the epitaxial cavity, introducing silane and a nitrogen source into the epitaxial cavity, and etching the GaN film by the silane;
and when the reflectivity of the GaN film is reduced to a second preset value, stopping introducing the silane into the epitaxial cavity, introducing a gallium source and a nitrogen source into the epitaxial cavity, and continuing to epitaxially grow the GaN film on the semiconductor substrate, wherein the second preset value is 1/3-1/2 of the first preset value.
2. The method of claim 1, wherein after the reflectivity of the GaN film decreases to the second predetermined value, and before the gallium source and the nitrogen source are introduced into the epitaxial chamber, an aluminum source, a gallium source, and a nitrogen source are introduced into the epitaxial chamber to form Al on the surface of the GaN filmxGa(1-x)N film, x is between 0 and 1.
3. The method of claim 2, wherein when the reflectance of the AlxGa (1-x) N thin film increases to the first predetermined value, the introduction of the aluminum source into the epitaxial chamber is stopped, the gallium source and the nitrogen source are introduced into the epitaxial chamber, and the Al film is formed on the substratexGa(1-x)And epitaxially growing a GaN film on the surface of the N film.
4. The method of manufacturing a GaN thin film according to claim 3, wherein the Al isxGa(1-x)The thickness of the N thin film is 10nm-50 nm.
5. The method of claim 1, wherein the silane is introduced at a flow rate of 0.1sccm to 1.0 sccm.
6. The method of manufacturing a GaN film according to claim 1, wherein the nitrogen source is ammonia gas.
7. The method of fabricating a GaN film according to claim 1, wherein the temperature in the epitaxial chamber is 300 ℃ to 500 ℃.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005064204A (en) * 2003-08-11 2005-03-10 Toyoda Gosei Co Ltd Group iii nitride compound semiconductor light emitting device, and method for manufacturing gallium nitride (gan) substrate for use in device
CN1675746A (en) * 2002-07-11 2005-09-28 爱尔兰国家大学科克学院 Defect reduction in semiconductor materials
CN101431018A (en) * 2008-12-22 2009-05-13 武汉华灿光电有限公司 Method for gallium nitride film growth on graphic sapphire substrate
KR20110090576A (en) * 2010-02-04 2011-08-10 주식회사 엘지실트론 Method for manufacturing gallium nitride wafer
CN102754188A (en) * 2010-02-04 2012-10-24 Lg矽得荣株式会社 Method for manufacturing galium naitride wafer
CN104538282A (en) * 2014-12-17 2015-04-22 江苏能华微电子科技发展有限公司 Growing method of vertical structure power device epitaxial layer and power device

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1675746A (en) * 2002-07-11 2005-09-28 爱尔兰国家大学科克学院 Defect reduction in semiconductor materials
JP2005064204A (en) * 2003-08-11 2005-03-10 Toyoda Gosei Co Ltd Group iii nitride compound semiconductor light emitting device, and method for manufacturing gallium nitride (gan) substrate for use in device
CN101431018A (en) * 2008-12-22 2009-05-13 武汉华灿光电有限公司 Method for gallium nitride film growth on graphic sapphire substrate
KR20110090576A (en) * 2010-02-04 2011-08-10 주식회사 엘지실트론 Method for manufacturing gallium nitride wafer
CN102754188A (en) * 2010-02-04 2012-10-24 Lg矽得荣株式会社 Method for manufacturing galium naitride wafer
CN104538282A (en) * 2014-12-17 2015-04-22 江苏能华微电子科技发展有限公司 Growing method of vertical structure power device epitaxial layer and power device

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