CN113921376A - Silicon-based GaN film and epitaxial growth method thereof - Google Patents

Silicon-based GaN film and epitaxial growth method thereof Download PDF

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CN113921376A
CN113921376A CN202111004389.3A CN202111004389A CN113921376A CN 113921376 A CN113921376 A CN 113921376A CN 202111004389 A CN202111004389 A CN 202111004389A CN 113921376 A CN113921376 A CN 113921376A
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substrate
growing
epitaxial growth
silicon
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马金榜
张雅超
李一帆
姚一昕
张进成
马佩军
马晓华
郝跃
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Xidian University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • 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
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    • H01L21/02538—Group 13/15 materials
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    • H01—ELECTRIC ELEMENTS
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    • 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
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Abstract

The invention relates to a silicon-based GaN film and an epitaxial growth method thereof, wherein the epitaxial growth method comprises the following steps: s1, introducing trimethylaluminum and ammonia gas into the reaction chamber, and pretreating the Si substrate at the target temperature and the target gas flow rate; s2, epitaxially growing an AlN nucleating layer on the pretreated Si substrate; s3, growing an AlGaN buffer layer on the AlN nucleating layer; and S4, growing a GaN layer on the AlGaN buffer layer. The epitaxial growth method comprises the steps of pretreating a Si substrate, epitaxially growing an epitaxial layer, wherein the pretreatment can protect the Si substrate, so that the surface of the Si substrate is smoother, the migration of Al atoms in the deposition process of an AlN nucleating layer is facilitated, the Al atoms can reach a balance position more easily, the AlN nucleating layer is more prone to growth in a two-dimensional mode at the moment, the epitaxial layer on the AlN nucleating layer is more prone to growth in the two-dimensional mode, the dislocation extension is prevented, the obtained epitaxial layer is smoother, and the quality of an epitaxial GaN crystal is improved.

Description

Silicon-based GaN film and epitaxial growth method thereof
Technical Field
The invention belongs to the technical field of semiconductor materials, and particularly relates to a silicon-based GaN film and an epitaxial growth method thereof.
Background
GaN, a typical representative of wide bandgap semiconductors, has been widely studied in recent decades due to its unique advantages of wide bandgap, large breakdown field strength, and good radiation resistance. However, homoepitaxy of GaN has been difficult to be applied commercially in large scale because of the expensive homoepitaxial substrate, and heteroepitaxy of GaN on Si has the advantages of low cost, compatibility with the conventional Si process, etc., but there are many challenges in Si-based GaN due to the larger lattice mismatch and thermal mismatch between the Si substrate and GaN, such as high dislocation density, large wafer warpage, and thermal gradient on the wafer, etc.
To address the above challenges, researchers have proposed many buffer layer structures, such as low temperature AlN, high temperature AlN, graded AlGaN layers, etc., which greatly improve the quality of GaN by introducing compressive stress in GaN.
However, the dislocation density of Si-based GaN and the warpage of the wafer are still much greater than for sapphire and SiC substrates commonly used for GaN, which limits further applications of GaN-based devices.
Disclosure of Invention
In order to solve the above problems in the prior art, the present invention provides a silicon-based GaN thin film and an epitaxial growth method thereof. The technical problem to be solved by the invention is realized by the following technical scheme:
the embodiment of the invention provides an epitaxial growth method of a silicon-based GaN film, which comprises the following steps:
s1, introducing trimethylaluminum and ammonia gas into the reaction chamber, and pretreating the Si substrate at the target temperature and the target gas flow rate;
s2, epitaxially growing an AlN nucleating layer on the pretreated Si substrate;
s3, growing an AlGaN buffer layer on the AlN nucleating layer;
and S4, growing a GaN layer on the AlGaN buffer layer.
In one embodiment of the present invention, the target temperature is 1190-1210 ℃.
In one embodiment of the invention, the target temperature is 1200 ℃.
In one embodiment of the present invention, the target gas flow rate of trimethylaluminum is 180-.
In one embodiment of the present invention, the target gas flow rate of the ammonia gas is 1300-.
In one embodiment of the present invention, step S2 includes:
s21, introducing trimethylaluminum and ammonia gas into the reaction chamber by utilizing a metal organic compound chemical vapor deposition method, and growing AlN on the pretreated Si substrate under the conditions that the flow rate of the trimethylaluminum is 240-;
s22, introducing trimethylaluminum and ammonia gas into the reaction chamber by using a metal organic compound chemical vapor deposition method, and growing AlN on the pretreated first AlN nucleation layer under the conditions that the flow rate of the trimethylaluminum is 190-.
In one embodiment of the present invention, step S3 includes:
s31, growing a first AlGaN layer on the AlN nucleating layer;
and S32, growing a second AlGaN layer on the first AlGaN layer, wherein the first AlGaN layer and the second AlGaN layer form a step-change AlGaN buffer layer.
In an embodiment of the present invention, the step between S1 and S2 further includes the steps of:
and preparing pre-paved aluminum on the Si substrate.
In one embodiment of the present invention, the preparation conditions of the pre-paved aluminum are as follows: the temperature of the reaction chamber is 1080-.
Another embodiment of the present invention provides a silicon-based GaN thin film grown by the epitaxial growth method described in the above embodiment.
Compared with the prior art, the invention has the beneficial effects that:
the epitaxial growth method of the invention firstly pretreats the Si substrate, then epitaxially grows the epitaxial layer on the Si substrate, the pretreatment can protect the Si substrate, so that the surface of the Si substrate is smoother, the migration of Al atoms in the deposition process of the AlN nucleating layer is facilitated, and the Al atoms can reach a balance position more easily, so that the epitaxial layer on the Si substrate is converted into a two-dimensional growth mode more easily, the number of crystal boundaries caused by the formation and combination of three-dimensional islands can be reduced, the extension of dislocation is prevented, the obtained epitaxial layer is smoother, and the quality of the epitaxial GaN crystal is improved.
Drawings
FIG. 1 is a schematic flow chart of a method for epitaxial growth of a silicon-based GaN thin film according to an embodiment of the invention;
FIGS. 2 a-2 f are schematic process diagrams of a method for epitaxial growth of a silicon-based GaN thin film according to an embodiment of the invention;
FIGS. 3 a-3 b are schematic surface topography diagrams of a Si substrate before and after pretreatment according to an embodiment of the present invention;
FIGS. 4 a-4 b are XRD contrast diagrams of GaN grown on Si substrate before and after pretreatment according to an embodiment of the present invention;
FIG. 5 is a schematic flow chart illustrating another method for epitaxial growth of a silicon-based GaN film according to an embodiment of the invention;
fig. 6 is a schematic structural diagram of another silicon-based GaN thin film according to an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Example one
Referring to fig. 1 and fig. 2a to fig. 2f, fig. 1 is a schematic flow chart of an epitaxial growth method of a silicon-based GaN film according to the present invention, and fig. 2a to fig. 2f are schematic process diagrams of an epitaxial growth method of a silicon-based GaN film according to the present invention, the epitaxial growth method including the steps of:
and S1, introducing trimethylaluminum and ammonia gas into the reaction chamber, and pretreating the Si substrate 1 at the target temperature and the target gas flow rate.
Specifically, the material of the Si substrate 1 includes P-type Si (111), the thickness is 500-900 μm, the size is 2-6 inches, and the resistance is greater than 6000 Ω · cm, for example, the Si substrate 1 may be a P-type Si sheet with a large resistance, the thickness is 525 μm, 4 inches, and the resistance is greater than 6000 Ω · cm, as shown in fig. 2 a. In the embodiment, the Si sheet with the crystal direction of 111 is selected, so that the Ga surface can grow on the substrate, and the quality of a subsequent growing material is ensured.
The Si substrate 1 is cleaned and thermally cleaned before being subjected to the pretreatment.
The method for cleaning the Si substrate 1 includes: soaking the Si substrate in 20% HF acid solution for 60s, and then soaking in H2O2Alcohol and acetone washes and finally a rinse with running deionized water for 60 s.
The method for thermally cleaning the Si substrate 1 is: and putting the cleaned substrate into a low-pressure MOCVD reaction chamber, introducing hydrogen, raising the temperature to 1000 ℃, controlling the pressure of the reaction chamber to be 40Torr, and carrying out heat treatment on the substrate in a hydrogen atmosphere for 3 min.
The method for pretreating the Si substrate 1 includes: after the cleaning stage, the temperature of the reaction chamber, i.e. the target temperature, is raised to 1190-3The gas path enables the target gas flow to be 180 sccm and 1300 sccm respectively and 1400sccm, and the Si substrate 1 is pretreated. In one embodiment, the chamber temperature is 1200 deg.C, TMAl flow is 190sccm, NH3The flow rate is 1400sccm, and the pretreatment time is 10-20 min.
Referring to fig. 3 a-3 b, fig. 3 a-3 b are schematic surface morphologies of a substrate before and after a Si substrate is pretreated according to an embodiment of the present invention, where fig. 3a is a surface morphology of a substrate without pretreatment, and fig. 3b is a surface morphology of a substrate after pretreatment. Comparing fig. 3a and fig. 3b, it can be seen that the roughness of the substrate surface is greatly improved, the undulation of the processed substrate surface is very small, the surface is pm-order and flat, which is beneficial to the deposition of the pre-laid aluminum and AlN nucleation layer, and the quality of GaN can be further improved; in contrast, the untreated substrate surface had many pits and had large surface undulations, with surface roughness at 4-6nm, which affected the uniformity of the pre-laid aluminum and the deposition of the AlN nucleation layer.
And S2, epitaxially growing an AlN nucleating layer (3) on the pretreated Si substrate (1).
S21, epitaxially growing a first AlN nucleation layer 31 on the Si substrate 1, see fig. 2 b.
Specifically, the MOCVD method is used to simultaneously open trimethyl aluminum (TMAl) and NH3The air passage, adjusting the flow rate of TMAl to 240-3The flow rate is 3800-.
In one particular embodiment, the growth conditions of the first AlN nucleation layer 31 are: TMAl flow rate of 260sccm, NH3The flow rate is 4000sccm, the growth temperature is 900 ℃, the growth time is 60min, and the thickness of the formed first AlN nucleation layer 31 is 30 nm.
S22, epitaxially growing a second AlN nucleation layer 32 on the first AlN nucleation layer 31, see fig. 2 c.
Specifically, the temperature of the reaction chamber is raised to 1200-.
In one embodiment, of the second AlN nucleation layer 32The growth conditions were: TMAl flow rate of 190sccm, NH3The flow rate is 1400sccm, the growth temperature is 1210 ℃, the growth time is 60min, and the thickness of the formed second AlN nucleation layer 32 is 170 nm.
And S3, growing an AlGaN buffer layer (4) on the AlN nucleating layer (3).
S31, a first AlGaN layer 41 is prepared on the second AlN nucleation layer 32, see fig. 2 d.
Specifically, the temperature of the reaction chamber is lowered to 1140-3The flow rate is 190-.
In one embodiment, the first AlGaN layer 41 is grown under the conditions of a chamber temperature of 1150 ℃, TMAl, TMGa, NH3The flow rates are 190sccm,10sccm and 2700sccm respectively, the thickness of the grown first AlGaN layer 41 is 350nm, and the mass fraction of the Al component is 35%.
S32, a second AlGaN layer 42 is prepared on the first AlGaN layer 41, see fig. 2 e.
Specifically, the temperature of the reaction chamber is kept at 1140-1160 ℃, and TMAl, TMGa and NH are adjusted3The flow rate is 160-170sccm,20sccm,2920sccm-3580sccm respectively, and AlGaN with the thickness of 390-410nm is grown to form the second AlGaN layer 42 with the Al component mass fraction of 70-80%.
In one embodiment, the growth conditions for second AlGaN layer 42 are: the temperature of the reaction chamber is 1150 ℃, TMAl, TMGa and NH3The flow rates are respectively 162sccm,20sccm and 3000sccm, the thickness of the grown second AlGaN layer 42 is 400nm, and the mass fraction of the Al component is 75%.
Further, the first AlGaN layer 41 and the second AlGaN layer 42 together form the graded AlGaN buffer layer 4.
S4, growing a GaN layer (5) on the AlGaN buffer layer (3), see fig. 2 f.
Specifically, the temperature of the reaction chamber is kept constant, the TMAl source is closed, and TMGa and NH are adjusted3The flow rate is 190-,a GaN buffer layer 5 is formed.
In a specific embodiment, the growth conditions of the GaN buffer layer 5 are: the temperature of the reaction chamber is 1150 ℃, the TMGa flow is 192sccm, NH3The flow rate was 9000sccm, and the thickness of the GaN buffer layer 5 was 1 μm.
Referring to fig. 4 a-4 b, fig. 4 a-4 b are XRD contrast graphs of GaN grown on Si substrate before and after pretreatment according to an embodiment of the present invention, fig. 4a is a rocking curve of threading dislocation density, and fig. 4b is a rocking curve of edge dislocation density.
In fig. 4a, (002) full width at half maximum represents the density of threading dislocations, and it can be seen that the substrate without pretreatment is wider than that using the pretreated substrate, indicating that pretreatment is advantageous for threading dislocation reduction. In fig. 4b, (102) represents the edge dislocation density, and it can be seen that the substrate without pretreatment is significantly wider and the pretreatment is much smaller, indicating that pretreatment of the substrate can significantly reduce the edge dislocation density. And the lower the screw dislocation and the blade dislocation, the better the crystal quality, so the GaN screw dislocation and the blade dislocation which are grown on the pretreated Si substrate have lower density, and the GaN crystal has better quality.
In the embodiment, the Si substrate is pretreated, then the epitaxial layer is epitaxially grown on the Si substrate, the pretreatment can protect the Si substrate, so that the surface of the Si substrate is smoother, the migration of Al atoms in the deposition process of the AlN nucleation layer is facilitated, and the Al atoms can reach the equilibrium position more easily.
Example two
On the basis of the first embodiment, please refer to fig. 2f, and fig. 2f is a schematic structural diagram of a silicon-based GaN film prepared by the above epitaxial growth method, wherein the silicon-based GaN film comprises a Si substrate 1, an AlN nucleation layer 3, an AlGaN graded layer 4, and a GaN buffer layer 5, which are sequentially stacked.
Wherein, the Si substrate 1 is a pretreated substrate with surface fluctuation in pm magnitude; the AlN nucleation layer 3 includes a first AlN nucleation layer 31 and a second AlN nucleation layer 32; the AlGaN graded layer 4 includes a first AlGaN layer 41 and a second AlGaN layer 42. For specific structural parameters of each layer of the device, please refer to embodiment one, which is not described in detail herein.
The Si substrate 1 of this embodiment is a pretreated substrate with a surface fluctuating in pm order, which is beneficial to the migration of Al atoms in the deposition process of the AlN nucleation layer later and makes it easier to reach an equilibrium position, at this time, the reactive atoms and the sites of the substrate grow in a two-dimensional mode, i.e., the AlN nucleation layer is easier to be converted into a two-dimensional growth mode, each epitaxial layer on the AlN nucleation layer is also more prone to be converted into a two-dimensional growth mode, and thus the number of grain boundaries caused by the formation and merging of three-dimensional islands can be reduced, which is beneficial to blocking the extension of dislocations, the resulting nucleation layer and epitaxial layer are also smoother, and the two-dimensional growth mode also more effectively reduces the dislocation density, which is beneficial to improving the quality of the epitaxial GaN crystal.
EXAMPLE III
On the basis of the first embodiment, please refer to fig. 5, and fig. 5 is a schematic flow chart of another method for epitaxial growth of a silicon-based GaN film according to an embodiment of the present invention. The preparation method comprises the following steps:
and S1, introducing trimethylaluminum and ammonia gas into the reaction chamber, and pretreating the Si substrate 1 at the target temperature and the target gas flow rate.
S2, preparing pre-laid aluminum 2 on the Si substrate 1.
Specifically, the temperature of the reaction chamber is raised to 1080-.
In one embodiment, pre-plated aluminum 2 is prepared at a chamber temperature of 1085 deg.C and TMAl flow of 20 sccm.
And S3, epitaxially growing an AlN nucleating layer 3 on the pretreated Si substrate 1.
And S4, growing an AlGaN buffer layer 4 on the AlN nucleating layer 3.
And S5, growing a GaN layer 5 on the AlGaN buffer layer 3.
Please refer to embodiment i for the preparation processes of steps S1, S3-S6, which are not described in detail in this embodiment.
Referring to fig. 6, fig. 6 is a schematic structural diagram of another silicon-based GaN film according to an embodiment of the present invention.
The silicon-based GaN film comprises a Si substrate 1, pre-laid aluminum 2, an AlN nucleating layer 3, an AlGaN graded layer 4 and a GaN buffer layer 5 which are sequentially stacked. For specific structural parameters of each layer of the device, please refer to the preparation methods of the first embodiment and the third embodiment, which are not described herein again.
In this embodiment, pre-laid aluminum is disposed between the Si substrate and the AlN nucleation layer, which not only can improve the growth effect of the nucleation layer, but also can improve the crystal quality of GaN, thereby improving the device performance.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.

Claims (10)

1. An epitaxial growth method of a silicon-based GaN film is characterized by comprising the following steps:
s1, introducing trimethylaluminum and ammonia gas into the reaction chamber, and pretreating the Si substrate (1) at the target temperature and the target gas flow rate;
s2, epitaxially growing an AlN nucleating layer (3) on the pretreated Si substrate (1);
s3, growing an AlGaN buffer layer (4) on the AlN nucleating layer (2);
and S4, growing a GaN layer (5) on the AlGaN buffer layer (3).
2. The method as claimed in claim 1, wherein the target temperature is 1190-1210 ℃.
3. The method of epitaxial growth of silicon-based GaN thin films according to claim 2, wherein the growth temperature is 1200 ℃.
4. The method as claimed in claim 1, wherein the flow rate of the target gas of trimethylaluminum is 180-190 sccm.
5. The method as claimed in claim 1, wherein the target gas flow rate of the ammonia gas is 1300-1400 sccm.
6. The method for epitaxial growth of a silicon-based GaN film according to claim 1, wherein step S2 includes:
s21, introducing trimethylaluminum and ammonia gas into the reaction chamber by utilizing a metal organic compound chemical vapor deposition method, and growing AlN on the pretreated Si substrate (1) under the conditions that the flow rate of the trimethylaluminum is 240-;
s22, introducing trimethylaluminum and ammonia gas into the reaction chamber by using a metal organic compound chemical vapor deposition method, and growing AlN on the pretreated first AlN nucleation layer (31) under the conditions that the flow rate of the trimethylaluminum is 190-.
7. The method for epitaxial growth of a silicon-based GaN film according to claim 1, wherein step S3 includes:
s31, growing a first AlGaN layer (41) on the AlN nucleating layer (3);
s32, growing a second AlGaN layer (42) on the first AlGaN layer (41), wherein the first AlGaN layer (41) and the second AlGaN layer (42) form a step AlGaN buffer layer (4).
8. The method of epitaxial growth of Si-based GaN films according to claim 1, further comprising, between steps S1 and S2, the steps of:
preparing pre-laid aluminum (2) on the Si substrate (1).
9. The epitaxial growth method of GaN-based films on silicon according to claim 8, wherein the preparation conditions of the pre-laid aluminum (2) are: the temperature of the reaction chamber is 1080-.
10. A silicon-based GaN thin film grown by the epitaxial growth method according to any one of claims 1 to 9.
CN202111004389.3A 2021-08-30 2021-08-30 Silicon-based GaN film and epitaxial growth method thereof Pending CN113921376A (en)

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