CN115831719A - Preparation method of high-quality AlN thin film material on Si substrate - Google Patents

Preparation method of high-quality AlN thin film material on Si substrate Download PDF

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CN115831719A
CN115831719A CN202310052527.8A CN202310052527A CN115831719A CN 115831719 A CN115831719 A CN 115831719A CN 202310052527 A CN202310052527 A CN 202310052527A CN 115831719 A CN115831719 A CN 115831719A
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alumina
layer
alpha
transition layer
aln
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杨学林
沈波
陈正昊
吴俊慷
蔡子东
杨鸿才
郭富强
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Peking University
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Peking University
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Abstract

The invention discloses a preparation method of a high-quality AlN thin film material on a Si substrate, which takes Si (111) as the substrate and firstly forms an alumina layer on the surface of the substrate; then carrying out high-temperature treatment on the alumina layer to form an alpha-alumina transition layer or an AlON/alpha-alumina composite transition layer; and growing a high-quality AlN thin film on the alpha-alumina transition layer or the AlON/alpha-alumina composite transition layer. The invention utilizes the surface structure of the alpha-alumina to improve the orientation difference between crystal grains of the AlN nucleating layer, and takes the AlON as a good transition layer between the AlN nucleating layer and the alpha-alumina layer to realize the gradual change of the lattice constant and reduce the formation of defects. The alpha-alumina transition layer can balance stress and strain in the epitaxial growth process and reduce the warping of the epitaxial wafer; the screw dislocation density is effectively controlled, and the electric leakage of an electronic device is reduced; diffusion of Al into Si (111) substrates can also be reduced for radio frequency electronics, thereby reducing radio frequency losses.

Description

Preparation method of high-quality AlN thin film material on Si substrate
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a method for preparing an AlN thin film material by epitaxial growth on a Si substrate.
Background
Currently, si substrates have become one of the main substrates of choice for group III nitride epitaxial growth. The advantages of large size, low cost and mature preparation process of the Si substrate enable the III-group nitride material grown on the basis of the Si substrate to have excellent application prospect, and can be widely applied to application scenes such as power electronics, radio frequency electronics, light-emitting devices and the like.
However, both aluminum nitride (AlN) and gallium nitride (GaN) materials have huge lattice mismatch and thermal mismatch with Si substrates, and the lattice mismatch causes a large number of threading dislocations in the group III nitride epitaxial layer, and these high-density dislocations appear as leakage channels, non-radiative recombination centers, carrier traps in the materials, and also affect the composition uniformity of the ternary alloy, and finally have many adverse effects on electronic devices and optoelectronic devices. The thermal mismatch makes the surface of the III-nitride epitaxial layer easily generate cracks in the process of cooling, and the device preparation process cannot be carried out. In particular, si and Ga undergo a melting reaction at high temperature, gaN cannot be directly grown on a Si substrate, and it is currently most widely accepted to use AlN as a transition layer between Si and GaN, so that the GaN crystal quality is inevitably affected by the crystal quality of the underlying AlN. In summary, for epitaxial III-nitride materials on Si substrates, whether AlN, alGaN or GaN, it is necessary to first obtain a high quality Si substrate AlN thin film.
However, in addition to the above-mentioned huge lattice mismatch between AlN and Si, the surface mobility of Al atoms is weak in a Metal Organic Chemical Vapor Deposition (MOCVD) growth environment, and Al and Si may also react to some extent during the Si substrate Al pretreatment loop to destroy the surface flatness of the Si substrate, resulting in large crystal orientation difference of the nucleation layer, difficulty in achieving a flat surface, and difficulty in folding. These factors make AlN dislocation density obtained by conventional MOCVD growth processes very high and difficult to significantly reduce, and also affect the crystal quality of subsequent epitaxial layers such as AlGaN, gaN layers, eventually leading to unexpected performance of related device properties. Therefore, a new transition layer structure between the Si substrate and GaN is needed to improve the crystal quality. At present, there are studies reporting that Si and AlN are inserted with a layer of alumina (doi: 10.1016/j. Jcrysgro.2009.07.022) to try to improve the crystal quality of AlN and GaN. However, the improvement effect of the method on the crystal quality is very limited at present, mainly because the aluminum oxide layer is mostly in a polycrystalline or amorphous state, and the lattice structures and orientations of different areas of the aluminum oxide layer are different, and these differences are transmitted to the nucleation layer, so that the improvement effect of the aluminum oxide layer on the grain orientation of the nucleation layer is greatly reduced. Further optimization of the alumina transition layer is needed, and the growth of AlN on the transition layer is correspondingly adjusted, so that the crystal quality of AlN and GaN thin films is effectively improved.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method for realizing a high-quality AlN thin film by adopting an alpha-alumina transition layer on a Si substrate. The invention is realized by the following technical scheme:
a preparation method of a high-quality AlN thin film material on a Si substrate comprises the following steps:
1) Selecting a Si (111) substrate, and forming an alumina transition layer on the surface of the Si (111) substrate;
2) Carrying out high-temperature treatment on the alumina transition layer to form an alpha-alumina transition layer or an AlON/alpha-alumina composite transition layer;
3) And growing an AlN layer on the alpha-alumina transition layer or the AlON/alpha-alumina composite transition layer to obtain the high-quality AlN thin film.
In the step 1), the surface of the Si substrate selected by the invention is a (111) crystal face, and firstly, a layer of alumina is prepared on the surface of the Si (111) substrate to form an alumina transition layer.
Specifically, a layer of alumina may be grown on the surface of the Si (111) substrate using an Atomic Layer Deposition (ALD), molecular Beam Epitaxy (MBE), or Physical Vapor Deposition (PVD) method; it is also possible to grow a layer of Al on the Si (111) substrate surface using ALD, MBE or PVD methods and then oxidize the Al layer to alumina using thermal oxidation methods.
And 2) carrying out high-temperature treatment on the alumina transition layer to form the alpha-alumina transition layer.
Specifically, the aluminum oxide transition layer is subjected to high-temperature treatment by using a thermal annealing or laser annealing method, amorphous aluminum oxide is converted into an alpha-phase single crystal structure, and a uniform alpha-aluminum oxide (0001) crystal face is formed on the surface of the amorphous aluminum oxide, so that the alpha-aluminum oxide transition layer is obtained. Wherein alpha-alumina is the most stable phase of all alumina structures.
Preferably, the surface of the alpha-alumina transition layer is further subjected to nitridation treatment to obtain the AlON/alpha-alumina composite transition layer. The nitridation treatment is carried out for a long time at high temperature in a nitrogen-containing atmosphere, and an AlON structure is formed on the surface of the alpha-alumina transition layer to form an AlON/alpha-alumina composite transition layer.
Specifically, the alpha-alumina transition layer is subjected to high-temperature treatment by using a thermal annealing or laser annealing method in a nitrogen or ammonia atmosphere, and an AlON composite structure is formed on the surface to obtain the AlON/alpha-alumina composite transition layer.
Preferably, in the step 3), the PVD-AlN nucleation layer is grown by a PVD method, and then the AlN film is grown on the PVD-AlN nucleation layer by MOCVD, or the PVD-AlN nucleation layer is subjected to a high temperature treatment and then the AlN film is grown thereon by MOCVD.
In one embodiment of the present invention, the Si (111) substrate has a resistivity of 0.01 to 10000 ohm-cm.
In one embodiment of the invention, the thickness of the Si (111) substrate is 100-1500 μm.
In one embodiment of the invention, the thickness of the alumina transition layer in step 1) is 1-100 nm.
In a preferred embodiment of the present invention, the thickness of the α -alumina transition layer in step 2) is 1 to 100 nm.
In a preferred embodiment of the present invention, the thickness of the AlON/α -alumina composite transition layer in step 2) is 1 to 100 nm.
In a preferred embodiment of the present invention, the PVD-AlN nucleation layer has a thickness of 10-200 nm.
In a preferred embodiment of the invention, the PVD-AlN nucleation layer is processed at a high temperature of 1000-1300 ℃.
The invention has the beneficial effects that:
the invention adopts the alpha-alumina transition layer, wherein the surface structure of the alpha-alumina can improve the orientation difference among crystal grains of the AlN nucleating layer, and the alpha-alumina has the same surface structure with the sapphire, so that the growth process of the AlN on the sapphire substrate can be used for reference, and the crystal quality of the AlN is improved. Preferably, the surface of the alpha-alumina transition layer is subjected to nitridation treatment to form an AlON/alpha-alumina composite transition layer structure, and AlON can be used as a good transition layer between the AlN nucleating layer and the alpha-alumina layer, so that the gradual change of the lattice constant is realized, and the formation of defects is reduced. When an AlN epitaxial structure grows on the alpha-alumina transition layer or the AlON/alpha-alumina composite transition layer, the PVD-AlN nucleating layer is introduced, so that the crystal quality of AlN can be further improved. The alpha-alumina transition layer can balance stress and strain in the epitaxial growth process and reduce the warping of the epitaxial wafer. In particular, the threading dislocation density of the nitride grown on the α -alumina transition layer can be controlled relatively more effectively, thereby contributing to a reduction in leakage current of the electronic device. In addition, aiming at the application of the radio frequency electronic device, compared with the traditional Si substrate AlN growth process, the method avoids pre-Al-introducing treatment on the Si (111) substrate in the MOCVD growth process, and the diffusion of Al to the Si (111) substrate can be reduced due to the existence of the alpha-alumina layer, so that the radio frequency loss of the radio frequency device is reduced.
Drawings
FIG. 1 is a flow chart of a method for preparing an alpha-alumina transition layer on a Si substrate and regrowing an AlN thin film according to an embodiment of the invention.
FIG. 2 is a flow chart of a method for preparing an α -alumina transition layer on a Si substrate and regrowing an AlN thin film according to a second embodiment of the present invention.
FIG. 3 is a flow chart of a method for preparing an AlON/alpha-alumina composite transition layer on a Si substrate and regrowing an AlN thin film according to a third embodiment of the invention.
Detailed Description
The present invention will be described in further detail below by way of examples with reference to the accompanying drawings, but the embodiments of the present invention are not limited thereto.
Example one
Referring to fig. 1, a high quality AlN thin film material was prepared on a Si substrate by the following steps:
1) Selecting a Si (111) substrate having a resistivity <0.1 ohm cm and a thickness of 430-1000 μm;
2) Forming an alumina layer with a thickness of 1-100 nm on a Si (111) substrate by using an Atomic Layer Deposition (ALD) method, wherein the growth temperature is 100-500 ℃, and the Al source is trimethylaluminum (TMAl) or aluminum chloride (AlCl) 3 ) The O source is water (H) 2 O) or ozone (O) 3 )；
3) Carrying out high-temperature treatment on the aluminum oxide layer by using a thermal annealing or laser annealing method to ensure that the aluminum oxide layer generates structural transformation to form a single-crystal-phase alpha-aluminum oxide layer, wherein the high-temperature treatment temperature is 1000-1300 ℃ and the time is 1-5 min;
4) Depositing a PVD-AlN layer on the alpha-alumina layer at 500-1000 ℃ with the deposition thickness of 10-200 nm, and performing high-temperature treatment at 1000-1300 ℃;
5) And growing an AlN thin film on the PVD-AlN layer by using a metal organic chemical vapor phase epitaxy (MOCVD) method.
Example two
Referring to fig. 2, a high quality AlN thin film material was prepared on a Si substrate by the following steps:
1) Selecting a Si (111) substrate having a resistivity <0.1 ohm cm and a thickness of 430-1000 μm;
2) Forming an aluminum layer with the thickness of 1-100 nm on a Si (111) substrate by utilizing an Atomic Layer Deposition (ALD) method, wherein the growth temperature is 50-500 ℃, and an Al source is trimethyl aluminum (TMAl) or metallic aluminum (Al);
3) Oxidizing the aluminum layer into an aluminum oxide layer by using a thermal oxidation method, wherein the treatment temperature is 500-700 ℃;
4) Carrying out high-temperature treatment on the aluminum oxide layer by using a thermal annealing or laser annealing method to ensure that the aluminum oxide layer generates structural transformation to form a single-crystal-phase alpha-aluminum oxide layer, wherein the high-temperature treatment temperature is 1000-1300 ℃ and the time is 1-5 min;
5) Depositing a PVD-AlN layer on the alpha-alumina layer at 500-1000 ℃ with the deposition thickness of 10-200 nm, and performing high-temperature treatment at 1000-1300 ℃;
6) And growing an AlN thin film on the PVD-AlN layer by using a metal organic chemical vapor phase epitaxy (MOCVD) method.
EXAMPLE III
Referring to fig. 3, a high quality AlN thin film material was prepared on a Si substrate by the following steps:
1) Forming a single-crystal-phase alpha-alumina layer on the Si substrate according to the method described in the first embodiment or the second embodiment;
2) Carrying out high-temperature treatment on the alpha-alumina layer for 5-30 min in a nitrogen-containing atmosphere (nitrogen or ammonia) by using a thermal annealing or laser annealing method to form an AlON layer on the surface and form an AlON/alpha-alumina composite transition layer;
3) Depositing a PVD-AlN layer on the AlON/alpha-alumina composite transition layer at the deposition temperature of 500-1000 ℃ and the deposition thickness of 10-200 nm, and performing high-temperature treatment at the temperature of 1000-1300 ℃;
4) And growing an AlN thin film on the PVD-AlN layer by using a metal organic chemical vapor phase epitaxy (MOCVD) method.
The foregoing is a more detailed description of the invention that is presented in connection with specific embodiments, and the practice of the invention is not intended to be limited to these descriptions. 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. A preparation method of a high-quality AlN thin film material on a Si substrate is characterized by comprising the following steps:
1) Selecting a Si (111) substrate, and forming an alumina transition layer on the surface of the Si (111) substrate;
2) Carrying out high-temperature treatment on the alumina transition layer to form an alpha-alumina transition layer or an AlON/alpha-alumina composite transition layer;
3) And growing an AlN layer on the alpha-alumina transition layer or the AlON/alpha-alumina composite transition layer to obtain the high-quality AlN thin film.
2. The method according to claim 1, wherein step 1) grows a layer of alumina on the surface of the Si (111) substrate by atomic layer deposition, molecular beam epitaxy or physical vapor deposition; alternatively, a layer of Al is grown on the surface of the Si (111) substrate using an atomic layer deposition, molecular beam epitaxy, or physical vapor deposition method, and then the Al layer is oxidized to aluminum oxide using a thermal oxidation method.
3. The method of claim 1, wherein the thickness of the alumina transition layer in step 1) is 1 to 100 nm.
4. The preparation method according to claim 1, wherein the step 2) is to perform high-temperature treatment on the alumina transition layer by using a thermal annealing or laser annealing method, so that amorphous alumina is converted into a single crystal structure of an alpha phase, and a uniform alpha-alumina (0001) crystal face is formed on the surface to obtain the alpha-alumina transition layer.
5. The preparation method according to claim 1, wherein in the step 2), the alumina transition layer is subjected to high-temperature treatment by using a thermal annealing or laser annealing method, so that amorphous alumina is converted into an alpha-phase single crystal structure, and a uniform alpha-alumina (0001) crystal face is formed on the surface to obtain the alpha-alumina transition layer; and then carrying out nitridation treatment on the surface of the alpha-alumina transition layer to obtain the AlON/alpha-alumina composite transition layer.
6. The preparation method according to claim 5, wherein in the step 2), the nitriding treatment is to perform high-temperature treatment on the alpha-alumina transition layer by using a thermal annealing or laser annealing method in a nitrogen or ammonia atmosphere to form an AlON composite structure on the surface to obtain the AlON/alpha-alumina composite transition layer.
7. The method of claim 1, wherein step 3) comprises growing a PVD-AlN nucleation layer by PVD, and growing an AlN film on the PVD-AlN nucleation layer by mocvd, or growing an AlN film on the PVD-AlN nucleation layer by mocvd after high temperature treatment.
8. The method of claim 7, wherein the PVD-AlN nucleation layer is processed at a high temperature of 1000-1300 ℃.
9. The method of claim 7, wherein the PVD-AlN nucleation layer has a thickness of 10-200 nm.
10. An AlN thin film material on a Si substrate obtained by the preparation method according to any one of claims 1 to 9.
CN202310052527.8A 2023-02-02 2023-02-02 Preparation method of high-quality AlN thin film material on Si substrate Pending CN115831719A (en)

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Publication number Priority date Publication date Assignee Title
JP2000164510A (en) * 1998-11-26 2000-06-16 Sony Corp Iii-v nitride compound semiconductor substrate and manufacture of the same, and semiconductor device and manufacture of the same
JP2004137142A (en) * 2002-03-14 2004-05-13 Rikogaku Shinkokai Single crystal aluminum nitride membrane and forming method thereof, underlying substrate for group iii nitride membrane, luminescent element, as well as surface elastic wave device
JP2011051862A (en) * 2009-09-04 2011-03-17 Tohoku Univ High orientation aluminum nitride crystal film and method for producing the same
CN103545348A (en) * 2012-07-16 2014-01-29 台湾积体电路制造股份有限公司 Diffusion barrier layer for group III nitride on silicon substrate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000164510A (en) * 1998-11-26 2000-06-16 Sony Corp Iii-v nitride compound semiconductor substrate and manufacture of the same, and semiconductor device and manufacture of the same
JP2004137142A (en) * 2002-03-14 2004-05-13 Rikogaku Shinkokai Single crystal aluminum nitride membrane and forming method thereof, underlying substrate for group iii nitride membrane, luminescent element, as well as surface elastic wave device
JP2011051862A (en) * 2009-09-04 2011-03-17 Tohoku Univ High orientation aluminum nitride crystal film and method for producing the same
CN103545348A (en) * 2012-07-16 2014-01-29 台湾积体电路制造股份有限公司 Diffusion barrier layer for group III nitride on silicon substrate

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