CN109728138B - Aluminum nitride self-supporting substrate and preparation method thereof - Google Patents
Aluminum nitride self-supporting substrate and preparation method thereof Download PDFInfo
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Abstract
The invention provides an aluminum nitride self-supporting substrate and a preparation method thereof, and relates to the technical field of semiconductors. When the fast-growth high-temperature aluminum nitride layer is manufactured, under the condition that the aluminum nitride material does not fill gaps among the three-dimensional island structures, the aluminum nitride material is fast folded, and a large number of holes can be formed in the gaps among the three-dimensional island structures which are not filled with the aluminum nitride material, and the holes can reduce the contact area between the fast-growth high-temperature aluminum nitride layer and the low-temperature aluminum nitride layer, so that the fast-growth high-temperature aluminum nitride layer and the fast-growth aluminum nitride thick film can be self-separated from other layers under the action of lattice mismatch and thermal mismatch strain, and a self-supporting substrate is obtained. The high density, small size voids facilitate strain relief to prevent surface cracking, provide dislocation terminated free surfaces to reduce threading dislocation density, and result in a free standing substrate with very low dislocation density. The method has simple separation process and high yield, and can realize large-scale industrialization of the high-quality aluminum nitride self-supporting substrate.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to an aluminum nitride self-supporting substrate and a preparation method thereof.
Background
In recent years, the third generation semiconductor material, aluminum indium gallium nitride (AlInGaN), has attracted much attention due to its excellent properties of high temperature resistance, radiation resistance, chemical corrosion resistance, high luminous efficiency, etc., and has been commercially applied in the fields of blue and white light emitting diodes and lasers, etc. However, optoelectronic and electronic devices based on high aluminum content aluminum gallium nitride (AlGaN) materials are still slow to advance, the underlying reason for this is the lack of high quality aluminum nitride (AlN) substrates. Because the direct synthesis of AlN single crystals requires extreme conditions of high temperature and high pressure, the AlN single crystals still stay at the laboratory research level at present, and the produced AlN single crystals have small size, poor quality, high price and the like, thereby seriously limiting the industrial application thereof. At present, commercial AlN substrates are mainly grown on heterogeneous substrates such as sapphire, silicon carbide, metal substrates, and the like, and due to large thermal mismatch and lattice mismatch between AlN and the heterogeneous substrates, and weak migration capability of Al atoms, large strain and high-density dislocation exist in an AlN epitaxial layer, and the problem that the most mainstream sapphire substrate has poor heat dissipation in a high-power device is obvious, which seriously affects the comprehensive performance of the device.
Disclosure of Invention
In view of the above, the present invention provides an aluminum nitride free-standing substrate and a method for manufacturing the same, which can obtain an aluminum nitride free-standing substrate with low dislocation density.
The technical scheme provided by the invention is as follows:
a method for preparing an aluminum nitride self-supporting substrate comprises the following steps:
providing a heterogeneous substrate;
growing an aluminum nitride buffer layer based on the foreign substrate, the aluminum nitride buffer layer comprising a plurality of buffer island structures;
growing a high temperature aluminum nitride layer based on the aluminum nitride buffer layer;
growing a low-temperature aluminum nitride layer based on the high-temperature aluminum nitride layer, wherein the low-temperature aluminum nitride layer comprises a plurality of three-dimensional island-shaped structures, and gaps are formed between adjacent three-dimensional island-shaped structures;
depositing an aluminum nitride material on the basis of the low-temperature aluminum nitride layer, wherein the aluminum nitride material is folded on the surface of the low-temperature aluminum nitride layer to form a fast-growth high-temperature aluminum nitride layer before the gap is filled, and gaps among the three-dimensional island-shaped structures form cavities at the interface of the fast-growth high-temperature aluminum nitride layer and the low-temperature aluminum nitride layer;
growing an aluminum nitride thick film based on the fast-growing high-temperature aluminum nitride layer;
separating the aluminum nitride thick film and the fast-growing high-temperature aluminum nitride layer from other layers, wherein the aluminum nitride thick film and the fast-growing high-temperature aluminum nitride layer form an aluminum nitride self-supporting substrate.
Further, the thickness of the aluminum nitride buffer layer is 5-50 nm.
Further, the cross-sectional dimension of the buffer island is 5-20 nm.
Furthermore, the growth temperature of the high-temperature aluminum nitride layer is 1100-1400 ℃, and the thickness of the high-temperature aluminum nitride layer is 100-500 nm.
Furthermore, the growth temperature of the low-temperature aluminum nitride layer is 800-1100 ℃, and the thickness of the low-temperature aluminum nitride layer is 50-500 nm.
Further, the growth speed of the fast-growth high-temperature aluminum nitride layer is more than 0.5 mu m/h, and the thickness of the fast-growth high-temperature aluminum nitride layer is more than or equal to 1 mu m.
Further, the thickness of the aluminum nitride thick film is greater than or equal to 50 μm.
Further, the foreign substrate includes a sapphire substrate, a silicon substrate, or a silicon carbide substrate.
Further, the aluminum nitride buffer layer is manufactured by any one of metal organic chemical vapor deposition, magnetron sputtering, atomic layer deposition, pulse laser deposition or molecular beam epitaxy;
the high-temperature aluminum nitride layer, the low-temperature aluminum nitride layer and the fast-growth high-temperature aluminum nitride layer are manufactured by a metal organic chemical vapor deposition method.
The invention also provides an aluminum nitride self-supporting substrate which is prepared by the preparation method.
In summary, in the embodiment of the present invention, when the aluminum nitride self-supporting substrate is manufactured, the aluminum nitride buffer layer, the high temperature aluminum nitride layer, the low temperature aluminum nitride layer, the fast growth high temperature aluminum nitride layer and the aluminum nitride thick film are sequentially manufactured on the heterogeneous substrate, in the manufacturing process, the low temperature aluminum nitride layer forms the three-dimensional island structures, and gaps are formed between the three-dimensional island structures, when the fast growth high temperature aluminum nitride layer is manufactured, under the condition that the aluminum nitride material does not fill the gaps between the three-dimensional island structures, the aluminum nitride material can be rapidly folded to form the fast growth high temperature aluminum nitride layer which seals the three-dimensional island structures, and the gaps between the three-dimensional island structures which are not filled by the aluminum nitride material can form a large number of cavities at the interface between the low temperature aluminum nitride layer and the fast growth high temperature aluminum nitride layer, and the cavities can reduce the contact area between the fast growth, the self-separation of the fast-growing high-temperature aluminum nitride layer and the aluminum nitride thick film from other layers can be realized under the action of lattice mismatch strain and thermal mismatch strain, and the self-supporting substrate consisting of the fast-growing high-temperature aluminum nitride layer and the aluminum nitride thick film is obtained. The high-density and small-size cavities between the high-temperature aluminum nitride layer and the low-temperature aluminum nitride layer are grown quickly, so that the strain is released, the surface cracking is prevented, meanwhile, a dislocation-stopped free surface is provided to reduce the threading dislocation density, and a self-supporting substrate with low dislocation density can be obtained. The preparation method has simple separation process and high yield, and can realize large-scale industrialization of the high-quality aluminum nitride self-supporting substrate.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic flow chart of a method for preparing an aluminum nitride free-standing substrate according to an embodiment of the present invention.
Fig. 2 is a schematic structural diagram corresponding to step S101 in the method for preparing an aluminum nitride free-standing substrate according to an embodiment of the present invention.
Fig. 3 is a schematic structural diagram corresponding to step S102 in the method for preparing an aluminum nitride free-standing substrate according to an embodiment of the invention.
Fig. 4 is a schematic structural diagram corresponding to step S103 in the method for preparing an aluminum nitride free-standing substrate according to the embodiment of the invention.
Fig. 5 is a schematic structural diagram corresponding to step S104 in the method for preparing an aluminum nitride free-standing substrate according to the embodiment of the invention.
Fig. 6 is a schematic structural diagram corresponding to step S105 in the method for preparing an aluminum nitride free-standing substrate according to the embodiment of the invention.
Fig. 7 is a schematic structural diagram corresponding to step S106 in the method for preparing an aluminum nitride free-standing substrate according to an embodiment of the present invention.
Fig. 8 is a schematic structural diagram corresponding to step S107 in the method for preparing an aluminum nitride free-standing substrate according to the embodiment of the invention.
Fig. 9 is a schematic structural diagram of an aluminum nitride free-standing substrate obtained by a method for preparing an aluminum nitride free-standing substrate according to an embodiment of the present invention.
Icon: 101-a foreign substrate; 102-an aluminum nitride buffer layer; 103-a high temperature aluminum nitride layer; 104-low temperature aluminum nitride layer; 105-rapidly growing a high-temperature aluminum nitride layer; 106-aluminum nitride thick film; a 10-aluminum nitride free-standing substrate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures. Meanwhile, in the description of the present invention, the terms "first", "second", and the like are used only for distinguishing the description, and are not to be construed as indicating or implying relative importance.
In the research process, the inventor finds that in order to solve the problems of the AlN substrate, a preparation method of the type AlN is developed: firstly, a few microns of AlN is grown on a substrate of sapphire, silicon carbide, or the like by a Metal-organic Chemical Vapor Deposition (MOCVD) technique; then, growing thick-film AlN at high speed by Hydride Vapor Phase Epitaxy (HVPE) technology; then, peeling off the substrate such as sapphire, silicon carbide and the like by means of chemical etching, self-separation, ion beam peeling or laser peeling and the like to obtain an untreated AlN self-supporting substrate; and finally, obtaining the AlN self-supporting substrate which can be industrially applied through the subsequent procedures of chemical mechanical polishing and the like.
However, the dislocation density of the conventional AlN self-supporting substrate is still high, the substrate peeling process is excessively complicated, and the substrate peeling has serious in-plane non-uniformity and low yield.
In order to solve the above problem, the present embodiment provides a method for preparing an aluminum nitride free-standing substrate 10, as shown in fig. 1, including the following steps.
Step S101, as shown in fig. 2, provides a foreign substrate 101.
The foreign substrate 101 may be a sapphire substrate, a silicon carbide substrate, or the like, and the specific material of the foreign substrate 101 is not limited in the embodiments of the present application.
Step S102, as shown in fig. 3, growing an aluminum nitride buffer layer 102 on the foreign substrate 101, where the aluminum nitride buffer layer 102 includes a plurality of buffer island structures.
The aluminum nitride buffer layer 102 can be grown on the foreign substrate 101 by adopting a metal organic chemical vapor deposition method, magnetron sputtering, atomic layer deposition, pulsed laser deposition or molecular beam epitaxy, and the growth thickness of the aluminum nitride buffer layer 102 can be 5-50 nm. The aluminum nitride buffer layer 102 may include a plurality of buffer island structures, a diameter of a cross section of each buffer island structure may be 5 to 20nm, a density of the buffer island structures may be grown according to actual needs, preferably, the buffer island structures form an arrangement form with a higher density, and the aluminum nitride buffer layer 102 requires a single Al polarity.
Step S103, as shown in fig. 4, a high temperature aluminum nitride layer 103 is grown on the aluminum nitride buffer layer 102.
After the fabrication of the aluminum nitride buffer layer 102 is completed, the metal organic chemical vapor deposition method may be continuously employed to fabricate the high temperature aluminum nitride layer 103, and the growth temperature of the high temperature aluminum nitride layer 103 may be controlled between 1100-. Optionally, the growth thickness of the high temperature aluminum nitride layer 103 may be 100-500 nm.
Step S104, as shown in fig. 5, growing a low-temperature aluminum nitride layer 104 on the basis of the high-temperature aluminum nitride layer 103, where the low-temperature aluminum nitride layer 104 includes a plurality of three-dimensional island-shaped structures, and a gap is formed between adjacent three-dimensional island-shaped structures.
After the high-temperature aluminum nitride layer 103 is manufactured, the low-temperature aluminum nitride layer 104 may be manufactured by a metal organic chemical vapor deposition method, and the shape of the three-dimensional island-shaped structure forming the low-temperature aluminum nitride layer 104 may be determined according to actual manufacturing requirements, for example, the three-dimensional island-shaped structure may be a cone, a truncated cone, a pyramid, or the like, and a gap is formed between adjacent three-dimensional island-shaped structures. The size of the gaps between the three-dimensional island structures is.
In the embodiment of the present application, the growth temperature of the low temperature aluminum nitride layer 104 may be 800-1100 ℃, and the thickness of the low temperature aluminum nitride layer 104 may be 50-500 nm.
Step S105, as shown in fig. 6, depositing an aluminum nitride material on the basis of the low-temperature aluminum nitride layer 104, wherein the aluminum nitride material is folded on the surface of the low-temperature aluminum nitride layer 104 to form a fast-growth high-temperature aluminum nitride layer 105 before the gap is filled, and the gap between the three-dimensional island structures forms a void at the interface between the fast-growth high-temperature aluminum nitride layer 105 and the low-temperature aluminum nitride layer 104.
After the low temperature aluminum nitride layer 104 is formed, the rapidly grown high temperature aluminum nitride layer 105 may be formed, and the rapidly grown high temperature aluminum nitride layer 105 may be formed under a high growth rate. Under the high-speed growth condition, the growth speed of the fast-growth high-temperature aluminum nitride layer 105 can be more than 0.5 μm/h, at such a fast growth speed, the aluminum nitride material can be rapidly folded on the surfaces of the three-dimensional island structures to form a closed surface, and because the growth speed of the aluminum nitride material is fast, the gaps between the three-dimensional island structures are not filled with the aluminum nitride material, the aluminum nitride material can be completely folded on the surfaces of the three-dimensional island structures, so that the gaps between the three-dimensional island structures form cavities. Since the gaps between the three-dimensional island-shaped structures are on the nanometer scale, the size of the formed cavities is also on the nanometer scale, and meanwhile, the density of the three-dimensional island-shaped structures in the low-temperature aluminum nitride layer 104 is high, and the density of the formed cavities is also high. These high density, small size voids are located between the rapidly grown high temperature aluminum nitride layer 105 and the low temperature aluminum nitride layer 104 to relieve strain to prevent surface cracking while providing free surface for dislocation termination to reduce threading dislocation density.
In the embodiment of the present application, the thickness of the rapidly grown high temperature aluminum nitride layer 105 may be greater than or equal to 1 μm.
Step S106, as shown in fig. 7, an aluminum nitride thick film 106 is grown based on the fast-growth high-temperature aluminum nitride layer 105.
After the rapid growth of the high temperature aluminum nitride layer 105 is completed, the growth of the aluminum nitride thick film 106 may be resumed, and the aluminum nitride thick film 106 may be fabricated by a hydride vapor phase epitaxy method. The thickness of aluminium nitride thick film 106 can be greater than 50 μm, aluminium nitride thick film 106 can release the strain through self-separation under the effect of accumulation meeting an emergency, because there is the nanometer cavity between high temperature aluminium nitride layer 105 of fast growth and the low temperature aluminium nitride layer 104, make the area of contact between high temperature aluminium nitride layer 105 of fast growth and the low temperature aluminium nitride layer 104 little, so the separation at this interface very easily, and nanometer cavity density high distribution is even, can solve the fracture and the in-plane inhomogeneous problem that leads to from the separation in-process.
Step S107, as shown in fig. 8 and 9, separating the aluminum nitride thick film 106 and the fast-growing high-temperature aluminum nitride layer 105 from other layers, wherein the aluminum nitride thick film 106 and the fast-growing high-temperature aluminum nitride layer 105 form an aluminum nitride free-standing substrate 10.
After the preparation of accomplishing aluminium nitride thick film 106, the self-separation of high temperature aluminium nitride layer 105 and aluminium nitride thick film 106 of growing fast just can be realized with other layers under the effect of cavity, and in the disengaging process, because the existence of cavity, the cavity can release the internal stress that exists in the high temperature aluminium nitride layer 105 of growing fast, makes the high temperature aluminium nitride layer 105 of growing fast can not take place the fracture, and the surface is more even.
The separated aluminum nitride thick film 106 and the rapidly grown high temperature aluminum nitride layer 105 can be further subjected to chemical and mechanical polishing to obtain the aluminum nitride self-supporting substrate 10 which can be industrially applied.
The invention also provides an aluminum nitride self-supporting substrate which is prepared by the preparation method.
In summary, in the embodiment of the present invention, when the aluminum nitride self-supporting substrate is manufactured, the aluminum nitride buffer layer, the high temperature aluminum nitride layer, the low temperature aluminum nitride layer, the fast growth high temperature aluminum nitride layer and the aluminum nitride thick film are sequentially manufactured on the heterogeneous substrate, in the manufacturing process, the low temperature aluminum nitride layer forms the three-dimensional island structures, and gaps are formed between the three-dimensional island structures, when the fast growth high temperature aluminum nitride layer is manufactured, under the condition that the aluminum nitride material does not fill the gaps between the three-dimensional island structures, the aluminum nitride material can be rapidly folded to form the fast growth high temperature aluminum nitride layer which seals the three-dimensional island structures, and the gaps between the three-dimensional island structures which are not filled by the aluminum nitride material can form a large number of cavities at the interface between the low temperature aluminum nitride layer and the fast growth high temperature aluminum nitride layer, and the cavities can reduce the contact area between the fast growth, the fast-growing high-temperature aluminum nitride layer and the aluminum nitride thick film can be separated from other layers, and therefore the self-supporting substrate consisting of the fast-growing high-temperature aluminum nitride layer and the aluminum nitride thick film is obtained. The high-density and small-size cavities between the high-temperature aluminum nitride layer and the low-temperature aluminum nitride layer are grown quickly, so that the strain is released, the surface cracking is prevented, meanwhile, a dislocation-stopped free surface is provided to reduce the threading dislocation density, and a self-supporting substrate with low dislocation density can be obtained. The preparation method has simple separation process and high yield, and can realize large-scale industrialization of the high-quality aluminum nitride self-supporting substrate.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A method for preparing an aluminum nitride free-standing substrate, comprising:
providing a heterogeneous substrate;
growing an aluminum nitride buffer layer based on the foreign substrate, the aluminum nitride buffer layer comprising a plurality of buffer island structures;
growing a high temperature aluminum nitride layer based on the aluminum nitride buffer layer;
growing a low-temperature aluminum nitride layer based on the high-temperature aluminum nitride layer, wherein the low-temperature aluminum nitride layer comprises a plurality of three-dimensional island-shaped structures, and gaps are formed between adjacent three-dimensional island-shaped structures;
depositing an aluminum nitride material on the basis of the low-temperature aluminum nitride layer, wherein the aluminum nitride material is folded on the surface of the low-temperature aluminum nitride layer to form a fast-growth high-temperature aluminum nitride layer before the gap is filled, and the gap between the three-dimensional island structures forms a cavity at the interface of the fast-growth high-temperature aluminum nitride layer and the low-temperature aluminum nitride layer, wherein the growth speed of the fast-growth high-temperature aluminum nitride layer is more than 0.5 μm/h, and the thickness of the fast-growth high-temperature aluminum nitride layer is more than or equal to 1 μm;
growing an aluminum nitride thick film based on the fast-growing high-temperature aluminum nitride layer;
separating the aluminum nitride thick film and the fast-growing high-temperature aluminum nitride layer from other layers, wherein the aluminum nitride thick film and the fast-growing high-temperature aluminum nitride layer form an aluminum nitride self-supporting substrate.
2. The method of claim 1, wherein the aluminum nitride buffer layer has a thickness of 5-50 nm.
3. The method of claim 1, wherein the buffer islands have a cross-sectional dimension of 5-20 nm.
4. The method as claimed in claim 1, wherein the growth temperature of the high temperature aluminum nitride layer is 1100-1400 ℃ and the thickness of the high temperature aluminum nitride layer is 100-500 nm.
5. The method as claimed in claim 1, wherein the growth temperature of the low temperature aluminum nitride layer is 800-1100 ℃, and the thickness of the low temperature aluminum nitride layer is 50-500 nm.
6. The method of claim 1, wherein the thickness of the aluminum nitride thick film is 50 μm or more.
7. The method for producing an aluminum nitride free-standing substrate according to any one of claims 1 to 6, wherein the foreign substrate comprises a sapphire substrate, a silicon substrate, or a silicon carbide substrate.
8. The method for preparing an aluminum nitride free-standing substrate according to any one of claims 1 to 6, wherein the aluminum nitride buffer layer is fabricated by any one of metal organic chemical vapor deposition, magnetron sputtering, atomic layer deposition, pulsed laser deposition or molecular beam epitaxy;
the high-temperature aluminum nitride layer, the low-temperature aluminum nitride layer and the fast-growth high-temperature aluminum nitride layer are manufactured by a metal organic chemical vapor deposition method.
9. An aluminum nitride free-standing substrate, characterized in that it is produced by the production method of any one of claims 1 to 8.
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