CN115881514A - Method for manufacturing single crystal self-supporting substrate - Google Patents
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- CN115881514A CN115881514A CN202211493168.1A CN202211493168A CN115881514A CN 115881514 A CN115881514 A CN 115881514A CN 202211493168 A CN202211493168 A CN 202211493168A CN 115881514 A CN115881514 A CN 115881514A
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Abstract
The invention provides a method for manufacturing a single crystal self-supporting substrate, which comprises the following steps: 1) Providing a substrate; 2) Growing beta-Ga on a substrate using an HVPE apparatus 2 O 3 A buffer layer; 3) Growing a GaN epitaxial layer on the buffer layer by using HVPE equipment in a nitrogen atmosphere without hydrogen; 4) Introducing a hydrogen-containing gas into the reactor at a decomposition temperature to obtain beta-Ga by using HVPE equipment 2 O 3 The buffer layer is completely decomposed, and the GaN epitaxial layer is separated from the substrate; 5) GaN epitaxy is performed using HVPE equipment to increase the thickness of the GaN epitaxial layer to a target thickness to obtain a single crystal free-standing substrate. The invention can avoid the problem of low yield caused by a laser stripping process and a self-separation process, improve the growth quality of the GaN epitaxy, and reduce the warping or splitting of the GaN epitaxy layer caused by stress accumulation caused by thermal adaptation and lattice mismatch.
Description
Technical Field
The invention belongs to the field of semiconductor integrated circuit design and manufacture, and particularly relates to a method for manufacturing a single crystal self-supporting substrate.
Background
The third generation semiconductor material represented by gallium nitride (GaN) and its alloy is a new semiconductor material which has been paid more attention internationally in recent decades, has a large forbidden bandwidth, a high electron saturation drift velocity, a small dielectric constant, a good heat conductivity, a stable structure and other excellent properties, and has a great application prospect in the technical fields of photoelectrons and microelectronics. In the photoelectron field, because the forbidden band width of the III group nitride is continuously adjustable within the range of 0.7-6.2eV, the III group nitride covers the wave band from red light to ultraviolet light, and can be used for manufacturing green, blue and even ultraviolet wave band light-emitting devices and white light illumination. In addition, the recently emerging ultraviolet light LEDs also show special applications in screen printing, polymer curing and environmental protection, and have greatly stimulated research interest of researchers. GaN lasers are also used in the field of information storage, and can be used in medical diagnostics, submarine exploration, communications, and other aspects.
The preparation of GaN bulk single crystals is difficult and it is difficult to obtain large-sized and good quality bulk single crystal GaN substrates, so the epitaxial growth of GaN is usually performed by heteroepitaxy. However, theories and experiments show that when GaN is used as a substrate homoepitaxy device, the performance of the device is greatly improved. The fabrication of self-supporting GaN substrates has therefore become a focus of attention.
At present, a large-area GaN self-supporting substrate is generally obtained by growing a GaN thick film on a foreign substrate in a vapor phase mode and then separating the original foreign substrate. With sapphire substrates being the most commonly used substrate. In order to obtain a free-standing substrate, the sapphire substrate must be removed. Sapphire is hard and chemically stable and is therefore difficult to remove by chemical etching or mechanical grinding. The GaN and sapphire substrates are currently separated by laser lift-off. But laser lift-off techniques are expensive; in the laser lift-off process, high-pressure gas generated after GaN is decomposed at the interface at high temperature easily damages the prepared GaN self-supporting substrate, a large amount of dislocation and microcrack are generated on the GaN self-supporting substrate to influence the quality of a later device, and the GaN self-supporting substrate is completely cracked to greatly reduce the yield. The other separation process is stress-induced self-separation, but the stress condition of the epitaxial layer is complex and difficult to be uniform, the separation point has larger uncertainty, and the yield is low.
Generally speaking, when epitaxial growth is carried out on the epitaxy of the heterogeneous material, the thickness of the heteroepitaxial gallium nitride is limited due to lattice mismatch and thermal mismatch, and meanwhile, the process difficulty of dissociating the gallium nitride single crystal is large, and the heteroepitaxial gallium nitride single crystal is particularly obvious on a large-size sapphire/gallium nitride thick film composite substrate (HVPE primary epitaxial wafer).
It should be noted that the above background description is only for the convenience of clear and complete description of the technical solutions of the present application and for the understanding of those skilled in the art. Such solutions are not considered to be known to the person skilled in the art merely because they have been set forth in the background section of the present application.
Disclosure of Invention
In view of the above drawbacks of the prior art, an object of the present invention is to provide a method for manufacturing a single crystal self-supporting substrate, which is used to solve the problems in the prior art that when epitaxial growth is performed on a hetero material epitaxy, the thickness of hetero epitaxial gallium nitride is limited due to lattice mismatch and thermal mismatch, and the process difficulty of dissociating a gallium nitride single crystal is high.
To achieve the above and other related objects, the present invention provides a method of fabricating a single crystal self-supporting substrate, the method comprising: 1) Providing a substrate; 2) Growing beta-Ga on the substrate using HVPE apparatus 2 O 3 A buffer layer; 3) Growing a GaN epitaxial layer on the buffer layer under a nitrogen atmosphere without hydrogen using the HVPE apparatus; 4) Introducing a hydrogen-containing gas into the HVPE apparatus to decompose beta-Ga at a decomposition temperature 2 O 3 The buffer layer is completely decomposed, and the GaN epitaxial layer is separated from the substrate; 5) Performing GaN epitaxy using the HVPE apparatus, increasing the thickness of the GaN epitaxial layer to a target thickness to obtain a single crystal free-standing substrate.
Optionally, the substrate is a c-plane sapphire substrate, and the beta-Ga is 2 O 3 The buffer layer is beta-Ga with (-201) plane 2 O 3 A buffer layer.
Alternatively, the beta-Ga 2 O 3 The thickness of the buffer layer is 10 nanometers to 10 micrometers.
Optionally, the temperature of growing the GaN epitaxial layer on the buffer layer in step 3) is above 1000 ℃, and the thickness of the GaN epitaxial layer is 50-150 microns.
Optionally, step 4) comprises: setting the HVPE equipment temperature to 890 deg.C or above, introducing hydrogen and waterNitrogen gas to make beta-Ga 2 O 3 The buffer layer is completely decomposed to realize the separation of the GaN epitaxial layer and the substrate, wherein the beta-Ga 2 O 3 The products of the buffer layer decomposition are all gaseous.
Optionally, step 4) comprises: the temperature of HVPE equipment is reduced to 600-890 ℃, and hydrogen and nitrogen-containing gas are introduced to lead beta-Ga 2 O 3 The buffer layer is completely decomposed to realize the separation of the GaN epitaxial layer and the substrate, wherein the beta-Ga 2 O 3 The products of the buffer layer decomposition include liquid gallium.
Alternatively, the flow ratio of the hydrogen gas to the nitrogen-containing gas is 1.
Optionally, the nitrogen-containing gas of step 4) comprises one or both of ammonia and nitrogen.
Optionally, step 4) comprises: reducing the temperature of HVPE equipment to below 600 ℃, and introducing hydrogen to ensure that beta-Ga 2 O 3 The buffer layer is completely decomposed to realize the separation of the GaN epitaxial layer and the substrate, wherein the beta-Ga 2 O 3 The products of the buffer layer decomposition include liquid gallium.
Optionally, the target thickness in step 5) is greater than or equal to 250 micrometers.
As described above, the method for manufacturing a single crystal self-standing substrate of the present invention has the following advantageous effects:
the invention is achieved by applying beta-Ga between the substrate and the GaN epitaxial layer 2 O 3 Buffer layer of beta-Ga 2 O 3 The buffer layer has higher decomposition temperature in the hydrogen-free environment and greatly reduced decomposition temperature in the hydrogen-containing environment, so that the beta-Ga can be subjected to low-temperature treatment in the hydrogen-containing environment 2 O 3 The buffer layer is decomposed to separate the GaN epitaxial layer from the substrate, so that the problem of low yield (especially suitable for large-size GaN substrate) caused by a laser stripping process and a self-separation process is avoided on the first aspect, and meanwhile, the beta-Ga is decomposed at the early stage of growth 2 O 3 The buffer layer can ensure that the GaN epitaxial layer is not physically and firmly connected with the substrate, and reduces the warping or splitting of the epitaxial layer caused by stress accumulation caused by thermal adaptation and lattice mismatch; first, theIn two aspects beta-Ga 2 O 3 The buffer layer and the GaN epitaxial layer have smaller lattice mismatch, so that the quality of the grown crystal of the GaN epitaxial layer can be effectively improved, and the stress of the GaN epitaxial layer is reduced; in a third aspect, the whole preparation process can be completed in one HVPE device, the epitaxial wafer does not need to be transferred among different devices for multiple times, a GaN composite substrate is not needed, dependence on MOCVD equipment is avoided, the process is simple, and impurities or dust introduced in the process of transferring the epitaxial wafer is reduced.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the application, are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the principles of the application. It is to be understood that the drawings in the following description are of some embodiments of the application only.
FIGS. 1-6 show schematic structural views of steps of a method for fabricating a single crystal self-supporting substrate according to an embodiment of the present invention.
Description of the element reference numerals
101. Substrate
102 β-Ga 2 O 3 Buffer layer
103 GaN epitaxial layer
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It should be emphasized that the term "comprises/comprising" when used herein, is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, integers, steps or components.
Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments, in combination with or instead of the features of the other embodiments.
As in the detailed description of the embodiments of the present invention, the cross-sectional views illustrating the device structures are not partially enlarged in general scale for convenience of illustration, and the schematic views are only examples, which should not limit the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in the actual fabrication.
For convenience in description, spatial relational terms such as "below," "beneath," "below," "under," "over," "upper," and the like may be used herein to describe one element or feature's relationship to another element or feature as illustrated in the figures. It will be understood that these terms of spatial relationship are intended to encompass other orientations of the device in use or operation in addition to the orientation depicted in the figures. Further, when a layer is referred to as being "between" two layers, it can be the only layer between the two layers, or one or more intervening layers may also be present.
In the context of this application, a structure described as having a first feature "on" a second feature may include embodiments in which the first and second features are formed in direct contact, and may also include embodiments in which additional features are formed in between the first and second features, such that the first and second features may not be in direct contact.
It should be noted that the drawings provided in the present embodiment are only for illustrating the basic idea of the present invention, and the drawings only show the components related to the present invention rather than being drawn according to the number, shape and size of the components in actual implementation, and the type, quantity and proportion of each component in actual implementation may be changed arbitrarily, and the layout of the components may be more complicated.
After the growth of the GaN self-supporting substrate is completed, the GaN self-supporting substrate needs to be peeled from the growth substrate, and the peeling method can be a laser peeling process and a self-separation process, but the laser peeling process and the self-separation process are prone to problems such as cracking or increased surface defects, so that the yield of epitaxial wafers is reduced, and especially for large-size GaN substrates, the cracking problem is more serious. Meanwhile, the GaN epitaxial wafer and the growth substrate have large thermal adaptation and lattice mismatch, which may cause stress accumulation of the GaN epitaxial wafer to generate warpage or cracking.
Example 1
As shown in fig. 1 to 6, the present embodiment provides a method for manufacturing a single crystal self-supporting substrate, the method comprising the steps of:
as shown in fig. 1, step 1) is performed first, providing a substrate 101.
In one embodiment, the substrate 101 may be a sapphire substrate, which may be, for example, a c-plane sapphire substrate.
Before the subsequent epitaxy, the substrate 101 may be cleaned to remove impurities on the surface of the substrate 101, so as to improve the growth quality of the subsequent epitaxy layer.
As shown in fig. 2, step 2) is then performed to grow β -Ga on the substrate 101 using a Hydride Vapor Phase Epitaxy (HVPE) apparatus 2 O 3 A buffer layer 102.
In one embodiment, the growth of β -Ga on the substrate 101 is performed using a Hydride Vapor Phase Epitaxy (HVPE) apparatus 2 O 3 The buffer layer 102 includes: at 800-900 deg.c, gallium chloride is produced through the reaction of gallium metal and hydrogen chloride or chlorine as gallium source, and oxygen as oxygen source at 900-1050 deg.c 2 Mixing and reacting to grow beta-Ga on the surface of the substrate 101 2 O 3 The buffer layer 102 may be formed by performing the above reaction at normal pressure or lower pressure, and the O/Ga ratio of the reaction may be 1.5 to 100.
In one embodiment, the beta-Ga 2 O 3 The buffer layer 102 is beta-Ga of (-201) plane 2 O 3 Buffer layer 102 of the beta-Ga 2 O 3 The buffer layer 102 and the GaN epitaxial layer 103 have smaller lattice mismatch, so that the quality of the grown crystal of the subsequent GaN epitaxial layer 103 can be effectively improved, and the stress of the GaN epitaxial layer 103 is reduced.
In one embodiment, the beta-Ga 2 O 3 The buffer layer 102 has a thickness of 10 nm to 10 μm. The beta-Ga 2 O 3 The thickness of the buffer layer 102 can be compatible with the growth effect of the subsequent GaN epitaxial layer 103 (i.e., can effectively buffer lattice mismatch and thermal mismatch between the substrate 101 and the GaN epitaxial layer 103), and can also be compatible with the growth time and the beta-Ga during the subsequent lift-off 2 O 3 Efficiency of complete removal of the buffer layer 102 (over-thick beta-Ga) 2 O 3 Long buffer layer 102 growth time and long dissolution and exfoliation time), in a preferred embodiment, the beta-Ga 2 O 3 The buffer layer 102 has a thickness of 100 nm to 1 μm to further enhance the above-mentioned compatibility.
As shown in fig. 3, followed by step 3), growing a GaN epitaxial layer 103 on the buffer layer 102 under a nitrogen atmosphere without hydrogen using the Hydride Vapor Phase Epitaxy (HVPE) apparatus;
in one embodiment, the temperature for growing the GaN epitaxial layer 103 on the buffer layer 102 is above 1000 ℃, and the thickness of the GaN epitaxial layer 103 is 50-150 microns.
In one embodiment, the GaN epitaxial layer 103 is a 002 plane GaN epitaxial layer 103.
In the GaN epitaxial layer 103 of the present embodiment, beta-Ga is avoided in a nitrogen atmosphere without containing hydrogen 2 O 3 The buffer layer 102 reacts with hydrogen to result in beta-Ga 2 O 3 The buffer layer 102 is decomposed too early to ensure its supporting ability for the GaN epitaxial layer 103 and to avoid the GaN epitaxial layer 103 from being cracked.
As shown in fig. 4 to 5, then, step 4) of introducing a hydrogen-containing gas at a decomposition temperature using the Hydride Vapor Phase Epitaxy (HVPE) apparatus is performed to allow β -Ga 2 O 3 The buffer layer 102 is completely decomposed to separate the GaN epitaxial layer 103 from the substrate 101.
In one embodiment, the temperature of Hydride Vapor Phase Epitaxy (HVPE) equipment is set to be more than 890 ℃, and hydrogen and nitrogen-containing gas are introduced to enable beta-Ga 2 O 3 The buffer layer 102 is completely decomposed to separate the GaN epitaxial layer 103 from the substrate 101, wherein the beta value-Ga 2 O 3 The products of the decomposition of the buffer layer 102 are all in a gaseous state. Preferably, this embodiment maintains the temperature of the Hydride Vapor Phase Epitaxy (HVPE) apparatus during the growth of the GaN epitaxial layer 103, and introduces a hydrogen-containing gas to cause the beta-Ga to be in a decomposition temperature 2 O 3 The buffer layer 102 is completely decomposed, so that the GaN epitaxial layer 103 is separated from the substrate 101, and the time and steps for cooling are saved.
In one embodiment, the flow ratio of the hydrogen gas to the nitrogen-containing gas is between 1 and 10. In one embodiment, the flow ratio of the hydrogen gas to the nitrogen-containing gas is 2:1-3:1.
In one embodiment, the nitrogen-containing gas comprises one or both of ammonia and nitrogen. In this embodiment, the nitrogen-containing gas is ammonia.
As shown in fig. 6, step 5) of performing GaN epitaxy using the Hydride Vapor Phase Epitaxy (HVPE) apparatus is finally performed to increase the thickness of the GaN epitaxial layer 103 to a target thickness to obtain a single crystal free-standing substrate.
In one embodiment, the target thickness is greater than or equal to 250 micrometers.
The whole preparation process can be completed in one Hydride Vapor Phase Epitaxy (HVPE) device, epitaxial wafers do not need to be transferred among different devices for multiple times, a GaN composite substrate is not needed, dependence on MOCVD (metal organic chemical vapor deposition) devices is avoided, the process is simple, and impurities or dust introduced in the process of transferring the epitaxial wafers is reduced.
Example 2
This example provides a method for manufacturing a single crystal self-supporting substrate, the basic steps of which are substantially the same as those of example 1, wherein the difference from example 1 is that step 4) includes: reducing the temperature of Hydride Vapor Phase Epitaxy (HVPE) equipment to 600-890 ℃, and introducing hydrogen and nitrogen-containing gas to ensure that beta-Ga 2 O 3 The buffer layer 102 is completely decomposed to separate the GaN epitaxial layer 103 from the substrate 101, wherein the beta-Ga is 2 O 3 The products of the decomposition of the buffer layer 102 include liquid gallium. The temperature required for decomposition is lower in this embodiment, and the decomposed liquid gallium and GaN epitaxial layer 103 are not presentThe physical hard coupling allows separation of the GaN epitaxial layer 103 from the substrate 101 to be achieved at a relatively low temperature.
Example 3
This example provides a method for manufacturing a single crystal self-supporting substrate, the basic steps of which are substantially the same as those of example 1, wherein the difference from example 1 is that step 4) includes: reducing the temperature of Hydride Vapor Phase Epitaxy (HVPE) equipment to below 600 ℃, and introducing hydrogen to ensure that beta-Ga 2 O 3 The buffer layer 102 is completely decomposed to separate the GaN epitaxial layer 103 from the substrate 101, wherein the beta-Ga is 2 O 3 The products of the decomposition of the buffer layer 102 include liquid gallium. The temperature required by decomposition of the embodiment is only below 600 ℃, the decomposition temperature is very low, and the decomposed liquid gallium is not physically and firmly connected with the GaN epitaxial layer 103, so that the GaN epitaxial layer 103 can be separated from the substrate 101 at a relatively low temperature.
As described above, the method for manufacturing a single crystal self-standing substrate of the present invention has the following advantageous effects:
the present application is achieved by applying beta-Ga between a substrate and a GaN epitaxial layer 2 O 3 Buffer layer, beta-Ga 2 O 3 The buffer layer has higher decomposition temperature in the hydrogen-free environment, and the decomposition temperature in the hydrogen-containing environment can be greatly reduced, so that the beta-Ga can be carried out at low temperature in the hydrogen-containing environment 2 O 3 The buffer layer is decomposed to separate the GaN epitaxial layer from the substrate, so that the problem of low yield (especially suitable for large-size GaN substrate) caused by a laser stripping process and a self-separation process is avoided on the first aspect, and meanwhile, the beta-Ga is decomposed at the early stage of growth 2 O 3 The buffer layer can ensure that the GaN epitaxial layer is not physically and firmly connected with the substrate, and reduces the warping or splitting of the epitaxial layer caused by stress accumulation caused by thermal adaptation and lattice mismatch; second aspect of beta-Ga 2 O 3 The buffer layer and the GaN epitaxial layer have smaller lattice mismatch, so that the quality of the grown crystal of the GaN epitaxial layer can be effectively improved, and the stress of the GaN epitaxial layer is reduced; in a third aspect, the whole preparation process of the invention can be completed in one Hydride Vapor Phase Epitaxy (HVPE) device without switching among different devices for many timesAnd the epitaxial wafer is moved without a GaN composite substrate, so that the dependence on MOCVD equipment is avoided, the process is simple, and impurities or dust introduced in the process of transferring the epitaxial wafer is reduced.
Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which may be made by those skilled in the art without departing from the spirit and scope of the present invention as defined in the appended claims.
Claims (10)
1. A method of fabricating a single crystal self-supporting substrate, the method comprising:
1) Providing a substrate;
2) Growing beta-Ga on the substrate using HVPE equipment 2 O 3 A buffer layer;
3) Growing a GaN epitaxial layer on the buffer layer in a nitrogen atmosphere without hydrogen using the HVPE apparatus;
4) Introducing a hydrogen-containing gas into the HVPE apparatus to decompose beta-Ga at a decomposition temperature 2 O 3 The buffer layer is completely decomposed, and the GaN epitaxial layer is separated from the substrate;
5) Performing GaN epitaxy using the HVPE apparatus, increasing the thickness of the GaN epitaxial layer to a target thickness to obtain a single crystal free-standing substrate.
2. The method of making a single crystal self-supporting substrate of claim 1, wherein: the substrate is a c-plane sapphire substrate, and the beta-Ga 2 O 3 The buffer layer is beta-Ga with (-201) plane 2 O 3 A buffer layer.
3. The single crystal self supporting liner of claim 1The manufacturing method of the bottom is characterized in that: the beta-Ga 2 O 3 The thickness of the buffer layer is 10 nanometers to 10 micrometers.
4. The method of manufacturing a single crystal self-supporting substrate according to claim 1, wherein: and 3) growing a GaN epitaxial layer on the buffer layer at a temperature of over 1000 ℃, wherein the thickness of the GaN epitaxial layer is 50-150 microns.
5. The method of making a single crystal self-supporting substrate of claim 1, wherein: the step 4) comprises the following steps: setting the temperature of HVPE equipment to be above 890 ℃, and introducing hydrogen and nitrogen-containing gas to ensure that the beta-Ga 2 O 3 The buffer layer is completely decomposed to realize the separation of the GaN epitaxial layer and the substrate, wherein the beta-Ga 2 O 3 The products of the buffer layer decomposition are all gaseous.
6. The method of making a single crystal self-supporting substrate of claim 1, wherein: the step 4) comprises the following steps: the temperature of HVPE equipment is reduced to 600-890 ℃, and hydrogen and nitrogen-containing gas are introduced to lead beta-Ga 2 O 3 The buffer layer is completely decomposed to realize the separation of the GaN epitaxial layer and the substrate, wherein the beta-Ga 2 O 3 The products of the buffer layer decomposition include liquid gallium.
7. Method for producing a monocrystalline self-supporting substrate according to claim 5 or 6, characterized in that: the flow ratio of the hydrogen gas to the nitrogen-containing gas is 1.
8. Method for producing a monocrystalline self-supporting substrate according to claim 5 or 6, characterized in that: and 4) the nitrogen-containing gas in the step 4) comprises one or two of ammonia gas and nitrogen gas.
9. The method of making a single crystal self-supporting substrate of claim 1, wherein: the step 4) comprises the following steps: reducing the temperature of HVPE equipment to below 600 ℃, and introducing hydrogenReacting beta-Ga 2 O 3 The buffer layer is completely decomposed to realize the separation of the GaN epitaxial layer and the substrate, wherein the beta-Ga 2 O 3 The products of the buffer layer decomposition include liquid gallium.
10. The method of making a single crystal self-supporting substrate of claim 1, wherein: the target thickness in step 5) is greater than or equal to 250 micrometers.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116314278A (en) * | 2023-05-22 | 2023-06-23 | 江西兆驰半导体有限公司 | High electron mobility transistor epitaxial structure, preparation method and HEMT device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116314278A (en) * | 2023-05-22 | 2023-06-23 | 江西兆驰半导体有限公司 | High electron mobility transistor epitaxial structure, preparation method and HEMT device |
| CN116314278B (en) * | 2023-05-22 | 2023-08-15 | 江西兆驰半导体有限公司 | High electron mobility transistor epitaxial structure, preparation method and HEMT device |
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