CN111128689B - Polarity control method, nitride film preparation method and nitride film - Google Patents
Polarity control method, nitride film preparation method and nitride film Download PDFInfo
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- CN111128689B CN111128689B CN201911408963.4A CN201911408963A CN111128689B CN 111128689 B CN111128689 B CN 111128689B CN 201911408963 A CN201911408963 A CN 201911408963A CN 111128689 B CN111128689 B CN 111128689B
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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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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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Abstract
The embodiment of the application provides a polarity control method, a nitride film preparation method and a nitride film, and relates to the technical field of semiconductors. The polarity control method grows an interface layer having an inverted center of symmetry on a single crystal substrate for providing a nitrogen polarity surface, wherein atoms of the single crystal substrate in a vertical direction have a hexagonal close-packed arrangement. By growing an interface layer having an inverted center of symmetry on the single crystal substrate, effective control of nitrogen polarity can be achieved.
Description
Technical Field
The application relates to the technical field of semiconductors, in particular to a polarity control method, a nitride film preparation method and a nitride film.
Background
Group III nitride semiconductor materials having a zincblende structure exhibit polarity due to lack of inversion symmetry in the [0001] direction, and are referred to as metal polarity in the [0001] polarization direction and nitrogen polarity in the [000-1] direction. Polarity is an important property of group iii nitride semiconductor materials (e.g., alN, gaN, inN, etc.) and has a significant impact on material growth and device performance. Conventional gallium nitride-based electronic and optoelectronic devices are metallic in polarity because high quality metallic materials are easier to grow and polarity is easier to control. The nitride semiconductor film with nitrogen polarity and the device thereof are receiving more and more attention because of having a polarization electric field opposite to the metal polarity, and the application of the nitride semiconductor film with nitrogen polarity and the device thereof in the high electron mobility transistor can bring lower contact resistance, higher voltage endurance capability and faster switching frequency to the device.
Compared with the growth of metal polar films, the growth of high-quality nitrogen polar III-group nitride films and device structures on sapphire, silicon carbide, silicon and other substrates by adopting metal organic gas phase epitaxy or molecular beam epitaxy has certain challenges, and one of the challenges is the control of nitrogen polarity. How to achieve control over nitrogen polarity is a considerable problem to be investigated.
Disclosure of Invention
In view of the above, embodiments of the present application provide a polarity control method, a nitride thin film preparation method, and a nitride thin film to solve the above problems.
The embodiment of the application can be realized as follows:
in a first aspect, an embodiment provides a polarity control method, including:
growing an interface layer having an inverted center of symmetry on a single crystal substrate, the interface layer for providing a nitrogen polar group iii nitride film growth surface, wherein atoms of the single crystal substrate in a vertical direction have a hexagonal close-packed arrangement.
In an alternative embodiment, the single crystal substrate is a silicon substrate.
In an alternative embodiment, the single crystal substrate is a single crystal substrate prepared with a group iii nitride having a metal polarity.
In an alternative embodiment, the step of growing an interface layer having an inverted center of symmetry on a single crystalline substrate comprises:
and generating an interface layer with an inverted symmetry center on the single crystal substrate based on a surface oxidation process, wherein the interface layer is a metal oxide thin film with an oxygen polarity surface.
In an alternative embodiment, the step of growing an interface layer having an inverted center of symmetry on a monocrystalline substrate comprises:
introducing a metal source and a nitrogen source based on a metal organic gas phase epitaxy method or a molecular beam epitaxy method, and depositing an interface layer with an inversion symmetry center on the monocrystal substrate;
in a second aspect, embodiments provide a method of fabricating a nitride film, wherein an interfacial layer is formed by using the polarity control method of any one of the previous embodiments, wherein the interfacial layer is configured to provide a nitrogen polar surface.
In an alternative embodiment, the method further comprises:
and growing a group III nitride film with nitrogen polarity on the interface layer based on a vapor phase epitaxy method.
In an alternative embodiment, the step of growing a group iii nitride film having nitrogen polarity on the interfacial layer based on vapor phase epitaxy comprises:
growing a nitrogen polarity protection layer on the interface layer to protect the interface layer from decomposition;
and a group III nitride film grown on the nitrogen polar protective layer based on a vapor phase epitaxy method.
In an alternative embodiment, the nitrogen polarity protection layer is grown at the same temperature as the interfacial layer.
In a third aspect, embodiments provide a nitride film formed by the method of any one of the preceding embodiments.
The embodiment of the application provides a polarity control method, a nitride film preparation method and a nitride film, wherein an interface layer with an inversion symmetry center is grown on a single crystal substrate, so that the nitrogen polarity is effectively controlled.
Drawings
To more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and those skilled in the art can also obtain other related drawings based on the drawings without inventive efforts.
FIG. 1 is a schematic structural diagram of a single crystal substrate provided in an embodiment of the present application;
FIG. 2 is a schematic view of the structure of an embodiment of the present application after an interfacial layer is grown on a single crystal substrate;
FIG. 3 is a schematic structural diagram of an embodiment of the present invention after a nitrogen polarity layer is grown on the interfacial layer;
FIG. 4 is a flow chart illustrating the sub-steps of a method for fabricating a nitride thin film provided in an embodiment of the present application;
FIG. 5 is a schematic structural diagram of an embodiment of the present invention after a nitrogen polarity layer is grown on the interfacial layer;
fig. 6 is a schematic structural diagram of a nitrogen polar layer grown on the nitrogen polar protection layer in the embodiment of the present application.
An icon: 1-a single crystal substrate; 2-an interfacial layer; a 3-group III nitride film; a 4-nitrogen polar protective layer.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. The components of the embodiments of the present application, generally described and illustrated in the figures herein, can be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present application, presented in the accompanying drawings, is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
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.
In the description of the present application, it should be noted that if the terms "upper", "lower", "inside", "outside", etc. are used for indicating the orientation or positional relationship based on the orientation or positional relationship shown in the drawings or the orientation or positional relationship which the present invention product is usually put into use, it is only for convenience of describing the present application and simplifying the description, but it is not intended to indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation and be operated, and thus, should not be construed as limiting the present application.
It should be noted that the features of the embodiments of the present application may be combined with each other without conflict.
Currently, the growth of nitrogen polar thin films is generally carried out by the following three methods:
the first is to directly grow a nitrogen polar film on a substrate, for example, to grow nitrogen polar gallium nitride on the surface of a sapphire substrate by a surface nitridation process, to grow a metal polar film on the Si-face of a SiC substrate, to grow a nitrogen polar film on the C-face, and the like. It is currently more difficult to directly grow nitrogen-polar films on silicon substrates.
Secondly, a polarity reversal technology is adopted: a metal polar film is firstly grown on a substrate, and then magnesium is heavily doped, namely, magnesium atoms (generally more than 10 percent) are doped in high concentration in the process of growing the III-nitride semiconductor single crystal film 20 /cm 3 ) Thereby introducing a large number of reversed polarity domain areas to realize the growth of the nitrogen polarity film. A disadvantage of this approach is that there is a polar transition layer between the metal polar face and the nitrogen polar face of a thickness typically between 20nm and 200nm (depending on doping concentration and temperature), which in some applications will affect the band structure of the device or the electron/hole transport at the interface.
The third method is a substrate lift-off technique: after a film structure with metal polarity grows on a substrate, the film structure is bonded with another supporting substrate, then an epitaxial substrate is removed, and the original film structure with metal polarity is inverted, so that a nitrogen polarity surface is exposed. The method has the advantages of complex process, low repeatability and higher cost, and is not generally adopted.
Thus, how to control the nitrogen polarity is a considerable problem to be solved.
Based on the above findings, embodiments of the present application provide a polarity control method that controls nitrogen polarity by growing an interface layer having an inversion symmetry center on a single crystal substrate to provide a nitrogen polarity surface for growing a nitride thin film. The above method is explained in detail below.
Referring to fig. 1, fig. 1 is a schematic structural diagram of a single crystal substrate 1 according to an embodiment of the present disclosure. Referring to fig. 2, the present embodiment provides a polarity control method, including:
an interface layer 2 having an inverted center of symmetry is generated on a single crystal substrate 1, the interface layer 2 for providing a nitrogen polar group iii nitride film growth surface, wherein atoms of the single crystal substrate 1 in a vertical direction have a hexagonal close-packed arrangement.
After the interface layer 2 is formed on the single crystal substrate 1, the single crystal substrate 1 and the interface layer 2 have a schematic structure as shown in fig. 2.
The hexagonal close-packed arrangement structure is a closest packing mode of the isodiametric spheres, the spheres are packed according to the ABABAB … … layer sequence, and the sphere centers of the spheres are connected to form a hexagonal bottom center lattice. I.e. the unit cell of the hexagonal close-packed arrangement contains six atoms. In the embodiment of the present application, a hexagonal close-packed arrangement structure is adopted to provide a surface of a hexagonal atomic structure, so as to grow an interface layer 2 having an inversion symmetry center, and realize control of nitrogen polarity.
Further, since the interface layer having the inversion symmetry center can realize the inversion from the metal polarity to the nitrogen polarity on the nitride single crystal substrate of the metal polarity, in the embodiment of the present application, the interface layer 2 having the inversion symmetry center is grown so as to further realize the growth control of the nitrogen polarity group iii nitride thin film.
As an alternative embodiment, the single crystal substrate 1 may be a single crystal substrate 1 prepared with a group iii nitride having a metal polarity or a group iii nitride thin film having a metal polarity.
When the single crystal substrate 1 is the single crystal substrate 1 prepared with the group iii nitride having the metal polarity or the group iii nitride thin film having the metal polarity, the interface layer 2 having the inversion symmetry center can be generated on the single crystal substrate 1 by the following method.
Generating an interface layer 2 with an inverted symmetry center on the single crystal substrate 1 based on a surface oxidation process, wherein the interface layer 2 is a metal oxide thin film with an oxygen polarity surface.
Alternatively, the surface oxidation process may be a thermal oxidation process, in which a metal oxide film is grown on the surface in an oxygen-containing atmosphere at a high temperature (600 ℃ to 1200 ℃). The specific principle can refer to the prior art, and is not described herein.
In one implementation, the surface oxidation process may also be an oxygen plasma surface treatment process. The plasma, which is the fourth state of the substance, is an ionized gaseous substance consisting of atoms from which some electrons have been deprived and positive and negative electrons generated by ionization of the atoms. The ionized gas is composed of atoms, molecules, atomic groups, ions and electrons. The plasma surface coating film can be coated on the surface of the object by acting on the surface of the object.
In one implementation, the surface oxidation process may also be performed by introducing an oxygen-containing gas and a metal-containing source into the reaction chamber at a high temperature to react sufficiently to grow a metal oxide film, such as Ga, on the surface of the single crystal substrate 1 2 O 3 The thin oxide layer has an oxygen-polar surface, i.e., the interface layer 2.
Thus, the polarity of the metal can be rapidly reversed to the polarity of nitrogen on the single crystal substrate 1 having the polarity of the metal, thereby avoiding the problem of a thick polarity transition layer when the polarity reversing process is implemented by using a magnesium heavy doping technology as in the prior art. Thus, nitrogen polarity control is realized, thereby improving the performance of the device.
As another alternative embodiment, the single crystal substrate 1 may be a silicon substrate.
When the single crystal substrate 1 is a silicon substrate, on the one hand, the interface layer 2 having an inverted center of symmetry can be generated on the single crystal substrate 1 by the above surface oxidation process. On the other hand, the interface layer 2 having an inversion symmetry center may be deposited on the single crystal substrate 1 by introducing a metal source and a nitrogen source based on a metal organic vapor phase epitaxy method or a molecular beam epitaxy method.
Illustratively, the apparatus may be operated by passing a source of a magnesium-containing metallorganic gas, such as Cp 2 Mg，Cp 2 Zn and nitrogen-containing gas sources, e.g. NH 3 Or N 2 Carrying out chemical reaction at the high temperature of 600-900 ℃ to generate Mg on the (111) crystal face of the silicon substrate 3 N 2 Or Zn 3 N 2 Deposited on the single crystal substrate 1, forming the above-mentioned interface layer 2.
Therefore, a nitrogen polar III-group nitride film or a nitrogen polar III-group nitride device can be directly grown on the silicon substrate, and the complexity that a metal polar film is grown firstly in the prior art and then the polarity is reversed into the nitrogen polarity through a magnesium heavy doping technology is not needed, so that the efficient nitrogen polarity control is realized.
In summary, the polarity control method provided in the embodiment of the present application realizes effective control of the nitrogen polarity by growing the interface layer 2 having an inversion symmetry center on the single crystal substrate 1 in which atoms in the vertical direction have a hexagonal close-packed arrangement structure.
Referring to fig. 3, the present embodiment further provides a method for preparing a nitride thin film, in which the interfacial layer 2 is grown by the aforementioned polarity control method, and the interfacial layer 2 is used to provide a nitrogen polar surface.
Further, the method further comprises:
a group iii nitride thin film 3 having a nitrogen polarity is grown on the interface layer 2 based on a vapor phase epitaxy method.
Fig. 3 is a schematic view of the structure after the group iii nitride thin film 3 is formed on the interfacial layer 2 by the above-mentioned method.
As an embodiment, a group iii nitride thin film 3 having nitrogen polarity may be directly grown on the interfacial layer 2 to produce a nitride thin film.
Since the interface layer 2 is thin, the surface is easily detached during the growth of the material, so that the group iii nitride thin film 3 grown on the interface layer 2 has a mixed polarity of nitrogen polarity and metal polarity.
Therefore, further, in order to avoid the interfacial layer 2 from being decomposed before the growth of the group iii nitride film 3 with nitrogen polarity, as another embodiment, please refer to fig. 4 and 5 in combination, the growth of the group iii nitride film 3 with nitrogen polarity can be realized through steps S21-S22 to complete the preparation of the nitride film.
S21, growing a nitrogen polarity protection layer 4 on the interface layer 2 to protect the interface layer 2 from being decomposed.
And S22, growing the group III nitride film 3 with the nitrogen polarity on the nitrogen polarity protection layer 4 based on a vapor phase epitaxy method.
Referring to fig. 5 and fig. 6 in combination, fig. 5 is a schematic structural diagram of the interface layer after the nitrogen polarity protection layer is grown on the interface layer in the step S21. Fig. 6 is a schematic structural view after the group iii nitride thin film 3 having a nitrogen polarity is grown on the nitrogen polarity protective layer 4 by the above-described steps S21 to S22.
Wherein the growth temperature of the nitrogen polarity protection layer 4 is the same as that of the interface layer 2, that is, at the same temperature, a nitrogen polarity protection layer 4 is grown on the interface layer 2 immediately after the interface layer 2 is prepared, conditions are changed to the growth temperature required for the group iii nitride thin film 3, and finally the group iii nitride thin film 3 having nitrogen polarity is grown on the nitrogen polarity protection layer 4, thereby preparing a nitride thin film.
Thus, the interfacial layer 2 can be prevented from being decomposed, thereby effectively controlling the polarity and improving the quality of the prepared nitride film.
The nitrogen polarity protection layer 4 may be any group iii nitride, such as GaN, inN, alN, inGaN, or AlInGaN.
Further, the above vapor phase epitaxy method may be a hydride vapor phase epitaxy method (halid-VPE, HVPE). Taking GaN film generation as an example, in the embodiment of the present application, gaCl may be used as a gallium source, and NH may be used 3 Is an N source, and a GaN film with excellent quality can be rapidly grown on the interface layer 2 or the nitrogen polar protective layer 4 at the temperature of about 1000 ℃.
The nitrogen polarity protection layer 4 may be any group iii nitride, such as GaN, inN, alN, inGaN, or AlInGaN.
Further, the above-described method for growing the group iii nitride thin film 3 or the nitrogen polarity protective layer 4 may also be a metal organic chemical vapor deposition Method (MOCVD). MOCVD is an epitaxial growth process in which a substance is transferred from a vapor phase to a solid phase, a gas containing an epitaxial film component is transported from the vapor phase onto a heated substrate or an epitaxial surface, arranged in a certain crystal structure by thermal decomposition, diffusion of gas molecules and chemical reaction near the substrate or on the epitaxial surfaceAs an epitaxial film or as a deposited layer. The growth technique generally uses III-metal organic as III-source and NH 3 As a source of N, group III nitride growth is carried out at high temperatures (typically > 1000 ℃).
Further, the above-mentioned method for growing the nitride thin film or the nitrogen polar protective layer 4 may be other, for example, a Molecular Beam Epitaxy (MBE) method in which one or more kinds of atoms constituting an epitaxial film fall onto the interface layer 2 or the nitrogen polar protective layer 4 in a vacuum in the form of atoms, atomic beams, or molecular beams like meteoric shower, and a part of them is subjected to a physical-chemical process and is orderly arranged on the surface in a certain structure to form a crystal thin film.
The embodiment of the application also provides a preparation method of the nitride film, the interface layer 2 is generated by adopting the polarity control method, and the nitrogen polarity III-group nitride film 3 is further directly grown on the interface layer 2. Alternatively, the above polarity control method is used to generate the interface layer 2, and a nitride protection layer is further grown on the interface layer 2, and further a group iii nitride thin film 3 having nitrogen polarity is grown on the nitrogen polarity protection layer 4. Thus, by controlling the nitrogen polarity, a group III nitride film having nitrogen polarity is rapidly manufactured.
The embodiment also provides a nitride film which is manufactured and formed by the nitride film manufacturing method. The preparation method of the nitride film can refer to the specific explanation of the nitride film, and is not described herein again. Thus, by controlling the nitrogen polarity, a high-quality nitride thin film is rapidly manufactured.
Further, the embodiment of the application also provides a semiconductor device which is manufactured by adopting the nitride film.
Among them, the semiconductor device may be a Light Emitting Diode (LED) made of the above nitride thin film, and since a Light and cost-effective monochromatic Light source for visible Light, especially a Laser Light source, is not currently available, there is a high demand for visible Light and semiconductor Laser Diodes (LDs). Illustratively, by combining red, green and blue light emitting diodes made of the nitride thin films, clear full color display can be obtained. At present, white flat light sources with the maximum brightness of 500cd/m can be prepared by using LEDs with ultrahigh brightness, and become a new generation of illumination light sources, the power consumption of the white flat light sources is only 10% -20% of that of incandescent lamps (the service life of the incandescent lamps is 6-12 months) with the same brightness, and the service life of the white flat light sources is 5-10 months.
The semiconductor device may also be an ultraviolet photodetector, and conventional ultraviolet-visible photodetectors, including photocathodes and solid state detectors, such as Si and SiC detectors, have provided excellent performance. However, group iii nitride (i.e., nitride films as described above) based photodetectors offer a range of superior performance that greatly exceeds conventional UV (ultraviolet) and visible light photodetectors. The main reasons include: high quantum efficiency due to their direct bandgap structure; the ability to implement a heterojunction; low surface recombination rate; an intrinsic white light blind zone; a suitably steep cut-off wavelength can be obtained by adjusting the alloy composition; and high stability in harsh physical and chemical environments. The above properties allow group iii nitride based UV and visible photodetectors to be used in many applications. The method mainly comprises the applications of flame sensing, ozone monitoring, pollution monitoring, mercury lamp disinfection monitoring, laser detectors, spaceship monitoring and identification, space communication, positioning welding, engine and combustion chamber monitoring and the like.
It is understood that other semiconductor devices, such as Laser Diodes (LDs), may also be fabricated using the above-described nitride thin films, such as group iii nitride blue LDs developed with sapphire as the substrate or SiC as the substrate. The blue-ray LD can increase the optical storage density of information and can be applied to deep sea communication, material processing and laser printing. The specific principle can refer to the prior art, and is not described herein.
Further, other semiconductor devices, such as high-frequency, high-power and high-temperature electronic devices and other devices, can be manufactured by using the nitride film, and specific principles can refer to the prior art and are not described herein again.
In summary, the present embodiment provides a polarity control method, a nitride thin film manufacturing method, and a nitride thin film, the polarity control method growing an interface layer 2 having an inversion symmetry center on a single crystal substrate 1, the interface layer 2 being used to provide a nitrogen polar surface, wherein atoms of the single crystal substrate 1 in a vertical direction have a hexagonal close-packed arrangement. In this manner, by growing the interface layer 2 having an inverted center of symmetry on the single crystal substrate 1, effective control of the nitrogen polarity is achieved.
The above description is only for the specific embodiments of the present application, but the scope of the present application is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present application should be covered within the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (8)
1. A polarity control method, characterized by comprising:
growing an interface layer having an inverted center of symmetry on a single crystal substrate, the interface layer for providing a nitrogen polar group iii nitride film growth surface, wherein atoms of the single crystal substrate in a vertical direction have a hexagonal close-packed arrangement;
growing a nitrogen polarity protection layer on the interface layer to protect the interface layer from decomposition;
and growing a group III nitride thin film having a nitrogen polarity on the nitrogen polarity protective layer based on a vapor phase epitaxy method.
2. The polarity control method according to claim 1, wherein the single crystal substrate is a silicon substrate.
3. The polarity control method according to claim 1, wherein the single crystal substrate is a single crystal substrate prepared with a group iii nitride having a metal polarity.
4. The polarity control method of claim 3, wherein the step of growing an interface layer having an inverted center of symmetry on a single crystalline substrate comprises:
and generating an interface layer with an inverted symmetry center on the single crystal substrate based on a surface oxidation process method, wherein the interface layer is a metal oxide film with an oxygen polarity surface.
5. The polarity control method according to claim 2 or 3, wherein the step of growing an interface layer having an inverted center of symmetry on a single crystalline substrate comprises:
and introducing a metal source and a nitrogen source based on a metal organic gas phase epitaxy method or a molecular beam epitaxy method, and depositing an interface layer with an inversion symmetry center on the monocrystal substrate.
6. A method for producing a nitride thin film, characterized in that an interface layer for providing a nitrogen polar surface is formed by the polarity control method according to any one of claims 1 to 5.
7. The method of claim 6, wherein the nitrogen polarity protection layer and the interfacial layer are grown at the same temperature.
8. A nitride thin film formed by the method for forming a nitride thin film according to any one of claims 6 to 7.
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| CN109599329B (en) * | 2018-12-05 | 2023-08-08 | 江西兆驰半导体有限公司 | Method for growing nitrogen polar III-nitride semiconductor layer on silicon substrate |
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