CN110896024A - Silicon carbide epitaxial gallium oxide film method and silicon carbide epitaxial gallium oxide film structure - Google Patents
Silicon carbide epitaxial gallium oxide film method and silicon carbide epitaxial gallium oxide film structure Download PDFInfo
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Abstract
The invention discloses a method for extending a gallium oxide film by silicon carbide, which comprises the following steps: selecting a silicon carbide substrate layer; preparing (Al) on the surface of the silicon carbide substrate layerxGa1‑x)2O3A buffer layer; in the presence of (Al)xGa1‑x)2O3Preparation of Ga on the surface of buffer layer2O3A thin film layer. The preparation method of the epitaxial gallium oxide film of silicon carbide provided by the invention firstly forms (Al) on the surface of the silicon carbide substrate layerxGa1‑x)2O3Buffer layer to reduce dislocation defect due to lattice mismatch, and then (Al)xGa1‑x)2O3Ga is formed on the surface of the buffer layer2O3Thin film layer to improve subsequent Ga growth2O3The crystallinity of the thin film layer finally realizes the preparation of high-crystalline Ga on the silicon carbide substrate layer2O3The structure of the film material.
Description
Technical Field
The invention belongs to the technical field of microelectronics, and particularly relates to a silicon carbide epitaxial gallium oxide film method and a silicon carbide epitaxial gallium oxide film structure.
Background
In recent years, Ga as a third generation semiconductor2O3The material has a large forbidden band width, a high breakdown electric field strength and a small on-resistance, so that the material is widely concerned by people and is the best material for developing power devices. Ga can be prepared by a method of high temperature or the like at present2O3And Ga having excellent optical properties and electrical properties which can be homoepitaxially grown thereon2O3The thin film can be used as a power electronic device, an ultraviolet photoelectric detector and an ultraviolet sensor with high performance, and has wide application prospect, however, the application of the power electronic device at high temperature is limited due to the lower thermal conductivity of the thin film.
SiC has excellent performance as the third-generation semiconductor material and has higher thermal conductivity, SiC and Ga2O3Not only can exert their respective advantages, but also can solve the problem of low thermal conductivity of gallium oxide, however, SiC and Ga2O3The existence of many defects due to large lattice mismatch limits its wide application.
Thus, SiC and Ga are solved2O3Growing gallium oxide film with high crystallization quality on the silicon carbide substrate due to defect problem caused by lattice mismatch, for future SiC and Ga2O3The combination of materials has great significance in the application of power electronic devices in high-temperature environments.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for extending a gallium oxide film by silicon carbide and a gallium oxide film structure by silicon carbide extension. The technical problem to be solved by the invention is realized by the following technical scheme:
a method of epitaxial growth of gallium oxide films on silicon carbide comprising:
selecting a silicon carbide substrate layer;
preparing (Al) on the surface of the silicon carbide substrate layerxGa1-x)2O3A buffer layer;
in the presence of (Al)xGa1-x)2O3Preparation of Ga on the surface of buffer layer2O3A thin film layer.
In one embodiment of the present invention, the (Al) isxGa1-x)2O3The value range of x in the buffer layer is 0.18-0.46.
In one embodiment of the present invention, the (Al) is prepared on the surface of the silicon carbide substrate layerxGa1-x)2O3A buffer layer, comprising:
sputtering Ga on the surface of the silicon carbide substrate layer by utilizing a magnetron sputtering process2O3Target material and Al2O3Target formation (Al)xGa1-x)2O3；
To the silicon carbide substrate layer and (Al) on the surface of the silicon carbide substrate layerxGa1-x)2O3Annealing to form the (Al)xGa1-x)2O3A buffer layer.
In one embodiment of the present invention, the sputtering gas of the magnetron sputtering process comprises oxygen and argon.
In one embodiment of the present invention, a magnetron sputtering process is used to sputter Ga on the surface of the silicon carbide substrate layer2O3Target material and Al2O3Target formation (Al)xGa1-x)2O3The method comprises the following steps:
under vacuum degree of 4X 10-4～6×10-4Sputtering Ga on the surface of the silicon carbide substrate layer by utilizing a magnetron sputtering process under the condition of Pa2O3Target material and Al2O3Target formation (Al)xGa1-x)2O3Wherein the Ga is sputtered2O3The sputtering power of the target material is 60W, and the Al is sputtered2O3The sputtering power of the target is 70W-100W.
In one embodiment of the invention, the silicon carbide substrate layer and (Al) on the surface of the silicon carbide substrate layerxGa1-x)2O3Annealing to form the (Al)xGa1-x)2O3A buffer layer, comprising:
sequentially subjecting the silicon carbide substrate layer and (Al) on the surface of the silicon carbide substrate layer in an oxygen, vacuum and nitrogen environmentxGa1-x)2O3Annealing to form the (Al)xGa1-x)2O3A buffer layer.
In one embodiment of the present invention, in the (Al)xGa1-x)2O3Formation of Ga on the surface of the buffer layer2O3A film layer, comprising:
using magnetron sputtering technique on the (Al)xGa1-x)2O3Sputtering Ga on the surface of the buffer layer2O3Target material generation of Ga2O3A thin film layer.
In one embodiment of the present invention, the (Al) is formed by a magnetron sputtering processxGa1-x)2O3Sputtering Ga on the surface of the buffer layer2O3Target material generation of Ga2O3A film layer, comprising:
in a vacuum degree of 4.8X 10-4～7×10-4Under the condition of Pa, the (Al) is treated by a magnetron sputtering processxGa1-x)2O3Sputtering Ga on the surface of the buffer layer2O3Target material generation of Ga2O3And the sputtering target material base distance is 5cm, and the working current is 2A.
In one embodiment of the invention, the thickness of the silicon carbide substrate layer is 300-700 mu m, and the (Al) isxGa1-x)2O3The thickness of the buffer layer is 100 +/-5 nm, and the Ga2O3The thickness of the thin film layer is 300 +/-5 nm.
An embodiment of the present invention further provides a silicon carbide epitaxial gallium oxide thin film structure, which is prepared by using the method for preparing a silicon carbide epitaxial gallium oxide thin film according to any one of the above embodiments, wherein the silicon carbide epitaxial gallium oxide thin film structure includes:
a silicon carbide substrate layer;
(AlxGa1-x)2O3the buffer layer is positioned on the surface of the silicon carbide substrate layer;
Ga2O3a thin film layer on the (Al)xGa1-x)2O3On the surface of the buffer layer.
The invention has the beneficial effects that:
the preparation method of the epitaxial gallium oxide film of silicon carbide provided by the invention firstly forms (Al) on the surface of the silicon carbide substrate layerxGa1-x)2O3Buffer layer to reduce dislocation defect due to lattice mismatch, and then (Al)xGa1-x)2O3Ga is formed on the surface of the buffer layer2O3Thin film layer to improve subsequent Ga growth2O3The crystallinity of the thin film layer finally realizes the preparation of high-crystalline Ga on the silicon carbide substrate layer2O3The structure of the film material.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing a GaN epitaxial silicon carbide film according to an embodiment of the invention;
FIG. 2 is a schematic flow chart of a method for epitaxial growth of gallium oxide thin film on silicon carbide according to an embodiment of the present invention;
FIGS. 3 a-3 c are schematic diagrams of a method for epitaxial growth of gallium oxide thin film on silicon carbide according to an embodiment of the present invention;
FIG. 4 shows an embodiment of the present invention with (Al)xGa1-x)2O3Buffer layer annealing environment schematic diagram;
fig. 5 is a schematic diagram of a structure of a gan epitaxial silicon carbide film according to an embodiment of the present invention.
Description of reference numerals:
a silicon carbide substrate layer-1; (Al)xGa1-x)2O3A buffer layer-2; ga2O3Film layer-3; a radio frequency power supply-4; a target material container-5; a target baffle-6; an air inlet-7; an air exhaust pipeline-8; a substrate baffle-9; a tray-10; the substrate is heated by the heating disc-11; a rotary machine-12; sputtering chamber-13.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Example one
Before describing the method for preparing a silicon carbide epitaxial gallium oxide thin film provided by the embodiment, the embodiment first provides an apparatus for preparing a silicon carbide epitaxial gallium oxide thin film, please refer to fig. 1, fig. 1 is a schematic structural diagram of the apparatus for preparing a silicon carbide epitaxial gallium oxide thin film provided by the embodiment of the present invention, and the apparatus includes a radio frequency power source 4, two target containers 5, two target baffles 6, a gas inlet 7, a gas exhaust duct 8, a substrate baffle 9, a tray 10, a substrate heating plate 11, a rotator 12 and a sputtering chamber 13. A radio frequency power supply 4 is connected to the target material container 5 through the sputtering chamber 13 for providing a power supply for the sputtering target material. The target container 5 is used for placing sputtering target materials, and the two target material baffle plates 6 are respectively arranged above the two target material containers 5. The gas inlet 7 can be provided with a plurality of gas pipelines respectively filled with different gases, and in the embodiment, the gas inlet 7 can be filled with sputtering gas oxygen and argon gas at the same time. The evacuation line 8 is connected to a vacuum system for evacuating the sputtering chamber 13. The lower end of the rotating machine 12 is sequentially connected with the substrate heating plate 11 and the tray 10, so that the substrate heating plate 11 and the tray 10 can rotate simultaneously, and the uniformity of a deposited film on the surface of the substrate in the sputtering process is guaranteed.
The method for preparing the epitaxial gallium oxide film of silicon carbide provided by the embodiment of the invention can be prepared based on the above-mentioned equipment, and can also be prepared based on other equipment, which is not specifically limited in this embodiment.
In order to better describe the method for preparing the epitaxial gallium oxide thin film of silicon carbide provided in this embodiment, this embodiment describes a method for preparing an epitaxial gallium oxide thin film of silicon carbide on the basis of the above apparatus for preparing an epitaxial gallium oxide thin film of silicon carbide, please refer to fig. 2, where fig. 2 is a schematic flow diagram of a method for preparing an epitaxial gallium oxide thin film of silicon carbide provided in an embodiment of the present invention, and the method for preparing an epitaxial gallium oxide thin film of silicon carbide specifically includes the following steps:
s1, please refer to fig. 3a, selecting a silicon carbide substrate layer 1;
specifically, the production technology of the silicon carbide substrate layer is mature, and the quality of the prepared device is good; in addition, the silicon carbide has high thermal conductivity and good stability, and can be applied to the high-temperature growth process; finally, silicon carbide has excellent physicochemical properties, and the combination with gallium oxide enables high-power electronic devices with high performance. Therefore, the substrate layer of the present embodiment is made of silicon carbide.
Further, the thickness of the silicon carbide substrate layer is 300-700 mu m, and preferably the thickness of the silicon carbide substrate layer is 500 mu m.
S2, please refer to FIG. 3b, prepared on the surface of the silicon carbide substrate layer 1 (Al)xGa1-x)2O3 A buffer layer 2;
s21, sputtering Ga on the surface of the silicon carbide substrate layer by utilizing a magnetron sputtering process2O3Target material and Al2O3Target formation (Al)xGa1-x)2O3The magnetron sputtering process utilizes the interaction of a magnetic field and an electric field to enable electrons to run spirally near the surface of a target, so that the probability that the electrons collide with argon gas to generate ions is increased, and the generated ions collide with the surface of the target under the action of the electric field to sputter out the target. Since the radius of Al atoms is smaller than that of Ga atoms, Al is doped into Ga2O3Form (Al)xGa1-x)2O3Resulting in a decrease of the lattice constant, and in the case of an appropriate value of x, (Al)xGa1-x)2O3With SiC and (Al)xGa1-x)2O3And Ga2O3The mismatching degree of the lattice constant between the two is small, so that the defect density caused by dislocation can be reduced.
Specifically, oxygen and argon are first used asSputtering gas is simultaneously introduced into the sputtering cavity; then utilizing magnetron sputtering technology to simultaneously sputter Ga on the surface of the silicon carbide substrate layer2O3Target material and Al2O3Target material to form (Al) on the surface of the silicon carbide substrate layerxGa1-x)2O3。
Preferably, (Al)xGa1-x)2O3Wherein x is in the range of 0.18-0.46. When the value of x is in the range of 0.18-0.46, (Al) can be ensuredxGa1-x)2O3With SiC and (Al)xGa1-x)2O3And Ga2O3The mismatching degree of the lattice constant between the two is small, so that the defect density caused by dislocation can be reduced. If the value of X is too small, the effect of reducing the lattice constant is not achieved, but if the value of X is too large, phase transformation occurs due to limited saturation of the alloy compound, and the effect of reducing the lattice constant and reducing dislocation is not achieved.
Further, the purity of oxygen and argon in percentage by mass is 99.999%, and the flow rate of oxygen can be 2cm3A/second; the flow rate of argon gas may be 20cm3Second while Ga2O3Target material and Al2O3The mass ratio purity of the target material is more than 99.99 percent.
In addition, this example is on the preparation of (Al)xGa1-x)2O3The conditions of the magnetron sputtering process provided by the buffer layer comprise: substrate temperature (i.e., substrate layer heating temperature), degree of vacuum, Ga2O3Sputtering power of target material, Al2O3Sputtering power of the target, sputtering target base distance and sputtering duration. Wherein the sputtering target base distance refers to the distance between the sputtering target and the silicon carbide substrate layer. The substrate temperature was room temperature. This example is on the preparation of (Al)xGa1-x)2O3The magnetron sputtering process conditions for the buffer layer are preferably: the substrate temperature is 25 ℃; the vacuum degree is 4.8 multiplied by 10-4～7×10-4Pa, preferably 5.0X 10-4Pa；Ga2O3The sputtering power of the target is 60W; al (Al)2O3The sputtering power of the target is 70W-100W; the sputtering target base distance is 5 cm; the sputtering time was 1 hour. In this embodiment, since (Al) having a suitable lattice constant is to be grownxGa1-x)2O3The crystal lattice constant of the SiC substrate can be similar to that of the SiC substrate, the range of x determines the change of the crystal lattice constant, the value range of x is determined by experimental growth conditions, and the appropriate crystal lattice constant (Al) can be grown only under the conditions through a large number of experimentsxGa1-x)2O3That is, the value of x can be made to range from 0.18 to 0.46 only under the above conditions.
This example is achieved by setting different Al2O3The sputtering power of the target can obtain (Al) with different Al componentsxGa1-x)2O3A material. When Al is present2O3(Al) produced when the sputtering power of the target is adjusted within a range of 70W to 100WxGa1-x)2O3The value of x in the material is in the range of 0.18-0.46. For example, when Al2O3When the sputtering power of the target is 75W, x is 0.21; when Al is present2O3When the sputtering power of the target is 80W, x is 0.27; when Al is present2O3When the target sputtering power was 90W, x was 0.31.
Preferably, (Al)xGa1-x)2O3The thickness of the buffer layer is 100 +/-5 nm. (Al)xGa1-x)2O3If the thickness of the buffer layer is too small, Ga tends to be adversely affected due to large crystal grains2O3Growth of thin film layers, and if too thick, SiC/Ga is affected2O3Performance of heterojunction devices.
S22, and a silicon carbide substrate layer and (Al) on the surface of the silicon carbide substrate layerxGa1-x)2O3Annealing to form (Al)xGa1-x)2O3A buffer layer.
Specifically, referring to fig. 4, a silicon carbide substrate layer and (Al) on the surface of the silicon carbide substrate layer are sequentially subjected to oxygen, vacuum and nitrogen environmentsxGa1-x)2O3Annealing treatment is carried out to enable (Al)xGa1-x)2O3Is changed into (Al)xGa1-x)2O3Buffer layer of prepared (Al)xGa1-x)2O3The buffer layer has the structural characteristics of amorphous and nanocrystalline. Annealing first under oxygen mainly for the purpose of reduction (Al)xGa1-x)2O3Concentration of oxygen vacancies in the buffer layer, followed by annealing in vacuum, is primarily for enhancement (Al)xGa1-x)2O3The crystalline quality of the buffer layer, finally annealed in nitrogen, is mainly to improve (Al)xGa1-x)2O3And the conductive performance of the buffer layer.
Further, the temperature of the annealing treatment in the embodiment is 600 ± 5 ℃, preferably 600 ℃, the annealing time in oxygen is 2 hours, the annealing time in vacuum is 1 hour, the annealing time in nitrogen is 2 hours, and when the annealing time is short, the film cannot fully react and is not beneficial to recrystallization; when the time is longer, the internal stress of the film is larger, so that the film is broken, and therefore, the proper annealing time is required.
S3, please see 3c, in (Al)xGa1-x)2O3Ga is formed on the surface of the buffer layer 22O3A thin film layer 3;
specifically, the (Al) is prepared by magnetron sputtering processxGa1-x)2O3Sputtering Ga on the surface of the buffer layer2O3Target material generation of Ga2O3A thin film layer.
Further, argon gas is first introduced into the sputtering chamber as a sputtering gas, wherein the argon gas has a purity of 99.999% by mass and a flow rate of 20cm, for example3A/second; then utilizing magnetron sputtering technology to (Al)xGa1-x)2O3Sputtering Ga on the surface of the buffer layer2O3Target material generation of Ga2O3A thin film layer.
Preferably, Ga2O3The mass specific purity of the target material is more than 99.99 percent.
In addition, this example was carried out to prepare Ga2O3The conditions of the magnetron sputtering process provided by the film layer comprise: vacuum degree, sputtering target base distance and working current. This example is in the preparation of Ga2O3The magnetron sputtering process conditions in the thin film layer are as follows: the vacuum degree is 4.8 multiplied by 10-4～7×10-4Pa, preferably 5.0X 10-4Pa, sputtering target base distance of 5cm, working current of 2A, and if vacuum degree is lower, impurity gas in the chamber is more, which can pollute Ga prepared2O3And when the vacuum degree is higher, the required time is increased, which is not beneficial to the experiment.
Preferably, Ga2O3The thickness of the thin film layer is 300 +/-5 nm. Ga2O3Too thick a film thickness will result in SiC/Ga2O3The performance of the heterojunction device is affected.
The method for preparing the silicon carbide epitaxial gallium oxide film provided by the embodiment of the invention is to prepare the material (Al) on the silicon carbide substrate layerxGa1-x)2O3The buffer layer can reduce the defects caused by lattice mismatch between the buffer layer and the silicon carbide substrate layer after annealing treatment is sequentially carried out in oxygen, vacuum and nitrogen environments, thereby being more beneficial to preparing Ga with high crystallization quality at proper temperature2O3A thin film layer.
Example two
Referring to fig. 5, fig. 5 is a schematic view of a structure of a gan epitaxial silicon carbide film according to an embodiment of the present invention. The embodiment of the invention provides a silicon carbide epitaxial gallium oxide film structure, which comprises: silicon carbide substrate layer 1, (Al)xGa1-x)2O3Buffer layer 2 and Ga2O3A thin film layer 3 of, wherein (Al)xGa1-x)2O3A buffer layer 2 is arranged on the surface of the silicon carbide substrate layer 1, Ga2O3The thin film layer 3 is located at (Al)xGa1-x)2O3On the surface of the buffer layer 2.
The silicon carbide epitaxial gallium oxide thin film structure of the embodiment is prepared by using the silicon carbide epitaxial gallium oxide thin film method provided by the above embodiment, and the implementation principle and the technical effect are similar, and are not described again
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples described in this specification can be combined and combined by those skilled in the art.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (10)
1. A method for epitaxial growth of gallium oxide film on silicon carbide is characterized by comprising the following steps:
selecting a silicon carbide substrate layer;
preparing (Al) on the surface of the silicon carbide substrate layerxGa1-x)2O3A buffer layer;
in the presence of (Al)xGa1-x)2O3Preparation of Ga on the surface of buffer layer2O3A thin film layer.
2. The method of claim 1, wherein the (Al) is selected from the group consisting ofxGa1-x)2O3The value range of x in the buffer layer is 0.18-0.46.
3. The method of claim 2, wherein (Al) is prepared on the surface of the silicon carbide substrate layerxGa1-x)2O3A buffer layer, comprising:
sputtering Ga on the surface of the silicon carbide substrate layer by utilizing a magnetron sputtering process2O3Target material and Al2O3Target formation (Al)xGa1-x)2O3；
To the silicon carbide substrate layer and (Al) on the surface of the silicon carbide substrate layerxGa1-x)2O3Annealing to form the (Al)xGa1-x)2O3A buffer layer.
4. The method of epitaxial gallium oxide films of silicon carbide according to claim 3, wherein the sputtering gases of the magnetron sputtering process comprise oxygen and argon.
5. The method of claim 4, wherein the Ga is sputtered on the surface of the SiC substrate layer by magnetron sputtering2O3Target material and Al2O3Target formation (Al)xGa1-x)2O3The method comprises the following steps:
under vacuum degree of 4X 10-4～6×10-4Sputtering Ga on the surface of the silicon carbide substrate layer by utilizing a magnetron sputtering process under the condition of Pa2O3Target material and Al2O3Target formation (Al)xGa1-x)2O3Wherein the Ga is sputtered2O3The sputtering power of the target material is 60W, and the Al is sputtered2O3The sputtering power of the target is 70W-100W.
6. The method of claim 3, wherein the silicon carbide substrate layer and the (Al) on the surface of the silicon carbide substrate layer are treatedxGa1-x)2O3Annealing to form the (Al)xGa1-x)2O3A buffer layer, comprising:
sequentially subjecting the silicon carbide substrate layer and (Al) on the surface of the silicon carbide substrate layer in an oxygen, vacuum and nitrogen environmentxGa1-x)2O3Annealing to form the (Al)xGa1-x)2O3A buffer layer.
7. The method of claim 1, wherein the step of growing the gallium oxide film on the silicon carbide substrate is carried out in the presence of (Al)xGa1-x)2O3Formation of Ga on the surface of the buffer layer2O3A film layer, comprising:
using magnetron sputtering technique on the (Al)xGa1-x)2O3Sputtering Ga on the surface of the buffer layer2O3Target material generation of Ga2O3A thin film layer.
8. The method of claim 7, wherein the (Al) is applied by magnetron sputteringxGa1-x)2O3Sputtering Ga on the surface of the buffer layer2O3Target material generation of Ga2O3A film layer, comprising:
in a vacuum degree of 4.8X 10-4～7×10-4Under the condition of Pa, the (Al) is treated by a magnetron sputtering processxGa1-x)2O3Sputtering Ga on the surface of the buffer layer2O3Target material generation of Ga2O3And the sputtering target material base distance is 5cm, and the working current is 2A.
9. The method of claim 1, wherein the thickness of the silicon carbide substrate layer is 300-700 μm, and the (Al) isxGa1-x)2O3The thickness of the buffer layer is 100 +/-5 nm, and the Ga2O3The thickness of the thin film layer is 300 +/-5 nm.
10. A silicon carbide epitaxial gallium oxide thin film structure prepared by the method of preparing a silicon carbide epitaxial gallium oxide thin film according to any one of claims 1 to 9, wherein the silicon carbide epitaxial gallium oxide thin film structure comprises:
a silicon carbide substrate layer;
(AlxGa1-x)2O3the buffer layer is positioned on the surface of the silicon carbide substrate layer;
Ga2O3a thin film layer on the (Al)xGa1-x)2O3On the surface of the buffer layer.
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