CN113130296A - Method for growing gallium nitride on hexagonal boron nitride - Google Patents
Method for growing gallium nitride on hexagonal boron nitride Download PDFInfo
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- 229910002601 GaN Inorganic materials 0.000 title claims abstract description 83
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 82
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 82
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 44
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 24
- 239000001301 oxygen Substances 0.000 claims abstract description 24
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
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- 150000002902 organometallic compounds Chemical class 0.000 claims description 3
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 239000010980 sapphire Substances 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 230000037303 wrinkles Effects 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims 1
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- 229910052682 stishovite Inorganic materials 0.000 claims 1
- 229910052905 tridymite Inorganic materials 0.000 claims 1
- 210000002381 plasma Anatomy 0.000 abstract description 12
- 239000013078 crystal Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 239000010410 layer Substances 0.000 description 31
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- 238000005411 Van der Waals force Methods 0.000 description 1
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- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
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- 238000002360 preparation method Methods 0.000 description 1
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- 238000012546 transfer Methods 0.000 description 1
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for growing gallium nitride on hexagonal boron nitride, which adopts a chemical vapor deposition method to grow hexagonal boron nitride on a copper foil; the surface of the material is continuously and uniformly wrinkled after the temperature reduction treatment; transferring the hexagonal boron nitride with folds on the copper foil to other substrates to be used as an insertion layer for growing gallium nitride; treating the hexagonal boron nitride folds by using oxygen plasma; growing a low V/III ratio gallium nitride nucleating layer by adopting a metal organic chemical vapor deposition method; and growing a gallium nitride layer with a high V/III ratio by adopting a metal organic chemical vapor deposition method. According to the invention, the hexagonal boron nitride folds are treated by adopting oxygen plasmas, defects and atomic steps are formed at the hexagonal boron nitride folds, and the edges of the hexagonal boron nitride folds are taken as nucleation points to laterally grow to form a complete and continuous gallium nitride film. The dislocation in the epitaxial layer is reduced in the lateral growth process, the crystal quality of the gallium nitride is further improved, and the method has strong practicability.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and relates to a gallium nitride film growth method based on oxygen plasma treatment of hexagonal boron nitride folds.
Background
Gallium nitride is used as a representative wide bandgap semiconductor material, is very suitable for preparing optoelectronic devices and microwave radio frequency devices due to excellent photoelectric properties and stability, and has wide prospects in the fields of illumination and display, 5G communication, high-frequency high-power photoelectric equipment and the like.
Due to the lack of a gallium nitride homogeneous substrate, most gallium nitride-based devices are mainly prepared on sapphire, silicon carbide (SiC), silicon (Si), and the like in a heteroepitaxial manner. However, due to the lattice mismatch and thermal mismatch between the heteroepitaxial substrate and the epitaxial layer, the generated large residual biaxial stress may cause cracks or even fractures in the gallium nitride material, which affects the crystal quality of gallium nitride and is not beneficial to the subsequent device preparation. Obtaining high quality, low defect gallium nitride material is the key of research.
The hexagonal boron nitride and the gallium nitride are III group nitrides, and are very suitable to be used as a substrate for growing the gallium nitride. The influence of the surface roughness of hexagonal boron nitride on the dislocation density of gallium nitride film is studied in the literature Snare Michael, et al, Journal of Crystal growth, 464(2016), and the lowest dislocation density of gallium nitride reaches 109 cm-1And the order of magnitude is far from the standard of high-quality gallium nitride. The document Kong Wei, et al, Nature materials, 17.11(2018) utilizes hexagonal boron nitride for the remote epitaxy of gallium nitride. Even with a single layer of hexagonal boron nitride, a single crystal gallium nitride film with uniform orientation cannot be obtained.
Disclosure of Invention
In order to solve the defect of poor crystal quality of a gallium nitride material on hexagonal boron nitride, the invention provides a method for growing gallium nitride on hexagonal boron nitride, which comprises the following steps:
(1) growing hexagonal boron nitride on the copper foil by adopting a chemical vapor deposition method;
(2) carrying out cooling treatment on hexagonal boron nitride on the copper foil to enable the surface of the hexagonal boron nitride to have continuous and uniform folds;
(3) transferring the hexagonal boron nitride with folds on the copper foil to other substrates; hexagonal boron nitride with folds is used as an insertion layer for growing gallium nitride;
(4) treating folds of the hexagonal boron nitride by using oxygen plasma;
(5) growing a low V/III ratio gallium nitride nucleating layer by adopting a metal organic chemical vapor deposition method;
(6) and growing a gallium nitride layer with a high V/III ratio by adopting a metal organic chemical vapor deposition method.
Hexagonal boron nitride has a hexagonal in-plane lattice arrangement, and the interlayer bonds by weak van der waals forces, and can serve as a substrate for gallium nitride growth. The interaction between hexagonal boron nitride and the epitaxial layer is two orders of magnitude weaker and the thermal conductivity better than conventional heteroepitaxy, without the need to strictly follow the lattice match. This epitaxy can relieve stress and defects caused by lattice mismatch and thermal mismatch.
And forming defects and atomic steps on the edges of the hexagonal boron nitride folds by the oxygen plasmas, and forming a complete and continuous gallium nitride film by laterally growing by taking the edges of the hexagonal boron nitride folds as nucleation points by utilizing the characteristic of high adsorption energy of the edges of the defects and the steps. The lateral growth process also reduces dislocations in the epitaxial layer, improving crystal quality.
Preferably, the number of layers of the hexagonal boron nitride is 5-30.
Preferably, the substrate for transfer is selected from one of sapphire, silicon carbide and silicon.
Preferably, the hexagonal boron nitride transferred to the substrate has a typical corrugation, the width of the hexagonal boron nitride is 50-300 nm, the height of the hexagonal boron nitride is 20-40 nm, and the hexagonal boron nitride uniformly covers the surface of the substrate.
Preferably, the oxygen flow is 50-200 sccm, the plasma power is 50-400W, and the etching time is 0.5-5 min.
Preferably, the width of the hexagonal boron nitride folds after oxygen plasma treatment is 40-200nm, the height of the hexagonal boron nitride folds is 15-30nm, and defects and atomic steps in the form of N-O and B-O dangling bonds appear on the folds. The perfect surface of the hexagonal boron nitride is damaged through the treatment of the oxygen plasma, and the folds are easier to etch, so that N-O and B-O dangling bond form defects and atomic steps are generated in space. Nucleation of gallium nitride occurs in areas where defects and atomic steps are concentrated, as this is where the surface state changes. The mode of preferential nucleation at the folds is beneficial to subsequent lateral growth, and the gallium nitride film with low dislocation density is obtained.
Preferably, the gallium nitride nucleation layer is grown by the metal organic compound vapor deposition method, the growth temperature is 450-.
Preferably, the gallium nitride layer is grown by the metal organic compound vapor deposition method, the growth temperature is 1000-1100 ℃, the V/III ratio is 20000-30000, and the growth time is 1.5-3 h.
Preferably, the gallium nitride nucleation layer preferentially nucleates along the edges of the hexagonal boron nitride folds and then grows laterally to form a flat gallium nitride film.
The invention also provides gallium nitride produced by the gallium nitride growth method. The gallium nitride layer grown by the method is stripped from the substrate by a mechanical stripping method. The method comprises the following specific steps: the heat release adhesive tape is slowly and uniformly adhered to the surface of the gallium nitride layer, the heat release adhesive tape adhered to the gallium nitride layer is completely peeled off from the substrate layer, and then the heat release adhesive tape is tightly attached to a target substrate and then heated, so that the heat release adhesive tape loses viscosity, is separated from the gallium nitride layer, and is peeled off.
Advantageous effects
Firstly, the invention adopts hexagonal boron nitride as an insertion layer, reduces lattice mismatch and thermal mismatch between the substrate and the epitaxial layer, and improves the quality of gallium nitride.
Secondly, the invention adopts oxygen plasma to treat the hexagonal boron nitride folds, and gallium nitride preferentially nucleates on the folds and then laterally grows to form a continuous film. The lateral growth of gallium nitride also reduces dislocations in the epitaxial layer, further improving the crystal quality of gallium nitride.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a schematic structural view of the present invention;
FIG. 3 is a scanning electron microscope image of a hexagonal boron nitride pleat before and after oxygen plasma treatment in accordance with the present invention;
FIG. 4 is an X-ray photoelectron spectrum of an oxygen plasma of the present invention before and after treatment of a hexagonal boron nitride pleat;
FIG. 5 is an atomic force microscope image of a low temperature gallium nitride buffer layer on hexagonal boron nitride in accordance with the present invention;
FIG. 6 is a transmission electron microscope image of a cross-section of a gallium nitride buffer layer on hexagonal boron nitride in accordance with the present invention;
FIG. 7 is an atomic force microscope image of a gallium nitride film on hexagonal boron nitride in accordance with the present invention;
FIG. 8 shows E before and after stripping of a GaN film grown on hexagonal boron nitride in accordance with the present invention2-raman spectrogram of high peak position;
FIG. 9 is a scanning electron microscope image of the bottom surface of a gallium nitride film exfoliated on hexagonal boron nitride in accordance with the present invention.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
Examples
A method for growing gallium nitride on hexagonal boron nitride, according to the steps shown in fig. 1, the structure shown in fig. 2 is grown, and the specific steps are as follows:
the method comprises the following steps: growing hexagonal boron nitride on the copper foil by adopting a chemical vapor deposition method, wherein the number of layers of the hexagonal boron nitride is 10;
step two: cooling and shrinking hexagonal boron nitride on the copper foil, enabling the surface to have continuous and uniform folds, enabling the width to be 50-300 nm and the height to be 20-40 nm, and uniformly covering the surface of the substrate;
step three: transferring the hexagonal boron nitride with folds on the copper foil to a substrate;
step four: treating the hexagonal boron nitride folds by using oxygen plasmas, wherein the oxygen flow is 100 sccm, the plasma power is 200W, and the etching time is 2 min;
referring to fig. 3, scanning electron micrographs of the oxygen plasma before and after treatment of hexagonal boron nitride as provided in this example are shown. In the figure, a shows a typical morphology of hexagonal boron nitride wrinkles; graph b shows that the hexagonal boron nitride pleats flatten out after oxygen plasma treatment. The width of the hexagonal boron nitride folds after the oxygen plasma treatment is 40-200nm, and the height of the hexagonal boron nitride folds is 15-30 nm;
referring to fig. 4, an X-ray photoelectron spectrum before and after the oxygen plasma treatment of the hexagonal boron nitride corrugation is shown. (a) Panels (B) and (c) are XPS characteristic peaks for N1s and B1s before oxygen plasma treatment of the hexagonal boron nitride pleat. (c) Panels (d) and (d) are XPS characteristic peaks for N1s and B1s after oxygen plasma treatment of the hexagonal boron nitride pleat. The result shows that the hexagonal boron nitride generates N-O bonds and B-O bonds after oxygen plasma treatment to provide nucleation sites for subsequent gallium nitride growth;
step five: growing a low V/III ratio gallium nitride nucleating layer by adopting a metal organic chemical vapor deposition method, wherein the growth temperature is 475 ℃, the V/III ratio is 6000, and the growth time is 5 min. The MOCVD technology adopts ammonia gas as a nitrogen source, hydrogen or nitrogen gas as carrier gas and trimethyl gallium as a gallium source;
referring to fig. 5, an atomic force microscope image of a gallium nitride nucleation layer provided in this example is shown; indicating that gallium nitride will nucleate preferentially along the hexagonal boron nitride folds;
referring to fig. 6, a cross-sectional tem of a gan nucleation layer provided in this example is shown; indicating that a large number of atomic steps exist at the folds of the hexagonal boron nitride;
step six: growing a gallium nitride layer with a high V/III ratio by adopting a metal organic chemical vapor deposition method, wherein the growth temperature is 1070 ℃, the V/III ratio is 25000, and the growth time is 2.5 h;
referring to fig. 7, it is an atomic force microscope image of the gallium nitride film provided in this example, which shows that the gallium nitride surface has a clear atomic step;
step seven: the grown gallium nitride layer is stripped from the substrate by a mechanical stripping method, and the method comprises the following specific steps: the heat release adhesive tape is slowly and uniformly adhered to the surface of the gallium nitride layer, the heat release adhesive tape adhered to the gallium nitride layer is completely peeled off from the substrate layer, and then the heat release adhesive tape is tightly attached to a target substrate and then heated, so that the heat release adhesive tape loses viscosity, is separated from the gallium nitride layer, and is peeled off.
Referring to FIG. 8, it shows E before and after stripping of GaN thin film grown on hexagonal boron nitride film provided in this example2Raman spectrum of high peak position. Indicating that the gallium nitride film has very little stress after peeling and is close to the unstressed state (568 cm)-1）。
Referring to FIG. 9, it is a scanning electron microscope photograph of the bottom surface of the gallium nitride film provided in this example, which shows that the grown gallium nitride film is peelable.
According to the gallium nitride growth method in the technical scheme, the hexagonal boron nitride folds are processed by the oxygen plasmas, defects and atomic steps are formed at the hexagonal boron nitride folds, and the edges of the hexagonal boron nitride folds are used as nucleation points to laterally grow to form a complete and continuous gallium nitride film. The dislocation in the epitaxial layer is reduced in the lateral growth process, the crystal quality of the gallium nitride is further improved, and the method has strong practicability.
Finally, it should be noted that: the above description is only a preferred embodiment, and it will be obvious to those skilled in the art that modifications may be made to the technical solutions described in the above embodiments, or some technical features may be replaced with equivalents. 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.
Claims (10)
1. A method for growing gallium nitride on hexagonal boron nitride is characterized by comprising the following steps:
growing hexagonal boron nitride on the copper foil by adopting a chemical vapor deposition method;
carrying out cooling treatment on hexagonal boron nitride on the copper foil to enable the surface of the hexagonal boron nitride to have continuous and uniform folds;
transferring the hexagonal boron nitride with folds on the copper foil to other substrates; hexagonal boron nitride with folds is used as an insertion layer for growing gallium nitride;
treating folds of the hexagonal boron nitride by using oxygen plasma;
growing a low V/III ratio gallium nitride nucleating layer by adopting a metal organic chemical vapor deposition method;
and growing a gallium nitride layer with a high V/III ratio by adopting a metal organic chemical vapor deposition method.
2. The method for growing gallium nitride on hexagonal boron nitride according to claim 1, wherein the number of layers of hexagonal boron nitride grown in step (1) is 5-30.
3. The method of claim 1, wherein the substrate of step (3) is selected from the group consisting of gallium nitride, sapphire, SiC, Si, AlN, and SiO2One kind of (1).
4. The method for growing gan on hexagonal boron nitride according to claim 1, wherein the folds in step (3) have a width of 50-300 nm and a height of 20-40 nm and uniformly cover the surface of the substrate.
5. The method for growing gallium nitride on hexagonal boron nitride according to claim 1, wherein the oxygen flow rate of the folds of hexagonal boron nitride in step (4) is 50-200 sccm, the plasma power is 50-400W, and the etching time is 0.5-5 min.
6. The method for growing gallium nitride on hexagonal boron nitride according to claim 1, wherein the hexagonal boron nitride after the oxygen plasma treatment in the step (4) is wrinkled, and defects and atomic steps in the form of N-O and B-O dangling bonds are formed on the wrinkles.
7. The method of claim 1, wherein the step (5) comprises growing the GaN nucleation layer by vapor deposition at a temperature of 450-.
8. The method of claim 1, wherein the step (6) employs a metal organic compound vapor deposition method to grow the GaN layer, the growth temperature is 1000-1100 ℃, the V/III ratio is 20000-30000, and the growth time is 1.5-3 h.
9. The method of claim 6, wherein the gallium nitride nucleation layer of step (5) is first nucleated along the edges of the hexagonal boron nitride corrugations and then grown laterally to form a planar gallium nitride film.
10. Gallium nitride grown on hexagonal boron nitride, produced by the method of growing gallium nitride on hexagonal boron nitride according to any one of claims 1 to 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113549898A (en) * | 2021-08-13 | 2021-10-26 | 安徽泽众安全科技有限公司 | Two-dimensional gallium nitride film domain-limited template preparation method and prepared two-dimensional gallium nitride film |
| CN114635186A (en) * | 2022-01-26 | 2022-06-17 | 西安电子科技大学 | Substrate structure with hexagonal boron nitride for assisting gallium nitride epitaxy and preparation method thereof |
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| CN105861987A (en) * | 2016-05-19 | 2016-08-17 | 西安电子科技大学 | Gallium nitride growing method based on hexagonal boron nitride and magnetron-sputtered aluminum nitride |
| CN110211869A (en) * | 2019-05-28 | 2019-09-06 | 北京大学 | Utilize the method for stress in two-dimentional boron nitride insert layer relaxation nitride epitaxial structure |
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| CN105861987A (en) * | 2016-05-19 | 2016-08-17 | 西安电子科技大学 | Gallium nitride growing method based on hexagonal boron nitride and magnetron-sputtered aluminum nitride |
| CN110211869A (en) * | 2019-05-28 | 2019-09-06 | 北京大学 | Utilize the method for stress in two-dimentional boron nitride insert layer relaxation nitride epitaxial structure |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113549898A (en) * | 2021-08-13 | 2021-10-26 | 安徽泽众安全科技有限公司 | Two-dimensional gallium nitride film domain-limited template preparation method and prepared two-dimensional gallium nitride film |
| CN113549898B (en) * | 2021-08-13 | 2023-07-25 | 安徽泽众安全科技有限公司 | Preparation method of two-dimensional gallium nitride film finite field template and prepared two-dimensional gallium nitride film |
| CN114635186A (en) * | 2022-01-26 | 2022-06-17 | 西安电子科技大学 | Substrate structure with hexagonal boron nitride for assisting gallium nitride epitaxy and preparation method thereof |
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