CN111243942A - Method for improving crystallization quality of hexagonal boron nitride by using transition metal or alloy as buffer layer - Google Patents
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- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 38
- 150000003624 transition metals Chemical class 0.000 title claims abstract description 38
- 239000000956 alloy Substances 0.000 title claims abstract description 22
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 20
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000002425 crystallisation Methods 0.000 title claims abstract description 13
- 230000008025 crystallization Effects 0.000 title claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 36
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 23
- 239000010980 sapphire Substances 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
- 238000000151 deposition Methods 0.000 claims abstract description 9
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 9
- 238000005516 engineering process Methods 0.000 claims abstract description 7
- 230000008021 deposition Effects 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 4
- 229910052802 copper Inorganic materials 0.000 claims abstract description 4
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 3
- 238000005566 electron beam evaporation Methods 0.000 claims abstract description 3
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- 238000002207 thermal evaporation Methods 0.000 claims abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 3
- 239000010408 film Substances 0.000 claims description 35
- 238000004544 sputter deposition Methods 0.000 claims description 11
- 238000000137 annealing Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 238000004518 low pressure chemical vapour deposition Methods 0.000 claims description 7
- 229910015844 BCl3 Inorganic materials 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 12
- 239000004065 semiconductor Substances 0.000 abstract description 7
- 230000000052 comparative effect Effects 0.000 description 9
- 239000011888 foil Substances 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000001534 heteroepitaxy Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
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- 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
- H01L21/02367—Substrates
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Abstract
A method for improving the crystallization quality of hexagonal boron nitride by using transition metal or alloy as a buffer layer belongs to the technical field of semiconductor material epitaxial growth. Before growing the hexagonal boron nitride epitaxial film, depositing transition metal or alloy on a silicon, sapphire or other substrate with larger lattice mismatch as a buffer layer in advance by using magnetron sputtering, electron beam evaporation, pulse laser deposition or thermal evaporation film preparation technology, and then epitaxially growing the hexagonal boron nitride film on the substrate with the buffer layer by adopting chemical vapor deposition, magnetron sputtering or pulse laser deposition technology; the buffer layer is annealed before the hexagonal boron nitride film is epitaxially grown so as to further improve the quality of the buffer layer, thereby achieving the purpose of further improving the crystallization quality of the hBN film. The buffer layer is made of transition metal alloy material formed by transition metal such as Cu, Cr, Mo, Ni, W, Mn, Co and the like or combination thereof.
Description
Technical Field
The invention belongs to the technical field of epitaxial growth of semiconductor materials, and particularly relates to a method for improving the crystallization quality of hexagonal boron nitride by using transition metal or alloy as a buffer layer.
Background
Hexagonal boron nitride (hBN) is a group iii-V wide bandgap semiconductor material with a bandgap width of about 6 eV. Due to its many excellent physical and chemical properties, such as high temperature resistance, low expansion coefficient, extremely high dielectric strength, high thermal conductivity and high chemical stability, it has potential applications in deep ultraviolet light electronics and high power electronics. Due to the shortage of hBN substrate materials, most hBN thin film materials are prepared by heteroepitaxy on foreign substrates, which mainly include silicon, sapphire and transition metal foils. Silicon and sapphire materials are substrate materials commonly used for manufacturing MOS (metal oxide semiconductor) devices, LED (light emitting diode) devices and the like in the semiconductor industry, and heteroepitaxy hBN film on the silicon and sapphire substrates can realize the hybrid integration of electronic devices and photoelectric devices with different functions. However, because of the large lattice mismatch between the silicon and sapphire and hBN, the hBN film epitaxially grown using these two materials as the substrate material has large stress, which causes the degradation of hBN quality. Transition metals (such as Cu, Ni, Cr, Ru, Pt and the like) generally have small lattice constants and small lattice mismatch rate with hBN, when a transition metal foil is used as a substrate material, the transition metal foil is extremely thin and cannot ensure the surface flatness, so that hBN films grown on the foil have certain bending, folding, cracking and the like, the crystallization quality of the hBN films is reduced due to internal stress or cracks, the growth of the hBN films with large area and high quality is difficult to realize, and the device performance based on the hBN films is influenced.
Disclosure of Invention
In order to improve the crystallization quality of the heteroepitaxial hBN film, reduce the internal stress of the hBN epitaxial film and improve the flatness of the film, the invention provides a method for improving the crystallization quality of hexagonal boron nitride by using transition metal or alloy as a buffer layer. The method can not only improve the crystallinity of the hBN on the large lattice mismatch substrate, but also reduce the internal stress of the epitaxial film and improve the flatness of the hBN film. The method can also be extended to the epitaxial growth process of other III-V semiconductor materials.
The technical scheme adopted by the invention for solving the technical problems is as follows: before growing the hexagonal boron nitride epitaxial film, depositing a transition metal or alloy on a silicon, sapphire or other substrate with larger lattice mismatch as a buffer layer in advance by using magnetron sputtering, electron beam evaporation, pulse laser deposition or thermal evaporation film preparation technology, and then epitaxially growing the hexagonal boron nitride film on the substrate with the buffer layer by adopting chemical vapor deposition, magnetron sputtering or pulse laser deposition technology; the buffer layer is annealed before the hexagonal boron nitride film is epitaxially grown so as to further improve the quality of the buffer layer, thereby achieving the purpose of further improving the crystallization quality of the hBN film. The buffer layer is made of transition metal alloy material formed by transition metal such as Cu, Cr, Mo, Ni, W, Mn, Co and the like or combination thereof.
The steps of preparing a transition metal buffer layer on a large lattice mismatch substrate (taking silicon or sapphire as an example) by using a radio frequency magnetron sputtering process and epitaxially growing an hBN film (taking a Low Pressure Chemical Vapor Deposition (LPCVD) technology as an example) are as follows:
(1) at 1X 10-3Sputtering a transition metal or alloy buffer layer on a silicon or sapphire substrate at the temperature of 600-800 ℃ under the vacuum degree of Pa and with the sputtering power of 60-200W, wherein the thickness of the buffer layer is 200-2000 nm (when the buffer layer is made of transition metal alloy, a mixed target can be prepared according to the mass ratio of the transition metal, then sputtering is carried out), and cooling the substrate to room temperature after sputtering is finished;
(2) putting the silicon or sapphire substrate sputtered with the transition metal or alloy buffer layer obtained in the step (1) into an annealing furnace, annealing for 10-30 minutes at 500-900 ℃ to further improve the quality of the transition metal Cr buffer layer, and cooling to room temperature after annealing;
(3) loading the silicon or sapphire substrate with the transition metal or alloy buffer layer obtained in the step (2) into a reaction chamber of an LPCVD system, and vacuumizing to 5 x 10-4Less than Pa, and then introducing BCl under the conditions of 100-300 Pa and 1000-1400 DEG C3And NH3The precursor is used for 30-120 min (hydrogen or nitrogen is used as carrier gas, the flow rate is 100-300 sccm; BCl3The introduction amount of (2) is 10-30 sccm, NH3The introduction amount of (3) is 30-90 sccm), so that an hBN epitaxial thin film layer with the thickness of 1-3 mu m is obtained on the surface of the buffer layer.
The invention has the beneficial effects that the transition metal or alloy buffer layer can be used as a bottom electrode of the hexagonal boron nitride-based vertical device, and the crystallization quality of the epitaxial hBN film on the substrate with large lattice mismatch rate is improved. The method can be expanded to be applied to epitaxial growth of other semiconductor materials.
Drawings
FIG. 1: comparative example 1 process flow schematic of epitaxially growing hBN film (a) and example 1 epitaxially growing hBN film (b); wherein: 1 is a sapphire substrate, 2 is an hBN epitaxial layer, 3 is a sputtered transition metal Cr buffer layer, and 4 is an annealed transition metal Cr buffer layer.
FIG. 2: comparative example 1X-ray diffraction patterns of the epitaxially grown hBN film (a) and the epitaxial hBN film (b) of example 1;
FIG. 3: room temperature raman spectra of comparative example 1 (epitaxially grown hBN film a) and example 1 epitaxial hBN film (b);
Detailed Description
Comparative example 1:
the cleaned sapphire substrate 1 was loaded into an LPCVD reaction chamber, and the reaction chamber pressure was extracted to 1X 10-3Introducing carrier gas (nitrogen gas 200sccm) below Pa, controlling the pressure of the reaction chamber to about 200Pa, heating the substrate to 1400 ℃, and introducing BCl3And NH3,BCl3At a flow rate of 10sccm, NH3At a flow rate of 30sccm, and performing epitaxial growth for 60min, thereby directly growing the hBN layer 2 on the large lattice mismatched sapphire substrate 1, wherein the schematic process of the preparation is shown in fig. 1 (a).
Example 1:
firstly, loading a clean sapphire substrate 1 into a radio frequency magnetron sputtering table, loading a transition metal Cr sputtering target material, adjusting the target distance to 60mm, vacuumizing the system to 5 multiplied by 10-4Introducing argon gas into the reactor, wherein the input flow is 80sccm, the sputtering pressure is adjusted to be 1Pa, the sputtering power is adjusted to be 80W, the sputtering time is 30 minutes, the substrate heating temperature is 700 ℃, and a Cr buffer layer 3 with the thickness of about 1 mu m is obtained on the surface of the sapphire substrate; stopping sputtering, recovering the growth chamber to normal pressure, opening the radio frequency magnetron sputtering platform after the substrate is cooled to room temperature, and taking out the sapphire substrate with the Cr buffer layer.
And annealing the sapphire substrate with the Cr buffer layer in situ for 20min at 850 ℃ to obtain a better-quality and smoother transition metal Cr buffer layer 4, cooling to room temperature after the annealing is finished, and loading the substrate into an LPCVD reaction chamber.
The LPCVD reaction chamber was evacuated to 5X 10-4Pa, adopting nitrogen as carrier gas, controlling the pressure of the reaction chamber to 200Pa, wherein the flow rate of the carrier gas is 100 sccm; heating to 1400 ℃, introducing BCl3And NH3,BCl3At a flow rate of 10sccm, NH3The flow rate of (2) was 30sccm, and the hBN layer 2 was epitaxially grown for 60 min. The preparation method is schematically shown in FIG. 1 (b).
Fig. 2(a) is an X-ray diffraction (XRD) (002) plane diffraction peak of the hBN epitaxial layer 2 on the sapphire substrate 1 prepared in comparative example 1, and fig. 2(b) is an X-ray diffraction (002) plane diffraction peak of the hBN epitaxial layer 2 on the transition metal Cr buffer layer 4 prepared in example 1, and the half-peak widths of the (002) diffraction peaks of the hBN epitaxial layer 2 in comparative example 1 and example 1 are 0.79 ° and 0.40 °, respectively, indicating that the crystalline quality of hBN can be significantly improved by epitaxially growing the hBN layer 2 using the transition metal Cr buffer layer 4.
FIG. 3(a) is a room temperature Raman (Raman) spectrum of the hBN epitaxial layer 2 on the sapphire substrate 1 prepared in comparative example 1, and E of the hBN epitaxial layer 2 can be seen2gThe phonon frequency is 1369.5cm-1For unstressed hBN films, E2gThe phonon frequency is 1366.5cm-1When the film is subjected to in-plane tensile/compressive stress, E is caused2gThe phonon frequency is red-shifted (i.e. E)2gPhonon frequency lower than 1366.5cm-1) Blue shift (i.e. E)2gThe phonon frequency is higher than 1366.5cm-1). E of hBN epitaxial layer 2 prepared in example 12gThe degree of blue shift of phonon frequency is 3.0cm-1The film is subjected to a compressive stress of about 0.699 GPa. FIG. 3(b) is the room temperature Raman spectrum of the hBN epitaxial layer 2 on the transition metal Cr buffer layer 4 prepared in example 1, and E of the hBN epitaxial layer 2 can be seen2gThe phonon frequency is 1366.7cm-1The raman results show E of the hBN epitaxial layer 2 prepared in example 12gThe degree of blue shift of phonon frequency is 0.2cm-1The film is subjected to a compressive stress of about 0.047GPa, which is much less than that of the film in comparative example 1, and E of the hBN epitaxial layer 2 prepared in example 12gThe half-peak width of the phonon vibration peak is 29.3cm-1The width at half maximum of phonon vibration peak of the hBN epitaxial layer 2 prepared by the comparative example 1 is smaller than 46.9cm-1. Therefore, the transition metal buffer layer can effectively reduce the internal stress of the hBN film during heteroepitaxy, and the crystallization quality of the hBN is improved.
Claims (3)
1. A method for improving the crystallization quality of hexagonal boron nitride by using transition metal or alloy as a buffer layer is characterized in that: before growing the hexagonal boron nitride epitaxial film, depositing a transition metal or alloy on a silicon, sapphire or other substrate with larger lattice mismatch as a buffer layer in advance by using magnetron sputtering, electron beam evaporation, pulse laser deposition or thermal evaporation film preparation technology, and then epitaxially growing the hexagonal boron nitride film on the substrate with the buffer layer by adopting chemical vapor deposition, magnetron sputtering or pulse laser deposition technology; the buffer layer is annealed before the hexagonal boron nitride film is epitaxially grown so as to further improve the quality of the buffer layer, thereby achieving the purpose of further improving the crystallization quality of the hBN film.
2. The method of claim 1, wherein the hexagonal boron nitride crystalline quality is enhanced by using a transition metal or alloy as a buffer layer, wherein: the buffer layer is made of Cu, Cr, Mo, Ni, W, Mn, Co or their alloy.
3. The method of claim 1, wherein the hexagonal boron nitride crystalline quality is enhanced by using a transition metal or alloy as a buffer layer, wherein:
(1) is at 1X 10-3Sputtering a transition metal or alloy buffer layer on a silicon or sapphire substrate at the temperature of 600-800 ℃ with the sputtering power of 60-200W under the vacuum degree Pa, wherein the thickness of the buffer layer is 200-2000 nm, and cooling the substrate to room temperature after sputtering is finished;
(2) putting the silicon or sapphire substrate sputtered with the transition metal or alloy buffer layer obtained in the step (1) into an annealing furnace, annealing for 10-30 minutes at 500-900 ℃, and cooling to room temperature after annealing;
(3) loading the silicon or sapphire substrate with the transition metal or alloy buffer layer obtained in the step (2) into a reaction chamber of a low-pressure chemical vapor deposition system, and vacuumizing to 5 x 10-4Less than Pa, and then introducing BCl under the conditions of 100-300 Pa and 1000-1400 DEG C3And NH3The precursor is used for 30-120 min, hydrogen or nitrogen is used as carrier gas, and the flow rate is 100-300 sccm; BCl3The introduction amount of (2) is 10-30 sccm, NH3The introduction amount of the buffer layer is 30-90 sccm, so that a hexagonal boron nitride epitaxial thin film layer with the thickness of 1-3 mu m is obtained on the surface of the buffer layer.
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Cited By (3)
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CN112962082A (en) * | 2021-03-15 | 2021-06-15 | 吉林大学 | Two-dimensional hBN film with magnetron sputtering Cu film as buffer layer and preparation method thereof |
CN113089091A (en) * | 2021-04-01 | 2021-07-09 | 北京化工大学 | Boron nitride template and preparation method thereof |
CN114075695A (en) * | 2020-08-12 | 2022-02-22 | 中国科学院半导体研究所 | Method for preparing high-stoichiometric-ratio two-dimensional hexagonal boron nitride |
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