WO2012064050A2 - 화학적 리프트 오프 방법을 이용한 iii족 질화물 기판의 제조방법 - Google Patents
화학적 리프트 오프 방법을 이용한 iii족 질화물 기판의 제조방법 Download PDFInfo
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- WO2012064050A2 WO2012064050A2 PCT/KR2011/008370 KR2011008370W WO2012064050A2 WO 2012064050 A2 WO2012064050 A2 WO 2012064050A2 KR 2011008370 W KR2011008370 W KR 2011008370W WO 2012064050 A2 WO2012064050 A2 WO 2012064050A2
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- group iii
- iii nitride
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- 150000004767 nitrides Chemical class 0.000 title claims abstract description 120
- 239000000758 substrate Substances 0.000 title claims abstract description 104
- 238000000034 method Methods 0.000 title claims abstract description 66
- 239000000126 substance Substances 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 230000008569 process Effects 0.000 title abstract description 24
- 238000005530 etching Methods 0.000 claims description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 21
- 229910052710 silicon Inorganic materials 0.000 claims description 21
- 239000010703 silicon Substances 0.000 claims description 21
- 238000003486 chemical etching Methods 0.000 claims description 13
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 238000000407 epitaxy Methods 0.000 claims description 10
- 229910052594 sapphire Inorganic materials 0.000 claims description 9
- 239000010980 sapphire Substances 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 8
- 208000012868 Overgrowth Diseases 0.000 claims description 7
- 150000001447 alkali salts Chemical class 0.000 claims description 3
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 60
- 229910002601 GaN Inorganic materials 0.000 description 59
- 239000013078 crystal Substances 0.000 description 18
- 239000004065 semiconductor Substances 0.000 description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 7
- 239000010408 film Substances 0.000 description 7
- NWAIGJYBQQYSPW-UHFFFAOYSA-N azanylidyneindigane Chemical compound [In]#N NWAIGJYBQQYSPW-UHFFFAOYSA-N 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 229910052733 gallium Inorganic materials 0.000 description 5
- 230000005693 optoelectronics Effects 0.000 description 5
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 description 4
- 238000000206 photolithography Methods 0.000 description 4
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- 238000000926 separation method Methods 0.000 description 4
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 4
- 229910002704 AlGaN Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
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- 229910052738 indium Inorganic materials 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000001451 molecular beam epitaxy Methods 0.000 description 3
- 238000000059 patterning Methods 0.000 description 3
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 230000002269 spontaneous effect Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- XOYLJNJLGBYDTH-UHFFFAOYSA-M chlorogallium Chemical compound [Ga]Cl XOYLJNJLGBYDTH-UHFFFAOYSA-M 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002017 high-resolution X-ray diffraction Methods 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000005701 quantum confined stark effect Effects 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000001039 wet etching Methods 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910004613 CdTe Inorganic materials 0.000 description 1
- 229910000807 Ga alloy Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- 230000005699 Stark effect Effects 0.000 description 1
- 229910007709 ZnTe Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
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- 238000000295 emission spectrum Methods 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 238000001657 homoepitaxy Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- CDAISMWEOUEBRE-GPIVLXJGSA-N inositol Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@@H]1O CDAISMWEOUEBRE-GPIVLXJGSA-N 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000007261 regionalization Effects 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Definitions
- the present invention relates to a method of manufacturing a group III nitride substrate. More specifically, the present invention relates to a method of manufacturing a non-polar or semi-polar group III nitride substrate using a chemical lift off (CLO) method.
- CLO chemical lift off
- LEDs applied to backlight light sources, display light sources, general light sources and full color displays, etc. are widely used by using the characteristics of compound semiconductors.
- group III-V nitride semiconductors such as GaN (Gallium Nitride), AlN (Aluminum Nitride), and InN (Indium Nitride) are known, and the material is a large energy band gap of direct transition type.
- the optoelectronic device such as having a gap () to obtain light in the near-wavelength region according to the composition of the nitride, the light emitting device using the same is applied in various fields such as flat panel display device, optical communication.
- Such devices are typically grown in a thin film form on a substrate by growth methods such as molecular beam epitaxy (MBE), metalorganic chemical vapor deposition (MOCVD), and hydride vapor phase epitaxy (HVPE).
- MBE molecular beam epitaxy
- MOCVD metalorganic chemical vapor deposition
- HVPE hydride vapor phase epitaxy
- semiconductors based on group III nitrides represented by GaN typically fabricate device structures on (0001) planes using c-plane substrates (eg, sapphire substrates). Spontaneous polarization is formed in the growth direction (0001).
- an LED having a typical InGaN / GaN quantum well structure generates internal strain due to lattice mismatch in the quantum well structure when the structure is grown on the (0001) plane, and thus, due to piezoelectric fields. Since the quantum-confined Stark effect (QCSE) is caused, there is a limit to increasing the internal quantum efficiency.
- QCSE quantum-confined Stark effect
- group III nitrides particularly GaN and alloys thereof (eg, alloys with InN and / or AlN), are most stable in hexagonal Wrtzite structures, which The crystal structure is represented by two or three equal basal plane axes in which the crystals are rotated 120 ° relative to each other and are all perpendicular to the c-axis.
- any plane lying perpendicular to the c-axis by the group III element and nitrogen atom position in the urchite crystal structure will contain only one type of atom. Proceeding to the c-axis, each face may contain only one type of atom (group III element or nitrogen).
- group III element or nitrogen the GaN crystal has an N-face containing only nitrogen atoms and a Ga-face containing only Ga atoms at each end. Located in As a result, group III nitride crystals are polar along the c-axis. Such spontaneous polarization depends on the structure and composition of the crystal as a bulk property.
- the conventional c-plane quantum well structure in group III nitride-based optoelectronic and electronic devices is characterized in that the electrostatic field caused by piezoelectric and spontaneous polarization changes the energy band structure of the quantum well structure, Since the distribution of electrons and holes by the electric field is distorted, the spatial separation of electrons and holes by such an electric field is called a quantum constrained stark effect, which lowers the internal quantum efficiency and causes a red shift of the emission spectrum.
- non-polar or semi-polar group III nitrides have been proposed.
- the nonpolar or semipolar planes thus obtained contain the same number of group III atoms and nitrogen atoms and thus exhibit charge neutrality, with the result that the entire crystal is not polarized in the growth direction.
- nonpolar Group III nitride crystals growing on heterogeneous substrates exhibit high defect densities resulting in a problem of reducing quantum efficiency.
- a thick film group III nitride layer is grown on a heterogeneous substrate, such as a sapphire substrate, and then laser lifted off.
- a group III nitride layer grown from a heterogeneous substrate is separated by a laser lift off (LLO) method and used as a substrate.
- LLO laser lift off
- the reason why the laser lift-off method is used in this way is that the conventional nitride layer grown in the c-axis direction is difficult to achieve substantially wet etching because the surface shows Ga-polarity.
- the laser lift off method may be more preferable because of the high cost and complexity.
- group III nitride layers for nonpolar or semipolar substrates can be prepared, it is not easy to separate them by chemical lift-off, which would cause damage to the group III nitride layers to be used as substrates in the chemical etching process. Because it can. In particular, this problem may be more prominent in the process of applying to the separation of the substrate having a diameter of 2 inches or more suitable for commercialization.
- the present invention seeks to provide a method of manufacturing high quality nonpolar or semipolar III-nitride substrates which can alleviate the problems resulting from the use of polar nitrides as well as reduce defects.
- the present invention seeks to provide a method for producing a nonpolar or semipolar III-nitride substrate by a chemical lift off method.
- a method for producing a group III nitride substrate is provided, wherein at least one region of the inner surface of the cavity exhibits N-polarity.
- step d) separating the group III nitride layer formed in step c) by performing a chemical etch on at least some thickness of the group III nitride layer grown in step b);
- the growth surface of the non-polar or semi-polar epitaxy layer has a (111) facet, and at least one region of the inner surface of the cavity exhibits N-polarity, thereby providing a method of manufacturing a group III nitride substrate. do.
- the electronic device may include a light emitting device (LED), a laser diode (LD), a transistor, and the like.
- Group III nitride substrates prepared in accordance with embodiments of the present invention are nonpolar or semipolar substrates, which can alleviate the technical limitations of polar nitrides, and in particular can be manufactured by chemical lift-off methods.
- 1 (a) is a diagram showing nonpolar planes (a-plane and m-plane) of the crystal structure of GaN;
- Fig. 1 (b) is a diagram showing a semi-polar plane in the crystal structure of GaN;
- FIG. 2 is a cross-sectional view showing the formation of a group III nitride layer (template) on a substrate in one embodiment according to the present invention
- FIG. 3 is a cross-sectional view showing a process of forming a mask pattern (stripe pattern) on the first group III nitride layer in one embodiment according to the present invention
- FIG. 4 is a cross-sectional view showing, in one embodiment according to the present invention, a second III-nitride layer regrown by side growth (or overgrowth) on a first III-nitride layer;
- FIG. 5 is a cross-sectional view showing a cross section in which a third III-nitride layer is formed on the second III-nitride layer in one embodiment according to the present invention
- FIG. 6 is a cross-sectional view schematically illustrating a process of chemically etching a Group II III nitride layer located below to separate a Group III III nitride layer (substrate use) in one embodiment of the present invention
- FIG. 7 illustrates a nonpolar or semipolar III-nitride layer as a cavity is formed on a silicon substrate, and a nonpolar or semipolar III-nitride layer of a thick film is formed on the silicon substrate according to another embodiment of the present invention.
- FIG. 8 is a view showing an example in which the Group III-nitride layer obtained in accordance with one embodiment of the present invention is separated and applied to the substrate of the LED device;
- FIG. 9 is a SEM photograph showing a cross section of the laterally grown second GaN layer (sample 1) in Example 1 of the present invention.
- FIG. 10 is a SEM photograph showing a cross section of a side-grown second GaN layer (sample 2) in Example 1 of the present invention.
- FIG. 11 is a SEM photograph showing a cross section of a second GaN layer (sample 3) regrown without a mask pattern on the first GaN layer in Example 1 of the present invention
- Example 12 is a SEM photograph showing a cross section of a side-grown second GaN layer (sample 4) in Example 1 of the present invention.
- FIG. 13 is a SEM photograph showing a cross section of a third GaN layer thickly formed by HVPE on Sample 2 in Example 1 of the present invention.
- the expressions “on” and “on” are used to refer to the concept of relative location, where other components or layers are directly present in the layers mentioned, as well as other layers in between. It can be understood that (intermediate layer) or components may be interposed or present. Similarly, the expressions “below”, “below”, “below” and “between” may also be understood as a relative concept of position.
- Group III nitride may refer to a semiconductor compound formed of a group III element on the periodic table and nitrogen.
- a group III element aluminum (Al), gallium (Ga), indium (In), or the like can be exemplified, and these can be included alone or in combination of two or more. Therefore, it can be understood as a concept including GaN, AlN, InN, AlGaN, AlInN, GaInN, AlInGaN and the like.
- the group III nitride can be represented by the following general formula (1).
- side growth or “side overgrowth” is a concept that includes lateral epitaxy overgrowth (LEO, ELO or ELOG), PENDEO epitaxy, and the like, and is easier to lateral growth than vertical growth. By doing so, it is possible to suppress propagation of defects or dislocations in a direction perpendicular to the layer surface.
- Such processes are commonly known in the art for the purpose of reducing defects or dislocations during c-plane GaN growth by MOCVD or the like.
- nonpolar means to have crystallographic directions (e.g., a-plane and m-plane) perpendicular to the c-axis.
- the nonpolar plane of the group III nitride crystal structure is shown in FIG. as in a).
- the term "semipolar” means having a crystal orientation between 0 and 90 ° with respect to (0001) or (000-1).
- the “semipolar plane” then extends across the hexagonal unit cell diagonally and forms an angle other than 90 ° with the c-axis. In particular, compared to the polar layer, the influence of polarity is reduced because the polar vector is inclined with respect to the growth direction.
- Semipolar planes commonly found in group III nitrides are (11-22), (1-101), (10-11), (10-13), (10-12), (20-21). ), (10-14) and the like, but the present invention is not limited to the above specific values.
- Such a semipolar plane may be represented as shown in FIG. 1 (b). For example, in the case of semipolar GaN in the (11-22) direction, the semipolar plane is inclined about 58 ° with the (0002) plane.
- FIG. 2 is a view showing that a group III nitride layer (mold) is formed on a substrate in one embodiment according to the present invention.
- the first, second and third group III nitrides may refer to nonpolar or semipolar layers, preferably semipolar layers, respectively.
- an epitaxial layer 102 of group III-nitride is grown on the substrate 101.
- any substrate suitable for growth of the nonpolar or semipolar III-nitride layer as the substrate 101 may be used without particular limitation.
- Such substrates can broadly include symmetry-equivalent planes such as a-plane, r-plane or m-plane. have.
- an r-plane substrate is prepared for the production of a nonpolar group III nitride layer, and a semipolar m-plane substrate (for example, (1-100) orientation for the production of a group III nitride layer. With silver).
- the material of the substrate sapphire, silicon carbide (SiC), lithium aluminate, spinel, and the like may be exemplified, and in some cases, a group III nitride or alloy material thereof (for example, gallium nitride) (GaN), aluminum nitride (AlN) or the like) may be used.
- a group III nitride or alloy material thereof for example, gallium nitride) (GaN), aluminum nitride (AlN) or the like
- GaN gallium nitride
- AlN aluminum nitride
- an m-plane sapphire substrate to implement semipolarity as the substrate.
- removal of residual oxygen in the reaction zone, annealing or heat treatment of the reaction zone using hydrogen and / or nitrogen (high temperature, eg, to a growth temperature) Step can be performed.
- an intermediate layer or a buffer layer may be formed on the substrate 101 before the first group III nitride layer 102 is grown.
- This intermediate layer is selectively introduced to obtain better physical properties of the group III nitride layer 102, an exemplary material being the growth of non-polar, in particular semi-polar, group III nitride layers as well as group III-V compounds such as AlN and AlGaN. It may be another material suitable for promoting the process.
- deposition or epitaxial growth techniques known in the art, such as MOCVD, HVPE, etc. may be utilized.
- the dimension of the intermediate layer thus selectively introduced is not particularly limited but may be in the range of at least about 10 to 50 nm.
- the process conditions can be adjusted to, for example, about 550 to 750 ° C. at atmospheric pressure for the formation of the intermediate layer, which should be understood as an exemplary meaning and the present invention is not limited to the above numerical range.
- nonpolar or semipolar III-nitride layers can be formed on the substrate (or intermediate layer on the substrate) using conventional layer growth techniques such as MOCVD, HVPE, MBE, etc. It may be desirable to use MOCVD to ensure a better quality template.
- the first group III nitride layer 102 may be formed to a thickness, specifically about 1 to 10 ⁇ m, more specifically about 2 to 5 ⁇ m.
- a growth reaction may be performed for about 60 to 300 minutes under a temperature of about 800 to 1100 ° C. and a pressure of about 200 to 500 torr.
- the specific growth conditions are described for illustrative purposes, and may be changed according to the size of the substrate and the like, but the present invention is not necessarily limited thereto.
- the first group III nitride layer 102 has a semi-polar direction characteristic, and specifically, substrate characteristics and growth conditions may be adjusted to have a (11-22) direction. .
- 3 and 4 illustrate a specific pattern of a cavity 105 below the interior of the Group III nitride layer 104 regrown on the Group III nitride layer 102 by lateral growth or overgrowth. It is a figure which shows the process of forming a kind of tunnel by being formed continuously along the mask of (a stripe pattern in drawing).
- the lateral growth method can be carried out, for example, under ammonothermal growth conditions, and the ELOG method can be used as an example of the various lateral growth methods mentioned above.
- a conventional growth method for example, MOCVD, HVPE, etc. may be used, it may be preferable to use MOCVD to facilitate the formation of a cavity as described below. The reason for this is that it may be easy to implement a cavity, particularly a triangular cavity, by showing a tendency to grow into an inverted leg shape in the lateral growth process, as described below.
- the ELOG method is a modification of the selective crystal growth technique, and is used to prevent vertical propagation of dislocations occurring in the initial growth stage by partially patterning the insulating layer of the thin film on the already grown group III nitride layer. The following description will focus on the ELOG method.
- a patterned mask layer 103 ' is formed on the first semipolar group III nitride layer 102 in the form of a stripe.
- the mask of the stripe pattern may typically be a dielectric material, and may typically represent SiO 2 , SiN x (eg, Si 3 N 4 ), and the like.
- the insulating layer 103 is first formed by, for example, plasma enhanced chemical vapor deposition (PECVD). Then, one set on the group III nitride layer 102 using conventional photolithography method (in the above method, for etching, a conventional manner such as, for example, ICP-RIE, etc. may be adopted).
- PECVD plasma enhanced chemical vapor deposition
- the parallel stripe pattern 103 'remains. In this case, an area between the masks of the stripe pattern may be referred to as a "window area".
- the width of the mask may be set in a range of about 2 to 50 ⁇ m (specifically, about 2 to 10 ⁇ m), and the width of the window is about 2 to 20 ⁇ m (more specifically, about 2 to 10 ⁇ m). have.
- the mask may also be suitable if it is in the range of about 500-2,000 mm 3 thickness.
- the mask may be formed by setting in all the directions that can be placed on the plane, preferably in the (1-100) direction. The reason for considering the orientation of the mask pattern is because it affects the characteristics such as the facet formation of the over-grown group III nitride layer.
- group III nitrides are characterized by a much faster growth rate in the c-plane direction than other planes.
- a mask for example, SiO 2 material
- the quality of the overall growth layer is improved as well as flat and smooth.
- a surface can be obtained.
- the mask pattern is formed in the (1-100) direction
- a smoother surface can be formed.
- the mask is patterned in the (-1-123) direction
- the uneven surface of the micro unit may be formed. Therefore, although the present embodiment is not necessarily limited to the mask pattern in a specific direction, it may be more preferable to set the mask pattern in the (1-100) direction.
- a group III nitride regrowth process is performed, which begins in the window region, where the microstructure of the underlying group III nitride layer 102 is reproduced, while the growth is over the mask region. It won't happen. Over time, crystals growing in the window region gradually grow (overgrowth) over the mask. As such, the growth layer of group III nitride extends vertically and laterally, wherein the laterally grown regions are referred to as " wing regions " whereby high quality crystals can be obtained with significantly reduced defects. It is.
- the rate of extension between vertical and side depends on growth conditions, such that a nitride overgrown layer extending from the window to the side (e.g., the right direction) over time will have a side ( For example, it may meet and merge with the nitride overgrowth layer extending in the left direction.
- a cavity 105 is formed below the joining boundary, which is formed continuously along the mask pattern to form a kind of tunnel structure.
- the cavity 105 may exhibit various shapes such as a triangle, a square, a rectangle, a circle, and the like, depending on process conditions, but may have a triangular shape as shown.
- semi-polar III-nitride may be suitable for forming a kind of tunnel by continuously connecting the cavity in the II-III nitride layer, but the present invention is not limited thereto.
- Non-polar group III nitrides are also possible if one cavity is available.
- the thickness of the group III-nitride layer 104 may be, for example, in the range of about 3 to 10 ⁇ m, and the size (diameter or height) of the cavity is about 2 to 50 ⁇ m, more specifically about 2 to May be in the range of 10 ⁇ m. These numerical ranges are exemplary and can be adjusted according to changes in process conditions.
- the triangular cavity size may be formed differently according to the size of the pattern mask.
- the diameter of the triangular cavity will have a width of about 6 ⁇ m. . If the width of the mask increases, the diameter of the triangular cavity also increases in proportion to this, and the growth time will also increase as the width of the mask increases.
- the second group III nitride layer 104 may be formed (grown) by various parameter combinations, for example, the growth temperature is about 700 to 1,100 ° C. (more specifically about 800 to 1,000). ° C), and the pressure may range from about 200 to 400 mTorr.
- the mask pattern when the mask pattern is in the (1-100) direction, the mask pattern may be performed at about 800 to 1100 ° C. for about 240 to 600 minutes.
- the flow rate of the Ga source eg, trimethylgallium, triethylgallium, etc.
- supplied may range from about 10 to 30 sccm.
- the second III-nitride layer 104 grows in an inverted trapezoidal shape from the window and gradually forms a triangular-shaped cavity 105.
- the lateral growth layer obtained as described above can be characterized by x-ray diffraction (XRD) analysis, and in the case of nonpolar and semipolar layers, it is usually anisotropic according to the angle (direction angle).
- XRD x-ray diffraction
- the semipolar group III nitrides obtainable by lateral growth in this embodiment for example, the range of about 300 to 500 arc sec (the FWHM value in arcsec (degree ⁇ 3600)) It is preferable to indicate.
- FIG. 5 shows a cross section in which a Group III-nitride layer 106 is formed on the Group II-nitride layer 104 in an embodiment of the invention.
- the third III-nitride layer 106 is separated from the lower substrate through a subsequent lift-off process, and thus a substrate (eg, homoepitac) for manufacturing electronic (or optoelectronic) devices such as LEDs, LDs, and transistors in the future. Can be used as a substrate for growing).
- a substrate eg, homoepitac
- HVPE has a relatively low growth cost and is particularly suitable for manufacturing thick growth layers because of its high growth rate.
- Ga is typically placed in a temperature range of about 700 to 900 ° C. in a horizontal reactor having a two-step temperature gradient, and the target obtained previously (a structure in which first and second group III-nitride layers are formed on a substrate) is grown in a growth region ( For example, about 900 to 1100 ° C.).
- Ga and HCl gas placed in a quartz container are reacted to supply GaCl synthesized with a carrier gas to a target, and ammonia gas is supplied to a region where the target is located through a separate quartz plate.
- Group III nitride is grown on the target by the reaction formula of GaCl + NH 3 ⁇ GaN + HCl + H 2 (for GaN growth).
- the thickness of the Group III-nitride layer 106 may be at least about 200 ⁇ m, more typically in the range of about 300 to 500 ⁇ m, to be suitable for growth substrate applications.
- the group III-nitride layer 106 may exhibit the same crystal properties as the lower semi-polar or nonpolar group III-nitride layer corresponding to the template, that is, the semi-polar or non-polar property.
- FIG. 6 illustrates a process of separating the Group III-nitride layer to be applied as an independent substrate by performing chemical etching on the Group II-nitride layer 104 in one embodiment of the present invention. It is a figure which shows schematically. As shown, the etching is carried out in a horizontal direction or in a vertical / horizontal direction, particularly around the tunnel shaped cavity.
- Representative Group III nitride GaN crystals have two different faces, a Ga-face and an N-face. At this time, the Ga-plane is terminated at the end by a gallium atom, while the N-plane is terminated by the nitrogen atom at the end. Ga-plane is chemically stable, whereas N-plane is chemically unstable and highly reactive.
- an N-polar surface will be present in the cavity inner surface (eg, at least one region of the cavity inner surface).
- the -c plane and the (n- or r-) plane exist on both sides of the triangular cavity, respectively, while the bottom surface of the cavity is formed of SiO 2 .
- the chemical etching may also proceed on the surfaces of the first and second III-nitride layers having nonpolar or semipolar properties.
- the first and second III-nitride layers are removed such that the III-III nitride layer can be separated from the underlying structure.
- a large area (eg, at least two inches) of Group III-nitride layer can be effectively separated.
- the outer surface of the Group III-nitride layer during the etching process if a cavity tunnel across the Group II-nitride layer is not formed even if chemical (wet) etching is possible for the nonpolar or semipolar Group III nitride. Again, the phenomenon of etching to some extent is inevitable.
- the cavity tunnels exist at intervals of several tens of micrometers, only the gap between the cavity tunnels can be etched to separate the group III-nitride layer.
- etching conditions may be set to be performed for about 0.5 to 20 minutes under temperature conditions of at least about 300 ° C, more typically about 400 to 600 ° C.
- the present invention is not necessarily limited to the above conditions, and can be changed depending on the crystal properties in the object to be etched, the diameter size of the cavity according to the pattern mask size, and the like. For example, if the cavity diameter is large, the etching rate may be faster.
- a method of manufacturing a nonpolar or semipolar group III nitride substrate using a silicon (Si) substrate is provided.
- non-polar or semi-polar group III nitride layer is formed while forming a cavity on a silicon substrate according to another embodiment of the present invention, the non-polar or semi-polar group III nitride layer of a thick film on the upper side (for example)
- the non-polar or semi-polar group III nitride layer of a thick film on the upper side for example, it is a cross section which shows schematically the state in which at least about 200 micrometers thickness) was formed.
- a (111) facet is formed on the upper surface of the silicon substrate 111.
- the silicon substrate may be, for example, a (311) or (001) silicon substrate.
- a patterning step specifically, a patterning process through an anisotropic etching, may be performed to form the (111) facet.
- the (111) facets formed on the silicon substrate may selectively grow (form) group III nitride (ie, selective growth). That is, the group III nitride layer 114 may be grown (formed) by forming, for example, a triangular cavity 115 by a (111) facet formed on a silicon substrate.
- the group III nitride layer 114 grown while the cavity 115 is formed is semipolar (eg, (1-101) or (11-22)) or nonpolar (eg, ( 11-20)). Accordingly, the group III nitride layer 114 serves as a kind of template, and the group III nitride layer 116 formed thereon may also exhibit semipolar or nonpolar characteristics.
- the group III nitride layer 116 is formed (grown), for example, to a thickness of at least about 200 ⁇ m, and is chemically etched and separated from the group III nitride layer 114 having a cavity formed thereon as described above. freestanding) can be used as a III-nitride substrate.
- a pattern mask layer (for example, SiO 2 mask) can also be used.
- a SiO 2 mask (eg, about 70 nm thick, about 1 ⁇ m or less mask width, about 1 to 3 ⁇ m pattern spacing) on a (311) silicon substrate is subjected to photolithography techniques and the like.
- a pattern e.g., stripe pattern
- etch at about 30 to 50 [deg.] C with an etchant (e.g., KOH solution), and then, for example, HF (e.g., diluted HF), buffered oxide etchant (HF + NH4F mixture; BOE) and the like can be used to remove the mask layer.
- HF e.g., diluted HF
- BOE buffered oxide etchant
- the (111) facets are formed on the silicon substrate by the etching process.
- a III-nitride layer 114 having a predetermined thickness is formed on the silicon substrate through (re) growth such as MOCVD.
- MOCVD metal-organic chemical vapor deposition
- the intermediate layer or the buffer layer (not shown) described above may be selectively formed.
- the growth of the above-mentioned group III nitride may be performed at, for example, about 900 to 1,100 ° C.
- the growth and growth of the Group III nitride layer 116 of the thick film that is subsequently formed, and the chemical etching principles and detailed processes are the same as described above and will be omitted.
- the group III nitride substrate prepared according to the above-described embodiment suppresses the mismatch due to hetero epitaxy caused by using a heterologous substrate (for example, sapphire) which is widely used now. It can be applied to the substrate of the electronic (or optoelectronic) device by the time growth.
- a light emitting diode (LED), a laser diode (LD), a transistor (for example, HEMT), and the like can be exemplified.
- FIG. 8 is a diagram showing an example in which the Group III-nitride layers 106 and 116 obtained according to the above-described embodiments are separated and applied to the substrate of the LED element.
- the LED element is a group III nitride substrate 201, an n-type (or p-type) semiconductor layer 202, an active layer 203 and a p-type (or n-type) semiconductor layer (from below) 204).
- a p-electrode 205 is formed on the p-type semiconductor layer 204
- an n-electrode 206 is formed on an exposed surface of the n-type semiconductor layer 202.
- the illustrated layer structure is provided for illustrative purposes, and various modified configurations are possible.
- the materials of the semiconductor layers 202 and 204 and the active layer 203 formed on the substrate 201 are not particularly limited, and various semiconductor materials (III-V and II-VI known in the art for manufacturing LEDs).
- Etc. GaN, InN, AlN, InP, InS, GaAs, CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, ZnO, Al x Ga 1-x N, In x Ga 1-x N, In x Ga 1-x As, Zn x Cd 1-x S, or the like can be used, and these can be used alone or in combination (0 ⁇ x ⁇ 1).
- the active layer 203 may be formed of at least two materials selected from, for example, GaN, AlN, InN, InGaN, AlGaN, InAlGaN, or the like. Among them, a material having a small energy band gap may be used as a quantum well, and a material having a large energy band gap may be configured as a quantum barrier, and both single and multi quantum well structures may be used.
- electrodes 205 and 206 for electrical application for example, platinum (Pt), palladium (Pd), aluminum (Al), gold (Au), nickel / gold (Ni / Au) alone Or in combination.
- platinum (Pt), palladium (Pd), aluminum (Al), gold (Au), nickel / gold (Ni / Au) alone Or in combination for this electrode pattern formation, conventional methods such as photoresist patterning-etching, which are known in the art, may be performed.
- a planar semipolar GaN layer was formed on an m-sapphire substrate (Crystal-On Company: M-plane 2 "sapphire wafer, thickness 430 ⁇ m) using the MOCVD equipment (Veeco) under the conditions of Table 1 below. At this time, tremethylgallium and ammonia were used as the gallium source and the nitrogen source, respectively.
- ELOG was performed on the first GaN layer using masks of stripe patterns arranged at regular intervals (samples 1 and 2).
- a SiO 2 layer was first deposited to a thickness of 100 nm by PECVD, and then the width (mask area) and stripe spacing (window area) of the stripe were respectively determined by ICP-RIE etching using standard photolithography. It adjusted to 7 micrometers and 4 micrometers.
- the mask pattern was formed in the (1-100) direction.
- the GaN layer was then regrown at 880 ° C. and 300 mTorr using MOCVD (ELOG). At this time, the thickness of sample 1 was about 2 ⁇ m, and the thickness of sample 2 was about 4 ⁇ m.
- Sample 3 was regrown without a mask pattern (thickness: about 1.2 mu m), and Sample 4 had a mask pattern direction of (-1-123) (thickness: about 2 mu m).
- the GaN layer regrown from the window region gradually grew laterally overgrown over the mask region over time, and laterally grown from the left and right over the wing region as the lateral growth continued.
- the triangular cavities are continuously connected along the mask pattern to form a tunnel.
- a planar regrowth layer was formed as shown in FIG.
- a second GaN layer having a triangular cylinder shape is formed along the mask pattern on the first GaN layer.
- FWHM full width at half maximum; unit: arcsec
- XRD analyzer PANalytical, product name: High-resolution X-Ray diffraction
- a third GaN layer was grown by HVPE on a sample 2 having a cavity tunnel (thickness: 300 mu m).
- the HVPE process conditions are shown in Table 3 below.
- the third GaN layer (ie, (11-22) GaN layer) of the thick film is formed in the same manner as the lower second GaN layer (ie, (11-22) GaN layer). .
- a molten KOH was placed in a beaker at a height sufficient to contain the structure obtained as described above (first, second and third GaN layers formed on the substrate), which was then hot plated. Put on the table. After heating up to 550 ° C. to sufficiently melt the KOH to maintain the liquid phase, the structure was added thereto.
- the SEM image confirmed the change of the second GaN layer due to etching. Changes in the second GaN layer after 20, 40, and 60 seconds have been shown in FIGS. 14A to 14C, respectively.
- a 70 nm thick SiO 2 mask layer was sputter deposited on the (311) substrate, and a stripe pattern was formed using a photolithography method (mask width of 1 ⁇ m, pattern spacing of 2 ⁇ m).
- the silicon substrate was then etched at 40 ° C. with KOH solution (25%).
- KOH solution 25%
- (111) facets formed on the silicon substrate surface, which were removed using diluted HF solution.
- GaN was grown using trimethyl gallium (TMG) and ammonia as sources in the MOCVD apparatus.
- TMG trimethyl gallium
- the flow rates of TMG and ammonia were 15.0 ⁇ mol / min, and 0.5 slm, respectively
- the growth temperature was 1,050 ° C.
- the growth time was 60 minutes.
- the GaN layer of the thick film was formed on the III-nitride layer thus formed as in Example 1, and then subjected to chemical etching, the possibility of fabrication of a self-supporting GaN substrate by separation of the GaN layer of the thick film was confirmed.
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Abstract
Description
온도(℃) | 시간(min) | Pg(Torr) | |
질화반응(nitridation) | 1080 | 0.75 | 500 |
저온 성장(중간층) | 700 | 4 | 200 |
재결정 | 1060 | 5 | 200 |
고온 성장 | 880 | 180 | 300 |
샘플번호 | 1 | 2 | 3 | 4 |
마스크 패턴 방향 | (1-100) | (1-100) | - | (-1-123) |
성장 시간(분) | 180 | 360 | 180 | 180 |
갈륨 소스의 유속(sccm) | 20 | 20 | 20 | 20 |
소스(Ga) 온도 | 800℃ |
성장 온도 | 1000℃ |
소스 HCl 가스 유속 | 500 sccm |
암모니아(NH3) 가스 유속 | 1000 sccm |
N2 캐리어 가스 유속 | 2000/3500(HCl/NH3) sccm |
전체 유속(total flow) | 40 slm |
성장 시간 | 600 min |
홀더 회전(holder rotation) | 30 RPM |
Claims (15)
- a) 무극성 또는 반극성 에피탁시층의 성장 표면을 제공하는 기판 상에 제1 III족 질화물 층을 형성하는 단계;b) 1 또는 2 이상의 캐비티가 내부에 형성된 제2 III족 질화물 층을 측면 성장(lateral growth) 방식에 의하여 상기 제1 III족 질화물 층 상에 형성하는 단계;c) 상기 제2 III족 질화물 층 상에 제3 III족 질화물 층을 형성하는 단계; 및d) 상기 제2 III족 질화물 층의 적어도 일부 두께에 대한 화학적 에칭을 수행하여 분리된 제3 III족 질화물 층을 얻는 단계;를 포함하며,상기 캐비티 내면의 적어도 일 영역이 N-극성을 나타내는 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- 제1항에 있어서,상기 무극성 또는 반극성 에피탁시층의 성장 표면을 제공하는 기판은 m-면 사파이어 기판인 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- 제1항에 있어서,상기 제1 III족 질화물 층은 (11-22) 방향의 반극성 층인 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- 제1항에 있어서,상기 측면 성장 방식은 ELOG(epitaxial lateral overgrowth) 방식인 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- 제1항에 있어서,상기 단계 b)는,(i) 상기 제1 III족 질화물 층 상에 패턴화된 마스크 층을 형성하는 단계; 및(ii) 상기 패턴화된 마스크 층이 형성된 제1 III족 질화물 층 상에 III족 질화물 층을 측면 성장시키는 단계;를 포함하는 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- 제5항에 있어서,상기 마스크 층은 (1-100) 방향으로 패턴화된 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- 제5항에 있어서,상기 마스크 층은 SiO2 또는 SiNx 재질인 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- 제5항에 있어서,상기 마스크 층은 스트라이프 패턴으로 형성되고,상기 스트라이프의 폭 및 스트라이프 간격은 각각 2 내지 50 ㎛ 및 2 내지 20 ㎛ 범위인 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- 제1항에 있어서,상기 제3 III족 질화물 층은 HVPE에 의하여 형성되는 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- 제1항에 있어서,상기 제3 III족 질화물 층의 두께는 적어도 200 ㎛인 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- 제1항에 있어서,상기 화학적 에칭은 용융 알칼리 염 내에서 이루어지는 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- 제11항에 있어서,상기 화학적 에칭은 400 내지 600 ℃의 온도 조건 하에서 0.5 내지 20 분 동안 수행되는 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- a) 실리콘(Si) 기판 상에 무극성 또는 반극성 에피탁시층의 성장 표면을 제공하도록 이방성 에칭(anisotropic etching)을 수행하는 단계;b) 상기 에칭된 실리콘 기판 상에 1 또는 2 이상의 캐비티를 형성하면서 III족 질화물 층을 성장시키는 단계;c) 상기 단계 b)에서 성장된 III족 질화물 층 상에 III족 질화물 층을 형성하는 단계; 및d) 상기 단계 b)에서 성장된 III족 질화물 층의 적어도 일부 두께에 대한 화학적 에칭을 수행함으로써 상기 단계 c)에서 형성된 III족 질화물 층을 분리하는 단계;를 포함하며,상기 무극성 또는 반극성 에피탁시층의 성장 표면은 (111) 파셋(facet)을 갖고, 그리고 상기 캐비티 내면의 적어도 일 영역이 N-극성을 나타내는 것을 특징으로 하는 III족 질화물 기판의 제조방법.
- 제1항 내지 제13항 중 어느 한 항에 따라 제조된 III족 질화물 기판.
- 제14항에 따른 III족 질화물 기판을 포함하는 전자 소자.
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