WO2012056928A1 - 光学素子の製造方法 - Google Patents
光学素子の製造方法 Download PDFInfo
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- WO2012056928A1 WO2012056928A1 PCT/JP2011/073831 JP2011073831W WO2012056928A1 WO 2012056928 A1 WO2012056928 A1 WO 2012056928A1 JP 2011073831 W JP2011073831 W JP 2011073831W WO 2012056928 A1 WO2012056928 A1 WO 2012056928A1
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- Prior art keywords
- aluminum nitride
- single crystal
- optical element
- layer
- crystal layer
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- 230000003287 optical effect Effects 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 140
- 239000013078 crystal Substances 0.000 claims abstract description 120
- 239000000758 substrate Substances 0.000 claims abstract description 112
- 238000005229 chemical vapour deposition Methods 0.000 claims description 17
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 238000002834 transmittance Methods 0.000 abstract description 8
- 239000010410 layer Substances 0.000 description 143
- 150000004767 nitrides Chemical class 0.000 description 39
- 239000004065 semiconductor Substances 0.000 description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 15
- 239000007789 gas Substances 0.000 description 15
- 238000005498 polishing Methods 0.000 description 11
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 9
- 229910021529 ammonia Inorganic materials 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000010409 thin film Substances 0.000 description 7
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 7
- 239000012535 impurity Substances 0.000 description 5
- QBJCZLXULXFYCK-UHFFFAOYSA-N magnesium;cyclopenta-1,3-diene Chemical compound [Mg+2].C1C=CC=[C-]1.C1C=CC=[C-]1 QBJCZLXULXFYCK-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000013067 intermediate product Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 229910052594 sapphire Inorganic materials 0.000 description 3
- 239000010980 sapphire Substances 0.000 description 3
- 238000005092 sublimation method Methods 0.000 description 3
- VCZQFJFZMMALHB-UHFFFAOYSA-N tetraethylsilane Chemical compound CC[Si](CC)(CC)CC VCZQFJFZMMALHB-UHFFFAOYSA-N 0.000 description 3
- 239000012808 vapor phase Substances 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910021478 group 5 element Inorganic materials 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 1
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
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- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
- H01L33/30—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table
- H01L33/32—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table containing nitrogen
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/20—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/301—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C23C16/303—Nitrides
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- C23C16/34—Nitrides
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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Definitions
- the present invention relates to a novel optical element manufacturing method and an optical element laminate.
- an optical method includes a step of forming an aluminum nitride single crystal layer having excellent optical characteristics on an aluminum nitride seed substrate, forming an optical element layer on the aluminum nitride single crystal layer, and removing the aluminum nitride seed substrate.
- the present invention relates to a method for manufacturing an element.
- the present invention also includes an aluminum nitride seed substrate, an aluminum nitride single crystal layer having excellent optical properties formed on the aluminum nitride seed substrate, and an optical element formed on the aluminum nitride single crystal layer.
- the present invention relates to an optical element laminate.
- the optical element laminate is an intermediate product in the optical element manufacturing process, and facilitates the transportation and storage of the intermediate product in the optical element manufacturing process, thereby contributing to an improvement in manufacturing efficiency.
- a group III nitride semiconductor containing aluminum (Al) has a direct transition band structure in the ultraviolet region corresponding to a wavelength of 200 nm to 360 nm, a highly efficient ultraviolet light emitting device can be manufactured.
- Group III nitride semiconductor devices are generally produced by chemical vapor deposition such as metal organic chemical vapor deposition (MOCVD), molecular beam epitaxy (MBE), or halide vapor epitaxy (HVPE). It is manufactured by growing a group III nitride semiconductor thin film on a crystal substrate.
- MOCVD metal organic chemical vapor deposition
- MBE molecular beam epitaxy
- HVPE halide vapor epitaxy
- a group III nitride semiconductor crystal containing Al is formed on a dissimilar material substrate such as a sapphire substrate or a silicon carbide substrate.
- a dissimilar material substrate such as a sapphire substrate
- the interface between the group III nitride semiconductor crystal layer and the seed substrate is large because the lattice constant difference between the group III nitride semiconductor crystal layer and the seed substrate is large. Therefore, there is a problem that high-density dislocations are generated in the group III nitride semiconductor crystal layer, and as a result, the dislocation density in the device layer is also increased.
- the following method has been proposed as a method of forming a group III nitride semiconductor crystal containing Al on a group III nitride seed substrate (same substrate). Specifically, first, a group III nitride single crystal thin film layer containing Al and a group III nitride non-single crystal layer containing Al are stacked on a dissimilar material substrate. Next, the dissimilar material substrate is removed, and a group III nitride single crystal layer containing Al is further laminated on the exposed thin film layer.
- a group III nitride semiconductor crystal containing Al is formed on a group III nitride seed substrate (same type substrate) produced by a physical vapor phase method represented by a sublimation method.
- a group III nitride seed substrate (same type substrate) produced by a physical vapor phase method represented by a sublimation method.
- the same kind of substrate having a small lattice constant difference from the group III nitride semiconductor crystal layer is used, generation of dislocations at the interface between the group III nitride semiconductor crystal layer and the seed substrate can be suppressed.
- the physical vapor phase method can obtain a low dislocation density group III nitride seed crystal, the use of such a substrate reduces the dislocation density in the group III nitride semiconductor crystal layer.
- Non-Patent Document 1 a seed substrate manufactured by a physical vapor phase method has many impurities or point defects, so that the seed substrate has a disadvantage that an absorption coefficient at a wavelength of 200 nm to 300 nm is remarkably large (non-patent document).
- Reference 2). As a result, since ultraviolet light is absorbed by the substrate, it has been difficult to produce a highly efficient optical element, particularly a highly efficient ultraviolet LED.
- the present invention has been made in view of the above problems, and an object of the present invention is to provide an optical element using an aluminum nitride single crystal layer having a high ultraviolet transmittance and a low dislocation density as a free-standing substrate.
- the present invention for solving the above-mentioned problems includes the following matters as a gist.
- the optical element laminate according to the present invention has an aluminum nitride seed substrate, which is the same kind of substrate, as the aluminum nitride single crystal layer and the optical element layer. is there.
- FIG. 1 is a schematic view showing one embodiment of the production process of the laminate of the present invention.
- an optical element manufacturing method of the present invention forms an aluminum nitride single crystal layer 12 by chemical vapor deposition on an aluminum nitride seed substrate 11 whose outermost surface is an aluminum nitride single crystal surface 11a.
- a first step of forming the optical element layer 20 on the aluminum nitride single crystal layer 12 to obtain the optical element laminate 2, and the optical nitride layer 2 from the optical element laminate 2 A third step of removing the seed substrate 11.
- an aluminum nitride single crystal layer 12 is formed by chemical vapor deposition on an aluminum nitride seed substrate 11 that is the same kind of substrate to obtain a first stacked body (self-standing substrate) 1.
- the manufacturing method of the aluminum nitride seed substrate 11 whose outermost surface is the aluminum nitride single crystal surface 11a is not particularly limited, and a known method is used.
- the aluminum nitride seed substrate 11 may be an aluminum nitride substrate manufactured by a chemical vapor deposition method and having an aluminum nitride single crystal surface on the outermost surface, and is a nitride manufactured by a physical vapor method such as a sublimation method.
- An aluminum single crystal substrate may be used.
- an aluminum nitride single crystal seed substrate produced by chemical vapor deposition and having an aluminum nitride single crystal surface on the outermost surface will be described below.
- an aluminum nitride single crystal substrate as proposed in Japanese Patent Application Laid-Open No. 2010-89971 may be used.
- an aluminum nitride-based laminate including an aluminum nitride non-single crystal layer as proposed in WO2009 / 090821 and JP2010-10613 may be used.
- an aluminum nitride non-single crystal layer is formed among the seed substrates manufactured by such chemical vapor deposition. It is preferable to use an aluminum nitride-based laminate including the same. Specifically, an aluminum nitride-based laminate in which an aluminum nitride single-crystal thin film layer that forms the outermost surface is laminated on a non-single-crystal aluminum nitride layer made of polycrystalline, amorphous, or a mixture thereof is used. Is preferred.
- the thickness of the aluminum nitride single crystal thin film layer forming the outermost surface is 10 nm to 1.5 ⁇ m, It is preferable to use an aluminum nitride-based laminate in which the thickness of the crystal layer is 100 times or more that of the aluminum nitride single crystal thin film layer.
- such an aluminum nitride-based laminate has a non-single crystal layer, it has a low ultraviolet transmittance and is unsuitable as a component of an optical element.
- the seed substrate itself is removed during the manufacturing process. Therefore, there is no particular problem in the optical element as the final product.
- a dissimilar substrate such as a sapphire substrate
- the non-single crystal layer has an advantage that it can be easily removed in the third step.
- a method for forming the aluminum nitride single crystal layer 12 on the aluminum nitride single crystal surface 11a located on the outermost surface of the aluminum nitride seed substrate 11 by the chemical vapor deposition method is not particularly limited. Is used. As the chemical vapor deposition method, an HVPE method or the like is common.
- the aluminum nitride single crystal layer 12 thus obtained can have an absorption coefficient as low as 30 cm ⁇ 1 or less at a wavelength of 240 nm to 300 nm and a dislocation density of 10 9 cm ⁇ 2 or less.
- the thickness of the aluminum nitride single crystal layer 12 formed in the first step is preferably as thin as possible from the viewpoint of manufacturing cost. However, handling in the manufacturing step is facilitated, and yield reduction due to generation of cracks is suppressed.
- the thickness is preferably 50 ⁇ m or more, and from a practical viewpoint, it is more preferably 100 to 300 ⁇ m, and particularly preferably 100 to 250 ⁇ m.
- the thickness of the aluminum nitride single crystal layer 12 is 500 ⁇ m or less, further 300 ⁇ m or less, particularly 250 ⁇ m or less, handling in the manufacturing process can be facilitated.
- the optical element layer 20 is formed on the first laminated body (self-standing substrate) having the aluminum nitride seed substrate 11 to be finally removed. That is, since the aluminum nitride seed substrate 11 is provided, the first stacked body (self-standing substrate) has sufficient strength even if the aluminum nitride single crystal layer 12 is thin.
- the optical element 22 obtained by the present invention has the aluminum nitride single crystal layer 12 having a relatively thin thickness, the ultraviolet transmittance can be increased. When the aluminum nitride single crystal layer 12 is thick, it is difficult to transmit ultraviolet rays. However, according to the method of the present invention, the single crystal layer 12 can be thinned, which is advantageous in this respect.
- the thickness of the aluminum nitride seed substrate 11 is not particularly limited, but considering the productivity of the optical element laminate described below, handling properties, and the ease of the third step, It is preferably 100 to 500 ⁇ m. In addition, when the said aluminum nitride type laminated body is used as this seed substrate, it is preferable that the thickness of this laminated body itself satisfies the said range.
- the surface roughness after the formation of the aluminum nitride single crystal layer 12 is not particularly limited. However, when the surface immediately after the growth of the aluminum nitride single crystal layer 12 is rough, thereby reducing the performance of the optical element layer formed in the second step, the aluminum nitride single crystal layer after the first step is finished. It is preferable to perform surface polishing of 12 to smooth the surface.
- the surface roughness of the aluminum nitride single crystal layer 12 is preferably 5 nm or less in terms of root mean square roughness (RMS value), and more preferably 1 nm or less. Preferably there is. Even when this polishing is performed, since the substrate having the seed substrate portion is handled, the substrate has sufficient strength and can be easily polished.
- the optical element layer 20 is formed on the first laminate (self-standing substrate) 1 obtained in the first step, and the second laminate, that is, the laminate for optical elements. Obtain body 2.
- the method for forming the optical element layer 20 on the aluminum nitride single crystal layer 12 is not particularly limited, and a known method is used. Normally, the optical element layer 20 is formed by chemical vapor deposition such as MOCVD.
- the formation of the optical element layer 20 by the MOCVD method will be described below.
- an organometallic group III source gas and a nitrogen source source gas are supplied onto a substrate, and a group III nitride single crystal layer is grown on the substrate.
- a known raw material can be used without particular limitation depending on the composition of the target group III nitride single crystal layer. Specifically, it is preferable to use a trimethylaluminum, triethylaluminum, trimethylgallium, triethylgallium, or trimethylindium gas as the group III source gas.
- the MOCVD apparatus used in the present invention is not particularly limited as long as the structure can implement the present invention, and a known apparatus or a commercially available MOCVD apparatus can be used.
- the LED structure described below is an example of a structure in which an N-type group III nitride semiconductor layer, an active layer, a P-type group III nitride semiconductor layer, and a P-type group III nitride contact layer are sequentially stacked on a substrate.
- the present invention is not limited to the following structure.
- the free-standing substrate 1 is heated to 1050 ° C. or higher, more preferably 1150 ° C. or higher, and a hydrogen atmosphere
- trimethylaluminum, trimethylgallium, ammonia, monosilane or tetraethylsilane, and hydrogen, nitrogen, etc. as a carrier gas of the source gas are introduced into the MOCVD apparatus, and N-type A group III nitride semiconductor layer is formed.
- a buffer layer can be formed for the purpose of improving N-type characteristics before forming the N-type Group III nitride semiconductor layer.
- the buffer layer is preferably an N-type Group III nitride layer having the same or intermediate lattice constant as the Group III nitride semiconductor layer and the aluminum nitride single crystal layer.
- the buffer layer may be a single layer or a plurality of laminated bodies having different compositions.
- the quantum well structure is a stacked structure in which a well layer having a thickness of several to several tens of nm and a barrier layer having a larger band gap energy than the well layer are combined.
- the film thickness and the like may be appropriately set so that desired optical characteristics can be obtained.
- trimethylindium, N-type or P-type impurity raw materials may be added for the purpose of improving optical characteristics.
- trimethylaluminum, trimethylgallium, ammonia, biscyclopentadienylmagnesium, and hydrogen, nitrogen or the like as a source gas carrier gas are introduced into the MOCVD apparatus to form a P-type group III nitride semiconductor layer.
- trimethylgallium, ammonia, biscyclopentadienylmagnesium, and hydrogen, nitrogen, etc. as a source gas are introduced into the MOCVD apparatus to form a P-type group III nitride semiconductor contact layer.
- the raw material supply ratio, the growth temperature, the ratio of the group V element (nitrogen, etc.) to the group III element (V / III ratio), etc. when forming the group III nitride semiconductor layer are the desired optical characteristics and What is necessary is just to set suitably so that an electroconductive characteristic may be acquired.
- the optical element laminate 2 of the present invention is an intermediate product obtained through the second step, and is an aluminum nitride seed substrate and nitrided with excellent optical properties formed on the aluminum nitride seed substrate.
- An aluminum single crystal layer and an optical element formed on the aluminum nitride single crystal layer are included.
- the optical element laminate 2 of the present invention facilitates its transportation, storage, and the like in the optical element manufacturing process, and improves manufacturing efficiency.
- the aluminum nitride seed substrate 11 is removed from the optical element laminate 2 obtained in the second step to obtain the optical element 22.
- the optical element 22 manufactured by the above-described process function as a device it is necessary to perform processing for elementization, such as etching processing for exposing a predetermined conductive layer, electrode formation processing on the surface of the conductive layer, etc. There is.
- the third step of the present invention can be performed before performing the processing step for forming the device, or can be performed after performing the processing for forming the device.
- the order in which the processing steps for elementization and the third step of the present invention are performed may be determined as appropriate in the implementation of the present invention in consideration of productivity and handling properties.
- the method for removing the aluminum nitride seed substrate 11 from the optical element laminate 2 is not particularly limited, and known methods such as polishing, reactive ion etching, and wet etching using an alkaline solution can be used. It is preferable to remove by polishing.
- forming irregularities on the surface of the aluminum nitride single crystal layer 12 on the side from which the aluminum nitride seed substrate 11 has been removed is also preferable as a means for improving the performance of the optical element.
- the optical element 22 obtained in this way is subjected to processing such as chipping if necessary and used for various purposes.
- Examples of the optical element include an LED (light emitting diode).
- the aluminum nitride single crystal layer 12 is formed by the chemical vapor deposition method on the aluminum nitride single crystal seed substrate 11 which is the same type substrate manufactured by the chemical vapor deposition method. 1 laminate (free-standing substrate) 1 is prepared.
- the dislocation density of the aluminum nitride single crystal seed substrate 11 is low, the dislocation density can be reduced also in the aluminum nitride single crystal layer 12 and the optical element layer 20 formed thereon.
- the aluminum nitride single crystal layer 12 is formed by chemical vapor deposition, low dislocations and high ultraviolet transmission efficiency can be realized.
- the difference in refractive efficiency between the aluminum nitride single crystal layer 12 and the optical element layer 20 is small, the light extraction efficiency is also improved as compared with the conventional case.
- the aluminum nitride single crystal seed substrate 11 may be produced by a physical vapor deposition method such as a sublimation method other than the above-described chemical vapor deposition method.
- the ultraviolet light emitting element is exemplified as the optical element according to the present invention, but the electronic component according to the present invention is not limited to a light emitting element such as a light emitting diode element.
- the optical element manufacturing method of the present invention can also be applied to manufacturing a light receiving element in which a semiconductor element having a wide range of sensitivity from ultraviolet to infrared is sealed.
- the aluminum nitride seed substrate 11 was produced by the method described in WO2009 / 090821.
- the thickness of the aluminum nitride single crystal thin film layer constituting the aluminum nitride single crystal surface 11a is 200 nm
- the thickness of the aluminum nitride non-single crystal layer (aluminum nitride polycrystalline layer) therebelow is A laminate having a thickness of 300 ⁇ m was used.
- two aluminum nitride seed substrates 11 having an 8 mm square were prepared.
- the aluminum nitride seed substrate 11 is flowed at a flow rate of 10 slm of hydrogen and 200 sccm of ammonia.
- the seed substrate 11 was heated to 1450 ° C. and held for 20 minutes to perform surface cleaning.
- aluminum trichloride gas 5 sccm obtained by reacting metallic aluminum heated to 500 ° C. and hydrogen chloride gas, ammonia gas 15 sccm, nitrogen gas 1500 sccm and hydrogen 5000 sccm as carrier gases are supplied onto the aluminum nitride seed substrate 11.
- the single crystal layer 12 was grown to 150 ⁇ m.
- the surface of the aluminum nitride single crystal layer 12 was observed with a differential interference optical microscope, and in each sample, it was confirmed that the surface of the aluminum nitride single crystal layer 12 was free of cracks. Further, although the surface of the aluminum nitride single crystal layer 12 was very flat locally, relatively large irregularities existed on the entire surface of the substrate as an entire 8 mm square.
- the non-single-crystal aluminum nitride layer (aluminum nitride polycrystalline layer) on the back surface is removed by mechanical polishing, and then CMP is performed. By polishing until the RMS value became 5 nm or less, a single body of the aluminum nitride single crystal layer 12 in a substantially double-sided mirror state was taken out.
- the film thickness of the aluminum nitride single crystal layer 12 after polishing was 100 ⁇ m.
- the threading dislocation density on the surface of the polished aluminum nitride single crystal layer 12 was measured by plane observation using a transmission electron microscope (acceleration voltage 300 kV), it was 3 ⁇ 10 8 cm ⁇ 2 . Further, when the transmittance of the aluminum nitride single crystal layer 12 was measured with an ultraviolet-visible spectrophotometer (UV-2550, manufactured by Shimadzu Corporation), the external transmittance at a wavelength of 240 nm to 350 nm was 40% or more. When the refractive index of the aluminum nitride single crystal was 2.4 and the absorption coefficient was calculated from the film thickness and transmittance, the absorption coefficient at wavelengths from 240 nm to 350 nm was 20 cm ⁇ 1 or less.
- one of the first laminates 1 was placed on a susceptor in the MOCVD apparatus so that the polished aluminum nitride single crystal layer 12 surface was the outermost surface. Thereafter, while flowing hydrogen at a flow rate of 13 slm, the free-standing substrate 1 was heated to 1250 ° C. and held for 10 minutes to perform surface cleaning.
- the aluminum nitride buffer layer is formed on the aluminum nitride single crystal layer 12 under the conditions that the temperature of the self-supporting substrate 1 is 1200 ° C., the trimethylaluminum flow rate is 25 ⁇ mol / min, the ammonia flow rate is 1 slm, the total flow rate is 10 slm, and the pressure is 50 Torr. Was formed to a thickness of 0.1 ⁇ m. Then, the 1120 ° C.
- the substrate temperature on the susceptor trimethylgallium flow rate 20 [mu] mol / min, trimethylaluminum 35 [mu] mol / min, ammonia flow rate 1.5 slm, entire flow 10 slm, the pressure is under the condition of 50 Torr Al 0.7 Ga
- a 0.3 N buffer layer was formed to 0.2 ⁇ m.
- an N-type Al 0.7 Ga 0.3 N layer was formed to 1.2 ⁇ m under the same conditions as the buffer layer except that 3 nmol / min of tetraethylsilane was simultaneously supplied.
- an Al 0.3 Ga 0.7 N well layer was formed to 2 nm under the same conditions as the buffer layer except that the trimethylgallium flow rate was 40 ⁇ mol / min and trimethylaluminum was 3 ⁇ mol / min.
- a 15 nm barrier layer was formed under the same conditions as the buffer layer.
- a triple quantum well layer was formed by repeating the growth of the well layer and the barrier layer three times.
- a P-type Al 0.8 Ga 0.2 N layer is formed to a thickness of 20 nm under the same conditions as the buffer layer except that the trimethylgallium flow rate is 15 ⁇ mol / min and biscyclopentadienyl magnesium 0.8 ⁇ mol / min is simultaneously supplied. did.
- a 0.2 ⁇ m P-type GaN contact layer is formed under the conditions of a trimethylgallium flow rate of 40 ⁇ mol / min, biscyclopentadienyl magnesium 0.3 ⁇ mol / min, an ammonia flow rate of 2.0 slm, a total flow rate of 8 slm, and a pressure of 150 Torr. did.
- the substrate was taken out of the MOCVD apparatus and heat-treated in a nitrogen atmosphere for 20 minutes at 800 ° C.
- Ti (20 nm) / Al (100 nm) / A Ti (20 nm) / Au (50 nm) electrode was formed, and heat treatment was performed in a nitrogen atmosphere at 1000 ° C. for 1 minute.
- a Ni (20 nm) / Au (100 nm) electrode was formed on the P-type GaN contact layer by vacuum deposition, and heat treatment was performed in a nitrogen atmosphere for 5 minutes at 500 ° C.
- the second laminated body 2 (optical element laminated body 2) in which the optical element layer 20 was laminated on the aluminum nitride single crystal layer 12 of the first laminated body was produced.
- the light emitting characteristics of the optical element laminate 2 produced in this way were evaluated from the back side of the device at the time of DC 10 mA operation, a weak single emission peak with an emission wavelength of 265 nm could be confirmed.
- the aluminum nitride non-single-crystal layer (aluminum nitride polycrystal layer) on the back surface of the optical element laminate 2 is removed by mechanical polishing, and then polished by CMP until the RMS value becomes 5 nm or less, whereby the optical element 22 is formed.
- the optical element 22 had a thickness of about 100 ⁇ m.
- this optical element 22 was measured for light emission by the same method as that for the optical element laminate 2, it was a single peak emission with an emission wavelength of 265 nm.
- the emission peak intensity of this optical element 22 was the same as that of the optical element laminate 2. It was confirmed that it was 10 times or more than the strength.
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Abstract
Description
(1)最表面が窒化アルミニウム単結晶面である窒化アルミニウム種基板上に、化学気相成長法により窒化アルミニウム単結晶層を形成する第1の工程と、
前記窒化アルミニウム単結晶層上に、光学素子層を形成して光学素子用積層体を得る第2の工程と、
前記光学素子用積層体から前記窒化アルミニウム種基板を除去する第3の工程と
を含む光学素子の製造方法。
(2) 前記第1の工程における前記窒化アルミニウム単結晶層の厚みは50μm以上である(1)に記載の光学素子の製造方法。
(3) 前記第2の工程における前記光学素子層はLED素子層であることを特徴とする(1)または(2)に記載の光学素子の製造方法。
(4) 最表面が窒化アルミニウム単結晶面である窒化アルミニウム種基板と、
前記窒化アルミニウム種基板上に形成された窒化アルミニウム単結晶層と、
前記窒化アルミニウム単結晶層上に形成された光学素子層と、を有する光学素子用積層体。
(5) 前記窒化アルミニウム単結晶層の波長240nmから300nmにおける吸収係数が30cm-1以下である(4)に記載の光学素子用積層体。
(6) 前記窒化アルミニウム単結晶層の転位密度が109cm-2以下である(4)または(5)に記載の光学素子用積層体。
本発明の第1の工程では、同種基板である窒化アルミニウム種基板11上に、化学気相成長法により窒化アルミニウム単結晶層12を形成して第1の積層体(自立基板)1を得る。
本発明の第2の工程では、第1の工程で得られた、第1の積層体(自立基板)1上に光学素子層20を形成して、第2の積層体、すなわち光学素子用積層体2を得る。
本発明の第3の工程では、第2の工程で得られた光学素子用積層体2から窒化アルミニウム種基板11を除去して、光学素子22を得る。
窒化アルミニウム種基板11は、WO2009/090821に記載の方法により作製した。この窒化アルミニウム種基板11は、窒化アルミニウム単結晶面11aを構成する窒化アルミニウム単結晶薄膜層の厚みが200nmであって、その下の窒化アルミニウム非単結晶層(窒化アルミニウム多結晶層)の厚みが300μmである積層体を用いた。また、この窒化アルミニウム種基板11は、8mm角のものを2枚準備した。
2枚の前記窒化アルミニウム種基板11を窒化アルミニウム単結晶面11aが最表面となるようにHVPE装置内のサセプター上に設置した後、水素を10slm、アンモニアを200sccmの流量で流しながら、該窒化アルミニウム種基板11を1450℃に加熱し、20分間保持することにより表面クリーニングを行った。次いで、500℃に加熱した金属アルミニウムと塩化水素ガスを反応させて得られる三塩化アルミニウムガス5sccm、アンモニアガス15sccm、キャリアガスとして窒素1500sccm、水素5000sccmを窒化アルミニウム種基板11上に供給し、窒化アルミニウム単結晶層12を150μm成長させた。
次いで、上記窒化アルミニウム単結晶層12の表面をCMP(Chemical Mechanical Polishing)研磨によって、RMS値が1nm以下になるまで研磨し、第1の積層体1(自立基板1)を得た。
次いで、第1の積層体1(自立基板1)の1枚を、研磨された窒化アルミニウム単結晶層12表面が最表面となるようにMOCVD装置内のサセプター上に設置した。その後、水素を13slmの流量で流しながら、該自立基板1を1250℃まで加熱し、10分間保持することで表面クリーニングを行った。
前記光学素子用積層体2の裏面の窒化アルミニウム非単結晶層(窒化アルミニウム多結晶層)を機械研磨により除去し、その後CMP研磨によってRMS値が5nm以下になるまで研磨して、光学素子22を作製した。なお、この光学素子22の厚みは、約100μmであった。この光学素子22を光学素子用積層体2と同様の方法で発光測定を行ったところ、発光波長265nmのシングルピーク発光であり、この光学素子22の発光ピーク強度は、光学素子用積層体2の強度よりも10倍以上であることが確認された。
1 第1の積層体(自立基板)
11 窒化アルミニウム種基板
11a 窒化アルミニウム単結晶面
12 窒化アルミニウム単結晶層
20 光学素子層
22 光学素子
Claims (6)
- 最表面が窒化アルミニウム単結晶面である窒化アルミニウム種基板上に、化学気相成長法により窒化アルミニウム単結晶層を形成する第1の工程と、
前記窒化アルミニウム単結晶層上に、光学素子層を形成して光学素子用積層体を得る第2の工程と、
前記光学素子用積層体から前記窒化アルミニウム種基板を除去する第3の工程と
を含む光学素子の製造方法。 - 前記第1の工程における前記窒化アルミニウム単結晶層の厚みは50μm以上である請求項1に記載の光学素子の製造方法。
- 前記第2の工程における前記光学素子層はLED素子層であることを特徴とする請求項1または2に記載の光学素子の製造方法。
- 最表面が窒化アルミニウム単結晶面である窒化アルミニウム種基板と、
前記窒化アルミニウム種基板上に形成された窒化アルミニウム単結晶層と、
前記窒化アルミニウム単結晶層上に形成された光学素子層と、を有する光学素子用積層体。 - 前記窒化アルミニウム単結晶層の240nmから300nmにおける吸収係数が30cm-1以下である請求項4に記載の光学素子用積層体。
- 前記窒化アルミニウム単結晶層の転位密度が109cm-2未満である請求項4または5に記載の光学素子用積層体。
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JP2020537360A (ja) * | 2017-10-16 | 2020-12-17 | クリスタル アイエス, インコーポレーテッドCrystal Is, Inc. | 電子及び光電子デバイスのための窒化アルミニウム基板の電気化学的除去 |
Also Published As
Publication number | Publication date |
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EP2634294A1 (en) | 2013-09-04 |
EP2634294B1 (en) | 2020-04-29 |
JPWO2012056928A1 (ja) | 2014-03-20 |
US20130214325A1 (en) | 2013-08-22 |
EP2634294A4 (en) | 2015-05-13 |
KR101852519B1 (ko) | 2018-04-26 |
JP5931737B2 (ja) | 2016-06-08 |
KR20130122727A (ko) | 2013-11-08 |
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