WO2010001760A1 - アルミナセラミック - Google Patents
アルミナセラミック Download PDFInfo
- Publication number
- WO2010001760A1 WO2010001760A1 PCT/JP2009/061334 JP2009061334W WO2010001760A1 WO 2010001760 A1 WO2010001760 A1 WO 2010001760A1 JP 2009061334 W JP2009061334 W JP 2009061334W WO 2010001760 A1 WO2010001760 A1 WO 2010001760A1
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- Prior art keywords
- alumina ceramic
- alumina
- phase
- light
- mass
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 6
- 229910052788 barium Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 21
- 239000000843 powder Substances 0.000 description 17
- 239000002002 slurry Substances 0.000 description 16
- 239000002994 raw material Substances 0.000 description 14
- 238000010304 firing Methods 0.000 description 13
- 239000000919 ceramic Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- 239000011230 binding agent Substances 0.000 description 11
- 239000000758 substrate Substances 0.000 description 10
- 150000001553 barium compounds Chemical class 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 9
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 8
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 8
- 238000000465 moulding Methods 0.000 description 8
- 229920005989 resin Polymers 0.000 description 8
- 239000011347 resin Substances 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000000314 lubricant Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 3
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000004014 plasticizer Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 1
- 229920002799 BoPET Polymers 0.000 description 1
- HIZCTWCPHWUPFU-UHFFFAOYSA-N Glycerol tribenzoate Chemical compound C=1C=CC=CC=1C(=O)OCC(OC(=O)C=1C=CC=CC=1)COC(=O)C1=CC=CC=C1 HIZCTWCPHWUPFU-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- ZGLFRTJDWWKIAK-UHFFFAOYSA-M [2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]-triphenylphosphanium;bromide Chemical compound [Br-].C=1C=CC=CC=1[P+](C=1C=CC=CC=1)(CC(=O)OC(C)(C)C)C1=CC=CC=C1 ZGLFRTJDWWKIAK-UHFFFAOYSA-M 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 description 1
- 229910001632 barium fluoride Inorganic materials 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- -1 for example Substances 0.000 description 1
- 239000011361 granulated particle Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 238000001579 optical reflectometry Methods 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
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Definitions
- the present invention relates to an alumina ceramic having excellent light reflectivity.
- ceramic packages have been used as light-emitting element storage packages (hereinafter also simply referred to as packages) for storing light-emitting elements such as high-intensity light-emitting diodes (LEDs) and semiconductor lasers (LDs). .
- LEDs high-intensity light-emitting diodes
- LDs semiconductor lasers
- a conventional ceramic package includes a base body on which a light emitting element is mounted and a frame body provided on the base body and having a through hole.
- the base is provided with a power distribution conductor for energizing from the outside, and the light emitting element is electrically connected to the power distribution conductor by a bonding wire. Then, the light emitting element emits light when it is energized from the outside through the power distribution conductor and the bonding wire, and the emitted light is directly emitted to the outside or reflected to the surface of the base or the inner peripheral surface of the through hole of the frame. Released to the outside. Therefore, the shape and composition of the surface of the substrate and the inner peripheral surface of the through hole of the frame body have a great influence on the light emission efficiency of the light emitting device.
- the frame of the light emitting device As the frame of the light emitting device as described above, one made of a metal having a high reflectance is known. In this case, since the thermal expansion coefficient of the ceramic base and the metal frame is different, the frame may be peeled off from the base due to heat generated from the light emitting element. In addition, in order to prevent such peeling, a ceramic frame that has been subjected to metal plating is also known (see, for example, Patent Document 1). Ag is known as a plating material having a high reflectance. In this case, the reflectance is about 90% with respect to the reflectance of barium sulfate in light having a wavelength of about 460 nm. However, the reflectance of light having a wavelength of about 460 nm or less is low, and the reflectance is 77% when averaged in the range of 250 nm to 800 nm.
- the conventional ceramic package cannot obtain a sufficient light reflection performance even when the metal plating is applied to the ceramic surface.
- the present invention has been made in view of the above circumstances, and an object thereof is to provide an alumina ceramic excellent in light reflection performance without depositing metal plating on the ceramic.
- it is to provide an alumina ceramic excellent in reflectance of light having a wavelength of 300 to 400 nm.
- it is providing the light reflection material for light emitting elements excellent in light reflection performance.
- an alumina ceramic containing a Ba 0.808 Al 1.71 Si 2.29 O 8 phase has excellent light reflection performance.
- the intensity ratio (the former / the latter) of the peak at the diffraction angle (2 ⁇ ) of 43.3 ° and the peak at the diffraction angle (2 ⁇ ) of 22.5 ° is in the range of 0.5 to 2.5.
- the inventors of the present invention in an alumina ceramic containing a Ba 0.808 Al 1.71 Si 2.29 O 8 phase, have a Ba / Si molar ratio (Ba / Si) of 8/1 to 8/12 . It was found that the alumina ceramic present in the range is excellent in the reflectance of light having a wavelength of 300 to 400 nm.
- the alumina ceramic containing the Ba 0.808 Al 1.71 Si 2.29 O 8 phase of the present invention has excellent light reflection performance. Further, in the X-ray diffraction, the intensity ratio between the peak at the diffraction angle (2 ⁇ ) of 43.3 ° and the peak at the diffraction angle (2 ⁇ ) of 22.5 ° is in the range of 0.5 to 2.5.
- An alumina ceramic containing 0.808 Al 1.71 Si 2.29 O 8 phase exhibits particularly excellent light reflection performance.
- the alumina ceramic of the present invention is particularly excellent in the reflectance of light having a wavelength of 300 to 400 nm.
- FIG. 1 is an X-ray diffraction pattern of the alumina ceramic of the present invention of Example 1.
- FIG. 2 is an X-ray diffraction pattern of the alumina ceramic of the present invention in Example 2.
- FIG. 3 is a graph showing the results of measuring the reflectance of light of each wavelength for the alumina ceramics of the present invention of Examples 1 to 4 and the conventional alumina substrate of Comparative Example 1.
- FIG. 4 is an X-ray diffraction pattern represented by the Ba 0.808 Al 1.71 Si 2.29 O 8 phase described in ICDD card number 01-088-1050.
- Figure 5 is described in ICDD card No. 01-070-7049 is an X-ray diffraction pattern shown corundum (Al 2 O 3) phase.
- the alumina ceramic containing the Ba 0.808 Al 1.71 Si 2.29 O 8 phase of the present invention is obtained by firing a raw material containing alumina (Al 2 O 3 ), silica (SiO 2 ), and a barium compound. Can be made.
- alumina having an average particle size of 5 ⁇ m or less It is preferable to use an alumina having an average particle size of 5 ⁇ m or less. Considering the light reflection performance, flexibility, sinterability during production, etc. of alumina ceramic, it is particularly preferable to use alumina having an average particle size of 0.1 to 3 ⁇ m.
- a plurality of types of alumina having different average particle diameters may be mixed and used for manufacturing the alumina ceramic of the present invention. be able to.
- the average particle diameters are 3 ⁇ m and 0.2 ⁇ m, 3 ⁇ m and 0.3 ⁇ m, 3 ⁇ m and 0.4 ⁇ m, 3 ⁇ m and 0.5 ⁇ m, 3 ⁇ m and 0.3 ⁇ m, respectively.
- Combinations of 6 ⁇ m, 2 ⁇ m and 0.2 ⁇ m, 2 ⁇ m and 0.3 ⁇ m, 2 ⁇ m and 0.4 ⁇ m, 2 ⁇ m and 0.5 ⁇ m, 2 ⁇ m and 0.6 m, etc. are not limited to these, but three types The above may be combined.
- the blending ratio according to the weight parts of large particle alumina / small particle alumina is preferably 100/1 to 60/40.
- the blending ratio by weight parts of large particle alumina / small particle alumina is preferably 85/15 to 65/35, 80/20 to 70/30 is more preferable.
- silica used for producing the alumina ceramic of the present invention it is preferable to use one having an average particle diameter of 1 ⁇ m or less.
- silica having an average particle size of 0.1 to 0.7 ⁇ m it is preferable to use silica having an average particle size of 0.3 to 0.6 ⁇ m.
- the barium compound used for producing the alumina ceramic of the present invention is not particularly limited, and examples thereof include barium hydride, barium fluoride, barium hydroxide, barium oxide, barium chloride, barium carbonate, barium sulfate, and barium nitrate. Of these, barium oxide and barium carbonate are preferable, and barium carbonate is particularly preferable.
- the barium compound having an average particle size of 1.0 to 2.0 ⁇ m is preferably used.
- the molar ratio of Ba and Si (Ba / Si) in the alumina ceramic after sintering the raw material is 8/1 to 8 / It is preferable to mix the barium compound and silica so that the molar ratio is 12, more preferably the molar ratio is 8/3 to 8/12.
- the method for producing the alumina ceramic of the present invention is not particularly limited, and a known method can be used.
- an appropriate binder, solvent, etc. are added to the raw materials containing the above-mentioned alumina, silica, and barium compounds to form a slurry, which is converted into a green sheet by a doctor blade method, a calender roll method, or the like, and then heated to a high temperature (1400 ° C. It can be produced by a green sheet method of baking at ⁇ 1600 ° C.). It can also be produced by a powder molding method in which a raw material powder is filled in a molding machine and compacted, and then the compact is fired. When obtaining a plate-like ceramic sintered body, it is preferable to produce it by a green sheet method.
- the binder resin things, such as an acrylic type and PVA (polyvinyl alcohol) type, can be used, for example.
- the content of the binder resin with respect to the solid content of the slurry is preferably 0.5% by mass to 5.0% by mass, and more preferably 1.5% by mass to 3.5% by mass.
- strength of a powder molded product will become weak.
- the lubricant for example, a stearic acid emulsion can be used, and the content of the lubricant with respect to the solid content of the slurry is preferably 0.05% by mass to 0.5% by mass, more preferably 0.1% by mass. Is 0.3 mass%.
- the solvent for example, water can be used. The amount of the solvent used is preferably 20 to 80% by mass, more preferably 40 to 60% by mass.
- the slurry is dried and the raw powder particles are granulated to a size suitable for molding with a powder molding machine.
- a spray dryer can be used for granulating the particles.
- the granulated particle diameter is preferably 25 ⁇ m to 200 ⁇ m, more preferably 30 ⁇ m to 150 ⁇ m.
- the granulated powder is classified using a sieve or the like. If the particles are too large at the time of powder molding, the filling property into the mold deteriorates. If the particles are too fine, the particles enter the clearance of the mold and burrs tend to occur.
- the granulated raw material powder is filled in a mold and molded by applying pressure at room temperature.
- the pressure applied to the powder is preferably 0.5t / cm 2 ⁇ 2.0t / cm 2, more preferably a 0.7t / cm 2 ⁇ 1.5t / cm 2.
- the molded body obtained by the above molding is fired in a firing furnace.
- the firing temperature condition is preferably 1400 ° C. to 1600 ° C.
- Firing is carried out at a rate of temperature rise to the firing temperature, firing time, a cooling rate from the firing temperature, etc. suitable for producing an alumina ceramic containing the Ba 0.808 Al 1.71 Si 2.29 O 8 phase.
- the molded body is first held at 600 ° C. for 8 hours, then heated to 1600 ° C. over 8 hours, held for 2 hours, and then allowed to cool for 6 hours.
- polishing is performed using a barrel polishing machine or the like to remove burrs and the like as desired.
- an alumina ceramic containing the Ba 0.808 Al 1.71 Si 2.29 O 8 phase of the present invention can be produced.
- alumina ceramic containing Ba 0.808 Al 1.71 Si 2.29 O 8 phase according to the present invention, an example of a manufacturing method using a green sheet method is explained.
- Alumina, silica, and barium compounds were each pulverized to a predetermined size to prepare raw material powders, and then these raw material powders were weighed to achieve the above-mentioned blending ratio, and this was mixed with solvent, binder resin, dispersant, plastic A slurry is obtained by adding an agent and kneading.
- a ball mill can be used for pulverizing the raw materials and kneading the raw material powders.
- binder resin binders, such as an acrylic type and PVB (polyvinyl ptyral) type, can be used, for example.
- content of the binder resin with respect to the solid content of the slurry is preferably 4.0% by mass to 20% by mass, and more preferably 6.0% by mass to 8.0% by mass.
- dispersant various surfactants can be used, and the content of the dispersant with respect to the solid content of the slurry is preferably 0.1% by mass to 1.0% by mass, and more preferably 0.3%. % By mass to 0.5% by mass.
- the plasticizer for example, DOP (Dioctyl Phthalate), DBP (Dlbutyl Phthalate) and the like can be used, and the plasticizer content in the solid content of the slurry is preferably 3.0% by mass to 15% by mass. More preferably, it is 4.0 mass to 6.0 mass%.
- the amount of the solvent used is preferably such that the total amount of solid content of the slurry is 70% by mass to 80% by mass.
- the viscosity of the slurry is preferably 3000 cps to 30000 cps, more preferably 10,000 cps to 20000 cps.
- the obtained slurry is poured into a film coated with a release agent, and the solvent is evaporated by drying.
- the drying temperature is preferably 80 ° C. to 130 ° C., more preferably 100 ° C. to 120 ° C.
- the drying speed is preferably 0.2 m / min to 2.0 m / min.
- a green sheet is generated.
- This green sheet is punched into a desired shape with a press molding machine and fired in a firing furnace.
- the firing temperature is preferably 1400 ° C. to 1600 ° C.
- Firing is appropriately selected from a heating rate to a firing temperature, a firing time, a cooling rate from the firing temperature, and the like suitable for the production of an alumina ceramic containing the Ba 0.808 Al 1.71 Si 2.29 O 8 phase. And do it.
- the temperature is first held at 600 ° C. for 8 hours, then heated to 1600 ° C. over 8 hours, held for 2 hours, and then allowed to cool for 6 hours.
- polishing can be performed using a sandblasting machine or the like.
- an alumina ceramic containing the Ba 0.808 Al 1.71 Si 2.29 O 8 phase of the present invention can be produced.
- the presence of the Ba 0.808 Al 1.71 Si 2.29 O 8 phase in the alumina ceramic of the present invention can be confirmed by measuring X-ray diffraction by the following [X-ray diffraction measurement method].
- the light reflection performance of the alumina ceramic of the present invention is evaluated by the following [Reflectance measuring method].
- X-ray diffraction measurement method X-ray diffraction is measured in accordance with JIS 1481 asbestos qualitative analysis conditions using a Spectris X-ray diffractometer X'pert PRO. The measurement conditions are as follows. The measurement result confirms the presence of the Ba 0.808 Al 1.71 Si 2.29 O 8 phase as compared with the reference data of ICDD (International Center for Diffraction Data). Measurement conditions X-ray counter cathode Cu Tube voltage (kV) 40 Tube current (mA) 40 Scanning speed 0.02 ° x 10 seconds Monochromatization (removal of K ⁇ rays) Ni filter Scanning range (°, 2 ⁇ ) 5-80 Divergent slit (°) 1
- the reflectance is measured using a Hitachi spectrophotometer U-4000. Based on JIS K7105, the wavelength dependence of the sum of specular reflection and diffuse reflection is obtained. Aluminum oxide is used as the standard white plate, and the reflectance of each standard white plate is 100%, and the reflectance of each material is evaluated using relative values.
- the alumina ceramic containing the Ba 0.808 Al 1.71 Si 2.29 O 8 phase of the present invention is used for a light emitting element such as a substrate for mounting a light emitting element or a frame body that reflects light emitted from the light emitting element. It can be used as a reflective material.
- Example 1 89 parts by weight of high-purity alumina “AES-12 (average particle size 0.4 ⁇ m)” (purity 99.5%) manufactured by Sumitomo Chemical Co., Ltd., and high-purity barium carbonate “LSR (average particle size 1. 4 ⁇ m) ”, 8 parts by weight of fine-grain silica“ SO-C2 (average particle size 0.5 ⁇ m) ”manufactured by Shin-Etsu Quartz, 3 parts by weight of“ NCB-156 ”binder manufactured by Dainippon Ink, Further, 0.1 part by weight of a lubricant “Cerosol 920” manufactured by Chukyo Yushi Co., Ltd.
- This granulated product was filled in a frame mold and molded using a 10-ton press manufactured by Sanken Seiki Co., Ltd. at room temperature with a pressure of 1 t / cm 2 to obtain a frame-shaped product. . And this frame-shaped object was baked at 1550 degreeC for 2 hours, and the alumina ceramic frame was produced.
- Example 2 68.8 parts by weight of low soda alumina “ALM-42E (average particle size 2.0 ⁇ m)” (purity 99.9%) manufactured by Sumitomo Chemical Co., Ltd., high purity alumina “AES-12 (average particle size) manufactured by Sumitomo Chemical Co., Ltd.
- Parts, 4 parts by weight of “DOP” as a plasticizer, and 0.5 parts by weight of sorbitan sesquiolate as a lubricant, and 30 parts by weight of a toluene / ethanol mixed solvent (weight ratio 50/50) were added thereto.
- Mix for 48 hours in a ball mill A slurry was obtained by the.
- the slurry was applied to a release PET film, dried at a temperature of 110 ° C., and then peeled off to obtain a green sheet. This was punched into an arbitrary shape and fired at 1600 ° C. for 2 hours to produce an alumina ceramic substrate.
- Example 3 As the alumina, 60.2 parts by weight of low soda alumina “ALM-42E (average particle size 2.0 ⁇ m)” (purity 99.9%) and high-purity alumina “AES-12 (average particle size 0.4 ⁇ m)” ( An alumina ceramic substrate was produced in the same manner as in Example 2 except that 25.8 parts by weight of 99.5% purity was used.
- ALM-42E average particle size 2.0 ⁇ m
- AES-12 average particle size 0.4 ⁇ m
- Example 4 An alumina ceramic substrate was produced in the same manner as in Example 2 except that 86 parts by weight of low soda alumina “ALM-42E (average particle size 2.0 ⁇ m)” (purity 99.9%) was used as alumina. .
- the alumina ceramics of Examples 1 and 2 have an intensity ratio between the peak at the diffraction angle (2 ⁇ ) of 43.3 ° due to the corundum (Al 2 O 3 ) phase and the peak at the diffraction angle (2 ⁇ ) of 22.5 °. Were 2.0 and 1.1, respectively.
- FIG. 4 are described in ICDD card No. 01-088-1050, the X-ray diffraction pattern exhibited Ba 0.808 Al 1.71 Si 2.29 O 8 phase, in Figure 5, ICDD card number
- the X-ray diffraction patterns shown by the corundum (Al 2 O 3 ) phase described in 01-070-7049 were shown, respectively.
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Abstract
Description
上記滑剤としては、例えばステアリン酸エマルジョンを使用することができ、スラリーの固形分中に対する滑剤の含有量は、0.05質量%~0.5質量%が好ましく、さらに好ましくは0.1質量%~0.3質量%である。
上記溶媒としては、例えば水を使用することができる。溶媒の使用量は、20~80質量%が好ましく、40~60質量%がより好ましい。
このようにして本発明のBa0.808 Al1.71Si2.29O8 相を含有するアルミナセラミックを作製することができる。
上記分散剤としては、各種界面活性剤を使用することができ、スラリーの固形分中に対する分散剤の含有量は、0.1質量%~1.0質量%が好ましく、さらに好ましくは0.3質量%~0.5質量%である。
上記可塑剤としては、例えばDOP(Diocty lPhthalate)、DBP(Dlbutyl Phthalate)等を使用することができ、スラリーの固形分中に対する可塑剤の含有量は、3.0質量%~15質量%が好ましく、さらに好ましくは4.0質量~6.0質量%である。
このようにして本発明のBa0.808 Al1.71Si2.29O8 相を含有するアルミナセラミックを作製することができる。
X線回折は、スペクトリス社製X線回折装置X’pert PROを使用して、JIS1481のアスベスト定性分析条件に準拠し測定する。測定条件は以下の通りである。測定結果は、ICDD (International Centre for Diffraction Data)のリファレンスデータと比較して、Ba0.808 Al1.71Si2.29O8 相の存在を確認する。
測定条件
X線対陰極 Cu
管電圧(kV) 40
管電流(mA) 40
走査速度 0.02°×10秒
単色化(Kβ線の除去) Niフィルタ
走査範囲(°、2θ) 5~80
発散スリット(°) 1
反射率は、日立製作所製分光光度計U-4000を使用して測定する。JIS K7105に準拠し、鏡面反射と拡散反射の和の波長依存性を求める。標準白板として酸化アルミニウムを使用し、この標準白板の反射率を100%として各資料の反射率を相対値を用いて評価する。
住友化学社製の高純度アルミナ「AES-12(平均粒径0.4μm)」(純度99.5%)を89重量部、日本化学社製の高純度炭酸バリウム「LSR(平均粒径1.4μm)」を8重量部、信越石英社製の微粒子シリカ「SO-C2(平均粒径0.5μm)」を3重量部、大日本インキ社製のバインダー「NCB-156」を3重量部、および中京油脂社製の滑剤「セロゾール920」を0.1重量部、を配合して水を加え、ボールミル中で混合することによりスラリーを得た。次いで、110℃の温度条件により乾燥して造粒し、目開き25μmおよび150μmの篩いを用いて、微細粒子および粗大粒子を除去した。
住友化学社製のローソーダアルミナ「ALM-42E(平均粒径2.0μm)」(純度99.9%)を68.8重量部、住友化学社製の高純度アルミナ「AES-12(平均粒径0.4μm)」(純度99.5%)を17.2重量部、日本化学社製の高純度炭酸バリウム「LSR(平均粒径1.4μm)」を8重量部、信越石英社製の微粒子シリカ「SO-C2(平均粒径0.5μm)」を6重量部、バインダーとして積水化学社製のブチラール樹脂「BLS」を4重量部と積水化学社製の「BL-SZ」を4重量部、可塑剤として「DOP」4重量部、および滑剤としてソルビタンセスキオレートを0.5重量部、を配合し、これにトルエン/エタノール混合溶剤(重量比50/50)を30重量部加えて、ボールミル中で48時間混合することによりスラリーを得た。次いで、離型PETフィルムにスラリーを塗布し、110℃の温度条件にて乾燥した後にフィルムを剥離してグリーンシートを得た。これを任意の形状に打ち抜き、1600℃で2時間焼成することによりアルミナセラミック製基板を作製した。
アルミナとして、ローソーダアルミナ「ALM-42E(平均粒径2.0μm)」(純度99.9%)を60.2重量部および高純度アルミナ「AES-12(平均粒径0.4μm)」(純度99.5%)を25.8重量部用いた他は、実施例2と同様にして、アルミナセラミック製基板を作製した。
アルミナとして、ローソーダアルミナ「ALM-42E(平均粒径2.0μm)」(純度99.9%)を86重量部用いた他は、実施例2と同様にして、アルミナセラミック製基板を作製した。
実施例1および2で作製したアルミナセラミック製枠体およびアルミナセラミック製基板を、上述したX線回折測定方法に従ってX線回折を測定した。その結果を図1および図2に示す。図1および図2から明らかなように、本発明のアルミナセラミックからなる枠体およびセラミック基板は、回折角度(2θ)22.5°の位置にピークが存在し、Ba0.808 Al1.71Si2.29O8 相を含有していることが確認された。また、実施例1および2のアルミナセラミックは、コランダム(Al2 O3 )相による回折角度(2θ)43.3°のピークと、上記回折角度(2θ)22.5°のピークとの強度比がそれぞれ2.0および1.1であった。尚、図4に、ICDDカード番号01-088-1050に記載されている、Ba0.808 Al1.71Si2.29O8 相が示すX線回折パターンを、図5に、ICDDカード番号01-070-7049に記載されている、コランダム(Al2 O3 )相が示すX線回折パターンを、それぞれ示した。
実施例1~4で作製したアルミナセラミック製枠体およびアルミナセラミック製基板を、上述した反射率測定方法に従って反射率を測定した。また、比較例1として北陸セラミック社製のアルミナ基板(アルミナ純度96%)の反射率を測定した。その結果を図3に示す。
Claims (4)
- Ba0.808 Al1.71Si2.29O8 相を含有することを特徴とするアルミナセラミック。
- X線回折において、回折角度(2θ)43.3°におけるピークと回折角度(2θ)22.5°におけるピークとの強度比(前者/後者)が0.5~2.5であることを特徴とする請求項1に記載のアルミナセラミック。
- アルミナセラミック中のBaとSiとのモル比(Ba/Si)が8/1~8/12であることを特徴とする請求項1または2に記載のアルミナセラミック。
- 請求項1~3の何れか一項に記載のアルミナセラミックを用いた発光素子用光反射材料。
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US12/992,386 US8198204B2 (en) | 2008-06-30 | 2009-06-22 | Alumina ceramic |
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WO2012011587A1 (ja) * | 2010-07-23 | 2012-01-26 | 日本カーバイド工業株式会社 | アルミナセラミック、及び、これを用いた発光素子搭載用基板 |
JP2012025623A (ja) * | 2010-07-23 | 2012-02-09 | Nippon Carbide Ind Co Inc | アルミナセラミックの製造法 |
JP2013228603A (ja) * | 2012-04-26 | 2013-11-07 | Kyocera Corp | 反射材およびこの反射材上に発光素子を搭載してなる発光素子モジュール |
WO2015098555A1 (ja) * | 2013-12-26 | 2015-07-02 | 日本カーバイド工業株式会社 | 発光素子搭載用セラミック基板及び発光装置 |
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- 2009-06-22 EP EP09773338.0A patent/EP2292569B1/en not_active Not-in-force
- 2009-06-22 KR KR1020107024235A patent/KR101508296B1/ko active IP Right Grant
- 2009-06-22 US US12/992,386 patent/US8198204B2/en not_active Expired - Fee Related
- 2009-06-22 CN CN200980117425.8A patent/CN102026935B/zh not_active Expired - Fee Related
- 2009-06-22 WO PCT/JP2009/061334 patent/WO2010001760A1/ja active Application Filing
- 2009-06-22 JP JP2010519000A patent/JP5479335B2/ja active Active
- 2009-06-29 TW TW098121906A patent/TWI438170B/zh not_active IP Right Cessation
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Cited By (5)
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JP2011222674A (ja) * | 2010-04-07 | 2011-11-04 | Kyoritsu Elex Co Ltd | 反射板の製造方法 |
WO2012011587A1 (ja) * | 2010-07-23 | 2012-01-26 | 日本カーバイド工業株式会社 | アルミナセラミック、及び、これを用いた発光素子搭載用基板 |
JP2012025623A (ja) * | 2010-07-23 | 2012-02-09 | Nippon Carbide Ind Co Inc | アルミナセラミックの製造法 |
JP2013228603A (ja) * | 2012-04-26 | 2013-11-07 | Kyocera Corp | 反射材およびこの反射材上に発光素子を搭載してなる発光素子モジュール |
WO2015098555A1 (ja) * | 2013-12-26 | 2015-07-02 | 日本カーバイド工業株式会社 | 発光素子搭載用セラミック基板及び発光装置 |
Also Published As
Publication number | Publication date |
---|---|
KR101508296B1 (ko) | 2015-04-06 |
TW201014814A (en) | 2010-04-16 |
EP2292569B1 (en) | 2014-04-16 |
US8198204B2 (en) | 2012-06-12 |
JP5479335B2 (ja) | 2014-04-23 |
TWI438170B (zh) | 2014-05-21 |
EP2292569A4 (en) | 2013-03-06 |
CN102026935B (zh) | 2014-04-02 |
EP2292569A1 (en) | 2011-03-09 |
CN102026935A (zh) | 2011-04-20 |
JPWO2010001760A1 (ja) | 2011-12-15 |
US20110065565A1 (en) | 2011-03-17 |
KR20110033979A (ko) | 2011-04-04 |
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