CN102026935B - 氧化铝陶瓷 - Google Patents
氧化铝陶瓷 Download PDFInfo
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- CN102026935B CN102026935B CN200980117425.8A CN200980117425A CN102026935B CN 102026935 B CN102026935 B CN 102026935B CN 200980117425 A CN200980117425 A CN 200980117425A CN 102026935 B CN102026935 B CN 102026935B
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- alumina
- ceramic
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- light
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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 60
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 23
- 238000000034 method Methods 0.000 description 18
- 239000000843 powder Substances 0.000 description 17
- 239000002994 raw material Substances 0.000 description 14
- 239000002002 slurry Substances 0.000 description 14
- 239000002245 particle Substances 0.000 description 13
- 238000002310 reflectometry Methods 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- 229910052814 silicon oxide Inorganic materials 0.000 description 11
- 150000001553 barium compounds Chemical class 0.000 description 10
- 239000004840 adhesive resin Substances 0.000 description 9
- 229920006223 adhesive resin Polymers 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- 238000010304 firing Methods 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000005469 granulation Methods 0.000 description 6
- 230000003179 granulation Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 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 5
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 5
- 239000000314 lubricant Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000004902 Softening Agent Substances 0.000 description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
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- 229910052710 silicon Inorganic materials 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 2
- RUFJMLKBWUXJMX-UHFFFAOYSA-N barium;carbonic acid Chemical compound [Ba].OC(O)=O RUFJMLKBWUXJMX-UHFFFAOYSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004939 coking Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- -1 hydrated barta Chemical compound 0.000 description 2
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- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-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
- 238000005270 abrasive blasting Methods 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229940045511 barium chloride Drugs 0.000 description 1
- 229910001626 barium chloride Inorganic materials 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
- 229910001864 baryta Inorganic materials 0.000 description 1
- 230000005250 beta ray Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005259 measurement 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
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007747 plating Methods 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
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明的氧化铝陶瓷含有Ba0.808Al1.71Si2.29O8相。本发明的氧化铝陶瓷具有优异的光反射性能，且作为发光元件用光反射材料是有用的。特别是，含有在X射线衍射中衍射角度(2θ)为43.3°的峰与衍射角度(2θ)为22.5°的峰的强度比为0.5～2.5的范围的Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷显示出优异的光反射性能。另外，本发明的氧化铝陶瓷在波长为300～400nm的光下的反射率特别优异。
Description
技术领域
本发明涉及光反射性优异的氧化铝陶瓷。
背景技术
以往，作为用于收纳高亮度的发光二极管(LED)、半导体激光器(LD)等发光元件的发光元件收纳用封装体(以下也仅称为封装体)，使用陶瓷制的封装体。
以往的陶瓷制的封装体具备搭载发光元件的基体和设置在基体上且具有贯通孔的框体。在基体上设有用于从外部通电的配电导体，发光元件与该配电导体通过接合线而电连接。而且，发光元件经由配电导体和接合线由外部通电而发光，其发出的光被直接释放到外部，或在基体的表面或框体的贯通孔的内周面反射而释放到外部。因此，基体的表面以及框体的贯通孔内周面的形状和组成对发光装置的发光效率有很大的影响。
作为上述发光装置的框体，已知有由反射率高的金属形成的框体。此时，由于由陶瓷形成的基体与由金属形成的框体的热膨胀率不同，有时会因发光元件产生的热而使框体从基体剥离。另外，为了防止这样的剥离，还已知有在陶瓷制的框体上被覆金属镀层的框体(例如参照专利文献1)。作为反射率高的镀材，已知有Ag，此时，在波长为约460nm的光下，相对于硫酸钡的反射率，其具有约90％的反射率。但是，在约460nm以下的波长的光下反射率低，在250nm～800nm的范围内平均反射率为77％。
如上所述，以往的陶瓷制的封装体即使在陶瓷表面被覆金属镀层，也无法得到充分的光反射性能。
专利文献1：日本特开2004-228531号公报
发明内容
本发明是鉴于上述情况而完成的，其目的在于提供无需在陶瓷上被覆金属镀层而光反射性能优异的氧化铝陶瓷。尤其是提供波长为300～400nm的光的反射率优异的氧化铝陶瓷。另外，还提供光反射性能优异的发光元件用光反射材料。
本发明人等为了实现上述目的进行了潜心研究，结果发现：含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷具有优异的光反射性能。特别是，如果以在X射线衍射中衍射角度(2θ)为43.3°的峰与衍射角度(2θ)为22.5°的峰的强度比(前者/后者)为0.5～2.5的范围的方式在氧化铝陶瓷中含有Ba0.808Al1.71Si2.29O8相，能显示出优异的光反射性能。即，在X射线衍射中，刚玉(Al2O3)相的衍射角度(2θ)为43.3°的峰与Ba0.808Al1.71Si2.29O8相的衍射角度(2θ)为22.5°的峰的强度比为0.5～2.5范围的氧化铝陶瓷光反射性能优异。
另外，本发明人等还发现，在含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷中，Ba与Si的摩尔比(Ba/Si)在8/1～8/12的范围内的氧化铝陶瓷在波长为300～400nm的光下的反射率优异。
本发明的含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷具有优异的光反射性能。此外，以在X射线衍射中衍射角度(2θ)为43.3°的峰与衍射角度(2θ)为22.5°的峰的强度比为0.5～2.5的范围内的方式含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷，能显示出特别优异的光反射性能。另外，本发明的氧化铝陶瓷特别是在波长为300～400nm的光下反射率优异。
附图说明
图1是实施例1的本发明的氧化铝陶瓷的X射线衍射图。
图2是实施例2的本发明的氧化铝陶瓷的X射线衍射图。
图3是表示对实施例1～4的本发明的氧化铝陶瓷以及比较例1的以往的氧化铝基板测定各波长的光的反射率而得到的结果的曲线。
图4是ICDD卡号01-088-1050中记载的Ba0.808Al1.71Si2.29O8相所示的X射线衍射图。
图5是ICDD卡号01-070-7049中记载的刚玉(Al2O3)相所示的X射线衍射图。
具体实施方式
本发明的含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷可以通过将含有氧化铝(Al2O3)、氧化硅(SiO2)以及钡化合物的原料烧成来制作。
作为上述氧化铝，优选使用平均粒径5μm以下的氧化铝。考虑到氧化铝陶瓷的光反射性能、可挠性、制造时的烧结性等，特别优选使用平均粒径为0.1～3μm的氧化铝。
另外，在本发明的氧化铝陶瓷的制造时，为了调节上述光反射性能、可挠性、烧结性，可以根据需要混合具有不同平均粒径的多种氧化铝而使用。例如，作为平均粒径不同的2种氧化铝的组合，可以列举平均粒径分别为3μm和0.2μm、3μm和0.3μm、3μm和0.4μm、3μm和0.5μm、3μm和0.6μm、2μm和0.2μm、2μm和0.3μm、2μm和0.4μm、2μm和0.5μm、2μm和0.6μm的组合等，但不限于这些，还可以组合3种以上。当使用平均粒径不同的2种氧化铝时，由大粒径氧化铝/小粒径氧化铝的重量份数得出的配比优选为100/1～60/40。特别是为了得到将不同平均粒径的氧化铝混合后产生的效果，由大粒径氧化铝/小粒径氧化铝的重量份数得出的配比优选为85/15～65/35，更优选为80/20～70/30。
作为在本发明的氧化铝陶瓷的制作中使用的氧化硅，优选使用平均粒径为1μm以下的氧化硅。特别是为了降低氧化铝陶瓷的吸湿性，优选使用平均粒径0.1～0.7μm的氧化硅，更优选平均粒径为0.3～0.6μm的氧化硅。
作为在本发明的氧化铝陶瓷的制作中使用的钡化合物，没有特殊限制，可以列举氢化钡、氟化钡、氢氧化钡、氧化钡、氯化钡、碳酸钡、硫酸钡、硝酸钡等，其中优选氧化钡、碳酸钡，特别优选碳酸钡。上述钡化合物优选使用平均粒径为1.0～2.0μm的钡化合物。
本发明的氧化铝陶瓷的制作中使用的氧化铝(Al2O3)、氧化硅(SiO2)、钡化合物(BaO换算)的重量份数得出的配比优选为(BaO+SiO2)/(Al2O3)＝4/96～24/76的范围。
另外，本发明的氧化铝陶瓷的制作中使用的钡化合物(BaO换算)和氧化硅(SiO2)的重量份数得出的配比优选为BaO/SiO2＝8/1～8/12。
此外，为了制作波长为300～400nm的光的反射率优异的氧化铝陶瓷，优选以原料烧结后的氧化铝陶瓷中的Ba和Si的摩尔比(Ba/Si)为8/1～8/12的方式配合钡化合物和氧化硅，更优选使上述摩尔比为8/3～8/12。
本发明的氧化铝陶瓷的制造方法没有特殊限制，可以使用周知的方法。例如可以采用生片法(green sheet method)来制作：在上述含有氧化铝、氧化硅、钡化合物的原料中添加混合适当的粘合剂、溶剂等制成浆料状，将其用刮刀法或压辊法等制成生片，然后在高温(1400℃～1600℃)下烧成。另外，还可以采用粉体成型法来制作：将原料粉体填充到成型机中压密成型后，将成型体烧成。在得到板状的陶瓷烧结体时，优选采用生片法来制造。
以下，对本发明的含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷的采用粉体成型法的制造方法的一个例子进行说明。
首先，将氧化铝、氧化硅、钡化合物分别粉碎成规定的尺寸来制作原料粉末后，将这些原料粉末按上述配比称量，在其中加入粘合剂树脂、润滑剂以及溶剂并混合，得到浆料。上述原料的粉碎和原料粉末等的混合可以采用例如球磨机。另外，粉碎工序可以适当省略。
作为上述粘合剂树脂，例如可以使用丙烯酸类、PVA(聚乙烯醇)类等粘合剂树脂。另外，浆料中的粘合剂树脂相对于固体成分的含量优选为0.5质量％～5.0质量％，更优选为1.5质量％～3.5质量％。若浆料的固体成分中的粘合剂树脂的量多，则在原料粉末的造粒时粒子变硬，容易产生疏密。另外，若粘合剂树脂的量少，则粉末成型品的强度变弱。
作为上述润滑剂，例如可以使用硬脂酸乳液，浆料中的润滑剂相对于固体成分的含量优选为0.05质量％～0.5质量％，更优选为0.1质量％～0.3质量％。
作为上述溶剂，例如可以使用水。溶剂的用量优选为20～80质量％，更优选为40～60质量％。
接着，将浆料干燥，将原料粉末的粒子造粒成适合用粉末成型机成型的尺寸。粒子的造粒例如可以使用喷雾干燥机。造粒得到的粒径优选为25μm～200μm，更优选为30μm～150μm。经造粒处理后的粉末使用筛子等进行分级。若粉末成型时粒子过大，则向模具中的填充性下降；若粒子过小，则粒子进入模具的间隙，容易产生毛边。
接着，将造粒后的原料粉末填充到模具中，在常温下加压成型。此时，施加于粉末的压力优选为0.5t/cm2～2.0t/cm2，更优选为0.7t/cm2～1.5t/cm2。
将由上述成型得到的成型体用烧成炉烧成。烧成的温度条件优选为1400℃～1600℃。关于烧成，适当选择适于制作含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷的升温至烧成温度的升温速度、烧成时间、从烧成温度冷却的冷却速度等来进行。举一例子，将上述成型体首先在600℃下保持8小时，接着花8小时升温至1600℃，在此条件下保持2小时后，花6小时放冷。烧成后，根据需要使用滚筒研磨机等进行研磨以除去毛边等。
如此操作即可制作本发明的含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷。
另外，对本发明的含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷的采用生片法的制造方法的一个例子进行说明。
将氧化铝、氧化硅、钡化合物分别粉碎成规定的尺寸制作原料粉末后，将这些原料粉末按上述配比称量，在其中加入溶剂、粘合剂树脂、分散剂、增塑剂等并混炼，由此得到浆料。上述原料的粉碎和原料粉末等的混炼可以采用例如球磨机。
作为上述粘合剂树脂，例如可以使用丙烯酸类、PVB(聚乙烯醇缩丁醛)类等粘合剂。另外，浆料中的粘合剂树脂相对于固体成分的含量优选为4.0质量％～20质量％，更优选为6.0质量％～8.0质量％。
作为上述分散剂，可以使用各种表面活性剂，浆料中的分散剂相对于固体成分的含量优选为0.1质量％～1.0质量％，更优选为0.3质量％～0.5质量％。
作为上述增塑剂，例如可以使用DOP(邻苯二甲酸二辛酯，DioctylPhthalate)、DBP(邻苯二甲酸二丁酯，Dibutyl Phthalate)等，浆料中的增塑剂相对于固体成分的含量优选为3.0质量％～15质量％，更优选为4.0质量％～6.0质量％。
作为上述溶剂，例如可以使用醇或甲苯等，关于溶剂的用量，优选使浆料的固体成分的总量为70质量％～80质量％。另外，浆料的粘度优选为3000cps～30000cps，更优选为10000cps～20000cps。
接着，将得到的浆料注入涂布了脱模剂的薄膜上，通过干燥使溶剂蒸发。此时，作为干燥温度，优选为80℃～130℃，更优选为100℃～120℃。另外，干燥速度优选为0.2m/min～2.0m/min。
之后，将薄膜剥离，即生成生片。将该生片用加压成型机冲压成所需的形状，在烧成炉中烧成。此时，烧成温度优选为1400℃～1600℃。关于烧成，适当选择适于制作含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷的升温至烧成温度的升温速度、烧成时间、从烧成温度冷却的冷却速度等来进行。举一例子，首先在600℃下保持8小时，接着花8小时升温至1600℃，在此条件下保持2小时后，花6小时放冷。烧成后，可以根据需要使用喷砂研磨机等进行研磨。
如此操作即可制作本发明的含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷。
关于本发明的氧化铝陶瓷中的Ba0.808Al1.71Si2.29O8相的存在，可以通过用下述[X射线衍射测定方法]测定X射线衍射来确认。另外，本发明的氧化铝陶瓷的光反射性能由下述[反射率测定方法]来评价。
[X射线衍射测定方法]
关于X射线衍射，使用Spectris公司制X射线衍射装置X’pert PRO，根据JIS1481的石棉定性分析条件来测定。测定条件如下所述。测定结果与ICDD(国际衍射数据中心，International Centre for Diffraction Data)的参考数据比较，确认Ba0.808Al1.71Si2.29O8相的存在。
测定条件
X射线对阴极 Cu
管电压(kV) 40
管电流(mA) 40
扫描速度 0.02°×10秒
单色化(Kβ射线的除去) Ni滤片
扫描范围(°、2θ) 5～80
发散狭缝(°) 1
[反射率测定方法]
反射率使用日立制作所制分光光度计U-4000来测定。根据JIS K7105，求出镜面反射和扩散反射之和的波长依存性。作为标准白板，使用氧化铝，将该标准白板的反射率设为100％，用相对值来评价各材料的反射率。
本发明的含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷可以用作发光元件搭载用的基板或使从发光元件发出的光反射的框体等发光元件用反射材料。
实施例
以下，基于实施例，对本发明的含有Ba0.808Al1.71Si2.29O8相的氧化铝陶瓷的制作方法进行说明，但本发明不限于这些实施例。
[实施例1]
将住友化学公司制的高纯度氧化铝“AES-12(平均粒径0.4μm)”(纯度99.5％)89重量份、日本化学公司制的高纯度碳酸钡“LSR(平均粒径1.4μm)”8重量份、信越石英公司制的微粒氧化硅“SO-C2(平均粒径0.5μm)”3重量份、大日本油墨公司制的粘合剂“NCB-156”3重量份、以及中京油脂公司制的润滑剂“Cellosol 920”0.1重量份配合并加入水，通过在球磨机中混合得到浆料。接着，在110℃的温度条件下干燥、造粒，使用孔径为25μm和150μm的筛子，除去微细粒子和粗大粒子。
将该造粒物填充到框体用的模具中，使用三研精机公司制的10t压力机，在室温下施加1t/cm2的压力来成型，得到框体形状物。然后，将该框体形状物在1550℃下烧成2小时，制作了氧化铝陶瓷制框体。
[实施例2]
将住友化学公司制的低钠氧化铝“ALM-42E(平均粒径2.0μm)”(纯度99.9％)68.8重量份、住友化学公司制的高纯度氧化铝“AES-12(平均粒径0.4μm)”(纯度99.5％)17.2重量份、日本化学公司制的高纯度碳酸钡“LSR(平均粒径1.4μm)”8重量份、信越石英公司制的微粒氧化硅“SO-C2(平均粒径0.5μm)”6重量份、作为粘合剂的积水化学公司制的缩丁醛树脂“BLS”4重量份和积水化学公司制的“BL-SZ”4重量份、作为增塑剂的“DOP”4重量份、以及作为润滑剂的山梨坦倍半油酸酯0.5重量份配合，在其中加入甲苯/乙醇混合溶剂(重量比50/50)30重量份，在球磨机中混合48小时，由此得到浆料。接着，在脱膜PET薄膜上涂布浆料，在110℃的温度条件下干燥后，将薄膜剥离，得到生片。将其冲压成任意的形状，在1600℃下烧成2小时，由此制作了氧化铝陶瓷制基板。
[实施例3]
作为氧化铝，使用低钠氧化铝“ALM-42E(平均粒径2.0μm)”(纯度99.9％)60.2重量份以及高纯度氧化铝“AES-12(平均粒径0.4μm)”(纯度99.5％)25.8重量份，除此以外均与实施例2同样操作，制作了氧化铝陶瓷制基板。
[实施例4]
作为氧化铝，使用低钠氧化铝“ALM-42E(平均粒径2.0μm)”(纯度99.9％)86重量份，除此以外均与实施例2同样操作，制作了氧化铝陶瓷制基板。
[X射线衍射的测定]
按照上述X射线衍射测定方法，对实施例1和实施例2中制作的氧化铝陶瓷制框体以及氧化铝陶瓷制基板进行X射线衍射测定。其结果示于图1和图2。图1和图2表明，由本发明的氧化铝陶瓷形成的框体和陶瓷基板在衍射角度(2θ)为22.5°的位置存在峰，证实含有Ba0.808Al1.71Si2.29O8相。另外，实施例1和实施例2的氧化铝陶瓷的刚玉(Al2O3)相产生的衍射角度(2θ)为43.3°的峰与上述衍射角度(2θ)为22.5°的峰的强度之比分别为2.0和1.1。另外，图4表示ICDD卡号01-088-1050中记载的Ba0.808Al1.71Si2.29O8相所示的X射线衍射图，图5表示ICDD卡号01-070-7049中记载的刚玉(Al2O3)相所示的X射线衍射图。
[反射率的测定]
按照上述反射率测定方法对实施例1～4中制作的氧化铝陶瓷制框体和氧化铝陶瓷制基板进行反射率测定。另外，测定了作为比较例1的北陆陶瓷公司制的氧化铝基板(氧化铝纯度96％)的反射率。其结果示于图3。
Claims (2)
1.一种发光元件用光反射材料，其是使用了氧化铝陶瓷的发光元件用光反射材料，其特征在于，所述氧化铝陶瓷含有Ba0.808Al1.71Si2.29O8相，
在X射线衍射中，衍射角度2θ为43.3°的峰与衍射角度2θ为22.5°的峰的强度比即前者/后者为0.5～2.5。
2.如权利要求1所述的发光元件用光反射材料，其特征在于，氧化铝陶瓷中的Ba与Si的摩尔比即Ba/Si为8/1～8/12。
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| JP5478404B2 (ja) * | 2010-07-23 | 2014-04-23 | 日本カーバイド工業株式会社 | アルミナセラミックの製造法 |
| JP2013211282A (ja) * | 2010-07-23 | 2013-10-10 | Nippon Carbide Ind Co Inc | 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 |
| 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 |
| JP2017037868A (ja) * | 2013-12-26 | 2017-02-16 | 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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| WO2007058361A1 (ja) * | 2005-11-21 | 2007-05-24 | Nippon Carbide Industries Co., Inc. | 光反射用材料、発光素子収納用パッケージ、発光装置及び発光素子収納用パッケージの製造方法 |
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| TW201014814A (en) | 2010-04-16 |
| TWI438170B (zh) | 2014-05-21 |
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| JP5479335B2 (ja) | 2014-04-23 |
| EP2292569A4 (en) | 2013-03-06 |
| EP2292569B1 (en) | 2014-04-16 |
| KR20110033979A (ko) | 2011-04-04 |
| KR101508296B1 (ko) | 2015-04-06 |
| CN102026935A (zh) | 2011-04-20 |
| WO2010001760A1 (ja) | 2010-01-07 |
| EP2292569A1 (en) | 2011-03-09 |
| US8198204B2 (en) | 2012-06-12 |
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