CN115038774A - 荧光体板和发光装置 - Google Patents
荧光体板和发光装置 Download PDFInfo
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- CN115038774A CN115038774A CN202180012396.XA CN202180012396A CN115038774A CN 115038774 A CN115038774 A CN 115038774A CN 202180012396 A CN202180012396 A CN 202180012396A CN 115038774 A CN115038774 A CN 115038774A
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- phosphor
- phosphor plate
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- sialon
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 169
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000002131 composite material Substances 0.000 claims abstract description 14
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims description 19
- 229910044991 metal oxide Inorganic materials 0.000 claims description 13
- 150000004706 metal oxides Chemical class 0.000 claims description 13
- 239000011029 spinel Substances 0.000 claims description 13
- 229910052596 spinel Inorganic materials 0.000 claims description 13
- 239000004065 semiconductor Substances 0.000 claims description 12
- 150000004767 nitrides Chemical class 0.000 claims description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 238000002834 transmittance Methods 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 229910002483 Cu Ka Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 230000005855 radiation Effects 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 35
- 239000002994 raw material Substances 0.000 description 23
- 238000000034 method Methods 0.000 description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- 239000000203 mixture Substances 0.000 description 12
- 238000005259 measurement Methods 0.000 description 11
- 238000005245 sintering Methods 0.000 description 11
- 239000000758 substrate Substances 0.000 description 11
- 238000010304 firing Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 238000001354 calcination Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 7
- 229910003564 SiAlON Inorganic materials 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
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- 239000006104 solid solution Substances 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- 230000007423 decrease Effects 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
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- 238000012360 testing method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910017488 Cu K Inorganic materials 0.000 description 2
- 229910017541 Cu-K Inorganic materials 0.000 description 2
- 229910007991 Si-N Inorganic materials 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 229910006294 Si—N Inorganic materials 0.000 description 2
- 235000010724 Wisteria floribunda Nutrition 0.000 description 2
- 230000005260 alpha ray Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 238000003705 background correction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
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- 238000000295 emission spectrum Methods 0.000 description 2
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- 239000012535 impurity Substances 0.000 description 2
- 150000007529 inorganic bases Chemical class 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 239000011163 secondary particle Substances 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 238000002490 spark plasma sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910002704 AlGaN Inorganic materials 0.000 description 1
- 229910018509 Al—N Inorganic materials 0.000 description 1
- 229910018516 Al—O Inorganic materials 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 241001272720 Medialuna californiensis Species 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
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- 230000006866 deterioration Effects 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000001748 luminescence spectrum Methods 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-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
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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Abstract
本发明的荧光体板(100)是具有板状的复合体的荧光体板,该板状的复合体包含母材和存在于母材中的α型赛隆荧光体,在使用Cu-Kα射线的X射线衍射分析图案中,在将衍射角2θ为30.2°~30.4°的范围内的与α型赛隆荧光体对应的峰强度设为Iα并将衍射角2θ为26.6°~26.8°的范围内的峰的峰强度设为Iβ时,Iα、Iβ满足0<Iβ/Iα≤10。
Description
技术领域
本发明涉及荧光体板和发光装置。
背景技术
至今为止已经对荧光体板进行了各种开发。作为这种技术,例如已知专利文献1所记载的技术。在专利文献1中记载了在玻璃基体中分散无机荧光体而成的波长转换部件(专利文献1的权利要求1)。根据该文献,记载了波长转换部件的形状没有限定,可以是板状(段落0054)。
现有技术文献
专利文献
专利文献1:日本特开2015-199640号公报
发明内容
然而,本发明人进行了研究,结果发现,在上述专利文献1所记载的板状的波长转换部件中,在发光强度方面存在改善的余地。
本发明人进一步进行了研究,结果发现,在使用α型赛隆(Sialon)荧光体作为上述无机荧光体时,有荧光体板中发光强度降低的风险。基于这样的见解进一步进行了深入研究,结果发现,在荧光体板的X射线衍射分析图案中,将对于α型赛隆荧光体的峰强度与在规定的2θ的范围内存在的峰的峰强度之比(Iβ/Iα)作为指标,从而可以稳定地评价光学特性,通过进一步将指标Iβ/Iα的上限设为规定值以下,改善荧光体板的发光强度,完成了本发明。
根据本发明,提供一种荧光体板,
其为具备板状的复合体的荧光体板,该板状的复合体包含母材和存在于上述母材中的α型赛隆荧光体,
在使用Cu-Kα射线的该荧光体板的X射线衍射分析图案中,在将衍射角2θ为30.2°~30.4°的范围内的与上述α型赛隆荧光体对应的峰强度设为Iα并将衍射角2θ为26.6°~26.8°的范围内的峰的峰强度设为Iβ时,
Iα、Iβ满足0<Iβ/Iα≤10。
另外,根据本发明,提供一种发光装置,具备:
第III族氮化物半导体发光元件、和
设置于上述第III族氮化物半导体发光元件的一面上的上述的荧光体板。
根据本发明,提供发光强度优异的荧光体板和使用它的发光装置。
附图说明
图1是表示本实施方式的荧光体板的构成的一个例子的示意图。
图2(a)是示意性地表示倒装芯片型的发光装置的构成的截面图,(b)是示意性地表示引线接合型的发光元件的构成的截面图。
图3是用于测定荧光体板的发光效率的装置的概略图。
具体实施方式
以下,对本发明的实施方式使用附图进行说明。应予说明,在全部的附图中,对同样的构成要素标以同样的符号,适当省略说明。另外,图是概略图,与实际的尺寸比率不一致。
对本实施方式的荧光体板进行概述。
对本实施方式的荧光体板的概要进行说明。
本实施方式的荧光体板由具备包含母材和存在于母材中的α型赛隆荧光体的板状的复合体的板状部件构成。
荧光体板可以作为将照射的蓝色光转换为橙色光而发光的波长转换体发挥作用。
荧光体板构成为:在按照下述步骤测定的X射线衍射分析图案中,在将衍射角2θ为30.2°~30.4°的范围内的与上述α型赛隆荧光体对应的峰强度设为Iα并将衍射角2θ为26.6°~26.8°的范围内的峰的峰强度设为Iβ时,Iα、Iβ满足0<Iβ/Iα≤10。
(X射线衍射图案的测定方法)
对于荧光体板,基于下述测定条件使用X射线衍射装置测定衍射图案。
测定对象的荧光体板使用厚度约为0.18~0.22mm的荧光体板。
(测定条件)
输出设定:40kV·40mA
测定时光学条件:扩散狭缝=2/3°
散射狭缝=8mm
受光狭缝=开放
衍射峰的位置=2θ(衍射角)
测定范围:2θ=20°~40°
扫描速度:0.5度(2θ)/sec,连续扫描
试样制备:将板状的荧光体板置于样品架。
峰强度是进行背景校正而得到的值。
根据本发明人的见解,可知通过将对于α型赛隆荧光体的峰强度与在规定的2θ的范围内存在的峰的峰强度之比(Iβ/Iα)作为指标,可以评价荧光体板的光学特性,对与Iβ对应的峰的2θ范围进一步进行了研究,结果发现,通过使衍射角2θ为26.6°~26.8°的范围内,可以稳定地评价荧光体板的光学特性。进而,可知通过将这样发现的指标Iβ/Iα设为上述上限值以下,可以提高荧光体板的发光强度。
对于衍射角2θ为26.6°~26.8°的范围内的峰,其来源没有特别限定,但是可以包含与β型赛隆对应的峰,也可以包含与β型赛隆的(200)面对应的峰。
Iβ/Iα的上限可以为10以下,优选为9以下,更优选为8以下。由此,可以提高发光强度。另一方面,Iβ/Iα的下限没有特别限定,但是例如可以超过0,为0.01以上,为0.1以上。由此,可以提高荧光体板的制造稳定性。
在本实施方式中,例如通过适当选择荧光体板中的α型赛隆荧光体中包含的各成分的种类、配合量、α型赛隆荧光体、荧光体板的制备方法等,可以控制上述Iβ/Iα。其中,作为将上述Iβ/Iα设为所期望的数值范围的要素,例如,可以举出降低煅烧温度、缩短高温的煅烧时间等适当调整煅烧条件、适当调整荧光体的粒径等。
根据上述荧光体板,在照射波长455nm的蓝色光的情况下,从荧光体板发出的波长转换光的峰值波长优选为585nm~605nm。另外,由此,通过将荧光体板组合到发出蓝色光的发光元件,能够得到发出亮度高的橙色的发光装置。
对本实施方式的荧光体板的构成进行详细描述。
(母材)
在构成上述荧光体板的复合体中,成为荧光体(α型赛隆荧光体)混合存在于母材(基体相)中的状态。具体而言,混合存在是指在成为基体相的无机母材中分散有α型赛隆荧光体的状态。复合体中的α型赛隆荧光体也可以在粒子状态下均匀分散于无机母材(金属氧化物的烧结物)中。
母材可以由包含Al2O3的烧结物、SiO2的烧结物和尖晶石M2xAl4-4xO6-4x(其中,M为Mg、Mn、Zn中的至少一种,0.2<x<0.6)中的至少一种的金属氧化物的烧结物构成。可以单独使用它们,也可以组合使用2种以上。
由于Al2O3的烧结物对可见光的吸收少,所以可以提高荧光体板的荧光强度。另外,由于Al2O3的烧结物的热传导性高,所以可以提高荧光体板的耐热性。进而,由于Al2O3的烧结物的机械强度也优异,所以可以提高荧光体板的耐久性。
SiO2的烧结物可以由玻璃基体构成。作为玻璃基体,可以使用石英玻璃等。
包含尖晶石的烧结物通常通过将由通式MO(M为Mg、Mn、Zn中的至少一种)表示的金属氧化物的粉末与Al2O3的粉末混合并进行烧结来得到。
在化学计量上,尖晶石是由x=0.5(即通式MAl2O4)表示的组成。但是,根据原料的MO的量与Al2O3的量之比,尖晶石成为MO或Al2O3过度固溶的非化学计量组成的化合物。
包含由上述通式表示的尖晶石的烧结体相对透明。因此,荧光体板内的光的过度散射得到抑制。从透明性的观点出发,上述通式中的M优选为Mg。
(α型赛隆荧光体)
本实施方式的α型赛隆荧光体包含由下述通式(1)表示的含有Eu元素的α型赛隆荧光体。
(M)m(1-x)/p(Eu)mx/2(Si)12-(m+n)(Al)m+n(O)n(N)16-n··通式(1)
上述通式(1)中,M表示选自Li、Mg、Ca、Y和镧系元素(不包括La和Ce)中的1种以上的元素,p表示M元素的价数,0<x<0.5,1.5≤m≤4.0,0≤n≤2.0。n例如可以为2.0以下,可以为1.0以下,也可以为0.8以下。
α型赛隆的固溶组成是将α型氮化硅的晶胞(Si12N16)的m个Si-N键取代为Al-N键,将n个Si-N键取代为Al-O键,为了保持电中性,使m/p个阳离子(M、Eu)渗入固溶于晶格内,如上述通式那样地表示。特别是如果使用Ca作为M,则α型赛隆在宽广的组成范围稳定化,通过用成为发光中心的Eu取代其中一部分,从而激发从紫外到蓝色的宽广的波长范围的光,得到显示从黄色到橙色的可见发光的荧光体。
一般来说,对于α型赛隆,由于与该α型赛隆不同的第二晶相、不可避免地存在的非晶相,所以无法通过组成分析等来严格规定固溶组成。α型赛隆可以包含作为其他晶相的β型赛隆、氮化铝或其多型体、Ca2Si5N8、CaAlSiN3等。
作为α型赛隆荧光体的制造方法,有将由氮化硅、氮化铝和渗入固溶元素的化合物构成的混合粉末在高温的氮气氛中加热并使其反应的方法。在加热工序中构成成分的一部分形成液相,物质在该液相中移动,从而生成α型赛隆固溶体。合成后的α型赛隆荧光体的多个等轴状的一次粒子烧结而形成块状的二次粒子。本实施方式中的一次粒子是指粒子内的结晶方位相同且能够单独存在的最小粒子。
α型赛隆荧光体的平均粒径的下限例如优选为1μm以上,更优选为2μm以上。由此,可以提高发光强度。另外,α型赛隆荧光体的平均粒径的上限优选为30μm以下,更优选为20μm以下。α型赛隆荧光体的平均粒径是上述二次粒子的尺寸。通过使α型赛隆荧光体的平均粒径为5μm以上,可以进一步提高复合体的透明性。另一方面,通过使α型赛隆荧光体的平均粒径为30μm以下,可以在用切粒机等切断加工荧光体板时抑制切屑产生。
这里,α型赛隆荧光体的平均粒径是指,在通过激光衍射散射式粒度分布测定法(Beckman Coulter,Inc.制,LS13-320)进行测定而得到的体积基准粒度分布中,从小粒径侧起的通过量累计(累计通过分率)50%的粒径D50。
相对于复合体整体,α型赛隆荧光体的含量的下限值以体积换算计,例如为5Vol%以上,优选为10Vol%以上,更优选为15Vol%以上。由此,能够提高薄层的荧光体板的发光强度。另外,能够提高荧光体板的光转换效率。另一方面,相对于复合体整体,α型赛隆荧光体的含量的上限值以体积换算计,例如为50Vol%以下,优选为45Vol%以下,更优选为40Vol%以下。能够抑制荧光体板的热传导性的降低。
可以对上述荧光体板的至少主面或主面和背面这两面的表面进行表面处理。作为表面处理,例如,可以举出使用金刚石砂轮等的研削、擦光、抛光等研磨等。
上述荧光体板的主面的表面粗糙度Ra例如为0.1μm~2.0μm,优选为0.3μm~1.5μm。
另一方面,上述荧光体板的背面的表面粗糙度Ra例如为0.1μm~2.0μm,优选为0.3μm~1.5μm。
通过使上述表面粗糙度为上述上限值以下,能够抑制光的取出效率、面内方向的光强度的偏差。通过使上述表面粗糙度为上述下限值以上,从而期待提高与粘附物的密合性。
在上述荧光体板中,450nm的蓝色光的光线透射率的上限值例如为10%以下,优选为5%以下,更优选为1%以下。由此,能够抑制蓝色光透过荧光体板,因此能够发出亮度高的橙色光。通过适当调整α型赛隆荧光体的含量、荧光体板的厚度,能够减少450nm的蓝色光的光线透射率。
应予说明,450nm的蓝色光的光线透射率的下限值没有特别限定,但是例如可以为0.01%以上。
对本实施方式的荧光体板的制造工序进行详细描述。
本实施方式的荧光体板的制造方法可以具有工序(1)和工序(2):工序(1)为得到包含金属氧化物和α型赛隆荧光体的混合物;工序(2)为将得到的混合物进行煅烧。
另外,荧光体板的制造方法也可以将金属氧化物熔融并在得到的熔融物中混合α型赛隆荧光体的粒子。
在工序(1)中,作为原料使用的α型赛隆荧光体、金属氧化物的粉末优选尽量为高纯度,优选除构成元素以外的元素的杂质为0.1%以下。
原料粉末的混合可以应用干式、湿式的各种方法,但是优选尽量不粉碎作为原料使用的α型赛隆荧光体粒子、且混合时尽量不混入来自装置的杂质的方法。
作为原料的金属氧化物,可以使用包含Al2O3粉末、SiO2粉末和尖晶石原料粉末中的至少一种的金属氧化物。可以单独使用它们,也可以组合使用2种以上。
金属氧化物是微粉末即可,其平均粒径例如可以为1μm以下。
作为原料的金属氧化物,可以使用氧化铝粉末(Al2O3)。
氧化铝粉末的BET比表面积的上限例如为10.0m2/g以下,优选为9.0m2/g以下,更优选为8.0m2/g以下,进一步优选为6.0m2/g。由此,能够抑制荧光体板的黑色化。另一方面,氧化铝粉末的BET比表面积的下限例如为0.1m2/g以上,优选为0.5m2/g以上,更优选为1.0m2/g以上,进一步优选为2.0m2/g。由此,能够提高氧化铝粉末的烧结性,形成致密的复合体。
在工序(2)中,将氧化铝粉末与α赛隆荧光体粉末的混合物例如在1300℃~1650℃进行煅烧。烧结工序中的加热温度更优选为1500℃以上。为了使复合体致密化,煅烧温度优选高的温度,但是如果煅烧温度过高,则荧光体和氧化铝发生反应而荧光体板的荧光强度降低,因此优选为上述范围。
另外,在煅烧温度为约1600℃~1650℃的高温区域的情况下,保持该温度的保持时间例如为20分钟以下,优选为15分钟以下,也可以为0分钟。由此,能够提高荧光体板的发光强度。
作为原料的金属氧化物,可以使用玻璃粉末(包含SiO2的粉末)。
作为玻璃粉末,可以使用SiO2粉末(二氧化硅粉末)、一般的玻璃原料。可以单独使用它们,也可以组合使用2种以上。
作为原料的金属氧化物,可以使用尖晶石原料粉末。
这里,“尖晶石原料粉末”例如为(i)包含由上述通式M2xAl4-4xO6-4x表示的尖晶石的粉末和/或(ii)由通式MO(M为Mg、Mn、Zn中的至少一种)表示的金属氧化物的粉末与Al2O3的粉末的混合物。
在工序(2)中,可以将尖晶石原料粉末例如在1300℃~1650℃进行煅烧。烧结工序中的加热温度更优选为1500℃以上。为了使复合体致密化,煅烧温度优选高的温度,但是如果煅烧温度过高,则荧光体板的荧光强度降低,因此优选上述范围。
另外,在煅烧温度为约1600℃~1650℃的高温区域的情况下,保持该温度的保持时间例如为20分钟以下,优选为15分钟以下,也可以为0分钟。由此,能够提高荧光体板的发光强度。
在上述的制造方法中,煅烧方法可以是常压烧结也可以是加压烧结,但是为了抑制α型赛隆荧光体的特性降低且得到致密的复合体,优选比常压烧结更容易致密化的加压烧结。
作为加压烧结方法,可以举出热压烧结、放电等离子体烧结(SPS)、热等静压烧结(HIP)等。在热压烧结、SPS烧结的情况下,压力为10MPa以上,优选为30MPa以上,优选为100MPa以下。
为了防止α赛隆的氧化,煅烧气氛优选为氮、氩等非氧化性的非活性气体或真空气氛下。
由此,得到本实施方式的荧光体板。
也可以在不损害本发明效果的范围内对得到的荧光体板中的板状的复合体的表面实施研磨处理、等离子体处理、表面涂覆处理等公知的表面处理等。
对本实施方式的发光装置进行说明。
本实施方式的发光装置具备第III族氮化物半导体发光元件(发光元件20)和设置于第III族氮化物半导体发光元件的一面上的上述荧光体板10。第III族氮化物半导体发光元件例如是由AlGaN、GaN、InAlGaN系材料等第III族氮化物半导体构成的具备n层、发光层和p层的元件。作为第III族氮化物半导体发光元件,可以使用发蓝色光的蓝色LED。
荧光体板10可以直接配置于发光元件20的一面上,可以介由透光性部件或隔离物来配置。
配置于发光元件20上的荧光体板10可以使用图1所示的圆板形状的荧光体板100(荧光体晶片),可以使用将荧光体板100分片化而得的荧光体板。
图1是表示荧光体板的构成的一个例子的示意图。
图1所示的荧光体板100的厚度根据用途适当地设定。荧光体板100的厚度的下限例如为50μm以上,优选为80μm以上,更优选为100μm以上。荧光体板100的厚度的上限例如为1mm以下,优选为500μm以下,更优选为300μm以下。
荧光体板100的厚度可以在上述制造工序中得到后通过研削等来适当调整。
应予说明,与四边形的情况相比,圆板形状的荧光体板100抑制角部的缺口、破裂的产生,因此耐久性、搬运性优异。
将上述半导体装置的一个例子示于图2(a)、(b)。图2(a)是示意性地表示倒装芯片型的发光装置110的构成的截面图,图2(b)是示意性地表示引线接合型的发光装置120的构成的截面图。
图2(a)的发光装置110具备基板30、介由焊料40(固晶材料(ダイボンド材))而与基板30电连接的发光元件20以及设置于发光元件20的发光面上的荧光体板10。倒装芯片型的发光装置110可以是面朝上型和面朝下型的任意结构。
另外,图2(b)的发光装置120具备基板30、介由接合引线60和电极50而与基板30电连接的发光元件20以及设置于发光元件20的发光面上的荧光体板10。
图2中,用公知的方法粘贴发光元件20与荧光体板10,例如可以用有机硅系粘合剂、热熔接等方法粘合。
另外,发光装置110、发光装置120可以用透明密封材料将整体密封。
应予说明,可以对贴装于基板30的发光元件20粘贴分片化的荧光体板10。可以将多个发光元件20粘贴于大面积的荧光体板100后,通过切割来对每个带荧光体板10的发光元件20进行分片化。另外,可以将大面积的荧光体板100粘贴于在表面形成有多个发光元件20的半导体晶片,然后将半导体晶片和荧光体板100一并进行分片化。
以上,对于本发明的实施方式进行了说明,但是它们是本发明的示例,可以采用除上述以外的各种构成。另外,本发明不限定于上述实施方式,能够实现本发明的目的的范围内的变形、改良等也包含在本发明中。
实施例
以下,参照实施例对本发明详细进行说明,但是本发明不限定于这些实施例的记载。
<荧光体板的制作>
(实施例1)
作为实施例1的荧光体板的原料,使用氧化铝粉末(AA-03(住友化学株式会社制,BET比表面积:5.2m2/g)、Ca-α型赛隆荧光体(平均粒径D50:6.07μm)。
称量氧化铝粉末7.857g,称量Ca-α型赛隆荧光体粉末2.833g,用玛瑙乳钵进行干式混合。将混合后的原料通过网眼75μm的尼龙制网状筛而解开凝集,得到原料混合粉末。应予说明,由原料的真密度(氧化铝:3.97g/cm3,Ca-α型赛隆荧光体:3.34g/cm3)算出的配合比为氧化铝:Ca-α型赛隆荧光体=70:30体积%。
将约11g的原料混合粉末填充于设置有碳制下冲头的内径30mm的碳制模头,设置碳制上冲头,夹入原料粉末。应予说明,为了防止原料混合粉末与碳夹具之间粘结,设置厚度0.127mm的碳片(GraTech公司制,GRAFOIL)。
将填充有该原料混合粉末的热压夹具放于碳加热器的多用途高温炉(富士电波工业株式会社制,HIGHMULTI 5000)。将炉内真空排气至0.1Pa以下,保持减压状态用55MPa的压力加压上下冲头。维持加压状态,以每分钟5℃的速度升温至1600℃。到达1600℃后停止加热,逐渐冷却至室温,进行除压(煅烧工序)。然后,回收外径30mm的煅烧物,使用平面研削盘和圆筒研削盘研削外周部,得到直径25mm、厚度2mm的圆板状的荧光体板。
(实施例2)
在上述煅烧工序中,到达1600℃后在1600℃保持10分钟,然后停止加热,逐渐冷却至室温,进行除压,除此以外,与实施例1同样地进行,得到荧光体板。
(实施例3)
在上述煅烧工序中,升温至1650℃,除此之外,与实施例1同样地进行,得到荧光体板。
(实施例4)
代替实施例1的Ca-α型赛隆荧光体,使用Ca-α型赛隆荧光体(平均粒径D50:3.71μm),除此之外,与实施例1同样地进行,得到荧光体板。
(实施例5)
代替实施例1的氧化铝粉末,使用作为尖晶石原料粉末的氧化铝粉末(Al2O3,住友化学株式会社制,AA-03)5.135g、氧化镁粉末(MgO,富士胶片和光纯药株式会社制,平均粒径0.2μm,纯度99.9%)2.030g,除此之外,与实施例1同样地进行,得到荧光体板。
(比较例1)
在上述煅烧工序中,到达1600℃后在1600℃保持30分钟,然后停止加热,逐渐冷却至室温,进行除压,除此之外,与实施例1同样地进行,得到荧光体板。
(比较例2)
在上述煅烧工序中,升温至1700℃,除此之外,与实施例1同样地进行,得到荧光体板。
对于得到的荧光体板,对以下评价项目进行评价。
[X射线衍射分析图案]
对于各实施例·各比较例的荧光体板,使用X射线衍射装置(产品名:UltimaIV,Rigaku公司制),在下述测定条件下测定衍射图案。
(测定条件)
输出设定:40kV·40mA
测定时光学条件:扩散狭缝=2/3°
散射狭缝=8mm
受光狭缝=开放
衍射峰的位置=2θ(衍射角)
测定范围:2θ=20°~40°
扫描速度:0.5度(2θ)/sec,连续扫描
试样制备:将板状的荧光体板置于样品架。
峰强度是进行背景校正而得到的值。
X射线衍射分析图案的测定的结果确认了,在各实施例·各比较例的荧光体板中,在衍射角2θ为30.2°~30.4°的范围内存在与α型赛隆荧光体(Ca-α-SiAlON的(201)面)对应的峰,在衍射角2θ为26.6°~26.8°的范围内存在与β型赛隆(β-SiAlON的(200)面)对应的峰。测定这些峰强度,将与上述Ca-α-SiAlON对应的峰强度设为Iα,将与上述β-SiAlON对应的峰强度设为Iβ,表1中示出峰强度比(Iβ/Iα)的值。
[光学特性的评价]
对于各实施例·各比较例中得到的荧光体板,通过平面研削盘进一步进行研削,得到具有约0.22mm的板厚度的试验用荧光体板,使用该试验用荧光体板,使用图3的装置,按照以下步骤测定荧光强度。
图3是用于测定试验用荧光体板(荧光体板100)的发光光谱的装置(板上芯片型(COB型)的LED封装体130)的概略图。
对光学特性的评价的步骤进行说明。首先,准备形成有荧光体板100、凹部70的铝基板(基板30)。使凹部70的底面的直径φ为13.5mm,使凹部70的开口部的直径φ为16mm。
接着,在基板30的凹部70的内部安装蓝色LED(发光元件20)作为蓝色发光光源。
接着,以堵住基板30的凹部70的开口部的方式,在蓝色LED的上部设置圆形状的荧光体板100,制作图3所示的装置(板上芯片型(COB型)的LED封装体130)。
然后,使用总光通量测定系统(HalfMoon/φ1000mm积分球系统,大塚电子株式会社制),测定将制作的LED封装体130的蓝色LED点亮时的荧光体板100的表面的发光光谱。
在得到的发光光谱中,求出波长为585nm~605nm的橙色光(Orange)的荧光强度的最大值(W/nm)。表1表示对于荧光强度的最大值,将实施例1设为100%进行规格化时的其他实施例·比较例的相对值(%)。
与比较例1、2相比,实施例1~5的荧光体板显示了荧光强度优异的结果。
本申请基于2020年2月7日提交的日本申请特愿2020-019401号而要求优先权,并将其公开的全部内容纳入本文。
符号说明
10 荧光体板
20 发光元件
30 基板
40 焊料
50 电极
60 接合引线
70 凹部
100 荧光体板
100 发光装置
120 发光装置
130 LED封装体
Claims (9)
1.一种荧光体板,是具备板状的复合体的荧光体板,所述板状的复合体包含母材和存在于所述母材中的α型赛隆荧光体,
在使用Cu-Kα射线的该荧光体板的X射线衍射分析图案中,在将衍射角2θ为30.2°~30.4°的范围内的与所述α型赛隆荧光体对应的峰强度设为Iα,并将衍射角2θ为26.6°~26.8°的范围内的峰的峰强度设为Iβ时,
Iα、Iβ满足0<Iβ/Iα≤10。
2.根据权利要求1所述的荧光体板,其中,
所述母材由包含Al2O3的烧结物、SiO2的烧结物和尖晶石M2xAl4-4xO6-4x中的至少一种的金属氧化物的烧结物构成,且M为Mg、Mn、Zn中的至少一种,0.2<x<0.6。
3.根据权利要求1或2所述的荧光体板,其中,
所述α型赛隆荧光体的含量以体积换算计,在所述母材的体积100Vol%中为5Vol%~50Vol%。
4.根据权利要求1~3中任一项所述的荧光体板,其中,
所述α型赛隆荧光体的平均粒径D50为1μm~30μm。
5.根据权利要求1~4中任一项所述的荧光体板,其中,
该荧光体板的厚度为50μm~1mm。
6.根据权利要求1~5中任一项所述的荧光体板,
其作为将照射的蓝色光转换为橙色光并发光的波长转换体使用。
7.根据权利要求1~6中任一项所述的荧光体板,其中,
455nm的蓝色光的光线透射率为10%以下。
8.根据权利要求1~7中任一项所述的荧光体板,其中,
衍射角2θ为26.6°~26.8°的范围内的峰对应于β型赛隆。
9.一种发光装置,具备:
第III族氮化物半导体发光元件、和
设置于所述第III族氮化物半导体发光元件的一面上的权利要求1~8中任一项所述的荧光体板。
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