CN102282235B - 无机发光材料组合物 - Google Patents
无机发光材料组合物 Download PDFInfo
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- CN102282235B CN102282235B CN200980154727.2A CN200980154727A CN102282235B CN 102282235 B CN102282235 B CN 102282235B CN 200980154727 A CN200980154727 A CN 200980154727A CN 102282235 B CN102282235 B CN 102282235B
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- 239000000203 mixture Substances 0.000 title claims abstract description 107
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 238000000034 method Methods 0.000 claims abstract description 22
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 16
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 239000003870 refractory metal Substances 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 31
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- 229910052721 tungsten Inorganic materials 0.000 claims description 11
- 239000010937 tungsten Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 239000011733 molybdenum Substances 0.000 claims description 6
- 150000004767 nitrides Chemical class 0.000 abstract description 37
- 238000001429 visible spectrum Methods 0.000 abstract description 20
- 229910052712 strontium Inorganic materials 0.000 abstract description 17
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 abstract description 16
- 239000011575 calcium Substances 0.000 abstract description 15
- 229910052791 calcium Inorganic materials 0.000 abstract description 11
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 abstract description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 9
- 238000010304 firing Methods 0.000 abstract 1
- 239000007858 starting material Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 21
- 239000001257 hydrogen Substances 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 239000004411 aluminium Substances 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- 125000002091 cationic group Chemical group 0.000 description 7
- 238000005286 illumination Methods 0.000 description 7
- 239000012190 activator Substances 0.000 description 6
- 239000008246 gaseous mixture Substances 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- -1 calcium nitride Chemical class 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 3
- 229910052794 bromium Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 229910052688 Gadolinium Inorganic materials 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- 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 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 229910052765 Lutetium Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- XWOQSMOSNCMPSH-UHFFFAOYSA-N [Sm+2] Chemical compound [Sm+2] XWOQSMOSNCMPSH-UHFFFAOYSA-N 0.000 description 2
- GPBUGPUPKAGMDK-UHFFFAOYSA-N azanylidynemolybdenum Chemical compound [Mo]#N GPBUGPUPKAGMDK-UHFFFAOYSA-N 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 229910052792 caesium Inorganic materials 0.000 description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- XQTIWNLDFPPCIU-UHFFFAOYSA-N cerium(3+) Chemical compound [Ce+3] XQTIWNLDFPPCIU-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052701 rubidium Inorganic materials 0.000 description 2
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 2
- 229910052706 scandium Inorganic materials 0.000 description 2
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 229910017083 AlN Inorganic materials 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
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Abstract
公开了一种用于形成共混的无机发光材料组合物的方法。该方法包括步骤：在难熔金属坩埚中，将包括铕和至少钙、锶和铝的氮化物的前体组合物在气体存在下进行火烧，所述气体阻止在氮化物起始材料与形成坩埚的难熔金属之间形成氮化物组分。所形成的组合物可以包括无机发光材料，该无机发光材料将可见光谱蓝光部分的频率转换成可见光谱红光部分的频率。
Description
发明背景
本申请涉及无机发光材料(phosphor)。具体的，本申请涉及氮化物无机发光材料，其能够将来自发光二极管的蓝光光子转换成处于可见光谱的红光部分中的频率。这样的红色色调的产生有助于调节由LED灯所产生的颜色，并且具体的，红光光子有助于温暖由LED灯产生的白光。
照明是以多种不同的方式来进行的。白炽照明使用钨灯丝的发射来生产特有的光。荧光照明使用紫外光源(汞发射)来照射发冷光材料，其由荧光灯来产生白光发射。卤素照明也使用钨灯丝，但是包括痕量的卤素气体(典型的是碘或者溴)，其有助于在运行中再生钨灯丝，这依次提高了灯的寿命。当电流沿着p-n节(或者它的等价物)导向时，固态灯发射光子。
每种相关的照明形式具有相应的优缺点。白炽照明典型的产生更温暖的颜色，并且灯泡和固定物是低成本广泛能够获得的。但是，从能量效率的观点来说，白炽灯泡倾向于将它们大部分的能量作为热而非光来产生。确实的，未来的管理方案会使得大部分普通的白炽灯泡的应用变得最小。
荧光照明倾向于比白炽照明的能量效率更高，但是其需要启动电路和相关的硬件。结果，仅仅到最近才开发了能够用于白炽固定物中的成本有效的荧光照明。荧光灯泡典型的还包含汞，即使处于最小量。固态照明的优点是长寿命、更高的能量效率和潜在的更低的成本，但是历史上具有低亮度和(如其他地方所示的)能够产生白光的相关颜色的不可利用性。
更最近的，由于处于竞争性价格的基于能够产生白光的发光二极管的灯的提高的可用性，固态照明已经变成市售的。虽然固态装置(发光二极管)几十年来已经被用于指示器的目的，但是两种因素限制或者阻止了将发光二极管用作照明的基础：缺少能够产生白光所需频率的二极管；和一旦这样的二极管投入使用，它们通常是低亮度的。
所属领域的技术进步已经减少了这些(和其他的)对于固态照明的障碍。首先，在过去十年内蓝光发光二极管已经以竞争性价格用于商业规模使用。蓝光发光二极管是白光的必需部件，因为(如下面所解释的)蓝光光子是构成三色灯或者激励适当的无机发光材料所必需的。
作为第二个进步，能够利用的LED灯的亮度持续提高。
因为白光是可见光谱中许多频率的组合，因此它可以由蓝光，绿光和红光主光源来产生。因此，发射白光的灯可以由一种或多种红光发光二极管、一种或多种绿光发光二极管和一种或多种蓝光发光二极管来生产。但是，这种技术会是相当复杂的，这归因于所需的二极管数目。
在最近的使用发光二极管源的发射白光的灯的开发中，大部分普通方法已经引入到发光二极管中，该二极管发射电磁光谱的蓝光、紫光或者紫外光部分。这样的二极管然后与无机发光材料进行合并，通常合并到包括透镜的包装中，所述的无机发光材料吸收蓝光(紫光，UV)发射，并且相应的产生黄光发射。来自二极管的蓝光与来自该无机发光材料的黄光相组合产生了白光。
作为本领域公知的，无机发光材料是这样的组合物，其通常吸收光的给定频率或者频率范围，然后发射不同颜色的光子，通常是低频率的，并且通常包括频率范围。
典型的无机发光材料是一种固体组合物，其在主结构中包括(活化剂)离子。因为产生蓝光的发光二极管在商业上是新近才出现的(大约十年)，因此使用蓝光发光二极管与黄色无机发光材料相组合来生产白光也是新近才出现的。
但是，不同的白色光源对于人眼具有轻微不同的外观。它们有时候是使用称作色温的公认测量来量化的。当叙述性提到时，色彩中带有更多蓝色的白光被称作是较冷的，而具有更多的黄色或者红色成分的光通常被称作是较温暖的。取决于所期望的最终用途，较冷的灯在某些情况中是优选的，而较温暖的白色在另外的情况中是优选的。作为一个例子，皮肤的颜色倾向于在较温暖的灯下比在较冷的灯下看起来更自然。
通常，白炽照明比荧光照明更温暖；虽然较温暖的荧光灯也是能够获得的。在任何情况中，如果LED照明成功的替代白炽和荧光照明(因为除了它的能量优点之外的原因)，则期望的这样的二极管灯，其将发射红色或者黄色成分来产生更温暖的外观。
因为蓝光发光二极管是新近才出现的，因此在LED灯的情形中，对于能够将蓝光光子转换成红光发射的无机发光材料的需求或者商业渴求也是新近才出现的。国际申请号WO2005052087(并且还作为US20070007494而公开)中提出了一种用于这样的无机发光材料的主要来源。该公开文献描述了一种氮化物基无机发光材料，新近才出现它的商业应用。该无机发光材料组合物是由与水或者空气高反应性的材料形成的，并且因此不使用复杂的装置时，是相当难以生产的。
在大部分典型的LED应用中，无机发光材料必须具有颜色稳定性；即，它的化学组成随着时间的变化必须足够一致，以使得通过灯所发射的光的颜色保持一致。换句话说，如果该无机发光材料的化学组成破坏的相对快，则通过二极管灯所产生的颜色将快速变化，并且通常是以不期望的方式变化的。
'087公开中所述的无机发光材料还是昂贵的，仅仅能够从有限的来源获得，并且因为制造困难，有时候是难以获得的。例如，氮化硅(其是典型的起始材料之一)甚至在高温时也是相对惰性的。确实的，因为它的高温稳定性，氮化硅典型的被用于半导体组分的钝化。此外，存在于其他起始材料中的碱土金属与氧气和湿气是快速反应的(经常过快反应)。
因此，存在着对于改进的方法和所形成的无机发光材料组合物的需要，其当用蓝光光子激励时将产生红光发射，它们的组成和颜色输出是稳定的，并且其比目前能够获得的具有这种特性的无机发光材料更容易制造。
发明内容
在一方面，本发明是一种制造无机发光材料组合物的方法，该组合物将可见光谱的蓝光和紫外光部分的光子向下转换(down-convert)成可见光谱更长波长部分的光子。该方法包括混合下面的物质：含有选自钙、锶、锂、钠、钾、铷、铯、镁、钡、钪、钇、镧、钆和镥的阳离子的组合物；和含有选自铝、硅、硼、镓、碳、锗、和磷的阳离子的组合物；和选自氮、硫、氯、溴和碘的阴离子。该组合物还混合有选自铕(II)、铈(III)、镱(II)、钐(II)和锰(II)的活化剂。该混合物是在处于或者接近于大气压的组成气体(forming gas)的存在下，在难熔坩埚中加热的，该坩埚在组成气体混合物存在下是基本上惰性的。该加热的温度足以产生该无机发光材料，但是低于该前体组合物或者该无机发光材料分解或者与坩埚反应的温度，并且所述的反应进行了足够的时间，来生产无机发光材料，该发光材料将可见光谱的紫外光和蓝光部分的光子向下转换成可见光谱的更长波长部分的光子。
在另一方面，本发明是一种制造无机发光材料组合物的方法，其包括：将选自钙的氮化物和锶的氮化物的氮化物和选自铝的氮化物和硅的氮化物的氮化物与铕源组合物在基本上不存在水和氧的情况下进行混合。该混合物是在大约大气压下，在难熔坩埚(其在组成气体混合物存在下是基本上惰性的)中，在组成气体(其是氢和氮的混合物)存在下进行加热的。该加热的温度足以产生该无机发光材料，但是低于该前体组合物或者该无机发光材料分解或者与坩埚反应的温度，并且所述的反应进行了足够的时间，来生产无机发光材料组合物，该发光材料将光谱的蓝光和紫外光区的光子向下转换成可见光谱的更长波长区的光子。
在另一方面，本发明是一种制造无机发光材料组合物的方法，该组合物吸收了可见光谱的蓝光部分，并且发射了可见光谱的红光部分。该方法包括步骤：在基本上不存在水和氧的情况下混合钙的氮化物、锶的氮化物、铝的氮化物和硅的氮化物与氟化铕，在大约大气压下和在难熔坩埚(其在组成气体混合物存在下是基本惰性的)中，在组成气体存在下加热该混合物，该组成气体是大约5%氢和95%氮的混合物，该加热的温度足以产生该无机发光材料，但是低于该前体组合物或者该无机发光材料分解或者与坩埚明显反应的温度，并且该加热的时间足以产生这样的无机发光材料组合物，该无机发光材料组合物的名义组成是Ca1-x-ySrxEuyAlSiN3，并且混合有至少1%量的氧氮化硅铝。
在另一方面，本发明包括在难熔金属坩埚中和在气体存在下，火烧(fire)包括铕和至少钙、锶和铝的氮化物的前体组合物，所述气体阻止在氮化物起始材料和形成坩埚的难熔金属之间形成氮化物组分。
在另一方面，本发明是一种无机发光材料组合物，其将可见光谱的蓝光部分的频率转换成可见光谱红光部分的频率。该无机发光材料组合物包含Ca1-x-ySrxEuyAlSiN3(优选其中0 < x <1和0 < y <1)，并且组合有至少1重量%量的氧氮化硅铝。
基于随后的详细说明，并且结合附图，本发明的前述和其他目标和优点以及其实现方式将变得更清楚。
附图说明：
图1是对于本发明的无机发光材料组合物来说，相对于波长(单位纳米(nm))所绘制的无机发光材料发射的相对强度的图。
图2A绘制了相对于本发明无机发光材料中的锶的原子分数，所述发射的相对亮度的可变性的图，图2B绘制了所述发射的相对颜色的图。
图3和4是这样的图，其表示了市售的无机发光材料和本发明的无机发光材料的亮度和颜色的变化。
图5是本发明反应容器的内部的顶透视图。
图6是本发明反应排列的透视图。
图7是图5和6所示的反应容器的横截面图。
图8是本发明无机发光材料组合物的x射线粉末衍射图。
具体实施方式
在一个宽的方面，本发明是一种制造无机发光材料组合物的方法，该组合物将光子向下转换成可见光谱更长波长部分的光子。该方法包括混合下面的物质：含有选自钙、锶、锂、钠、钾、铷、铯、镁、钡、钪、钇、镧、钆和镥的阳离子的组合物，和含有选自铝、硅、硼、镓、碳、锗、和磷的阳离子的组合物，和选自氮、硫、氯、溴和碘的阴离子。
作为此处使用的，措词“含有阳离子的组合物”指的是这样的组合物，其在反应条件下将在所形成的无机发光材料组合物中产生作为阳离子的元素。该元素不是必需作为阳离子存在于源材料中。
该组合物还混合有选自下面的活化剂：铕(II)，铈(III)，镱(II)，钐(II)和锰(II)。作为在阳离子的情况中，该活化剂可以以任何的这样的组合物的形式加入，该组合物在所形成的无机发光材料的晶格中产生了期望的活化剂原子(典型的是离子)，并且不会以不期望的方式干涉加工步骤或者其他起始组合物。
该混合物是在组成气体存在下，并且(在大部分实施方案中)是在基本上不存在水和氧的情况下，在大约大气压和难熔坩埚中进行加热的。在大部分的实施方案中，该坩埚在该组成气体混合物存在下是基本惰性的。该加热的温度足以产生该无机发光材料，但是低于该前体组合物或者该无机发光材料分解或者与坩埚反应的温度，并且该反应进行的时间足以产生无机发光材料，该发光材料将可见光谱的紫外光和蓝光部分的光子向下转换成在可见光谱的更长波长部分的光子。
在另一方面，本发明是一种制造氮化物无机发光材料组合物的方法，其包括：在基本上不存在水和氧的情况下，将选自钙的氮化物和锶的氮化物的氮化物与选自铝的氮化物和硅的氮化物的氮化物以及铕源组合物进行混合。
术语“氮化物无机发光材料”在此用于描述无机发光材料，对其来说，阳离子主要是氮化物，并且在其中晶体结构中所存在的任何氧的量是如此的小，以至于避免了改变主要由该氮化物所形成的晶体结构。换句话说，此处所述的无机发光材料不是“氧氮化物”无机发光材料。
本领域技术人员认可这里没有明确的界限或者准确的边界，来定义将该组合物归类为氧氮化物，而非氮化物的氧的存在量，但是一般来说，在氮化物无机发光材料中，仅仅存在非常少量的氧；例如与氮的存在量相比，小于百分之五(5%)。
作为此处使用的，措词“铕源组合物”指的是这样的组合物，其在此处所述的反应条件下，将在无机发光材料的晶格中产生作为活化剂阳离子的铕。作为此处和其他地方所述的，氟化铕是示例性的。
该混合物是在氢和氮混合物组成气体存在下，在大约大气压和在难熔坩埚(其在该组成气体混合物存在下是基本惰性的)中进行加热的。该加热的温度足以产生该无机发光材料，但是低于该前体组合物或者该无机发光材料分解或者与坩埚反应的温度，并且该反应进行的时间足以产生无机发光材料组合物，该无忌发光材料组合物将光谱的蓝光和紫外光区的光子向下转换成在可见光谱的更长波长区的光子。
在一个示例性方面，本发明是一种制造无机发光材料组合物的方法，该组合物吸收了可见光谱的蓝光部分(即，大约430-480nm)，并且在可见光谱的红光部分(即，大约530-750nm)或者朝着该部分进行发射。本领域技术人员当然认可该可见光谱的颜色边界是用于说明性的，而非限制性含义。
此处所述的关于组合物合成和它的性能测量(例如，x射线粉末衍射)的全部技术通常是本领域公知的，并且可以由本领域技术人员无需过度试验就能够进行。因此，这样公知的技术是不必赘述的。
在这种实施方案中，所述方法包括在基本上不存在水和氧的情况下，混合钙的氮化物，锶的氮化物，铝的氮化物和硅的氮化物与氟化铕。将这种混合物在组成气体存在下加热。该加热步骤是在难熔坩埚(典型的金属)中进行的，该坩埚更详细的参考图5-7来描述，并且其在组成气体存在下是基本惰性的。该加热步骤在足够高的温度进行，来以合理的速度生产该组合物，但是其低于前体或者产物组合物分解的温度或者该组合物和坩埚彼此明显反应的温度。
最典型的，该加热步骤是在大约1500℃-1800℃的温度进行了这样的时间，该时间足以生产名义组成Ca1-x-ySrxEuyAlSiN3，并且混合有至少1重量%量的氧氮化硅铝(典型的Si2Al4O4N4)的无机发光材料组合物。在典型的实施方案中，X是大约0.5-0.7，Y是大约0.013-0.017。
在这些条件下，该无机发光材料可以在处于或者接近于环境(即，大气)压力时合成，因此通过避免对于高压技术和装置的需要，而提供了明显的工艺优势。
在本发明的方法中，措词“处于或者接近于大气压”目的并非将该反应精确的限定到一个大气压，而是代替的用于描述这样一种反应方案，在其中高压(或者任何的加压过的或者正在加压的)装置不是必需的。虽然本发明的方法可以在大气压进行，但是它不限于大气压。因此，如果期望，该反应可以在更高的高压进行。但是，在许多情况中，在大气压时生产该无机发光材料的能力是有利的，因为它简化了工艺步骤和所必需的装置二者。
术语“组成气体”是以它公知的含义来使用的；即，氮和氢的混合物，其用于多种应用中，在这里氢的存在是有利的，并且在其中氮的存在有利于降低或者消除燃烧的可能性。组成气体通常具有高的氮含量和小的氢含量，并且典型的氢量是大约5-10%。在许多情况中，95%氮和5%氢的混合物是市售的，因此从实践的观点来说是有利的。
虽然申请人不希望受限于任何具体的理论，但是迄今已经观察到在本发明的反应条件下，纯氮(即，99.9%或者更高的纯度)不形成合适的氮化物无机发光材料。该组成气体还有助于将铕保持在(II)氧化态，而非(III)氧化态。该组成气体还有助于防止氮以直接类似于氧化的方式来与坩埚反应。在这些条件下，虽然申请人不希望受限于任何具体理论，但是所形成的1%的氧氮化硅铝可以获取起始材料中存在的大部分或者全部的任何的氧。
在另一方面，本发明包含了根据所述方法形成的无机发光材料组合物。
在一种示例性实施方案中，钙氮化物起始材料典型的是(Ca3N2)，锶氮化物典型的是(Sr2N)，铝氮化物是化学计量的(AlN)，和硅氮化物典型的同样是化学计量的(Si3N4)。
难熔坩埚在组成气体混合物存在下是基本惰性的。本领域技术人员将认可在不适当的或者不太适当的坩埚材料中合成无机发光材料会降低无机发光材料的光学性能。这样的降解通常是由坩埚材料和反应物之间的一些反应而形成的。例如，当氧化铝坩埚用于类似于此处所述的这些的反应中时，来自坩埚的氧倾向于混入到所形成的无机发光材料粉末中，其依次显示出差的发光品质。将组成气体与氮化硼坩埚一起使用倾向于生产比优选的实施方案更差的结果。
在本发明中，已经确定钨(W)和钼(Mo)的坩埚是有利的。钨和钼是难熔金属，它们能够经受高温，并且在相应的气氛下是惰性的。与该方法相反，钨和钼在'494公开文献(100%氮)中所述的'494火烧条件中是不稳定的，因为它们每个分别形成氮化物；即，氮化钨和氮化钼。
在本发明中，火烧气氛是氮和氢的共混物，典型的是95%的氮和5%的氢。氢的存在有助于防止形成不期望的氮化钨和氮化钼。
该加热步骤(火烧)能够在处于不同温度的几个步骤中进行，在步骤之间具有适当的升温。本发明的组合物已经使用下面的步骤来成功的生产：在800℃的1小时加热步骤，随后在1200℃另外1小时的加热步骤。和在高于1600℃的2小时加热步骤，并且在加热步骤之间的350℃/小时的升温步骤。目前为止最佳的样品是通过将组合物加热到1750℃来获得的。相当的无机发光材料还通过直接加热该材料(即，并非逐步升温)来生产。
使用本发明，已经观察到产率处于90%的范围中，并且在大部分情况中，基于信息和信心是至少95%。
所形成的组合物包括摩尔分数(“Y”)是大约0.013-0.017的铕和摩尔分数是大约0.5-0.65的锶(“X”)。因此，钙典型的存在摩尔分数是大约0.333-0.487。
该方法还能够用于生产式Sr2Si5N8的无机发光材料。
图1是本发明的无机发光材料组合物的相对强度对波长的图。该图所示的发光颜色是使用基于1931 CIE色品图的色坐标来算术描述的，并且其缩写为ccx和ccy。因此，该图代表了混入有本发明的无机发光材料的使用蓝光的二极管的ccy值，并且ccx坐标恒定保持在0.290。在图1-4中，无机发光材料是在大约450-470纳米(例如454nm)的波长照射的，并且该发射是在常规的分光计(例如Instrument Systems Optische Messtechnik GmbH，德国慕尼黑)上测量的。
如图1所示，在不存在锶的情况中，峰输出波长倾向于在大约660nm，并且加入增加量的锶产生了愈加类似于市售红光无机发光材料(例如'494公开文献中所述的该发光材料)的峰输出。
术语“峰波长”在此是以它常规的含义来使用的；即，光源(这里是二极管)的光强度最大时的波长。大部分二极管发射接近于该峰波长的范围的频率，因此在某些情况中，二极管的颜色表示为在最大值一半时的宽度，以此作为一种方式来为本领域技术人员提供关于所发射的光的特性的信息。
图2代表了本发明所要求保护的组合物的相对亮度和色坐标与锶的量的图。如图2的顶部(明亮)所示，最佳的结果是在大约0.55-0.67的锶原子分数时获得的。图2的底部表示了在大约0.58-0.67的锶原子分数时，颜色最一致。
图3和4以条形图的形式表示了市售的红光无机发光材料和本发明的无机发光材料的亮度和颜色的变化。对于市售的红光无机发光材料和根据本发明所形成的具有不同量的锶的无机发光材料来说，图3表示了亮度的变化，而图4表示了当ccx =0.290时所达到的ccy。
图5，6和7表示了本发明另外的方面。图5是泛称为10的相对大的氧化铝坩埚的顶部透视图。在该本发明的方法中，将钙，锶，铝和硅的氮化物与氟化铕在手套箱(未示出)中混合(典型的作为粉末)，其基本上没有水和氧。该粉末然后加入到钨或者钼坩埚中，该坩埚表示为位于大氧化铝坩埚10的基底12上的圆形坩埚11。气体流动管13通过圆柱壁14伸入到坩埚10的内部。
图6表示了坩埚10和盖子15以及气体管16的外面部分。氧化铝坩埚10置于泛称为17的盒式炉中。氧化铝坩埚10并非绝对需要的。如果该炉子本身适于包含组成气体气氛，则附图所示的氧化铝坩埚10可以是任选的。
管16典型的是由陶瓷材料形成的，同样对该陶瓷材料进行选择，以使得其不受组成气体的影响或者不受用于形成该无机发光材料的任何组分的影响或者不受该无机发光材料本身的影响。
盒式炉17然后用于使用前述的热循环来加热该材料。
图7是氧化铝坩埚10的横截面图，表示了圆柱壁14和盖子15。陶瓷管16、13穿过壁14延伸到氧化铝坩埚10的内部，并且箭头示意性的表示了流过钨或者钼坩埚11的组成气体。
所形成的组合物可以是化学计量的配方，或者它可以包括作为单独组分的氧氮化硅或者该氧氮化硅可以与铕基无机发光材料相组合。申请人不希望受限于任何具体的理论，并且使用此处所提供的信息，该无机发光材料的精确分子组成仍然是部分未确定的。
该混合物是以常规的方式来研磨成粉的，根据期望或者需要来使用。该研磨的粒子的尺寸取决于最终的应用，并且在大部分情况中可以由终端用户选择。
图8是本发明的无机发光材料组合物的x射线粉末衍射图。该粉末衍射是以常规方式来进行的(Cu的Ka线，从10-60度(2 θ)扫描)，并且该结果通常是本领域技术人员公知的。这些结果还能够无需过度试验来再现。
在图8中，实心圆代表了该无机发光材料所产生的衍射峰，空心正方形代表了氧氮化硅铝所产生的峰，空心三角形表示了存在着氮化铝，并且一个峰代表了未知的(迄今)材料。
最重要的，图8表明存在着氧氮化硅铝相。出于对比的目的，不同组分的x射线衍射图是在用于分类x射线衍射图的JCPDS文件系统(Joint Committee on Powder Diffraction Standards)下索引的。
在附图和申请文件中已经提出了本发明优选的实施方案，并且虽然使用了具体的术语，但是它们仅仅是以通用的和描述性的含义来使用的，目的并非限制，本发明的范围定义在权利要求中。
Claims (9)
1.一种制造无机发光材料组合物的方法，该方法包括：
在不存在水和氧的情况下，将Ca3N2，Sr2N，AlN和Si3N4与铕源组合物混合到一起形成混合物：
在处于或者接近于大气压的含氢和氮的组成气体的存在下，在难熔坩埚中加热该混合物，该加热的温度足以形成该无机发光材料组合物，但是低于前体组合物或者该无机发光材料分解或者与坩埚反应的温度，该无机发光材料组合物包含Ca1-x-ySrxEuyAlSiN3，其中0 < x <1和0 < y <1，并且混合有至少1重量%量的氧氮化硅铝。
2.根据权利要求1的方法，其中温度是1500-1800℃。
3. 根据权利要求1的方法，其中该难熔坩埚包含选自钨和钼的难熔金属。
4. 根据权利要求1的方法，其中该混合物的加热包括在逐渐提高的温度的至少3个加热步骤。
5. 根据权利要求1的方法，其中y是0.013-0.017和x是0.50-0.70。
6. 根据权利要求1的方法，其中氧氮化硅铝包括Si2Al4O4N4。
7. 一种无机发光材料组合物，其包含：
Ca1-x-ySrxEuyAlSiN3，其中0 < x <1和0 < y <1，和
至少1重量%量的氧氮化硅铝。
8. 根据权利要求7的无机发光材料组合物，其中y是0.013-0.017，并且x是0.50-0.70。
9. 根据权利要求7或8的无机发光材料组合物，其中x是0.55-0.67。
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| JP2012509364A (ja) | 2012-04-19 |
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