CN103068953A - 表面改性的硅酸盐发光体 - Google Patents
表面改性的硅酸盐发光体 Download PDFInfo
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- CN103068953A CN103068953A CN2011800396821A CN201180039682A CN103068953A CN 103068953 A CN103068953 A CN 103068953A CN 2011800396821 A CN2011800396821 A CN 2011800396821A CN 201180039682 A CN201180039682 A CN 201180039682A CN 103068953 A CN103068953 A CN 103068953A
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- silicate
- fluoridizing
- surface modification
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- 150000004760 silicates Chemical class 0.000 title abstract 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 8
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- 239000010410 layer Substances 0.000 claims description 26
- 229910052731 fluorine Inorganic materials 0.000 claims description 22
- 230000004048 modification Effects 0.000 claims description 22
- 238000012986 modification Methods 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 19
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 17
- 239000011737 fluorine Substances 0.000 claims description 17
- 239000011247 coating layer Substances 0.000 claims description 15
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- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
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- 229910052720 vanadium Inorganic materials 0.000 claims description 6
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- 230000000903 blocking effect Effects 0.000 claims description 4
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052593 corundum Inorganic materials 0.000 abstract description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 abstract 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 abstract 1
- 229910003443 lutetium oxide Inorganic materials 0.000 abstract 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 abstract 1
- 238000001354 calcination Methods 0.000 description 15
- 238000000034 method Methods 0.000 description 15
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- IUVCFHHAEHNCFT-INIZCTEOSA-N 2-[(1s)-1-[4-amino-3-(3-fluoro-4-propan-2-yloxyphenyl)pyrazolo[3,4-d]pyrimidin-1-yl]ethyl]-6-fluoro-3-(3-fluorophenyl)chromen-4-one Chemical compound C1=C(F)C(OC(C)C)=CC=C1C(C1=C(N)N=CN=C11)=NN1[C@@H](C)C1=C(C=2C=C(F)C=CC=2)C(=O)C2=CC(F)=CC=C2O1 IUVCFHHAEHNCFT-INIZCTEOSA-N 0.000 description 9
- 230000003287 optical effect Effects 0.000 description 9
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- -1 alkaline-earth metal orthosilicate Chemical class 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- KIDNIBDFWYHALR-UHFFFAOYSA-N silicic acid dihydrate Chemical compound O.[Si](O)(O)(O)O.O KIDNIBDFWYHALR-UHFFFAOYSA-N 0.000 description 6
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
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- 229910052917 strontium silicate Inorganic materials 0.000 description 5
- QSQXISIULMTHLV-UHFFFAOYSA-N strontium;dioxido(oxo)silane Chemical compound [Sr+2].[O-][Si]([O-])=O QSQXISIULMTHLV-UHFFFAOYSA-N 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 229910004283 SiO 4 Inorganic materials 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 4
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
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- 238000013112 stability test Methods 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- 238000004381 surface treatment Methods 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910016569 AlF 3 Inorganic materials 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
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- 230000004907 flux Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
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- 239000000320 mechanical mixture Substances 0.000 description 2
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- 229910052763 palladium Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000010671 solid-state reaction Methods 0.000 description 2
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- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical group FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 1
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- 229910016036 BaF 2 Inorganic materials 0.000 description 1
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
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- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 229910017768 LaF 3 Inorganic materials 0.000 description 1
- 241000283986 Lepus Species 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910017639 MgSi Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001341 alkaline earth metal compounds Chemical class 0.000 description 1
- 229910001618 alkaline earth metal fluoride Inorganic materials 0.000 description 1
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
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- 238000010894 electron beam technology Methods 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
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- 238000003682 fluorination reaction Methods 0.000 description 1
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- 229910052746 lanthanum Inorganic materials 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7734—Aluminates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
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- C09K11/77342—Silicates
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Abstract
一种表面改性的硅酸盐发光体包括硅酸盐发光体以及包覆层,包覆层包括以下的至少一种:(a)氟化的包覆层,包括氟化的无机试剂、氟化的有机试剂或者氟化的无机试剂和有机试剂的组合,所述氟化的包覆层产生疏水的表面位点,以及(b)氟化的包覆层和至少一个潮气阻挡层的组合。所述潮气阻挡层包括MgO、Al2O3、Y2O3、La2O3、Gd2O3、Lu2O3和SiO2或者对应的前驱物,包覆层设置在硅酸盐发光体的表面上。
Description
技术领域
本发明的示例性实施例涉及基于掺杂的碱土金属硅酸盐化合物的无机发光体,所述无机发光体能够将高能一次辐射,即例如,紫外(UV)辐射或蓝光转换成可见光谱区域内的波长较长的二次辐射,所述无机发光体可以用作诸如发射彩色光或白光的发光二极管(LED)的发光装置中的辐射转换体。本发明的示例性实施例还涉及可具有增加的工作寿命且对空气湿度和其他环境因素可具有改善的稳定性的硅酸盐无机发光体。
背景技术
包括掺杂铕的碱土金属正硅酸盐、相应的氧正硅酸盐和Ba(Sr)3MgSi2O8:Eu形式的二硅酸盐的碱土金属硅酸盐发光体己经被人们了解多时。Hollemann-Wiberg在“Lehrbuch der Anorganischen Chemie”无机化学102版(Walter de Gruyter & Co.,柏林,2007)报道了碱土金属硅酸盐化合物的分类的综述。在各种专利和出版物中已经详细描述了它的制备和基本的发光性质,例如:授权给Tews等人的第6,489,716号美国专利;Ouwerkerk等人申请的第0550937号欧洲申请公布;Hase等人申请的第0877070号欧洲申请公布;以及W.M.Yen等人编著的“Phosphor Handbook”,第二版,CRC出版社(2007)。这些出版物指出这样的发光体对于高能辐射到可见光的转换具有高的量子产率和辐射产率,并且由于这些性质,这类发光体的许多代表可以用于照明、发光和显示技术的产品中。
然而,基于碱土金属硅酸盐的发光体还具有各种不利的性质。缺点中的一些包括相对低的辐射稳定性以及发光体对水、空气湿度和其他环境因素的高敏感性。所述敏感性取决于发光体的具体组成、结构状况以及发光体的激活剂离子的性质。对于波长转换发光体的一些当前应用,这些性质可能是成问题的。考虑到高寿命的需求,可以将其应用于LED应用。一种已知的解决方案是使用合适的技术和材料来产生(在粉状无机发光体的表面上)阻挡层以减少水蒸气的影响。
这些工艺可以包括用有机聚合物包封、用诸如SiO2或Al2O3的纳米级氧化物包覆或者这些氧化物的化学气相沉积(CVD)。然而,对于硅酸盐发光体,可实现的保护可能不足以将相应的LED灯的寿命改善到期望的程度。此外,在被包覆的发光体的情况下,可能必须接受亮度损失、颜色位置改变和其他的品质损失。通过气相工艺将发光体颗粒微包封的工艺可能是不方便的并且可能是昂贵的。
发明内容
技术问题
本发明的示例性实施例提供了硅酸盐发光体,所述硅酸盐发光体可以提供潮气稳定性、对辐射和其他环境影响的稳定性以及改善的工作寿命。
本发明的示例性实施例还提供了已经用氟化的无机或有机试剂进行了表面处理的发光体。
本发明的示例性实施例还提供了精细分散的氟化物或氟化合物在发光体表面上的可检测到的固定,或者能够使发光体表面疏水并可以消除表面缺陷的这样的化合物的表面网络的形成。
本发明另外的特征将在以下的描述中进行阐述,部分地通过描述将是明显的,或者可通过本发明的实践而明了。
技术方案
本发明示例性实施例公开了一种表面改性的硅酸盐发光体,所述表面改性的硅酸盐发光体包括:(a)硅酸盐发光体以及包覆层,包覆层包括以下的至少一种:氟化的包覆层,包括氟化的无机试剂、氟化的有机试剂或者氟化的无机试剂和氟化的有机试剂的组合,所述氟化的包覆层产生疏水的表面位点;以及(b)氟化的包覆层和至少一个潮气阻挡层的组合,所述潮气阻挡层包括MgO、Al2O3、Ln2O3、Y2O3、La2O3、Gd2O3、Lu2O3和SiO2或者对应的前驱物。
将理解的是,前面的总体描述和下面的详细描述是示例性的和说明性的,并且意图对要求保护的发明提供进一步的解释。
附图说明
包括附图以提供对本发明进一步的理解,且附图被包括在本说明书中并构成本说明书的一部分,附图示出了本发明的实施例并与描述一起用于解释本发明的原理。
图1a是参考材料Sr2.9Ba0.01Ca0.05Eu0.04SiO5、市售Sr3SiO5:Eu发光体以及根据本发明示例性实施例的氧正硅酸盐发光体F-103、F-202、F-202T、F-320和F-TS-600的发射光谱。
图1b是参考材料Sr0.876Ba1.024Eu0.1SiO4以及根据本发明示例性实施例的两种碱土金属正硅酸盐发光体F-401和F-401TS的发射光谱。
图2a是未氟化的和氟化的碱土金属氧正硅酸盐发光体的电子显微照片,左侧示出了发光体Sr2.9Ba0.01Ca0.05SiO的未处理的颗粒,右侧示出了根据本发明示例性实施例的发光体F-202的氟化的颗粒。
图2b是根据本发明示例性实施例的发光体F-202的表面的放大电子显微照片。
图3是根据本发明示例性实施例的基础晶格组成Sr0.876Ba1.024SiO4:Eu0.1的未包覆的、氟化的以及SiO2包覆的碱土金属正硅酸盐发光体的电子显微照片,左侧示出了未包覆的起始材料的扫描电子显微照片,中间示出了氟化的发光体表面的扫描电子显微照片,右侧示出了用SiO2另外包覆的发光体样品的扫描电子显微照片。
图4是根据本发明示例性实施例的具有明显的氟化表面结构的发光体F-103的能量散射X射线(EDX)光谱图像;
图5是根据本发明示例性实施例的发光体F-103的X射线光电子(XPS)谱;
图6是示出了对于不同发光体样品的典型氟XPS峰的曲线图。曲线1涉及根据工作示例A1的组成为Sr2.9Ba0.01Ca0.05Eu0.04SiO5的发光体与一定量的NH4F的机械混合物,曲线2涉及根据本发明示例性实施例的氟化的发光体F-103的氟1s峰。
具体实施方式
以下,参照附图更充分地描述本发明,附图中示出了本发明的示例性实施例。然而,本发明可以以许多不同的形式来实施,而不应该解释为局限于这里所阐述的示例性实施例。确切地说,提供这些示例性实施例使得本公开是彻底的,且这些示例性实施例将把本发明的范围充分地传达给本领域技术人员。在附图中,为了清晰起见,会夸大层和区域的尺寸和相对尺寸。在附图中相同的标号表示相同的元件。
将理解的是,当元件或层被称作“在”另一元件或层“上”或“连接到”另一元件或层时,该元件或层可以直接在另一元件或层上或直接连接到另一元件或层,或者可以存在中间元件或中间层。相反,当元件被称作“直接在”另一元件或层“上”或“直接连接到”另一元件或层时,不存在中间元件或中间层。
在用高能UV辐射、蓝光、电子束、X射线或者伽马射线激发时,并根据发光体的特定化学组成和激活剂的性质,与现有技术相比,根据本发明示例性实施例的发光体可以以高辐射产率和对H2O、空气湿度和其他环境因素的显著提高的稳定性发射可见光和红外辐射。由于这个原因,它们可以用在长寿命的工业产品中,例如,阴极射线管和其他成像***(扫描激光束***)中、X射线图像转换器中、高性能光源、用于室内和室外照明的所有颜色的LED、LCD显示器的背光、太阳能电池、温室膜和玻璃中作为辐射转换体。
根据本发明的示例性实施例的发光体(包括表面改性的硅酸盐发光体)的特征可在于:其表面具有用于产生疏水表面位点的氟化的无机或者有机试剂的包覆层,或者所述氟化的包覆层与由诸如氧化物MgO、A12O3、Ln2O3(其中Ln=Y、La、Gd或者Lu)和SiO2或者相应的前驱物(或者溶胶-凝胶技术)的层形成材料构成的一个或多个潮气阻挡层的组合。
根据本发明示例性实施例的包括表面改性的硅酸盐发光体的发光体可以包括粉状的碱土金属硅酸盐发光体。表面改性的硅酸盐发光体可以具有通式:
(Me1+Me2+Me3+)x·(Si,P,Al,B,V,N,C,Ge)y·(O,N)z:(A,F,S)
其中,A是从镧系元素或者锰的组选择的激活剂;F是表面固定的并且可选择地交联的氟或者氟化合物;S表示使用未氟化的层形成材料的可选择的附加包覆层。Me1+是一价金属,Me2+是二价金属,Me3+是从元素周期表的第III族或者从镧系元素中选择的三价金属。一些硅可以被P、Al、B、V、N、Ge或C取代。系数x、y和z可以具有以下的范围:0<x<5、0<y<12以及0<z<24。
根据可以优化发光性质和稳定性性能的本发明的示例性实施例,表面改性的硅酸盐发光体中的一些碱土金属离子可以被其他二价离子(例如Mg、Zn)取代,或者为了电荷平衡而实施适当措施,被来自碱金属的组或稀土的组的一价或三价阳离子取代。另外,P、B、V、N、Ge或者C可以取代一些硅而进入表面改性的硅酸盐发光体的阴离子亚晶格中。
根据本发明的示例性实施例,可以使用Si(OR)3X形式(其中R=CH3,C2H5,...,X=F官能化的有机配体)的氟官能化的有机硅烷将碱土金属硅酸盐发光体氟化,受控的水解和缩合可以实现在硅酸盐发光体基质上形成氟化的阻挡层,该氟化的阻挡层可以是阻挡体并还可以具有疏水性质。
根据本发明示例性实施例的表面改性的硅酸盐发光体可以通过通式表征:
Sr3-x-y-zCaxBaySiO5:Euz,F,S
其中,0≤x≤2,0≤y≤2以及0<z<0.5。根据本发明示例性实施例的表面改性的硅酸盐发光体还可以通过式表征:
Sr3-x-y-zCaxBaySiO5:Euz,F,S
其中,0≤x≤0.05,0≤y≤0.5以及0<z<0.25。
可以通过在1000℃以上的温度下,碱土金属碳酸盐(可以用作起始材料)或者相应的金属氧化物和SiO2之间的多级高温固态反应来合成用作用于制备根据本发明示例性实施例的表面改性的发光体的基础的发光体粉末。另外,可以将矿化添加剂(例如,NH4Cl、NH4F或者碱金属或者碱土金属的卤化物或者三价金属的卤化物)加入到反应混合物中,以促进反应性并控制得到的发光体的颗粒尺寸分布。根据化学计量比的特定选择,可以生成期望组成的掺杂的碱土金属硅酸盐发光体,更具体地,对应的正硅酸盐发光体和氧正硅酸盐发光体。
因此,将计算的量的起始材料剧烈混合,然后在期望的温度范围内,在惰性或还原性气氛中进行多级煅烧工艺。为了优化发光体性质的目的,主煅烧工艺还可以可选地具有在不同的温度范围内的若干煅烧阶段。在煅烧工艺已经结束之后,冷却样品至室温,并进行针对例如熔剂残留物的去除、表面缺陷的最少化或者颗粒尺寸分布的微调的合适的后处理工艺。可选择地,也可以使用氮化硅(Si3N4)或者其他含有硅的前驱物代替氧化硅作为与使用的碱土金属化合物发生反应的反应物。用于制造示例性实施例的发光体的多晶发光体粉末的合成不限于上述的制备工艺。
为了将根据本发明的粉状碱土金属硅酸盐发光体的表面氟化,可以使用诸如碱金属氟化物(例如LiF、NaF、KF)、碱土金属氟化物(MgF2、CaF2、SrF2、BaF2)、AlF3和稀土的氟化物(例如YF3、LaF3或GdF3)、NH4F和NH4HF2的不同的无机氟化合物,还有其他的无机或者有机的氟化合物(例如,含有氟化物的胺)。将选择的材料与硅酸盐发光体粉末混合,这种情况下可以使用水悬浮液。加入的氟化剂的所需比例取决于化合物的溶解度和反应条件(pH、温度、混合强度、停留时间等),并可以通过实验确定。
在表面处理结束之后,从悬浮液中去除氟化的发光体,可以用合适的溶剂洗涤然后在80℃和200℃之间的温度下干燥。在冷却和筛选之后,氟化的发光体处于备用的形式。
为了获得最优的发光体性质,根据发明的发光体的特定组成、使用的氟化剂的类型和量以及另外的因素,使依照本发明制造的发光体另外地经历300℃到600℃的温度范围内还原性气氛下的热后处理(热处理),或者代替干燥工艺经历300℃到600℃的温度范围内还原性气氛下的热后处理(热处理)。下文通过若干工作示例给出了有关制造根据本发明示例性实施例的发光体的详细的信息。
工作示例A1
工作示例A1描述了根据本发明示例性实施例的设置有氟化的表面层并且具有基础晶格组成Sr2.9Ba0.01Ca0.05SiO5:Eu0.04的发光体的制备,该发光体被描述为样品F-103,它的光学数据在表1中,在图1a中样品F-103的发射光谱指定为“3”。
表1包含已经用不同量的NH4F处理过的铕激活的氧正硅酸锶发光体样品的光学数据和潮气稳定性数据。为了合成相应的发光体基质,将化学计量量的SrCO3、BaCO3、CaCO3、Eu2O3和SiO2以及0.2mol的NH4Cl剧烈混合,然后在刚玉坩埚中以及包含2%氢气的N2/H2气氛中,在1400℃下进行5小时的煅烧工艺。在煅烧工艺已经结束之后,将煅烧的材料均质化、研磨并用H2O洗涤。随后,将100g干燥并筛选的发光体与1.1g NH4F、200g玻璃珠以及1公升水一起引入到合适的塑料容器中,并在罐式磨机上以低速剧烈混合30分钟。几分钟的沉淀时间之后,首先轻轻倒出上清液,然后通过布氏漏斗抽吸过滤。随后干燥并筛选最终产物。
工作示例A2
为了制备根据本发明示例性实施例的包含样品F-202的发光体(在表2中列出了其光学数据,其发射光谱在图1a中被指定为“4”),将100g工作示例A1中描述的发光体基质与2.474g NH4HF2混合。表2包含已经用不同量的NH4HF2处理过的铕激活的氧正硅酸锶发光体样品的光学数据和潮气稳定性数据。在这种情况下,通过将上述混合物放入1L去离子水和400g玻璃珠中在辊式磨机上进行湿化学沉淀来应用氟化的表面层。处理一小时之后,从溶液中去除被包覆的发光体并进行与工作示例A1类似的后处理。
工作示例A3
这里,将30g根据工作示例A2制造的发光体在400℃下以及包含35%氢气的N2/H2气氛中在刚玉坩埚中热处理60分钟。冷却之后,通过筛选将样品F-202T均质化以制造出本发明的示例性实施例,在表2中列出了样品F-202T的光学数据,在图1a中其发射光谱被指定为“5”。
工作示例A4
根据工作示例A1以固态合成根据本发明示例性实施例的具有基础晶格组成Sr2.948Ba0.01Cu0.002SiO5:Eu0.04的氧正硅酸盐发光体,并使用前驱物材料四乙氧基硅烷(TEOS)包覆有SiO2网络。为了这个目的,将50g发光体与500mL溶液(1L乙醇、18.2g TEOS和100ml32%的氨水)混合,并在反应容器中搅拌2小时。其后,抽吸过滤被包覆的发光体,用乙醇洗涤,并在160℃下干燥24小时。
在这种预备的表面处理之后,如工作示例A1中那样,用NH4F作为氟化剂使发光体经历氟化。为了这个目的,使80g预包覆的发光体在工作示例1的条件下与1.98g NH4F反应。由此以样品F-TS-600的形式制造出根据本示例性实施例的发光体。如工作示例A1、A2和A3中描述的发光体那样,在表6中描述了样品F-TS-600的光学数据,在图1a中其发射光谱被指定为“7”,并且根据本示例性实施例的发光体与传统的氧正硅酸盐发光体相比可以具有显著改善的抗潮气性,并且可与未包覆的基础发光体具有相同的基础晶格组成。在表1、2和6中汇总了根据本发明示例性实施例的这些发光体的性能特性。
工作示例B1
为了制造根据本发明示例性实施例的样品F-320形式的发光体,合成组成为Sr2.9485Ba0.01Cu0.0015SiO5:Eu0.04的基础晶格。为了这个目的,将化学计量量的SrCO3、BaCO3、CuO、Eu2O3,65g SiO2和0.3mol的NH4Cl混合,引入到合适的煅烧坩埚中并在高温炉中煅烧24小时的时间段。煅烧过程具有在1200℃和1350℃下的两个主煅烧区间,其中每个温度下煅烧3个小时。在第一煅烧阶段期间,在具有5%氢气浓度的合成气体下进行煅烧,在后续的第二煅烧阶段,氢气的浓度增加到20%。
基质材料的冷却、洗涤和均质化之后,对发光体表面进行氟化。为了这个目的,使用的氟化剂是氟化铝AlF3而不是NH4F或者NH4HF2。为了与发光体颗粒的表面反应,在60℃下将1.2g AlF3引入到1L H2O中并将混合物剧烈搅拌1小时。随后,将100g合成的发光体基质加入到悬浮液中。反应时间可以是60分钟。类似于工作示例A1、A2、A3和A4,对样品F-320形式的被包覆的发光体进行后处理。表3中示出了光学数据,在图1a中其发射光谱被指定为“6”。表3包含进一步氟化的Eu2+掺杂的氧正硅酸锶发光体的光学数据和稳定性数据。
工作示例C1
下面的工作示例涉及根据本发明示例性实施例包覆的并具有组成Sr0.876Ba1.024SiO4:Eu0.1的碱土金属正硅酸盐发光体。在本示例性实施例中,通过高温固态反应制造基体材料,其中,起始混合物包括化学计量量的SrCO3、BaCO3、Eu2O3、SiO2以及0.2mol的NH4Cl。
煅烧工艺包括在氮气氛中加热填充有起始混合物的坩埚到1275℃,保持这个温度10小时的时间段,随后冷却到室温。当达到高温斜坡时,加入20%的氢气到保护气体。冷却之后,洗涤得到的材料以去除熔剂残留物,然后干燥并筛选。
为了使基体材料氟化,在3L H2O中悬浮150g发光体粉末和4.268g NH4F并搅拌2小时的时间段。包覆过程已经结束之后,抽吸过滤氟化的发光体以得到样品F-401,在吸滤器上用乙醇洗涤,并在130℃干燥24小时。在表4中示出了样品F-401的光学数据,在图1b中F-401的发射光谱被指定为“3”。表4包含另外地包覆有SiO2的氟化的发射绿波长的碱土金属正硅酸盐发光体的光学数据和稳定性数据。
在另外的步骤中,根据本示例性实施例的样品F-401形式的发光体可以设置有SiO2包覆层。为了这个目的,将50g氟化的Sr0.876Ba1.024SiO4:Eu0.1发光体粉末加入到500mL TEOS溶液(由1L的乙醇、25g的TEOS和150mL的32%的氨水构成)中,所述TEOS溶液在使用前24小时已经制备好。搅拌5小时的时间之后,终止反应。抽吸过滤样品F-401TS形式的表面包覆的发光体,再次用乙醇洗涤,并干燥。在表4中列出了样品F-401TS的光学数据,在图1b中F-401TS的发射光谱被指定为“4”。
在图1a和图1b中描述了不同基质组成的氟化发光体与每种情况下未处理的发光体相比的发射光谱,其示出了根据本发明示例性实施例的具有氟化的表面结构的发光体的发光强度与参考材料的发光强度略有不同。在表1、表2、表3、表4、表5、表6和表7中汇总的根据示例性实施例的发光体样品的发光数据也证实这一点,而在氟化的和可选地另外SiO2包覆的样品的某些情况下测量出稍微低的发光强度。在表中还有涉及表面处理导致发光效率稍微增加的示例。后一种效果可能归因于在被包覆的材料的情况下光的发射稍微要好些。
在图2a和图2b中,将根据本发明示例性实施例的氟化的Sr3SiO5:Eu发光体的电子显微照片与未处理的起始材料的电子显微照片相比。这些显微照片表明,在工作示例中描述的用合适的氟化剂的表面处理使得形成了特定的表面结构,可借助扫描电子显微镜看到所述表面结构。
对于图3中示出的绿波长发光碱土金属正硅酸盐发光体的电子显微照片,情况是可比较的。图3中的显微照片示出了未处理的发光体样品的特征颗粒表面、根据本发明示例性实施例制造的氟化的材料的特征颗粒表面以及从起始材料获得的另外的样品(已经另外地用SiO2包覆)的特征颗粒表面。
同时,从图4中示出的相应的能量散射X射线光谱(EDX)分析的结果来看,清楚的是表面结构包含氟。除了发光体基质特有的锶(Sr)、硅(Si)和氧(O)的峰之外,在根据本发明氟化的发光体的EDX光谱中发现了具有显著峰高的明显的单一反射(singular reflection),根据峰的能量位置这种明显的单一反射明确地确定为元素氟(F)。此外,示出的光谱还包含确定为金(Au)和钯(Pd)的反射,这是由于与分析方法有关的原因用金和钯包覆发光体样品引起的。
通过X射线光电子光谱(XPS)分析的结果在图5和图6中记录了在根据本发明示例性实施例的发光体表面上精细分散的氟化物或者氟化合物的固定或者形成这些化合物的网络的进一步证据。固定可以包括吸附和与化学吸附或者物理吸附相似的方法。图5中示出的根据工作示例1用NH4F处理的发光体(基础晶格组成为Sr2.9Ba0.01Ca0.05Eu0.04SiO5)的XPS光谱表明,用这种固态分析法也能够检测到作为氟化的发光体的表面结构的组成部分的元素氟(F)。从XPS光谱中还可以得到进一步的结论。例如,通过比较NH4F氟化的氧正硅酸盐发光体的内部校准的XPS光谱(图6中的曲线2)与对应的发光体基质和相同量的NH4F的机械混合物的样品的内部校准的XPS光谱(图6中的曲线1),如图6中所示明显的是,在每种情况下确定的F1s峰具有不同的强度并且还表现出相对于彼此的结合能的移动。
标记为曲线2的样品的F1s峰的较低的强度可以被解释为在处理过程中一些添加的氟从发光体表面的损失。曲线1的F1s峰向较低结合能的移动可表明应用的氟化剂与发光体基质的表面之间的化学键的形成。
在表1、表2、表3、表4、表5和表6中,汇总了根据本发明示例性实施例构造的不同硅酸盐发光体的若干发光参数和稳定性测试的结果,并将其与未改变的(即,表面未氟化的)发光体粉末的若干发光参数和稳定性测试的结果比较,以及在某些情况下与市售的对比发光体的若干发光参数和稳定性测试的结果比较。表5包含氟化的以及氟化的并且SiO2包覆的Eu2+包覆的氧正硅酸锶发光体的光学数据和稳定性数据。表6包含已经氟化的SiO2包覆的氧正硅酸锶发光体的光学数据和稳定性数据。
通过在于85℃的温度和85%的空气湿度下工作的温控柜中储存对应的发光体样品七天来评估材料的潮气稳定性。随后,在150℃下干燥发光体24小时,然后进行发光产率的比较测量。
比较发光测量的结果表明,根据本发明示例性实施例的发光体的发光效率及其温度依赖性与市售的铕激活的碱土金属氧正硅酸盐或者对应的正硅酸盐发光体的发光效率及其温度依赖性相同,或者甚至超过它们。其次,如表4、表5和表6中示出的,稳定性测试的结果表明,与具有相同基质组成的未改变的(即,表面未氟化的)发光体相比,根据本发明示例性实施例的具有氟化的表面结构以及可选的附加SiO2包覆层的发光体具有显著改善的抗潮气性。
本领域技术人员将清楚的是,在不脱离本发明的精神或范围的情况下,对本发明可以作出各种修改和变形。因此,本发明意图覆盖本发明的修改和变形,只要它们落入所附权利要求及其等同物的范围内。
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Claims (8)
1.一种表面改性的硅酸盐发光体,包括:
硅酸盐发光体;以及
包覆层,包括以下的至少一种:
氟化的包覆层,包括氟化的无机试剂、氟化的有机试剂或者氟化的无机试剂和氟化的有机试剂的组合,所述氟化的包覆层产生疏水的表面位点;以及
氟化的包覆层和至少一个潮气阻挡层的组合,所述潮气阻挡层包括MgO、Al2O3、Y2O3、La2O3、Gd2O3、Lu2O3和SiO2或者对应的前驱物,
其中,包覆层设置在硅酸盐发光体的表面上。
2.根据权利要求1所述的表面改性的硅酸盐发光体,其中,表面改性的发光体包括粉状的碱土金属硅酸盐发光体。
3.根据权利要求1所述的表面改性的硅酸盐发光体,其中,氟化的包覆层包括氟官能化的有机硅烷,氟官能化的有机硅烷包括通式Si(OR)3X,其中R=CH3、C2H5或者更高级的烷,X包括氟官能化的有机配体,以及
其中,氟化层设置在硅酸盐发光体上,氟化的阻挡层包括疏水性质。
4.根据权利要求1所述的表面改性的硅酸盐发光体,其中,硅酸盐发光体包括通式(Me1+Me2+Me3+)x·(Si,P,Al,B,V,N,C,Ge)y·(O,N)z:(A,F,S),其中,A是从镧系元素和/或锰的组选择的激活剂,F是表面固定的或者交联的氟或氟化合物,S是使用未氟化的层形成材料的附加包覆层,Me1+是一价金属,Me2+是二价金属,Me3+是从第III族或者镧系元素中选择的三价金属,一些硅可以被P、Al、B、V、N、Ge或者C取代,并且0<x<5,0<y<12,0<z<24。
5.根据权利要求1所述的表面改性的硅酸盐发光体,其中,硅酸盐发光体包括式Sr3-x-y-zCaxBaySiO5:Euz,F,S,其中,0≤x≤2,0≤y≤2以及0<z<0.5。
6.根据权利要求1所述的表面改性的硅酸盐发光体,其中,硅酸盐发光体包括式Sr3-x-y-zCaxBaySiO5:Euz,F,S,其中,0≤x≤0.05,0≤y≤0.5以及0<z<0.25。
7.根据权利要求2所述的表面改性的硅酸盐发光体,其中,所述粉状的碱土金属硅酸盐发光体还包括被包括Mg、Zn的二价离子,从碱金属的组和稀土的组选择的一价阳离子以及从稀土的组选择的三价阳离子取代的碱土金属。
8.根据权利要求2所述的表面改性的硅酸盐发光体,其中,所述粉状的碱土金属硅酸盐发光体还包括被P、B、V、N、Ge或C取代的硅。
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TW201211209A (en) | 2012-03-16 |
TWI522444B (zh) | 2016-02-21 |
WO2012023714A2 (en) | 2012-02-23 |
KR101761855B1 (ko) | 2017-07-27 |
EP2603937B1 (en) | 2016-11-23 |
EP2603937A2 (en) | 2013-06-19 |
US20120205674A1 (en) | 2012-08-16 |
RU2013111293A (ru) | 2014-09-20 |
EP2603937A4 (en) | 2014-10-22 |
RU2569167C2 (ru) | 2015-11-20 |
CN103081140A (zh) | 2013-05-01 |
KR20120023496A (ko) | 2012-03-13 |
US8581286B2 (en) | 2013-11-12 |
RU2013111302A (ru) | 2014-09-20 |
WO2012023714A3 (en) | 2012-05-18 |
US20120037850A1 (en) | 2012-02-16 |
KR20120023495A (ko) | 2012-03-13 |
JP2013541828A (ja) | 2013-11-14 |
US8945421B2 (en) | 2015-02-03 |
BR112013003417A2 (pt) | 2020-10-27 |
BR112013003416B1 (pt) | 2022-01-11 |
BR112013003417B1 (pt) | 2021-10-13 |
EP2603571A4 (en) | 2014-10-22 |
JP2013536283A (ja) | 2013-09-19 |
KR101752428B1 (ko) | 2017-07-05 |
DE102010034322A1 (de) | 2012-02-16 |
EP2603571A2 (en) | 2013-06-19 |
TW201211208A (en) | 2012-03-16 |
TWI541325B (zh) | 2016-07-11 |
BR112013003416A2 (pt) | 2020-10-27 |
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