CN114096641A - 铝酸锶混合氧化物及其制备方法 - Google Patents
铝酸锶混合氧化物及其制备方法 Download PDFInfo
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- CN114096641A CN114096641A CN202080050303.8A CN202080050303A CN114096641A CN 114096641 A CN114096641 A CN 114096641A CN 202080050303 A CN202080050303 A CN 202080050303A CN 114096641 A CN114096641 A CN 114096641A
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- Prior art keywords
- suspension
- strontium
- strontium aluminate
- mixed oxide
- aluminate mixed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000005084 Strontium aluminate Substances 0.000 title claims abstract description 176
- FNWBQFMGIFLWII-UHFFFAOYSA-N strontium aluminate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Sr+2].[Sr+2] FNWBQFMGIFLWII-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 238000002360 preparation method Methods 0.000 title description 8
- 238000000034 method Methods 0.000 claims abstract description 62
- 239000002243 precursor Substances 0.000 claims abstract description 42
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000012798 spherical particle Substances 0.000 claims abstract description 9
- 239000000725 suspension Substances 0.000 claims description 173
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 76
- 239000002245 particle Substances 0.000 claims description 37
- 239000011148 porous material Substances 0.000 claims description 37
- 150000003438 strontium compounds Chemical class 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 229910003669 SrAl2O4 Inorganic materials 0.000 claims description 13
- FHPAAYZTTWZXEB-UHFFFAOYSA-N aluminum strontium oxygen(2-) Chemical compound [O-2].[Al+3].[Sr+2] FHPAAYZTTWZXEB-UHFFFAOYSA-N 0.000 claims description 12
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 12
- 238000010335 hydrothermal treatment Methods 0.000 claims description 11
- 229910001593 boehmite Inorganic materials 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 159000000008 strontium salts Chemical class 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 6
- 229910052693 Europium Inorganic materials 0.000 claims description 6
- 239000007900 aqueous suspension Substances 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 6
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 6
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 claims description 6
- 239000012190 activator Substances 0.000 claims description 5
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 5
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 5
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 5
- 229910001631 strontium chloride Inorganic materials 0.000 claims description 3
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims 2
- 150000002910 rare earth metals Chemical class 0.000 claims 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 25
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000499 gel Substances 0.000 description 8
- 238000000227 grinding Methods 0.000 description 8
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 7
- 238000004626 scanning electron microscopy Methods 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 5
- 229910003668 SrAl Inorganic materials 0.000 description 4
- 238000003801 milling Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910001680 bayerite Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 229910001648 diaspore Inorganic materials 0.000 description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910001679 gibbsite Inorganic materials 0.000 description 2
- 238000000634 powder X-ray diffraction 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
- 239000000243 solution Substances 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 description 2
- 229910001866 strontium hydroxide Inorganic materials 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- RNAMYOYQYRYFQY-UHFFFAOYSA-N 2-(4,4-difluoropiperidin-1-yl)-6-methoxy-n-(1-propan-2-ylpiperidin-4-yl)-7-(3-pyrrolidin-1-ylpropoxy)quinazolin-4-amine Chemical compound N1=C(N2CCC(F)(F)CC2)N=C2C=C(OCCCN3CCCC3)C(OC)=CC2=C1NC1CCN(C(C)C)CC1 RNAMYOYQYRYFQY-UHFFFAOYSA-N 0.000 description 1
- 238000005169 Debye-Scherrer Methods 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- -1 Strontium Aluminates Chemical class 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000011143 downstream manufacturing Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 238000002356 laser light scattering Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006194 liquid suspension Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000006069 physical mixture Substances 0.000 description 1
- 238000004375 physisorption Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229910009112 xH2O Inorganic materials 0.000 description 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 1
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- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
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Abstract
本发明涉及铝酸锶混合氧化物前体及其制备方法,以及铝酸锶混合氧化物及其制备方法。铝酸锶混合氧化物前体可以在相对较低的温度下转化为铝酸锶混合氧化物。铝酸锶混合氧化物的特征在于具有海绵状或多孔骨状的微结构的基本上球形的颗粒。还提供了一种包含铝酸锶混合氧化物的发光材料。
Description
技术领域
本发明通常涉及用于制备发光材料的混合氧化物。更具体地,本发明涉及铝酸锶混合氧化物前体及其制备方法、铝酸锶混合氧化物及其制备方法以及包含铝酸锶混合氧化物的发光材料。
背景技术
掺杂有作为活化剂的铕(Eu2+)和镝(Dy3+)的铝酸锶(特别是SrAl2O4:Eu和SrAl2O4:Dy及其衍生物)以其作为具有长余辉性质的发光颗粒的应用而众所周知。此类颗粒例如用于水泥、应急标志、发光时钟内的指针和时间间隔标记、道路标志或织物中。
通常,这些材料通过常规制陶法制备,例如通过相应的金属氧化物和/或碳酸盐的物理混合物的固态反应。这些方法包括在约1300℃至1500℃的高温下进行强化热处理。有时,为了提高反应性,在热处理之前,对混合氧化物前体进行球磨。这导致这种混合氧化物的制备过程中的高能量消耗。
EP 0622440 A1描述了一种磷光性荧光体的制备方法,其包括在球磨机中研磨SrCO3、Eu2O3、Al2O3和硼酸(作为熔剂)的物理混合物,随后在1300℃下加热1小时。为了获得用于在期望的最终应用(例如作为树脂或作为涂层)中应用并分散材料的期望的粒径分布,能量密集和昂贵的研磨步骤是必要的。Kutty T.R.N.等人的出版物“Luminescence of EUin Strontium Aluminates prepared by hydrothermal methods”(1990年11月1日,MATERIALS RESEARCH BULLETIN,ELSEVIER,KIDLINGTON,GB第1355至1362页,ISSN0025-5408)描述了使用氧化铝凝胶和SrO2制备发光材料。在凝胶中,固体是连续相。凝胶不是悬浮体。
由于通过高温处理(这是常规制陶法的一个组成部分)获得的铝酸锶混合氧化物具有高度烧结的特性,因此研磨步骤需要高能量输入和长持续时间。这使得通过常规制陶法制备铝酸锶混合氧化物的制备方法的效率低下;此外,强化研磨步骤会在材料中产生缺陷,从而降低其发光性质。
本领域提出的降低铝酸锶混合氧化物的形成温度的解决方案为应用溶胶-凝胶和燃烧合成技术。这些技术通常通过混合金属硝酸盐和有机燃料并将混合物加热至约500℃至700℃来进行。该方法通过利用有机燃料燃烧的放热能,以比常规制陶法更低的相对能量输入制备混合氧化物。然而,这种方法需要大量的废气后处理系统,以避免将不需要的气体排放到环境中。此外,会产生蓬松的细颗粒,这些颗粒在下游工艺中处理的过程中趋于形成灰尘。
因此,需要一种更加节能的方法来生产铝酸锶混合氧化物。换言之,需要一种可以在相对较低的温度(相对于常规制陶法)下生产铝酸锶混合氧化物的方法以及一种能够生产具有在研磨处理的过程中易于破碎的微结构的铝酸锶混合氧化物的方法。
发明内容
根据本发明的第一方面,提供了一种制备铝酸锶混合氧化物前体的方法,所述方法包括:
i)提供铝氧化物悬浮体;
ii)向铝氧化物悬浮体中加入锶化合物,以形成锶铝氧化物悬浮体(Sr-Al悬浮体);
iii)其中对以下应用水热处理
a)铝氧化物悬浮体(无需对随后获得的Sr-Al悬浮体进行水热处理)或者
b)Sr-Al悬浮体(无需对之前获得的铝氧化物悬浮体进行水热处理)或者
c)铝氧化物悬浮体和Sr-Al悬浮体两者
以获得
来自a)的经水热处理的铝氧化物悬浮体,
来自b)的经水热处理的Sr-Al悬浮体,或者
来自c)的经水热处理的铝氧化物悬浮体和经水热处理的Sr-Al悬浮体;以及
iv)干燥经水热处理的Sr-Al悬浮体(通过b)或c)获得)或者Sr-Al悬浮体(通过a)获得)
以生产铝酸锶混合氧化物前体,
这意味着步骤iv)的Sr-Al悬浮体包括经水热处理的铝氧化物悬浮体形式的铝氧化物悬浮体,其中在水热处理之后加入锶化合物,而无需对Sr-Al悬浮体进行额外的水热处理。
因此,根据本发明的第一方面的第一种选择,提供了一种制备铝酸锶混合氧化物前体的方法,所述方法包括:
i)提供铝氧化物悬浮体;
ii)水热处理铝氧化物悬浮体,以获得经水热处理的铝氧化物悬浮体;
iii)向经水热处理的铝氧化物悬浮体中加入锶化合物,以形成锶铝氧化物悬浮体(Sr-Al悬浮体);以及
iv)干燥Sr-Al悬浮体,以产生铝酸锶混合氧化物前体。
根据本发明的第一方面的第二种选择,提供了一种制备铝酸锶混合氧化物前体的方法,所述方法包括:
i)提供铝氧化物悬浮体;
ii)向铝氧化物悬浮体中加入锶化合物,以形成锶铝氧化物悬浮体(Sr-Al悬浮体);
iii)水热处理Sr-Al悬浮体,以获得经水热处理的Sr-Al悬浮体;以及
iv)干燥经水热处理的Sr-Al悬浮体,以产生铝酸锶混合氧化物前体。
根据本发明的第一方面的第三种选择,提供了一种制备铝酸锶混合氧化物前体的方法,所述方法包括:
i)提供铝氧化物悬浮体;
ii)水热处理铝氧化物悬浮体,以获得经水热处理的铝氧化物悬浮体;
iii)向经水热处理的铝氧化物悬浮体中加入锶化合物,以形成锶铝氧化物悬浮体(Sr-Al悬浮体);
iv)水热处理Sr-Al悬浮体,以获得经水热处理的Sr-Al悬浮体;以及
v)干燥经水热处理的Sr-Al悬浮体,以产生铝酸锶混合氧化物前体。
本发明的第一方面的第二种选择是优选的。
以下说明适用于本发明的所有方面,而不是仅适用于第一方面。
铝氧化物悬浮体可以为氢氧化铝氧化物(AlO(OH))、氢氧化铝(Al(OH)3)、氧化铝(Al2O3)或其任何组合的悬浮体。氢氧化铝氧化物可以为勃姆石、水铝石或其任何组合。氢氧化铝可以为三水铝石、三羟铝石或其任何组合。氧化铝可以为过渡型氧化铝,例如γ-(gamma)氧化铝、δ(delta)氧化铝、θ-(theta)氧化铝、α-(alpha)氧化铝或其任何组合。
优选地,铝氧化物悬浮体为氢氧化铝氧化物悬浮体,更优选地,氢氧化铝氧化物悬浮体为勃姆石悬浮体。勃姆石的晶体尺寸((021)和/或(020)反射)可以在3nm和50nm之间,优选在4nm和45nm之间。
铝氧化物悬浮体优选为水性悬浮体。水性悬浮体意指将氧化铝至少加入到水中。
铝氧化物悬浮体的固体含量可以在1重量%至30重量%的范围内,优选在3重量%至15重量%的范围内。
铝氧化物悬浮体中的固体通过激光衍射法(如后文所述)测得的平均颗粒尺寸(d50)可以在0.01μm至100μm的范围内,优选在0.2μm至30μm的范围内。
术语d50是本领域公知的,并且表示这样的颗粒尺寸直径,其中样品中颗粒体积的50%小于所述颗粒尺寸直径且样品中颗粒体积的50%大于所述直径。
悬浮体优选为水性悬浮体,更优选地,液体悬浮介质为水。
锶化合物可以为锶盐、氧化锶、氢氧化锶或其任何组合。锶盐可以为乙酸锶、硝酸锶、碳酸锶、氯化锶或其混合物。优选地,锶化合物为锶盐的混合物。更优选地,锶化合物可以为乙酸锶和碳酸锶的混合物。
可以通过在水的存在下将铝氧化物悬浮体、Sr-Al悬浮体或两者加热到100℃至250℃范围内的温度,优选加热到180℃至220℃范围内的温度来进行水热处理铝氧化物悬浮体、Sr-Al悬浮体或两者,持续时间在0.5h至14h的范围内,优选地持续时间在1h至8h的范围内。可以在5和12之间的pH下,优选在6和11之间的pH下进行水热处理。
可以通过喷雾干燥进行干燥经水热处理的Sr-Al悬浮体或Sr-Al悬浮体以产生铝酸锶混合氧化物前体。
根据本发明的第二方面,提供了一种根据本发明的第一方面(包括第一方面的第一种选择、第二种选择和第三种选择)生产的铝酸锶混合氧化物前体,所述铝酸锶混合氧化物前体的特征在于在900℃至1100℃范围内的温度进行煅烧,持续时间在0.5h至5h的范围内,优选地,持续时间为3h。
根据本发明的第三方面,提供了一种制备铝酸锶混合氧化物的方法,所述方法包括:
i)提供铝氧化物悬浮体;
ii)向铝氧化物悬浮体中加入锶化合物,以形成锶铝氧化物悬浮体(Sr-Al悬浮体);
iii)水热处理i)铝氧化物悬浮体、ii)Sr-Al悬浮体、或者iii)铝氧化物悬浮体和Sr-Al悬浮体两者,以获得经水热处理的铝氧化物悬浮体、经水热处理的Sr-Al悬浮体、或者经水热处理的铝氧化物悬浮体和经水热处理的Sr-Al悬浮体两者;
iv)干燥经水热处理的Sr-Al悬浮体或者锶铝氧化物悬浮体,以产生铝酸锶混合氧化物前体;以及
v)煅烧铝酸锶混合氧化物前体,以产生铝酸锶混合氧化物。
本发明的第三方面与上文针对本发明的第一方面的描述相同,除了额外应用煅烧步骤v),从而获得铝酸锶混合氧化物。
因此,根据本发明的第三方面的第一种选择,提供了一种制备铝酸锶混合氧化物的方法,所述方法包括:
i)提供铝氧化物悬浮体;
ii)水热处理铝氧化物悬浮体,以获得经水热处理的铝氧化物悬浮体;
iii)向经水热处理的铝氧化物悬浮体中加入锶化合物,以形成锶铝氧化物悬浮体(Sr-Al悬浮体);
iv)干燥Sr-Al悬浮体,以产生铝酸锶混合氧化物前体;以及
v)煅烧铝酸锶混合氧化物前体,以产生铝酸锶混合氧化物。
根据本发明的第三方面的第二种选择,提供了一种制备铝酸锶混合氧化物的方法,所述方法包括:
i)提供铝氧化物悬浮体;
ii)向铝氧化物悬浮体中加入锶化合物,以形成锶铝氧化物悬浮体(Sr-Al悬浮体);
iii)水热处理Sr-Al悬浮体,以获得经水热处理的Sr-Al悬浮体;
iv)干燥经水热处理的Sr-Al悬浮体,以产生铝酸锶混合氧化物前体;以及
v)煅烧铝酸锶混合氧化物前体,以产生铝酸锶混合氧化物。
根据本发明的第三方面的第三种选择,提供了一种制备铝酸锶混合氧化物前体的方法,所述方法包括:
i)提供铝氧化物悬浮体;
ii)水热处理铝氧化物悬浮体,以获得经水热处理的铝氧化物悬浮体;
iii)向经水热处理的铝氧化物悬浮体中加入锶化合物,以形成锶铝氧化物悬浮体(Sr-Al悬浮体);
iv)水热处理Sr-Al悬浮体,以获得经水热处理的Sr-Al悬浮体;
v)干燥经水热处理的Sr-Al悬浮体,以产生铝酸锶混合氧化物前体;以及
vi)煅烧铝酸锶混合氧化物前体,以产生铝酸锶混合氧化物。
本发明的第三方面的第一种选择是优选的。
铝氧化物悬浮体可以为氢氧化铝氧化物(AlO(OH))、氢氧化铝(Al(OH)3)、氧化铝(Al2O3)或其任何组合的悬浮体。氢氧化铝氧化物可以为勃姆石、水铝石或其任何组合。氢氧化铝(Al(OH)3)可以为三水铝石、三羟铝石或其任何组合。氧化铝可以为过渡型氧化铝,例如γ-氧化铝、ó-氧化铝、θ-氧化铝、α-氧化铝或其任何组合。
优选地,铝氧化物悬浮体为氢氧化铝氧化物悬浮体,更优选地,氢氧化铝氧化物悬浮体为勃姆石悬浮体。勃姆石的晶体尺寸(021反射)可以在3nm和50nm之间,优选在3nm和45nm之间。
铝氧化物悬浮体优选为水性悬浮体。水性悬浮体意指将氧化铝至少加入到水中,反之亦然。
铝氧化物悬浮体的固体含量可以在1重量%至30重量%的范围内,优选在3重量%至15重量%的范围内。
铝氧化物悬浮体中的固体通过激光衍射法(如后文所述)测得的平均颗粒尺寸(d50)可以在0.01μm至100μm的范围内,优选在0.2μm至30μm的范围内。d50如上定义。
锶化合物可以为锶盐、氧化锶、氢氧化锶或其任何组合。锶盐可以为乙酸锶、硝酸锶、碳酸锶、氯化锶或其混合物。优选地,锶化合物为锶盐的混合物。更优选地,锶化合物可以为乙酸锶和碳酸锶的混合物。
可以通过将铝氧化物悬浮体、Sr-Al悬浮体或两者(在两个处理步骤中)加热到100℃至250℃范围内的温度,优选加热到180℃至220℃范围内的温度来进行水热处理铝氧化物悬浮体、Sr-Al悬浮体或两者,持续时间在0.5h至14h的范围内,优选地持续时间在1h至8h的范围内。可以在5和12之间的pH下,优选在6和11之间的pH下进行水热处理。
可以通过喷雾干燥进行干燥Sr-Al悬浮体或Sr-Al悬浮体以产生铝酸锶混合氧化物前体。
可以在900℃至1100℃范围内的温度进行煅烧铝酸锶混合氧化物前体以产生铝酸锶混合氧化物,持续时间在0.5h至5h的范围内。优选地,在900℃至1100℃范围内的温度进行煅烧铝酸锶混合氧化物前体以产生铝酸锶混合氧化物,持续时间为3h。
可以使用本领域已知的任何煅烧方法(例如回转窑式锻烧炉或马弗炉)进行煅烧铝酸锶混合氧化物前体。这些方法是本发明的领域的技术人员已知的。
根据本发明的第四方面,提供了一种根据本发明的第三方面生产的铝酸锶混合氧化物,其特征在于铝酸锶混合氧化物的颗粒具有海绵状或多孔骨状的微结构。
在本说明书中,术语“海绵状或多孔骨状的微结构”旨在意指这样的颗粒结构,其特征在于其由颗粒的非多孔一级框架构成,所述颗粒通过薄而易碎的烧结颈状部互相连接,以形成优选球形的三维二级结构,其具有明显的大孔结构,并且可以通过Hg侵入法测量孔隙尺寸。通过扫描电子显微镜(SEM)可以进一步观察到这种结构。
铝酸锶混合氧化物可以为SrAl2O4、SrAl4O7、Sr3Al2O6、SrAl12O19、Sr4Al14O25或其混合物。优选地,铝酸锶混合氧化物为SrAl2O4。
铝酸锶混合氧化物通过激光衍射测得的颗粒尺寸可以在1μm至150μm的范围内,优选在5μm和150μm之间。
铝酸锶混合氧化物可以具有基本上球形的颗粒。基本上意指至少60%的铝酸锶混合氧化物颗粒将具有球形形状。独立于此,球形颗粒的基于体积的球度优选在0.90和1.00之间。
铝酸锶混合氧化物的BET表面积可以小于20m2/g。
根据本发明的第五方面,提供了一种铝酸锶混合氧化物,其特征在于铝酸锶混合氧化物的颗粒具有海绵状或多孔骨状的微结构。
术语“海绵状或多孔骨状的微结构”具有如上文定义的含义。
铝酸锶混合氧化物可以为SrAl2O4、SrAl4O7、Sr3Al2O6、SrAl12O19、Sr4Al14O25或其混合物。优选地,铝酸锶混合氧化物为SrAl2O4。
铝酸锶混合氧化物通过激光衍射法(如后文所述)测得的颗粒尺寸可以在1μm至150μm的范围内,优选在5μm和150μm之间。
铝酸锶混合氧化物可以具有基本上球形的颗粒。基本上意指至少60%的铝酸锶混合氧化物颗粒将具有球形形状。独立于此,所述颗粒的基于体积的球度优选在0.90和1.00之间。
铝酸锶混合氧化物的BET表面积可以小于20m2/g。
根据本发明的第六方面,提供了一种铝酸锶混合氧化物,其特征在于铝酸锶混合氧化物的颗粒具有海绵状或多孔骨状微结构,并且铝酸锶混合氧化物具有至少一个、优选大于1个并且最优选全部的以下性质:
通过激光衍射(如后文所述)测得的颗粒尺寸在1μm至150μm的范围内,优选在5μm和150μm之间;
基本上球形的颗粒,优选地所述颗粒基于体积的球度在0.90和1.00之间;以及
BET表面积小于20m2/g。
铝酸锶混合氧化物可以为SrAl2O4、SrAl4O7、Sr3Al2O6、SrAl12O19、Sr4Al14O25或其混合物。优选地,铝酸锶混合氧化物为SrAl2O4。
本发明的不同方面中的任一个的铝酸锶混合氧化物均可以掺杂有活化剂,以形成经掺杂的铝酸锶混合氧化物。活化剂可以为稀土氧化物。稀土氧化物可以为铕(Eu)、镝(Dy)或者Eu和Dy两者。优选地,铝酸锶混合氧化物掺杂有Eu和Dy两者。经掺杂的铝酸锶混合氧化物优选掺杂有小于5重量%的总稀土氧化物质量,优选在0.5重量%和小于5重量%之间。
根据本发明的第七方面,提供了一种发光材料,所述发光材料包含上述所述的铝酸锶混合氧化物,或者包含根据本发明的方法生产的铝酸锶混合氧化物。
根据本发明的方法生产的铝酸锶混合氧化物或者如上文所述的铝酸锶混合氧化物可以用于发光材料中。
如上文所述,本发明的不同方面2至7中的任何一个的铝酸锶混合氧化物的特征优选在于,对于通过Hg侵入测得的在和的范围内的空隙半径(介孔区域),孔隙体积小于0.05ml/g,并且对于通过Hg侵入测得的在至的范围内的孔隙半径,孔隙体积在0.7ml/g至1.5ml/g的范围内。这种明显的大孔结构表明铝酸锶混合氧化物的颗粒的海绵状或多孔骨状的微结构。通过扫描电子显微镜(SEM)可以进一步观察到这种结构。
本发明的详细描述
如图1所示,通过扫描电子显微镜(SEM)可以容易地观察到本发明的铝酸锶混合氧化物的海绵状或多孔骨状的微结构。
相比之下,根据常规制陶法制备的铝酸锶混合氧化物的SEM图像(例如,如图2所示)显示了强烈附聚的大颗粒的致密结构。
在不受理论约束的情况下,本发明人认为,本发明的铝酸锶混合氧化物的海绵状或多孔骨状的微结构至少部分地解释了在混合氧化物(例如在磷光剂中)的更有效的研磨行为的方面中实现的益处。
本发明人已经发现,本发明的铝酸锶混合氧化物前体可以在低至900℃的温度下转化为铝酸锶混合氧化物。这是有利的,因为转化在低于常规已知技术的温度下发生。
此外,本发明人已经发现,本发明的铝酸锶混合氧化物具有球形颗粒和海绵状或多孔骨状的微结构,其在研磨处理中易于破碎。因此,通过使用本发明的铝酸锶混合氧化物前体和本发明的铝酸锶混合氧化物(例如用于磷光剂),可提高工艺效率,因为减少了整体能源需求和研磨吞吐时间,同时降低了由强化研磨导致的发光性质的劣化。
所应用的分析方法和参数定义
颗粒尺寸和颗粒尺寸分布:
使用Malvern Mastersizer 2000在水性分散体中应用Fraunhofer理论通过激光散射测量分散介质中的无机颗粒的d50值。d表示直径。所测量的颗粒基本上不包括附聚颗粒。
晶体尺寸:
通过Scherrer法使用X射线粉末衍射图谱中的(021)反射确定勃姆石的晶体尺寸。
表面积:
在液氮温度下使用典型的体积测量装置(例如来自Quantachrome的Quadrasorb)通过N2物理吸附测量BET表面积和孔隙体积。使用Brunauer–Emmett–Teller(BET)法(DINISO 9277:2003-05)确定表面积。
孔隙体积和孔隙半径:
使用Barrett、Joyner和Halenda(BJH)提供的方法在77K下通过Hg侵入测量本文提供的孔隙体积和孔隙半径。
根据DIN 66133使用来自Micromeritics的Porosimeter Autopore IV 9500通过汞侵入确定孔径分布。孔径提供为半径。
通过FEI Phenom设备在背散射电子模式下拍摄SEM图片。在测量之前,用金溅射样品。
如ISO 13322-2(2006)所述,使用来自Retsch的Camsizer P4通过动态图像分析确定基于体积的球度(也称为短球度)。使用以下等式根据所测量的周长P和颗粒投影的面积A计算球度(SPHT3)。
所确定的值是无量纲的,并且对于理想的球体(也称为“球形”),其为1,并且对于非理想球体的球形颗粒,其通常小于1。在当前情况下,球度为约0.9。
通过SEM可以看到球形以及海绵状或多孔骨状的结构。
附图说明
现将参考以下非限制性实施例和附图描述本发明,在附图中:
图1为根据实施例1生产的铝酸锶混合氧化物的SEM图像;
图2为根据对比实施例1生产的铝酸锶混合氧化物的SEM图像;
图3为根据对比实施例2生产的铝酸锶混合氧化物的SEM图像;
图4为比较实施例1和对比实施例1的孔隙体积和孔隙尺寸的图表;
图5为根据实施例1生产的铝酸锶混合氧化物的相组成的XRD;
图6为显示单斜SrAl2O4与作为根据对比实施例1的产物的副产物的SrAl12O19和Sr3Al2O6的混合物的XRD;以及
图7为比较实施例1和对比实施例1的颗粒尺寸(通过Malvern Mastersizer测得)和研磨时间的图表。
具体实施方式
实施例1
根据本发明的方法生产铝酸锶混合氧化物。混合208.8g的固体含量为7.1%的含勃姆石的悬浮体与在200g的蒸馏水中包含16.3g的乙酸锶和17.2g的SrCO3的溶液。在210℃下水热处理5h之后,在8.5的pH下对悬浮体进行喷雾干燥,以获得铝酸锶混合氧化物前体。在1000℃下煅烧铝酸锶混合氧化物前体3h,以形成铝酸锶混合氧化物。通过SEM和X射线衍射(XRD)分析铝酸锶混合氧化物。
图1清楚地表明铝酸锶混合氧化物的海绵状或多孔骨状的微结构。
图5表明在根据本发明的方法生产的铝酸锶混合氧化物的相组成中存在SrAl2O4。
对比实施例1
根据常规制陶法,在研钵中混合SrCO3和γ-Al2O3(以商品名PURALOX SBa-150商购获得,平均颗粒尺寸(d50)为30μm)的化学计量的混合物,并在1500℃下煅烧3h。
图2显示了通过常规制陶法制备的产物的致密的、高度烧结的特性。通过所测量的孔隙体积证实了材料的高度烧结的特性。如图4所示,对于通过Hg侵入确定的孔隙半径在和之间的孔隙尺寸,孔隙体积小于0.01ml/g,并且对于通过Hg侵入确定的在和之间的孔隙尺寸,孔隙体积同样小于0.01ml/g。
图6显示了单斜SrAl2O4与作为副产物的SrAl12O19和Sr3Al2O6的混合物,表明在1500℃下固态反应仍未完全完成。
研磨测试
将来自实施例1和对比实施例1的材料各自悬浮在水中,直至5重量%的固体含量。在以600rpm操作的ULTRA-TURRAX高剪切混合器中处理每种悬浮体。
在5、10和15分钟之后,通过激光衍射测量每种悬浮体中的固体的颗粒尺寸(d50)。出于比较的目的,在10分钟和15分钟之后测得的d50值参考在5分钟后测得的d50值。
如表1和图7所示,明显的是,实施例1的发明材料在研磨过程中易于破碎,而在这些研磨条件下,未观察到从对比实施例1获得的材料的颗粒减小。
表1
5min | 10min | 15min | ||
实施例1 | 相对d<sub>50</sub> | 100% | 64% | 59% |
对比实施例1 | 相对d<sub>50</sub> | 100% | 102% | 98% |
对比实施例2
根据Kutty等人的Mat.Res.Bull.25,(1990),1355制备铝酸锶。
在60℃下将25重量%NH3的水溶液加入到硫酸铝的水溶液中,以沉淀Al2O3*xH2O凝胶。用水清洗凝胶至不含硫酸盐。该凝胶的X射线粉末衍射分析显示出明显的拟勃姆石特征,其测得的晶体尺寸为1.5nm。
以Al:Sr为2:1的摩尔比混合所述凝胶与通过煅烧SrCO3新鲜制备的SrO。在240℃下水热老化混合物6h。通过过滤分离固体,用水清洗,丙酮干燥,并在1000℃下煅烧3h。
表2示出了获得的孔隙体积
表2
从图3可以看出,颗粒的形状不是球形,并且微结构与海绵骨特征不同。
因此,表明通过Kutty等人描述的方法无法获得本发明中描述的材料性质。
Claims (21)
1.一种制备铝酸锶混合氧化物前体的方法,所述方法包括:
i)提供铝氧化物悬浮体;
ii)向铝氧化物悬浮体中加入锶化合物,以形成Sr-Al悬浮体;
iii)水热处理i)铝氧化物悬浮体、ii)Sr-Al悬浮体、或者iii)铝氧化物悬浮体和Sr-Al悬浮体两者,以获得经水热处理的铝氧化物悬浮体、经水热处理的Sr-Al悬浮体、或者经水热处理的铝氧化物悬浮体和经水热处理的Sr-Al悬浮体两者;以及
iv)干燥经水热处理的Sr-Al悬浮体或者Sr-Al悬浮体,以产生铝酸锶混合氧化物前体。
2.一种铝酸锶混合氧化物前体,其可通过根据权利要求1所述的方法,通过在900℃至1100℃范围内的温度持续在0.5h至5h范围内的时间进一步煅烧铝酸锶混合氧化物前体获得。
3.一种制备铝酸锶混合氧化物的方法,所述方法包括:
i)提供铝氧化物悬浮体;
ii)向铝氧化物悬浮体中加入锶化合物,以形成Sr-Al悬浮体;
iii)水热处理i)铝氧化物悬浮体、ii)Sr-Al悬浮体、或者iii)铝氧化物悬浮体和Sr-Al悬浮体两者,以获得经水热处理的铝氧化物悬浮体、经水热处理的Sr-Al悬浮体、或者经水热处理的铝氧化物悬浮体和经水热处理的Sr-Al悬浮体两者;
iv)干燥经水热处理的Sr-Al悬浮体或者Sr-Al悬浮体,以产生铝酸锶混合氧化物前体;以及
v)煅烧铝酸锶混合氧化物前体,以产生铝酸锶混合氧化物。
4.根据权利要求1或3所述的方法,所述方法包括:
a)根据第一方法:
i)提供铝氧化物悬浮体;
ii)水热处理铝氧化物悬浮体,以获得经水热处理的铝氧化物悬浮体;
iii)向经水热处理的铝氧化物悬浮体中加入锶化合物,以形成锶铝氧化物悬浮体(Sr-Al悬浮体);以及
iv)干燥Sr-Al悬浮体,以产生铝酸锶混合氧化物前体;或者
b)根据第二方法:
i)提供铝氧化物悬浮体;
ii)向铝氧化物悬浮体中加入锶化合物,以形成锶铝氧化物悬浮体(Sr-Al悬浮体);
iii)水热处理Sr-Al悬浮体,以获得经水热处理的Sr-Al悬浮体;以及
iv)干燥经水热处理的Sr-Al悬浮体,以产生铝酸锶混合氧化物前体;或者
c)根据第三方法:
i)提供铝氧化物悬浮体;
ii)水热处理铝氧化物悬浮体,以获得经水热处理的铝氧化物悬浮体;
iii)向经水热处理的铝氧化物悬浮体中加入锶化合物,以形成锶铝氧化物悬浮体(Sr-Al悬浮体);
iv)水热处理Sr-Al悬浮体,以获得经水热处理的Sr-Al悬浮体;以及
v)干燥经水热处理的Sr-Al悬浮体,以产生铝酸锶混合氧化物前体。
5.根据权利要求1、3或4所述的方法,其中,通过在水的存在下将铝氧化物悬浮体、Sr-Al悬浮体或两者加热到100℃至250℃范围内的温度,优选加热到180℃至220℃范围内的温度来进行水热处理,持续时间在0.5h至14h的范围内,优选地持续时间在1h至8h的范围内;优选在5和12之间的pH下,甚至更优选在6和11之间的pH下。
6.根据权利要求1、3、4和5中的一项或多项所述的方法,其中,铝氧化物悬浮体为勃姆石悬浮体,其中勃姆石的晶体尺寸(021和/或020反射)优选在3nm和50nm之间,更优选在3nm和45nm之间。
7.根据权利要求1和3至6中的一项或多项所述的方法,其中,锶化合物为锶盐或锶盐的混合物,优选乙酸锶、硝酸锶、碳酸锶、氯化锶或其混合物。
8.根据权利要求3至7中的一项或多项所述的方法,其中,在900℃至1100℃范围内的温度进行煅烧铝酸锶混合氧化物前体以产生铝酸锶混合氧化物,持续时间在0.5h至5h的范围内。
9.根据权利要求1和3至8中的一项或多项所述的方法,其中,铝氧化物悬浮体的特征还在于以下一项或多项:
a)铝氧化物悬浮体为水性悬浮体;
b)铝氧化物悬浮体的固体含量可以在1重量%至30重量%的范围内,优选在3重量%至15重量%的范围内;和/或
c)铝氧化物悬浮体中的铝氧化物的平均颗粒尺寸(d50)在0.01μm至100μm的范围内。
10.一种根据权利要求1和3至9中的一项或多项生产的铝酸锶混合氧化物,其中,铝酸锶混合氧化物的特征还优选在于颗粒具有海绵状或多孔骨状的结构。
11.根据权利要求10所述的铝酸锶混合氧化物,其中,所述铝酸锶混合氧化物为SrAl2O4、SrAl4O7、Sr3Al2O6、SrAl12O19、Sr4Al14O25或其混合物,优选SrAl2O4。
14.根据权利要求10至13中的一项或多项所述的铝酸锶混合氧化物,其中,铝酸锶混合氧化物的颗粒尺寸在1μm至150μm的范围内,优选在5μm和150μm之间。
15.根据权利要求10至14中的一项或多项所述的铝酸锶混合氧化物,其中,所述铝酸锶混合氧化物具有基本上球形的颗粒。
16.根据权利要求10至15中的一项或多项所述的铝酸锶混合氧化物,其中,铝酸锶混合氧化物掺杂有活化剂,所述活化剂优选为稀土金属或稀土金属氧化物,更优选为Eu和Dy。
17.根据权利要求11至16中的一项或多项所述的铝酸锶混合氧化物,其中,所述铝酸锶混合氧化物的BET表面积小于20m2/g。
19.根据权利要求18所述的铝酸锶混合氧化物,其中,所述铝酸锶混合氧化物为SrAl2O4、SrAl4O7、Sr3Al2O6、SrAl12O19、Sr4Al14O25或其混合物,优选SrAl2O4。
20.根据权利要求18或19所述的铝酸锶混合氧化物,其中,铝酸锶混合氧化物掺杂有活化剂,所述活化剂优选为稀土金属或稀土金属氧化物,更优选为Eu和Dy两者。
21.一种发光材料,所述发光材料包含根据权利要求8至20中的一项或多项所述的铝酸锶混合氧化物。
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