CN108774517A - 一种氧化铝-氧化镁复合材料及制备方法 - Google Patents

一种氧化铝-氧化镁复合材料及制备方法 Download PDF

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CN108774517A
CN108774517A CN201810479976.XA CN201810479976A CN108774517A CN 108774517 A CN108774517 A CN 108774517A CN 201810479976 A CN201810479976 A CN 201810479976A CN 108774517 A CN108774517 A CN 108774517A
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CN108774517B (zh
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于立新
郭琪煌
满孝琴
钟检林
高震宇
邹颖璇
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Tianjin Zexi New Material Co ltd
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Nanchang University
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Abstract

一种氧化铝‑氧化镁复合材料及制备方法,各组分及摩尔百分比为Al2O3:0‑98.04%,MgO:0‑98.04%,Eu2O3:1.96%。制备方法:(1)按照配比称取原料,将Eu2O3、MgO、Al2O3置于玛瑙研钵中,充分研磨一后得到混合均匀的粉末,倒入干燥,清洁的刚玉坩埚中;(2)将以上装有混合均匀粉末的刚玉坩埚置于马弗炉中,在空气气氛中进行1200‑1350oC的高温固相反应,烧结10‑12h,待炉冷却至900oC时立即取出冷却至室温。本发明操作简单、原料来源广泛、成本低廉、无毒无污染、产物物理化学性能稳定。该产品具有发光稳定高效,在紫外具有有效的吸收。

Description

一种氧化铝-氧化镁复合材料及制备方法
技术领域
本发明属于固体发光材料领域。
背景技术
稀土掺杂材料由于其独特的发光特性,和巨大的应用潜力引起了科研人员的广泛关注。Eu2+是重要的低价稀土离子,其在近紫外区有4f→5d宽带吸收(300-500 nm,不同基质中吸收范围可以移动),可以很好的与近紫外LED芯片匹配;由于二价的铕的发射为f-d跃迁,对于基质和结构极其敏感,这意味着其发光颜色可以实现有效调控。Eu3+主要发射波长为589 nm和620 nm左右的窄带橙红光。如果在基质同时存在Eu2+和Eu3+,并调制Eu2+/Eu3+的相对比例和相对发射强度,可以实现发光颜色的有效调控,这种荧光体在LED的领域具有潜在的应用前景。在空气中实现三价铕还原为二价铕易于量产,且安全环保。近年来以Al2O3为基质的Eu掺材料被广泛研究,其制备方法主要有高温固相法、溶胶-凝胶法、溶剂蒸发、共沉淀法等,但在实际生产过程中也存在着一定的缺陷,如制备设施昂贵、反应不充分、无法量产,及制备所需的还原性气体的安全问题等。因此找出一种高效安全,还能够大量生产的制备方法是具有研究价值的。
发明内容
本发明目的是提出一种具有高效蓝/红光发射的Eu2+-Eu3+激活Al2O3-MgO复合材料的制备方法。
本发明是通过以下技术方案实现的。
本发明所述的一种氧化铝-氧化镁复合材料复合材料,各组分及其摩尔百分比(mol%)为Al2O3:0-98.04%,MgO:0-98.04%,Eu2O3:1.96%。
本发明所述的复合材料的制备方法,采用自还原法制备,通过控制掺杂基质中Al2O3和MgO相对的比例,控制稀土离子相对含量进而改变发光颜色,包括如下步骤。
(1)复合材料配料的混合。
按照配比称取原料,将Eu2O3、MgO、Al2O3置于玛瑙研钵中,充分研磨一后得到混合均匀的粉末,倒入干燥,清洁的刚玉坩埚中。
(2)复合材料的烧结。
将以上装有混合均匀粉末的刚玉坩埚置于马弗炉中,在空气气氛中进行1200-1350oC的高温固相反应,烧结10-12h,待炉冷却至900oC时立即取出冷却至室温。
本发明所述的氧化物Al2O3、MgO皆为分析纯,稀土离子Eu3+选择纯度为99.99%的氧化物Eu2O3
本发明的有益效果是: (1) 本发明的制备工艺简单、原材料丰富且成本低廉,无毒无污染,产物物化性能稳定,退火温度低; (2)本发明制备的Eu2+-Eu3+激活的Al2O3-MgO复合材料,具有高效稳定的发光,在紫外具有有效的吸收,有望广泛应用。
附图说明
图1为实施例1-4中荧光材料样品的X射线衍射图。
图2为实施例1-4中荧光材料样品在325纳米紫外激发下的发射光谱。
图3为实施例1-4中荧光材料样品在395纳米紫外激发下的发射光谱。
具体实施方式
本发明将通过以下实施例作进一步说明。
实施例1-4按如下步骤制备用稀土掺杂的Al2O3-MgO复合材料。
(a)原料的选取。
该复合材料的主要原料均为分析纯的Al2O3、MgO,稀土离子Eu3+选择纯度为99.99%的氧化物Eu2O3
(b)配合料的混合。
精确地按照配比称取原料,按照配比称取原料,将Al2O3、MgO、Eu2O3,置于玛瑙研钵中,充分研磨20-30min使其碾成混合均匀的粉末,再将其倒入干燥洁净的刚玉坩埚中,并密封,防止杂质混入。
(2)玻璃的烧结。
将以上装有混合均匀粉末的刚玉坩埚置于马弗炉中,在空气气氛中进行1200-1350oC的高温固相反应,烧结10-12h,待炉冷却至900oC时立即取出冷却至室温。
实施例1。
按照摩尔百分比(mol%)为Eu2O3:1.96%,Al2O3:0%,MgO:98.04%,的比例称取原料。各原料质量如表1所示,该实施例高温固相反应温度为1300℃。X射线衍射结果(如图1所示)。经过研磨成粉末,用F-4600荧光分光光度计测量其室温发射谱(如图2图3所示)。在325纳米近紫外光激发下,检测到Eu2+在409nm处,Eu3+在630nm处均较强的发射。证明其发射有多种颜色组合而成。
表1 实施例1的玻璃组成
原料 Eu2O3 Al2O3 MgO
实施例1 0.17464 0 1.00000
实施例2。
按照摩尔百分比(mol%)为Eu2O3:1.96%,Al2O3:98.04%,MgO:0%的比例称取原料,将高温固相反应温度设置为1300oC。X射线衍射结果(如图1所示)。用F-4600荧光分光光度计测量其室温发射谱(如图2所示)在325纳米近紫外光激发下,探测到Eu2+和Eu3+的发射,且其发射有多种颜色组合而成。
实施例3。
按照摩尔百分比(mol%)为Eu2O3:1.96%,Al2O3:32.68%,MgO:65.36%的比例称取原料,将高温固相反应温度设置为1300oC。X射线衍射结果(如图1所示)。用F-4600荧光分光光度计测量其室温发射谱(如图2所示)在325纳米近紫外光激发下,探测到Eu2+和Eu3+的发射,且其发射有多种颜色组合而成。
实施例4。
按照摩尔百分比(mol%)为Eu2O3:1.96%,Al2O3:19.61%,MgO:78.43%的比例称取原料,将高温固相反应温度设置为1300oC。X射线衍射结果(如图1所示)。用F-4600荧光分光光度计测量其室温发射谱(如图2所示)在325纳米近紫外光激发下,探测到Eu2+和Eu3+的发射,且其发射有多种颜色组合而成。

Claims (3)

1.一种氧化铝-氧化镁复合材料,其特征是各组分及其摩尔百分比为Al2O3:0-98.04%,MgO:0-98.04%,Eu2O3:1.96%。
2.权利要求1所述的复合材料的制备方法,其特征是包括如下步骤:
(1)按照配比称取原料,将Eu2O3、MgO、Al2O3置于玛瑙研钵中,充分研磨一后得到混合均匀的粉末,倒入干燥,清洁的刚玉坩埚中;
(2)将以上装有混合均匀粉末的刚玉坩埚置于马弗炉中,在空气气氛中进行1200-1350oC的高温固相反应,烧结10-12h,待炉冷却至900oC时立即取出冷却至室温。
3.根据权利要求2所述的复合材料的制备方法,其特征是所述的氧化物Al2O3、MgO为分析纯,Eu2O3纯度为99.99%。
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CN106433628A (zh) * 2016-08-30 2017-02-22 南昌大学 一种Eu掺杂的高效蓝光发射的铝硅酸盐荧光材料及制备方法

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