CN110205120A - 一种近紫外激发的混合物红色荧光粉、制备方法及应用 - Google Patents
一种近紫外激发的混合物红色荧光粉、制备方法及应用 Download PDFInfo
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- A01G7/00—Botany in general
- A01G7/04—Electric or magnetic or acoustic treatment of plants for promoting growth
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Abstract
本发明涉及发光材料无机合成技术领域,具体涉及一种近紫外激发的混合物红色荧光粉、制备方法及其应用此混合物主要是由两种成分构成,即:MgAl2O4和CaAl12O19:Mn4+。本发明的采用高温固相法或化学合成法,制备得到一种铝酸盐混合物红色荧光粉,其混合比为:MgAl2O4/CaAl12O19:Mn4+=x/1,其中0≤x≤3;该红色荧光粉在近紫外光线的蓝光的激发下,能发射出峰值在658nm的红光,且亮度高,纯度好,物理化学性能稳定,对环境友好。可用于近紫外激发的三基色白光LED和植物LED灯中的红粉;也可以用于植物工厂或温室顶层中转光玻璃与转光薄膜。
Description
技术领域
本发明涉及发光材料无机合成技术领域,特别涉及一种近紫外激发的红色荧光粉、制备方法及其应用。
背景技术
发光二极管(light emitting diodes, LEDs)是本世纪最有前景的固态光源,已广泛用于道路照明、室内照明、灯光装饰,交通、平板显示等领域。考虑到经济效益,目前已商业化的白光LED主要是在发蓝光的InGaN芯片敷上黄色YAG:Ce荧光粉而成,使其发出的黄光与部分透射出的蓝光混合并互补产生白光。但这种白光LED发出的光由于缺少了红光的成分,造成色温偏高,显色指数低,限制其更广阔的应用领域。而由激发近紫外光的LED芯片敷上红、黄、蓝三基色荧光粉而成的白光LED,可以克服上述缺点,得到显色指数高、色温可调,热稳定性好,易于控制等优点的白光LED, 从而受到广泛的关注和大量的研究。而相对于蓝粉和黄粉,红粉仍然存在较大的挑战,如,已商业化的Y2O2S:Eu3+等硫化物红粉,存在着在大气中物化性质不稳定的问题;而氮化物、氮氧化物红粉,虽然物化性能稳定,发光效率也高,但需要在保护气氛中,在条件苛刻的高温下才能完成,大大增加成本。
另外,众所周知,植物并不是对整个太阳光谱都均匀吸收,植物吸收光能进行光合作用时,叶绿素a 和b 对光的吸收占绝大部分。在叶绿素a 和b 的吸收光谱中,吸收峰大概在430nm~460nm和630nm~680nm之间,即植物对蓝光和红光部分有两个很强的吸收峰值。因此,为了达到人工光源利用的最大化及植物的健康、茁壮成长的需求,研究能发射出与植物光合作用匹配的红光和蓝光的LEDs具有十分重要的意义。这种植物成长LED灯也同样需要高性能、低成本的红色荧光粉。
为此,寻找一种能被近紫外光有效激发,发光效率高,在大气中具有良好的稳定性,不会对周围环境产生不良影响的、成本较低的红色荧光粉变成十分有必要。首先,在发光离子方面,已有报道,Mn4+在合适的基质中也能发出高量子效率的红光,而且相对于稀土离子,材料成本较低。在众基质中,铝酸盐体系的性能较为突出,特别是作为红色荧光粉,有着优异的性能,主要表现在如下几个方面:1) 具有非常好的物理化学稳定性;2)在近紫外光波段(<400nm)存在较强的吸收;3)铝酸盐资源丰富,具有价格上的优势;4)环境友好等。
因此,如何制备出四价锰掺杂的铝酸盐基质发光效率高的成对近紫外光有效吸收的红色荧光粉,一直是人们关注的问题。
发明内容
针对上述情况,本发明的目的是提供一种锰掺杂的、发光效率高、性能稳定、环境友好、成本低且能被近紫外线激发的混合物红色荧光粉。
所述荧光粉是由MgAl2O4(缩写:MA)和CaAl12O19:Mn4+(缩写:CA)组成,其混合物配比为:MgAl2O4/CaAl12O19:Mn4+=x/1,其中0≤x≤3。所述的红色荧光粉在近紫外光线激发下,能发射出峰值约在658nm的红光。
本发明还提供了的制备方案为高温固相法。
所述荧光粉采用高温固相法制备,包括以下步骤:
(1)按混合物配比为:MgAl2O4/CaAl12O19:Mn4+=x/1分别称取含镁的化合物原料、含钙的化合物原料、含铝的化合物原料和含锰的化合物原料;
(2)将步骤(1)称取的原料混合在一起研磨30min后在氧化性气氛中预烧,以5℃/min的速度升温度到900℃,保持2~4小时;
(3)将步骤(2)预煅烧后的样品取出,研磨均匀后在氧化性气氛中煅烧,以3℃/min的速度升温到1100~1500℃,保持4~6小时,冷却后得到所述近紫外激发的红色荧光粉。
进一步,所述铝的化合物为氧化铝;所述的含钙的化合物为CaO、CaCO3、Ca(NO3)2中的一种;所述的含镁的化合物为MgO、MgCO3、Mg(NO3)2中的一种;所述的含锰的化合物为MnO、MnCO3、Mn(NO3)2中的一种。
进一步,步骤(2)、(3)中所述的氧化性气氛为空气或氧气气氛。
本发明所述的近紫外激发的荧光粉,可用于三基色(红,蓝,绿)白光LED中的红粉;植物工厂或温室中用于补光的植物LED灯中的红粉;也可以用于植物工厂或温室顶层中转光玻璃与转光薄膜荧光粉,以增强植物生长所必需的红光成份。
现有技术相比,本发明技术方案的优点在于:
1、本发明制备的锰离子掺杂的铝酸盐基质混合物荧光粉具有很好的化学稳定性和热稳定性,能在近紫外有效激发,发光效率高,可以作为白光LED和植物成长LED灯中荧光粉,还可以用于温室顶层玻璃中的转光粉。
2、本发明提供的红色荧光粉原料来源广,制备工艺简单,易操作,不需要保持气氛,可有效地降低成本。
3、本发明提供的红色荧光粉色坐标接近美国国家电视委员会(NTSC)的标准值,红光纯正,样品结晶性好,重复性好,无废水废气排放,环境友好,适合连续性生产。
附图说明
图1为所制备的红色荧光粉在319nm波长激发时的发射谱及在658nm监测的激发谱。图2为本发明所述的红色荧光粉xMgAl2O4/CaAl12O19:Mn4+混合物不同配比时(0≤x≤3)的X射线粉末衍射图谱。
图3 为所制备的红色荧光粉xMgAl2O4/CaAl12O19:Mn4+混合物不同配比时(0≤x≤3)的发光强度的变化趋势。
具体实施方式
实施实例1
用固相反应法制备2MgAl2O4/CaAl12O19:Mn4+混合物红色荧光粉。
根据化学式MgAl2O4/CaAl11.92O19:0.08Mn4+=2/1各元素的化学配比,分别称取0.7699克的碳酸钙,6.2431克的氧化铝,0.62克的氧化镁,0.0707碳酸锰和0.1541克的硼酸作为助熔剂。在玛瑙研钵中研磨并混合均匀后,选择在空气气氛中预煅烧3小时,温度为900℃,升温速率为5℃/min,自然冷后取出样品。将第一次预煅烧后的样品再次研磨混合均匀,在空气氛中再次煅烧,以3℃/min的速度升温到温度为1400℃,煅烧4小时,然后冷却至室温,就得到所述的2MgAl2O4/CaAl12O19:Mn4+混合物红色荧光粉。
参见附图1,它是所制备的红色荧光粉在319nm波长激发时的发射谱(右边)及在658nm监测的激发谱(左边)。说明该荧光粉能在近紫外线上高效激发,并发射出颜色纯正的红光。
实施例2
与实施例1类似,其区别在于:按组合配比通式xMgAl2O4/CaAl11.92O19:0.08Mn4+(x=0,0.1, 0.2,0.5,1,2和3),所得到荧光粉的发射谱与实施例1相似。
参见附图2,其为按本实施例技术方案制备的荧光粉在xMgAl2O4/CaAl12O19:Mn4+混合物不同配比时(0≤x≤3)的X射线粉末衍射图谱,XRD测试结果表明,所制备的荧光粉材料为MgAl2O4 (缩写:MA)和CaAl12O19:Mn4+(缩写:CA)混合相。
参见附图3,其为按本实施例技术方案制备的红色荧光粉xMgAl2O4/CaAl12O19:Mn4+混合物不同配比时(0≤x≤3)的发光强度的变化趋势。图中容易看出,开始随着MgAl2O4比例的增加发光强度有明显的加强,当x=2时达到最大值,再继续增加,强度反而减小,最佳配比为MgAl2O4/CaAl12O19:Mn4+=2/1. 说明此混合物荧光粉比单相的CaAl12O19:Mn4+发光强度有较大的改善。
以上所述,仅为本发明的较佳实施例而已,故不能依此限定本发明实施的范围,即本发明专利范围及说明书内容所作的等效变化与修饰,皆应仍属本发明涵盖的范围内。
Claims (5)
1.一种近紫外激发的混合物红色荧光粉,其特性于:其混合物主要是由两种成分构成,即:MgAl2O4和CaAl12O19:Mn4+;其组合配比的通式为:MgAl2O4/CaAl12O19:Mn4+=x/1,其中0≤x≤3;所述的红色荧光粉在近紫外光的激发下,能发射出峰值在658nm的红光。
2.根据权利要求1所述的一种近紫外激发的红色荧光粉,其特征在于:所述红色荧光粉采用高温固相法来制备,包括以下步骤:
(1)按组合配比通式MgAl2O4/CaAl12O19:Mn4+=x/1分别称取含镁的化合物原料、含钙的化合物原料、含铝的化合物原料和含锰的化合物原料;
(2)将步骤(1)称取的原料混合在一起研磨30Min后在氧化性气氛中预烧,以5℃/min的速度升温度到900℃,保持2~4小时;
(3)将步骤(2)预煅烧后的样品取出,研磨均匀后在氧化性气氛中煅烧,以3℃/min的速度升温度到1100~1500℃,保持4~6小时,冷却后得到所述近紫外激发的红色荧光粉。
3.根据权利要求2所述的一种近紫外激发的红色荧光粉,其特征在于:步骤(2)、(3)中所述的氧化性气氛为空气或氧气气氛。
4.根据权利要求2所述的一种近紫外激发的红色荧光粉,其特征在于:所述铝的化合物为氧化铝;所述的含钙的化合物为CaO、CaCO3、Ca(NO3)2中的一种;所述的含镁的化合物为MgO、MgCO3、Mg(NO3)2中的一种;所述的含锰的化合物为MnO、MnCO3、Mn(NO3)2中的一种。
5.根据权利要求1所述的红色荧光粉的应用,其特征在于:所述红色荧光粉用于制造白光LED中的红粉,植物成长灯中的红粉及温室或植物工厂中的转光玻璃。
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