CN112094110A - 一种Al2O3-YAG:Ce3+复相荧光陶瓷的制备方法 - Google Patents
一种Al2O3-YAG:Ce3+复相荧光陶瓷的制备方法 Download PDFInfo
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- 229910052782 aluminium Inorganic materials 0.000 title abstract description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title abstract description 4
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 claims abstract description 23
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 6
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- 229910000420 cerium oxide Inorganic materials 0.000 claims description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 6
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
一种Al2O3‑YAG:Ce3+复相荧光陶瓷的制备方法，该方法适用于制备x wt％ Al2O3‑(Y1‑yCey)3Al5O12的复相荧光陶瓷，其中0.01≤x＜100，0.0001≤y≤0.1。具体制备方法为：按照x wt％ Al2O3‑(Y1‑yCey)3Al5O12组份配置好原料，加入0.4wt％的正硅酸乙酯作为添加剂，粉料经过球磨、烘干、单轴压片后，对其施加200MPa以上冷等静压压制成坯体，再预烧去除有机成分；最后放入管式炉或箱式炉中进行常压烧结，得到Al2O3‑YAG:Ce3+复相荧光陶瓷。本发明制备的Al2O3‑YAG:Ce3+复相荧光陶瓷具有高热导率、高量子效率和合适的透过率，制备方法具有制备工艺简单、低成本以及制备过程无毒害等优点。
Description
技术领域
本发明属于化工领域，涉及一种复相荧光陶瓷的制备方法，具体来说是一种Al2O3-YAG:Ce3+复相荧光陶瓷的低成本制备方法。
背景技术
随着人们对航空航天、投影显示、汽车大灯等超大功率超高亮度照明领域的不断需求，新一代的激光照明技术应运而生。在激光照明中，荧光陶瓷体在高电流密度下工作仍有高的转换效率，保证了照明光源的高效性及光色的稳定性。
YAG:Ce3+荧光材料因其高量子效率等特性被选作为荧光转换材料，为了获得更高的热导率，需要对YAG:Ce3+荧光陶瓷进行改性。作为用途最广泛的陶瓷之一，Al2O3因其高导热率备受研究人员的关注。
一些研究人员制备了Al2O3-YAG:Ce3+复相荧光陶瓷，并对他们的微观结构、物相组成和发光性能进行了研究，证明了其在激光照明中具有较高的热导率和流明效率。不过，现有Al2O3-YAG:Ce3+复相荧光陶瓷的制备方法同城需要真空烧结、热压烧结等要求高、价格昂贵的无压或压力烧结设备，这在很大程度上提高了陶瓷发光材料的制备成本，严重限制了陶瓷荧光粉的商业竞争力。本发明提供了一种在流动氧气氛中通过固相反应烧结制备Al2O3-YAG:Ce3+复相荧光陶瓷的简便、低成本制备方法。
发明内容
针对现有技术中的上述技术问题，本发明提供了一种Al2O3-YAG:Ce3+复相荧光陶瓷的低成本制备方法，本发明制备的复相荧光陶瓷高热导率、高量子效率和合适的透过率，制备方法具有制备工艺简单、低成本以及制备过程无毒害等优点。
一种Al2O3-YAG:Ce3+复相荧光陶瓷的制备方法，该方法适用于制备x wt％Al2O3-(Y1-yCey)3Al5O12的复相荧光陶瓷，其中0.01≤x≤100，0.0001≤y≤0.1。具体制备方法为：按照x wt％Al2O3-(Y1-yCey)3Al5O12组份配置好原料，加入0.4wt％的正硅酸乙酯作为添加剂，粉料经过球磨、烘干、单轴压片后，对其施加200MPa以上冷等静压压制成坯体，再预烧去除有机成分；最后放入管式炉或箱式炉中进行常压烧结，得到Al2O3-YAG:Ce3+复相荧光陶瓷。本发明制备的Al2O3-YAG:Ce3+复相荧光陶瓷具有高热导率、高量子效率和合适的透过率，制备方法具有制备工艺简单、低成本以及制备过程无毒害等优点。
上述的一种Al2O3-YAG:Ce3+复相荧光陶瓷的制备方法，包括如下步骤：
(1)初始原料采用原料纯度不低于99.99％的氧化铈、氧化钇、氧化铝的粉体；
(2)根据需要制备的复相荧光陶瓷的分子式x wt％Al2O3-(Y1-yCey)3Al5O12的组成确定x，y的取值，并按摩尔比称量相应的粉体原料，加入0.4wt％的正硅酸乙酯作为添加剂，经球磨将粉料混匀、细化；
(3)粉料烘干后经造粒、单轴压片，对其施以200MPa以上冷等静压压制成坯体，再预烧去除有机成分；
(4)最后放入管式炉或箱式炉中进行常压烧结，得到Al2O3-YAG:Ce3+复相荧光陶瓷。常压烧结过程中，管式炉或箱式炉的保温温度为1200℃～1800℃，保温时间为5小时。
本发明的技术效果：
该Al2O3-YAG:Ce3+复相荧光陶瓷制备工艺比较简单，成品率高，成本低，易批量制备，且其在制备过程中无需使用对人体环境有毒害的助熔剂，具有良好的人体、环境友好性。
附图说明
图1为采用荧光光谱仪对实施例1所得10wt％Al2O3-(Y0.9834Ce0.0166)3Al5O12复相荧光陶瓷材料在450nm蓝光激发下的发光光谱。
图2为采用荧光光谱仪对实施例1所得10wt％Al2O3-(Y0.9834Ce0.0166)3Al5O12复相荧光陶瓷材料在450nm蓝光激发下检测波长为550nm时的荧光寿命。
图3为采用荧光光谱仪对实施例2所得10wt％Al2O3-(Y0.9834Ce0.0166)3Al5O12复相荧光陶瓷材料在450nm蓝光激发下的发光光谱。
图4为采用荧光光谱仪对实施例2所得10wt％Al2O3-(Y0.9834Ce0.0166)3Al5O12复相荧光陶瓷材料在450nm蓝光激发下检测波长为550nm时的荧光寿命。
具体实施方式
为了进一步理解本发明，下面结合实施例对本发明优选实施方案进行描述，但是应当理解，这些描述只是为进一步说明本发明的特征和优点，而不是对本发明权利要求的限制。
实施例1
初始原料采用原料纯度不低于99.99％的氧化铈(化学式:CeO2)、氧化钇(化学式:Y2O3)和氧化铝(化学式:Al2O3)的粉体；
根据需要制备的复相荧光陶瓷的分子式10wt％Al2O3-(Y0.9834Ce0.0166)3Al5O12的组成并确定x＝10，y＝0.0166的取值,纯度不低于99.99％的氧化铈(化学式:CeO2)、氧化钇(化学式:Y2O3)和氧化铝(化学式:Al2O3)的粉末为原料，按照组分中各离子的摩尔比相应的配置好分体原料共30g，加入0.4wt％的正硅酸乙酯作为添加剂，经球磨将粉料混匀、细化；
粉料烘干后经造粒、单轴压片，对其施以200MPa以上冷等静压压制成坯体，再预烧去除有机成分；
最后放入管式炉或箱式炉中进行常压烧结，得到10wt％Al2O3-(Y0.9834Ce0.0166)3Al5O12复相荧光陶瓷：
常压烧结：管式炉或箱式炉的保温温度为1600℃，保温时间为5小时。
采用荧光光谱仪，测试本发明实施例1制备得到的复相陶瓷在450nm蓝光激发下的发射光谱，测试结果如图1所示。
由图1可知，本发明实施例1制备得到的Al2O3-YAG:Ce3+复相荧光陶瓷在蓝光激发下可产生黄光宽带发射，发光峰位在550nm左右。
采用荧光光谱仪，测试本发明实施例1制备得到的复相陶瓷在450nm蓝光激发下监测波长为550nm时的荧光寿命，测试结果如图2所示。
由图2可知，本发明实施例1制备得到的Al2O3-YAG:Ce3+复相荧光陶瓷的荧光寿命可以通过单指数函数完美拟合：
y(t)＝A+B1*exp(-t/τ1)
其中，y(t)指的是荧光粉在时间t时的荧光发射强度；A、B1和τ1都是常数；τ1代表的就是荧光粉的荧光寿命。根据拟合结果，Al2O3-YAG:Ce3+复相荧光陶瓷的荧光寿命为81.01ns。
实施例2
初始原料采用原料纯度不低于99.99％的氧化铈(化学式:CeO2)、氧化钇(化学式:Y2O3)和氧化铝(化学式:Al2O3)的粉体；
根据需要制备的复相荧光陶瓷的分子式10wt％Al2O3-(Y0.9834Ce0.0166)3Al5O12的组成并确定x＝10，y＝0.0166的取值,纯度不低于99.99％的氧化铈(化学式:CeO2)、氧化钇(化学式:Y2O3)和氧化铝(化学式:Al2O3)的粉末为原料，按照组分中各离子的摩尔比相应的配置好分体原料共30g，加入0.4wt％的正硅酸乙酯作为添加剂，经球磨将粉料混匀、细化；
粉料烘干后经造粒、单轴压片，对其施以200MPa以上冷等静压压制成坯体，再预烧去除有机成分；
最后放入管式炉或箱式炉中进行常压烧结，得到10wt％Al2O3-(Y0.9834Ce0.0166)3Al5O12复相荧光陶瓷：
常压烧结：管式炉或箱式炉的保温温度为1780℃，保温时间为5小时。
采用荧光光谱仪，测试本发明实施例2制备得到的复相陶瓷在450nm蓝光激发下的发射光谱，测试结果如图3所示。
由图3可知，本发明实施例2制备得到的Al2O3-YAG:Ce3+复相荧光陶瓷在蓝光激发下可产生黄光宽带发射，发光峰位在550nm左右。
采用荧光光谱仪，测试本发明实施例2制备得到的复相陶瓷在450nm蓝光激发下监测波长为550nm时的荧光寿命，测试结果如图4所示。
由图4可知，本发明实施例2制备得到的Al2O3-YAG:Ce3+复相荧光陶瓷的荧光寿命可以通过单指数函数完美拟合：
y(t)＝A+B1*exp(-t/τ1)
其中，y(t)指的是荧光粉在时间t时的荧光发射强度；A、B1和τ1都是常数；τ1代表的就是荧光粉的荧光寿命。根据拟合结果，Al2O3-YAG:Ce3+复相荧光陶瓷的荧光寿命为75.13ns。
综上，该方法具有材料制备成本低、制备工艺简单，适于大规模工业生产等优点，上转换发光材料领域具有重要应用。
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以对本发明进行若干改进和修饰，这些改进和修饰也落入本发明权利要求的保护范围内。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (1)
1.本发明提供了一种Al2O3-YAG:Ce3+复相荧光陶瓷的制备方法，该方法适用于制备xwt％Al2O3-(Y1-yCey)3Al5O12的复相荧光陶瓷，其中0.01≤x≤100，0.0001≤y≤0.1；该复相陶瓷制备方法的具体步骤如下：
(1)初始原料采用原料纯度不低于99.99％的氧化铈、氧化钇、氧化铝的粉体；
(2)根据需要制备的复相荧光陶瓷的分子式x wt％Al2O3-(Y1-yCey)3Al5O12的组成确定x，y的取值，并按摩尔比称量相应的粉体原料，加入0.4wt％的正硅酸乙酯作为添加剂，经球磨将粉料混匀、细化；
(3)粉料烘干后经造粒、单轴压片，对其施以200MPa以上冷等静压压制成坯体，再预烧去除有机成分；
(4)最后放入管式炉或箱式炉中进行常压烧结，得到Al2O3-YAG:Ce3+复相荧光陶瓷。常压烧结过程中，管式炉或箱式炉的保温温度为1200℃～1800℃，保温时间为0.5～72小时。
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