CN111286328A - 一种稀土掺杂铋层状结构半导体上转换发光材料及其制备方法 - Google Patents
一种稀土掺杂铋层状结构半导体上转换发光材料及其制备方法 Download PDFInfo
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Abstract
本发明公开一种稀土掺杂铋层状结构半导体上转换发光材料及其制备方法,属于稀土发光材料领域。本发明光学器件的化学通式为Ca1‑x‑ yYbxREyBiNb2O9,其中RE为稀土元素Ho、Tm或Tb;x=0.01~0.1,0.01≤x≤0.1,y=0.005~0.05,0.01≤y≤0.05。该材料在近红外激光照射下,展现出强烈的绿光或蓝光发射。该上转换发光材料物理化学性质稳定,合成方法简单易操作、成本低、发光性能良好,在照明、显示、太阳能电池、温度传感及光电多功能器件方面具有良好的应用前景。
Description
技术领域
本发明涉及一种稀土掺杂铋层状结构半导体上转换发光材料及其制备方法,属于稀土发光材料领域。
背景技术
近年来,稀土掺杂上转换发光材料由于其在照明、显示、太阳能电池、温度传感及光电多功能器件方面具有良好的应用前景,得到了广泛的关注。目前上转换发光材料多采用氟化物、硫化物和氯化物等基质,但这些材料热稳定性差较差,容易潮解,且制备工艺复杂,在一定程度上限制了上转换发光材料在很多领域的应用。开发新型优良的多功能稀土掺杂上转换发光材料具有重要意义。
最近,半导体氧化物与稀土离子的结合已成为一类新型材料,在许多领域具有巨大的应用潜力潜力,例如显示器、照明和生物医学成像。CaBi2Nb2O9是一种典型的钙钛矿型铋层状结构半导体材料,由类钙钛矿层(CaNb2O7)2-和(Bi2O2)2+层有规律的交替排列而成,具有优良的热稳定性和化学性质、居里温度高等优点,近年来在高温压电传感等领域被广泛研究。此外,CaBi2Nb2O9带隙大,声子能量较低,兼具半导体结构易于调控从而实现调控稀土离子发光性能的特点,有望成为一种理想的发光材料基质。但是目前对稀土掺杂CaBi2Nb2O9层状半导体发光性质的研究却相对较少,其层状结构对稀土离子的作用机理尚不清楚。
发明内容
本发明目的在于提供一种稀土掺杂铋层状结构半导体上转换发光材料,其化学通式为:Ca1-x-yYbxREyBi2Nb2O9,其中RE为稀土元素Ho、Tm或Tb;x=0.01~0.1,y=0.005~0.05,该材料制备工艺简单且成本低,具有良好的发光性能。
本发明的另一目的在于提供所述稀土掺杂铋层状结构半导体上转换发光材料的制备方法,本发明采用高温固相法制备,具体步骤如下:
(1)根据化学计量比分别称量高纯Bi2O3、CaCO3、Nb2O5、Yb2O3、稀土氧化物,所有原料纯度均大于等于99.5%;其中,稀土氧化物为Ho2O3、Tm2O3或Tb4O7,置于(玛瑙)研钵中,加入分散剂研磨,使原料充分混合均匀后烘干。
(2)将烘干后的原料置于(氧化铝)坩埚中,放入马弗炉中在800~950℃条件下预烧1~3h,然后在空气气氛下1000-1150℃下烧结2~5h;冷却至室温,将烧结好的样品再次研磨,即可得到化学式为Ca1-x-yYbxREyBi2Nb2O9的稀土离子掺杂铋层状结构半导体上转换发光材料。
优选的,本发明选用Yb3+离子作为敏化剂。
优选的,所述分散剂为无水乙醇。
本发明的有益效果是:
(1)本发明所述铋层状结构半导体材料为钙钛矿型结构,具有强烈的晶体场环境和高的热稳定性,带隙较宽,其声子能量也较低,容易实现Ho3+、Tm3+、Tb3+离子高效的绿色、蓝色上转换发光,是一种新型的多功能稀土上转换发光材料,有利于扩展稀土上转换发光材料的应用领域。
(2)本发明成本低,制备工艺简单,所制备的上转换发光材料物理化学性质稳定、发光性能良好,在照明、显示、太阳能电池、温度传感及光电多功能器件方面具有良好的应用前景。
附图说明
图1为本发明实施例1制备得到的稀土掺杂铋层状结构半导体上转换发光材料的XRD图。
图2为本发明实施例1制备得到的稀土掺杂铋层状结构半导体上转换发光材料的SEM图。
图3为本发明实施例1制备得到的稀土掺杂铋层状结构半导体上转换发光材料吸收光谱图。
图4为本发明实施例1制备得到的稀土掺杂铋层状结构半导体上转换发光材料在980nm激光照射下的发射光谱图。
图5为本发明实施例1制备得到的稀土掺杂铋层状结构半导体上转换发光材料在980nm激光照射下的上转换发光强度与激发功率的关系图。
图6为本发明实施例2制备得到的稀土掺杂铋层状结构半导体上转换发光材料在980nm激光照射下的发射光谱图。
具体实施方式
下面结合附图和具体实施例对本发明作进一步详细说明,但本发明的保护范围并不限于所述内容。
实施例1
一种稀土掺杂铋层状结构半导体绿色上转换发光材料Ca0.89Yb0.1Ho0.01Bi2Nb2O9的制备方法,具体步骤如下:
根据Ca0.89Yb0.1Ho0.01Bi2Nb2O9化学计量比分别称量高纯Bi2O3、CaCO3、Nb2O5、Yb2O3、Ho2O3五种原料,置于玛瑙研钵中,加入分散剂研磨,使原料充分混合均匀后烘干;将烘干后的原料置于氧化铝坩埚,放入马弗炉中在850℃条件下预烧2h,然后在空气气氛下1000℃下烧结4h;冷却至室温,将烧结好的样品再次研磨,即可得到化学式为Ca0.89Yb0.1Ho0.01Bi2Nb2O9的稀土离子掺杂铋层状结构半导体上转换发光材料。
本实施例所得化学式为Ca0.89Yb0.1Ho0.01Bi2Nb2O9的稀土掺杂铋层状结构半导体上转换发光材料的X射线衍射图谱如图1所示,从图1可知,稀土掺杂铋层状结构半导体上转换发光材料衍射峰位置和相对强度与CaBi2Nb2O9标准卡片完全吻合,说明Ca0.89Yb0.1Ho0.01Bi2Nb2O9的相结构为纯相;此外,材料的衍射峰尖锐且强度较高,说明材料具有较高的结晶度。
本实施例所得化学式为Ca0.89Yb0.1Ho0.01Bi2Nb2O9的稀土掺杂铋层状结构半导体上转换发光材料的扫描电镜图谱如图2所示;从图2可知,合成的Ca0.89Yb0.1Ho0.01Bi2Nb2O9为尺寸不均匀形状不规则团聚的颗粒,表面较为光滑,结晶良好,有利于稀土发光。图3为本实施例所得化学式为Ca0.89Yb0.1 Ho0.01-Bi2Nb2O9的吸收光谱。从图3可知,合成的Ca0.89Yb0.1Ho0.01 Bi2Nb2O9材料吸收边在420nm左右,是一种宽禁带半导体,适合作为发光基质。
本实施例所得化学式为Ca0.89Yb0.1Ho0.01Bi2Nb2O9的稀稀土掺杂铋层状结构半导体上转换发光材料在980nm激光激发下的发射光谱如图4所示,从图4可知,在980激光激发下,样品显示出明亮的绿色,发射波长分别位于548、663和756nm。
图5为本实施例所得化学式为Ca0.89Yb0.1 Ho 0.01Bi2Nb2O9在980nm激光照射下的上转换发光强度与激发功率的关系图;由图5可知,548、663和756nm发射强度和功率对数曲线拟合值n分别为1.8、1.7和1.7,表明在980nm激光激发下,548、663和756nm发射均为一个两光子过程。
实施例2
一种稀土掺杂铋层状结构半导体绿色上转换发光材料Ca0.94Yb0.01Ho0.05Bi2Nb2O9的制备方法,具体步骤如下:
根据Ca0.94Yb0.01Ho0.05Bi2Nb2O9化学计量比分别称量高纯Bi2O3、CaCO3、Nb2O5、Yb2O3、Ho2O3五种原料,置于玛瑙研钵中,加入分散剂研磨,使原料充分混合均匀后烘干;将烘干后的原料置于氧化铝坩埚,放入马弗炉中在950℃条件下预烧1h,然后在空气气氛下1100℃下烧结3h;冷却至室温,将烧结好的样品再次研磨,即可得到化学式为Ca0.94Yb0.01Ho0.05Bi2Nb2O9的稀土离子掺杂铋层状结构半导体上转换发光材料。
本实施例制备得到的上转换发光材料的结构和性能与实施例1相似。
实施例3
一种稀土掺杂铋层状结构半导体绿色上转换发光材料Ca0.935Yb0.06Ho0.005Bi2Nb2O9的制备方法,具体步骤如下:
根据Ca0.935Yb0.06Ho0.005Bi2Nb2O9化学计量比分别称量高纯Bi2O3、CaCO3、Nb2O5、Yb2O3、Ho2O3五种原料,置于玛瑙研钵中,加入分散剂研磨,使原料充分混合均匀后烘干;将烘干后的原料置于氧化铝坩埚,放入马弗炉中在850℃条件下预烧2h,然后在空气气氛下1000℃下烧结4h;冷却至室温,将烧结好的样品再次研磨,即可得到化学式为Ca0.935Yb0.06Ho0.005Bi2Nb2O9的稀土离子掺杂铋层状结构半导体上转换发光材料。本实施例制备得到的上转换发光材料的结构和性能与实施例1相似。
实施例4
一种稀土掺杂铋层状结构半导体蓝色上转换发光材料Ca0.89Yb0.1Tm0.01Bi2Nb2O9的制备方法,具体步骤如下:
根据Ca0.89Yb0.1Tm0.01Bi2Nb2O9化学计量比分别称量高纯Bi2O3、CaCO3、Nb2O5、Yb2O3、Tm2O3五种原料,置于玛瑙研钵中,加入分散剂研磨,使原料充分混合均匀后烘干;将烘干后的原料置于氧化铝坩埚,放入马弗炉中在850℃条件下预烧2h,然后在空气气氛下1000℃下烧结4h;冷却至室温,将烧结好的样品再次研磨,即可得到化学式为Ca0.89Yb0.1Tm0.01Bi2Nb2O9的稀土离子掺杂铋层状结构半导体上转换发光材料。
本实施例所得化学式为Ca0.89Yb0.1Tm0.01Bi2Nb2O9的稀土离子掺杂卤氧化铋半导体上转换发光材料在980nm激光激发下的荧光光谱如图6所示,从图6可知,在980nm近红外激光激发下,样品显示出明亮的蓝色,发射波长分别位于478、648、695、780nm。
实施例5
一种稀土掺杂铋层状结构半导体绿色上转换发光材料Ca0.89Yb0.1Tb0.01Bi2Nb2O9的制备方法,具体步骤如下:
根据Ca0.89Yb0.1Tb0.01Bi2Nb2O9化学计量比分别称量高纯Bi2O3、CaCO3、Nb2O5、Yb2O3、Tb4O7五种原料,置于玛瑙研钵中,加入分散剂研磨,使原料充分混合均匀后烘干;将烘干后的原料置于氧化铝坩埚,放入马弗炉中在850℃条件下预烧2h,然后在空气气氛下1000℃下烧结4h;冷却至室温,将烧结好的样品再次研磨,即可得到化学式为Ca0.89Yb0.1Tb0.01Bi2Nb2O9的稀土离子掺杂铋层状结构半导体上转换发光材料。
本实施例制备得到的上转换发光材料的结构和性能与实施例1相似。
Claims (4)
1.一种稀土掺杂铋层状结构半导体上转换发光材料,其特征在于:该发光材料的化学通式为:Ca1-x-yYbxREyBi2Nb2O9,其中RE为稀土元素Ho、Tm或Tb;x=0.01~0.1,y=0.005~0.05。
2.权利要求1所述稀土掺杂铋层状结构半导体上转换发光材料,其特征在于:所述的稀土元素为Ho、Tm或Tb。
3.根据权利要求2所述的稀土掺杂铋层状结构半导体上转换发光材料的制备方法,其特征在于,具体步骤如下:
(1)根据化学计量比分别称量Bi2O3、CaCO3、Nb2O5、Yb2O3、稀土氧化物,其中,稀土氧化物为Ho2O3、Tm2O3或Tb4O7,置于研钵中,加入分散剂研磨,使原料充分混合均匀后烘干;
(2)将烘干后的原料置于坩埚中,放入马弗炉中在800~950℃条件下预烧1~3h,然后在空气气氛下于1000-1150℃下烧结2~5h;冷却至室温,将烧结好的样品再次研磨,即可得到化学式为Ca1-x-yYbxREyBi2Nb2O9的稀土离子掺杂铋层状结构半导体上转换发光材料。
4.根据权利要求3所述的稀土掺杂铋层状结构半导体上转换发光材料的制备方法,其特征在于:所述分散剂为无水乙醇。
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HUA ZOU ET AL.: "Upconversion photoluminescence properties of Er3+ doped CaBi2Nb2O9 phosphors for temperature sensing", 《J MATER SCI: MATER ELECTRON》 * |
LEI YU ET AL.: "Ho-doped SrBi2Nb2O9 multifunctional ceramics with bright green emission and good electrical properties", 《PHYS. STATUS SOLIDI A》 * |
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