CN108314325A - 具有超宽带近红外发光的自析晶微晶玻璃及其制备方法和应用 - Google Patents
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Abstract
本发明公开了具有超宽带近红外发光的自析晶微晶玻璃，以Ni2+掺杂的KMgF3为微晶相；所述Ni2+:KMgF3的组成为KF‑MgF2‑K2CO3‑Al2O3‑SiO2‑NiO，各组分的摩尔百分比分别为：10～20％的KF；2～10％的MgF2；0～15％的K2CO3；0～10％的Al2O3；0.001～1％的NiO；余量的SiO2。本发明的微晶玻璃具有近中红外发光性能，其发光峰位于1670～1800nm，发光范围为1300～2200nm，覆盖可燃性气体的吸收谱，可有望作为近中红外激光增益介质和可燃性气体探测器。
Description
技术领域
本发明涉及发光材料，特别涉及一种具有超宽带近红外发光的自析晶微晶玻璃及其制备方法和应用。
背景技术
气体探测在环境监测、医疗诊断和安全监视等方面具有重要应用。人们对于可燃性气体探测器的探索更是付出了很多努力。相比于传统的基于表面化学反应的气体传感器，光学气体传感器由于其快速响应、高选择性、原位探测和实时探测的特点引起了人们广泛的注意。基于此，覆盖可燃性气体吸收峰的宽带可调谐近红外光源备受关注。例如C2H4，NH3和CO的吸收峰分别在能吸收1μm，1.5μm和5μm。基于稀土例子掺杂的传统光源很难覆盖这些可燃性气体的吸收峰，尤其是1.4-2μm范围内缺乏相应的稀土发光区域，而这些区域对应着重要的可燃性气体的吸收峰，例如C2H6(～1.6μm)，CH4(1.65μm)，H2CO(1.7μm)and NO(1.9μm)。因此探索新型能覆盖1.4-2μm波段的近红外发光材料具有重要的意义。
过渡金属的d-d跃迁对基质环境十分敏感，因此有望在过渡金属掺杂的基质中实现上述的近红外发光，从而覆盖大部分的可燃性气体的吸收峰，有望应用于可燃性气体的检测。然而从传统的技术来制备这些过渡金属激活的近红外发光材料还存在很大的挑战，比如材料的制备通常涉及单晶的生长而光纤的制备方面也存在着很大的挑战。由于玻璃能制备成各种形状和其优良的成纤性能，因此过渡金属掺杂的玻璃和光纤应该是制备过渡金属掺杂材料的首选。然而由于玻璃的无序结构和较高的声子能，在玻璃中很难观测到过渡金属的近红外发光。过渡金属掺杂的微晶玻璃材料由于结合了玻璃优良的成纤性能和晶体的低声子能的特点引起了研究者的广泛关注。过渡金属在热处理时会富集到玻璃中析出的纳米晶体中从而具有较好的发光。因此可以保证玻璃成纤性能的同时还能确保过渡金属在晶体中的高效发光。然而文献中报道的过渡金属掺杂微晶玻璃中Ni2+的发射峰很难逾越1.5μm，限制了Ni2+掺杂微晶玻璃在中红外激光领域的应用。另一方面，传统报道的Ni2+微晶玻璃大多是通过对母体玻璃进行热处理，进而通过成核、长晶的过程来控制晶体的大小。然而一旦析晶被触发，将会导致晶体的过度生长，从而导致玻璃失去透过率。这在制备优异的Ni2+掺杂微晶玻璃及光纤方面造成很大的问题。因此需要探索新型Ni2+掺杂微晶玻璃作为宽带光源、可调谐激光的增益介质从而拓宽光纤和激光的应用。
发明内容
为了克服现有技术的上述缺点与不足，本发明的目的在于提供一种具有超宽带近红外发光的自析晶微晶玻璃，可不经过传统的热处理直接获得，且具有近红外超宽带发光，经过热处理后，发光显著增强，发光范围为1300-2200nm，发光峰位为1600～1800nm。
本发明的另一目的在于提供上述具有超宽带近红外发光的自析晶微晶玻璃的制备方法，制备较为简单，可大量生产。
本发明的在一目的在于提供上述具有超宽带近红外发光的自析晶微晶玻璃的应用。
本发明的目的通过以下技术方案实现：
具有超宽带近红外发光的自析晶微晶玻璃，以Ni2+掺杂的KMgF3为微晶相；所述Ni2 +:KMgF3的组成为KF-MgF2-K2CO3-Al2O3-SiO2-NiO，各组分的摩尔百分比分别为：
KMgF3纳米晶体均匀的镶嵌在玻璃基质中。
所述的具有超宽带近红外发光的自析晶微晶玻璃，包括以下步骤：
(1)分别称量原料KF、MgF2、K2CO3、Al2O3、SiO2、和NiO，均匀混合后，将粉末样品于1450-1600℃熔制，得到均匀玻璃熔体；
(2)将玻璃熔体冷却，即制备成Ni2+:KMgF3微晶玻璃。
所述的具有超宽带近红外发光的自析晶微晶玻璃，步骤(2)之后还进行以下步骤：
(3)将步骤(2)所制Ni2+:KMgF3微晶玻玻璃于500～750℃热处理，随炉冷却至室温，得到红外发光增强的透明Ni2+:KMgF3自析晶微晶玻璃。
步骤(1)所述均匀混合，具体为：置于玛瑙研钵中研磨搅拌至均匀。
步骤(2)所述熔制，具体为：于1450～1600℃熔制30～60min。
步骤(3)所述于500～750℃热处理，具体为：于500～750℃热处理0～20小时。
具有超宽带近红外发光的自析晶微晶玻璃的应用，作为近中红外激光增益介质和可燃性气体传感器。
与现有技术相比，本发明具有以下优点和有益效果：
(1)本发明的具有超宽带发光的Ni2+:KMgF3自析晶微晶玻璃，可不经过传统热处理过程直接获得。且热处理后发光显著增强，发光范围为1300～2200nm，发光峰位于1600～1800nm。
(2)本发明的Ni2+:KMgF3自析晶微晶玻璃的红外超宽带发光覆盖可燃性气体的吸收谱，且可作为近中红外激光增益介质。
(3)本发明的Ni2+:KMgF3自析晶微晶玻璃的制备方法，制备较为简单，成本低，可大量生产。
(4)本发明的Ni2+:KMgF3微晶玻璃，泵浦激光可采用常见的808nm半导体激光，易于获得，十分便捷。
附图说明
图1为实施例1制备的Ni2+:KMgF3微晶玻璃的X射线衍射图。
图2为实施例1制备的Ni2+:KMgF3微晶玻璃的透射电镜图。
图3为实施例1制备的Ni2+:KMgF3微晶玻璃的吸收光谱。
图4为实施例1制备的Ni2+:KMgF3微晶玻璃的荧光光谱。
图5为实施例1制备的Ni2+:KMgF3微晶玻璃热处理前后的荧光光谱对比。
具体实施方式
下面结合实施例，对本发明作进一步地详细说明，但本发明的实施方式不限于此。
实施例1
本实施例制备的Ni2+:KMgF3微晶玻璃，其组成为KF-MgF2-K2CO3-Al2O3-SiO2-NiO，各原料摩尔百分比分别为:18％KF，7％MgF2，10％K2CO3，15％Al2O3，50％SiO2，0.05％NiO。将各原料分别称量好，置于玛瑙研钵中研磨搅拌使其混合均匀，将粉末样品转移入氧化铝坩埚中。在1550℃的高温箱式电阻炉中熔融50mins，然后把玻璃熔体倒在光滑钢板上形成玻璃块，即形成了Ni2+:KMgF3微晶玻璃。把玻璃块切割成规则的玻璃片，在700℃的马弗炉保温5小时，然后随炉冷却至室温，得到荧光增强的透明Ni2+:KMgF3微晶玻璃。
本实施例制备的Ni2+:KMgF3微晶玻璃的X射线衍射图谱如图1所示，由图可知该Ni2 +:KMgF3微晶玻璃析出的晶体与Ni2+:KMgF3的标准PD卡片PDF#18-1033对应良好，证实了本实施例所得晶相为KMgF3。图2为本实施例所得荧光增强的Ni2+:KMgF3透明微晶玻璃的透射电镜图，可见尺寸35nm左右的KMgF3纳米晶体均匀的镶嵌在玻璃基质中。图3为本实施例所得Ni2+:KMgF3透明微晶玻璃的吸收光谱，吸收峰分别为391nm，696nm和1207nm，源于八配位Ni2+离子的电子跃迁。图4为实施例所得荧光增强的Ni2+:KMgF3透明微晶玻璃的荧光光谱，可以看到样品在1300～2200nm具有超宽带发光，发光峰位于1760nm处，源于八配位Ni2+离子3T2g(F)→3A2g(F)电子跃迁。
图5为实施例所得Ni2+:KMgF3微晶玻璃热处理前后的荧光光谱对比，可见热处理后其荧光强度显著增加。
实施例2
本实施例制备的KMgF3微晶玻璃，其组成为KF-MgF2-K2CO3-Al2O3-SiO2-NiO，各原料摩尔百分比分别为:18％KF，7％MgF2，15％Al2O3,60％Si02，0.5％NiO。将各原料分别称量好，置于玛瑙硏钵中搅拌、混合玓匀，将粉末样品转移入坩埚中。在1550℃的高温箱式电阻炉中熔融60min，然后把玻璃熔体倒在光滑钢板上形成玻璃块，即制成Ni2+:KMgF3微晶玻璃。把玻璃块切割成规则的玻璃薄片，在750℃的马弗炉保温15小时，然后随炉泠却至室温，得到透明的Ni2+:KMgF3微晶玻璃，在近中红外具有宽带发光，发光峰位于1700nm处。
实施例3
本实施例制备的KMgF3微晶玻璃，其组成为KF-MgF2-K2CO3-Al2O3-SiO2-NiO，各原料摩尔百分比分别为:15％KF，5％MgF2，5K2CO3，10％Al2O3,65％SiO2，0.1％NiO。将各原料分别称量好，置于玛瑙硏钵中搅拌、混合玓匀，将粉末样品转移入坩埚中。在1600℃的高温箱式电阻炉中熔融60min，然后把玻璃熔体倒在光滑钢板上形成玻璃块，即制成Ni2+:KMgF3微晶玻璃。把玻璃块切割成规则的玻璃薄片，在600℃的马弗炉保温10小时，然后随炉泠却至室温，得到透明的Ni2+:KMgF3微晶玻璃，在近中红外具有宽带发光，发光峰位于1680nm处。
实施例4
本实施例制备的KMgF3微晶玻璃，其组成为KF-MgF2-K2CO3-Al2O3-SiO2-NiO，各原料摩尔百分比分别为:15％KF，5％MgF2，5K2CO3，0％Al2O3，75％SiO2，0.001％NiO。将各原料分别称量好，置于玛瑙硏钵中搅拌、混合玓匀，将粉末样品转移入坩埚中。在1500℃的高温箱式电阻炉中熔融60min，然后把玻璃熔体倒在光滑钢板上形成玻璃块，即制成Ni2+:KMgF3微晶玻璃。把玻璃块切割成规则的玻璃薄片，在700℃的马弗炉保温10小时，然后随炉泠却至室温，得到透明的Ni2+:KMgF3微晶玻璃，该微晶玻璃具有在近中红外发光的特性。
对比例1
本实施例制备的KMgF3微晶玻璃，其组成为KF-MgF2-K2CO3-Al2O3-SiO2，各原料摩尔百分比分别为:15％KF，5％MgF2，5K2CO3，10％Al2O3,65％SiO2，0％NiO。将各原料分别称量好，置于玛瑙硏钵中搅拌、混合玓匀，将粉末样品转移入坩埚中。在1600℃的高温箱式电阻炉中熔融60min，然后把玻璃熔体倒在光滑钢板上形成玻璃块，即制成KMgF3微晶玻璃。把玻璃块切割成规则的玻璃薄片，在600℃的马弗炉保温10小时，然后随炉泠却至室温，得到透明无Ni的KMgF3微晶玻璃，实验结果表明，不含Ni的微晶玻璃没有发光特性。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受所述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (8)
1.具有超宽带近红外发光的自析晶微晶玻璃，其特征在于，以Ni2+掺杂的KMgF3为微晶相；所述Ni2+:KMgF3的组成为KF-MgF2-K2CO3-Al2O3-SiO2-NiO，各组分的摩尔百分比分别为：
2.根据权利要求1所述的具有超宽带近红外发光的自析晶微晶玻璃，其特征在于，KMgF3纳米晶体均匀的镶嵌在玻璃基质中。
3.根据权利要求1所述的具有超宽带近红外发光的自析晶微晶玻璃，其特征在于，包括以下步骤：
(1)分别称量原料KF、MgF2、K2CO3、Al2O3、SiO2、和NiO，均匀混合后，将粉末样品于1450-1600℃熔制，得到均匀玻璃熔体；
(2)将玻璃熔体冷却，即制备成Ni2+:KMgF3微晶玻璃。
4.根据权利要求1所述的具有超宽带近红外发光的自析晶微晶玻璃，其特征在于，步骤(2)之后还进行以下步骤：
(3)将步骤(2)所制Ni2+:KMgF3微晶玻玻璃于500～750℃热处理，随炉冷却至室温，得到红外发光增强的透明Ni2+:KMgF3自析晶微晶玻璃。
5.根据权利要求1所述的具有超宽带近红外发光的自析晶微晶玻璃，其特征在于，步骤(1)所述均匀混合，具体为：置于玛瑙研钵中研磨搅拌至均匀。
6.根据权利要求1所述的具有超宽带近红外发光的自析晶微晶玻璃，其特征在于，步骤(2)所述熔制，具体为：于1450～1600℃熔制30～60min。
7.根据权利要求4所述的具有超宽带近红外发光的自析晶微晶玻璃，其特征在于，步骤(3)所述于500～750℃热处理，具体为：于500～750℃热处理0～20小时。
8.权利要求1所述的具有超宽带近红外发光的自析晶微晶玻璃的应用，其特征在于，作为近中红外激光增益介质和可燃性气体传感器。
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| WO2024018928A1 (ja) * | 2022-07-19 | 2024-01-25 | パナソニックＩｐマネジメント株式会社 | 構造体、赤外線検知装置、発光装置及び構造体の製造方法 |
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