CN110282969A - 一种同时提高蓄光陶瓷光效及稳定性的方法 - Google Patents

一种同时提高蓄光陶瓷光效及稳定性的方法 Download PDF

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CN110282969A
CN110282969A CN201910587378.9A CN201910587378A CN110282969A CN 110282969 A CN110282969 A CN 110282969A CN 201910587378 A CN201910587378 A CN 201910587378A CN 110282969 A CN110282969 A CN 110282969A
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light
powder
added
calcium
accumulating
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CN110282969B (zh
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张乐
杨顺顺
王蕊
李涛
朱晓雯
姜欣宇
黄国灿
康健
孙炳恒
邵岑
周天元
陈浩
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Jiangsu Normal University
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Jiangsu Normal University
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Priority to PCT/CN2019/096257 priority patent/WO2021000344A1/zh
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  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

本发明公开了一种同时提高蓄光陶瓷光效及稳定性的方法，首先将将钙的乙醇溶液加入到钛前驱体液中，加入分散剂油酸，随后加入纯水、蓄光粉，得到蓄光粉‑钛酸钙凝胶，干燥、粉碎、过筛得到干凝胶粉；将玻璃基质原料、过筛的干凝胶粉、分散剂放入造粒机内，加入纯水后直接机械搅拌造粒，搅拌4～8小时后加入增塑剂，继续搅拌1～3小时得到混料，压片、干燥、炉窑烧制即可。通过人工可控引入钛酸钙为第二相来包裹蓄光粉形成“核壳结构”保护蓄光粉不会发生水解或高温氧化；作为蓄光粉镀层的钛酸钙还能改变荧光在陶瓷内部的传播路径，提高光吸收和荧光输出效率；同时，表面为钛酸钙的蓄光粉改善了陶瓷浆料瘠性，利于陶瓷成型。

Description

一种同时提高蓄光陶瓷光效及稳定性的方法
技术领域
本发明涉及蓄光陶瓷领域，具体涉及一种同时提高蓄光陶瓷光效及稳定性的方法。
背景技术
蓄光性自发光材料可以利用日光或灯光储光在夜晚或黑暗处发光，广泛应用在夜间应急指示、光电子器件或元件、仪表显示，低度照明，家庭装饰及国防军事诸多方面。
国内外使用的蓄光型产品的载体材质有薄铝板材(在其上印刷蓄光材料图案)、塑料、油墨、树脂等经过常温或较低温度处理就能定型的材料。由于是简单将发光材料涂覆或者混合进基质里，因而会带来热冲击性差的问题。特别是一旦发生火灾，带来的高温会很容易造成发光粉体氧化失效或者产品熔融；且存在技术问题加上发光涂层厚度仅在1～2mm的限制条件，此方法显然无法提供足够的发光中心来实现高亮度指示或者照明，其余辉时间也相对较短。由此，研究人员提出“一体化”蓄光型复相陶瓷方案，其优势在于：(1)将长余辉材料蓄光功能相结合石英陶瓷基质相，可以实现陶瓷通体发光以达到高光效的要求；(2)避免发光釉层与陶瓷基质因膨胀系数不同造成的釉层开裂；(3)石英陶瓷由于具有较高的耐酸碱侵蚀性能和抗热震性，此外热膨胀系数低，体积稳定性好等优势，可作为基质实现蓄光粉性能。
然而，此方案虽优势明显，但是由于介质折射率差异(铝酸盐荧光粉折射率：～1.6，石英基陶瓷折射率：～1.45-1.50)在陶瓷内部必然会引起的双折射现象(birefringence)，导致激发光以及荧光的散射损耗，以及整体透过率的降低。因此，为实现“一体化”蓄光型陶瓷在消防指示、园艺景观等领域更为广泛的应用，迫切需要一种简便、有效的方法来提高蓄光陶瓷的光提取率和荧光输出率。
发明内容
本发明的目的是提供一种同时提高蓄光陶瓷光效及稳定性的方法，能够消除陶瓷内部的双折射现象，提高荧光输出强度和持续时间。
为实现上述目的，本发明采用的技术方案如下：一种同时提高蓄光陶瓷光效及稳定性的方法，包括以下步骤：
(1)按照质量比10：0.5～1.5分别称取硝酸钙和柠檬酸，并溶于无水乙醇中，形成钙的乙醇溶液；称取钛酸四正丁酯并溶于无水乙醇中，同时在搅拌状态下滴加冰醋酸，形成钛前驱体液；在搅拌状态下，将钙的乙醇溶液加入到钛前驱体液中，加入分散剂油酸，随后加入纯水、蓄光粉，继续搅拌1～4h，得到蓄光粉-钛酸钙凝胶；
(2)将步骤(1)得到的蓄光粉-钛酸钙凝胶于80～150℃条件下加热2～8小时，得到钛酸钙包覆的蓄光粉干凝胶，粉碎，过80～200目筛待用；
(3)将玻璃基质原料、过筛的干凝胶粉、分散剂放入造粒机内，加入纯水后直接机械搅拌造粒，搅拌4～8小时后加入增塑剂，继续搅拌1～3小时得到混料；整个搅拌过程的搅拌转速在100～300rad/min；
(4)将步骤(3)得到的混料分装进模具中，利用自动压片机进行压片，模具形状为产品要求所需，压力在5～40MPa，保压时间5～20s，随后脱模送进窑炉进行干燥并烧制；
(5)窑炉升温制度为：室温～200℃左右，速率在2～5℃/min，保温10～30min，保证坯体水分完全蒸发；随后继续升温至400～900℃，保温60～120min，保证无色玻璃粉在半熔融状态内完成结晶和晶核长大，且不会对长余辉自发光材料造成热损伤；然后随炉冷却至100℃以下取出成品，即可得到透光率好、余辉亮度高、有玉质观感的蓄光陶瓷。
优选的，步骤(1)中，硝酸钙与钛酸四正丁酯的质量比为1：0.8～2.5；在钙的乙醇溶液中，溶质溶液比为1：1.5～3；在钛的前驱体液中，溶质溶液比为1：0.5～2.5；冰醋酸的添加量占硝酸钙和钛酸四正丁酯的总质量比的35％～55％；分散剂油酸的添加量占硝酸钙和钛酸四正丁酯的总质量比的5％～15％；纯水的添加量与硝酸钙和钛酸四正丁酯的总质量比为1：3.5～5；蓄光粉的添加量与硝酸钙和钛酸四正丁酯的总质量比为1:8～10。
优选的，步骤(1)中，所述蓄光粉选用但不限于碱土铝酸盐长余辉蓄光粉体系，优选SrAl2O4为基质的蓄光粉，粒径为10～500微米。
优选的，步骤(3)中，所述玻璃基质原料为玻璃粉，粒径范围在10～400微米，玻璃粉添加量为90％～98％。
优选的，步骤(3)中，干凝胶粉与玻璃粉的质量比为9～49：1；分散剂的添加量占干凝胶粉和玻璃粉的总质量的0.1～0.6％；增塑剂的添加量占干凝胶粉和玻璃粉的总质量的0.1～0.9％；纯水的添加量占干凝胶粉和玻璃粉的总质量的20％～50％。
优选的，步骤(3)中，所述增塑剂为甲基纤维素，所述分散剂为三聚磷酸钠。
与现有技术相比，本发明具有如下有益效果：
1.通过人工可控引入钛酸钙(折射率～1.57)，钛酸钙在蓄光粉表面形成完全包覆的镀层，该镀层介于铝酸盐荧光粉(折射率：～1.6)和石英基陶瓷(折射率：～1.45-1.50)之间，消除了陶瓷内部的双折射现象，提高荧光输出强度和持续时间；
2.通过钛酸钙包覆解决“一体化”蓄光型陶瓷耐候性的问题；
3.通过在陶瓷浆料中加入表面为钛酸钙的蓄光粉改善陶瓷浆料瘠性；
4.在20min蓄光的条件下，可实现720min的持续发光：初始1min强度，>4000mcd/m2；60min，>400mcd/m2；720min，>5mcd/m2(室外阳光直射20min，日光灯30min，紫外线灯5min，室温25℃测试)。
5.使用寿命跟建筑陶瓷同寿命，至少15年以上不老化，水中8年以上。
附图说明
图1为本发明实施例1制得的蓄光陶瓷与市售蓄光指示牌发光强度对比(1为本实施例1陶瓷，2为市售蓄光指示牌)；
图2为本发明实施例1制得的蓄光陶瓷实物图；
图3为本发明实施例1制得的蓄光陶瓷的扫描电镜图：(a)5μm；(b)100nm。
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。
下述实施例中，除非另有说明，所述的实验方法通常按照常规条件或制造厂商建议的条件实施；所用的原料、试剂均为市售商品。
以下六个实施例配方如表1、表2所示。
表1蓄光粉—钛酸钙凝胶配料表
表2蓄光陶瓷配料表
序号 干凝胶粉(％) 玻璃粉(％) 增塑剂(％) 分散剂(％)
1 2 98 0.1 0.1
2 10 90 0.6 0.4
3 2 98 0.3 0.3
4 10 90 0.5 0.6
5 5 95 0.9 0.2
6 7 93 0.8 0.1
实施例1
具体制备方法包括下列步骤：
(1)按照质量比10：0.5分别称取硝酸钙和柠檬酸，并溶于无水乙醇中，磁力搅拌20min，转速150r/min，形成钙的乙醇溶液；称取钛酸四正丁酯并溶于无水乙醇中，磁力搅拌20min，转速150r/min，并在搅拌过程中滴加冰醋酸，形成钛前驱体液；在搅拌条件下，将钙的乙醇溶液加入到钛前驱体液中，加入分散剂油酸，随后加入纯水、蓄光粉(选用Sr4Al14O25：Eu，Dy，粒径为500微米)，继续搅拌1h，得到蓄光粉-钛酸钙凝胶；
(2)将步骤(1)得到的蓄光粉-钛酸钙凝胶于80℃条件下加热2小时，得到钛酸钙包覆的蓄光粉干凝胶，粉碎，过80目筛待用；
(3)将粒径400微米的玻璃粉、80目干凝胶粉、分散剂三聚磷酸钠放入造粒机内，加入纯水后直接机械搅拌造粒，搅拌8小时后加入增塑剂甲基纤维素，继续搅拌3小时得到混料，为糊料、砂浆或粘稠物；整个搅拌过程的搅拌转速在300rad/min；
(4)选用自动压片机将步骤(3)得到的混料分装进模具中进行压片；模具形状为正方形片状(20cm*20cm)，压力在40MPa，保压时间20s，随后脱模送进窑炉进行干燥并烧制。
(5)窑炉升温制度为：室温～200℃，速率在5℃/min，保温30min；随后继续升温至900℃，升温速率3℃/min，保温120min；然后随炉冷却至100℃以下取出成品。
图1为本发明实施例1制得的蓄光陶瓷与市售蓄光指示牌发光强度对比，由此可知，本实施例制得的蓄光陶瓷的发光强度较高。
图2为本发明实施例1制得的蓄光陶瓷实物图，黑暗中可观察到发蓝绿色的光。
图3为本发明实施例1制得的蓄光陶瓷的扫描电镜图：(a)5μm；(b)100nm，由此可知，钛酸钙镀层包裹在蓄光粉表面，介于铝酸盐荧光粉和石英基陶瓷之间。
在20min蓄光的条件下，可实现720min的持续发光：初始1min强度，>4000mcd/m2；60min，>400mcd/m2；720min，>5mcd/m2(室外阳光直射20min，日光灯30min，紫外线灯5min，室温25℃测试)。
实施例2
具体制备方法包括下列步骤：
(1)按照质量比10：1.5分别称取硝酸钙和柠檬酸，并溶于无水乙醇中，磁力搅拌60min，转速300r/min，形成钙的乙醇溶液；称取钛酸四正丁酯并溶于无水乙醇中，磁力搅拌60min，转速300r/min，并在搅拌过程中滴加冰醋酸，形成钛前驱体液；在搅拌条件下，将钙的乙醇溶液加入到钛前驱体液中，加入分散剂油酸，随后加入纯水、蓄光粉(选用Sr4Al14O25：Eu，Dy，粒径为500微米)，继续搅拌4h，得到蓄光粉-钛酸钙凝胶；
(2)将步骤(1)得到的蓄光粉-钛酸钙凝胶于150℃条件下加热8小时，得到钛酸钙包覆的蓄光粉干凝胶，粉碎，过200目筛待用；
(3)将粒径400微米的玻璃粉、200目干凝胶粉、分散剂三聚磷酸钠放入造粒机内，加入纯水后直接机械搅拌造粒，搅拌8小时后加入增塑剂甲基纤维素，继续搅拌3小时得到混料，为糊料、砂浆或粘稠物；整个搅拌过程的搅拌转速在300rad/min；
(4)选用自动压片机将步骤(3)得到的混料分装进模具中进行压片；模具形状为正方形片状(20cm*20cm)，压力在40MPa，保压时间20s，随后脱模送进窑炉进行干燥并烧制；
(5)窑炉升温制度为：室温～200℃，速率在5℃/min，保温30min；随后继续升温至900℃，升温速率3℃/min，保温120min；然后随炉冷却至100℃以下取出成品。
实施例3
具体制备方法包括下列步骤：
(1)按照质量比10：1分别称取硝酸钙和柠檬酸，并溶于无水乙醇中，磁力搅拌30min，转速200r/min，形成钙的乙醇溶液；称取钛酸四正丁酯并溶于无水乙醇中，磁力搅拌40min，转速200r/min，并在搅拌过程中滴加冰醋酸，形成钛前驱体液；在搅拌条件下，将钙的乙醇溶液加入到钛前驱体液中，加入分散剂油酸，随后加入纯水、蓄光粉(选用Sr4Al14O25：Eu，Dy，粒径为10微米)，继续搅拌2h，得到蓄光粉-钛酸钙凝胶；
(2)将步骤(1)得到的蓄光粉-钛酸钙凝胶于150℃条件下加热8小时，得到钛酸钙包覆的蓄光粉干凝胶，粉碎，过100目筛待用；
(3)将粒径10微米的玻璃粉、100目干凝胶粉、分散剂三聚磷酸钠放入造粒机内，加入纯水后直接机械搅拌造粒，搅拌4小时后加入增塑剂甲基纤维素，继续搅拌1小时得到混料，为糊料、砂浆或粘稠物；整个搅拌过程的搅拌转速在100rad/min；
(4)选用自动压片机将步骤(3)得到的混料分装进模具中进行压片；模具形状为矩形(20cm*30cm)，压力在5MPa，保压时间5s，随后脱模送进窑炉进行干燥并烧制；
(5)窑炉升温制度为：室温～200℃，速率在5℃/min，保温10min；随后继续升温至400℃，速率在5℃/min，保温60min；然后随炉冷却至100℃以下取出成品。
实施例4
具体制备方法包括下列步骤：
(1)按照质量比10：1.5分别称取硝酸钙和柠檬酸，并溶于无水乙醇中，磁力搅拌50min，转速200r/min，形成钙的乙醇溶液；称取钛酸四正丁酯并溶于无水乙醇中，磁力搅拌50min，转速200r/min，并在搅拌过程中滴加冰醋酸，形成钛前驱体液；在搅拌条件下，将钙的乙醇溶液加入到钛前驱体液中，加入分散剂油酸，随后加入纯水、蓄光粉(选用Sr4Al14O25：Eu，Dy，粒径为10微米)，继续搅拌3h，得到蓄光粉-钛酸钙凝胶；
(2)将步骤(1)得到的蓄光粉-钛酸钙凝胶于150℃条件下加热6小时，得到钛酸钙包覆的蓄光粉干凝胶，粉碎，过100目筛待用；
(3)将粒径10微米的玻璃粉、100目干凝胶粉、分散剂三聚磷酸钠放入造粒机内，加入纯水后直接机械搅拌造粒，搅拌4小时后加入增塑剂甲基纤维素，继续搅拌1小时得到混料，为糊料、砂浆或粘稠物；整个搅拌过程的搅拌转速在100rad/min；
(4)选用自动压片机将步骤(3)得到的混料分装进模具中进行压片；模具形状为矩形(20cm*30cm)，压力在5MPa，保压时间5s，随后脱模送进窑炉进行干燥并烧制；
(5)烧制：窑炉升温制度为：室温～200℃，速率在5℃/min，保温10min；随后继续升温至400℃，速率在5℃/min，保温60min；然后随炉冷却至100℃以下取出成品。
实施例5
具体制备方法包括下列步骤：
(1)按照质量比10：1分别称取硝酸钙和柠檬酸，并溶于无水乙醇中，磁力搅拌40min，转速150r/min，形成钙的乙醇溶液；称取钛酸四正丁酯并溶于无水乙醇中，磁力搅拌30min，转速150r/min，并在搅拌过程中滴加冰醋酸，形成钛前驱体液；在搅拌条件下，将钙的乙醇溶液加入到钛前驱体液中，加入分散剂油酸，随后加入纯水、蓄光粉(选用Sr4Al14O25：Eu，Dy，粒径为200微米)，继续搅拌4h，得到蓄光粉-钛酸钙凝胶；
(2)将步骤(1)得到的蓄光粉-钛酸钙凝胶于100℃条件下加热6小时，得到钛酸钙包覆的蓄光粉干凝胶，粉碎，过100目筛待用；
(3)将粒径300微米的玻璃粉、100目干凝胶粉、分散剂三聚磷酸钠放入造粒机内，加入纯水后直接机械搅拌造粒，搅拌6小时后加入增塑剂甲基纤维素，继续搅拌2小时得到混料，为糊料、砂浆或粘稠物；整个搅拌过程的搅拌转速在200rad/min；
(4)选用自动压片机将步骤(3)得到的混料分装进模具中进行压片；模具形状为正方形(20cm*20cm)，压力在30MPa，保压时间15s，随后脱模送进窑炉进行干燥并烧制；
(5)窑炉升温制度为：室温～200℃，速率在3℃/min，保温30min；随后继续升温至800℃，速率在3℃/min，保温120min；然后随炉冷却至100℃以下取出成品。
实施例6
具体制备方法包括下列步骤：
(1)按照质量比10：1分别称取硝酸钙和柠檬酸，并溶于无水乙醇中，磁力搅拌40min，转速150r/min，形成钙的乙醇溶液；称取钛酸四正丁酯并溶于无水乙醇中，磁力搅拌40min，转速150r/min，并在搅拌过程中滴加冰醋酸，形成钛前驱体液；在搅拌条件下，将钙的乙醇溶液加入到钛前驱体液中，加入分散剂油酸，随后加入纯水、蓄光粉(选用Sr4Al14O25：Eu，Dy，粒径为400微米)，继续搅拌3h，得到蓄光粉-钛酸钙凝胶；
(2)将步骤(1)得到的蓄光粉-钛酸钙凝胶于100℃条件下加热6小时，得到钛酸钙包覆的蓄光粉干凝胶，粉碎，过100目筛待用；
(3)将粒径400微米的玻璃粉、100目干凝胶粉、分散剂三聚磷酸钠放入造粒机内，加入纯水后直接机械搅拌造粒，搅拌8小时后加入增塑剂甲基纤维素，继续搅拌2小时得到混料，为糊料、砂浆或粘稠物；整个搅拌过程的搅拌转速在150rad/min；
(4)选用自动压片机将步骤(3)得到的混料分装进模具中进行压片；模具形状为产品要求所需，压力在25MPa，保压时间15s，随后脱模送进窑炉进行干燥并烧制；
(5)窑炉升温制度为：室温～200℃，速率在2℃/min，保温30min；随后继续升温至600℃，速率在2℃/min，保温90min；然后随炉冷却至100℃以下取出成品。

Claims (6)

1.一种同时提高蓄光陶瓷光效及稳定性的方法，其特征在于，包括以下步骤：
(1)按照质量比10：0.5～1.5分别称取硝酸钙和柠檬酸，并溶于无水乙醇中，形成钙的乙醇溶液；称取钛酸四正丁酯并溶于无水乙醇中，同时在搅拌状态下滴加冰醋酸，形成钛前驱体液；在搅拌状态下，将钙的乙醇溶液加入到钛前驱体液中，加入分散剂油酸，随后加入纯水、蓄光粉，继续搅拌1～4h，得到蓄光粉-钛酸钙凝胶；
(2)将步骤(1)得到的蓄光粉-钛酸钙凝胶于80～150℃条件下加热2～8小时，得到钛酸钙包覆的蓄光粉干凝胶，粉碎，过80～200目筛待用；
(3)将玻璃基质原料、过筛的干凝胶粉、分散剂放入造粒机内，加入纯水后直接机械搅拌造粒，搅拌4～8小时后加入增塑剂，继续搅拌1～3小时得到混料；整个搅拌过程的搅拌转速在100～300rad/min；
(4)将步骤(3)得到的混料分装进模具中，利用自动压片机进行压片，模具形状为产品要求所需，压力在5～40MPa，保压时间5～20s，随后脱模送进窑炉进行干燥并烧制。
(5)窑炉升温制度为：室温～200℃，速率在2～5℃/min，保温10～30min，保证坯体水分完全蒸发；随后继续升温至400～900℃，保温60～120min；然后随炉冷却至100℃以下取出成品，即得到透光率好、余辉亮度高、有玉质观感的蓄光陶瓷。
2.根据权利要求1所述的一种同时提高蓄光陶瓷光效及稳定性的方法，其特征在于，步骤(1)中，硝酸钙与钛酸四正丁酯的质量比为1：0.8～2.5；在钙的乙醇溶液中，溶质溶液比为1：1.5～3；在钛的前驱体液中，溶质溶液比为1：0.5～2.5；冰醋酸的添加量占硝酸钙和钛酸四正丁酯的总质量比的35％～55％；分散剂油酸的添加量占硝酸钙和钛酸四正丁酯的总质量比的5％～15％；纯水的添加量与硝酸钙和钛酸四正丁酯的总质量比为1：3.5～5；蓄光粉的添加量与硝酸钙和钛酸四正丁酯的总质量比为1:8～10。
3.根据权利要求1所述的一种同时提高蓄光陶瓷光效及稳定性的方法，其特征在于，步骤(1)中，所述蓄光粉选用SrAl2O4为基质的蓄光粉，粒径为10～500微米。
4.根据权利要求1所述的一种同时提高蓄光陶瓷光效及稳定性的方法，其特征在于，步骤(3)中，所述玻璃基质原料为玻璃粉，粒径范围在10～400微米，玻璃粉添加量为90％～98％。
5.根据权利要求4所述的一种同时提高蓄光陶瓷光效及稳定性的方法，其特征在于，步骤(3)中，干凝胶粉与玻璃粉的质量比为9～49：1；分散剂的添加量占干凝胶粉和玻璃粉的总质量的0.1～0.6％；增塑剂的添加量占干凝胶粉和玻璃粉的总质量的0.1～0.9％；纯水的添加量占干凝胶粉和玻璃粉的总质量的20％～50％。
6.根据权利要求1所述的一种同时提高蓄光陶瓷光效及稳定性的方法，其特征在于，步骤(3)中，所述增塑剂为甲基纤维素，所述分散剂为三聚磷酸钠。
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