CN112573907B - 一种轻质发光块体的制备方法 - Google Patents
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Abstract
一种轻质发光块体的制备方法，它包括发光材料颗粒、轻质助剂、硬质助剂，其特征在于：发光材料颗粒、轻质助剂、硬质助剂充分混合，轻质助剂是由孔连剂、稳定剂、助溶剂按比例混合构成；发光材料颗粒、轻质助剂、硬质助剂混合后制备成各种形状的块体或颗粒，在高温500‑1300度中烧结3‑10小时，再使用表面处理剂处理，形成孔径1‑10微米的多孔的轻质发光块体。轻质发光块体内部不规则分布有1‑100微米的封闭孔洞，大量的气孔可以使得轻质发光块体表面积增加1.5倍，提高了发光强度，并可漂浮于液体中，表面状态稳定、透光性与发光效率高，轻质发光块体或发光颗粒能加工可形成透明或半透明任意形体。
Description
技术领域
本发明属于发光材料制备与显示照明应用领域。
技术背景
现阶段无机类发光材料制备是建立在无机微晶粉末合成基础上，其包括微米颗粒、纳米颗粒，它们的共同特性是具备独立的晶体结构，发光效率依赖于完整的晶体结构与独立的表面状态，使用时需具备良好分撒特性，它们经常被喷涂成薄膜，或与塑料混合压板。通常发光材料的密度比重与其无机微晶结构主体成分质量比重对应，比重集中在3-6g/cm³，由于无机发光材料的质量比重较大，其应用工艺过程中需要不断搅拌；当与塑料或玻璃混合制成形体后激发其发光也仅处于表面。
本发明一种轻质发光块体的制备方法，它包括发光材料颗粒、轻质助剂、硬质助剂，其特征在于：发光材料颗粒、轻质助剂、硬质助剂充分混合，轻质助剂是由孔连剂、稳定剂、助溶剂按比例混合构成；发光材料颗粒、轻质助剂、硬质助剂混合后制备成各种形状的块体或颗粒，在高温500-1300度中烧结30分钟，再使用表面处理剂处理，形成孔径1-10微米的多孔的轻质发光块体。
本发明优点在于：轻质发光块体内部不规则分布有1-100微米的封闭孔洞，大量的气孔可以使得轻质发光块体表面积增加1.5倍，提高了发光强度，并可漂浮于液体中，其稳定性好、不团聚、不沉淀，表面状态稳定、透光性与发光效率高，轻质发光块体或发光颗粒能加工可形成透明或半透明任意形体。可广泛应用于照明、显示、发光领域。
发明内容
一种轻质发光块体的制备方法，它包括发光材料颗粒、轻质助剂、硬质助剂，其特征在于：发光材料颗粒、轻质助剂、硬质助剂充分混合，轻质助剂是由孔连剂、稳定剂、助溶剂按比例混合构成；发光材料颗粒、轻质助剂、硬质助剂混合后制备成各种形状的块体或颗粒，在高温500-1300度中烧结3-10小时，再使用表面处理剂处理，形成孔径1-10微米的多孔的轻质发光块体。本发明中制备的轻质发光块体与现有制备技术获得的材料相比较，相同体积时本发明的材料重量明显轻0.3-2倍；或者是相同重量比较下本发明发光块体或颗粒体积明显大于传统发光产品，发光强度因块体或颗粒内部透明或半透明对激发光穿透与折射效率高于原有材料20%以上。
本发明中的轻质发光块体中按重量比含有80%的发光材料颗粒，含有重量比为10%的轻质助剂，含有重量比为10%的硬质助剂。轻质助剂添加多可促使发光块体颗粒体积增大，发光材料颗粒添加量增大可提高发光强度，发光材料颗粒度与轻质助剂颗粒度越小则有利于形成更小的轻质发光颗粒。发光材料颗粒与轻质助剂均匀充分混合，混合方式可以是液态混合或粉体物理混合，如搅拌、球磨等。可通过磨具压制成各种形状块体，也可制备成直径微米或厘米级的颗粒，根据需要控制颗粒大小。随后在高温中烧结，轻质助剂在颗粒内部形众多成封闭气孔，较好的温度在500-1300度中烧结3-10小时形成轻质上转换发光颗粒，烧结次数可以多次形成，缓慢升温烧结有利于气孔形成。烧结时可以根据材料的成分在保护气氛、真空、空气环境下实施。
本发明中的硬质助剂是KAlSi3O8或NaAlSi3O8或CaAl2Si2O8中的一种，硬质助剂粉碎成颗粒度为1-100微米粉体，以硅铝石为主成分的硬质助剂可以提高轻质发光块体或颗粒的硬度及耐候性，适合户外使用。
本发明中的轻质助剂中的孔连剂是氟化钠、氟化钙、硼酸中的一种，孔连剂可以使得气孔在发光材料颗粒度间形成封闭连接，孔连剂颗粒度越小形成的颗粒也越小，小于10微米效果较好，颗粒纳米尺度会更好，孔连剂的加入量占轻质助剂总重量的40%。
本发明中的轻质助剂中的稳定剂是氧化铝、氧化硅、氧化钛中的至少一种，稳定剂可隔离发光材料颗粒，形成均一的气孔，稳定剂颗粒大小较为重要，通常颗粒度小于50微米，颗粒纳米尺度会更好。稳定剂的加入量为轻质助剂总重量的40%。氧化铝、氧化硅、氧化钛使用熔胶凝法获得的颗粒较小。
本发明中的轻质助剂中的助溶剂是碳酸钙、碳酸钠中的一种，助溶剂高温分解形成气孔，其可以降低孔连剂的温度，助溶剂粒径越小气孔也就小并均匀，助溶剂物理方法粉碎后颗粒度为10-50纳米；助溶剂的加入量为轻质助剂总重量的20%。
本发明中的发光材料颗粒是无机高温制备的发光材料粉体，粉体颗粒度1-50微米，发光材料粉体是光致发光材料、阴极射线发光材料、长余辉发光材料、电致发光材料、X射线发光材料、上转换发光材料、红外发光材料中的一种。无机发光材料制备是高温烧结形成粉体。它们可以制备成夜光板，LED白光、X射线成像板多孔荧光转换片等，并可漂浮在水面。
本发明中的表面处理剂是硅酸钾或硅酸钠中的一种，表面处理剂的水溶液涂敷在轻质发光材料表面，密封表面裸露微孔并干燥，使得表面平滑，同时其它液体无法扩散到孔中。
具体实施方法
一种轻质发光块体的制备方法，它包括发光材料颗粒、轻质助剂、硬质助剂，其特征在于：发光材料颗粒、轻质助剂、硬质助剂充分混合，轻质助剂是由孔连剂、稳定剂、助溶剂按比例混合构成；发光材料颗粒、轻质助剂、硬质助剂混合后制备成各种形状的块体或颗粒，在高温500-1300度中烧结30分钟，再使用表面处理剂处理，形成孔径1-10微米的多孔的轻质发光块体，发光材料颗粒越大气孔性相对越好。
本发明中的轻质发光块体中按重量比含有80%的发光材料颗粒，含有重量比为10%的轻质助剂，含有重量比为10%的硬质助剂，具有较好发光效率及体积。轻质助剂添加多可促使气孔多发光颗粒体积增大，发光材料颗粒添加量增大可提高发光强度，有利于发光。发光材料颗粒度与轻质助剂颗粒度越小则有利于形成更小的轻质发光颗粒。发光材料颗粒、轻质助剂、硬质助剂充分混合，混合方式可以是液态混合或粉体物理混合，如搅拌、球磨等，混合均匀对气孔分布与大小有直接关联。通常气孔在1-100微米，如果混合不均匀气孔直径可以达到毫米级，影响轻质上转换发光颗粒度。在高温中烧结，轻质助剂在颗粒内部形众多成封闭气孔，较好的温度在500-1300度中烧结3-10小时形成轻质发光块体与颗粒，烧结时缓慢阶梯升温有利于气孔形成，烧结时可以根据材料的成分在保护气氛、真空、空气环境下实施。
本发明中的轻质助剂中的孔连剂是氟化钠、氟化钙、硼酸中的一种，优级纯有较少杂质，氟化物更有利于发光，尤其氟化钠。硼酸可以提高稳定性。它们可以研磨或溶解后构成轻质助剂一部分，市售试剂产品均可以使用。孔连剂颗粒度越小形成的颗粒也越小，小于10微米效果较好，孔连剂的加入量占轻质助剂总重量的40%。
本发明中的轻质助剂中的稳定剂是氧化铝、氧化硅、氧化钛中的至少一种，加入量占轻质助剂总重量的40%。纳米氧化硅更有利于透明，纳米氧化铝更有利于气孔的均匀。稳定剂可隔离纳米上转换发光材料颗粒，形成均一的气孔，稳定剂颗粒大小较为重要，颗粒度20-30微米较好。
本发明中的轻质助剂中的助溶剂是碳酸钙、碳酸钠中的一种，助溶剂高温分解形成气孔，其可以降低孔连剂的温度，助溶剂粒径越小气孔也就小并均匀，助溶剂物理方法粉碎时尽量保持密封状态，其成分可以保持气孔的生率，颗粒度为10-30微米较好；助溶剂的加入量为轻质助剂总重量的20%。
本发明中的发光材料颗粒是无机高温制备的发光材料粉体，粉体颗粒度1-50微米，发光材料粉体是光致发光材料，如紫外发光材料；发光材料粉体是阴极射线发光材料；发光材料粉体是长余辉发光材料，如制造成漂浮夜光板；发光材料粉体是电致发光材料，发光材料粉体是X射线发光材料，如射线成像板；发光材料粉体是上转换发光材料、；发光材料粉体是红外发光材料中的一种。无机发光材料制备是高温烧结形成粉体。它们可以制备成夜光板，LED白光、X射线成像板多孔荧光转换片等，并可漂浮在水面。
本发明中的表面处理剂是硅酸钾或硅酸钠中的一种，常温或120度烘干，表面处理剂的水溶液涂敷在轻质发光材料表面，密封表面裸露微孔，提高寿命，并使得表面平滑，防止水渗入。
本发明优点
1.轻质发光块体可以漂浮于液体中，其稳定性好、不团聚、不沉淀，表面状态稳定，颗粒度根据需要可以控制，制备成水上漂浮夜光浮漂，其寿命高于塑料，可以使用20年以上。
2.轻质上转换发光颗粒透光性与发光效率高，轻质上转换发光颗粒加工可形成透明或半透明任意形体，如制造成平板射线成像，其整体可以漂浮在水面，同时硬度也较高，是塑料制品的2-3倍，可以用于道路警示，建筑表面。表面积增大可以接受更多的激发光。
3.可广泛应用于照明、显示、发光、生物免疫分析、疾病诊断、药物筛选、显微成像、防伪油墨、红外激光探测等领域。其可以制备成陶瓷发光，具有硬度高于单纯稀土结晶2-3倍。
具体实施例
取颗粒度30微米米的绿色铝酸盐长余辉发光材料颗粒80克，加入硼酸4克，氧化硅4克，碳酸钙2克，硬质助剂加入的是KAlSi3O8充分混合，压制成20毫米厚板，在高温1000度氮气保护中烧结4小时，取出冷却后表面喷涂硅酸钾，干燥24小时。
在上面针对本发明较好的实施方式作了举例说明后，对本领域的技术人员来说应明白的是，在不偏离本发明的精神和范围的情况下，对本发明所作的任何改变和改进都在本发明的范围内。
Claims (1)
1.一种轻质发光块体的制备方法，它由发光材料颗粒、轻质助剂、硬质助剂组成，其特征在于：发光材料颗粒、轻质助剂、硬质助剂充分混合，在高温500-1300度中烧结3-10小时，再使用表面处理剂处理，形成孔径1-10微米的多孔的轻质发光块体；轻质助剂是由孔连剂、稳定剂、助溶剂按比例混合构成；发光材料颗粒、轻质助剂、硬质助剂混合后制备成各种形状的块体；轻质发光块体中按重量比含有80%的发光材料颗粒，含有重量比为10%的轻质助剂，含有重量比为10%的硬质助剂；硬质助剂是KAlSi3O8或NaAlSi3O8或CaAl2Si2O8中的一种，硬质助剂粉碎成颗粒度为1-100微米粉体；轻质助剂中的孔连剂是氟化钠、氟化钙、硼酸中的一种，孔连剂颗粒度小于10微米，孔连剂的加入量为轻质助剂重量的40%；轻质助剂中的稳定剂是氧化铝、氧化硅、氧化钛中的至少一种，稳定剂颗粒度小于50微米，稳定剂的加入量为轻质助剂重量的40%；轻质助剂中的助溶剂是碳酸钙、碳酸钠中的一种，助溶剂粉碎后颗粒度为10-50微米；助溶剂的加入量为轻质助剂重量的20%；发光材料颗粒是无机高温制备的发光材料粉体，粉体颗粒度1-50微米，发光材料粉体是光致发光材料、阴极射线发光材料、长余辉发光材料、电致发光材料、X射线发光材料、上转换发光材料、红外发光材料中的一种；表面处理剂是硅酸钾或硅酸钠中的一种，表面处理剂的水溶液涂敷在轻质发光材料表面，干燥后密封表面裸露微孔；大量的气孔可以使得轻质发光块体表面积增加1.5倍，提高了发光强度，并可漂浮于液体中。
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