CN112341183A - 一种激光照明的荧光复合陶瓷光纤的制备方法 - Google Patents
一种激光照明的荧光复合陶瓷光纤的制备方法 Download PDFInfo
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Abstract
本发明公开了一种激光照明的荧光复合陶瓷光纤的制备方法,采用多喷嘴微挤出成型工艺同步连续生产,利用凝胶膏状浆料配制Ce3+:YAG,Mn4+:YAG和Ce3+:LuAG等不同组分的荧光陶瓷光纤材料作为黄光、红光和绿光的荧光转换照明材料,用光斑大小可调的蓝光激光器作为点光源端面激发荧光陶瓷光纤,实现单一或复合激发的光电分离的高功率照明。本发明操作简单,可实现连续化生产作业,可用于石油、化工、天然气、游泳池等安全要求高的场所,也可以用于建筑文物、医疗或实验室等特殊场所。
Description
技术领域
本发明涉及陶瓷光纤制备技术领域,具体涉及一种激光照明的荧光复合陶瓷光纤的制备方法。
背景技术
光纤照明是指透过光纤导体的传输,可以将光源传导到光纤中的任意区域里,是近年来兴起的高科技照明技术。传统光纤在照明里的应用方式分成两种,一种是端面发光,另一种是体发光。其中应用最为普遍的是端面发光,主要是由两种组件所组成:光源投射机以及光纤。在照明领域里所使用的光纤,大多数是塑料光纤,发光方式是端面发光,如室内装饰、水景照明、城市建筑、道路交通以及古建筑文物照明等。
随着激光照明光源的兴起,与传统的作为塑料光纤光源的LED相比,激光照明具有发光效率高、耗电量小、使用寿命长、工作温度低、单元体积小、安全可靠等特点。为了适应激光光源的迅猛发展必然要求一种与之相匹配的光纤照明材料。而具有立方相结构,不存在双折射现象的YAG、LuAG作为基质材料的透明陶瓷材料凭借高热导率、成型灵活、可高掺杂的特点能很好的适应光纤材料的要求。其中高掺杂的特性非常有助于Ce3+、Mn3+、Gd3+、Pr3+等稀土离子、过渡金属离子等高浓度掺杂,从而在蓝色激光激发下,形成各种颜色的荧光陶瓷光纤。更为重要的是,分别发射黄光、红光和绿光的Ce3+:YAG,Mn4+:YAG和Ce3+:LuAG等不同组分的荧光陶瓷光纤可以进一步复合形成色温、光效可调的白光,适用于室内等场合。
目前尚未有用于激光照明的荧光陶瓷光纤的报道。在制备方法上也大都为挤出成型、凝胶注模、注浆成型等方法,一次只能制备一条光纤,生产效率低。且LED光源不具备激光光源光斑的单色性好、光斑大小可调等优势。
发明内容
本发明的目的是提供一种激光照明的荧光复合陶瓷光纤的制备方法。
为实现上述目的,本发明采用的技术方案如下:一种激光照明的荧光复合陶瓷光纤的制备方法,包括如下步骤:
S1、按照透明陶瓷材料分子式中各元素的化学计量比称取高纯氧化物原料粉体,除杂预处理,所述透明陶瓷材料为稀土离子或过渡金属离子掺杂的YAG透明陶瓷、稀土离子或过渡金属离子掺杂的LuAG透明陶瓷中的一种或多种;
S2、将所述原料粉体混合并加入烧结助剂、磨球、溶剂组成预混液,放入球磨罐中混合球磨,得到混合浆料;
S3、球磨结束后将混合浆料烘干,过筛,再放入马弗炉中煅烧,得到凝胶注模成型的陶瓷原料粉;
S4、使用上述原料粉配制凝胶成型体系所需浆料,浆料固含量为50vol.%以上,真空除泡后注入微型挤出机的不同储料室,通过柱塞泵的高压强挤出,干燥后形成各种荧光陶瓷光纤素坯;
S5、上述光纤依次进行排胶、真空烧结、抛光处理,得到直径几十到几百微米的荧光陶瓷光纤;
S6、采用激光器作为点光源端面激发荧光陶瓷光纤,满足光电分离及通过调节光斑大小和强度来满足照明需求。
优选的,步骤S2中,所述烧结助剂为MgO和/或SiO2,烧结助剂的加入量为陶瓷原料粉体总质量的0.5%;所述磨球为高纯Al2O3磨球,球料比为1~3:1;所述溶剂为无水乙醇;球磨转速为120-160r/min,球磨时间为24-36h。
优选的,步骤S3中,所述烘干的温度为40~100℃,时间为24~48h。
优选的,步骤S3中,所述过筛的筛网目数为100~200目。
优选的,步骤S3中,所述煅烧的温度为800~1000℃,保温时间为8~24h。
优选的,步骤S4中,所述的凝胶成型体系为AM(丙烯酰胺)、PIBM(异丁烯和马来酸酐的共聚物)和MAM(甲基丙烯酰胺)凝胶体系中的一种。
优选的,步骤S4中,所述干燥工艺为在100~120℃的烘箱中干燥4~8h。
优选的,步骤S5中,所述排胶的参数为:室温下以升温速率为0.5~2℃/分钟升温到450℃,再以升温速率为0.5~3℃/分钟升温到800℃,并在800℃保温2~6h。
优选的,步骤S5中,所述真空烧结的参数为:首先按5~10℃/min从室温升温到200℃并保温10~30min,其次按10~20℃/min升温到1000℃并保温10~30min,然后按1~5℃/min升温到1650℃并保温6~10h,最后以5~10℃/min降温到室温,整个烧结过程中真空度保持在1×10-2~1×10-5Pa。
与现有技术相比,本发明具有如下有益效果:
1.本发明提供的制备方法,采用多喷嘴微挤出成型工艺同步连续生产,利用凝胶膏状浆料配制Ce3+:YAG,Mn4+:YAG和Ce3+:LuAG等不同组分的荧光陶瓷光纤材料作为黄光、红光和绿光的荧光转换照明材料,生产效率高;
2.本发明提供的制备方法,只需通过调节激光光源的直径大小和位置就可以根据具体需要激发荧光光纤产生不同颜色甚至可复合成白光,操作简单,便于数字化控制,实现光电分离、色彩可调可控的远程照明。
附图说明
图1实施例3中的激光照明荧光复合陶瓷光纤的结构原理图。
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。
以下实施例中所使用的原料粉体均为高纯纳米粉体,纯度>99.99%。
实施例1
一种用于激光照明的荧光复合陶瓷光纤的制备方法,它包括以下步骤:
S1、按照0.01%Ce3+:YAG分子式中各元素的化学计量比分别称量高纯纳米Y2O3粉体71.315g、高纯纳米α-Al2O3粉体53.674g,高纯纳米CeO2粉体0.011g,除杂预处理;
S2、使用烧结助剂SiO20.75g、高纯Al2O3磨球450g、无水乙醇180ml、充分搅拌后放入球磨罐中,在160r/min转速下混合球磨24h均匀后得到混合浆料;再将混合浆料置于40℃恒温烘箱中烘48h后过200目筛,将过筛后的粉体置于马弗炉中煅烧,从室温升温到1000℃,保温8h后自然冷却,作为光纤成型的原料粉;
S3、采用AM(丙烯酰胺)凝胶体系,在34.5g去离子水中,加入AM有机单体7.5g,交联剂N,N-亚甲基双丙烯酰胺0.624g,用氨水调节pH到10,再加入分散剂柠檬酸铵0.45g,催化剂过硫酸铵0.15g,最后加入原料粉150g后充分球磨,制备固含量为50vol.%的陶瓷浆料,再加入1.5g的增塑剂聚乙烯醇后,用真空除泡机进行除泡处理后作为挤出成型所需的浆料;
S4、将此浆料注入微型挤出机的储量室,用50MPa的柱塞泵的压力挤出,通过直径80μm的喷嘴得到Ce3+:YAG荧光陶瓷光纤素坯;
S5、将素坯进行干燥处理:放入100℃烘箱中保温8h;干燥后进行排胶处理,从室温开始以2℃/min升温速度到450℃,再以3℃/min升温速度到800℃,并保温6h;最后真空烧结,室温开始以10℃/min升温到200℃,保温10min,再次按10℃/min升温到1000℃并保温10min,然后按5℃/min升温到1650℃并保温6h,最后以5℃/min降温到室温,整个烧结过程中真空度保持在1×10-2Pa。再经过抛光处理,得到约80μm Ce3+:YAG发黄光的陶瓷光纤;
S6、采用蓝色激光器激发,调节光斑直径大小至80μm左右端面激发一根Ce3+:YAG荧光陶瓷光纤,通过激光器功率的强弱调节照明的颜色。
实施例2
一种用于激光照明的荧光复合陶瓷光纤的制备方法,它包括以下步骤:
S1、先按照实施例1中的步骤S1-S3制备Ce3+:YAG荧光陶瓷光纤所需浆料;
S2-1、按照0.2%Mn3+:YAG分子式的化学计量比分别称量高纯纳米Y2O3粉体85.447g、高纯纳米Al2O3粉体64.433g,高纯纳米Mn2O3粉体0.120g,除杂预处理;
S2-2、使用烧结助剂MgO 0.75g、高纯Al2O3磨球450g、无水乙醇180ml、充分搅拌后放入球磨罐中,在120r/min转速下混合球磨36h均匀后得到混合浆料;将混合浆料置于100℃恒温烘箱中烘24h后过150目筛,将过筛后的粉体置于马弗炉中煅烧,从室温升温到800℃,保温24h后自然冷却,作为光纤成型的原料粉;
S2-3、采用PIBM凝胶体系,在30g的去离子水中,加入Isobam104#0.45g,用四甲基氢氧化铵调节pH到11,采用柠檬酸铵分散剂0.30g,并加入原料粉150g后充分球磨,制备固含量为52vol.%的陶瓷浆料,再加入7.5g增塑剂聚氯乙烯后,用真空除泡机进行除泡处理后作为挤出成型所需的浆料;
S3、将步骤S1和步骤S2-3得到的两种浆料分别注入微型挤出机的不同储量室,用100MPa的柱塞泵的压力挤出,通过两个直径100μm的喷嘴同步得到Ce3+:YAG和Mn4+:YAG荧光陶瓷光纤素坯;
S4、将两种素坯同时进行干燥处理:放入120℃烘箱中保温4h;干燥后进行排胶处理,从室温开始以0.5℃/min升温速度到450℃,再以0.5℃/min升温速度到800℃,并保温2h;最后真空烧结,室温开始以5℃/min升温到200℃,保温30min,再次按20℃/min升温到1000℃并保温30min,然后按1℃/min升温到1650℃并保温10h,最后以10℃/min降温到室温,整个烧结过程中真空度保持在1×10-5Pa。再经过抛光处理,得到约100μm发黄光的Ce3+:YAG和发红光的Mn4+:YAG陶瓷光纤;
S5、采用蓝色激光器激发,调节光斑直径大小至100μm左右可端面激发一根Ce3+:YAG或Mn4+:YAG荧光陶瓷光纤,若扩大光斑直径大小(>200μm)同时激发两种光纤并通过激光器功率的强弱调节照明的颜色。
实施例3
一种用于激光照明的荧光复合陶瓷光纤的制备方法,它包括以下步骤:
S1、先按照实施例1中的步骤S1-S3制备Ce3+:YAG荧光陶瓷光纤所需浆料;
S2、先按照实施例2中的步骤S2-1~S2-3制备Mn4+:YAG荧光陶瓷光纤所需浆料;
S3-1、按照0.2%Ce3+:LuAG分子式的化学计量比分别称量高纯纳米Lu2O3粉体(纯度>99.99%)69.99g、高纯纳米Al2O3粉体(纯度>99.99%)29.95g,高纯纳米CeO2粉体(纯度>99.99%)0.06g,除杂预处理;
S3-2、使用烧结助剂SiO20.4g、MgO0.1g,高纯Al2O3磨球300g、无水乙醇120ml、充分搅拌后放入球磨罐中,在150r/min转速下混合球磨30h均匀后得到混合浆料;将混合浆料置于60℃恒温烘箱中烘36h后过100目筛,将过筛后的粉体置于马弗炉中煅烧,从室温升温到900℃,保温12h后自然冷却,作为光纤成型的原料粉;
S3-3、采用MAM凝胶体系,在15g的去离子水中,加入MAM有机单体4g,交联剂二丙烯基酒石酸二酰胺(DATDA)0.4g,用四甲基氢氧化铵调节pH到11,加入原料粉100g后充分球磨,制备固含量为55vol.%的陶瓷浆料,再加入2g增塑剂聚乙烯亚胺后,用真空除泡机进行除泡处理后作为挤出成型所需的浆料;
S4、将步骤S1、S2和S3-3制得的三种浆料分别注入微型挤出机的不同储量室,用80MPa的柱塞泵的压力挤出,通过三个直径50μm的喷嘴同步得到Ce3+:YAG、Mn4+:YAG和Ce3+:LuAG荧光陶瓷光纤素坯;
S5、将三种素坯进行干燥处理:放入110℃烘箱中保温6h;干燥后进行排胶处理,从室温开始以1℃/min升温速度到450℃,再以2℃/min升温速度到800℃,并保温4h;最后真空烧结,室温开始以8℃/min升温到200℃,保温20min,其次按15℃/min升温到1000℃并保温20min,然后按3℃/min升温到1650℃并保温8h,最后以8℃/min降温到室温,整个烧结过程中真空度保持在1×10-3Pa。再经过抛光处理,得到约50μm发黄光Ce3+:YAG、发红光Mn4+:YAG和发绿光Ce3+:LuAG的陶瓷光纤;
S6、采用蓝色激光器激发,调节光斑直径大小至50μm左右可端面激发一根Ce3+:YAG或Mn4+:YAG或Ce3+:LuAG荧光陶瓷光纤;若扩大光斑直径大小(>150μm)可同时激发三种光纤并通过激光器功率的强弱调节照明的颜色;
图1为本发明实施例3中的激光照明荧光复合陶瓷光纤的结构原理图。最里层为发黄光的Ce3+:YAG陶瓷光纤,中间层为发红光的Mn4+:YAG陶瓷光纤,最外层为发绿光的Ce3+:LuAG陶瓷光纤。激光器发射蓝色激光光束,若需要单色光则调节光斑大小与其中一根荧光陶瓷光纤直径相一致,强度满足所需照明颜色要求;若需要复合则可调节光斑直径和强度同时激发二~三种荧光陶瓷光纤。
Claims (9)
1.一种激光照明的荧光复合陶瓷光纤的制备方法,其特征在于,包括如下步骤:
S1、按照透明陶瓷材料分子式中各元素的化学计量比称取高纯氧化物原料粉体,除杂预处理,所述透明陶瓷材料为稀土离子或过渡金属离子掺杂的YAG透明陶瓷、稀土离子或过渡金属离子掺杂的LuAG透明陶瓷中的一种或多种;
S2、将所述原料粉体混合并加入烧结助剂、磨球、溶剂组成预混液,放入球磨罐中混合球磨,得到混合浆料;
S3、球磨结束后将混合浆料烘干,过筛,再放入马弗炉中煅烧,得到凝胶注模成型的陶瓷原料粉;
S4、使用上述原料粉配制凝胶成型体系所需浆料,浆料固含量为50vol.%以上,真空除泡后注入微型挤出机的不同储料室,通过柱塞泵的高压强同步挤出,干燥后形成各种荧光陶瓷光纤素坯;
S5、将得到的光纤素坯依次进行排胶、真空烧结、抛光处理,得到直径几十到几百微米的荧光陶瓷光纤;
S6、采用激光器作为点光源端面激发荧光陶瓷光纤,满足光电分离及通过调节光斑大小和强度来满足照明需求。
2.根据权利要求1所述的一种激光照明的荧光复合陶瓷光纤的制备方法,其特征在于,步骤S2中,所述烧结助剂为MgO和/或SiO2,烧结助剂的加入量为陶瓷原料粉体总质量的0.5%;所述磨球为高纯Al2O3磨球,球料比为1~3:1;所述溶剂为无水乙醇;球磨转速为120~160r/min,球磨时间为24~36h。
3.根据权利要求1所述的一种激光照明的荧光复合陶瓷光纤的制备方法,其特征在于,步骤S3中,所述烘干的温度为40~100℃,时间为24~48h。
4.根据权利要求1所述的一种激光照明的荧光复合陶瓷光纤的制备方法,其特征在于,步骤S3中,所述过筛的筛网目数为100~200目。
5.根据权利要求1所述的一种激光照明的荧光复合陶瓷光纤的制备方法,其特征在于,步骤S3中,所述煅烧的温度为800~1000℃,保温时间为8~24h。
6.根据权利要求1所述的一种激光照明的荧光复合陶瓷光纤的制备方法,其特征在于,步骤S4中,所述的凝胶成型体系为丙烯酰胺、PIBM和甲基丙烯酰胺凝胶体系中的一种。
7.根据权利要求1所述的一种激光照明的荧光复合陶瓷光纤的制备方法,其特征在于,步骤S4中,所述干燥工艺为在100~120℃的烘箱中干燥4~8h。
8.根据权利要求1所述的一种激光照明的荧光复合陶瓷光纤的制备方法,其特征在于,步骤S5中,所述排胶的参数为:室温下以升温速率为0.5~2℃/分钟升温到450℃,再以升温速率为0.5~3℃/分钟升温到800℃,并在800℃保温2~6h。
9.根据权利要求1所述的一种激光照明的荧光复合陶瓷光纤的制备方法,其特征在于,步骤S5中,所述真空烧结的参数为:首先按5~10℃/min从室温升温到200℃并保温10~30min,其次按10~20℃/min升温到1000℃并保温10~30min,然后按1~5℃/min升温到1650℃并保温6~10h,最后以5~10℃/min降温到室温,整个烧结过程中真空度保持在1×10-2~1×10-5Pa。
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CN211542274U (zh) * | 2019-12-23 | 2020-09-22 | 湖北华隆橡塑制品有限公司 | 一种具有恒温热度板的光缆填充料生产挤出成型装置 |
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CN116332646A (zh) * | 2023-04-11 | 2023-06-27 | 江苏师范大学 | 一种激光照明用高光效荧光复合陶瓷及其制备方法 |
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