CN113248256B - 一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法 - Google Patents

一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法 Download PDF

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CN113248256B
CN113248256B CN202110498820.8A CN202110498820A CN113248256B CN 113248256 B CN113248256 B CN 113248256B CN 202110498820 A CN202110498820 A CN 202110498820A CN 113248256 B CN113248256 B CN 113248256B
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姚庆
孔璐璐
田俊杰
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Nantong University
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Abstract

本发明公开了一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法，属于光纤制备技术领域。所述用于陶瓷光纤挤出成型的强韧性膏料的配制方法，具体是先将特制的粘结剂和凝胶剂按一定比例混合，并经过混合机、混炼机、挤出机等机器，充分混合后，制备出一种运用挤出成型得到陶瓷光纤的强韧性膏料。本发明提供的一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法，结合了KL‑7系列粘结剂“流塑特性”和Isobam凝胶剂能够提供的三维网格内部结构，有助于提高成品韧性的特点，挤出制备强韧性陶瓷光纤素坯。

Description

一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法
技术领域
本发明属于光纤制备技术领域，具体涉及一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法。
背景技术
自1995年制备出世界上首块激光透明陶瓷以来，透明陶瓷以其可高浓度稀土离子的均匀掺杂、热导率高、生产周期短、成本低、易实现极限尺寸，为激光增益介质提供了充分的设计灵活性，使得激光器件向多元化、多功能化发展。目前，在光纤新材料选择和制备方面，美国空军实验室的科学家利用透明陶瓷材料，成功实现了直径30μm陶瓷光纤的制备和微、宏观表征，验证了作为光纤激光器增益介质的可行性。
陶瓷光纤所用的材料是最具有代表性的钇铝石榴石结构(Y3Al5O12，YAG)透明陶瓷，具有用途广泛、光学性能好、量子效率高等优势，其良好的物化性能很好地适应高功率光纤激光器的要求。
然而，目前关于YAG陶瓷光纤制备的文献或专利不多，主要集中在日本Ikesue和美国空军实验室Kim、Fair等人的挤出成型和纺丝成型，以及上海光机所张龙、姜本学等人的注浆成型等(专利CN 104451953 B)。经过前期调研，专利CN 112390641A一种基于3D凝胶打印技术的YAG透明陶瓷光纤制备方法中提到了3D凝胶打印技术是较为创新的一种制备方法，但其制备原料的选择和操作流程相比较为复杂，设备条件高；西南技术物理研究所提及的有稀土离子掺杂的陶瓷光纤(专利CN 105565810A)和采用Isobam凝胶态浸涂技术(CN112341184A)，其也由于原料配比方面的缺陷易造成成型后韧性方面不足。
在YAG透明陶瓷光纤制备过程中，既要利用凝胶注模高素坯强度、净几尺寸、有机物少的特点，又要解决光纤柔韧性不足的问题。因此，非常有必要设计出适用于陶瓷光纤挤出成型的强韧性膏料来制备陶瓷光纤，使陶瓷光纤韧性好，成型体完整、不断裂。在传统的陶瓷挤出成型工艺中，为改善超细陶瓷光纤的可塑性及润滑性，强韧性膏料配方研发迫在眉睫。
发明内容
本发明的目的是提供一种陶瓷光纤强韧性膏料的配制方法，膏料使用一体型粘结剂，成型性良好，挤出成型的陶瓷光纤易加工，烧结后无残留。
为了实现上述发明目的，本发明采用以下技术方案：
一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法，先将特制的粘结剂和凝胶剂按一定比例混合，并经过混合机、混炼机、挤出机等机器，充分混合后，制备出一种运用挤出成型得到陶瓷光纤的强韧性膏料。具体包括如下步骤：
步骤一、按照透明陶瓷材料Y3Al5O12分子式的化学计量比称取高纯氧化物原料粉体，除杂预处理；
步骤二、向步骤一的原料粉体中加入由南昌虹盾技术材料有限公司生产的KL系列粉体粘结剂组成预混粉体，在混合机中进行粉体混合；
步骤三、向Isobam凝胶剂粉体中加入去离子水、分散剂，得到预混液；
步骤四、将预混液中加入烧结助剂和步骤二得到的混合粉体，在捏合机中进行充分混合，得到混合膏料；
步骤五、将混合膏料放进混炼机进行混炼，经熟化处理即可得到可实现挤出成型所需的强韧性膏料。
优选地，步骤一中，所述原料粉体为高纯的氧化铝(Al2O3)和氧化钇(Y2O3)(纯度99.99％以上)；除杂处理采用煅烧方法。
优选地，步骤二中，所述KL系列粉体粘结剂为KL-86L、KL-72M1或KL-56A的一种或几种的组合。
优选地，步骤三中，所述预混液中Isobam凝胶剂粉体占比20～25wt.％。
优选地，步骤四中，所述烧结助剂为MgO、SiO2中的一种或两种的组合。
优选地，步骤五中，所述熟化处理是将膏料用保鲜膜包裹好，放入温度10～20℃、湿度80～90％的恒温恒湿箱里面进行熟化处理24～48h。
将上述得到的强韧性膏料作为挤出机等挤出成型工艺设备的原料应用，通过挤出成型工艺制成凝胶固化的陶瓷光纤，经干燥、排胶、真空烧结、抛光处理，得到陶瓷光纤成品。
具体地：所述干燥工艺是在100～120℃的烘箱中干燥4～8h；所述排胶为室温～450℃升温速度为0.5～2℃/min，450～800℃升温速度为0.5～3℃/min，在800℃保温2～6h；所述真空烧结工艺为：室温下首先按5～10℃/min升温到200℃，保温10～30min，再按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，本发明具有如下的有益效果：
1.本发明提供的一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法，结合了KL-7系列粘结剂“流塑特性”和Isobam凝胶剂能够提供的三维网格内部结构，有助于提高成品韧性的特点，挤出制备强韧性陶瓷光纤。
2.本发明提供的一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法，强韧性膏体挤出成型后，塑性韧性良好、成型体完整、不断裂。
3.本发明可替代陶瓷光纤制备时的复杂混合原料，可解决挑选复合粘结剂困难的问题，可操作性强，可实现工业化。
附图说明
图1是实施例1挤出成型后的强韧性的YAG陶瓷光纤素坯实物图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清晰，结合具体实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，但不应以此限制本发明的保护范围。
实施例1
一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法，它包括以下步骤：
步骤一、按照Y3Al5O12分子式的化学计量比分别称量高纯纳米Y2O3粉体(纯度>99.99％)21.47g、高纯纳米Al2O3粉体(纯度>99.99％)28.53g，除杂预处理；
步骤二、在陶瓷粉体中加入KL-86L 0.25g在混合机内充分混合；
步骤三、采用PIBM凝胶注模体系，在24g的去离子水中，加入Isobam104#4.8g，用四甲基氢氧化铵调节pH到11，采用柠檬酸铵分散剂0.20g，混合后得到预混液；
步骤四、在预混液中加入烧结助剂SiO2 0.25g、混合粉体，充分搅拌后放入捏合机中，捏合24h均匀后得到混合膏料；
步骤五、将混合膏料放进混炼机混炼24h后，用保鲜膜包裹好，放入温度10℃，湿度80％的恒温恒湿箱里面进行熟化处理24h制备出强韧性陶瓷膏料；
将此膏料作为挤出机等挤出成型工艺设备的原料，通过挤出成型工艺制成凝胶固化的陶瓷光纤。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2h。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10h，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50μmYAG透明陶瓷光纤。
图1为成型后的强韧性的YAG陶瓷光纤素坯实物图(可打圈，直径800μm)。
实施例2
一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法，它包括以下步骤：
步骤一、按照Y3Al5O12分子式的化学计量比分别称量高纯纳米Y2O3粉体(纯度>99.99％)42.94g、高纯纳米Al2O3粉体(纯度>99.99％)57.06g，除杂预处理；
步骤二、在陶瓷粉体中加入KL-72M1 0.5g在混合机内充分混合；
步骤三、采用PIBM凝胶注模体系，在50g的去离子水中，加入Isobam104#10g，用四甲基氢氧化铵调节pH到11，采用柠檬酸铵分散剂0.40g，混合后得到预混液；
步骤四、在预混液中加入烧结助剂MgO 0.5g、混合粉体，充分搅拌后放入捏合机中，捏合24h均匀后得到混合膏料；
步骤五、将混合膏料放进混炼机混炼24h后，用保鲜膜包裹好，放入温度15℃，湿度85％的恒温恒湿箱里面进行熟化处理36h制备出强韧性陶瓷膏料。
将此膏料作为螺旋式挤出机等挤出成型工艺设备的原料，通过挤出成型工艺制成凝胶固化的陶瓷光纤。将素坯进行干燥处理：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6h。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50μmYAG透明陶瓷光纤。
实施例3
一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法，它包括以下步骤：
步骤一、按照Y3Al5O12分子式的化学计量比分别称量高纯纳米Y2O3粉体(纯度>99.99％)21.47g、高纯纳米Al2O3粉体(纯度>99.99％)28.53g，除杂预处理；
步骤二、在陶瓷粉体中加入KL-56A 0.25g在混合机内充分混合；
步骤三、采用PIBM凝胶注模体系，在24g的去离子水中，加入Isobam104#5.4g，用四甲基氢氧化铵调节pH到11，采用柠檬酸铵分散剂0.20g，混合后得到预混液；
步骤四、在预混液中加入烧结助剂SiO2 0.2g、MgO 0.05g、混合粉体，充分搅拌后放入捏合机中，捏合36h均匀后得到混合膏料；
步骤五、将混合膏料放进混炼机混炼24h后，用保鲜膜包裹好，放入温度20℃，湿度90％的恒温恒湿箱里面进行熟化处理48h制备出强韧性陶瓷膏料。
将此膏料作为挤出机等挤出成型工艺设备的原料，通过挤出成型工艺制成凝胶固化的陶瓷光纤。将素坯进行干燥处理：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50μmYAG透明陶瓷光纤。

Claims (6)

1.一种用于陶瓷光纤挤出成型的强韧性膏料的配制方法，其特征在于：包括如下步骤：
步骤一、按照透明陶瓷材料Y3Al5O12分子式的化学计量比称取高纯氧化物原料粉体，除杂预处理；
步骤二、向步骤一的原料粉体中加入KL系列粉体粘结剂组成预混粉体，在混合机中进行粉体混合；
步骤三、向Isobam凝胶剂粉体中加入去离子水、分散剂，得到预混液；
步骤四、将预混液中加入烧结助剂和步骤二得到的混合粉体，在捏合机中进行充分混合，得到混合膏料；
步骤五、将混合膏料放进混炼机进行混炼，经熟化处理即可得到可实现挤出成型所需的强韧性膏料；
所述KL系列粉体粘结剂为KL-86L、KL-72M1或KL-56A的一种或几种的组合；
所述预混液中Isobam凝胶剂粉体占比为20～25 wt.%。
2.根据权利要求1所述的配制方法，其特征在于：步骤一中，所述原料粉体为纯度在99.99 %以上的氧化铝和氧化钇；除杂预处理采用煅烧法。
3.根据权利要求1所述的配制方法，其特征在于：步骤四中，所述烧结助剂为MgO、SiO2中的一种或两种的组合。
4.根据权利要求1所述的配制方法，其特征在于：步骤五中，所述熟化处理是将膏料用保鲜膜包裹好，放入温度10～20 ℃、湿度80～90 ％的恒温恒湿箱里面进行熟化处理24～48 h。
5.采用权利要求1所述的配制方法得到的强韧性膏料在制备陶瓷光纤中的应用。
6.根据权利要求5所述的应用，其特征在于：将强韧性膏料通过挤出成型工艺制成凝胶固化的陶瓷光纤，经干燥、排胶、真空烧结、抛光处理，即可得到陶瓷光纤成品。
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