CN113151932B - 一种硅酸钇纳米纤维的制备方法及其制备材料 - Google Patents

一种硅酸钇纳米纤维的制备方法及其制备材料 Download PDF

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CN113151932B
CN113151932B CN202110469645.XA CN202110469645A CN113151932B CN 113151932 B CN113151932 B CN 113151932B CN 202110469645 A CN202110469645 A CN 202110469645A CN 113151932 B CN113151932 B CN 113151932B
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赵步月
黄海明
陈群教
李玮洁
王爽
黄杰
陈嘉龙
明四维
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Abstract

本发明公开一种硅酸钇纳米纤维的制备方法及其制备材料，属于化工材料制备方法技术领域，在正硅酸乙酯中滴入一定剂量的催化液，搅拌后得到硅溶胶；向硅溶胶中加入钇源，搅拌后得到钇硅溶胶；向钇硅溶胶中加入纺丝助剂，得到硅酸钇前驱体纺丝液；将步骤一中得到的硅酸钇前驱体纺丝液通过静电纺丝得到硅酸钇前驱体纤维；将步骤二中得到的硅酸钇前驱体纤维在空气环境下经过高温热处理，得到硅酸钇纳米纤维材料制品。采用溶胶凝胶法制备出可纺性良好的硅酸钇前驱体纺丝液，通过静电纺丝技术制备结构致密的硅酸钇纳米纤维。该方法制备出的纤维，克服在制备过程中引入其余成分，提高了产品的纯度，保证了产品的质量。

Description

一种硅酸钇纳米纤维的制备方法及其制备材料
技术领域
本发明涉及一种硅酸钇纳米纤维的制备方法及其制备材料，属于化工材料制备方法技术领域。
背景技术
硅酸钇材料具有硅酸钇材料是稀土硅酸盐中的一类，常见的三种硅酸钇晶体结构有 Y2SiO5、Y2Si2O7 和 Y4Si3O12，前两种结构的硅酸钇因其极高的熔点而应用广泛。也由于具有优异的晶体结构和物化性质，硅酸钇材料具有了很多良好的特性，如低热导率、低热膨胀系数、低氧气渗透率、低挥发率、良好的高温稳定性、良好的耐高温腐蚀性和优良的力学性能等。因此，硅酸钇材料被用作高性能陶瓷、高温抗氧化涂层、光学基质材料以及介电材料等。
中国专利文献，申请公布号为：CN102817094A，公开了一种制备掺铕焦硅酸钇红色发光纳米纤维的方法: 称取一定量的氧化钇Y2O3和氧化铕Eu2O3，两者的摩尔比为95∶5，即铕离子的摩尔百分数为5％，用稀硝酸HNO3溶解后蒸发，得到Y(NO3)3和Eu(NO3)3混合晶体，加入正硅酸乙酯Si(C2H5O)4，使Y3+加Eu3+与Si(C2H5O)4的摩尔比为1:1，再加入适量的N，N-二甲基甲酰胺DMF溶剂和聚乙烯吡咯烷酮PVP，于室温下磁力搅拌4h，并静置2h，形成纺丝液，经静电纺丝和空气中热处理得到掺铕焦硅酸钇红色发光纳米纤维。但该方法制备过程中使用了大量的硝酸，对人体健康及生态环境都有很大的危害；并且纺丝液成分中有机物含量超过90%，热处理后纤维表面不光滑，气孔较多。
中国专利文献，申请公布号为：CN110670171A，公开了一种致密硅酸钇陶瓷纤维的制备方法：将硝酸钇、正硅酸乙酯和TiSi2加入到N-N二甲基甲酰胺中，得到混合液，对混合液进行湿法球磨，向湿法球磨后的混合液中添加聚乙烯吡咯烷酮并在室温下搅拌混合液，搅拌完成后静置，得到纺丝液；利用步骤一得到的纺丝液进行静电纺丝，得到复合纤维；将步骤二得到的复合纤维进行热处理，得到致密硅酸钇陶瓷纤维。但是该专利在制备过程中引入了TiSi2，这将会大大降低纤维的纯度，影响产品质量。
制备陶瓷纤维的传统方法，一般是将氧化物原料加热到熔融状态，融法纺丝成型。然而许多特种陶瓷纤维的熔点很高，融体粘度很低，难以用传统方法制备。溶胶凝胶法解决了这一难题。溶胶凝胶法是一种湿化学方法，与传统方法相比，具有化学组分均匀性好、产物纯度高、过程易于控制、掺杂范围宽、工艺设备简单等优点，是常用的制备玻璃纤维和多晶陶瓷纤维的方法之一。溶胶凝胶法工艺过程温度低，当溶胶达到合适粘度后，可以在室温下纺丝成形，因此一种利用溶胶凝胶法制备出可纺性良好的硅酸钇纳米纤维的方法成为目前的迫切需求。
发明内容
针对现有技术的不足，本发明的目的在于提供一种硅酸钇纳米纤维的制备方法及其制备材料，解决了现有技术中出现的问题。
本发明所述的一种硅酸钇纳米纤维的制备方法，包括以下步骤：
步骤一：在正硅酸乙酯中滴入一定剂量的催化液，搅拌后得到硅溶胶；向硅溶胶中加入钇源，搅拌后得到钇硅溶胶；向钇硅溶胶中加入纺丝助剂，得到硅酸钇前驱体纺丝液；
步骤二：将步骤一中得到的硅酸钇前驱体纺丝液通过静电纺丝得到硅酸钇前驱体纤维；
步骤三：将步骤二中得到的硅酸钇前驱体纤维在空气环境下经过高温热处理，得到硅酸钇纳米纤维材料制品。
进一步的，步骤一中催化液为将一水合柠檬酸溶于溶剂中所得到，溶剂为去离子水与乙醇或去离子水与甲醇的混合物。
进一步的，步骤一中催化液的组分一水合柠檬酸：醇：水的摩尔比为0.01：（1~2）：（6~7）。
进一步的，步骤一中钇源为六水硝酸钇、六水氯化钇之一或其组合。
进一步的，步骤一中正硅酸乙酯：钇源的摩尔比为1：（1~2）。
进一步的，步骤一中纺丝助剂为聚氧化乙烯(PEO)、聚乙烯吡咯烷酮(PVP)、聚乙烯醇(PVA)之一或其组合。
进一步的，纺丝助剂与硅酸钇前驱体纺丝液的质量比为(0.015～0.12)：1；
进一步的，硅酸钇前驱体纺丝液的粘度为100～1000mPa·s。
进一步的，步骤二中静电纺丝的工艺参数为：纺丝电压15～30kV，推进速度0 .6～1 .5mL/h，接收距离15～25cm，纺丝湿度20～45％，纺丝温度20～40℃。
进一步的，步骤三中高温热处理时以1-5℃/min的升温速率升温至1000-1500℃，保温时间为0.5~2h。
本发明所述的一种硅酸钇纳米纤维材料，由硅酸钇纳米晶粒组成，硅酸钇纳米纤维直径为300-700nm，纤维表面无气孔和裂纹。
本发明与现有技术相比，具有如下有益效果：
本发明所述的一种硅酸钇纳米纤维的制备方法及其制备材料，采用溶胶凝胶法制备出可纺性良好的硅酸钇前驱体纺丝液，通过静电纺丝技术制备结构致密的硅酸钇纳米纤维。该方法制备出的纤维，克服在制备过程中引入其余成分，提高了产品的纯度，保证了产品的质量。
本发明提供的制备的硅酸钇纳米纤维直径为 300-700 nm，由硅酸钇纳米晶粒组成；纤维在微观上结构致密，表面光滑，没有气孔和裂纹，纯度高，在高温隔热材料、结构增强材料以及柔性光学材料等领域有着广阔的应用前景。本发明具有方法简单、成本低、无污染、可操作性好的特点。解决了现有技术中存在的问题。
附图说明
图1为实施例1制备方法的硅酸钇SEM图；
图2为实施例1制备方法的硅酸钇XRD图。
具体实施方式
下面结合附图和实施例对本发明作进一步的说明：
实施例1：
作为优选，本发明所述的一种硅酸钇纳米纤维的制备方法，包括的步骤如下：
步骤一：将2g的一水合柠檬酸溶解于18g的质量分数为18%的乙醇溶液中，充分搅拌溶解后得到催化液；将20g的催化液逐滴滴加至20.83g正硅酸乙酯中，高速搅拌6h后得到均一透明的硅溶胶；向硅溶胶中加入38.3g的硝酸钇，充分搅拌溶解后得到钇硅溶胶；向钇硅溶胶中加入助纺剂，搅拌溶解，搅拌时间3～6h，并用溶剂调节粘度，制得硅酸钇前驱体纺丝液；纺丝助剂为聚氧化乙烯(PEO)、聚乙烯吡咯烷酮(PVP)、聚乙烯醇(PVA)之一或其组合；优选采用PVA，将PVA溶于质量分数30%的乙醇溶液中，得到12%的PVA溶液；向钇硅溶胶中加入等质量的PVA溶液，充分搅拌3h后得到硅酸钇前驱体纺丝液；
步骤二：对步骤一得到的硅酸钇前驱体纺丝液在温度25℃，湿度40%的环境下进行静电纺丝制备硅酸钇前驱体纤维。所述静电纺丝电压为30kV，固化距离20cm，推进速度0.8mL/h。
步骤三：将步骤二获得的硅酸钇前驱体纤维在空气氛围下，以1℃/min的升温速率升温至600℃，保温2h；再以10℃/min的升温速率升温至1300℃，保温2h，获得硅酸钇纳米纤维。
本实施例的工作原理为：本实施例经过1300℃热处理后得到的硅酸钇纤维SEM照片如图1所示，由图1可知，本发明制备结构致密的硅酸钇纤维，纤维直径300-700nm，由硅酸钇纳米晶粒组成，纤维表面无气孔、裂纹等缺陷。
本实施例1300℃热处理所得的硅酸钇纤维测试XRD图谱如图2所示。由图2可知，所得纤维组分为Y2Si2O7。
实施例2：
本发明所述的一种硅酸钇纳米纤维的制备方法制备的硅酸钇纳米纤维，由硅酸钇纳米晶粒组成，硅酸钇纳米纤维直径为300-700nm，纤维表面无气孔和裂纹。用于高温隔热材料、结构增强材料、光学基质材料以及介电材料等。
采用以上结合附图描述的本发明的实施例的一种硅酸钇纳米纤维的制备方法及其制备材料，采用溶胶凝胶法制备出可纺性良好的硅酸钇前驱体纺丝液，通过静电纺丝技术制备结构致密的硅酸钇纳米纤维。该方法制备出的纤维，克服在制备过程中引入其余成分，提高了产品的纯度，保证了产品的质量。解决了现有技术中存在的问题。但本发明不局限于所描述的实施方式，在不脱离本发明的原理和精神的情况下这些对实施方式进行的变化、修改、替换和变形仍落入本发明的保护范围内。

Claims (7)

1.一种硅酸钇纳米纤维的制备方法，其特征在于：所述的方法包括以下步骤：
步骤一：在正硅酸乙酯中滴入一定剂量的催化液，所述催化液为将一水合柠檬酸溶于溶剂中所得到，溶剂为去离子水与乙醇或去离子水与甲醇的混合物，其中水合柠檬酸：醇：水的摩尔比为0.01：（1~2）：（6~7），搅拌后得到硅溶胶；向硅溶胶中加入钇源，搅拌后得到钇硅溶胶；向钇硅溶胶中加入纺丝助剂，得到硅酸钇前驱体纺丝液；所述的硅酸钇前驱体纺丝液的粘度为100～1000mPa· s；
步骤二：将步骤一中得到的硅酸钇前驱体纺丝液通过静电纺丝得到硅酸钇前驱体纤维；
步骤三：将步骤二中得到的硅酸钇前驱体纤维在空气环境下经过高温热处理，得到硅酸钇纳米纤维材料制品；采用溶胶凝胶法制备出可纺性良好的硅酸钇前驱体纺丝液，通过静电纺丝技术制备结构致密的硅酸钇纳米纤维，硅酸钇纳米纤维由硅酸钇纳米晶粒组成，纤维表面无气孔、裂纹缺陷。
2.根据权利要求1所述的一种硅酸钇纳米纤维的制备方法，其特征在于：所述的步骤一中钇源为六水硝酸钇、六水氯化钇之一或其组合。
3.根据权利要求1所述的一种硅酸钇纳米纤维的制备方法，其特征在于：所述的步骤一中正硅酸乙酯：钇源的摩尔比为1：（1~2）。
4.根据权利要求1所述的一种硅酸钇纳米纤维的制备方法，其特征在于：所述的步骤一中纺丝助剂为聚氧化乙烯(PEO)、聚乙烯吡咯烷酮(PVP)、聚乙烯醇(PVA)之一或其组合。
5.根据权利要求1所述的一种硅酸钇纳米纤维的制备方法，其特征在于：所述的纺丝助剂与硅酸钇前驱体纺丝液的质量比为(0.015～0.12)：1。
6.根据权利要求1所述的硅酸钇纳米纤维的制备方法，其特征在于，步骤二中静电纺丝的工艺参数为：纺丝电压15～30kV，推进速度0 .6～1 .5mL/h，接收距离15～25cm，纺丝湿度20～45％，纺丝温度20～40℃；步骤三中高温热处理时以1-5℃/min的升温速率升温至1000-1500℃，保温时间为0.5~2h。
7.一种根据权利要求1-6任一所述的制备方法制备的硅酸钇纳米纤维材料，其特征在于：所述的硅酸钇纳米纤维由硅酸钇纳米晶粒组成，硅酸钇纳米纤维直径为300-700nm，纤维表面无气孔和裂纹。
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