郭夏溥,杨来侠,徐超,等.静电纺丝工艺及煅烧温度对Dy0.05Ce0.95O0.975纳米纤维形貌影响研究[J].精密成形工程,2023,15(12):95-105.
GUO Xia-pu,YANG Lai-xia,XU Chao,et al.Effect of Electrospinning Process and Calcination Temperature on Morphology of Dy0.05Ce0.95O0.975 Nanofibers[J].Journal of Netshape Forming Engineering,2023,15(12):95-105. |
| 静电纺丝工艺及煅烧温度对Dy0.05Ce0.95O0.975纳米纤维形貌影响研究 |
| Effect of Electrospinning Process and Calcination Temperature on Morphology of Dy0.05Ce0.95O0.975 Nanofibers |
| 投稿时间：2023-07-24 |
| DOI：10.3969/j.issn.1674-6457.2023.12.012 |
| 中文关键词: 静电纺丝 固体氧化物燃料电池 纳米纤维 形貌 煅烧 |
| 英文关键词: electrospinning solid oxide fuel cell nanofiber morphology calcination |
| 基金项目:陕西省秦创原“科学家+工程师”队伍建设(2022KXJ-071) |
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| 中文摘要: |
| 目的 为了制备出直径能够达到纳米级别的纤维，调节静电纺丝的参数，包括电压、聚乙烯吡咯烷酮(PVP)含量、溶液流速、稀土硝酸盐含量，以确定最佳工艺数值，并通过煅烧获得纳米级别、无杂质生成的粉体颗粒，了解纤维形貌随温度的变化规律。方法 采用Dy元素对CeO2进行掺杂，其掺杂量x=0.05(原子数分数)，并使用PVP配制纺丝前驱液，而后通过单因素分析法，分别研究4种工艺参数对纳米纤维形貌及直径的影响，采用扫描电镜(SEM)进行观察，并用软件测量纤维样品的直径分布范围。在制备了纳米级别的纤维后，进行热重(TG/DTA)分析，并观察不同温度下纤维的失重情况，确定了热处理温度范围，而后将纤维在700、800、900 ℃下煅烧，通过SEM观察纤维在煅烧之后的形貌。采用能谱仪测定了煅烧后样品的组成元素及分布情况。结果 利用优化后的工艺参数可以制备出直径为200~500 nm、形貌良好的纤维，通过煅烧可以形成100~200 nm的球型颗粒纤维，煅烧后的粉体没有杂质产生。结论 最佳工艺参数如下:电压为15 V，PVP的质量分数为10%，溶液流速为0.2 mm/min，硝酸盐质量分数为6.5%。煅烧温度会对纤维形貌及晶粒产生较大影响，煅烧温度越高，晶粒生长速度越快，在3种煅烧温度下，纤维能够完全转变为氧化物，没有C元素生成。 |
| 英文摘要: |
| The work aims to prepare fiber with nano-scale diameter, and adjust the parameters of electrospinning, including voltage, mass fraction of polyvinylpyrrolidone (PVP), solution flow rate and mass fraction of rare earth nitrate, to determine the optimum process, obtain nano-scale powder particles without impurities by calcination, and learn the law of fiber morphology changing with temperature. CeO2 was doped with Dy element at doping amount x=0.05. PVP was used to prepare spinning precursor solution. Then, the effects of four process parameters on the morphology and diameter of nanofibers were studied by single factor analysis. Scanning electron microscopy (SEM) was used to observe and the diameter distribution range of fiber samples was measured by software. After the preparation of nano-scale fibers, the weight loss of the fibers with the change of temperature was observed by thermogravimetric (TG/DTA) analysis, and the heat treatment temperature range was determined. Then the fibers were calcined at 700, 800, 900 ℃, and the morphology of the fibers after calcination was observed with a SEM. Finally, the composition and distribution of the calcined samples were determined by energy spectrum. The optimized process parameters could be used to prepare fibers with good morphology in the diameter range of 200-500 nm. Spherical granular fibers of 100-200 nm could be formed by calcination, and the calcined powder had no impurities. The voltage of 15 V, PVP 10 %, solution flow rate of 0.2 mm/min, and nitrate mass fraction of 6.5% are the best process parameters. The calcination temperature has a great effect on the morphology and grain size of the fiber. The higher the calcination temperature, the faster the grain growth rate. Under the three calcination temperatures, the fiber can be completely converted into oxide, and no C element is generated. |
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