微/纳米ZnO粉体在Glu-BF4离子液体水溶液中的诱导生长

doi:10.7503/cjcu20160471

摘要/Abstract

摘要：

以一定浓度谷氨酸-氟硼酸(Glu-BF₄)离子液体水溶液为反应介质, 摩尔比为1∶6的二水合醋酸锌和氢氧化钠为反应物, 在室温下制备前驱体, 再通过微波辅助加热制备了具有绒球形貌的微/纳米ZnO粉体. 利用扫描电子显微镜(SEM)、 X射线衍射仪、比表面积测试仪、能谱仪、拉曼光谱仪和透射电子显微镜(TEM)等对产物形貌、晶型、比表面积、组成和晶面分布进行了测定. 结果显示, 所得产物为六方晶系纤锌矿结构, 平均粒径20.4 nm, 绒球大小1.6~3.0 μm, 比表面积为28.3 m²/g, 产物纯度较高. 当反应物浓度一定, 离子液体浓度分别为0.02, 0.04, 0.08和0.12 mol/L时都得到了类似形貌的微/纳米ZnO粉体, 且随着离子液体使用量的增加, 绒球尺寸分布更加均一. 当离子液体浓度一定, 而反应物浓度逐渐下降时, 产物形貌发生递变性变化. ZnO晶粒在Glu-BF₄离子液体诱导下首先生成不规则的纳米片, 纳米片进一步聚集, 在一定反应物浓度范围内生成绒球形貌粉体, 反应物浓度较低时只生成绒球的核心部分, 而浓度更高时则生成纳米针阵列. 通过不同条件下纳米ZnO粉体形貌变化规律, 探讨了强碱性条件下Glu-BF₄离子液体水溶液中微/纳米ZnO粉体的生长机制.

关键词: 谷氨酸-氟硼酸离子液体, 微波辅助加热, 微/纳米ZnO, 生长机制

Abstract:

In this study, pompon-like micro/nano ZnO powders have been synthesized via microwave assisted heating of the precursors which were prepared with Zn(OAc)₂·2H₂O and NaOH(molar ratio 1∶6) as reactants and Glu-BF₄ ionic liquid aqueous solution as reaction medium at room temperature. The products were characterized by scanning electron microscopy(SEM), X-ray diffraction(XRD), specific surface area analysis, energy spectroscopy(EDS), Raman spectroscopy and transmission electron microscopy(TEM), respectively. The results show that the prepared product has hexagonal wurtzite structure with high purity, the average particle diameter is 20.4 nm, the size of pompon-like structure is about 1.6—3.0 μm and the BET surface area is 28.3 m²/g. When the concentration of the reactant was fixed, micro/nano ZnO with similar morphologies was synthesized using different dosages of ionic liquid, and with increase of the ionic liquid dosage, the size distribution of particles became more uniform. When the ionic liquid concentration was fixed, the morphology of product changed gradually with the decrease of the reactant concentration. Under the induction of Glu-BF₄ ionic liquid, ZnO crystal grains firstly formed irregular nanosheets, then those nanosheets further aggregated to form the pompon-like powder in certain range of reactants concentration. Only the core part of the pompon-like powder was synthesized when the reactants concentration was relatively lower, while the nano-array morphologies were generated at higher reactant concentrations. In addition, the growth mechanism of micro/nano ZnO powder induced by Glu-BF₄ ionic liquid aqueous solution under strong alkaline condition was discussed via morphology change tendency of nano ZnO powder under different conditions.

Key words: Glu-BF4 ionic liquid, Microwave assisted heating, Micro/nano ZnO, Formation mechanism

中图分类号:

O614.24
O643

TrendMD:

佟拉嘎, 任广生, 党晓峰, 林世静, 荣华. 微/纳米ZnO粉体在Glu-BF₄离子液体水溶液中的诱导生长. 高等学校化学学报, 2016, 37(11): 1939.

TONG Laga, REN Guangsheng, DANG Xiaofeng, LIN Shijing, RONG Hua. Induced Growth of Micro/nano ZnO Powder via Glu-BF₄Ionic Liquid Aqueous Solution^†. Chem. J. Chinese Universities, 2016, 37(11): 1939.

图/表 11

Fig.1 SEM images of nano-ZnO without(A) and with 0.06 mol/L Glu-BF4 ionic liquid(B)

Fig.2 XRD patterns of ZnO nano-needles(a) and nano-pompons(b)

Fig.3 EDS diagram of nano-ZnO pompons

Fig.4 Raman spectra of nano-ZnO pompons(A) and nano-ZnO needles(B)

Fig.5 TG-DTA curves of nano-ZnO pompons

Fig.6 SEM image of nano-ZnO pompons after calcination at 1000 ℃ for 5 h

Fig.7 SEM images of ZnO nanostructures obtained using different concentrations of Glu-BF4 ionic liquid (A) 0.5 g(0.02 mol/L); (B) 1.0 g(0.04 mol/L); (C) 2.0 g(0.08 mol/L); (D) 3.0 g(0.12 mol/L).

Fig.8 SEM images of ZnO nanostructures obtained with different concentrations of reactants(A) c(NaOH)=0.75 mol/L, c[Zn(OAc)2·2H2O]=0.125 mol/L; (B) c(NaOH)=0.5 mol/L, c[Zn(OAc)2·2H2O]=0.083 mol/L; (C) c(NaOH)=0.38 mol/L, c[Zn(OAc)2·2H2O]=0.063 mol/L; (D) c(NaOH)=3.0 mol/L, c[Zn(OAc)2·2H2O]=0.5 mol/L.

Fig.9 XRD patterns of the products obtained with different concentrations of reactantsa. c(NaOH)=0.75 mol/L, c[Zn(OAc)2·2H2O]=0.125 mol/L; b. c(NaOH)=0.5 mol/L, c[Zn(OAc)2·2H2O]=0.083 mol/L; c. c(NaOH)=0.38 mol/L, c[Zn(OAc)2·2H2O]=0.063 mol/L.

Fig.10 TEM(A, C) and HRTEM(B, D) images of nano-ZnO needles(A, B) and nano-ZnO pompons(C, D)Insets of (A) and (C): SAED images of nano-ZnO needles and nano-ZnO pompons, respectively.

Fig.11 Schematic diagram of the proposed formation processes of the basic ZnO structures

参考文献 31

[1]	Motaung D., E. , Mhlongo G., H. , Nkosi S., S. , Malgas G., F. , Mwakikunga B., W. , Coetsee, E. , Swart H., C. , Abdallah H. M., I. , Moyo, T. , Ray S., S. , ACS Appl. Mater. Interfaces, 2014, 6, 8981- 8995
[2]	Zhang Y., C. , Deng J., X. , Chen, J. , Yu R., B. , Xing X., R. , Inorganic Chemistry Communications, 2014, 43, 138- 141
[3]	Wang H., Q. , Li C., H. , Zhao H., G. , Li, R. , Liu J., R. , Powder Technology, 2013, 239, 266- 271
[4]	王志芳, 李密, 张红霞. 无机化学学报, 2012, 28( 4), 715- 720
	Wang Z., F. , Li, M. , Zhang H. X, . , Chinese J. Inorg. Chem., 2012, 28( 4), 715- 720 (
[5]	Lang J., H. , Wang J., Y. , Zhang, Q. , Xu S., S. , Han, Q. , Zhang, Y. , Zhai H., J. , Cao, J. , Yan Y., S. , Yang J., H. , Chem. Res. Chinese Universities, 2014, 30( 4), 538- 542
[6]	Xu S., G. , Guo W., H. , Du S., W. , Loy M. M., T. , Wang, N. , Nano Lett., 2012, 12, 5802- 5807
[7]	Omar F., M. , Aziz H., A. , Stoll, S. , Science of the Total Environment, 2014, 468/469, 195- 201
[8]	Ren, X. , Jiang C., H. , Li D., D. , He, L. , Mater. Lett., 2008, 62, 3114- 3116
[9]	Razali, R. , Zak K., A. , Majid W. H., A. , Darroudi, M. , Ceramics International, 2011, 37, 3657- 3663
[10]	Wang, F. , Qin X., F. , Guo Z., L. , Meng Y., F. , Yang L., X. , Ming Y., F. , Ceramics International, 2013, 39, 8969- 8973
[11]	Shi R., X. , Yang, P. , Dong X., B. , Ma, Q. , Zhang A., Y. , Applied Surface Science, 2013, 264, 162- 170
[12]	Hamedani N., F. , Mahjoub A., R. , Khodadadi A., A. , Mortazavi, Y. , Sensors and Actuators B, 2011, 156, 737- 742
[13]	李奡麒, 陈玉娟, 胡晓宇, 卓克垒. 高等学校化学学报, 2015, 36( 1), 165- 170
	Li A., Q. , Chen Y., J. , Hu X., Y. , Zhuo K., L. , Chem. J. Chinese Universities, 2015, 36( 1), 165- 170 (
[14]	Goharshadi E., K. , Ding Y., L. , Nancarrow, P. , Journal of Physics and Chemistry of Solids, 2008, 69, 2057- 2060
[15]	Yu H., W. , Fan H., Q. , Wang, X. , Wang, J. , Optik., 2014, 125, 1461- 1464
[16]	胡晓宇, 刘千阁, 卓克垒, 王键吉. 高等学校化学学报, 2013, 34( 2), 324- 330
	Hu X., Y. , Liu Q., G. , Zhuo K. L, . , Wang J., J. , Chem. J. Chinese Universities, 2013, 34( 2), 324- 330 (
[17]	Movahedi, M. , Kowsari, E. , Mahjoub A., R. , Yavari, I. , Mater. Lett., 2008, 62, 3856- 3858
[18]	Sanes, J. , Carrion F., J. , Bermudez M., D. , Applied Surface Science, 2009, 255, 4859- 4862
[19]	Chen C., Y. , Li, Q. , Nie, M. , Lin, H. , Li, Y. , Wu H., J. , Wang Y., Y. , Materials Research Bulletin, 2011, 46, 888- 893
[20]	Wang, L. , Xu S., Z. , Li H., J. , Chang L., X. , Su, Z. , Zeng M., H. , Wang L., N. , Huang Y., N. , Journal of Solid State Chemistry, 2011, 184, 720- 724
[21]	Lee K., M. , Chiu W., H. , Hsu C., Y. , Cheng H., M. , Lee C., H. , Wu C., G. , Journal of Power Sources, 2012, 216, 330- 336
[22]	Min Y., L. , Zhang, K. , Chen L., H. , Chen Y., C. , Zhang Y., G. , Diamond & Related Materials, 2012, 26, 32- 38
[23]	Sabbaghan, M. , Shahvelayati A., S. , Bashtani S., E. , Solid State Sciences, 2012, 14, 1191- 1195
[24]	Rong, H. , Li, W. , Chen Z., Y. , Wu X., M. , J. Phys. Chem. B, 2008, 112, 1451- 1455
[25]	Tong L., G. , Liu, Y. , Rong, H. , Gong L., F. , Mater. Lett., 2013, 112, 5- 7
[26]	佟拉嘎, 刘金艳, 王岑晨, 荣华, 李巍. 物理化学学报, 2015, 31( 8), 1615- 1620
	Tong L., G. , Liu J., Y. , Wang C., C. , Rong, H. , Li, W. , Acta Phys.-Chim. Sin., 2015, 31( 8), 1615- 1620 (
[27]	佟拉嘎, 欧阳萍, 马小丽, 荣华. 功能材料, 2015, 46( 6), 06020- 06025
	Tong L., G. , Ouyang, P. , Ma X., L. , Rong, H. , Journal of Functional Materials, 2015, 46( 6), 06020- 06025 (
[28]	Zhang, Y. , Jia H., B. , Wang R., M. , Chen C., P. , Luo X., H. , Yu D., P. , Appl. Phys. Lett., 2003, 83, 4631- 4633
[29]	管秋梅, 张辉朝, 叶永红, 崔一平, 张家雨. 高等学校化学学报, 2012, 33( 10), 2315- 2319
	Guan Q., M. , Zhang H., C. , Ye Y., H. , Cui Y., P. , Zhang J., Y. , Chem. J. Chinese Universities, 2012, 33( 10), 2315- 2319 (
[30]	Fré, déric D. , Romain, P. , Fré, déric B. , Crystal Growth & Design, 2014, 14, 5388- 5396
[31]	Cho, S. , Jung S., H. , Lee K., H. , J. Phys. Chem. C, 2008, 112, 12769- 12776

微/纳米ZnO粉体在Glu-BF₄离子液体水溶液中的诱导生长

Induced Growth of Micro/nano ZnO Powder via Glu-BF₄Ionic Liquid Aqueous Solution^†

RichHTML

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

图/表 11

参考文献 31

相关文章 2

编辑推荐

Metrics

本文评价

[1]	王林香. Na⁺, Li⁺, Bi³⁺掺杂CaWO₄:Eu³⁺荧光粉的制备及发光特性[J]. 高等学校化学学报, 2018, 39(1): 25.
[2]	骆丽杰, 童张法, 莫丽玢, 梁钟媛, 陈拥军. 气氛对MnCr₂O₄尖晶石纳米线生长的影响[J]. 高等学校化学学报, 2009, 30(4): 647.