以高锰酸钾(KMnO4)为锰源,柠檬酸(C6H8O7)为还原剂,采用水热合成技术在160℃条件下一步制备了碳酸锰(MnCO3)微球.用X射线衍射(XRD)、扫描电镜(SEM)、同步热分析(TG-DSC)、傅里叶变换红外光谱(FT-IR)、N2吸附脱附技术及激光粒度仪对制备产物的结构、形貌、热稳定性、孔结构和粒度分布进行了表征.系统研究了柠檬酸用量、反应温度、反应时间对合成产物晶型和形貌的影响,探讨了MnCO3在空气氛围中不同温度下的热分解行为.研究结果表明,产物MnCO3为介孔材料,其孔径、比表面积和孔容分别为20.9 nm、27.9m2·g-1和0.19 cm3·g-1.柠檬酸用量对制备产物的晶体结构具有控制作用,其浓度达1.49 mol/L时产物为高纯MnCO3微球.反应温度和时间对产物MnCO3的晶型和形貌几乎没有影响.MnCO3在空气氛围中发生热分解,300～400℃时产物以MnO2为主,560℃时煅烧产物为Mn2O3,1000℃时分解生成Mn3O4.
参考文献
| [1] | 周晚珠;叶红齐;韩凯;陈龙;刘辉.球形MnCO3粉的制备及其粒径控制[J].稀有金属与硬质合金,2011(4):13-16. |
| [2] | He Hu;Jie-yan Xu;Hong Yang;Jie Liang;Shiping Yang;Huixia Wu.Morphology-controlled hydrothermal synthesis of MnCO_3 hierarchical superstructures with Schiff base as stabilizer[J].Materials Research Bulletin,201111(11):1908-1915. |
| [3] | Jordens, Jeroen;De Coker, Nico;Gielen, Bjorn;Van Gerven, Tom;Braeken, Leen.Ultrasound precipitation of manganese carbonate: The effect of power and frequency on particle properties[J].Ultrasonics sonochemistry,2015:64-72. |
| [4] | Yang LX;Zhu YH;Tong H;Wang WW.Submicrocubes and highly oriented assemblies of MnCO3 synthesized by ultrasound agitation method and their thermal transformation to nanoporous Mn2O3[J].Ultrasonics sonochemistry,20072(2):259-265. |
| [5] | 粟海锋;屈雄;文衍宣;童张法;黎铉海.球形碳酸锰微晶制备过程中的形貌控制[J].过程工程学报,2008(2):280-284. |
| [6] | Wang X.;Li YD..Hydrothermal reduction route to Mn(OH)(2) and MnCO3 nanocrystals[J].Materials Chemistry and Physics,20032(2):419-422. |
| [7] | 杜泽伟;曹秀华.水热晶化法制备超细MnCO3的研究[J].电子元件与材料,2006(3):12-14. |
| [8] | Lichun Zhang;Zong-Huai Liu;Xiuhua Tang;Jianfang Wang;Kenta Ooi.Synthesis and characterization of β-MnO_2 single crystals with novel tetragonous morphology[J].Materials Research Bulletin: An International Journal Reporting Research on Crystal Growth and Materials Preparation and Characterization,20078(8):1432-1439. |
| [9] | Zhao, Shuoqing;Liu, Tianmo;Shi, Dongfeng;Zhang, Yu;Zeng, Wen;Li, Tianming;Miao, Bin.Hydrothermal synthesis of urchin-like MnO2 nanostructures and its electrochemical character for supercapacitor[J].Applied Surface Science: A Journal Devoted to the Properties of Interfaces in Relation to the Synthesis and Behaviour of Materials,2015Oct.1(Oct.1):862-868. |
| [10] | Song XC;Zhao Y;Zheng YF.Synthesis of MnO2 nanostructures with sea urchin shapes by a sodium dodecyl sulfate-assisted hydrothermal process[J].Crystal growth & design,20071(1):159-162. |
| [11] | 徐宇桑;陈建铭;宋云华.水热控制合成球形碱式磷酸铁及生长机理研究[J].人工晶体学报,2013(9):1757-1761. |
| [12] | Kang LP;Zhang MM;Liu ZH;Ooi K.IR spectra of manganese oxides with either layered or tunnel structures[J].Spectrochimica acta, Part A. Molecular and biomolecular spectroscopy,20073-4(3-4):864-869. |
| [13] | 齐海霞;张安然;吴艳;刘峰.7-氧-双环[2.2.1]环庚烷-2,3,5,6-四酸二酐的合成研究[J].化工新型材料,2013(5):91-93. |
| [14] | 吕春玲;张景林.柠檬酸对碳酸锰单分散粒子表面的电荷改性[J].硅酸盐学报,2011(5):753-757. |
| [15] | Michael Kruk;Mietek Jaroniec.Gas Adsorption Characteriztaion of Ordered Organic-Inorganic Nancomposite Materials[J].Chemistry of Materials,200110(10):3169-3183. |
| [16] | Shaoyan Wang;Xiaoan Li;Shaofeng Wang;Yang Li;Yuchun Zhai.Synthesis of γ-alumina via precipitation in ethanol[J].Materials Letters,200820(20):3552-3554. |
| [17] | 刘国全;张俊卿;宋义全.氨水沉淀法制备氧化镧粉体及表征[J].内蒙古科技大学学报,2009(1):20-23. |
上一张
下一张
上一张
下一张
计量
- 下载量()
- 访问量()
文章评分
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%