为制备分散均匀且超细的纳米 Cr2 O3粉体，以 Cr（NO3）3·9H2 O 为主原料，以聚乙烯吡咯烷酮（即PVP）为分散剂，采用两步沉淀法制备了纳米 Cr2 O3粉体。在 Cr（NO3）3浓度为0．0316 mol·L －1的条件下，研究了沉淀剂种类（氨水、碳酸钾和水合肼）、pH（4．8、5．2、6．5、7和7．9）及煅烧温度（300、400、450和500℃）等对合成纳米 Cr2 O3粉体晶粒尺寸的影响，并采用差热分析、FE－SEM及 XRD 等对所合成粉体进行了表征。结果表明：随煅烧温度及 pH 的升高，纳米 Cr2 O3粉体的晶粒尺寸先减小后增加。在 Cr（NO3）3浓度为0．0316 mol·L －1、以氨水为沉淀剂、pH ＝7、煅烧温度为450℃及保温时间为2 h 的条件下可以制得晶粒尺寸在20 nm 左右、分散良好的纳米 Cr2 O3粉体。
To prepared well dispersed ultra-fine nano-Cr2 O3 powders,Cr(NO3 )3 ·9H2 O was used as the main starting material and PVP was used as the dispersant by a two-step precipitation method.Fixing the Cr(NO3 )3 content at 0.031 6 mol·L -1 ,the effects of different kinds of precipitator (NH3 ·H2 O,K2 CO3 , N2 H4 ·H2 O),pH values (4.8,5.2,6.5,7 and 7.9)and calcination temperatures (300,400,450,and 500℃)on the crystalline size of nano-Cr2 O3 were investigated.The prepared Cr2 O3 nanopowders were char-acterized by TG-DSC,FE-SEM and XRD.The results show that crystalline size of nano-Cr2 O3 first decrea-ses and then increases with the elevating calcination temperature and pH value.The well dispersed nano-Cr2 O3 powders with crystalline size of about 20 nm are obtained under the conditions of [Cr(NO3 )3 · 9H2 O]=0.031 6 mol·L -1 ,NH3 ·H2 O as the precipitator,pH value of 7,calcination temperature of 450 ℃and holding time of 2 h.
参考文献
| [1] | T.Tsuzuki;P.G.McCormick.Synthesis of Cr_2O_3 nanoparticles by mechanochemical processing[J].Acta materialia,200011(11):2795-2801. |
| [2] | 彭超;杨卫波.浸渍锆盐法制备 MgO－Cr2 O3－ZrO2砖的性能研究[J].耐火材料,2015(4):304-305. |
| [3] | 杨秀丽;李冰;刘会林;郑军锋;程远;吴燕萍.Al2O3-Cr2O3-ZrO2砖在医疗垃圾焚烧炉上的应用[J].耐火材料,2014(2):143-144. |
| [4] | 孙红刚;李鹏涛;付建莹;闫双志;王刚;耿可明.Al2O3-Cr2O3砖显微结构对抗渣性能的影响[J].耐火材料,2014(3):188-193. |
| [5] | Zhou Gui;Rong Fan;Weiqin Mo;Xianhui Chen;Ling Yang;Yuan Hu.Synthesis and characterization of reduced transition metal oxides and nanophase metals with hydrazine in aqueous solution[J].Materials Research Bulletin: An International Journal Reporting Research on Crystal Growth and Materials Preparation and Characterization,20031(1):169-176. |
| [6] | Haitao Xu;Tianjun Lou;Yadong Li.Synthesis and characterize of trivalent chromium Cr(OH)_3 and Cr_2O3 microspheres[J].Inorganic Chemistry Communications,20045(5):666-668. |
| [7] | 施鹰;陈启伟;施剑林.沉淀剂对共沉淀法制备Lu2O3发光粉体形貌的影响[J].无机材料学报,2008(4):824-828. |
| [8] | 李素平;贾晓林;孙绍基;钟香崇.沉淀法制备纳米氧化铬粉体的影响因素[J].人工晶体学报,2009(2):362-366. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%