无机-有机前驱体法制备ZrO2纳米微晶.pdfVIP

无机一有机前驱体法制备 ZrOz纳米微晶／刘 超等 ·133 · FabricationofZirconiaNan0crystallitesUsingInorganic-OrganicPrecursors LIU Chao，LIXiaogai，HUO Da，XU Shuhe (CNNCEvercleanCo．，Ltd，Beiiing100037) Abstract Zirconiananocrystalliteshavebeensuccessfullysynthesizedusinginorganic-organichybridprecursors ofzirconium tetraehloride(ZrC44)andtoluene( H8)．Scanningelectronmicroscopeimag~ suggestedthattheparticle sizesofthesynthesizedpowderdistributedover30~40nm withhomogeneousequiaxedsphericalmorphology，andno agglomerationsappeared．CrystalstructuralcharacterizationofthesynthesizedZr02powdersusingX-raydiffraction andRamanspectroscopyrevealedthatthecrystalphasewerethemonoclinicphaseandtetragonalphase．High-resolu— tiontransmissionelectronmicroscopyimagesfurthershowedthattheaveragediametersofgrainswereabout36．4nm and32．1nm formonoclinicZ andtetragonalZ ，respectively．Moreover，thethermodynma icchangeprocessof theZrCh—C7H8systemandthesynthesismechanismofZ powderswerediscussed． Keywords zirconia，nanocrystallite，inorganic-organic，precursor 无机一有机前驱体法制备ZrO2纳米微晶 刘 超，李小该，霍 达，许书河 (中核清原环境技术工程有限责任公司，北京 100037) 摘要 采用四氯化锆、甲苯作为无机、有机前驱体成功制得ZKh纳米微晶粉末。扫描 电镜分析结果表明，制 得的Zr(h纳米粉末为尺寸介于30~40nm的各向同性等轴球形颗粒，无团聚。采用XRD和 RAMAN谱对合成的 z 粉末晶体结构进行了表征，结果表明所得晶粒为单斜相和四方相。高分辨透射电镜分析结果进一步表明生成 单斜和四方相Z 微粒，尺寸分别约为316．4nm和32．Inm。此外，分析了ZrCh—C7Ha体系的热力学过程及Z 的 合成机理 。 关键词 z 纳米微晶 无机-有机 前驱体 lysynthesizedusingZrC14and H8asinorganic-organichy— 0 Introduction brid precursor． Structuresofas—synthesized zirconia are Zirconia (ZrO2)haswideap