河南化工
河南化工
하남화공
HENAN CHEMICAL INDUSTRY
2012年
13期
31-35
,共5页
李群%王宝和%夏良志%于才渊
李群%王寶和%夏良誌%于纔淵
리군%왕보화%하량지%우재연
氧化铜%络合沉淀%纳米粉体%正交实验
氧化銅%絡閤沉澱%納米粉體%正交實驗
양화동%락합침정%납미분체%정교실험
copper oxide%complex precipitation%nanopowders%orthogonal experiment
以三水硝酸铜为反应物,氨水为络合剂,氢氧化钠为沉淀剂,乙醇水混合溶液为反应溶剂,聚乙二醇为分散剂,采用络合沉淀法,成功制备出平均粒径约20nm的氧化铜单晶纳米粉体。通过单因素实验和正交实验考察了硝酸铜溶液初始浓度、反应温度及氢氧化钠与硝酸铜物质的量比等因素对产物粒径大小的影响,利用x射线衍射(XRD)、透射电镜(TEM)和红外光谱仪(FT-IR)等对产物进行表征分析。研究结果表明,影响其粒径大小主要因素的主次顺序依次是:反应温度,硝酸铜溶液初始浓度及氢氧化钠与硝酸铜的物质的量比;优化制备工艺条件为:反应温度70℃,硝酸铜溶液初始浓度0.3mol/L,氢氧化钠与硝酸铜的物质的量比3:1,氨与硝酸铜的物质的量比5:1;氧化铜纳米粉体的红外吸收峰出现了红移和蓝移同时并存的反常现象。
以三水硝痠銅為反應物,氨水為絡閤劑,氫氧化鈉為沉澱劑,乙醇水混閤溶液為反應溶劑,聚乙二醇為分散劑,採用絡閤沉澱法,成功製備齣平均粒徑約20nm的氧化銅單晶納米粉體。通過單因素實驗和正交實驗攷察瞭硝痠銅溶液初始濃度、反應溫度及氫氧化鈉與硝痠銅物質的量比等因素對產物粒徑大小的影響,利用x射線衍射(XRD)、透射電鏡(TEM)和紅外光譜儀(FT-IR)等對產物進行錶徵分析。研究結果錶明,影響其粒徑大小主要因素的主次順序依次是:反應溫度,硝痠銅溶液初始濃度及氫氧化鈉與硝痠銅的物質的量比;優化製備工藝條件為:反應溫度70℃,硝痠銅溶液初始濃度0.3mol/L,氫氧化鈉與硝痠銅的物質的量比3:1,氨與硝痠銅的物質的量比5:1;氧化銅納米粉體的紅外吸收峰齣現瞭紅移和藍移同時併存的反常現象。
이삼수초산동위반응물,안수위락합제,경양화납위침정제,을순수혼합용액위반응용제,취을이순위분산제,채용락합침정법,성공제비출평균립경약20nm적양화동단정납미분체。통과단인소실험화정교실험고찰료초산동용액초시농도、반응온도급경양화납여초산동물질적량비등인소대산물립경대소적영향,이용x사선연사(XRD)、투사전경(TEM)화홍외광보의(FT-IR)등대산물진행표정분석。연구결과표명,영향기립경대소주요인소적주차순서의차시:반응온도,초산동용액초시농도급경양화납여초산동적물질적량비;우화제비공예조건위:반응온도70℃,초산동용액초시농도0.3mol/L,경양화납여초산동적물질적량비3:1,안여초산동적물질적량비5:1;양화동납미분체적홍외흡수봉출현료홍이화람이동시병존적반상현상。
Using Cu (NO3 )2 3 HzO as reactants, ammonia as complex agent, sodium hydroxide as precipita- tor, and polyethylene glycol as dispersant, ethanol and distilled water as solvent, copper oxide single crys- tal nanopowders which have average diameter about 20 nm are prepared by complex precipitation method. Mono -factor experiments and muhifactor orthogonal experiments are adopted to explore the influences of these factors, such as, the initial concentration of Cu ( NO3 ) 2, reaction temperature, molar ratio of sodium hydroxide and copper ion etc. on diameter of copper oxide nanopowders. And transmission electron micro- scope (TEM) and fourier transform infrared spectroscopy (FT -IR) , X -ray diffraction (XRD) are used to characterize and analyze the morphology, structure and property of products prepared. The experiment result shows that the diameter of copper oxide nanopowders is mostly influenced by reaction temperature, concentration of copper nitrate, ratio of sodium hydroxide and copper ion. The optimum conditions prepar- ing copper oxide nanopowders are as follows: reaction temperature 70 C, concentration of copper nitrate O. 3 mol/L, molar ratio of sodium hydroxide and copper nitrate 3 : 1, molar ratio of ammonia and copper ion 5 : 1. FT - IR absorption spectrum declares that copper oxide nanopowders are characterized by both red and blue shift anomaly