一步法制备高稳定性纳米α-H2Pc及其光电导性能研究  

One-step preparation of high stability nano-α-H2Pc andits photoconductive properties

作　　者：韩明明 刘流 张亚琴 王世荣[1,2,3] 刘红丽 董晓菲[1,2,3] 李祥高 HAN Mingming;LIU Liu;ZHANG Yaqin;WANG Shirong;LIU Hongli;DONG Xiaofei;LI Xianggao(School of Chemical Engineering and Technology,Tianjin University,Tianjin 3000354,China;Collaborative Innovation Center of Chemical Science and Engineering,Tianjin 300072,China;Tianjin Engineering Research Center of Functional Fine Chemicals,Tianjin 300354,China)

机构地区：[1]天津大学化工学院,天津300354 [2]天津化学化工协同创新,天津300072 [3]天津市功能精细化学品技术工程中心,天津300354

出　　处：《功能材料》2020年第10期10028-10035,10068,共9页Journal of Functional Materials

基　　金：国家自然科学基金资助项目(21676188);天津市科技计划资助项目(19ZXNCGX00020)。

摘　　要：α型无金属酞菁(H 2Pc)是重要的有机光电子材料之一,具有良好的近红外光电响应性能。本文以H 2Pc的硫酸溶液直接滴加到以不同比例的丁酮(MEK)与水组成的二元分散介质中,一步法制备了高晶型稳定和高分散稳定的纳米α-H2Pc。研究了分散介质组成、搅拌速度、晶型调节温度和时间等对α-H2Pc结晶度的影响。结果表明,体积比为1:3的丁酮/水的混合溶剂是制备α-H2Pc的合适介质,在600 r/min、40℃和晶型调节5 h的条件下,得到了粒度为68.8 nm、结晶度>90%的α-H2Pc,在丁酮/环己酮体系中球磨分散4 h保持晶型稳定,制备的分散液24天透过率的变化率为1.26%。将其作为载流子产生材料制备有机光电导器件的光电导响应性能为:V 0=698.24 V,Vr=29.30 V,Rd=12.24 V/s,E 1/2=0.60μJ/cm^2,适用于耐疲劳高速激光打印和复印机中光导鼓的制备。本工作建立了一种简便、成本低、性能优良的纳米α-H2Pc光电导材料的制备方法。Alpha-type metal-free phthalocyanine(H 2Pc)is one of the important organic optoelectronic materials and have better near infrared photoelectric response performance.In this paper,by adding H 2Pc sulfuric acid solution directly to the binary dispersion medium composed of different ratios of MEK and water,nano-α-H 2Pc with high stability and dispersion stability was prepared by one-step method.The effects of the dispersion medium composition,stirring speed,crystalline adjustment temperature and time on the crystallinity ofα-H 2Pc were studied.The results showed that a mixed solvent of butanone/water volume ratio of 1:3 was a suitable medium for preparingα-H 2Pc.Under the conditions of 600 rpm,40℃and crystal form adjustment for 5 h,the particle size of the crystals obtained was 68.8 nm and the crystallinity of the crystals obtained was more than 90%.α-H 2Pc was dispersed in the butanone/cyclohexanone system by ball milling for 4 h and kept the crystal form stable.The change rate of the transmittance of the prepared dispersion in 24 days was 1.26%.The photoconductive response performance of organic photoconductive devices prepared with it as a carrier generation material was:V 0=698.24 V,V r=29.30 V,R d=12.24 V/s and E 1/2=0.60μJ/cm 2.The crystal form was suitable for fatigue resistance preparation of photoconductive drums in high-speed laser printing and copiers.In this work,a simple,low-cost,excellent performance nano-α-H 2Pc photoconductive material preparation method was established.

关 键 词：无金属酞菁 纳米 晶型稳定性 分散 光电导性能 

分 类 号：TB34[一般工业技术—材料科学与工程]