磷化法制备Ni_(x)P_(y)及其复合材料光解水性能  

Photocatalytic properties of Ni_(x)P_(y) and its composites prepared by phosphating method

作　　者：颜瑞 孙志超[1,2] 张蒙蒙 刘颖雅 遇治权 王伟[3] 王瑶 王安杰[1,2] YAN Rui;SUN Zhichao;ZHANG Mengmeng;LIU Yingya;YU Zhiquan;WANG Wei;WANG Yao;WANG Anjie(State Key Laboratory of Fine Chemicals,Dalian University of Technology,Dalian 116024,Liaoning,China;Liaoning Key Laboratory of Petrochemical Technology and Experiment,Dalian 116024,Liaoning,China;Yinchuan Energy Institute,Yinchuan 750105,Ningxia,China)

机构地区：[1]大连理工大学精细化工国家重点实验室,辽宁大连116024 [2]辽宁省高校石油化工技术与装备重点实验室,辽宁大连116024 [3]银川能源学院,宁夏银川750105

出　　处：《化工进展》2022年第5期2468-2475,共8页Chemical Industry and Engineering Progress

基　　金：国家重点研发计划政府间国际科技创新合作重点专项(2016YFE0109800);国家自然科学基金(21603024,21972014);辽宁省博士启动基金(201601038);宁夏重点研发计划(2018BEE03030);中央高校基本科研业务费项目(DUT19GJ205)。

摘　　要：磷化镍具有Ni_(3)P、Ni_(12)P_(5)、Ni_(2)P、Ni_(5)P_(4)等多种晶相,深入研究各个晶相的制备规律和稳定存在条件对开发磷化镍基催化材料至关重要。本文系统考察了磷化时间、磷化温度、Ni/P摩尔比、磷化气速和磷源种类对制备晶相的影响。结果发现,以Ni_(3)P为前体、红磷为磷源时,可以得到Ni_(5)P_(4)、Ni_(2)P、Ni_(12)P_(5)三种晶相;以次磷酸盐为磷源时只能得到Ni_(2)P和Ni_(12)P_(5)晶相。当以红磷为磷源时,反应温度是影响晶相的主要因素,磷化温度为500℃、600℃和800℃时分别得到Ni_(5)P_(4)、Ni_(2)P和Ni_(12)P_(5)晶相。将制备的Ni_(3)P、Ni_(2)P、Ni_(12)P_(5)和Ni_(5)P_(4)作为助剂,与CdS复合制备光催化复合材料,得到的4种Ni_(x)P_(y)/CdS复合材料均表现出良好的光解水制氢性能,Ni_(5)P_(4)/CdS表现出最优的产氢能力,为CdS的5.4倍。表征结果证明,引入Ni_(x)P_(y)能够有效抑制反应过程中CdS的载流子复合,提升其光解水反应活性。Nickel phosphide(Ni_(x)P_(y))has many crystalline phases,such as Ni_(3)P,Ni_(12)P_(5),Ni_(2)P,Ni_(5)P_(4),etc.It is important to study the preparation rule and stable existence conditions of each crystalline phase for the development of catalysts based on Ni_(x)P_(y).In this paper,the effects of phosphating time,phosphating temperature,Ni/P molar ratio,phosphating gas velocity and phosphorus source on the crystal phase were investigated.The results showed that three crystalline phases of Ni_(5)P_(4),Ni_(2)P and Ni_(12)P_(5)can be obtained with Ni_(3)P and red phosphorus as precursors.Only Ni_(2)P and Ni_(12)P_(5)crystal phases can be obtained with hypophosphite as phosphorus source.The reaction temperature was the main factor affecting the crystal phase when red phosphorus was used as the phosphorus source.Ni_(5)P_(4),Ni_(2)P and Ni_(12)P_(5)crystal phases were obtained at 500℃,600℃and 800℃,respectively.Ni_(3)P,Ni_(2)P,Ni_(12)P_(5)and Ni_(5)P_(4)were used as cocatalysts to prepare photocatalytic composites.All the four cocatalysts of Ni_(x)P_(y)can significantly enhance the hydrogen production activity of CdS.Ni_(5)P_(4)/CdS indicated the best hydrogen production capacity,which was 5.4 times that of CdS.The results of characterization showed that the introduction of Ni_(x)P_(y)could effectively inhibit the carrier recombination and enhance the photocatalytic activity of CdS.

关 键 词：催化 复合材料 光化学 磷化镍 晶相 硫化镉 

分 类 号：TQ138.1[化学工程—无机化工]