Page 68 - 《精细化工》2022年第6期
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第 39 卷第 6 期                             精   细   化   工                                  Vol.39, No.6
             2022 年 6 月                              FINE CHEMICALS                                 June  2022


              功能材料
                    超临界流体沉积法对钯铜纳米粒子制备的影响



                                                                                            *
                            魏   炜,王   焘,董   超,韩   宇,刘凤霞,刘志军
                                (大连理工大学  流体与粉体工程研究设计所,辽宁  大连  116024)


                 摘要:以乙酰丙酮钯、乙酰丙酮铜为金属前驱体,以氧化铝球为载体,采用超临界流体沉积法(SCFD)制备了
                 氧化铝球负载的 Pd-Cu 纳米粒子(Pd-Cu/Al 2 O 3 )。采用高角度环形暗场-扫描透射电子显微镜(HAADF-STEM)、
                 XRD 和称重法对金属前驱体负载状况与 Pd-Cu 纳米粒子平均粒径进行了表征。结果表明,在金属前驱体投料量
                 一定时,沉积时间存在最佳值。沉积温度与沉积压力对 Pd-Cu 纳米粒子的平均粒径有重要影响。在沉积温度 65
                 ℃、沉积压力 15 MPa、沉积时间 3.0 h 时,Pd-Cu 纳米粒子的平均粒径可达 2.37 nm。助溶剂和 Pd 理论负载量
                 也影响 Pd-Cu 纳米粒子的平均粒径。在上述条件下,使用 8 mL 二氯甲烷作为助溶剂,当 Pd 理论负载量为 0.50%
                 时,Pd-Cu 纳米粒子的平均粒径出现最小值(1.81 nm)。
                 关键词:超临界二氧化碳;超临界流体沉积法;纳米粒子;钯;铜;功能材料
                 中图分类号:TQ138;TB383.1      文献标识码:A      文章编号:1003-5214 (2022) 06-1134-08


                      Effect of supercritical fluid deposition method on preparation of

                                         palladium-copper nanoparticles

                                                                                            *
                            WEI Wei, WANG Tao, DONG Chao, HAN Yu, LIU Fengxia, LIU Zhijun
                 (Fluid and Powder Engineering Research and Design Institute, Dalian University of Technology, Dalian 116024, Liaoning,
                 China)


                 Abstract: Pd-Cu  nanoparticles were deposited on alumina balls (Pd-Cu/Al 2 O 3) by  supercritical fluid
                 deposition (SCFD) method using alumina balls as carriers and  palladium acetylacetonate and  copper
                 acetylacetonate as precursors. The loading status of metal precursors and the average particle size of Pd-Cu
                 nanoparticles were  characterized by high-angle  annular dark field-scanning  transmission  election
                 microscope (HAADF-STEM), XRD and weighing methods. The results showed that there was an optimal
                 value for the deposition time with a  fixed amount  of metal precursors. Deposition temperature and
                 deposition pressure had important effects on the average particle size of Pd-Cu nanoparticles. The average
                 particle size of Pd-Cu nanoparticles could reach 2.37 nm at deposition temperature of 65 ℃, deposition
                 pressure of 15 MPa and deposition time of 3.0 h. Co-solvent and Pd theoretical loading also had effect on
                 the average  particle size  of Pd-Cu  nanoparticles. Under the above conditions, using  8 mL  of
                 dichloromethane as co-solvent, when Pd theoretical loading was 0.50%, the average particle size of Pd-Cu
                 nanoparticles reached the minimum value (1.81 nm).
                 Key words: supercritical carbon dioxide; supercritical fluid deposition; nanoparticles; palladium; copper;
                 functional materials


                 纳米金属材料是指晶粒尺寸≤100 nm 的金属                       等纳米金属材料的固有缺陷,因此成为近年来的研
            材料,具有比表面积大、体积相对较小、表面能与                             究热点   [16-31] 。
            表面结合能大等优点          [1-2] ,在催化、环境修复、信息                  1995 年,WATKINS 等     [32] 针对化学气相沉积法
            存储、医疗材料等领域具有重要应用                  [3-15] 。而负载      (CVD)制备条件苛刻、沉积不均匀、微孔内部沉
            型纳米金属粒子避免了团聚失活、不易分离和回收                             积困难等缺点,提出超临界流体沉积(SCFD)法并

                 收稿日期:2021-12-13;  定用日期:2022-01-21; DOI: 10.13550/j.jxhg.20211274
                 作者简介:魏   炜(1980—),女,副教授,硕士生导师,E-mail:hjweiwei@dlut.edu.cn。联系人:刘志军(1969—),男,教授,博
                 士生导师,E-mail:liuzj@dlut.edu.cn。
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