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γ射线辐射法已成功地从含有铜和钯混合离子的较浓溶液中制备出粒径分布较均匀的Cu—Pd合金超细粉末。实验发现,用不同的络合物作配体时,虽然溶液的pH都调至10左右,得到的结果却不尽相同。用氨水作配体时,辐照后的溶液一部分自然沉降(样品1),另一部分经水热处理(样品2),得到的粉末经XRD测试,证实都是具有面心立方结构(fcc)的Cu—Pd合金(均匀固溶体),其格子常数分别为3.6886和3.6916A,在铜和钯的格子常数之间。用谢乐公式估计它们的粒径大小分别为8和9nm。TEM观察样品1和2的粒子形貌皆为准球形晶粒,两者的颗粒度都在10nm左右,与谢乐公式计算的结果相吻合。还发现这两个样品的粒子团聚现象严重,即使用超声也难以分散开来。XPS分析样品1中铜的原子含量为78.6%,把的原子含量为21.4%两者之比约为3.7:1,与溶液的原始配比3:1较为一致。用OH-作配体时,辐照后的溶液同样一部分自然沉降(样品3),另一部分经水热处理(样品4),这样得到的粉末经XRD检测,也表明了都是具有fcc结构的Cu—Pd固溶体,只是样品4是不均匀的固溶体,而样品3则是均匀的固溶体,说明水热处理反而破坏了固溶体的均匀性。经计算,?
γ-ray irradiation method has been successfully prepared from a concentrated solution containing copper and palladium mixed ions prepared Cu-Pd alloy particles with relatively uniform distribution of particle size. The experimental results show that when different complexes are used as ligands, the pH of the solution is adjusted to about 10, but the results obtained are not the same. When ammonia was used as the ligand, part of the irradiated solution naturally precipitated (Sample 1) and the other was hydrothermally treated (Sample 2). The resulting powders were tested by XRD and confirmed to be Cu with face-centered cubic structure (fcc) -Pd alloy (homogeneous solid solution) with lattice constants of 3.6886 and 3.6916A, respectively, between the lattice constants of copper and palladium. With Xie Le formula to estimate their size of the size of 8 and 9nm. The particle morphology of samples 1 and 2 were all quasi-spherical grains by TEM. The particle sizes of both samples were about 10 nm, which were in good agreement with the results of Xie Le formula. It was also found that the two samples had severe agglomeration of particles and were difficult to disperse even with ultrasound. The atomic content of copper in sample 1 of XPS was 78.6% and the atomic content of 21.4% was about 3.7: 1, which was consistent with the original ratio of solution of 3: 1. When OH- was used as ligand, the same part of the irradiated solution naturally precipitated (Sample 3) and the other part was hydrothermally treated (Sample 4). The resulting powder was examined by XRD and also showed that both of the Cu -Pd solid solution, except that Sample 4 is an inhomogeneous solid solution and Sample 3 is a uniform solid solution, indicating that the hydrothermal treatment destroys the solid solution homogeneity instead. Calculated,?