真空高温氢化法制备Pd-Zr复合膜

Preparation of Pd-Zr composite membranes by high temperature vacuum hydrogenation

为了获得低成本、高渗氢率、长寿命、高强度的选择渗氢膜,耐熔金属锆(Zr)被选作复合膜的基体。在真空 4.0×10-4 Pa、温度 650 ℃的反应条件下,锆表面氧化 膜 松动 、分解 ,氧化膜被去除 ;再在氢气氛中使其洁净表面上生成一层氢化锆 保 护 膜 ; 在真空度为 6.6×10-6 Pa 下,采用离子溅射镀膜法,在锆片(φ 50 mm×0.23 mm)的双表面上分别镀上了一层厚约 400 nm 的钯(Pd)薄膜,钯膜均 、细 腻 、光洁 , 膜厚易控制 ;再经过退火处理 ,制得了 Pd-Zr复合膜, 膜面致密 , 钯膜与基体锆结合力强 ,内应力消失 。采用 X 射线衍射(XRD)和 X 光电子能谱(XPS)对锆表面及复合膜表面进行了分析。制备的 Pd-Zr 选择渗氢复合膜对核燃料和聚变燃料的纯化及反应堆增殖剂中氚的提取将具有很大的应用前景。

In order to prepare low cost, high hydrogen permeability, long runtime and high stress H-permselective membranes, the refractory metal zirconium (Zr) was selected as the membrane’s substrate. Using high temperature vacuum hydrogenation method ( at the vacuum of 4.0×10-4 Pa and 650 ℃), the surface oxide film of Zr was relaxed, decomposed and removed; then ZrH2 film was formed on the clean Zr surface at hydrogen atmosphere. At the vacuum of 6.6×10-6 Pa, a Pd film about 400 nm thick was deposited on each surface of the zirconium disk (φ 50 mm ×0.23 mm) by the method of ion sputtering plating. The Pd membrane is bright, fine and smooth. It is easy to control the Pd film thickness. Having been annealed, the Pd film adheres strongly to the Zr substrate, and the internal stress between the Pd and the Zr disappears. The composite membranes are compact and bright. The surfaces of the zirconium and the composite membrane were analyzed by XRD and XPS. These Pd-Zr H-permselective composite membranes will be vastly applicable to the purification of nuclear and fusion fuel and the distillation of tritium from breeder reactor.