Dear fellow researchers:
I prepared Pd/MOFs powder via wet impregnation using PdCl2 as precursor solution. To reduce Pd(II) to Pd(0) before applying catalysis, and also to find a convenient alternative to the typical reduction process in a tube furnace under very high temperature, is it possible to dissolve my sample in water and transfer the solution to a sealed autoclave with 4MPa hydrogen flow under ambient temperature (e.g. 30C)? If not, what is the appropriate condition (e.g. time, temperature) of H2 reduction? Thank you!
From my experience when I analized Pd by TPR (temperature programmed reduction), my Pd (II) supported samples were reduced to Pd0 under H2 gas flow at temperatures between 30-60ºC. The sample amount was around 20mg and the pattern obtained was a sharp peak.
Manuel Checa-Gómez
Hi! Did you add solid samples directly or use solvents to disperse them before reduction？And how long should I reduce my samples?
Previously I dissolved my Pd(II) supported samples in water prior to reduction under 30C. Although the samples did turn black, a lower Pd content (tested by ICP-MS) and two rough, vague Pd(0) peaks (tested by XPS) were observed.
Hi, In my case, solid samples were placed in a quartz U-tube a reduced under H2 with a H2 flow rate of 50ml/min and a temperature ramp of 10ºC/min. The peak maximun was at 313K. I think a reduction time of 1h at 50ºC would be enought.
Nevertheless, I recommend you to perform a TPR of your samples to determine the minimal reduction temperature to reduce your Pd sample.
- Badges
- Science topic
- Similar topics
- Physical Sciences
- Materials Science