NIST Center for Neutron Research Materials Science and Engineering Laboratory NIST Center for Neutron Research National Institute of Standards and Technology
Welcome to Dr. Yildirim's Hydrogen Storage Website

H2 Storage Projects

Direct Observation of Hydrogen Adsorption Sites and Nano-Cage Formation in Metal-Organic Frameworks (MOF)

Introduction | Synthesis | MOF-host lattice | Adsorbtion sites 4-8H2/4Zn | Adsorption sites up to 26 H2/4Zn | H2-nanocage formation (32/46 H2/4Zn) | Conclusions |

 


Synthesis of Deuterated MOF5:

The deuterated MOF-5 used in this investigation was synthesized by combining 5.000 g of deuterated terephthalic acid (Sigma-Aldrich stock number 195553) with 25.942 g of zinc nitrate hexahydrate (Fluka stock number 96482) in 800 mL of N,N-diethylformamide (TCI-America stock number D0506). The reactants were stirred continuously until completely dissolved after which the mixture was evenly distributed amongst five 150 mL jars fitted with Teflon gasketed lids. The tightly sealed jars were placed in a furnace at 100 oC for a period of sixteen hours at which point the reaction mixture had a dark-yellow appearance and crystallites were clearly visible on the sides and bottom of the vessels. The reaction vessels were removed from the oven and placed in a glove bag that had been thoroughly purged with nitrogen gas. The dark yellow liquid above the crystallites was removed with a syringe and the crystallites were rinsed with N,N-dimethylformamide (Sigma-Aldrich stock number D158550). The N,N-dimethylformamide was subsequently extracted with a syringe and chloroform (Mallinckrodt stock number 4441) was put in its place. After 12 hours, the initial chloroform was removed and replaced with fresh chloroform, and the MOF crystals were allowed to soak in the fresh chloroform for a period of one week. The chloroform was removed from the MOF material through active evacuation with a turbo molecular pump at a pressure of ~1E-05 Torr. The evacuated mass of the deuterated MOF-5 was 3.752 g, corresponding to a 49% yield based upon the mass of terephthalic acid used in the reaction.

Address :
Taner Yildirim
Building 235 - E112
NIST Center for Neutron Research
National Institute of Standards and Technology
Gaithersburg, MD 20899
Phone : (301) 975-6228
FAX : (301) 921-9847
Click to Send Email taner@nist.gov

Last updated: Thursday 02nd of August 2007
Today's date: Monday 23rd of November 2009
Number of visitors so far is 44668
©2005 taner@nist.gov