In situ observation on dehydrogenation of MgH 2 was performed by using transmission electron microscope ͑TEM͒. 7-9 However, the detail of the catalytic reaction has not been understood yet. In this study, the change in the high resolution image before and after dehydrogenation was observed by using with TEM to examine the details of the catalytic reaction.In this study, two kinds of samples with 1 and 10 mol % of Nb 2 O 5 were prepared. For MgH 2 catalyzed with 1 mol % Nb 2 O 5 , MgH 2 powder ͑Alfa Aesar͒, and Nb 2 O 5 powder ͑me-soporous: Sigma-Aldrich͒ were ball-milled under the hydrogen atmosphere of 1.0 MPa for 20 h. On the other hand, for MgH 2 catalyzed with 10 mol % Nb 2 O 5 , MgH 2 powder, and Nb 2 O 5 powder ͑single-crystalline: Kojundo chemical Laboratory͒ were mixed by agate mortar in a glovebox filled with Ar gas. The samples were handled without exposure to air in whole process. The sample powder was placed on a microgrid and the grid was set into a heating specimen holder in the glove box under Ar atmosphere. The heating specimen holder was put into a plastic bag under Ar atmosphere and loaded into TEM equipment in order to prevent the oxidation. The samples were observed from room temperature to 200°C by using a TEM ͑JEOL-2010; 200 kV͒, and high resolution images of a 10 mol % catalyzed sample were obtained by using high voltage electron microscope ͑HVEM, JEM-ARM1300; 1250 kV͒. With respect to temperature control for in situ TEM observation, the temperature was rapidly raised up and kept at 100, 150, or 200°C. The TEM images were analyzed by the selected area electron diffraction pattern ͑SADP͒, fast Fourier transformation ͑FFT͒, and inverse fast Fourier transformation ͑IFFT͒.At the first step, observation by using a conventional TEM ͑200 kV͒ was carried out for MgH 2 catalyzed with 1 mol % Nb 2 O 5 , which showed a remarkable catalytic effect. APPLIED PHYSICS LETTERS 96, 223109 ͑2010͒