Sponge-Type Raney Nickel Catalysts Were Used As Anodes In Liquid Fuel Cells Utilizing Methanol Or Hydrazine. Raney Nickel Electrodes Were Prepared From Substrates Of Spongy Nickel Plates Coated With Aluminium By Use Of A Plasma Flame Gun. Electrode Performance In Both Methanol And Hydrazine Fuel Cells Was Improved With Increases In Both The Alloying And The Electrolyte Temperature. Good Polarization Characteristics Resulted From An Increase In Activated Nickel Grains, Which Were Observed By Sem, And From An Increase In Bet Surface Area Of The Electrode. The Broad Peaks Observed In X-Ray Diffraction Of Raney Nickel Implied Crystal Distortion, Which Should Be Related To An Increase In Surface Area. Surface Chemical Specification And Distribution Of Aluminium And Nickel In The Plate-Type Raney Nickel Catalyst Based On Xps, Shows That The Catalyst Surface Is Covered With Ni₂O₃ And/Or Ni(Oh)₂ Within 200 Å Of The Surface, While L₂O₃ And/Or Al(Oh)₃ Are Distributed Evenly In The Vertical Direction Over About 1200 Å. The Xanes Spectrum From The Ni K-Edge Of The Raney Nickel Did Not Change Much From That Of Nickel Metal. The Exafs Function, However, Diminished More Quickly, And From This, The Coordination Number Of Nickel In Raney Nickel Catalysts Was Estimated To Be 6, Compared With 12 For Ordinary Nickel. This Indicates That The Other Six Nickel Atoms Shift From The Original Sites. Exafs Studies As Well As Xrd, Indicate That The Crystal Structure Of The Activated Nickel Contains A Great Number Of Crystal Defects. Epr Measurements Indicate The G-Values Of The Active Raney Nickel Catalyst And The Catalyst When Deactivated By Electrochemical Removal Of Hydrogen To Be 2.07 And 2.22 Respectively. The Change Of G-Value Is Attributed Not To The Lattice Defects But To The Adsorption Of Hydrogen.