ABSTRACT
The synthesis of bulk nanoporous copper (npCu) from a copper-manganese alloy by electrochemical dealloying and free corrosion as well as the electrochemical behaviour of the dealloyed structures is investigated by in situ resistometry. In comparison to the well-established nanoporous gold (npAu) system, npCu shows strongly suppressed reordering processes in the porous structure (behind the etch front), which can be attributed to pronounced manganese oxide formation. Characteristic variations with the electrolyte concentration and potential applied for dealloying could be observed. Cyclic voltammetry was used to clarify the electrochemical behaviour of npCu. Oxide formation is further investigated by SEM and EDX revealing a hybrid composite of copper and manganese oxide on the surface of a metallic copper skeleton. Platelet-like structures embedded in the porous structure are identified which are rich in manganese oxide after prolonged dealloying. As an outlook, this unique heterogeneous structure with a large surface area and the inherent properties of manganese and copper oxides may offer application potential for the development of electrodes for energy storage and catalysis.
ABSTRACT
Temperature modulated thermophysical measurements can deliver valuable insights into the phase transformation behavior of many different materials. While especially for non-metallic systems at low temperatures numerous powerful methods exist, no high-temperature device suitable for modulated measurements of bulk metallic alloy samples is available for routine use. In this work a dilatometer for temperature modulated isothermal and non-isothermal measurements in the temperature range from room temperature to 1300 K is presented. The length measuring system is based on a two-beam Michelson laser interferometer with an incremental resolution of 20 pm. The non-contact measurement principle allows for resolving sinusoidal length change signals with amplitudes in the sub-500 nm range and physically decouples the length measuring system from the temperature modulation and heating control. To demonstrate the low-amplitude capabilities, results for the thermal expansion of nickel for two different modulation frequencies are presented. These results prove that the novel method can be used to routinely resolve length-change signals of metallic samples with temperature amplitudes well below 1 K. This high resolution in combination with the non-contact measurement principle significantly extends the application range of modulated dilatometry towards high-stability phase transformation measurements on complex alloys.
