Although the dry ice method used to synthesize turbostratic carbon/graphene is little known and used, it has significant advantages over others, such as the following: it is low cost, simple, and a large quantity of material can be obtained using some inorganic and highly available acids (which can be reused). Despite the above advantages, the main reason for its incipient development is the resulting presence of magnesium oxide in the final product. In the present work, three different treatments were tested to remove this remnant using some acid chemical leaching processes, including hydrochloric acid, aqua regia, and piranha solution. Based on the experimental evidence, it was determined that using aqua regia and combining the leaching process with mechanical milling was the most efficient way of removing such a remnant, the residue being only 0.9 wt.%. This value is low compared to that obtained with the other acid leaching solutions and purification processes (2.8–29.6 wt.%). A mandatory high-energy mechanical milling stage was necessary during this treatment to expose and dissolve the highly insoluble oxide without secondary chemical reactions on the turbostratic carbon. High-energy mechanical milling is an effective route to exfoliate graphite, which allows the magnesium oxide to be more susceptible to acid treatment. A yield of turbostratic carbon/graphene of 1 wt.% was obtained from the metallic Mg. The obtained surface area was 504.8 m²g⁻¹; this high value resulting from the intense exfoliation can potentiate the use of this material for a wide variety of applications.

Superparamagnetism in pure and Mn doped CuO nanofibers, originated by oxygen vacances - Volume 27 Issue S1

The copper (II) oxide nanofibers (NFs) synthesized with the electrospinning method showed a necklace-like morphology and nanometric size. The use of the XPS (X-ray Photoelectronic Spectroscopy) technique allowed the analysis of the Cu 2p and O 1s orbitals showing a CuxO type stoichiometry (x = 1, 2, 3), in turn, the UPS (Ultraviolet Photoelectronic Spectroscopy) region determined the conduction state associated to the dielectric function. These data are compared with the EELS technique. The NFs have presented a behavior with double magnetic phase associated to the non-stoichiometry and oxygen vacancies, and the non-presence of the AFM phase due to the increase of the vacancies. In addition, their electronic and magnetic structure reveal spin-orbit related changes shown in the Cu 2p spectra. The results showed in the conduction band holes and the Cu 2p and O 1s orbitals.

CuO and 3 % Mn-doped CuO nanofibers were synthesized employing the electrospinning method. X-ray diffraction (XRD) verified a monoclinic phase with a C 2/c space group. An electronic density analysis, obtained using Fullprof software, was projected on the (110) and (001) planes for both materials, showing modifications in the Cu positions. This fact generated vacancies involved in the paramagnetism formation in the Mn-doped CuO nanofibers, in contrast to the mixed magnetic phase composed by both ferromagnetic and paramagnetic behaviors found in the undoped CuO. The vacancy amount was quantified by X-ray absorption spectroscopy (XAS) applying CASTEP software. In addition, an analysis from Cu 2p XPS peaks supports the predicted Cu-Cu rearrangement by the Fullprof software study, while the presence of Cu1+ confirms the substitution of Mn for Cu in the doped sample.