Continuous wet chemical approaches for the production of inorganic nanoparticles are important for large scale production of nanoparticles. Here we describe a bottom-up, wet chemical method applying a microjet reactor. This technique allows the separation between nucleation and growth in a continuous reactor environment. Zinc oxide (ZnO), magnetite (Fe 3 O 4 ), as well as brushite (CaHPO 4 ·2H 2 O), particles with a small particle size distribution can be obtained continuously by using the rapid mixing of two precursor solutions and the fast removal of the nuclei from the reaction environment. The final particles were characterized by FT-IR, TGA, DLS, XRD and SEM techniques. Systematic studies on the influence of the different process parameters, such as flow rate and process temperature, show that the particle size can be influenced. Zinc oxide was obtained with particle sizes between 44 nm and 102 nm. The obtained magnetite particles have particle sizes in the range of 46 nm to 132 nm. Brushite behaves differently; the obtained particles were shaped like small plates with edge lengths between 100 nm and 500 nm.
Innovative synthetic approaches should be simple and environmentally friendly. Here, we present the surface modification of inorganic submicrometer particles with long alkyl chain organophosphorus coupling agents without the need of a solvent, which makes the technique environmentally friendly. In addition, it is of great benefit to realize two goals in one step: size reduction and, simultaneously, surface functionalization. A top-down approach for the synthesis of metal oxide particles with in situ surface functionalization is used to modify titania with long alkyl chain organophosphorus coupling agents. A high energy planetary ball mill was used to perform reactive milling using titania as inorganic pigment and long alkyl chain organophosphorus coupling agents like dodecyl and octadecyl phosphonic acid. The final products were characterized by IR, NMR and X-ray fluorescence spectroscopy, thermal and elemental analysis as well as by X-ray powder diffraction and scanning electron microscopy. The process entailed a tribochemical phase transformation from the starting material anatase to a high-pressure modification of titania and the thermodynamically more stable rutile depending on the process parameters. Furthermore, the particles show sizes between 100 nm and 300 nm and a degree of surface coverage up to 0.8 mmol phosphonate per gram.
The reaction of elemental rhodium and concentrated sulfuric acid (97 %) at 400°C leads to red plate-shaped single crystals of Rh 2 (SO 4 ) 3 [trigonal, R3, Z = 6, a = 806.8(1) pm, c = 2204.8(4) pm, V = 1242.8(4) × 10 6 pm 3 ]. The same reaction carried out at a temperature of 475°C leads to orange crystals of Rh 2 (SO 4 ) 3 ·2H 2 O [orthorhombic, Pnma, Z = 4, a = 920.46(2) pm, b = 1244.47(3) pm, c = 833.37(2) pm, V = 954.61(4) × 10 6 pm 3 ].[a]
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