Highly dispersive nanospheres of MnFe2O4 are prepared by template free hydrothermal method. The nanospheres have 47.3-nm average diameter, narrow size distribution, and good crystallinity with average crystallite size about 22 nm. The reaction temperature strongly affects the morphology, and high temperature is found to be responsible for growth of uniform nanospheres. Raman spectroscopy reveals high purity of prepared nanospheres. High saturation magnetization (78.3 emu/g), low coercivity (45 Oe, 1 Oe = 79.5775 A·cm−1), low remanence (5.32 emu/g), and high anisotropy constant 2.84 × 104 J/m3 (10 times larger than bulk) are observed at room temperatures. The nearly superparamagnetic behavior is due to comparable size of nanospheres with superparamagnetic critical diameter Dcrspam. The high value of Keff may be due to coupling between the pinned moment in the amorphous shell and the magnetic moment in the core of the nanospheres. The nanospheres show prominent optical absorption in the visible region, and the indirect band gap is estimated to be 0.98 eV from the transmission spectrum. The prepared Mn ferrite has potential applications in biomedicine and photocatalysis.

3-D flower like CoNi alloys nanostructures composed of nanorods have been synthesized by template free hydrothermal method at relatively low temperature (120 °C). The detailed characterizations confirm the formation of good crystalline fcc CoNi alloy, average crystallite size of 18.8 ± 1.0 nm, lattice parameter of 3.531 ± 0.01 Å, and the nearly equiatomic composition (Co₅₀Ni₅₀). Highly uniform flower like nano structures are built up with nanorod of diameter about 100 nm and length in range of 200–400 nm. The nanorods (building blocks of flower) have single crystalline nature with [111] preferred growth direction. The concentration of NaOH plays a vital role in formation of alloys and high concentration promotes the formation of CoNi alloy at low temperature. The concentration of NaOH also affects the morphology remarkably by changing the growth/reaction rate of CoNi nanostructures and results in hollow spheres to nanoplate flower of CoNi alloys. Based on the evolution of the morphology of the products, a step wise growth mechanism is rationally proposed for flower like nanostructures by considering the effects of kinetic parameters on growth. Magnetic measurements show Co₅₀Ni₅₀ flower like nanostructure have high saturation magnetization, coercivity, remanent magnetization, and high effective anisotropy constant of value 101.3 emu g⁻¹, 210.5 Oe, 16.2 emu g⁻¹, and 4.457 × 10⁴ J m⁻³ respectively. The enhancements of coercivity and effective anisotropy constant are attributed to nanoscale effects such as shape/surface anisotropy.