Dear respected RG members,

Recently, we tried to prepare Ni doped MgO nanoparticles using co-precipitation method. The XRD pattern of pure MgO-NPs is going well with five peaks (20-80 degree). We encountered unusual peak at around (64 degree) 2theta for 3% doped MgO-NPs. We follow the same procedure of preparing pure MgO. Stiocheiometric amount of magnesium nitrate hexahydrate (0.097 mol) and nickel nitrate hexahydrate (0.003 mol ) were dissolved in 200 ml water and the aqueous solution heated to 70 Celsius. Then, 0.2 mol of NaOH was add to the mixture as fast as possible till the precipitate occur (pH 10 ) and stirred for another 2 hrs at 70 C. The precipitate dried and crushed (using pestle and mortar) and calcined at 500 C for 2 hrs with a heating rate of 10 degree/min.

Our main concerns are:

1- The unknown peak at (64 degree) may come from impurity during grinding using pestle and mortal.

2- Is the incorrect calculation ( nonstoichiometric ) of the main precursor and the reagent cause this issue?

3- The Ni show very high solubility in MgO host lattice without phase separation, so we do not believe that the impurity is related to Ni, NiO or Ni2O3.

Please we are looking for your recommendation and help

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