To characterize the morphology and composition of the microwave synthesized nickel hydroxide nanosheets by SEM and EDS, prepare the sample by suspending a small amount of nickel hydroxide powder in one milliliter of ethanol using a water bath sonicator. Then drop cast the nickel hydroxide and ethanol mixture on an SEM stub and evaporate the ethanol by heating the stub in a sample oven at 70 degrees Celsius before collecting the SEM micrographs and EDS spectra. In order to determine the surface area and porosity of the nanosheets, add 25 milligrams of nickel hydroxide nanosheets into the sample tube.
Carry out a pre-analysis degassing and drying procedure under vacuum at 120 degrees Celsius for 16 hours. Lastly, transfer the sample tube from the degassing port to the analysis port to collect nitrogen isotherms. For structural analysis using X-ray diffraction or XRD, fill the sample well of a zero-background powder XRD holder with nickel hydroxide.
Collect powder X-ray diffractograms using a copper K-alpha radiation source between a 2-theta of 2 to 80 degrees with a 0.01 step increment. Equip the attenuated total reflectance or ATR attachment to the Fourier Transform Infrared or FTIR spectrometer. Press a small amount of nickel hydroxide powder between two glass slides to create a pellet.
Then place the nickel hydroxide pellet on the silicon ATR crystal and obtain an FTIR spectrum between 404, 000 reciprocal centimeters as an average of 16 individual scans with a resolution of four reciprocal centimeters. SEM revealed that the microwave synthesized nickel hydroxide was composed of randomly interwoven ultra thin nanosheet aggregates. However, increasing the reaction temperature from 120 to 180 degrees Celsius increased the lateral sheet dimensions of individual nanosheets in the aggregates.
Also, increasing the reaction time from 13 to 30 minutes at 120 degrees Celsius increased the nucleated aggregate sizes from about three to five microns. EDS showed a uniform distribution of nickel, oxygen, carbon, and nitrogen within all the synthesized nanosheets. The nanosheets had BET surface areas ranging from 61 to 85 square meters per gram, average pore diameter of 21 to 35 angstroms, and cumulative poor volumes of 0.4 to 0.6 cubic centimeters per gram.
The XRD patterns of all three microwave synthesized samples showed characteristic peaks of alpha nickel hydroxide. However, reaction time and temperature affected the peaks as demonstrated by the shifting of the 001 plane. The ATR-FTIR spectra of the microwave synthesized nanosheets showed characteristic nickel oxide lattice mode.
Modes from the ligands and structural molecules, cyanate bands and alpha hydroxide lattice modes. Increasing the reaction temperature from 120 to 180 degrees Celsius altered the frequencies and relative intensities of the cyanate, nitrate, hydroxyl, and water vibrational modes.
