Synthesis of Zirconium Diboride (ZrB2) Nanoparticles by Sol-gel Method

Synthesis of Zirconium Diboride (ZrB₂) Nanoparticles by Sol-gel Method

1. CHECK LIST

   Zirconium Propoxide (Zr(OPr)4), Boric Acid (H3BO3), Sucrose (C12H22O11), Acetic Acid (CH3COOH), Methanol (CH3OH), Acetylacetone (C5H8O2), Water
2. STEP 1.

   Add Zirconium Propoxide (6.3ml) and Acetylacetone (1.2ml) in 25ml of Methanol. Stirrer it at room temperature.
3. STEP 2.

   Add 4ml of water dropwise and stirrer for 30 minutes at room temperature.
4. STEP 3.

   In another beaker, Add Boric Acid (2.5g) and Sucrose (2.9g) in 45ml of Acetic Acid. Stirrer for 30 minutes a 80°C.
5. STEP 4.

   Add Zirconium Propoxide solution into Boric Acid solution and stirrer for 4 hours at 60°C to form the wet gel.
6. STEP 5.

   Dry the formed wet gel at 120°C for 3 hours to form the final precursor.
7. STEP 6.

   Now grind the dried sample with mortar-pestle. And Calcine it at 1550°C for 4 hours at a slow ramping rate of 2-3°C/min.
8. RESULTS

   Finally, Zirconium Diboride (ZrB2) Nanoparticles are formed as Gray color after calcination.
9. Factors Affecting Synthesis

   Calcination (in STEP 6) can also be done in 3 steps. First 30-800°C with 5°C/min, then 800-1200°C with 3°C/min for 2 hours and finally 1200-1550°C with 2°C/min for another 2 hours. Cooling rate should be 5°C/min. This elaborated calcination can increase the crystallinity of the formed Zirconium Diboride (ZrB2) Nanoparticles.
10. NOTE: All the experiments should be done under the guidance of lab Incharge; and proper lab safety instructions.