Hi,

Any muffle furnace (programmable) is fine for the synthesis. The only thing you can vary is the temperature, time and ramp rate.

All the best.

I tried to prepare them in box furnace with nitrogen flow at 550 C for 4 hrs heating with ramping rate 5 C per minute in silica crucible with lid. But surprisingly there is no pyrolysis product as well as starting material after cool down.

Hi,

You can take the starting precursor quantity more in order to get the product. After calcination, you will see very little quantity with a pale yellow color. So, increase the quantity and see in 500 degree Celcius.

All the best.

Dear Susanta Kumar, try sources like melamine. urea and cover crucible properly with lid and keep in a muffle furnace.

All the best.

Dear Harsha,

This is a Carboxyl-rich nanoparticles can be prepared through the hydrothermal oxidation of g-C3N4 nano sheet. It can be used as a florescence sensor for selective detetction of Hg2+ and Fe3+.

Synthesis methods:

Porous g-C3N4 can be synthesized with the assistance of some organic compounds, including ionic liquids, surfactants and amphiphilic block polymers. When these materials and g-C3N4 precursors are subjected to heat treatment, these organic compounds decompose and generate volatile intermediates, whose diffusion lead to porous structure. Nevertheless, the thermal decomposition of these organic compounds leads to high carbon doping contents for g-C3N4, resulting in the poor photoactivity. It is hypothesized that if a compound excluding carbon element can absolutely decompose during the thermal condensation of g-C3N4 precursors, the porous g-C3N4 not only will be obtained, but also with no high carbon doping.

The inorganic ammonium salts, NH4Cl as bubble-generated porogen for the preparation of porous g-C3N4. NH4Cl is a low-cost and widely available compound, and more importantly, it can absolutely decompose and generate gas bubbles (NH3 and HCl) during the condensation of melamine (g-C3N4 precursor).

[Ref: https://www.sciencedirect.com/science/article/pii/S0025540817340783] follow 22, 22 and 23 no. reference of the same article.

Ashish

Dear Sushanta,

This is a Carboxyl-rich nanoparticles can be prepared through the hydrothermal oxidation of g-C3N4 nano sheet. It can be used as a florescence sensor for selective detetction of Hg2+ and Fe3+.

Synthesis methods:

Porous g-C3N4 can be synthesized with the assistance of some organic compounds, including ionic liquids, surfactants and amphiphilic block polymers. When these materials and g-C3N4 precursors are subjected to heat treatment, these organic compounds decompose and generate volatile intermediates, whose diffusion lead to porous structure. Nevertheless, the thermal decomposition of these organic compounds leads to high carbon doping contents for g-C3N4, resulting in the poor photoactivity. It is hypothesized that if a compound excluding carbon element can absolutely decompose during the thermal condensation of g-C3N4 precursors, the porous g-C3N4 not only will be obtained, but also with no high carbon doping.

The inorganic ammonium salts, NH4Cl as bubble-generated porogen for the preparation of porous g-C3N4. NH4Cl is a low-cost and widely available compound, and more importantly, it can absolutely decompose and generate gas bubbles (NH3 and HCl) during the condensation of melamine (g-C3N4 precursor).

[Ref: https://www.sciencedirect.com/science/article/pii/S0025540817340783] follow 22, 22 and 23 no. reference of the same article.

Ashish

I started heating at 400 C even by taking 10 g melamine in muffle furnace. After reaching temperature at 350 C, a lot of fume came out and there was no product at all even after 45 minutes heating.

Please suggest some solution

Dear Sushanta,

It may come out fume because the condensation of melamine ad appropriate adjustment of mass ratio doe for precursor.. Have you adjusted the mass ratio of ammonium chloride and calcification temperature? what mass ratio and for calclination what temperature you have maintained? If mass ratio is high not adjusted appropriately they will generate gas bubbles. to control some water splitting is also required. Use intake of 0.8 gm of malamine along with 2 gm of ammonium chloride mix and ground to form the precursors. then precursor can be transfered to 10 ml crucible,, at 300 degree(not 400 degree centigrade) if purpose is not to get yoke shell structure for 2 hour. Hopefully it will work out. temperature and mass ratio is more important here due to ammonia.

Have you used solid or liquid ammonium chloride?

Ashish