Synthesis of Metal Nanoparticles Supported on Carbon Nanotube with Doped Co and N Atoms and its Catalytic Applications in Hydrogen Production

This protocol is about developing low cost and highly efficient catalyst with reliable performance and longstanding stability. The developed catalyst could be used for renewable energy productions and may even solve the problem of energy crisis. The advantage of this study is to construct both particle and atomically disperse metal atoms on the same catalyst supports, which may perform synergistically for certain types of catalystic reactions.

In exploring the potential of renewable energy for vehicles to meet future regulatory and sustainability needs, the rapid development of hydrogen fuel cells and vehicles as well as other related fields has effectively promoted the advancement of hydrogen energy technology. So the objective of this research is to develop a novel hydrogen powered fuel cell prototype using solid hydrogen storage materials for renewable energy to be used in various sectors like transport, logistics, et cetera. Begin by weighing 280 grams of diacid and diamide into an 800 milliliter beaker.

Then place the beaker into a muffle furnace and slowly raise the temperature from room temperature to 350 degrees Celsius for the ramp of five degrees per minute. Keep the temperature at 350 degrees Celsius for two hours. Then cool down the furnace by natural cooling.

Grind the obtained white solids into fine powder as the carbon nitride materials in the melem form. Begin by mixing and grinding 10 grams of carbon nitride in the melem form with 0.218 grams of cobalt acetyl acetate until the homogenous color is observed. Add six milliliters of citric acid solution in this homogenous mixture and further grind the materials.

Dry the materials in an oven at 60 degrees Celsius for six hours. Place these materials into a square shaped crucible and then into a tubular furnace. Heat the materials at a heating rate of 2.6 degrees Celsius per minute from room temperature to 800 degrees Celsius and place it under an argon flow of 100 milliliters per minute for two hours.

Slowly cool the furnace by natural cooling, then weigh out the catalyst samples. Set up the water filled inverted cylinder system and 0.1 molar sulfuric acid washing solution. Connect the schlenk flask with the washing solution and the water filled inverted cylinder.

Place 0.04 grams of the catalyst into the schlenk flask and sonicate the solution at 40 kilohertz in an ultrasonic bath for six minutes. Then prepare to add 0.04 grams of ammonia borane to 0.948 milliliters of water and inject one milliliter of the solution into the reactor to initiate the hydrolysis reaction. Monitor the drop in the water level as the reaction proceeds and carefully record the production volume at designated times.

Plot a graph of the volume of hydrogen production versus time in minutes. Place 0.04 grams of the catalyst and 10 milliliters of water into the schlenk flask and immerse it into the water bath at 40 degrees Celsius. Sonicate the solution at 40 kilohertz in an ultrasonic bath for six minutes, inject one milliliter of the ammonia borane solution to the reactor to initiate the hydrolysis reaction, then record the time for completion of the hydrogen release.

Inject one milliliter of the ammonia borane solution to the reactor to initiate the hydrolysis reaction, then record the time for completion of the hydrogen release. Filter off the catalyst by washing it three times with five milliliters of water. Then drive the catalyst in a 60 degree Celsius oven for three hours.

Place the catalyst in 10 milliliters of water and sonicate the solution at 40 kilohertz in an ultrasonic bath. Repeat these steps for 10 cycles. Then plot a graph of hydrogen production volume versus cycles.

Immerse the schlenk flask containing the catalyst and 0.5 molar sulfuric acid into the oil bath. Stir the reaction for two hours, then filter off the solid using a buchner funnel. Wash the solid three times with 10 milliliters of deionized water each time.

Dilute the obtained leachate further to 250 milliliters in a 250 milliliter volumetric flask and collect the metal nanoparticle leached solids by drying at 60 degrees Celsius in an oven. The strong and sharp x-ray defraction piece of metallic cobalt indicate a well-defined crystalline structure, remaining unchanged after recycles. While the structural defects were studied using Raman spectroscopy.

The XPS spectrum showed the presence of each element their bonding and the hybridization of carbon atoms during the formation of the carbon nanotube structures. The absorption desorption isotherm demonstrated a specific surface area of 42.02 meters square per gram and the average pore size distribution of 3.6 nanometers. The SEM and HRTEM images depicted the five micrometer tubular structure of cobalt nanoparticles resulting from the catalyzing growth of the nanofiber along with their EDS mapping.

The crystal in structure of the cobalt nanoparticle was characterized by selected area electron defraction. The main body of the carbon nanofiber was wrapped by a few layers of carbon of different orientations and defraction rings. The total metal content determined by ICP-OES was found to be 25.1%weight with 9.7%weight of cobalt nanoparticles and 15.4%weight of cobalt dopings on the carbon nanotubes.

The catalytic performance of the catalyst was studied and it was found that until the 10th time of ammonia borane edition, there was no obvious decline in the catalytic performance. The rate law of reaction was also studied and the activation energy was determined to be 42.8 kilojoules per mole. Avoid overloading the tubular furnace with catalyst precursors since too many decomposition products may block the tube.

Make sure the solids mixture are well mixed. High energy equipment such as milling can be used to facilitate a mixing. These catalysts can be applied in other types of organic transformation reactions and small molecule activation such as hydrogen protection from forming acid, cross reaction, and organic synthesis.