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Research Proposal: Synthesis of Nano-Particles Using Carbon Dioxide (CO2)

Maxwell Tommie Lajawai*, Fathia Farhana Agusalim

Department of Chemical Engineering, Faculty of Engineering, University of Malaya, 50603

Kuala Lumpur

*Corresponding Author. Tel: +6012-8351319

Email address:

1.0 Introduction

The rapid increase of anthropogenic carbon dioxide nowadays has become a major concern

since it contributes towards global warming. Many efforts have been made in order to

mitigate the increase of carbon dioxide emission to the atmosphere from all point and non-

point sources. One of the best initiatives that can reduce this greenhouse gas is by converting

CO2 into nano-particles. Scientifically, nano-particles can be described as very tiny objects

where the sizes are between 100 and 2500 nanometers for the fine particles; ultrafine particles

are of sizes between 1 and 100 nanometers. These nano-particles have numerous applications

especially in the semi-conductor and electrical industries, and are known for their great

durability and strength, thermal conductivity, electrical conductivity as well as exhibiting

lightweight properties.

There are many ways that can be done for the synthesization of nanoparticles. However, the

only method that will be used for this research study is by the chemical vapour deposition

(CVD) method. The CVD method has been approved as the most promising method to

produce high quality of nano-materials at relatively low cost. The other advantage of using

this method is because of its high product yield. This method involves by putting the gas-

phase, carbon-rich source flowing in the presence of a metal catalyst at elevated operating

temperature in the range between 550 and 1000°C, towards decomposing the gaseous carbon

molecules, and subsequently converted into carbon nano-particles. This particular method

also can be conducted by using different types of chemical reactors with different carbon


For the characterization of nano-particles, there are three common microscopes that are used

to study their morphologies and microstructures, which are Transmission Electron

Microscopy (TEM), Scanning Electron Microscopy (SEM) and Field Emission Electron

Microscopy (FESEM). These microscopes have the same principles with the light

microscope; the only difference between them is that electrons are used instead of light in

obtaining the images.

As for this project, the experiment will be conducted either by using a fixed bed reactor with

quartz wool or autoclave (this is however, subject to approval to procure), both iron and

cobalt (and possibly nickel) will be used for the catalyst preparation and the carbon sources

are carbon dioxide and methane. The reason carbon dioxide has been chosen as the main

source is because of its cheapness, availability and toxic-less.

2.0 Project Objectives

The objectives of this study are:

(i) To develop different carbon free catalyst for CO2 / CH4 reactions.

(ii) To convert CO2 into useful nanoparticles using other developed catalysts and coal/

biomass as well.

3.0 Methodology

The methodology of this experiment can be divided into three parts:

a) Catalyst Preparation

b) Synthesis of nano-particles

c) Characterization of nano-particles: morphology and microstructure

Two different types of reactors (equipments) will be used to conduct the experiment:

(I) Fixed bed reactor with quartz wool

(II) Autoclave (subject to approval)

a) Catalyst Preparation

The catalyst will be prepared by using precipitation (co-precipitation) method with

iron (Fe) and cobalt (Co) as the metallic materials. Firstly, a certain amount of Fe and

Co (approximately 0.5g) are dissolved in the distilled water and ammonia is added

into the mixed solution at atmospheric condition (atmospheric temperature and

pressure). The mixture is then left for 2 hours. Next, filtration will take place by

washing the mixture with distilled water. The solids from the filter are dried at high

temperature (110oC) for 12 hours and calcined at 450oC for 3 hours in air.

b) Production of nano-particles

i) Vertical Fixed bed reactor with quartz (tube diameter ~ 40mm)

The catalyst that has been prepared will be inserted directly into the preheated

zone of a furnace at 560oC where it is ignited and spontaneously burned. Then,

CO2 and N2 (possibly H2 also) with space velocity of 750cm3/min and

1500cm3/min respectively are then flown into the furnace. The temperature of

the sample is heated at different heating rates from room temperature to 800oC

(i.e 30, 50, 80, 100, 200,300… 800oC/min). After 45 minutes, the sample is

cooled to room temperature with air flown through it.

For the purification process, the products are added with nitric acid (HNO3)

for 2 hours at room temperature. The products are filtered and washed with

distilled water and dried at 100oC.

ii) Stainless steel autoclave (10ml)

The reaction is occurred in supercritical CO2 with a purity of 99.9%.

Approximately 8g of dry ice with catalyst that had been prepared previously is

added into the autoclave. Similar to the fixed bed reactor, the sample is

measured by using thermocouple and heated at different heating rates from

room temperature to 450oC (i.e. 50, 100, 200, 250…450oC/min). The main

products are identified (nano-particles or nanotubes produced) after 10 hours

of reaction time from the reaction between CO2 and Fe/Co. Next, the reaction

products are removed by nitric acid (HNO3) or hydrochloric acid (HCl). The

solid precipitate is finally weighed.

As for both the fixed bed reactor and autoclave, the experiment is repeated by

performing different isothermal times e.g. 1, 2, 3, 6 hours. In addition, to ensure the

stability of the nano-particles, similar experiments are performed but now with

relatively high temperatures while the heating rate and flow rates of the gases are kept

constant. Different gas flows are also conducted by injecting methane (CH4) gas into

the reactor to compare the quality of the production of nano-particles. The reaction of

CO2 with CH4 is done with mole ratio of 1:1. The experiment is conducted using

coal/biomass as well. During the experiment, the weight change of the samples, time

and temperature are also recorded simultaneously for all the experiments.

c) Characterization of nano-particles: morphology and microstructure

The samples will be analysed for BET surface areas as well as SEM, TEM or FESEM

analyses. The morphology and microstructures (i.e. shapes, sizes, and elemental

distributions) of the nano-particles produced are studied so that the best quality and

method of synthesization of nano-particles which using different parameters of studies

can be determined. For the reaction of CO2/CH4, the kinetics are calculated so as to

compare the results and the best way to produce nano-particles is selected.

4.0 Project Schedule
Semester I
Jul 2010 Aug 2010 Sep 2010 Oct 2010 Nov 2010 Dec 2010
ID Task Name Start Finish Duration
18/7 25/7 1/8 8/8 15/8 22/8 29/8 5/9 12/9 19/9 26/9 3/10 10/10 17/10 24/10 31/10 7/11 14/11 21/11 28/11 5/12 12/12 19/12

Briefing on Research Project by

1 16/7/2010 16/7/2010 1d

2 Literature review findings 19/7/2010 15/10/2010 65d

Finding companies that sell autoclave

3 20/8/2010 1/10/2010 31d
(experimental setup)

4 Talk on Design of Experiments 27/8/2010 27/8/2010 1d

Talk on how to write research proposal

5 1/10/2010 1/10/2010 1d
and review article
Meeting with BuchiGlass Company
6 25/10/2010 25/10/2010 1d
about the autoclave

7 Progress Evaluation (VIVA) 28/10/2010 28/10/2010 1d

8 Workshop on using Turnitin Software 1/11/2010 1/11/2010 1d

Finding companies that can modify the

9 8/11/2010 17/12/2010 30d
fixed bed reactor in pilot plant
Writing on research proposal and
10 8/11/2010 12/11/2010 5d
review paper
Submission of Review Paper and
11 19/11/2010 19/11/2010 1d
Research Proposal

Semester II

Dec 2010 Jan 2011 Feb 2011 Mar 2011 Apr 2011 May 2011
ID Task Name Start Finish Duration
5/12 12/12 19/12 26/12 2/1 9/1 16/1 23/1 30/1 6/2 13/2 20/2 27/2 6/3 13/3 20/3 27/3 3/4 10/4 17/4 24/4 1/5 8/5 15/5 22/5

Designing the experimental setup of

1 20/12/2010 22/12/2010 3d
fixed bed reactor
Starting the 1st experiment by
2 preparing the catalyst by co- 23/12/2010 27/12/2010 3d
precipitation method
Laboratory work by using fixed bed
3 28/12/2010 10/1/2011 10d
Analysis of data on production of
4 11/1/2011 18/1/2011 6d
Repeating the experiment by using
5 19/1/2011 25/2/2011 28d
different types of catalyst (or reactor)
Data analysis, calculations (chemical
6 28/2/2011 28/3/2011 21d

7 Writing the final report and article 30/3/2011 12/4/2011 10d

8 Submission of final report and article 15/4/2011 15/4/2011 1d

9 Poster presentation 18/5/2011 18/5/2011 1d