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UNIVERSITY OF PETROLEUM & ENERGY STUDIES 
Dehradun 
The Synthesis of Fe-Co MCM-41 Catalyst for the preparation of 
Carbon nanotubes by Catalytic Chemical Vapor Deposition 
MINOR PROJECT 
B.Tech MSNT(2012-16) 
5th - SEM 
Submitted By: Guided By: 
Anish Verma (007) G.Gopalakrishnan 
Shah Faisal (42) 
Vishal Jain (52) 
Mohammad Abubakar (59)
Chapter outline of the Project 
Introduction 
Problem Statement 
Objective 
Flowchart 
Methodology 
MCM-41 
Procedure 
Synthesis 
Conclusion 
References
Introduction/Background: 
Carbon nanotubes (CNTs) are allotropes of carbon with 
a cylindrical nanostructure. Nanotubes have been constructed with 
length-to-diameter ratio of up to 132,000,000:1.Current applications 
include Tips for atomic force microscope probes. In tissue engineering, 
carbon nanotubes can act as scaffolding for bone growth. 
CNT and hetro atom substituted CNT having potential application for 
Hydrogen storage devices. Search for efficient H-Storage devices is 
necessitated by the risk involved in transportation of hydrogen which is 
regarded as potential future auto fuels. 
Hence, efficient method of CNT & hetro atom substituted CNT is being 
sought. One of the method for CNT synthesis is by catalytic CVD 
(Chemical vapour deposition) and so effective efficient catalyst become 
important area for research. Hence it is proposed to synthesis Fe-Co 
substituted MCM-41 & characterized them for its application & catalyst for 
CNT synthesis by CVD.
Problem statement: 
The serious problems that are affecting the development of hydrogen 
cars are; hydrogen storage, the high reactivity of hydrogen, the cost 
and methods of hydrogen fuel production, consumer demand and the 
cost of changing the infrastructure to accommodate hydrogen 
vehicles. 
The concerns surrounding the storage of hydrogen are a major issue. 
Hydrogen must be stored at extremely low temperatures and high 
pressure. A container capable of withstanding these specifications is 
larger than a standard gas tank. Hydrogen storage could be viewed 
as a problem by consumers. Hydrogen is extremely reactive. 
Hydrogen is combustible and flammable. 
So in order to solve the above stated problem we are making Fe-Co 
substituted MCM-41 catalyst to synthesis CNT hetro atoms 
substituted CNT which have the potential to be used for hydrogen 
storage.
Objectives: 
• Develop high-capacity hydrogen storage material to meet 
the demand for a hydrogen Storage system. 
• To enhance the preparation of CNT’s produced by 
Catalytic CVD using the MCM-41 Catalyst. 
• Hydrogen capacity greater than 6 wt. % 
• Favourable thermodynamic and kinetics suitable for 
transportation applications. 
• Stable with hydrating/dehydrating cycling.
FLOWCHART OF THE PROJECT 
Literature Gathering 
Data collection and reading Time-3 months 
Catalyst Synthesis 
Catalyst Analysis 
Characterization and Verification 
of properites 
Time-3-4 months 
Chemical preperation and 
synthesis 
Time-4-5 months
Methodology 
MCM-41 
Mobil Composition of Matter (MCM) is the initial name given for a 
series of mesoporous materials that were first synthesized by Mobil's 
researchers in 1992. MCM-41 (Mobil Composition of Matter No. 41) 
and MCM-48 (Mobil Composition of Matter No. 48) are two of the most 
popular mesoporous molecular sieves that are keenly studied by 
researchers. 
The most striking fact about the MCM-41 and MCM-48 is that, 
although composed of amorphous silica wall, they possess long range 
ordered framework with uniform mesopores. These materials also 
possess large surface area, which can be up to more than 1000 m2g−1. 
Moreover, the pore diameter of these materials can be nicely 
controlled within mesoporous range between 1.5 to 20 nm by adjusting 
the synthesis conditions and/or by employing surfactants with different 
chain lengths in their preparation.
HYDROTHERMAL SYNTHESIS 
•Hydrothermal synthesis includes the various techniques of 
crystallizing substances from high-temperature aqueous 
solutions at high vapor pressures; also termed "hydrothermal 
method. 
•Hydrothermal synthesis can be defined as a method of synthesis 
of single crystals that depends on the solubility of minerals in hot 
water under high pressure.
PROCEDURE 
Synthesis of Fe-MCM-41 
Materials Required 
Fe-MCM-41 molecular sieve is to be synthesised 
hydrothermally using a gel composition of – 
1SiO2:0.01 Fe2O3:0.2 CTAB: 0.89 H2SO4. 
Sodium metasilicate, ferric nitrate and cetyl trimethyl 
ammonium bromide(CTAB) are to be used as the sources 
of silicon, iron and structure-directing agent, respectively.
Synthesis of catalyst 
In a typical synthesis, 21.2g of sodium metasilicate is added with ferric 
nitrate and dissolved in distilled water. The pH of the solution is adjusted to 
10.5 using 1M sulphuric acid and the content was stirred well to form a gel. 
An aqueous solution of CTAB was prepared by dissolving 7.2 g of it in 
distilled water and it is added slowly to the gel for a period of about 30 min. 
The resulting mixture is then stirred for 1 hrs. at room temperature and 
autoclaved at 145oC for 48 hr. The crystallized Fe-MCM-41 is recovered by 
filtration, washed several times with distilled water and dried at 80oC for 3 
Hr.The occluded surfactant was removed by calcination at 550oC in muffle 
furnace for 6 hrs. to obtain Fe-MCM-41. 
Synthesis of Fe-MCM-41 and Co-MCM-41 
Co-MCM-41 is synthesised by adopting the above procedure in which 
cobaltous nitrate is used as the source for cobalt and ferric nitrate for Fe 
(ratio 1:1).
CONCLUSION 
The synthesis of the Fe-Co-MCM-41 
catalyst for the catalytic CVD synthesis 
of CNT’s will be carried out 
successfully.
REFERENCES 
1. Silaghi, M.-C., Chizallet, C., Raybaud, P.; Challenges on molecular aspects of 
dealumination and desilication of zeolites, Microporous and Mesoporous Materials, 
191 (2014) 82-96. 
2. Laudise, R.A. (1958). R.H. Doremus, B.W. Roberts and D. Turnbull, ed. Growth and 
perfection of crystals. Proceedings of an International Conference on Crystal Growth 
held at Cooperstown, New York on August 27–29, 1958. Wiley, New York. pp. 458– 
463. 
3. "Chronological reference marks - Charles Chamberland (1851–1908)". Pasteur 
Institute.Archived from the original on 19 December 2006. Retrieved 2007-01-19. 
4. Hugo WB (July 1991). "A brief history of heat and chemical preservation and 
disinfection".J. Appl. Bacteriol. 71 (1): 9–18. doi:10.1111/j.1365- 
2672.1991.tb04657.x. PMID 1894581. 
5. Bulletin - United States Geological Survey, Issues 47-54, 1889, pp. 180 (834) 
6. Electric Muffle Furnace, C.A. Crowley, Popular Mechanics, 67:6, June 1937, pp. 941- 
945 
7. J.S. Beck, et al.,J. Am. Chem. Soc. 114 (1992) 10834. 
8. T. Somanathan, A. Pandurangan, et. al. A:Chem.256 (2006) 193.
fe-MCM-41 Catalyst for CNT synthesis

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fe-MCM-41 Catalyst for CNT synthesis

  • 1. UNIVERSITY OF PETROLEUM & ENERGY STUDIES Dehradun The Synthesis of Fe-Co MCM-41 Catalyst for the preparation of Carbon nanotubes by Catalytic Chemical Vapor Deposition MINOR PROJECT B.Tech MSNT(2012-16) 5th - SEM Submitted By: Guided By: Anish Verma (007) G.Gopalakrishnan Shah Faisal (42) Vishal Jain (52) Mohammad Abubakar (59)
  • 2. Chapter outline of the Project Introduction Problem Statement Objective Flowchart Methodology MCM-41 Procedure Synthesis Conclusion References
  • 3. Introduction/Background: Carbon nanotubes (CNTs) are allotropes of carbon with a cylindrical nanostructure. Nanotubes have been constructed with length-to-diameter ratio of up to 132,000,000:1.Current applications include Tips for atomic force microscope probes. In tissue engineering, carbon nanotubes can act as scaffolding for bone growth. CNT and hetro atom substituted CNT having potential application for Hydrogen storage devices. Search for efficient H-Storage devices is necessitated by the risk involved in transportation of hydrogen which is regarded as potential future auto fuels. Hence, efficient method of CNT & hetro atom substituted CNT is being sought. One of the method for CNT synthesis is by catalytic CVD (Chemical vapour deposition) and so effective efficient catalyst become important area for research. Hence it is proposed to synthesis Fe-Co substituted MCM-41 & characterized them for its application & catalyst for CNT synthesis by CVD.
  • 4. Problem statement: The serious problems that are affecting the development of hydrogen cars are; hydrogen storage, the high reactivity of hydrogen, the cost and methods of hydrogen fuel production, consumer demand and the cost of changing the infrastructure to accommodate hydrogen vehicles. The concerns surrounding the storage of hydrogen are a major issue. Hydrogen must be stored at extremely low temperatures and high pressure. A container capable of withstanding these specifications is larger than a standard gas tank. Hydrogen storage could be viewed as a problem by consumers. Hydrogen is extremely reactive. Hydrogen is combustible and flammable. So in order to solve the above stated problem we are making Fe-Co substituted MCM-41 catalyst to synthesis CNT hetro atoms substituted CNT which have the potential to be used for hydrogen storage.
  • 5. Objectives: • Develop high-capacity hydrogen storage material to meet the demand for a hydrogen Storage system. • To enhance the preparation of CNT’s produced by Catalytic CVD using the MCM-41 Catalyst. • Hydrogen capacity greater than 6 wt. % • Favourable thermodynamic and kinetics suitable for transportation applications. • Stable with hydrating/dehydrating cycling.
  • 6. FLOWCHART OF THE PROJECT Literature Gathering Data collection and reading Time-3 months Catalyst Synthesis Catalyst Analysis Characterization and Verification of properites Time-3-4 months Chemical preperation and synthesis Time-4-5 months
  • 7. Methodology MCM-41 Mobil Composition of Matter (MCM) is the initial name given for a series of mesoporous materials that were first synthesized by Mobil's researchers in 1992. MCM-41 (Mobil Composition of Matter No. 41) and MCM-48 (Mobil Composition of Matter No. 48) are two of the most popular mesoporous molecular sieves that are keenly studied by researchers. The most striking fact about the MCM-41 and MCM-48 is that, although composed of amorphous silica wall, they possess long range ordered framework with uniform mesopores. These materials also possess large surface area, which can be up to more than 1000 m2g−1. Moreover, the pore diameter of these materials can be nicely controlled within mesoporous range between 1.5 to 20 nm by adjusting the synthesis conditions and/or by employing surfactants with different chain lengths in their preparation.
  • 8. HYDROTHERMAL SYNTHESIS •Hydrothermal synthesis includes the various techniques of crystallizing substances from high-temperature aqueous solutions at high vapor pressures; also termed "hydrothermal method. •Hydrothermal synthesis can be defined as a method of synthesis of single crystals that depends on the solubility of minerals in hot water under high pressure.
  • 9. PROCEDURE Synthesis of Fe-MCM-41 Materials Required Fe-MCM-41 molecular sieve is to be synthesised hydrothermally using a gel composition of – 1SiO2:0.01 Fe2O3:0.2 CTAB: 0.89 H2SO4. Sodium metasilicate, ferric nitrate and cetyl trimethyl ammonium bromide(CTAB) are to be used as the sources of silicon, iron and structure-directing agent, respectively.
  • 10. Synthesis of catalyst In a typical synthesis, 21.2g of sodium metasilicate is added with ferric nitrate and dissolved in distilled water. The pH of the solution is adjusted to 10.5 using 1M sulphuric acid and the content was stirred well to form a gel. An aqueous solution of CTAB was prepared by dissolving 7.2 g of it in distilled water and it is added slowly to the gel for a period of about 30 min. The resulting mixture is then stirred for 1 hrs. at room temperature and autoclaved at 145oC for 48 hr. The crystallized Fe-MCM-41 is recovered by filtration, washed several times with distilled water and dried at 80oC for 3 Hr.The occluded surfactant was removed by calcination at 550oC in muffle furnace for 6 hrs. to obtain Fe-MCM-41. Synthesis of Fe-MCM-41 and Co-MCM-41 Co-MCM-41 is synthesised by adopting the above procedure in which cobaltous nitrate is used as the source for cobalt and ferric nitrate for Fe (ratio 1:1).
  • 11. CONCLUSION The synthesis of the Fe-Co-MCM-41 catalyst for the catalytic CVD synthesis of CNT’s will be carried out successfully.
  • 12. REFERENCES 1. Silaghi, M.-C., Chizallet, C., Raybaud, P.; Challenges on molecular aspects of dealumination and desilication of zeolites, Microporous and Mesoporous Materials, 191 (2014) 82-96. 2. Laudise, R.A. (1958). R.H. Doremus, B.W. Roberts and D. Turnbull, ed. Growth and perfection of crystals. Proceedings of an International Conference on Crystal Growth held at Cooperstown, New York on August 27–29, 1958. Wiley, New York. pp. 458– 463. 3. "Chronological reference marks - Charles Chamberland (1851–1908)". Pasteur Institute.Archived from the original on 19 December 2006. Retrieved 2007-01-19. 4. Hugo WB (July 1991). "A brief history of heat and chemical preservation and disinfection".J. Appl. Bacteriol. 71 (1): 9–18. doi:10.1111/j.1365- 2672.1991.tb04657.x. PMID 1894581. 5. Bulletin - United States Geological Survey, Issues 47-54, 1889, pp. 180 (834) 6. Electric Muffle Furnace, C.A. Crowley, Popular Mechanics, 67:6, June 1937, pp. 941- 945 7. J.S. Beck, et al.,J. Am. Chem. Soc. 114 (1992) 10834. 8. T. Somanathan, A. Pandurangan, et. al. A:Chem.256 (2006) 193.