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Objective

The Development of Mechanically & Electrically CNF & CNF Reinforced Composite Imran Syakir Mohamad. Objective. To develop high mechanically & electrically CNF and CNF reinforced composite using various substrates and catalysts. Scope.

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Objective

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  1. The Development of Mechanically & Electrically CNF & CNF Reinforced CompositeImranSyakirMohamad

  2. Objective • To develop high mechanically & electrically CNF and CNF reinforced composite using various substrates and catalysts

  3. Scope • To identify and evaluate several type of commercially available substrate • Inorganic-based (carbon cloth, fiberglass, silica, etc) • Plastic-based (polystyrene, nylon, polypropylene, etc) • To develop catalysts for carbon-growth process (cracking of carbon-carbon bond) • 3 monometallic catalysts • 2 bimetallic catalysts

  4. Scope • To develop methodology for grafting of catalyst onto the substrate • Identify suitable metal salt solution or metal • Condition of grafting for: • Deposition method (pH, temperature, concentration) • Sputtering method (radio frequency, time) • To grow nanocarbon onto the catalyst grafted substrate using a few technique • FCCVD • PECVD

  5. Scope • All samples will be characterized for their: • Compositional Analysis (EDX, XRF) • Morphology/Structure Analysis (FESEM, HRTEM) • Texture/Surface Area Analysis (BET) • Functionality (Raman, UV-Vis) • Mechanical & Electrical Properties Analysis

  6. Use as gases and ions transport media Applications • Energy storage • Have intrinsic properties. Can be used as an electrode in batteries & capacitor • Very high surface area • Good electrical conductivity • Their linear geometry makes their surface highly accessible to the electrolyte

  7. Air, Water and Gas Filtration these filters can not only block the smallest particles but also kill most bacteria Structural composite Good mechanical properties, such as stiffness, toughness, strength and lightweight. Possible to replace commercial fiber (e.g.Fiberglass) Applications COMMERCIAL AIR FILTRATION CARTRIDGE USING NANOFIBER FILTER MEDIA

  8. Challenges • Economic & reasonable cost, high production • Well homogeneous catalyst dispersion • Strong vertical align CNF attachment onto the substrate (inside the pore) • Enhance CNF properties (mechanical, electrical, thermal) • Control the CNF characteristic (diameter, length)

  9. Substrate Proposed: • Inorganic-based (Carbon Cloth) • Plastic-based (Polypropylene)

  10. Carbon Cloth as a Substrate • Reason • High microporosity • High surface area (>1000 m2/g) • Excellent adsorbent in gas & liquid media • Well establish/commercial • Narrow fiber diameter (10-20 micron) • Offer more catalytic property • Offer more adsorption ability

  11. Carbon Cloth • E-TEK CC Specifications • Weave = Plain • Weight = 116 g/m2 • Thickness = 0.35 mm • Size = 25 cm x 25 cm • Content = 99 % carbon, 1 % ash • Price = $43.75

  12. Fe Ni Co Catalyst Proposed (FCCVD) • 3 monometallic: Fe, Ni, Co • metallocene as a catalyst precursors • Ferrocene • Nickelocene • Cobaltocene • 2 bimetallic which are combination of two monometallic • Fe-Co • Ni-Fe

  13. Metallocene as Catalyst Precursor • Why choose metallocene? • Catalyst size – main important for CNF formation. • Nanosize cat. particles  catalyze CNF growth • Metallocene chosen because easy to vaporize at lower temp. (faster & simple process) • Vaporize metallocene molecule carried to reaction tube by H2 gas and C2H4. • Reduce by H2 to form Fe atom & deposite onto substrate.

  14. Catalyst Proposed (PECVD) • 3 monometallic: Fe, Ni, Co • Metal salt as a precursors • Iron nitrate, Fe • Nickel nitrate, Ni(NO3)2.6H2O • Cobalt nitrate, Co • 2 bimetallic which are combination of two monometallic • Fe-Co • Ni-Fe

  15. PECVD Technique Proposed • FCCVD • Floating Catalyst Chemical Vapor Deposition • Best for high productivity • High potential application in industry • PECVD • Plasma Enhanced Chemical Vapor Deposition • Best to synthesize vertical aligned CNF • Low temperature deposition

  16. Experimental Route (FCCVD) Substrate (CC) Washing (removes impurities; eg: Al, Si, Fe, K) Polymer (PP) • treat with HNO3, T=30oC, 24 hr • wash with deionized water (1L), dried T=200oC, 2 hr CNF Reinforced Treatment CNF After Treatment Catalyst Development Nanocarbon Growth • Use acid treatment (HCl) to remove catalyst & amorphous C. Characterization • Monometallic • Bimetallic • Carbon source (C2H4) • Carrier gas (H2 & N2) • Additive (Thiophene, H2S) • Compositional analysis (EDX,XRF) • Morphology/Structure analysis (SEM, HRTEM) • Texture/Surface Area analysis (BET) • Functionality (Raman) • Mechanical & Electrical Properties Analysis CNF

  17. Outlet Furnace Heating coil Catalyst Thiophene Mass flow meter Stainless steel tube Substrate H2 N2 C2H4 Setup (FCCVD) Schematic Diagram of a FCCVD system

  18. Growth Condition (FCCVD) To enhanced the catalytic activity Idea: Replace H2 with NH3. WHY? Catalyst deposition

  19. Aligned CNT was obtained in NH3 and N2 environment But why?

  20. Ni particles after pretreatment for 1h… Activated Nitrogen 300nm In pure NH3 300nm In H2+N2 Activated Nitrogen plays a significant role in vertically aligned CNT growth

  21. Role of activated nitrogen during CNT growth? Pretreatment Reaction

  22. Enhanced CNT growth in an NH3 environment is due to nitrogen incorporation into the CNT wall or cap. • Pretreatment in NH3 environment was neither a sufficient nor necessary for vertically aligned CNT growth • There are some relationship between nitrogen concentration in CNT and CNT growth rate • Nitrogen is chemically bonded with carbon atoms in graphite basal plane

  23. Experimental Route (PECVD) Substrate (CC) Washing (removes impurities; eg: Al, Si, Fe, K) • treat with HNO3, T=30oC, 24 hr • wash with deionized water (1L), dried T=200oC, 2 hr Polymer (PP) CNF Reinforced Treatment CNF After Treatment Catalyst Development Impregnation • Use acid treatment (HCl) to remove catalyst & amorphous C. • Cat. + deionized water + acetone • under ultrasonic, 30 min, 25oC (water bath) • aging 12 hr, 60oC • Monometallic • Bimetallic Characterization Nanocarbon Growth CNF • Compositional analysis (EDX,XRF) • Morphology/Structure analysis (SEM, HRTEM) • Texture/Surface Area analysis (BET) • Functionality (Raman) • Mechanical & Electrical Properties Analysis • Carbon source (C2H4) • Carrier gas (H2, N2, NH3)

  24. Setup (PECVD) Schematic Diagram of a PECVD system

  25. Growth Condition (PECVD) To enhanced the catalytic activity Vertical align CNF induce by plasma electric field

  26. CNF Reinforced Composite • Polymer (PP) blending process with CNF. • Enhanced the electrical and mechanical properties, light weight • Plastic itself is insulator. • Plastic is fragile when expose to high temp, sunlight. • Commercial fiber are heavy. CNF will reduce weight and cost efficiency (low fuel) if use in vehicle body part.

  27. PP • Polypropylene (polypropene) or (C3H6)n • Semi-rigid, good chemical resistance, tough, good fatigue resistance, good heat resistance, non toxic • Cheap • Density = 0.95 g/cm3 • Melting point = 173 oC • Chosen because PP is a linear polymer that can contribute to the development of highly aligned nanofiber system

  28. Blending Process Polypropylene CNF Melt Blend Spinning Process CNF Reinforced • Temp = 170-180oC • Speed Rotor = 30 rpm • Time = 5-10 min • Temp = 285oC • Speed Rotor= 600 rpm • Time = ?min

  29. Conclusion • CNF are expected to be produced with below criteria : • Vertically align • Strong attachment onto substrate • Improved mechanically & electrically properties • CNF-polymer reinforced composite are expected to be produced with below criteria: • Light weight • Good mechanical & electrical properties

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