A Novel Method for Carbon Nanotube Production and the Mechanisms Involved
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1 A Novel Method for Carbon Nanotube Production and the Mechanisms Involved Xinfeng Xie 1 Barry Goodell 1, Yuhui Qian 1, Geoffrey Daniel 2, Jody Jellison 3 1 Wood Science and Technology, University of Maine, Orono, USA 2 Wood Ultrastructure Research Centre, Swedish University of Agricultural Sciences, Uppsala, Sweden 3 Biological Sciences, University of Maine, Orono, USA
2 Outline Introduction Objectives Materials and Methods Results and Discussion Conclusions
3 Mechanical Properties of CNTs Compared with Other Materials Material Introduction cont. Carbon nanotubes (CNTs) are highly sought-after materials due to their exceptional physical, mechanical, and electronic properties. Young's Modulus (GPa) Tensile Strength (GPa) Density (g/cm 3 ) SWNTs MWNTs Steel Wood Scientists have designed a Space Elevator for travel from earth to the moon using CNTs as the construction materials. [httpwww.flickr.comphotosflyingsinger ]
4 Introduction cont. Last year, we reported a method to produce carbon nanotubes (CNTs) directly from plant materials using a cyclic oxidation process. Oxidative carbonization of raw materials at 240 C in air; Cyclic oxidation of the pretreated materials at 400 C.
5 Introduction cont. Nano channel Tubular structure 40 nm During the first two cycles, formation of nanochannels was observed in the material. The diameters of these channels fell within the range of the cross sectional dimensions of the cellulose microfibrils in the plant cell wall Structures observed after two cycles at 400 C using Bamboo as the raw material.
6 Introduction cont. 560nm x 16nm After 35 cycles, single carbon nanotubes (CNTs) and CNT bundles were observed in samples. These CNTs are nm in diameter and nm long. CNTs from wood fiber after 35 cycles of oxidation at 400 C.
7 Introduction cont. Experimental setup with a new sliding devise and computer control system
8 Introduction cont. Based on these results, we proposed that the formation of CNTs in the process occurred via template synthesis, with the nanochannels formed from the ablation of cellulose microfibrils functioning as a template.
9 Introduction cont. Proposed Mechanism Channel formed by ablation of microfibril carbon Carbon Vaporization Cellulose Microfibril Lignin hemicellulose matrix Low Temperature Partial Carbonization Carbon from the microfibril Carbon from lignin hemicelulose matrix Multicyclic process under oxidative conditions Carbon redeposition, rearrangement using the nanopore left by microfibril ablation as the template
10 Objectives The key point in the proposed mechanism is the differential ablation properties of the carbons derived from cellulose and matrix. Therefore the objectives of this study were to: Examine the property differences between cellulose carbon and lignin carbon formed under identical experimental conditions Determine how the carbonization temperature affects the properties of these two types of carbon
11 Materials and Methods Filter paper & Isolated lignin Heat at 240 C in air for about 8 hours Carbonization in Argon at 400 C, 500 C, 700 C and 1000 C for about 8 hours. Oxidative behaviors in air were studied using TGA (thermogravimetric analysis). Chemical compositions were monitored using FTIR Specific surface area was tested using nitrogen adsorption at 77 K
12 Materials and Methods cont. In order to better understand the oxidative behaviors of the two types of carbons in this study, apparent kinetic parameters were determined using the relationship between mass loss rate and temperature using the Friedman equation: dα E ln( ) = nln(1 α ) + dt RT ln A (1) DTG Curve TG Curve where α is the fraction of carbon ablated at time t; n is the order of reaction; A is the frequency factor (min -1 ); R is the gas constant (8.314 J K -1 mol -1 ); T is the absolute temperature (K), and E is the activation energy (kj mol -1 ). n ln( 1 α ) dα ln( ) dt = E RT ln A (2) Slope
13 TGA Results and Discussion Derivative Mass (%/min) C C Temper at ur e ( C) Cel l ul ose Car bon Li gni n Car bon DTG profiles for oxidation of 400 C cellulose carbon and lignin carbon in air. Considerable difference in oxidative mass change was observed when comparing cellulose carbon and lignin carbon prepared at 400 C and 500 C. (only 400 C shown)
14 Results and Discussion cont. TGA 700 C Derivative Mass ( %/ mi n ) Temper at ur e ( C) Cellulose Carbon Li gni n Car bon DTG profiles for oxidation of 700 C cellulose carbon and lignin carbon in air The difference in oxidative mass change between the two types of carbons decreased markedly in the 700 C and 1000 C samples. (700 C shown).
15 Results and Discussion cont. TGA Apparent kinetic parameters for samples prepared at different temperatures Cellulose Carbon Lignin Carbon Process Temperature n E (kj mol -1 ) n E (kj mol -1 ) 400 C C C C The difference in oxidative behaviors between these two types of carbon was primarily due to the difference in the order of reaction. Higher n values indicated higher reactivity of the materials.
16 Results and Discussion cont. Specific surface area Process Temperature Specific surface area and porosity for samples prepared at different temperatures Total Pore Langmuir BET Volume (cm 3 g -1 ) Surface Area (m 2 g -1 ) Surface Area (m 2 g -1 ) Cellulose Lignin Cellulose Lignin Cellulose Lignin 400 C C C C From the perspective of pore structure and specific surface area, cellulose carbon promotes oxidative reactions more readily than lignin carbon because cellulose carbon has greater pore volume and a larger surface area.
17 Results and Discussion cont. FTIR 1225 C-O 1430 CH C=C (Ar) 1723 C=O Carbonized at 1000 C Carbonized at 700 C Carbonized at 500 C Carbonized at 400 C -OH Oxidized at 240 C Untreated Wavenumber ( cm-1) Infrared spectrum (absorption) of cellulose carbon
18 Results and Discussion cont. FTIR Carbonized at 1000 C Carbonized at 700 C Carbonized at 500 C Carbonized at 400 C Oxidized at 240 C Untreated Wavenumber ( cm- 1) Infrared spectrum (absorption) of lignin carbon
19 Results and Discussion cont. FTIR Comparing the FTIR profiles of cellulose carbon and lignin carbon, we found that: At carbonization temperatures lower than 500 C, cellulose carbon had far more paraffinic structures than lignin carbon; When carbonization temperatures increased to 700 C or greater, the two types of carbon possessed a similar degree of carbonization with respect to their chemical structures; These results are consistent with those of the TGA study and they support the concept that oxidative mass loss in these two types of carbons is dictated primarily by their chemical structures.
20 Results and Discussion cont. CNTs in Damascus Swords [ The Damascus swords of the Middle East were legendarily sharp, strong and flexible. These Damascus blades were extraordinarily strong, but still flexible enough to bend from hilt to tip. And they were reputedly so sharp that they could cleave a silk scarf floating to the ground, just as readily as a knight s body. [
21 Results and Discussion cont. CNTs in Damascus Swords Cementite (iron carbide) CNT Thermal cycling forging and annealing may lead to the growth of carbon nanotubes (CNTs), which in turn initiate formation of cementite nanowires. Remnant of cementite nanowires encapsulated by carbon nanotubes. (Reibold et al. 2006)
22 Conclusions Oxidation of cellulose carbon and lignin carbon prepared at low temperatures (<500 C) follows different kinetic models, with cellulose carbon having a higher reaction order. The mass loss behaviors of these two types of carbon are dictated primarily by their chemical structures. The findings in this study support our earlier hypotheses on mechanisms for the production of carbon nanotubes in lignocellulose materials through the ablation of cellulose microfibrils within the lignin matrix of intact plant/wood cell walls at low carbonization temperatures. This research has significance related to the discovery of plant fiber-derived carbon nanotubes, formed at low carbonization temperatures, that have previously been identified in other materials such as Damascus steel.
23 Acknowledgements Prof. Dannis Nagle Dr. Dajie Zhang Advanced Technology Laboratory (ATL) at Johns Hopkins University
24 THANK YOU!
25 Yi el d ( %) Temper at ur e ( C) Cellulose Li gni n
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