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Process for purifying semiconducting single-walled carbon nanotubes

A single-wall carbon nanotube, semiconductor technology, applied in carbon nanotubes, nanotechnology for materials and surface science, chemical instruments and methods, etc., can solve the problems of high cost, lack of scalability, etc., to achieve The effect of increasing yield, increasing purity, and high yield

Active Publication Date: 2016-05-25
NAT RES COUNCIL OF CANADA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Current enrichment methods are limited by a combination of issues such as lack of scalability (DGU), prohibitive cost (chromatography), yield / efficiency, and device performance (selective polymer extraction)

Method used

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  • Process for purifying semiconducting single-walled carbon nanotubes
  • Process for purifying semiconducting single-walled carbon nanotubes
  • Process for purifying semiconducting single-walled carbon nanotubes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1: polyfluorene derivative

[0046] This example provides details of preferred conjugated polymers.

[0047] Prepared by the Suzuki reaction (Suzuki reaction) adapted from prior art methods (eg Ding2002) 8 to C 18 Polyfluorene with two alkyl groups of length. The obtained polymers with basic characterization data are listed in Scheme 1 and Table 1, where T d 1％ and T g is measured by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) curves.

[0048]

[0049] Scheme 1: Structure of polyfluorene

[0050] Table 1: Characterization data of polyfluorene

[0051] polymer

Embodiment 2

[0052] Example 2: Enrichment of original SWCNTs with polyfluorene derivatives

[0053] This example provides details of extraction of mixtures of sc-SWCNTs and m-SWCNTs using conjugated polymers to generate enriched sc-SWCNT dispersions.

[0054] A typical enrichment was performed by dispersing 25 mg of laser ablation-generated SWCNTs together with 20 mg of polyfluorene into 50 mL of toluene. The mixture was homogenized at 30° C. for 30 minutes using a horn sonicator with a 10 mm tip (Branson Sonicator 250, maximum power: 200 W) operated at 40% duty cycle and 50% output. The dispersion was then centrifuged at a relative centrifugal force (RCF) of 7600 g (8,000 rpm on a SS-34 rotor) for 30 minutes. Pass the supernatant through Teflon with 0.2 μm pore size TM Membrane filtration to collect the extracted SWCNTs. The collected SWCNTs were rinsed twice with 5 mL of toluene to remove free polyfluorene, and then redispersed in 5 mL of toluene for 5 to 10 min using a bath sonicator...

Embodiment 3

[0072] Example 3: Using an inorganic adsorption medium to improve the purity of large-diameter sc-SWCNTs enriched with polyfluorene derivatives

[0073] This example provides details of exposing the enriched sc-SWCNT dispersion from Example 1 to an inorganic adsorption medium in a non-polar solvent to further increase the purity of the sc-SWCNTs. The inorganic adsorption medium used in this example was unmodified silica gel and composed of various functional groups, namely 3-cyanopropyltriethoxysilane (CPTES), 3-aminopropyltriethoxysilane (APTES ) and 0.1% poly-L-lysine modified silica gel. Silica gel (Macherey-Nagel company, Pore ​​size) was purchased from Rose Scientific Co., Ltd. 3-cyanopropyltriethoxysilane (CPTES), 3-aminopropyltriethoxysilane (APTES) and 0.1% poly-L-lysine aqueous solution were obtained from Sigma-Aldrich (Sigma-Aldrich) obtained and used as is.

[0074] Preparation of silica gel and surface-modified silica gel

[0075] Macherey-Nagel silica gel wi...

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Abstract

A two-step sc-SWCNT enrichment process involves a first step based on selective dispersion and extraction of semiconducting SWCNT using conjugated polymer followed by a second step based on an adsorptive process in which the product of the first step is exposed to an inorganic absorptive medium to selectively bind predominantly metallic SWCNTs such that what remains dispersed in solution is further enriched in semiconducting SWCNTs. The process is easily scalable for large-diameter semi- conducting single-walled carbon nanotube (sc-SWCNT) enrichment with average diameters in a range, for example, of about 0.6 to 2.2 nm. The first step produces an enriched sc-SWCNT dispersion with a moderated sc-purity (98%) at a high yield, or a high purity (99% and up) at a low yield. The second step can not only enhance the purity of the polymer enriched sc-SWCNTs with a moderate purity, but also further promote the highly purified sample to an ultra-pure level. Therefore, this two-step hybrid process provides sc-SWCNT materials with a super high purity, as well as both a high sc-purity (for example greater than 99%) and a high yield (up to about 20% or higher).

Description

[0001] Cross References to Related Applications [0002] This application claims the benefit of US Patent Provisional Patent Application USSN 61 / 867,630 filed August 20, 2013, which is hereby incorporated by reference in its entirety. technical field [0003] This application relates to carbon nanotubes. Background technique [0004] An important class of carbon nanotubes are single walled carbon nanotubes (SWCNTs). They are generally produced as bulk samples containing both metallic and semiconducting nanotubes with a chirality distribution centered on the average diameter. Various methods can be used to produce SWCNTs that will differ in chiral distribution, diameter range, semiconductor / metal (sc / m) content, and average length. For example, HiPcoSWCNTs and CoMoCatSWCNTs have relatively smaller diameters (0.6nm-1.3nm), while arc-discharge SWCNTs, laser (laser ablation) SWCNTs, and plasmonic SWCNTs have relatively larger diameters (1.0nm-2.2nm) . Although sc-SWCNT conte...

Claims

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Application Information

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IPC IPC(8): B01D11/00B82Y30/00
CPCB01D11/0257B01D11/0265B82Y30/00B82Y40/00B01D11/0288B01D21/262C01B32/159C01B32/166C01B32/172C01B32/174
Inventor 丁建夫P·马朗方李兆J·莱夫布尔程福永B·西马德
Owner NAT RES COUNCIL OF CANADA
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