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WO2015034469A2 - Procédé de nettoyage de nanotubes de carbone et autres films nanostructurés - Google Patents

Procédé de nettoyage de nanotubes de carbone et autres films nanostructurés Download PDF

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Publication number
WO2015034469A2
WO2015034469A2 PCT/US2013/057872 US2013057872W WO2015034469A2 WO 2015034469 A2 WO2015034469 A2 WO 2015034469A2 US 2013057872 W US2013057872 W US 2013057872W WO 2015034469 A2 WO2015034469 A2 WO 2015034469A2
Authority
WO
WIPO (PCT)
Prior art keywords
carbon
acetic acid
carbon nanostructure
surfactants
surfactant
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US2013/057872
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English (en)
Other versions
WO2015034469A3 (fr
Inventor
Huaping Li
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ANEEVE NANOTECHNOLOGIES LLC
Original Assignee
ANEEVE NANOTECHNOLOGIES LLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by ANEEVE NANOTECHNOLOGIES LLC filed Critical ANEEVE NANOTECHNOLOGIES LLC
Priority to PCT/US2013/057872 priority Critical patent/WO2015034469A2/fr
Publication of WO2015034469A2 publication Critical patent/WO2015034469A2/fr
Publication of WO2015034469A3 publication Critical patent/WO2015034469A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/168—After-treatment
    • C01B32/17—Purification

Definitions

  • the field of the present invention is the cleaning of carbon nanostructure films used within devices such as transistors and transparent conductive films.
  • SWCNTs Pristine single-walled carbon nanotubes
  • SWCNTs Pristine single-walled carbon nanotubes
  • the common method is to use de-ionic water to clean up these dispersing agents from SWCNT surfaces on substrates either immobilized with amino groups or not.
  • Other methods can be used to clean dispersing agents from SWCNTs, including oxidization reaction and thermal burning.
  • these cleaning methods produce inconsistent results and don't remove all the dispersing agents from the SWCNT surfaces. Consequently, the end result of using the above cleaning methods often shows up as uncontrollable SWCNTs density and rough carbon nanotube surface that are indicative of chemical wrapping.
  • Density gradient ultracentrifuge (DGU) separated semi-conducting and metallic SWCNTs are wrapped with sodium cholate helices and dispersed with SDS, which exhibiting excellent water solubility. These separated semiconducting and metallic SWCNTs aqueous solutions are facilely ink-inject printed on silicon wafer and plastic substrates to form nice white films. Directly washing these films using de-ionic water, no single SWNTs can be imaged with scanning electron microscope (SEM). With aminopropyltris (ethoxy) silane (APTES) modified silicon-wafer and plastic surfaces, SWCNT films are obtained by inserting these substrates in SWCNT solutions for a long period (over 10 hours). Their atom force microscopy images show rough SWCNT surfaces, indicating the incomplete removal of chemicals.
  • SEM scanning electron microscope
  • the present invention is directed to a cleaning process for removal of surfactant chemicals from carbon nanostructures.
  • the process includes washing with a carboxylic acid selected from the group consisting of acetic acid, propanoic acid and butanoic acid. Glacial acetic acid has been found of specific utility.
  • the cleaning process may also be considered in carbon nanostructure film preparation with deposition of carbon nanostructures in solution with surfactant chemicals before washing.
  • surfactants include sodium cholate (SC) and sodium dodecyl sulfate (SDS).
  • Carbon nanostructure material deposition on a substrate may be by ink-jet printing, gravure roll-to-roll printing, screen and mask printing or various other printing methods. Accordingly, it is an object of the present invention to provide an improved wash process for carbon nanostructures. Other and further objects and advantages will appear hereafter.
  • FIG. 1 AFM image (scale: 2 ⁇ ⁇ 2 ⁇ ) illustrates printed
  • FIG. 2 AFM image (scale: 2 ⁇ ⁇ 2 ⁇ ) illustrates printed SWCNTs on a silicon wafer after being washed with glacial acetic acid showing clean SWCNT surfaces.
  • CNT and other similar carbon materials and structures are here collectively referred to as carbon nanostructures.
  • Embodiments of a cleaning process for films of such carbon nanostructures such as various CNT and other similar materials and structures such as nanoparticles, nanowires and monolayer materials from_solutions with surfactants are here disclosed that:
  • This cleaning process removes surfactant chemicals from carbon naonostructures.
  • the process includes washing the carbon nanostructures with a carboxylic acid selected from the group consisting of acetic acid, propanoic acid and butanoic acid. This process is applicable to any kind of carbon nanostructure.
  • the embodiments described employ glacial acetic acid but the group is contemplated for use.
  • glacial acetic acid neutralizes surfactants (i.e. sodium cholate and SDS) to form corresponding acids that are immediately immiscible with acetic acid leading then to a breakdown of the neutralizes surfactants (i.e. sodium cholate helices and SDS micelles).
  • surfactants i.e. sodium cholate and SDS
  • the carbon components then form networks under the influence of gravitational forces and van de Waals interactions.
  • This kinetic process may also be distinguished from a simple carbon nanostructure film wash using de-ionic water where surfactants slowly diffuse into the aqueous solution determined by their thermodynamic equilibrium. In such a slow thermodynamic process, there is a high probability that carbon components also diffuse with the surfactants into the aqueous solution resulting in reduced carbon component density.
  • the acetic acid wash has the advantageous results of increasing carbon nanostructure based transistor performance and increasing carbon nanostructure film optical transmissivity.
  • One embodiment of the process for fabricating a carbon nanostructure film ready for incorporation into electronic, optical and mechanical devices includes:
  • PEI polyethylamine
  • LiCIO 4 lithium perchlorate
  • a carbon nanostructure film typically employs chemical functionalization or surfactant dispersion of carbon nanostructure components.
  • Surfactants are used such as sodium dodecylsulfonate (SDS) and sodium cholate (SC).
  • SDS sodium dodecylsulfonate
  • SC sodium cholate
  • the surfactant dispersion is handled as ink and the film is deposited using printing techniques.
  • Application is to a substrate such as a silicon wafer.
  • a semiconducting SWCNT solution inkjet printed on a silicon wafer was conventionally washed.
  • the apparent diameters 10 of the CNT in Figure 1 are seen to be large and non-uniform, reflecting the presence of surfactant on the CNT.
  • the printed semiconducting SWCNT film illustrated in Figure 2 was washed in glacial acetic acid. This image is bright and clear with smaller diameters 12 in comparison to those in Figure 1 , indicating an absence of surfactant on the CNT.
  • Figure 2 also shows smooth SWCNT surfaces, sharply contrasting with the periodic bamboo structures observed in Figure 1. These images reflect that glacial acetic acid removes surfactants around the surface of SWCNTs compared to a conventional wash treatment.
  • TFT Thin film transistors
  • SWCNTs Thin film transistors
  • Silver nanoparticles were printed to form transistor electrodes and the cleaned SWNCTs made up the transistor's semiconducting channel.
  • the TFT backgated electric characteristics show mobility of 1.16 and an on/off ratio of 1000.
  • Top gating these devices with polyethylamine (PEI)/lithium perchlorate (LiCIO 4 ) ionic gel further enhanced the TFT device performance attributes.
  • PEI polyethylamine
  • LiCIO 4 lithium perchlorate

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

Cette invention concerne un procédé de nettoyage d'une nanostructure de carbone et autres matériaux et structures similaires destiné à éliminer des produits chimiques de type tensioactif. Le procédé comprend le lavage des nanostructures de carbone avec un acide acétique concentré qui peut être un acide acétique glacial. Le procédé de nettoyage selon l'invention est également envisagé dans la préparation des films à nanostructures de carbone avec dépôt des nanostructures de carbone en solution avec des produits chimiques de type tensioactif avant lavage. Les tensioactifs possibles comprennent le cholate de sodium (SC) et le dodécylsulfate de sodium (SDS). Le dépôt des nanostructures de carbone sur un substrat peut s'opérer par divers procédés d'impression.
PCT/US2013/057872 2013-09-03 2013-09-03 Procédé de nettoyage de nanotubes de carbone et autres films nanostructurés Ceased WO2015034469A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/US2013/057872 WO2015034469A2 (fr) 2013-09-03 2013-09-03 Procédé de nettoyage de nanotubes de carbone et autres films nanostructurés

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/US2013/057872 WO2015034469A2 (fr) 2013-09-03 2013-09-03 Procédé de nettoyage de nanotubes de carbone et autres films nanostructurés

Publications (2)

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WO2015034469A2 true WO2015034469A2 (fr) 2015-03-12
WO2015034469A3 WO2015034469A3 (fr) 2015-07-16

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
RU2743559C1 (ru) * 2019-12-31 2021-02-19 федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный технический университет имени Н.Э. Баумана (национальный исследовательский университет)" (МГТУ им. Н.Э. Баумана) Способ удаления остаточного растворителя из слоёв на основе углеродных нанотрубок

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US5695900A (en) * 1995-12-21 1997-12-09 Colorado School Of Mines Surface treatment of magnetic particles for use in reprographic processes
US20040126900A1 (en) * 2001-04-13 2004-07-01 Barry Stephen E High affinity peptide- containing nanoparticles
CN100419426C (zh) * 2002-04-22 2008-09-17 佛罗里达州立大学 功能化纳米微粒及其使用方法
JP2006513557A (ja) * 2002-05-21 2006-04-20 エイコス・インコーポレーテッド カーボンナノチューブ被覆物をパターン化する方法およびカーボンナノチューブ配線
US20040150312A1 (en) * 2002-11-26 2004-08-05 Mcelrath Kenneth O. Carbon nanotube particulate electron emitters
WO2005056474A1 (fr) * 2003-12-09 2005-06-23 Carbon Nanotechnologies, Inc. Procede pour purifier des nanotubes de carbone realises sur des supports d'oxyde refractaire
US8703092B2 (en) * 2005-09-15 2014-04-22 University Of Florida Research Foundation, Inc. Type separation of single-walled carbon nanotubes via two-phase liquid extraction
KR101748894B1 (ko) * 2009-08-14 2017-06-19 나노-씨, 인크. 제거가능한 첨가제를 지닌 용매계 및 수계 탄소 나노튜브 잉크
KR101172861B1 (ko) * 2010-02-26 2012-08-09 삼성전기주식회사 금속 나노입자의 세정방법
WO2011119995A2 (fr) * 2010-03-26 2011-09-29 Cerulean Pharma Inc. Formulations et procédés d'utilisation
US9490486B2 (en) * 2012-01-05 2016-11-08 Brookhaven Science Associates, Llc Method for removing strongly adsorbed surfactants and capping agents from metal to facilitate their catalytic applications

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2743559C1 (ru) * 2019-12-31 2021-02-19 федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный технический университет имени Н.Э. Баумана (национальный исследовательский университет)" (МГТУ им. Н.Э. Баумана) Способ удаления остаточного растворителя из слоёв на основе углеродных нанотрубок

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