WO2005120205A2 - Depot de reseaux nanotubulaires a transistor a temperature ambiante - Google Patents

Depot de reseaux nanotubulaires a transistor a temperature ambiante Download PDF

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Publication number
WO2005120205A2
WO2005120205A2 PCT/US2005/003821 US2005003821W WO2005120205A2 WO 2005120205 A2 WO2005120205 A2 WO 2005120205A2 US 2005003821 W US2005003821 W US 2005003821W WO 2005120205 A2 WO2005120205 A2 WO 2005120205A2
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WO
WIPO (PCT)
Prior art keywords
nanotubes
network
treated
solubilization
liquid
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PCT/US2005/003821
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English (en)
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WO2005120205A3 (fr
Inventor
George Gruner
J. Fraser Stoddart
Kelly S. Chichak
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The Regents Of The University Of California
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Publication of WO2005120205A2 publication Critical patent/WO2005120205A2/fr
Publication of WO2005120205A3 publication Critical patent/WO2005120205A3/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having potential barriers
    • H10K10/40—Organic transistors
    • H10K10/46—Field-effect transistors, e.g. organic thin-film transistors [OTFT]
    • H10K10/462—Insulated gate field-effect transistors [IGFETs]
    • H10K10/466—Lateral bottom-gate IGFETs comprising only a single gate
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/20—Carbon compounds, e.g. carbon nanotubes or fullerenes
    • H10K85/221—Carbon nanotubes

Definitions

  • the present invention relates generally to nanotube networks and the various methods that may be used to fabricate such networks. More particularly, the present invention is directed to nanotube networks that are suitable for use in electronic applications, such as transistors.
  • Mats of nanotubes (a dense set of nanotubes) have been fabricated before, such mats (often called bucky paper) have been used for exploration of the electrical characteristics of nanotubes or for sensors. Sensors with only a few (and ideally with a single) nanotube sensing elements have also been fabricated.
  • the CVD method requires high temperatures (typically 900°C). The high temperatures lead to difficulties in contact deposition. Problems also arise when using CVD for deposition in flexible electronics, such as a platform that involves plastic substrates. In addition there is a substantial cost associated with CVD-type manufacturing processes. At the same time, such CVD-type fabrication methods can be applied to a limited surface area, and therefore cannot support large area device arrays. [0007] There is a need for a deposition method that can be compatible with patterning methods, such as dip pen lithography and other printing techniques.
  • the present invention fulfills the above need by providing simple and efficient methods that are based on the solubilization of nanotubes to form a solution that may be used in solution deposition methods to form a wide variety of nanotube arrays.
  • the method of the present invention may be used to form networks of nanotubes on surfaces, such as those used in transistor devices.
  • a liquid is provided that includes nanotubes that have been treated with a solubilization agent. The liquid is deposited onto the surface to form a layer of the liquid. The solvent is removed to form a network layer of treated nanotubes. The solubilization agent is then removed to provide the final network of nanotubes.
  • the nanotube networks may be used as the conducting channel between the source electrode and the drain electrode of bottom-gated transistors, liquid-gated transistors and other electronic devices.
  • FIG. 1 is a schematic representation of an exemplary bottom gated transistor wherein the nanotube network that connects the drain electrode and the source electrode is made in accordance with the present invention.
  • FIG. 2 is a schematic representation of an exemplary transistor wherein the nanotube network that connects the drain electrode and the source electrode is made in accordance with the present invention and the gate electrode is applied through the liquid.
  • the geometry that can be fabricated by deposition methods in accordance with the present invention is fundamentally different, and allows device fabrication opportunities that mats do not possess.
  • the devices contain a random array of nanotubes, covering a relatively large surface area, with a specified nanotube density at the surface to provide desired transistor operation.
  • the geometry involves a large number of nanotubes, and therefore leads to statistical averaging.
  • Several requirements have to be obeyed by such network density: 1.
  • the network has to provide at least one conducting channel between the source and drain electrodes; and 2.
  • a specified nanotube density, must be chosen for full substrate coverage to be achieved.
  • the construction of networks using the solution method of the present invention has several advantages.
  • the main advantage is that it is fault tolerant: the destruction of one channel leaves other channels still open.
  • screening of the gate voltage by the conducting nanotubes is important, in a fashion similar to gate voltage screening due to a metal layer deposited on the device.
  • such screening is not important and the array can serve as the source-to-drain conducting channel.
  • the conductance of the off state (which can be reached by an application of a positive gate voltage) will be dominated by the conductance of the metallic tubes.
  • the present invention describes methods that can be used for low temperature (room temperature, but not above 100°C) deposition of nanotube (preferably carbon nanotube) networks with densities appropriate for a transistor operation both in air and in liquid environment.
  • An exemplary transistor for operation in air is shown schematically in FIG. 1.
  • the transistor is a conventional bottom-gated design that includes a source electrode 10, drain electrode 12, dielectric 14, gate 16 and a nanotube network 18 deposited using the method of the present invention.
  • An exemplary measurement arrangement for a liquid-gated transistor is shown schematically in FIG. 2.
  • the arrangement includes a non-conducting substrate 20, source electrode 22, drain electrode 24, a liquid 26 (such as a biological buffer), platinum electrode 28, reference electrode 30, a potentiostat 32 and a nanotube network 32 deposited using the method of the present invention.
  • the present invention provides for the deposition of treated nanotubes (nanotubes and solubilization agent) from solution onto pre-fabricated metal interconnects (electrodes) at room temperature (not above 100°C) followed by the removal of the solubilization agents at room temperature (not above 100°C).
  • the method involves the following steps: 1. Solubilization of treated nanotubes in an appropriate solvent to form a liquid.
  • the treated nanotubes are initially formed by adding an appropriate solubilization agent to the nanotubes; 2. Deposition of the liquid onto the desired surface; 3. Drying the solvent by any solvent removal method that leaves the nanotubes at the surface; and 4. Removing the solubilization agent.
  • the surface may be cleaned before and/or after deposition of the nanotube network in accordance with known cleaning techniques. Also, the device may be subjected to conditioning burn-in as is known.
  • the nanotubes that are treated with the solubilization agent can be pristine
  • nanotubes are modified by a chemical treatment, such as the attachment of a chemical
  • the functionalization agent may be added to the nanotube before, after or at the same time that the solubilization agent is added.
  • Exemplary functionalization agents include chemicals that donate electrons or holes, such as those listed as follows: 1. Organic compounds, such as: Tetracyanoquinodimathane (TCNQ) Tetracyanoethylene (TCNE) 2. Polymers with electron acceptor groups, such as: Polyethylene imine 3. Inorganic species, such as: bromine chlorine iodine thionyl chloride sulphur trioxide nitrogen dioxide nitrododium tetrafluoroborate; and nitronium tetrafluoroborate .
  • TCNQ Tetracyanoquinodimathane
  • TCNE Tetracyanoethylene
  • Inorganic species such as: bromine chlorine iodine thionyl chloride sulphur trioxide nitrogen dioxide nitrododium tetrafluoroborate; and nitronium tetrafluoroborate .
  • the nanotubes may also be functionalized with light absorbing functionalization agents, such as porphyrine.
  • light absorbing functionalization agents such as porphyrine.
  • carbon nanotubes were incubated in a solution that contains a light absorbing molecule porphyrine. After incubation the nanotube+porphyrine complex was deposited on a substrate and the response to light was measured. A weak response to light was observed for the pristine nanotubes. This effect has been observed before. Upon incubation with porphyrin, the response changes, which leads to a decrease of the resistance, which provides evidence for the effect of the porphyrin molecules leading to direct conversion of light into an electronic signal change. This observation demonstrates that: 1. the nanotube+porphyrine complex can be deposited jointly from the solution; and 2. the complex retained the functionality expected.
  • Non-covalent methods include side-wall and end-wall functionalizations with solvents, strong or weak acids, single molecules, surfactants and synthetic or biological polymers.
  • Covalent methods typically involve side-wall and end-wall modifications for the solubilization of SWNTs.
  • the covalent side- wall and end- wall modifications involve the addition of highly reactive organic, inorganic reagents, and synthetic or biological polymers to either defect sites or carboxylate functional groups present along or at the ends of SWNTs.
  • One non-covalent method involves the attachment of biological polymers as the solubilzation agent.
  • Biological polymers such as DNA, peptides, and starch, have been shown to effectively wrap helically around SWNTs which solubilizes them in aqueous solutions.
  • Exemplary synthetic polymer solubilization agents include: poly(m-phenylenevinylene-co-2,5-dioctoxy-p-phenylenevinylene) (PmPV), poly(para- phenylenevinylene) (PPV), polyphenylethylene (PPE), (polyphenylacetylene) PPA, NAFION, poly(N-vinylcarbazole) (PVK), Polyvinylpyrrolidone (PVP), poly(methylmethacrylate) (PMMA), poly(ethylmetacrylate) (PEMA), poly(vinylidene fluoride) (PVDF), poly(styrene-co-/>-(4-(4'-vinylpheny ⁇ )3-oxabutanoi) (PSV), poly(diallyldimethylammonium chloride) (PDMA), polyacrylonitrile (PAN) and derivatives of these polymers.
  • PmPV poly(m-phenyleneviny
  • Another non-covalent solubilization method involves the use of dynamic organic and inorganic polymers as the solubilization agent(s).
  • organic polymer solubilzation agents the potential exists to solubilize SWNTs by employing dynamic covalent polymers that closely resemble their covalent PmPV counterparts.
  • small building blocks can be designed to form oligomers and polymers through the reversible formation of imine bonds that should interact with the curved surfaces of SWNTs.
  • the polymeric product will interact with the SWNTs at different stages of its formation in such a way that these polymers can sense the polydispersity of lengths for the solubilized SWNTs.
  • SWNTs can be targeted for a range of organic and aqueous solutions by carefully tailoring the substituents on the periphery of each component. Again, the ability to render SWNTs soluble in almost any given solvent or water offers a larger range of deposition methods that can be used for device fabrication.
  • SWNTs With respect to inorganic polymer solubilization agents, the potential exists to solubilize SWNTs by employing dynamic reaction procedures that involve the formation of polymeric, discrete macrocyclic, and closed-shelled complexes constructed from organic ligands (pyridyl, carboxyl and transition metal complexes with or without counterions). These complexes can be functionalized in a manner to provide SWNT solubility in a range of organic and aqueous solutions.
  • organic ligands pyridyl, carboxyl and transition metal complexes with or without counterions
  • Another exemplary non-covalent solubilization method involves the attachment of surfactants, such as sodium dodecylsulfate (SDS), Triton-X and polyethylene glycol (PEG).
  • surfactants such as sodium dodecylsulfate (SDS), Triton-X and polyethylene glycol (PEG).
  • SDS sodium dodecylsulfate
  • PEG polyethylene glycol
  • SDS, Triton-X and PEGL have been shown to effectively solubilize SWNTs in aqueous solutions under mild temperatures by simple sonication.
  • the surfactants form uniform tubular micelles around individual and bundled SWNTs that can then be deposited onto any substrate in accordance with the present invention.
  • Another non-covalent method for solubilizing nanotubers in accordance with the present invention involves using solvents.
  • the use of a range of solvents and acids has been shown to effectively form stable suspensions of SWNTs under mild temperatures by simple sonication.
  • the solvent molecules form uniform solvent shells around individual and bundled SWNTs, which can then be deposited onto any substrate.
  • the solvent shells are very weakly bound and can be destroyed by changing pH, ionic strengths and temperatures, which can cause the precipitation of SWNTs from solutions.
  • solvents as the solubilzation agent, see the following references: (a) Zhang, M.; Yudasaka, M.; Koshio, A.; Iijima, S.
  • a covalent method for solubilizing nanotubes in accordance with the present invention involves the attachment of side-wall and end-wall functional groups.
  • the attachment of different small organic molecules, such as alkyl and aryl amines, alcohols cyclic and acyclic, and carbohydrates to the carboxylic end groups to form esters and amides has led to derivatives that are soluble in some organic solvents.
  • transition metal complexes may be attached to the nanotubes as the solubilization agent.
  • Reactive nitrenes, diazonium salts, azomethine ylides and carbenes have also been used for the direct side- wall modification of the SWNTs extended ⁇ framework which has led to their solubilization.
  • Another exemplary covalent method for solubilizing nanotubes in accordance with the present invention involves the use of side- wall / end- wall attached polymers.
  • the direct fluorination of the side-walls of SWNTs has been shown to effectively break apart bundles and ropes affording solubilities in a range of organic solvents.
  • Nanotube deposition from the liquid (solution) to the desired surface that has been conditioned and cleaned can occur in various ways. Examples of suitable deposition methods are as follows: direct deposition from the solution; spin -casting the solution; dip-pen deposition; and printing of the solution to a surface. [00040] These methods are well known in the literature and can be reproduced by artisans familiar with the art. For example, direct deposition involves the application of the solvent with the required nanotube density to a surface and subsequent drying of the deposited material.
  • Surface contours can be patterned on a surface using standard optical lithography. These contours can be decorated with molecules such that they are more hydrophilic or hydrophobic which will interact with the solubilizing agents so as to direct and control the deposition of SWNT solutions onto these surfaces.
  • spin-casting the method involves the use of a spin coater, a device well know in the literature. The rotating platform ensures the uniform distribution of the solution onto the surface. Drying and removal of the solubilization agent leads to the required nanotube network.
  • solutions of SWNTs can be deposited between patterned electrodes on a range of substrates by employing dip-pen lithography. This approach has been shown to be effective at depositing solutes in patterns with precision on the nanometer scale.
  • printing direct printing of the network from a solution to a desired surface is also possible, by using well-established screen printing technologies.
  • Lamination procedures may also be used where the nanotube network is deposited on the surface and then a second layer of parylene is deposited on top of the nanotube network. Portions of the second layer and the underlying nanotube network may then be removed by peeling off the second layer + nanotube network.
  • the solubilization agent is removed from the treated nanotubes once the liquid has been deposited, the network formed and the solvent removed.
  • the particular procedure for removing the solubilization agent will depend on the particular agent that is used.
  • biological polymer solubilization agents can be removed using purely biological methods where the polymer is degraded using enzymes which releases the SWNTs from their polymer coats in the device under biological conditions (standard pH, buffer, and temperatures).
  • the removal of synthetic polymer solubilization agents requires a suitable method that must (i) selectively break the carbon-carbon bonds of the polymer in order to release them from surface of SWNTs networks and (ii) avoid breaking the double-bond networks of SWNTs.
  • Methods may include the treatment with strong acids, strong bases, strong reducing agents, strong oxidizing agents, and ozonolysis.
  • the SWNTs' dynamic organic polymer coat can be removed by treating with mild acids which hydrolyze the imine bonds and cleaves the polymer back down into to its original starting components. Any of the components that remain on the substrate can be removed by washing with a suitable solvent.
  • the surfactants form micelles reversibly and can be destroyed by changing pH and temperature which can cause the precipitation of SWNTs from solutions.
  • These surfactant molecules can be removed after deposition by washing with any organic, inorganic, and/or aqueous solutions containing buffers, acids and bases.
  • the weakly bound solvent shells can be destroyed by changing pH, ionic strength, and temperatures which can cause the precipitation of SWNTs from solutions.
  • These solvent molecules can be removed after deposition by washing with any organic, inorganic, and/or aqueous solutions containing buffers, acids and bases. Residual solvent molecules can be removed after deposition by placing the device in a low-pressure vacuum chamber under relatively mild temperatures.
  • the removal of small molecule solubilzation agents that are covalently attached to the side-walls and end-walls of the nanotubes can be achieved by high- temperature heating. If the agents are attached as esters or amides these solubilizing agents can be removed using strong acids or bases and hydrogenation. If the solubilizing agents are biological molecules they can be removed by treatment with an appropriate enzyme.
  • the removal of polymer solubilization agents covalently attached to the side- walls and end-walls can be achieved by high-temperature heating. If the agents are attached as esters or amides these solubilizing agents can be removed using strong acids or bases and hydrogenation. If the solubilizing agents are biological polymers they can be removed by treatment with an appropriate enzyme.
  • An example of the deposition of a nanotube network in accordance with the present invention using the surfactant sodium doceylbenzenesulfonate (NaDDBS) as the solubilization agent is as follows:
  • Si substrates on which the liquid was to be deposited were treated with an H2O2:H2SO4 (1:4) solution at 100 °C for 20 minutes, so that the Si surface is hydrophilic.
  • the Si substrates were put into a vacuum container with a few drops of silanes inside for 2-10 hours. This silane treatment is preferred because it allows the tubes with surfactant to stick onto the substrates.
  • the liquid containing the treated carbon nanotubes was then deposited onto the substrate. After 5 minute's incubation at room temperature °C, methanol was dropped onto the substrate to drive away the water and leave the carbon nanotube network on the substrates.
  • the bundles of nanotubes that make up the network have less than about 10 nanotubes per bundle and in some cases have even less than 5 nanotubes per bundle.
  • the deposited network of treated nanotubes was then rinsed with isopropyl alcohol (IP A) in order to remove the solubilization agent and then blown to dry with nitrogen or air.
  • IP A isopropyl alcohol

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  • Nanotechnology (AREA)
  • Manufacturing & Machinery (AREA)
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Abstract

Un procédé de formation de réseaux de nanotubes sur une surface. Un liquide comprend des nanotubes ayant été traités par un agent de solubilisation. Le liquide est déposé sur une surface afin de former une couche de liquide. Le solvant est retiré afin de former une couche de réseau des nanotubes traités. L'agent de solubilisation est ensuite retiré afin d'obtenir le réseau final de nanotubes. Les réseaux de nanotubes peuvent être formés sous forme de supports conducteurs (18) entre l'électrode source (10) et l'électrode drain (12) d'un transistor à grille inférieure et d'autres dispositifs électroniques.
PCT/US2005/003821 2004-02-13 2005-02-07 Depot de reseaux nanotubulaires a transistor a temperature ambiante WO2005120205A2 (fr)

Applications Claiming Priority (2)

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US54484104P 2004-02-13 2004-02-13
US60/544,841 2004-02-13

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WO2005120205A2 true WO2005120205A2 (fr) 2005-12-22
WO2005120205A3 WO2005120205A3 (fr) 2006-07-20

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1751332A2 (fr) * 2004-06-03 2007-02-14 Nantero, Inc. Procede de fabrication d'un liquide applicateur pour processus de fabrication de dispositifs electroniques
DE102006027880A1 (de) * 2006-06-09 2007-12-13 Leibniz-Institut Für Festkörper- Und Werkstoffforschung Dresden E.V. Isolationsschichtmaterial für die Mikroelektronik
WO2013184222A3 (fr) * 2012-03-23 2014-01-30 Massachusetts Institute Of Technology Capteur d'éthylène
JP2017158484A (ja) * 2016-03-09 2017-09-14 国立大学法人名古屋大学 ナノワイヤデバイス、該ナノワイヤデバイスを含む分析装置、サンプルの加熱処理方法及びサンプルの分離方法

Citations (1)

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Publication number Priority date Publication date Assignee Title
US20020122765A1 (en) * 2001-03-02 2002-09-05 Fuji Xerox Co., Ltd. Carbon nanotube structures and method for manufacturing the same

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
US20020122765A1 (en) * 2001-03-02 2002-09-05 Fuji Xerox Co., Ltd. Carbon nanotube structures and method for manufacturing the same

Non-Patent Citations (2)

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Title
BACHTOLD A. ET AL.: 'Logic Circuits with Carbon Nanotube Transistors' SCIENCE vol. 294, November 2001, pages 1317 - 1320, XP001157485 *
STAR A. ET AL.: 'Noncovalent Side-Wall Functionalization of Single-Walled Carbon Nanotubes' MACROMOLECULAR vol. 36, 2003, pages 553 - 560, XP002997490 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1751332A2 (fr) * 2004-06-03 2007-02-14 Nantero, Inc. Procede de fabrication d'un liquide applicateur pour processus de fabrication de dispositifs electroniques
EP1751332A4 (fr) * 2004-06-03 2010-06-23 Nantero Inc Procede de fabrication d'un liquide applicateur pour processus de fabrication de dispositifs electroniques
DE102006027880A1 (de) * 2006-06-09 2007-12-13 Leibniz-Institut Für Festkörper- Und Werkstoffforschung Dresden E.V. Isolationsschichtmaterial für die Mikroelektronik
DE102006027880B4 (de) * 2006-06-09 2008-11-27 Advanced Micro Devices, Inc., Sunnyvale Verwendung von Kohlenstoffnanoröhren als Isolationsschichtmaterial für die Mikroelektronik
WO2013184222A3 (fr) * 2012-03-23 2014-01-30 Massachusetts Institute Of Technology Capteur d'éthylène
CN104412100A (zh) * 2012-03-23 2015-03-11 麻省理工学院 乙烯传感器
US9739737B2 (en) 2012-03-23 2017-08-22 Massachusetts Institute Of Technology Ethylene sensor
JP2017158484A (ja) * 2016-03-09 2017-09-14 国立大学法人名古屋大学 ナノワイヤデバイス、該ナノワイヤデバイスを含む分析装置、サンプルの加熱処理方法及びサンプルの分離方法
WO2017154614A1 (fr) * 2016-03-09 2017-09-14 国立大学法人名古屋大学 Dispositif à nanofil, appareil d'analyse comprenant le dispositif à nanofil, procédé de traitement à chaud d'échantillon et procédé de séparation d'échantillon

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