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WO2025188534A1 - Analyseur d'ions à base de nanotubes de carbone - Google Patents

Analyseur d'ions à base de nanotubes de carbone

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Publication number
WO2025188534A1
WO2025188534A1 PCT/US2025/017531 US2025017531W WO2025188534A1 WO 2025188534 A1 WO2025188534 A1 WO 2025188534A1 US 2025017531 W US2025017531 W US 2025017531W WO 2025188534 A1 WO2025188534 A1 WO 2025188534A1
Authority
WO
WIPO (PCT)
Prior art keywords
detector
nanotube
analyzer according
molecule
molecules
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.)
Pending
Application number
PCT/US2025/017531
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English (en)
Other versions
WO2025188534A8 (fr
Inventor
Tillmann Kubis
Christina Ferreira
Namita NARENDRA
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.)
Purdue Research Foundation
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Purdue Research Foundation
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Publication of WO2025188534A1 publication Critical patent/WO2025188534A1/fr
Publication of WO2025188534A8 publication Critical patent/WO2025188534A8/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/403—Cells and electrode assemblies
    • G01N27/414—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS
    • G01N27/4146—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS involving nanosized elements, e.g. nanotubes, nanowires
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors

Definitions

  • This disclosure relates to the field of atom and molecule analyzers. More particularly, this disclosure relates to systems and methods for universal analyzers, for example using carbon nanotubes.
  • Mass spectrometry has become an important method in analytical chemistry due to its high molecular specificity in combination with very wide applicability, speed, sensitivity and quantitative capability.
  • mass spectrometry has typically been large bench-top instruments, found only in laboratories, incapable of use for point-of-care needs. That limitation has led to attempts to develop much smaller (miniature) mass spectrometers that can be operated outside the laboratory.
  • Comparative examples of MS devices are challenging to scale down to small sizes. For example, comparative MS devices must operate in vacuum to maintain a low collision rate while ions pass through the MS device.
  • CNTs carbon nanotubes
  • a molecule analyzer includes a molecule detector comprising a first carbon nanotube (CNT) field effect transistor (FET) configured to receive the molecules from a molecule source and separate the molecules based on their mass.
  • CNT carbon nanotube
  • FET field effect transistor
  • a molecule analyzer comprises a first molecule detector configured to receive molecules from a molecule source and to measure a first time at which the molecule passes through the first molecule detector; a beam lensing device configured to receive the ions from the first ion detector and to measure a velocity of the ions; a second ion detector configured to receive the ions from the beam lensing device and to measure a second time at which the ions pass through the second ion detector; an accelerator lensing device configured to receive the ions from the second ion detector and to measure a mass of the ions; and a third ion detector configured to receive the ions from the accelerator lensing device and to measure a third time at which the ions pass through the third ion detector.
  • FIG. 1 illustrates an example of a carbon nanotube transistor in accordance with various aspects of the present disclosure.
  • FIG. 2A illustrates an example of a carbon nanotube transistor with a molecule or ion therein, in accordance with various aspects of the present disclosure.
  • FIG. 2B illustrates example current characteristics of the carbon nanotube transistor of FIG. 2 A.
  • FIG. 3 illustrates an example of a simulation setup in accordance with various aspects of the present disclosure.
  • FIG. 4 illustrates an example of simulation results in accordance with various aspects of the present disclosure.
  • FIG. 5 illustrates an example of an analysis system in accordance with various aspects of the present disclosure.
  • FIG. 6 illustrates an example of a charged carbon nanotube in accordance with various aspects of the present disclosure.
  • FIG. 7 illustrates an example of a mass spectrometer in accordance with various aspects of the present disclosure.
  • FIG. 8 illustrates an example of current-voltage characteristics for a transistor in accordance with various aspects of the present disclosure.
  • FIG. 9 illustrates an example of current-position characteristics for a transistor in accordance with various aspects of the present disclosure.
  • FIG. 10 illustrates an example of a linear accelerator in accordance with various aspects of the present disclosure.
  • FIG. 11 illustrates an example of a helical nanotube in accordance with various aspects of the present disclosure.
  • FIG. 12 illustrates an example of a particle detector in accordance with various aspects of the present disclosure.
  • FIG. 13 illustrates an example of a shutter device in accordance with various aspects of the present disclosure.
  • FIG. 14 illustrates an example of a detector configuration in accordance with various aspects of the present disclosure.
  • FIG. 15 illustrates an example of a detector configuration in accordance with various aspects of the present disclosure.
  • FIG. 16 illustrates an example of a geometrical catalyst in accordance with various aspects of the present disclosure.
  • FIG. 17 illustrates an example of a manufacturing method in accordance with various aspects of the present disclosure.
  • FIG. 18 illustrates an example of a transistor in accordance with various aspects of the present disclosure.
  • FIG. 19 illustrates an example of a manufacturing method in accordance with various aspects of the present disclosure.
  • FIG. 20 illustrates an example of a manufacturing method in accordance with various aspects of the present disclosure.
  • top As used herein, unless otherwise limited or defined, discussion of particular directions is provided by example only, with regard to particular embodiments or relevant illustrations. For example, discussion of “top,” “front,” or “back” features is generally intended as a description only of the orientation of such features relative to a reference frame of a particular example or illustration. Correspondingly, for example, a “top” feature may sometimes be disposed below a “bottom” feature (and so on), in some arrangements or embodiments. Further, references to particular rotational or other movements (e.g., counterclockwise rotation) is generally intended as a description only of movement relative a reference frame of a particular example of illustration.
  • discussion of “horizontal” or “vertical” features may in some implementations be relative to the earth’s surface; however, in other implementations a mass spectrometer may be installed in a different orientation such that a “horizontal” feature is not necessarily parallel to the earth’s surface.
  • horizontal or “longitudinal” may refer to the extending direction of spectrometer core components (i.e., of a carbon nanotube), whereas “vertical” or “radial” may refer to a direction perpendicular to horizontal.
  • the term “or” as used herein is intended to indicate exclusive alternatives only when preceded by terms of exclusivity, such as, e.g., “either,” “one of,” “only one of,” or “exactly one of.” Further, a list preceded by “one or more” (and variations thereon) and including “or” to separate listed elements indicates options of one or more of any or all of the listed elements.
  • the phrases “one or more of A, B, or C” and “at least one of A, B, or C” indicate options of: one or more A; one or more B; one or more C; one or more A and one or more B; one or more B and one or more C; one or more A and one or more C; and one or more of each of A, B, and C.
  • a list preceded by “a plurality of’ (and variations thereon) and including “or” to separate listed elements indicates options of multiple instances of any or all of the listed elements.
  • the phrases “a plurality of A, B, or C” and “two or more of A, B, or C” indicate options of: A and B; B and C; A and C; and A, B, and C.
  • spectroscopic instruments such as MS devices, detector devices, shutter devices, catalyst devices, and the like are challenging to scale down to small sizes.
  • comparative MS devices must operate in vacuum to maintain a low collision rate while ions pass through the MS device.
  • the present disclosure provides for MS devices based on CNT transistors.
  • the systems, methods, and devices according to the present disclosure provide several advantages associated with scaling down the size of a MS device, including but not limited to increased portability; the possibility of real-time mass analysis as a benchtop lab device or outside of a lab setting for real-world applications; the elimination of the need for vacuum, which could enable mass analysis of target molecules in a solvated state; the ability to detect neutral molecules with a strong dipole moment in addition to ionized molecules; and the like.
  • the present disclosure sets forth a time-of-flight (TOF) nanoscale MS device based on CNTs. The CNT confines the motion of the ions to within the CNT inner space.
  • TOF time-of-flight
  • Sections of the CNTs host field-effect transistor (FET) structures that act as nanoscale charge amplifiers.
  • a change in current of each FET is measured whenever a charge molecule/ion (or molecule having a strong dipole moment) is present in the gate region of the FET.
  • transistor architectures e.g., a sheathed CNT transistor
  • present disclosure describes examples of implementing certain transistor architectures (e.g., a sheathed CNT transistor)
  • the present disclosure is not so limited.
  • the systems, metrics, methods, etc. described herein may be applied using other transistor architectures, including top-gated CNT transistors, bottom-gated CNT transistors, suspended CNT transistors, wrapped-gate CNT transistors, and so on.
  • Other nanotube types can serve as molecule detectors as well, such as boron nitride nanotubes, gallium nitride nanotubes, silicon nanotubes, titanium nanotubes, and other non-carbon nanotubes.
  • a system or device is described below as having a “CNT,” it should be understood that such system or device may alternatively have another NT type, such as boron nitride NTs, gallium nitride NTs, silicon NTs, titanium NTs, and the like, as set forth above.
  • the systems, methods, and devices of the present disclosure may be used in any application where MS is used.
  • the systems, methods, and devices of the present disclosure may be used in food safety applications, ergot detection, substance detection, chemical detection, and the like. These may be applied to the analysis of gases, liquids, or solids.
  • the system, methods and devices of the present disclosure may be used in non-MS related applications.
  • the presence of ions and molecules in a nanotube effectively changes the electrostatics of the nanotube which can be used to tune the electrostatic, electrodynamic, optical, thermal, and mechanical response of the nanotube.
  • Moving ions and molecules in the nanotube by e.g. electric fields, trapping the ions or molecules by gates etc. allow for detailed control of the electrostatic, electrodynamic, optical, thermal, and mechanical response of the nanotube by gate fields.
  • the system, methods and devices of the present disclosure may be used to control the motion of molecules and ions in nanotubes. This allows to filter or trap specific ions and molecules, or to move specific molecules and ions close to each other to force them into bonding configurations. [0039]
  • the system, methods and devices of the present disclosure may be used to determine the detailed geometry of the ions and molecules, since molecules of similar mass but different geometry (aka chirality) cause different electrostatic response in the nanotube sensors and FETs effectively allowing to distinguish between geometrical factors of molecules, such as chirality, folding, protein structure, etc.
  • the system, methods and devices of the present disclosure may be used to convert the kinetic energy of ions or molecules into electric energy of the electrons in the enclosing nanotubes and their contacts, effectively creating a nano-generator.
  • the ions and molecules can be accelerated by the fields in the enclosing nanotubes, effectively creating a nano-engine or nano-pump.
  • the system, methods and devices of the present disclosure may be used to correlate ions and molecules in neighboring nanotubes to entangle the quantum phases of the molecules or ions or of the electrons in the enclosing nanotubes.
  • a plurality of neighboring nanotubes can host a plurality of such defined quantum bits for quantum information processing.
  • CNTs may be used as nanodevices. When used in nanotransistors (e.g., CNTFETs), CNTs show strong control of electron flow by gate fields.
  • FIG. 1 illustrates one example of a CNTFET. View (a) illustrates a perspective schematic view of the example CNTFET, whereas view (b) is a microscopy image of the electrodes of the example CNTFET. View (c) illustrates a graph showing current vs. gate voltage for the example CNTFET.
  • Transistors act as charge-signal amplifiers. For example, a comparatively small (e g., ⁇ 60 mV) change on the gate voltage results in a tenfold change in the source/drain currents.
  • CNTs are ultrasensitive given their small number of atoms (or low electron count).
  • An ion or molecule in the center of the CNT has a high impact on electron transport (e.g., can enable transport through the gate).
  • the ions or molecules within the CNT propagate on a ID transport path. Collisions thus have a much smaller phase space compared to the same ion in a 3D space.
  • the CNTFETs of the present disclosure leverage this relationship by using the CNTFET setup to sense single ions or molecules under atmospheric pressure.
  • FIGS. 2A and 2B illustrate this relationship.
  • FIG. 2A shows an example cross-section of a CNTFET, in which Contact 1 and Contact2 respectively refer to the source and drain electrodes, or vice versa depending on whether the CNTFET is p-type or n-type.
  • FIG. 2B shows the current spike.
  • FIG. 3 illustrates the simulation setup
  • FIG. 4 illustrates the simulation results.
  • the source-drain current increases as the ion/molecule gets closer to the gate, and decreases when the ion/molecule gets beyond the gate.
  • FIG. 5 illustrates one example of a MS device in accordance with the present disclosure.
  • FIG. 5 illustrates an ion source (or molecule source) 502 which produces ions (or molecules) 504 for analysis.
  • Particles from the ion or molecule source 502 pass through a first set of beam lenses 506 in the form of a charged CNT (see FIG. 6), having a length on the order of 10 pm.
  • a charged CNT By using a charged CNT, once the molecule/ion is in the CNT, it will stay along the center line.
  • the particles enter the ion/molecule detector 508 which is implemented as a CNTFET that will be described in more detail below.
  • the CNTFET has a length on the order of 100 nm or smaller.
  • the CNTFET may separate the particles depending on mass.
  • the particles under interrogation pass through a second set of beam lenses 510, also in the form of a charged CNT having a length on the order of 10 pm. Finally, the remaining particles are detected by a detector 512.
  • FIG. 7 illustrates one example of a possible CNTFET design for the ion/molecule detector in accordance with the present disclosure.
  • FIG. 7 is a schematic of a CNTFET mass spectrometer with two adjacent CNTFETs that share a drain, such that the drain (D) of the first CNTFET is also the drain of the second CNTFET.
  • the current between the source (S) and drain (D) of each FET is controlled by the respective gate (G).
  • G gate
  • an ion/molecule illustrated as a dashed circle
  • the change in time between the current spike corresponding to when the ion/molecule passes the first gate and the current spike corresponding to when the ion/molecule passes the second gate is proportional to the mass.
  • the sensitivity of the CNT allows it to act as a charge sensor.
  • FIG. 8 shows the IV characteristics of the CNTFET for different magnitude charges placed at a distance x along the CNTFET.
  • the high sensitivity of a small fractional charge makes the device sensitive to neutral molecules with a small dipole moment along the molecule’s structural extension. Fully charged ions will have a charge that is 100x larger or more, which will show significantly larger IV-characteristic changes.
  • FIG. 9 illustrates the source-drain current as a function of the incompletely ionized molecule’s position along the CNTFET transport direction.
  • the source-drain current increases as the ion/molecule approaches the gate region by an order of magnitude, moreover, CNTs of different chirality may show different sensitivity relative to the ion’s motion.
  • the ion/molecule detector of FIG. 5 may have a length that is determined by the minimum length of the CNT, which in turn is determined by the minimum time difference needed between two successive target ion’s/molecule’s arrival time at the gate region to successfully resolve their individual masses.
  • the minimum length Lmin may be given by the following Equation (1): where q is the magnitude of the charge, V is the voltage applied along the CNT FET, Tdock is the clock frequency period, and M2 and Mi are the masses of the two successive ions to be resolved. Assuming a clock frequency of 5 GHz, a voltage of IV and an ion charge of 1 elementary charge. Clock frequencies up to 100* higher may be possible depending on the equipment chosen.
  • the CNTFET minimum length is shown in Table 1.
  • the mean free path of gas molecules in ambient air is approximately 70 nm. Given the above dimension estimates of CNTs, and given that CNTs restrict the motion of gas molecules to ID in their cavity which increases the mean free path between collisions, ambient pressure mass spectrometry is possible with CNTFETs.
  • FIG. 10 illustrates an implementation with a CNT linear ion/molecule accelerator to accelerate ions/molecules with an electric field and measure the acceleration with multiple ion/molecule detectors.
  • ion/molecule detectors 1002-1006 are placed before the first set of beam lenses 1008, between the beam lenses 1008 and the accelerator lenses 1010, and after the accelerator lenses 1010.
  • the constant potential drop along the CNT axis (z) provides a constant acceleration force along the CNT (x).
  • the length L2 of the accelerator lenses is given by the following equation (2):
  • the present disclosure may also be practiced with helical CNTs.
  • Helical CNTs may extend the propagation path without extending the MS device thickness. The ion/molecule propagation occurs along a spiral path, which results in the emission of electromagnetic radiation. The helical CNT may be twisted back on itself, as shown in FIG. 11 . A twisted-spiral CNT can be used to run ions twice through the electrical field.
  • a CNTFET as described above may be implemented in a variety of different MS systems.
  • a CNTFET particle detector may be provided.
  • FIG. 12 illustrates an example circuit diagram for such a detector.
  • the detector includes a first ion detector 1202 and a second ion detector 1204, both of which are connected to a time-to-digital converter (TDC) 1206.
  • TDC time-to-digital converter
  • Each ion detector 1202/1204 comprises a CNT connected between a power supply voltage and a ground voltage via a resistor. The voltage drop across the resistor is provided to an analog front-end (AFE) circuit, which provides its output to an analog-to-digital converter (ADC).
  • AFE analog front-end
  • the ADC in turn is connected to a controller which outputs its respective detection signal to the TDC 1206.
  • the operation of the detector is shown in the inset.
  • the particle first passes through the first ion detector 1202 where it produces a signal at time 0.
  • the particle next passes through the second ion detector 1204 where it produces a signal at time ti.
  • the particle mass may be determined based on the time difference using the above methodology.
  • the gates of two adjacent CNTFETs can be used to trap ions/molecules when the gate fields are larger than the thermal kinetic energy (at room temperature, approximately 25 meV). This may yield an ion/molecule-trap device. If a higher mass resolution is needed, ions/molecules can be pre-filtered. If ions of only a certain range of masses are entering the CNT and only at a given time, overlapping signals in the source/drain current signals can be avoided.
  • two CNTFETs may be used as shutters to prefilter ions/molecules with respect to velocities (e.g., see FIG. 10).
  • FIG. 13 illustrates such an example, lon/molecule movement can be stopped with appropriate gate settings and timings (AC frequency).
  • the gates can be controlled such that passage therethrough requires a specific speed; thus, particles can only pass between the gates when coming at the appropriate time.
  • shutter applications can be realized.
  • this may be used to customize CNT analyzers for a specific mass range (i.e., velocity range).
  • CNTFETs may be used in detector configurations, as shown in FIGS. 14 and 15. As shown in FIG. 14, CNTFETs may be arranged so as to cause ion-ion collisions. As shown in FIG. 15, a CNTFET may be arranged so as to cause a collision between an ion and a splash target. Fragments after the collision are energy dependent. Scattering angles may be analyzed to provide spectroscopy information.
  • CNTFETs may further be used as a geometrical catalyst, as shown in FIG. 16. Once reactant molecules are within the CNT, they will meet and be forced to react. Physisorption on the inner CNT surface can increase the chance of reaction. [0061] Manufacturing Methods
  • FIGS. 17-18 illustrates one example in accordance with the present disclosure.
  • FIG. 17 is an image of CNT forests grown in chemical vapor deposition (CVD). As illustrated, the CNTs have a length of approximately 350 pm in this example. The CNTs should be parallel to avoid errors in the TOF measurements.
  • CVD chemical vapor deposition
  • FIG. 18 illustrates an example air-stable n-type CNTFET using CNTs manufactured as shown in FIG. 17.
  • the CNT includes a Si base layer, on which a SiCh layer (as illustrated, having a thickness of 500 nm) is deposited.
  • a CNT is disposed on the SiCh layer.
  • Near- ohmic Hf contacts are deposited over the CNT.
  • FIG. 18 also shows the gate-source voltage characteristics of the CNTFET at various temperatures. Note that the CNTFET functionality is improved by avoiding metallic nanotubes, such that the CNTFET can properly be turned off. Thus, after manufacturing the CNTs they may be placed in a centrifuge to separate metallic tubes from semiconducting tubes.
  • FIG. 19 illustrates another example manufacturing method according to the present disclosure.
  • a CNT forest may be grown (e.g., in a manner similar to that shown in FIG. 17). Then, the gaps between CNTs may be filled with layers of insulators and conductors, as shown by alternating yellow and blue areas.
  • a sequence of insulators and conductors may first be grown. Then, holes may be cleaved into the layers as CNT seeds. Finally, the CNT forest may be grown in the holes.
  • the present disclosure validates that CNTFETs work as a very sensitive charge sensor which forms the basis of a TOF mass spectrometer.
  • the CNT-based mass spectrometer can be scaled down significantly compared to comparative examples of mass spectrometers.
  • CNT mass spectrometers are sensitive to dipoles of neutral molecules.

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Abstract

L'invention concerne des analyseurs d'ions basés sur des nanotubes de carbone (CNT). Les analyseurs peuvent comprendre un détecteur comprenant un transistor à effet de champ CNT, et peuvent être conçus pour séparer des ions sur la base de la masse et/ou de la charge.
PCT/US2025/017531 2024-03-08 2025-02-27 Analyseur d'ions à base de nanotubes de carbone Pending WO2025188534A1 (fr)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090166523A1 (en) * 2004-04-27 2009-07-02 Koninklijke Philips Electronic, N.V. Use of carbon nanotubes (cnts) for analysis of samples
US20130233700A1 (en) * 2008-08-01 2013-09-12 Brown University System and methods for determining molecules using mass spectrometry and related techniques
US20140363821A1 (en) * 2011-11-15 2014-12-11 The Board Of Trustees Of The University Of Illinoi Thermal Control of Droplets by Nanoscale Field Effect Transistors
US20170038333A1 (en) * 2015-08-06 2017-02-09 Pacific Biosciences Of California, Inc. Systems and methods for selectively addressing sparsely arranged electronic measurement devices

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090166523A1 (en) * 2004-04-27 2009-07-02 Koninklijke Philips Electronic, N.V. Use of carbon nanotubes (cnts) for analysis of samples
US20130233700A1 (en) * 2008-08-01 2013-09-12 Brown University System and methods for determining molecules using mass spectrometry and related techniques
US20140363821A1 (en) * 2011-11-15 2014-12-11 The Board Of Trustees Of The University Of Illinoi Thermal Control of Droplets by Nanoscale Field Effect Transistors
US20170038333A1 (en) * 2015-08-06 2017-02-09 Pacific Biosciences Of California, Inc. Systems and methods for selectively addressing sparsely arranged electronic measurement devices

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