Nanolithography

Fountain pen nanowriting of liquids, gases, suspensions, and proteins

NanoCNT

The Fountain Pen Nanolithography (FPN) MultiProbe system is an SPM platform capable of both chemical nanolithography and online imaging with multiple probes.  Based on our revolutionary multiprobe technology, this system provides two completely independent SPM probes.  Thus one probe can write using two different materials, or one probe “writes” while the other probe "reads" or images the deposition with a high resolution AFM probe without moving the sample or exchanging the probe. The MultiProbe system has a modular design and can be upgraded to four SPM probes.  Different methods are used for nanometric control of the delivered and deposited material including capillary action, force control and capillary electrophoresis. 

FPN systems allow for unique online integrations with a variety of instruments such as optical microscopes, Raman spectroscopy, confocal microscopes, etc. Furthermore, it uses Nanonics NanoToolKitTM probes for a variety of SPM functional imaging techniques. 

 

 

 

Key Features

Flexibility

  • Total flexibility for your experiments
  • A variety of inks including organic liquids, aqueous liquids, gases, proteins, nanotubes, nanoparticles and rods
  • A variety of surfaces and samples including any geometry - flat or rough, and any material -  conducting or insulating.  Also suitable for deposition onto large samples such as wafers, petri dishes and microscope slides

 

Precision

  • Precise placement of liquid or gas within nanometers of accuracy
  • Electrophoretic lithography of gases via electrical pulses for accurate and controlled chemical deposition
  • Pressure controlled deposition of liquids

 

Comprehensive Characterization

  • Full characterization of your deposited/written features
  • Multiple probe lithography protocols for reading, writing and simultaneous imaging on one platform
  • Free optical axis allowing full integration with optical microscopes for optical and spectroscopic analysis including fluorescence, Raman, and near-field optics.
  • Full operation inside environmental chambers and flexible connection with chromatography systems. 
  • Online SPM characterization of written features including Electrical, Thermal Conductivity, Magnetic , optical near-field (NSOM) and far-field characterization operation.

 

FPN Technology 

  • FPN is a technique that uses very fine pipettes with small apertures on the order of ~100nm.  These pipettes are attached to an AFM cantilever arm allowing molecules to flow out through the tip, in a manner very similar to a fountain pen.  This process is shown in the schematic to the right.  This approach of nanolithography offers several distinct advantages including the ability to write any material on any substrate with total control to turn writing on or off.
  • In addition, FPN can be integrated with any optical methods so that probing or detection or written/etched lines can be performed with methods such as fluorescence and Raman.  
  • Powerful applications of FPN with other characterization methods include 1) using Raman microscopy to probe alignment of carbon nanotubes 2) electrical and thermal measurements to probe the conductivity of written contacts and 3) fluorescence imaging of written protein arrays.

 

Capillary Nanopipette Probes 

Quartz capillary nanopipette AFM probes for chemical nanolithography. FPM probes have a cantilevered bent probe geometry suitable for multiprobe operation and for integration with online techniques.

 

Tuning Fork 

Ultrasensitive Tuning Fork AFM feedback is used for control of the deposition and AFM imaging of the deposited patterns. Optical beam bounce feedback is also available.

 

Applications

Click the pictures for details...

FPN Nanolithography Writing And Online AFM Imaging Deposition of Protein Nanoarray Using Fountain Pen Nanolithography Nanolithography SPM Writing of a Protein

FPN Nanolithography On Previously Written Lithographic Pattern High Resolution Nanolithography With Nanonics FPN Multiprobe System Using Nanolithography To Work With Deep Trenches.

Nano Ink Jet Printing

Gold Line Using FPN Chlorine Gas Nanolithography
Protein Nanoprinting Protein Writing on Si Surface NanoEtching Using FPN
Protein Nanoarray TiO2 Nanolithography Two-Probe Nanolithography

 

 

 

Filling Trenches

Problems with a complicated surface structure, such as circuit edit, can be attacked only by FPN. It has a Z-range of >100 microns, allowing the AFM to see into deeper trenches than any other system. 

10 x 10 micron AFM image of a
10 micron deep/2 micron wide trench 

Filling a Trench: Before and After

Controlled filling of silicon trench with gold particles

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Ink Jet Printing

 

A: Confocal image of deposited Bovine Serum Albumin (BSA) protein deposited with 150nm AFM nanopipette probe with a driving pulsed voltage at the sequence shown in B. The image shows deposition of the protein at the negative provided pulses. Bar is 6 microns.

B: Diagrammatic spatial map of the provided voltage applied on the Nanopipette at a negative pulsed signal as shown in C.

C: Negative pulses voltage provided through two electrodes at the inner of the nanopipette and the metallic coating at the end of the nanopipette’s tip. The image (A) shows clearly that the protein was delivered out to the surface at the blue lines where the voltage is -1V and no writing at the zero voltage areas indicated by green at B.

“The general nanoprinting and nanoinjection of proteins on non-conducting or conducting substrates with a high degree of control both in terms of positional and timing accuracy is an important goal that could impact diverse fields from biotechnology (protein chips) to molecular electronics and from fundamental studies in cell biology to nanophotonics.

Nanonics combines capillary electrophoresis (CE), a separation method with considerable control of protein movement, with the unparalleled positional accuracy of an atomic force microscope(AFM). This combination provides the ability to electrophoretically or electroosmotically correlate the timing of protein migration with AFM control of the protein deposition at a high concentration in defined locations and highly confined volumes estimated to be 2 al.

Electrical control of bovine serum albumin printing on standard protein-spotting glass substrates is demonstrated. For this advance, fountain pen nanolithography (FPN) that uses cantilevered glass-tapered capillaries is amended with the placement of electrodes on the nanopipette itself. This results in imposed voltages that are three orders of magnitude less than what is normally used in capillary electrophoresis.

The development of atomic-forcecontrolled capillary electrophoretic printing (ACCEP) has the potential for electrophoretic separation, with high resolution, both in time and in space. The large voltage drop at the tip of the tapered nanopipettes allows for significant increases in concentration of protein in the small printed volumes.

All of these attributes combine to suggest that this methodology should have a significant impact in science and technology.”

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Gold Line using Fountain Pen Nanolithography

Gold NanoParticle Lines Printed on a Microchip

Figure 1: SEM and AFM gold nanoparticles line printed on semiconductor surface. (a) SEM image shows the gold nanoparticles line printed by FPN. Scale bar is 5 microns. (b) AFM image of smaller area than in (a) shows the same printed line as in (a).

Elemental Anaylsis of a Gold Line Written with the NanoFountain Pen

 

Figure 2: Gold nanoparticles line printed on semiconductor surface by FPN technique in close juxtaposition to a gold line produced by electron beam lithography technique. (a) AFM image shows the lines produced by electron beam lithography and the gold colloid line deposited by FPN on the right side of the image. Scale bar is 1.2 cm, (b) Zoom-in image of the marked area on (a) highlights the deposited line. Scale bar is 360 nm.(c) Height profile line between the marked arrows on (a) shows one of the electron beam lithography lines with width of 250 nm and height of 45 nm and the FPN deposited line 6 with width of 100 nm and height of 15 nm. (d) Electron-induced x-ray fluorescence spectrum of the FPN deposited line shows Au on the right peak. 

Comparison of Line Profiles of a Gold Line Written with The NanoFountain PenTMand a Gold Line Produced by Electron Beam Lithography

 

 

Elemental and I-V Characteristics of a Gold Line Written with The NanoFountain PenTM

EDS Measurement of the gold line

I-V Characterization of the gold line:

The line slope shows Ohmic behavior with resistance of ~ 650 ohms.

I-V Characteristics of a Gold Line Written with The NanoFountain PenTM

FPN Gold colloids line deposited in the interconnection of a 100 nm separation of two conducting wires for current-voltage characterization (a) Optical image shows the inner electrodes pattern for the I-V characterization (x100 magnification). (b) Optical image of the inner electrodes area (x1000 magnification).(c) AFM image shows the inner electrodes pattern with a printed gold nanoparticles wire crossing a space of 100 nm between two electrodes. (Scale bar is 800 nm.) (d) Height line profile of the dashed line on (c) shows the gold nanoparticles 120 nm line on top of one electrode. (e) I-V characterization of the printed line shows an Ohmic behavior with resistance of ~4000 Ohm (y-axis in units of microamps). 

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Chlorine Gas Nanolithography

Etching of Chrome Film with Free Chlorine Radical

 4.5 X 4.5 micron image of Chorine line etched onto chrome film

Protein printing is made possible by the Nanonics Chemical Delivery System and Nanopipette

Only Nanonics can deliver chemicals or gas onto the sample on line, with no need to remove the tip from the sample.

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Protein Printing

 40 x 40 micron Topgraphy 3D image

Only Nanonics can deliver chemicals or gas onto the sample on line, with no need to remove the tip from the sample.

Protein printing is made possible by the Nanonics Chemical Delivery System and Nanopipette

Using any of the Nanonics MultiView systems, chemicals, in liquid or gas form, can be fed into the pipette via a silicon tube. Apart from Protein Printing, applications of this setup include metallic nano-etching and nanolithography: an etchant can be introduced into the sample and scanned across it with nanometer precision using our 3D FlatScanning™ technology. The nanopipette is engaged by the sample using standard contact-mode atomic force microscopy, and our integrated system makes it possible to view the etching simultaneously through any optical microscope.

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 Protein Writing on Si Surface

 

BSA protein writing on Si surface using the Fountain Pen Nanolithography technique. On the left is an AFM image presenting two lines of the BSA. The plot on the right shows a height line profile of these lines. A pipette of 100nm aperture has been used with contact mode of 20µm /ms writing speed.

A silicon surface has been selected for writing due to its significance in the semiconductor industry. Using FPN for patterning on silicon could open the door for this technique to be integrated into different fields of semiconductors and materials.

Patterning with biological materials on silicon demonstrates the ability of FPN in biochip technology. FPN allows for patterning with biological materials onto Si surfaces, commonly used in integrated circuits and semiconductor devices.

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NanoEtching Using FPN

Nanoeteching of chrome by dispensing  liquid through a cantilevered force sensing nanopipette - a NanoFountainpenTM (middle and right frames recorded through the fully integrated optical microscope during the chemical etching process).

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Protein Nanoarray

4X4 micron Image of Protein dots printed with a Nanofountain Pen

 Protein printing is made possible by the Nanonics Chemical Delivery System and Nanopipette Only Nanonics can deliver chemicals or gas onto the sample on line, with no need to remove the tip from the sample.

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TiO2 Nanolithography

TiO2 Particles on Hydrophobic Surface

All the structures below were formed by online delivery of the chemical to the surface using the Nanonics Chemical Delivery System and Nanopipette. The Images were produced using the using the MultiView 4000™.

Only Nanonics can deliver chemicals or gas onto the sample on line, with no need to remove the tip from the sample.

4.5 X 4.5 micron AFM image of TiO2 line
AFM topography of TiO2 ring
AFM topography of TiO2 ring

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Two-Probe Lithography

 

A: Optical microscope picture (50x objective) shows two-probe lithography with a nanopipette probe for writing and an AFM probe for imaging. BSA protein deposition on an aldehyde modified surface is demonstrated.

B: Imaging of the deposited features with an AFM probe.


 

C: AFM topographic image shows the printed features as in B. 

Nanonics' two-probe systems are unique for nanolithography manipulation and imaging. A nanopipette is used as a first probe to perform the lithography under capillary forces or voltage controlled  deposition. The second probe is used for accurate SPM imaging.

  • The advantages of online writing and reading are:
  • It is not necessary to change the tips to perform lithography and subsequent AFM imaging – both tips can be mounted on one system. This allows for higher AFM resolution and for easier location of the deposited features.
  • Immediate scanning following the deposition procedure can be achieved.
  • Multiprobe systems are operated by tip and sample scanning modes which allow for flexible positioning and manipulation.
  • All probes, nanopipettes and AFM probes are completely exposed to the Z optical axis of upright and inverted microscopes.
  • Nanonics’ Fountain Pen Nanolithography permits the integration of a variety of inks and samples. 

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Integrations

FPN MultiProbe 

(Left) FPN system with two probes for nanolithographywriting and AFM/SPM imaging, mounted on a Dual Optical microscope with free Z optical axis.

(Right) Two probes close-up shows nanopipette probe (right) for nanolithography and a second probe (left) for AFM/SPM imaging. 

 

Environmental Chambers 

    

  • MultiProbe Operation inside environmental chamber
  • Full integration with environmental chambers allows for use with samples that cannot be viewed/manipulated in an ambient environment
  • Vacuum control
  • Gas inlets/outlets
  • Temperature control- Heating & Cooling
  • Free optical Axis from top and bottom- Complete integration with Dual optical microscope

 

Optical Microscopy 

  • Full integration with upright, inverted or dual (4 Pi) optical microscopes 
  • Full integration with non-linear and multi-photon microscopes (e.g second harmonic generation microscopes)
  • Completely free optical axis from above and below the sample
  • Complete freedom of optical microscope nose piece rotation from above or below
  • Open system architecture providing Transmission, Reflection and Collection modes

 

Integration with Complementary Technique 

  • Online Raman 
  • Online Scanning Electron Microscopy - SEM
  • Online Focused Ion Beam - FIB
  • Online Dual Focused Ion Beam with scanning electron microscope - SEM

Specifications

SPM Platfrom

MultiView SPM Series

  • Supports Imaging and manipulation standard SPM modes
  • Frequency Modulation Tuning Fork feedback with high Q factors and non-interfering feedback
  • Optical Beam Bounce feedback
  • MultiProbe SPM with up to four simultaneous probes for “writing” and “reading”

Scanning Stages

  • Tip and Sample scanning stages
  • Closed loop and opened loop scanning stages

Probes

  • FPN Capillary Nanopipette probes
  • All forms of cantilevered glass probes from Nanonics exclusive NanoToolKitTM, Nanosensors including Akiyama tuning forks probes and Si probes.
  • Suitable for 3rd Part probes

FPN Nanolithography

  • FPN Capillary Nanolithography via capillary forces
  • Electrophoretic FPN Nanolithography via pulsed voltage control

Samples and Stages

  • Large samples up to 120mm in XY and 30 mm in Z
  • Piezo rough positioning of 6mm
  • Motorized positioning

Optical Integrations

  • Free optical axis for integration with upright, inverted and dual optical microscope configurations.
  • Flexible integration with various spectroscopy tools such as Raman, Fluorescence, etc.

Environmental Chambers

  • Full operation in environmental chambers

Controller and Software

  • Modular hardware controller
  • Flexible software interface for scripting and user's own programming
  • Flexible signal access module

 

MultiView SPM Series

MultiView 4000TM

  • MultiProbe SPM system. Modular and upgradable from one to four online SPM probes for imaging and manipulation
  • Ultra-SensitiveTuning Fork feedback. Optical feedback is also available (Optional)
  • Tip and Sample scanning stages

MultiView 2000TM

  • UltraSensitive Tuning Fork feedback. Optical feedback is also available (Optional)
  • Tip and Sample scanning stages
  • Single probe. Upgradable to multiprobe

MultiView 1000TM

  • Beam bounce feedback
  • Sample scanning stage
  • Single probe, upgradable for multiprobe

 

FPN Nanolithography

FPN Nanolithography

  • Capillary Nanopipette Glass probes with atomic force controlled delivery
  • Nanolithography based capillary nanopipette probes with apertures of 5nm to 10um
  • Nanolithography based voltage controlled capillary nanopipette probes for accurate spatial control
  • Suitable for online MultiProbe lithography
  • 100nm – 10 um features size patterning
  • Flexible control of features size and shape through SPM
  • Ability for the nanochemical writing operation to be accomplished in parallel with optical confocal, near-field optical or Raman imaging
  • Special hardware and software.

Inks (Wet/Dry):

Lithography through

liquids & gases

  • Chemical fluids delivery with variety of liquids including organic and Aqueous solvents, proteins, metallic nanoparticles in different suspensions, chemical etchants, etc.
  • No chemical tip treatment
  • Hydrophobic and hydrophilic liquids
  • Gas delivery

Samples

  • Variety of sample including conducting semi-conducting and non-conducting substrates including glass, mica, Si, SiO2, metals and variety of other surfaces.
  • No chemical treatment is needed for sample
  • Suitable for large wafers

Electrophoretic FPN Lithography

  • Ability to impose voltage on chemical inks delivered by the nanofountain pen with electrodes placed directly on the atomic force sensing nanofoutain pen thus allowing to write with controlled voltage on nonconducting and conducting substrates

Reservoir

  • 1uL reservoir provided by the nanopipette probe
  • A syringe based reservoir can be used with a volume of 10ml and with a possibility for larger reservoirs
  • Simple probe filling via simple capillary actions

Software-Controlled Lithography

  • Intuitive graphical interface for liquid and gas deposition
  • Possibility of drawing polygons, sets of parallel lines with different spacing, and points
  • Possibility of changing the electrical bias and the force between tip and sample
  • Possibility of drawing on a previously acquired AFM scan
  • Software user interface for user own scripting and programming

 

Scanning stages (MV4000)

Scanning Stages

  • Piezo based flat scanning stage with central opening suitable for integration with optical microscopes with clear optical access from above and below
  • Optional: Closed loop scanner with capacitive XYZ sensors
  • Suitable for Tip and Sample scanning modes

Range

  • Up to 135µm XY and 100 µm in Z (open loop)
  • 100x100x20 µm (XYZ) sample scanning with closed loop option.

Resolution

  • XY = 0.005nm, Z = 0.002nm
  • Closed loop scanner: XY: 0.3nm, Z: 0.1nm
  • Closed loop scanner linearity: 0.03%

Z Imaging Noise

  • 0.05nm rms/ 0.2nm p-p obtained with AFM imaging of HOPG sample with atomic steps

Sample Size

  • Up to 120 mm in XY and 25mm in Z
  • Large samples with odd geometries including hanging positioning for cross section scans

Sample Weight

  • Up to 70 gr.
  • Up to 2500 gr. with closed loop scanner

Sample Positioning

  • 6 mm XY positioning through Piezo Innertial Motion with control through AFM software and  <1 micron positioning accuracy
  • Microns of fine XYZ positioning through Piezo offsets with accuracy of <1nm

Tip Positioning

  • Microns of fine XYZ positioning through Piezo offsets with accuracy of <1nm
  • 5mm XY and 12mm Z motorized motion

Manual or Motorized XY Stage

  • Manual or motorized stage for coarse motion
  • Optional Z stage

 

Probes

Cantilevered Glass Probes

  • Nanonics’ patented NanoToolKit based cantilevered bent probes for all standard SPM imaging and manipulation modes including: AFM, NSOM, Electrical, Thermal, TERS, etc…
  • Suitable for beam-bounced and tuning fork feedback.
  • Customized dimensions of tip size, cantilever length, spring constant and metallic coating.

All Forms of Standard Si Probes

  • Suitable with beam-bounced and tuning fork feedback
  • Supports all standard SPM imaging and manipulation modes

FPN Probes

  • Capillary nanopipette probes
  • 5nm – 10000nm tip aperture
  • Electrophoretic FPN probes
  • Standard Si probes for lithography

 

Tuning Fork Feedback

Tuning Fork Feedback

  • High Q factors
  • Large Spring constant
  • Ability to employ normal force atomic force feedback without any optical interference
  • Overcomes adhesion ringing and jump-to-contact effects.
  • Support Frequency modulation

 

Optical Integrations

Integration with Optical Microscope

  • Free optical axis from top and bottom for integration with true confocal optical microscopes
  • Upright
  • Inverted
  • Dual upright/inverted microscopes
  • Video Microscopes
  • Suitable for both opaque and transparent sample
  • Full correlation between AFM and optical images.

Objectives

  • 10x, 50x and 100x objective
  • Suitable for variety of objectives from below including oil immersion objectives

Online Integration

  • Raman microscopes and spectrometers.
  • Confocal and Fluorescence microscope
  • Variety of techniques such as FTIR, Life time measurements, CARS…
  • Near-field scanning optical microscopes (NSOM)

 

Environmental Control

Environmental Control

  • Full integration with optical microscopes
  • Humidity Control: 5%-90%
  • Optional: Vacuum control 10^-6 torr
  • Gas inlets
  • Optical fiber inlets
  • Easy feed-through of cable

Liquid cell

  • Liquid cell for AFM scanning inside liquid media
  • Suitable for petri dish

Sample Cooling/Heating

  • Cooling/Heating: +10ºC/+60ºC
  • Programmable temperature control
  • MilliKelvin resolution
  • Optional: -20ºC/+150ºC

 

Vibration & Acoustic Isolation

Vibration Isolation

  • Isolation from floor noises to allow AFM imaging of atomic steps of HOPG
  • Vertical and horizontal natural frequency of 1/2 Hz or less can be achieved over the entire load range
  • Active or Passive isolation

Acoustic Isolation

  • Acoustic shielding enclosure for protection from air current and temperature gradients

 

Hardware/Software Control

SPM Controller

  • Feedback speed of 4MHz
  • Digital PID gain control
  • FPGA based PID control
  • ADCs/DACs in 18 bit
  • 18 bit ADCs 4MHZ of sampling rate with 92 dB SFDR with various input ranges of +/-10V, +/-5V, +/-2.5V,  +/-1.25V
  • X, Y, & Z High Voltage Amplifiers, Voltage output of ± 150v, 4 voltage display channels, Hardware slop compensation.
  • 4 digital inputs and outputs
  • 8 analog inputs and outputs
  • MultiPass technique for MFM, EFM, KPM and other modes which require control of tip lifting above the surface.

 

Software

  • LabView based Software
  • Intuitive scan parameter setup
  • Real time processing of tilt removal and line normalization
  • Imaging and displaying 16 simultaneous channels
  • Zoom-in and offset scans
  • Inertial motion software interface for sample positioning
  • Z stepper motor interface for tip-sample approach
  • SmartScan for 3D scans
  • Extensive image processing options
  • Import data as Windows bitmaps and ACSII; export data as TIFF and Windows bitmaps and ACSII

Signal Access Module

  • Hardware and software access for all scanning and feedback signals
  • Convenient connection ports for outputting of different signals for monitoring and other external uses through digital and analog ports.

ScanControl Module

  • Built-in module allows user to actively control the AFM scan for integration and synchronization with external instrumentation (such as Raman spectrometers, pulsed lasers, etc.)
  • Easy and intuitive graphical interface for specifying measurement points
  • Possibility of taking extra ADC measurements during scan
  • Possibility of sending triggers to external hardware during scan
  • Possibility of running a user-defined Labview vi, allowing the user to perform any action or calculation during the scan

 

 

 

 

 

 

 

 

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