Spring 2009 EE 710: Nanoscience and Engineering

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1 Spring 2009 EE 710: Nanoscience and Engineering Part 1: Introduction Course Texts: Bhushan, Springer Handbook of Nanotechnology 2 nd ed., Springer 2007 Hornyak, et.al, Introduction ti to Nanoscience, CRC press, 2008 Goddard, et.al, Handbook of Nanoscience, Engineering, and Technology, CRC Press, 2004 Instructor: John D. Williams, Ph.D. Assistant Professor of Electrical and Computer Engineering Associate Director of the Nano and Micro Devices Center University of Alabama in Huntsville 406 Optics Building Huntsville, AL Phone: (256) Fax: (256) williams@eng.uah.edu 1

2 Molecule-Based Devices Top down fabrication of molecular devices utilizes conventional patterning and etching techniques to define nanoscale regions that can then be chemically sensitized for device applications. In nature, tiny molecular building blocks are assembled with remarkable structural control in a variety of materials, shapes, and sizes. However, much of this bottom up approach to nano-engineering has yet to be mastered by human intervention e to 2

3 Nucleic Acids Some of the best examples of bottom up nanoengineering are nucleic acids and proteins. Nucleic acids ensure the transmission and expression of genetic information. Nucleic acids are linear polymers with specific nucleotide repeating units that can contain enough information within a single molecule to describe all of the genetic structure of a living organism. DNA and RNA for example provide contain all of the information (commands) required to produce or functionalize a living organism using only 4 nucleic bases in a approximately 100 repeating units. Thus, nature has systematically engineered a mechanism to generate or 1.6*10 60 bits of information in a single molecule. 3

4 Proteins 20 different amino acids differing gprimarily in their side chains and all containing a similar backbone of carboncarbon bonds are used by nature to generate every protein known currently known to man. This is achieved by covalent bonding of different amino acids into polypeptides that then bond with other amino acids and polypeptides to form proteins varying in complexity from a few amino acids to over 4000 individual building blocks. Thus nature has found a way to fabricate more than 1* different molecular devices, each containing a specific biological function through the manipulation of 20 simple molecules. 4

5 Organic and Inorganic Byproducts Nanotubes: Carbon nanotubes are known byproducts of high temperature reactions with organic material Ex. Soot contains multi-wall carbon nanotubes Inorganic nanotubes and nanowires are known to form naturally under high pressures and temperatures (near volcanic systems, especially those in water environments) or in areas where crystallization occurs Living organisms also generate nanomaterials as byproducts. Spider silk, and several Group I and II crystallites are generated commonly by living organisms 5

6 Questions for Every Nanoscientist The question we must ask ourselves, is this: How can we use the simplicity of natural systems to engineer complex transducers capable of sensing, storing, and signaling such large amounts of information and integrate them into our current designs for modern micro and semiconductor devices? Furthermore: How will we interface with future generations of these transducers when we move beyond the need for current semiconductor and top down machining applications? 6

7 Modern Chemical Synthesis We have currently developed the technology required to join molecular components with structural control at the picoliter level. We know this through extensive use of chemical and spectroscopic testing developed over the course of the last century. Light, X-ray, electron, ion, and atomic spectroscopy techniques currently provide us with the exact chemical and structural composition of many simple molecular chemistries. However the chemical free energy present in very large molecules at room temperature prevents us from learning the exact structural shape of complex proteins and long chain polymers at any given time. Thus we rely on a combination of spectroscopy, molecular computing, and a solid understanding of various binding energies to predict the shape and functionality of very large organic molecules in order to interpret their true functionality. With this information, we can currently construct very large organic molecules designed using nature s template for the specific purpose of nanoscale transduction. 7

8 From Structural Control to Designed Functionality In a manner similar to that of nature, supramolecular organic chemists currently engineer new molecules capable of passing current, other molecules, or information for next generation transducers. 563 nm Absorption band No Visible Absorption 8

9 Easily Generated Chemically Active Sensor Materials Pyrozaline Anthracene Derivative Anthracene 9

10 Photochemical Optical Sensors No Visible Absorption and dencoders 563 nm Absorption band While colorless 5 will not absorb in the optical, heat sensitized 7 retains a deep purple color reducing the amount of 563 nm visible light from propagating through to the detector. In fact if just one of the three ultraviolet (or chemically reacted) inputs is turned on then, the optical output drops by 3-5% of the input signal. If two or three inputs are turned on simultaneously, then the total output power is reduced to 0%. Acetonitrile Solution 10

11 Photochemically Active Sensors and doptical lencoders Two communicating molecular switches in solution provide up to 4 possible combinations for a single state yielding much more information than a single molecule l switch measured by light or electrochemical response alone 11

12 Langmuir-Blodgett Films Used to apply monolayers of a chemical onto an active surface. Most common example is the application lipids to a glass, ceramic, or plastic substrate. The ability to transfer electroactive ti monolayers of from the air water interface is often used to fabricate arrays of molecule based electronic devices. 12

13 Self Assembled Monolayers (SAMS) Alternatively, certain compounds such as thiols absorb onto surfaces as single monolayers Prepatterning of the surface to prevent adhesion in particular locations provides an excelent means of binding chemically active monolayers over large areas for device technologies. Nitride, oxide, certain metals, and in some cases even resist can be used as the barrier for adhesion of SAMs SAM layers are then used to: Alter the surface tension of the substrate Promote nanoparticle adhesion Reduce friction and stiction Promote adhesion of organic or inorganic media for sensing 13

14 Combining Top Down and Bottom Up Combination of Top down patterning with bottom up chemistry Demonstrates that electroactive organic chemicals can be patterened uniformly over mesoscopic surfaces that t are micro patterned. The resulting surfaces can be used as catalyst t or sensors for either electrochemical, covalent, ionic, or photochemical detection 14

15 Patterning Gold Nanoparticles Uses Thiol chemistry to attach gold to surface Au nanoparticles provide single electron chemical sensitivity in solution near -0.2V 15

16 Solid State Devices Used in combination with Ti or Al electrodes, allows for stackable junctions that provide significant changes in current below -0.7V 16

17 Molecular Transistors 30 nm oxide 15 nm x 300 nm Au Formation of thiolate gold bonds between molecule and Au allowing the acceptance and donation of electrons to the Au leads via electromigration across a 20 nm gap. This nonlinear response produces a transistor like effect with an operational current of 0.05 na around 20 mv DNA transistors demonstrate 50nA when the gate voltage lowers from - 10Vt 1.0V to -1.3V 13V 17

18 Molecular Transistors (NOT gates) Off chip bias resistor connected to the train terminal of a single transistor while the source is grounded Micro scale silicon gate with nanotube contact Application of -1.5V lowers the nanotube resistance (26 MOhm) below that of the bias resistor (100 MOhm). As a result, the output bias drops to 0V. When no voltage is applied, the resistance of the nanotube increases leading to a -1.5V output 18

19 Molecular Transistors (NOR gates) Pair of off chip bias resistors connected to the train termainal of a single transistor while the source is grounded When both nanotubes are in a nonconducting output state (no applied voltage) then the terminal output of the device is -1.5V Application of -1.5V to either or both nanotubes lowers the nanotube resistance (26 MOhm) below that of the bias resistor (100 MOhm). As a result, the output bias drops to 0V. 19

20 Probing the Nanoscale Modern science and engineering uses electrons, photons, ions, and scannig probes and thermodynamic analysis to probe the nanoscale. Optical Confocal microscopy Near field Scanning Optical Microscopy Flouresence spectroscopy Electron SEM, TEM, RHEED Scanning Probe Techniques (mechanical) Contact and non-contact AFM, STM, MFM, CFM Photon Raman spectroscopy Energy Dispersive Spectroscopy (EDS) EDAX X-ray photoelectron Spectroscopy (XPS) X-ray diffraction Near IR Surface Plasmon Resonance Nuclear Magnetic Resonance (NMR) Particle Mass spectrometry Secondary ion mass spec Rutherford Backscattering Neutron scattering spectrometry Particle induced X-ray emission Thermodynamic Thermogravometric analysis Nanocalorimetry Thermoluminescence Bulk engineering Stiffness Elasticity Fluid response 20

21 Manufacturing at the Nanoscale Patterning Deposition E-beam lithographyh Thin film Evaporation Nano-imprint lithography Sputtering Focused Ion Beam lithography MBE (single crystal) X-ray Lithography PECVD Patterning/positioning LPCVD SPM techniques Laser Assisted CVD Electrostatic manipulators Atomic Layer Deposition Magnetic manipulators Surface Chemistry Microtechnologies SAMs Etching Langmuir Blodget Films Reactive ion Etching Chemical Etching Electrochemical deposition/etch/corrosion Supramolecular chemicals 21

22 Advances in Optical Microscopy Conventional and conformal microscopies that use conventional lenses to image multiple scattering orders of light reflected from a surface Thus the resolution limit of conventional optical microscopy is about 0.5 um Confocal microscopy that utilizes two image planes instead of one has a resolution of approximately 0.2 um with a much smaller depth of focus. Near field Scanning Optical Microscopy uses a sub wavelength aperture to image effervescent waves in very close proximity to a sample and can be used to resolve features smaller than 100 nm. Scanning NSOMS often use AFM type scanning systems to generate the proximity between the aperture and the sample 22

23 Advances in Optical Microscopy NSOMs generally use glass fiber tips that have been pulled to diameters much smaller than the wavelength and coated with an aluminum film to prevent light from exiting the fiber except at the end of the tip Light can be passed through the tip to illuminate a transparent surface, passed through the sample and collected in the tip, any combination of both. However signals passed through a tip in both directions significantly impact the background noise of the observation The transparent aperture is limited in size by the amount of optical power that can be transmitted through tip and distance placed above the surface Optical power squeezed into a very fine tip heats the aluminum film significantly causing local heating of the surface at very close proximities and thermal degradation of the fiber Thus NSOM tips are typically held to a diameter no less than 100 nm

24 Advances in Optical Microscopy The optical resolution lost by tip heating can be overcome using localized electric field enhancement. This technique uses reflected laser light focused on a tip as small as 10 nm to generate very large effervescent fields between the tip and the sample. The tip, and focal point are then scanned across the surface while constantly recording the potential generated in the tip during the scan. This produces highly accurate 10 nm optical images of surface being scanned. 24

25 Scanning Probe Microscopes How exactly does one scan a surface with a 10 nm tip? Answer: Scanning Probe Microscopes SPMs use a wide variety of different sense technologies coupled with a very sharp tip, piezoelectric displacement stage, and an optical positioning sensor to measure surfaces near the atomic scale. SPM resolutions range from 5 10 nm depending on the tip and the surface profile SPM tips are generally silicon or Si3N4 based but can be modified d by magnetic coatings, electrically isolated leads, carbon nanotubes, etc. They are sometimes even constructed of tapered optical fibers to be used in conjuction with an NSOM device. SPMs operate in three types of modes: Contact - STM/AFM Noncontact AFM Tapping Mode AFM The contact method is used to drag the tip across the surface. This allows for nanolithography and positioning of atoms on the surface Noncontact uses a specific physical force measurement in the feedback loop as the sense technique Tapping mode relies on the spring constant of the tip to and its response to surface forces to provide information about the substrate 25

26 Scanning Tunneling Microscope Original method (1981) for generating atomically resolved structures using a mechanical system Tip is driven by a tube containing multiple piezoelectric strips that direct the tube in x, z, and z directions. Original tips were generated by wet etching silicon crystals to a very sharp point. Measurements are made by measuring the tunneling voltage between the tip and the sample. Low temperature and UHV STMs became common in the early 90s for measuring pristine sample surfaces without thermal noise or oxidative effects. Two modes of operation: Constant-height mode Tip travels across the plane above the sample and records changes in the tunneling current Faster but provides information only from smooth surfaces Constant-current mode Tip height is governed by a specified tunneling current. Height is measured by the voltages recorded in the piezolelectric sensors Slow but can be used to measure irregular surfaces with high precision

27 AFM Technologies Shortly after the STM was developed, IBM researchers engineered a slightly different version that allowed the sample to be measured without direct contact The Atomic Force Microscope (AFM) became a commercial tool within 4 years of its inception. The system differs by placing the PZT stage under the sample, and using a cantilevered beam to regulate the vibration of the tip. An optical probe can then be used to measure the vibration of the cantilever allowing for angstrom resolution of its deflection The cantilever can then be dragged across, tapped over, or simply vibrate above the surface of the sample due to different electrostatic forces present at the surface of all materials However: AFM is unsuitable for UHV applications Modern SPM Dimension V SPM and 4nm 27 probe tip from Veeco Instruments

28 AFM Sensing Techniques Contact mode: Tip makes soft physical contact with the sample Van der Waals forces between the tip and the atoms on the surface prevent the tip from actually touching the atoms on the surface Measurement is made based on the strength of the Van der Waals repulsive force Force exerted on the cantilever is like that of a compressed spring, which allows deflections to be readily monitored by optical reflectometry t Operating forces at the tip are approx. 10E-6 to 10E-7 N Operation of contact AFM is very similar to that of an STM. Constant force Constant height Non-contact mode: Cantilever is vibrated near resonance ( KHz) near the surface at an amplitude of 1-10 nm Spacing is between 1 to 10s of Angstroms between tip and surface Vibration of the cantilever is altered by the attractive force near the surface Deflection force is low and therefore more difficult to measure than contact forces This method is prefered for measuring soft samples that may be compressed by applications of a few micronewtons such as liquids, biological samples, and soft polymers. Tapping Mode Similar to NC mode, but the cantilever is actually brought into contact with the surface. Measurements are then made of the elastic response of continued tapping of the spring 28

29 AFM Technologies Magnetic Force Microscopy Tips coated with ferromagnetic thin film (often NiFe) Vibrational response from NC mode operation provides nm scale resolution of magnetic domains as well as topographical properties of the sample Lateral Force Microscopy Contact mode operation in which twisting of the cantilever arises from sliding friction forces on the substrate surface. Soft cantilevers are used Provides topography and surface tension or frictional information simultaneously Force Modulation Microscopy Provides topographical and elastic material properties using NC and Tapping mode by observing the amplitude response change as the tip crosses the boundary from one material to another Phase Detection Microscopy Uses NC and tapping mode to examine phase shifts in the frequency response due to changes in material properties such as elasticity, adhesion, friction etc. Electrostatic Force Microscopy Charged tips are used to measure different electrical responses in substrates. This can be used to map TFTs and provide nm resolution for identifying response and defects in circuit design NC Constant Voltage technique Scanning Capacitance Microscopy NC Constant height Measures change in capacitance across the sample and provides information on dielectric strength in circuit designs Electrochemical Force Microscopy Liquid phase electrostatic and capacitance microscopy for examining cathodic potentials on the surface while mapping topography Near Field Scanning Optical Microscopy previously covered Nanolithography Becoming less important today due to the advent of nano-imprint Uses contact AFM to alter the surface chemistry in a 5 x 5 um area allowing for further bottom up application Uses contact AFM to alter the location of atoms at the surface to build nanodevices or quantum dot arrays Magnetic Resonance Force Microscopy Single Spin Detection High frequency RF coil used to oscillate the spin of local area magnetic moments NC magnetic AFM provides NMR elemental sensitivity with the topographical resolution of AFM. Requires specific geometry and uniform applied magnetic fields to create spin sensitive magnetic circuits at the tip head to achieve detection limits of 1E-18 N 29

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