SYNTHESIS AND CHARACTERIZATION OF NANOPARTICLES

Lokesh Kulkarni
Dept. of Industrial and Systems Engineering September 11th, 2009

OVERVIEW
Synthesis Techniques: Top-down and Bottom-up Synthesis Processes: i. Gold synthesis in laboratory ii. Inert gas condensation iii. Laser ablation process Characterization Tools: i. Scanning Probe Microscopy ii. Transmission Electron Microscope iii. Scanning Electron Microscope Current Research

SYNTHESIS OF NANOMATERIALS
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Top-down processes: Used to manufacture conventional products Newly developed techniques allow for much smaller sizes (close to 1m) Processes include: Milling, Grinding, Electron beam machining Examples of products: Traditional furniture, car chassis, etc.

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Source: Nanotechnology: An Introduction to Snthesis, Properties and Applications by Dieter Vollath

SYNTHESIS OF NANOMATERIALS
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Bottom-up Process: Uses atoms and molecules as building blocks of structures

Source: Nanotechnology: An Introduction to Snthesis, Properties and Applications by Dieter Vollath

Focus of nanotechnological manufacturing processes Examples: Chemical synthesis processes Because molecular chemistry dictates the structure and hence, properties of nanomaterials, it is very important to be able to control such processes

SYNTHESIS PROCESSES
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Laboratory method for synthesis of gold nanoparticles: Chemicals: Auric salt (source of Au ions), sodium citrate (reducing agent and surfactant), deionized water (medium of reaction Equipment: Flask, magnetic stirrer with heating capability Process: See figure Capable of producing spherical gold nanoparticles of around 10-20 nm in diameter Method first developed by J. Turkevich in 1951 and later refined by G. Frens

Image courtesy: Chiwoo Park

SYNTHESIS PROCESSES
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Inert Gas Condensation Process: Components: Metal (of desired nanoparticles), inert gas, vacuum vessel, nanoparticle-collection finger, liquid nitrogen for cooling Process: See diagram Typically results in a broad particle size distribution due to random nature of the process Basic IGC process leads to several variants, one variant, being physical vapor synthesis process

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Images adopted from Nanomaterials: An introduction to synthesis, properties, and applications by Dieter Vollath

SYNTHESIS PROCESSES
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Laser Ablation Process: Components: precursor target (metal or non-metal), high-power laser, optical focusing system, carrier gas, vacuum vessel, feeding system for precursor target Process: See figure More versatile than physical vapor synthesis because both, metals and non-metals can be used as targets Particle size depends on: i. gas pressure and ii. Laser pulse length Results in a broad particle size distribution

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Image adopted from Nanomaterials: An introduction to synthesis, properties, and applications by Dieter Vollath

CHARACTERIZATION OF NANOPARTICLES
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What is characterization? Characterization refers to study of materials features such as its composition, structure, and various properties like physical, electrical, magnetic, etc. Why is characterization of nanoparticles important? Nanoparticle properties vary significantly with size and shape Accurate measurement of nanoparticles size and shape is, therefore, critical to its applications Tools used to characterize nanoparticles
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CHARACTERIZATION OF NANOPARTICLES
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i. ii. iii. i. ii.

Scanning Probe Microscopy: Uses some type of probe that generates an image by physically scanning the sample surface in a raster scan pattern Depending on the type of microscope, several different surface characteristics can be analyzed Probe microscopes: Atomic Force Microscope Scanning Tunneling Microscope Near-field Scanning Optical Microscope Other microscopes: Transmission Electron Microscope Scanning Electron Microscope

CHARACTERIZATION OF NANOPARTICLES
i. ii. iii. -

Atomic Force Microscope: Operation: See figure Modes of operation: Contact mode Non-contact mode Tapping mode Image source: http://sahussain.files.wordpress.com/2007/11/fig-1.jpg Limitations: Probe tip radius, image processing speed, small image size Advantages: High resolution microscope (upto few nanometers), capable of producing 3-D images, pre-treatment of samples is not necessary, vacuum chamber 10 not required for some modes of operation
Image source: http://mcf.tamu.edu/images/IMG_0750.jpg/image

CHARACTERIZATION OF NANOPARTICLES
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Scanning Tunneling Microscope: Operation: Based on tunneling current, which is explained in quantum physics Modes of operation: i. Constant-current ii. Constant-distance Advantages: Very high image resolution (capable of seeing and manipulating atoms), wide temperature range and capable of operating in ultra-high vacuum and other gas environments Limitations: Again, radius of curvature of tip, extremely sensitive to ambient vibrations

Image source: http://www.almaden.i bm.com/vis/stm/imag es/stm10.jpg

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Image source: http://www.nisenet.org/publicbeta/articles/seeing_atoms/images/STMmed.jpg

CHARACTERIZATION OF NANOPARTICLES

Transmission Electron Microscope: Operation: Image is generated based on the interaction pattern of electrons that transmit through the specimen Variation: Scanning Transmission Electron Microscope Advantages: Additional analysis techniques like X-ray spectrometry are possible with the STEM, highresolution , 3-D image construction possible but aberrant Limitations: Needs high-vacuum chamber, sample preparation necessary, mostly used for 2-D images

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Image source: http://www.udel.edu/biology/Wags/histopage/illuspage/lec1/iintro9.gif

CHARACTERIZATION OF NANOPARTICLES
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Scanning Electron Microscope: Operation: Generates image by scanning the surface of the sample in a raster pattern, using an electron beam Modes of operation: i. Secondary electrons ii. Back-scattered electrons (BSE) iii. X-rays Advantages: Bulk-samples can be observed and larger sample area can be viewed, generates photo-like images, very high-resolution images are possible Disadvantages: Samples must have surface electrical conductivity, nonconductive samples need to be coated with a conductive layer

Image: http://www.engineering.a rizona.edu/news/media/i mage/matsci_pollen.jpg

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Image source: http://www.bioimaging.dk/uploads/pics/Scanning-electronmicroscop_03.gif

CURRENT RESEARCH
Challenges: Accurate characterization of nanoparticles is very critical to study their properties. Image analysis is very tedious and current methods are not robust, which reduces their compatibility. Faster, robust, and more accurate methods need to be developed Two methods: i. Remove white areas by identifying and eliminating those data points that correspond to a specific threshold pixel brightness value ii. Attempt to identify closed particle boundaries and eliminate data points that lie within those closed boundary and those which do not form a closed entity

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