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Material synthesis and characterization
Materials:
All the materials in this world are made of using one or more elements of the periodic table. They can be
classified based on either of its mechanical properties (Elastic, Non-elastic, Ductile and Brittle), electrical
properties (metals, semiconductors, and insulators), Magnetic properties (Ferro magnets, anti-ferro magnets,
Ferri magnets, Para magents and Dia magnets), Dielectric properties (Polarization), thermal properties etc. The
property of a certain material changes when its dimensions are changed. Based on the size of the materials, they
can be classified into 4 types :
Bulk materials : As such
2D materials (one of its dimensions is less than 100 nm): Thin films
1D materials (two of its dimensions is less than 100 nm): Nanotubes, Nanowires, Nanosheets, Quantum wires
0D materials (less than 100 nm in all directions): Quantum Dots, nanoparticles
Most of the materials can be fabricated into all the above said dimensions. Depending on the size of the
materials, their properties will be changed, and so depending on the applications one can choose the dimension
of the materials. The cause and effect of various properties with decrease in a size of material is discussed in
detail in the other chapters. In this chapter, I will discuss the available fabrication techniques to manufacture
various nanomaterials. With decrease in size of the materials, characterizing the same gets difficult. Here, I will
also mention basic principles of few of the various available characterization techniques.
These nanomaterials can be fabricated either by using physical methods or chemical (wet) methods. In the
physical methods, one can follow either top-down approach or bottom-up approach. Top-down approach is
nothing but breaking/etching the bulk materials until its dimensions are reduced to nano-size. Bottom-up
approach is called when the structures are built by assembling atom by atom to the required size.
Fabrication Techniques:

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Material synthesis and characterization | whynano 2 of 8 https://whynano. However.com/st/chemistry/lithography/process/ http://www. There are several techniques available to etch the substrates depending on the purpose. Apply (e-beam /photo) Resist 3.com/material-synthesis-and-characterization/ Top-down approach: The top-down approach is a well matured technology commonly used in the field of micro-electronics. which I will mention briefly in this chapter..memsnet.almaden. Etching (either Dry or Chemical) and metal deposition. Soft-lithography is commonly used in the biological fields to make microfluidics etc. http://www. is described in the chapter Bio-Nanotechnology. the constraints with morphology and the cost.ibm. Cleaning the wafer 2. laser interferometer lithography. Electron beam Lithography. Depending on the resolution aiming for.org/news/ The steps involved in the Lithography process are: 1. and nano-imprint lithography. one can chose from several lithographic techniques available such as Photo Lithography. there exists also other techniques such as so-called soft-Lithography. Expose pattern 4. The most important steps involved in this process are Lithography.wordpress. Develop film  Follow 12-May-16 11:45 AM .

This technique has been extensively studied by Fukui’s group in Japan using MOVPE deposition technique []. One can also choose ultrasonic baths to clean the wafer by using acetone followed by ethanol and blow dry with N2/ spin dry. Molecular beam epitaxy:  Follow 12-May-16 11:45 AM .com/material-synthesis-and-characterization/ 5. and MBE etc. Recently. Au has been traditionally used as a catalyst particle for the growth of NWs. The most commonly used bottom-up approach techniques to fabricate 2-D materials such as NWs. Fontcuberta’s group in Germany/Switzerland has demonstrated the growth of GaAs NWs by Ga-assisted VLS growth technique using MBE deposition method . Bottom-up approach: Bottom-up approach has become a choice for wide range of materials due to the limitations of the capabilities of the techniques used in top-down approach such as lithography. The most commonly used bottom-up approach methods to fabricate 2D materials such as thin films are CVD. MOVPE. The III-V materials deposited on such substrates lead to the growth of NWs from the holes in the SiO2 layer.. PLD. In some cases. Please note that ethanol should be dispensed on the substrate well before the acetone dries. and oxide assisted growth (OAG). The other commonly used growth technique for NWs is so-called VLS growth technique which uses metal particle as a catalyzing agent aiding the growth of the NWs. one should not let acetone dry on the sample by itself. the catalyst particles remains solid(S) and is so called VSS process. vapor-liquid-solid (VLS). The process of depositing different materials with different band gaps on each other epitaxially is called heteroepitaxy. Resist: There are two types of resist negative or positive resist. which leaves the residual marks on the substrate and is difficult to clean. Etching / Metal deposition Cleaning the wafer: Most of the wafers are cleaned by rinsing it with acetone followed by ethanol and blown dry with N2. In other words. and hence also called as Au-assisted VLS growth technique. and has attracted attention of few other groups who demonstrated to fabricate In-assisted InAs NWs and also the growth of these NWs on cheap substrates such as silicon. and such structures are called heterostructures.wordpress. whereEpitaxy is a process in which the deposited film adapts the crystal phase and orientation identical to those of the substrate. The SAE technique uses a 30 nm thick SiO2 layer deposited on the (111)B oriented substrates followed by opening holes in the SiO2 layer.Material synthesis and characterization | whynano 3 of 8 https://whynano. VLS process is so called because the material is supplied in vapor (V) form to the catalyst particle which is liquid (L) and results in the NW which is of solid (S) form. vaporsolid-solid (VSS). and nanotubes are using growth mechanisms such as selective area epitaxy (SAE).

magnetic.1 ML/s can be achieved by changing the temperatures of the effusion cells. mass spectrometer. ion pump.wordpress. In addition. arrangement of atoms (crystal structure).  Follow 12-May-16 11:45 AM . a flux of molecules or atoms towards the substrate can be abruptly released (closed) by controlling the shutter in front of the cell. Structural characterization involves determining the morphology (Shape and size) of nanomaterials. Characterization techniques: Characterization of nanomaterials involve determining the structural. So. Performing the deposition in UHV chamber not only makes it possible to grow highly pure materials but also to install in-situ characterization techniques such as reflection high energy electron diffraction (RHEED). and material composition of nanomaterials. the mean free path of elements evaporating from the furnaces will be very high which leads to no collisions until they reach the sample surface. depending on their applications. and mechanical properties. deposition rates of as low as 0. epitaxial films of a wide variety of materials []. electrical. MBE is one of the most versatile and widely used non-equilibrium growth techniques for growing thin. optical.com/material-synthesis-and-characterization/ Schematic drawing of the current MBE growth chamber at NTNU. Optical characterization involves determining the light emission and light absorption characteristics of the structures. and viewports are not included in the drawing. Only four of the effusion cells are included in the drawing. This allows growing heterostructures with abrupt interfaces. Ti-ball. More details about the light emitting materials and their properties has been discussed in the Nano-photonics page.Material synthesis and characterization | whynano 4 of 8 https://whynano. The deposition of material on the substrate is performed by evaporating the material from the effusion cells in a chamber maintained under ultrahigh vacuum (UHV). Due to the presence of UHV in the chamber.

the EDS equipped with SEM enables to determine the composition also by SEM although with less resolution compared to that of TEM. electrons scatter in different directions as shown in Fig. compared to μm for light microscopy. ~2 – 3 Å for conventional TEMs because of the aberrations in the lens system used in TEM. highlighting the basic difference between them. The schematic diagrams of SEM and TEM is shown in the Fig. TEM generates the image by detecting the electrons transmitted through the specimen. crystal defects and crystal composition. The wavelength (λ) of electron beam depends on the energy of the electron beam. the spatial resolution of TEM. BCC..matter. while TEM is used to investigate the crystal structure. in the ~nm-Å range.6. chiral number of CNTs Electron Microscopy: The most common technique used to determine the structural properties of the nano materials is by using electron microscopes. and so the TEM sample should be thin enough allowing the electron beam to pass through the sample. An electron microscope is a technique that uses an electron beam to illuminate a specimen and create a highly-magnified image.uk/tem/]. RECIPROCAL SPACE. and FCC.22/E^1/2 giving a λ of only 4 pm for 100 keV electrons. The most common crystal structures are SCC. and to check the abruptness of the interface of heterostructure materials. SEM generates the image by detecting the electrons scattered above the surface of a specimen. However. When an electron beam interacts with a specimen. SEM is commonly used for determining the morphology and distribution of nanomaterials. Determining the crystal structure. spherical aberration can be found else where [http://www. due to the lower wavelengths of electron beam (resolution ~ half of the wavelength). which uses the electron beam energy of 300 keV is worse than this. λ = 1.com/material-synthesis-and-characterization/ Crystal Structure: Crystal structure of any material indicates the pattern in which atoms are arranged.wordpress. More details about the lens aberrations which includes chromatic aberration.  Follow 12-May-16 11:45 AM . 3.org.Material synthesis and characterization | whynano 5 of 8 https://whynano. Of course. The advantage of using electrons instead of light is that the better resolution can be achieved.

The simplest SPM technique is Atomic Force Microscopy (AFM).mcgill. viscoelastic response.matter.com/material-synthesis-and-characterization/ http://barrett-group. and measuring its deflection.).wordpress. etc. Variations of the technique allow different aspects of the surface to be mapped out (such as density. http://barrett-group.mcgill. magnetic behavior. depth of focus. More details about the TEM can be found in http://www.htm Fluorescence Microscopy:  Follow 12-May-16 11:45 AM . This allows the topography of the surface to be mapped out.Material synthesis and characterization | whynano 6 of 8 https://whynano. density of electronic states.org.ca/teaching/nanotechnology/nano02.htm Some of the important terms the electron microscopy users usually know is resolution.ca/teaching/nanotechnology/nano02.com/ Scanning Probe Microscopy: Scanning probe microscopy (SPM) involves running a nanometre-sized probe along a surface.uk/tem/ and the latest developments in the TEM field can be found in http://superstem.

wordpress. emitted light has a longer wavelength. it is possible for one electron to absorb two photons. and therefore lower energy. (fluorescein or DyLight 448) enhances the contrast. Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation of a different wavelength. The technique has made it possible to identify cells and cellular components with a high degree of specificity. The most striking examples of fluorescence occur when the absorbed radiation is in the ultraviolet region of the spectrum and thus invisible.com  Follow 12-May-16 11:45 AM . and the emitted light is in the visible region.mccronemicroscopes. However. when the absorbed electromagnetic radiation is intense. For example. than the absorbed radiation. certain antibodies and disease conditions or impurities in inorganic material can be studied with the fluorescence microscopy. this two-photon absorption can lead to emission of radiation having a shorter wavelength than the absorbed radiation.Material synthesis and characterization | whynano 7 of 8 Fluorescence microscopy is https://whynano.fluorescence microscope (colloquially synonymous with epifluorescence microscope) is an optical microscope used to study properties of organic or inorganic substances using the phenomena of fluorescence and phosphorescence instead of. In most cases.com/material-synthesis-and-characterization/ a rapid expanding technique. both in the medical and biological sciences. Suppliers of Fluorescence microscope: http://www. reflection and absorption [Wiki]. The samples to be inspected are labelled with fluorescent molecules such as fluorophore (such as green fluorescent protein (GFP). or in addition to.

Nobel Laureates who discovered different materials: Name of Laureate Discovered Herbert Kroemer Year of winning Nobel prize Quantum wells 2000 Charles K. Solid-State Electronics Volume 21. LANG and C. George E.Material synthesis and characterization | whynano 8 of 8 https://whynano. Smith CCD camera 2009 A. whynano The Twenty Ten Theme.attocube.com/material-synthesis-and-characterization/ http://www. V. Boyle.  Follow 12-May-16 11:45 AM .com/ Scanning Near Optical Microscopy: Suppliers of Scanning Near Optical Microscopy: http://www. Geim and Novoselov Graphene 2010 Be the first to like this.com.com/ Scanning Photocurrent Microscopy (SPCM): References: D. Kao Optical Comm. Issues 11-12. Pages 1519. 2009 Willard S. Blog at WordPress. H. 1978.fluorescence-microscopes. HENRY.wordpress.