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    Infrastructure

    Nanotechnology Laboratory

  • img

    Infrastructure

    Nanotechnology Laboratory

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    Infrastructure

    Nanotechnology Laboratory

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    Infrastructure

    Nanotechnology Laboratory

NANO CHARACTERIZATION LABORATORY

 

X-ray diffraction (XRD)

 

Model                         : D2 Phaser

Manufacturer              : BRUKER

 

X-ray diffraction (XRD) is an instrumental technique to study crystalline materials. On diffraction of the X-ray beam from the sample, the distances between the planes of the atoms constituting the sample can be obtained by applying the Bragg's law

 

 

Application:

 

·         Identification of unknown crystalline materials

·         Characterization of crystalline materials

·         Determination of crystal structures using Rietveld refinement

·         Thin film characterization

 

 

Scanning Probe Microscopy (SPM)

 

Model                         : XE70

Manufacturer              : Park Systems

Modes                        : AFM (Atomic Force Microscopy),

                                     MFM (Magnetic Force Microscopy),

                                     STM (Scanning Tunneling Microscopy)

Sample State              : Solid, Powder, Thinfilm, Liquid

 

Principle:

 

All of the techniques are based upon scanning a probe (typically called the tip in STM , since it literally is a sharp metallic tip) just above a surface whilst monitoring some interaction between the probe and the surface.

 

STM - is the tunnelling current between a metallic tip and a conducting substrate which are in very close proximity but not actually in physical contact.

 

AFM - is the van der Waals force between the tip and the surface; this may be either the short range repulsive force (in contact-mode) or the longer range attractive force (in non-contact mode).

 

MFM – is similar to AFM, but the tip is magnetized.

 

Applications:

 

     Topography of different surfaces

     Magnetic samples

     Electrical properties

 

Fourier Transform Infrared (FTIR) Spectrophotometer

 

Model                         : Alpha T

Manufacturer              : Bruker

Spectral Coverage      : 500 to 4000 cm-1

Resolution                  : 0.9 cm-1

Modes                        : Transmission and ATR

Sample State              : Liquid, Powder, Thinfilm and Solid

 

Principle:

 

Infrared spectroscopy is based on the principle that molecules will absorb specific frequencies of light that match the vibrational electronic transitions of the molecule.  Once the sample is placed in the instrument, a beam of light is passed through the sample.  The intensity of the light transmitted through the sample is compared to that of the incident light at each frequency.  In FTIR, all frequencies of the incident radiation pass though the sample at the same time.  Fourier transform is the technique used to process the raw data to present it in a way that is more easily interpreted.

 

Spectra can be obtained in transmission mode with traditional sample cells.  However, attenuated total reflectance (ATR) mode is also commonly used.  In this method, light is passed through a waveguide that is in contact with the sample.  ATR is particularly useful for analysis of liquids, insoluble compounds and other materials that are not easily made into thin films.

 

The microscope accessory allows for the collection of IR spectra from specific points on surfaces.  It can operate in transmission, reflectance or ATR mode, and sampling of multiple areas of a surface can be automated.

 

Applications:

 

            FTIRspectroscopy can be used for both qualitative and quantitative applications.

 

     Identification of simple mixtures of organic and inorganic compounds both as solids or liquids.

     Identification of polymers and polymer blends.

     Indirect verification of trace organic contaminants on surfaces.

     Thin film analysis.

     Analysis of adhesives, coatings and adhesion promoters or coupling agents.

     Small visible particle chemical analysis.

     Analysis of stains and surface blemishes remnant fromcleaning and degreasing processes combined with optical microscopy, SEM/EDX, XPS and SIMS techniques.

     Analysis of resins, composite materials and release films .

     Solvent extractions of leachables or contaminants, plasticisers, mould release agents and weak boundary layers coupled with XPS surface chemical analysis techniques.

     Identification of rubbers and filled rubbers.

     Determination of degrees of crystallinity in polymers (eg LDPE and HDPE).

     Compararive chain lengths in organics.

     Extent of thermal, UV or other degredation or depolymerisation of polymers and paint coatings.

     Analysis of a gaseous samples using a gas cell for headspace analysis or environmental monitoring.

     Analysis of unknown solvents, cleaning agents and detergents.

 

Raman Spectrophotometer

 

Model                         : EzRaman-N-Analyzer

Manufacturer              : EnWAVE Optronics

Laser                           : 785 nm

Spectral Coverage      : 100 to 3200 cm-1

Sample State              : Liquid, Powder, Thinfilm and Solid

 

Principle:

 

Raman spectroscopy provides information about molecular vibrations that can be used for sample identification and quantitation. The technique involves shining a monochromatic light source (i.e. laser) on a sample and detecting the scattered light. The majority of the scattered light is of the same frequency as the excitation source; this is known as Rayleigh or elastic scattering. A very small amount of the scattered light (ca. 10 to 5% of the incident light intensity) is shifted in energy from the laser frequency due to interactions between the incident electromagnetic waves and the vibrational energy levels of the molecules in the sample. Plotting the intensity of this "shifted" light versus frequency results in a Raman spectrum of the sample. Generally, Raman spectra are plotted with respect to the laser frequency such that the Rayleigh band lies at 0 cm-1. On this scale, the band positions will lie at frequencies that correspond to the energy levels of different functional group vibrations. The Raman spectrum can thus be interpreted similar to the infrared absorption spectrum.

 

Applications:

 

Raman spectroscopy can be used for both qualitative and quantitative applications.  Given below is the list of Raman Application areas.

 


Pharmaceuticals and Cosmetics

     Compound distribution in tablets

     Blend uniformity

     High throughput screening

     API concentration

     Powder content and purity

     Raw material verification

     Polymorphic forms

     Crystallinity

     Contaminant identification

     Combinatorial chemistry

     In vivo analysis and skin depth profiling

 

Geology and Mineralogy

     Gemstone and mineral identification

     Fluid inclusions

     Mineral and phase distribution in rock sections

     Phase transitions

     Mineral behaviour under extreme conditions

 

Carbon Materials

     Single walled carbon nanotubes (SWCNTs)

     Purity of carbon nanotubes (CNTs)

     Electrical properties of carbon nanotubes (CNTs)

     sp2 and sp3 structure in carbon materials

     Hard disk drives

     Diamond like carbon (DLC) coating properties

     Defect/disorder analysis in carbon materials

     Diamond quality and provenance

 

Semiconductors

     Characterisation of intrinsic stress/strain

     Purity

     Alloy composition

     Contamination identification

     Superlattice structure

     Defect analysis

     Hetero-structures

     Doping effects

     Photoluminescence micro-analysis

 

Life Sciences

     Bio-compatibility

     DNA/RNA analysis

     Drug/cell interactions

     Photodynamic therapy (PDT)

     Metabolic accretions

     Disease diagnosis

     Single cell analysis

     Cell sorting

     Characterisation of bio-molecules

     Bone structure


 

Particle Size Analyzer

 

Model                         : DC12000

Manufacturer              : CPS Instruments

Laser                           : 785 nm

Particle Size Range    : 0.01 to 40 micron

Sample State              : Liquid and Powder

Max. Disk Speed        : 12,000 RPM

 

Principle:

 

The CPS Disc Centrifuge separates particles by size using centrifugal sedimentation in a liquid medium. The sedimentation is stabilized by a slight density gradient within the liquid.

 

The particles sediment within an optically clear, rotating disc. When particles approach the outside edge of the rotating disc, they block/scatter a portion of a light beam that passes through the disc. The change in light intensity is continuously recorded, and converted by the operating software into a particle size distribution.

 

Applications:

 


Chemical

     Polymer latexes and emulsions

     Fillers (CaCO3, clay, barites, etc.)

     SiO2 dispersions

     Abrasives (of all types)

     Impact modifier particles

     Oil emulsions

 

Pharmaceutical

     Virus particles/virus-like particles

     Cells (culture) and cell fragments

     Protein clusters

     Liposome's

     Particles in diagnostic tests

     Micro-encapsulated drugs

 

Semiconductor

     Micro-abrasives

     CMP compounds for integrated circuits

 

Printing and Painting

     Pigments - water and oil based

     Micro-fiber paint viscosity modifiers

     Printer/copier toner powders

     Inkjet inks

     Carbon black

     Magnetic iron oxide

 

Others

     Micro-spheres

     Agglomeration patterns

     Starch/flour particles


 

Thermogravimetric/Differential Thermal Analyzer (TG/DTA)

 

Model                         : Exstar 6300

Manufacturer              : SII NanoTechnology

Temperature Range    : Room Temp. to 1300 ºC

Sample State              : Solid, Thinfilms and Powder

 

Overview:

 

The TG/DTA is a simultaneous measurement instrument combining TG, which utilizes a horizontal differential type balance beam, with the highly flexible DTA feature. This instrument is used for reaction velocity and acceleration degradation tests, as well as analysis of the water and ash content in samples, and evaluation of decomposition, oxidation and heat resistance of samples.

 

Applications:

 

     Compositional analysis

     Decomposition and Transition temperatures

     Filler content

     Heat of Transition

     Measurement of volatiles (e.g. Water, oil)

     Oxidative and Thermal stabilities

 

UV-Vis Spectrophotometer

 

Model                         : 2202

Manufacturer              : Systronics

Spectral Coverage      : 200 to 1100 cm-1

Sample State              : Transparent Thinfilms, Liquid and Powder

 

Principle:

 

            Molecules containing π-electrons or non-bonding electrons (n-electrons) can absorb the energy in the form of ultraviolet or visible light to excite these electrons to higher anti-bonding molecular orbitals. The more easily excited the electrons (i.e. lower energy gap between the HOMO and the LUMO), the longer the wavelength of light it can absorb.Based on the fact of four type of transition- π-π*,n-π*,σ-σ*,n-σ*.The energy required for various transitions obey the following order σ-σ*>n-σ*>π-π*>n-π*.

 

            Ultraviolet and visible (UV-Vis) absorption spectroscopy is the measurement of the attenuation of a beam of light after it passes through a sample or after reflection from a sample surface. Absorption measurements can be at a single wavelength or over an extended spectral range. It works on the principle of beer and lambert's law.

 

Applications:

 

1.      Detection of Impurities

UV-Vis absorption spectroscopy is one of the best methods for determination of impurities in organic molecules. Additional peaks can be observed due to impurities in the sample and it can be compared with that of standard raw material. By also measuring the absorbance at specific wavelength, the impurities can be detected.

 

2.      Structure elucidation of organic compounds

UV-Vis spectroscopy is useful in the structure elucidation of organic molecules, the presence or absence of unsaturation, the presence of hetero atoms.

From the location of peaks and combination of peaks, it can be concluded that whether the compound is saturated or unsaturated, hetero atoms are present or not etc.

 

3.      Quantitative analysis

UV-Vis absorption spectroscopy can be used for the quantitative determination of compounds that absorb UV/Vis radiation. This determination is based on Beer’s law.

 

4.      Qualitative analysis

UV-Vis absorption spectroscopy can characterize those types of compounds which absorbs UV/Vis radiation. Identification is done by comparing the absorption spectrum with the spectra of known compounds.

UV-Vis absorption spectroscopy is generally used for characterizing aromatic compounds and aromatic olefins.

 

5.      Thickness measurements of Thinfilms.

 

Electrochemical Workstation

 

Model                         : 604D

Manufacturer              : CH Instruments, Inc.

 

Techniques                  : Cyclic Voltammetry

                                     Linear Sweep Voltammetry

                                     TAFEL

                                     Chronoamperometry

                                   Chronocoulometry

                                     Bulk Electrolysis with Coulometry

                                     Impedance

                                     Impedance-Time

                                     Impedance-Potential

                                     Open Circuit Potential-Time

 

Electrodes                  : Platinum Wire Electrode

                                     Platinum Working Electrode

                                     Glassy Carbon Working Electrode

                                     Ag/AgCl Reference Electrode

                                     Non-Aqueous Ag/AgCl Reference Electrode

                                     Calomel Reference Electrode

 

Bet Surface Area Analyzer

 

Model                         : Smart Sorb

Manufacturer              : Smart Instruments Company Pvt. Ltd.

Measurement Modes  : Surface Area and Pore Size

Sample State              : Powder

 

Principle:

            Bet Surface Area Analyzer is used for surface area measurement. Surface Area is an Intrinsic property of powdered porous materials that can reveal important information regarding the usefulness of a material for an application, Surface area plays critical role in the bio-availability of Pharmaceuticals, dispersion of dyes, adsorption capacity of carbon and many more.

 

By means of Physical adsorption. Surface Area can be calculated since physically adsorbed molecules are not restricted to specific sites and are free to cover the entire Surface. This process is reversible. Typically nitrogen gas is adsorbed at cryogenic temperatures (liquid nitrogen). Based on the amount of gas adsorbed (adsorbate) at a given pressure, the BET equation is used to calculate the number of adsorbed gas molecules that would be required to form a mono layer on the surface. With knowledge of the cross - sectional area of the gas molecule adsorbed, the Surface Area can be easily calculated.

 

Smart Sorb 93, Surface Area Analyzer is based on dynamic BET principle. Nitrogen gas is used for adsorption. The dynamic flow method uses a high sensitive thermal conductivity detector to measure the change in the concentration of an adsorbate / carrier gas mixture during adsorption or desorption process. It determines the surface area at single point and it can be enhanced for measuring multi point surface area and total pore volume analysis with different gas mixture percentage.

 

Applications:

 

     Pharmaceuticals – Surface area and porosity play major roles in the purification, processing, blending, tableting, and packaging of pharmaceutical products as well as the drug’s useful shelf life, its dissolution rate, and bio-availability.

     Ceramics – Surface area and porosity affect the curing and bonding of greenware and influence strength, texture, appearance, and density of finished goods. The surface area of glazes and glass frits affects shrinkage, crazing, and crawling.

     Adsorbents – Knowledge of surface area, total pore volume, and pore size distribution is important for quality control of industrial adsorbents and in the development of separation processes. Surface area and porosity characteristics affect the selectivity of an adsorbent.

     Activated Carbons – Surface area and porosity must be optimized within narrow ranges to accomplish gasoline vapor recovery in automobiles, solvent recovery in painting operations, or pollution controls in wastewater management.     

     Carbon Black – The wear lifetimes, traction, and performance of tires are related to the surface area of carbon blacks used in their production.

     Catalyst – The active surface area and pore structure of catalysts influence production rates. Limiting the pore size allows only molecules of desired sizes to enter and exit, creating a selective catalyst that will produce primarily the desired product.

     Paints and Coatings – The surface area of a pigment or filler influences the gloss, texture, color, color saturation, brightness, solids content, and film adhesion properties. The porosity of a print media coating is important in offset printing where it affects blistering, ink receptivity, and ink holdout.

     Projectile Propellant – The burn rate of propellants is a function of surface area. Too high a rate can be dangerous; too low a rate can cause malfunctions and inaccuracy.

     Medical Implants – Controlling the porosity of artificial bone allows a better imitation of real bone that is more acceptable to the body for tissue growth.

     Cosmetics – Surface area is often used by cosmetic manufacturers as a predictor of particle size when agglomeration tendencies of the fine powders make analysis with a particle-sizing instrument difficult.

     Aerospace – Surface area and porosity of heat shields and insulating materials affect weight and function.

     Electronics – By selecting high surface area material with carefully designed pore networks, manufacturers of super-capacitors can minimize the use of costly raw materials while providing more exposed surface area for storage of charge.

     Fuel Cells – Fuel cell electrodes require high surface area with controlled porosity to produce adequate power density.

     Geoscience – Porosity is important in groundwater hydrology and petroleum exploration because it relates to the quantity of fluid that a structure can contain as well as how much effort will be required to extract it.

 

RESEARCH FACILITIES

charge’s for testing & analysis

 

 

Sl.No.

Testing & Analysis

Purpose

Technique /Parameter

(Default)

Rate/Sample (D.R)

External

Internal

1

Atomic Force Microscopes

Surface roughness

Non-Contact Mode

Rs. 4000

Rs. 3500

5 x 5 µm - Area

0.5 Hz – Scan Rate

2

TG & DTA

Thermal Analysis

30 ⁰C– 800  ⁰C - Range

Rs. 750

Rs. 500

25 ⁰C – Heating rate

N2, Air – Atm.

3

UV

Absorption, Transmittance

200 – 800 nm, medium scan

Rs. 200

Rs. 100

4

FTIR

Chemical Functional groups identifications

ZnSe optics

550 cm-1 to 4000cm-1

Rs. 200

Rs. 100

5

Particle Size Analyser

Size distribution

Centrifugal force

Rs. 500

Rs. 400

6

Surface Area Analyser

Surface Area & Pore Volume

BET method

Rs. 800

Rs. 500

7

Electrochemical

Analysis

I-V, Redox, Chemical sensing

Three electrode system

Rs. 500

Rs. 300

8

Raman

vibrational, rotational

785 nm laser & Probe

Rs. 200

Rs. 100

9

Ball-Mill

Size Reduction

Planetary

Wet & Dry

Rs. 500

(4 hr.)

Rs. 300

(4 hr.)

10

XRD

Crystalline Structure

2 theta 10⁰ – 80⁰

Rs.500

Rs.250

D.R = Default Rate

 

 

 

 

Contact Details:

 

Dr. R. S. Rimal Isaac,

In-Charge - Nano Characterization Laboratory (NCL),

Department of Nanotechnology,

Noorul Islam Centre for Higher Education (NICHE),

Kumaracoil, Thuckalay, Kanyakumari District, Tamilnadu - 629 180.

Phone: 94433 14203