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Introduction to Nanotechnology

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ShriNRPrasad

1) Green synthesis of metals and metal oxide nanoparticles using plants and microorganisms provides an environmentally friendly approach for applications such as environmental remediation. 2) Nanoparticles exhibit different properties than bulk materials due to their high surface to volume ratio and quantum effects at the nanoscale. Their properties can be controlled through the capping agent used during synthesis. 3) Nanoparticles have many applications including in medicine, sensors, energy storage and more. Their small size allows for targeted drug delivery and improved efficacy of treatments.

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Green sysnthesis of Metals and their Oxide Nanoparticles: Application for Environmental Remedation. Dr Rai Dhirendra Prasad Bihar Veterinary College, Patna, India Col Amit Sinha SPPU, Pune, India 1
2 PART I What Is Nanotechnology?
“Nanotechnology is the art and science of manipulating matter at the nanoscale”
Nanotechnology in Ancient Period  Ras-Ratnakar: described the formation of metallic nanoparticles about 5000 years ago Shodhan: purification Maran: killing the metallic properties  Alchemist- Aurum potable & Luna potable about 1570  Dr Samuel Hahnemann- Organon of medicines  Lycurgus Cup: 4th century AD 4
History The idea of nanotechnology was born in December 29, 1959 when physicist “Richard Feynman” gave a lecture exploring the idea of building things at the atomic and molecular scale. He is regarded as Father of Nanotechnology and given the Famous statement “There is plenty of Room at the bottom” He imagined the entire Encyclopedia Britannica written on the head of a pin.
Nanoparticles  "A particle with the size of the order of 1-nm to 100nm in any dimension and at least any one property different from that of bulk".  During the synthesis of nanoparticles, size of nanoparticles depends on the steochiometric ratio of metal ion to capping ligands concentration. 6
Properties at nanoscale  Properties of nanoparticles: depend upon size, shape, stabilizing agent, method of preparation etc.  Changes in optical, thermal, electrical, electronic, magnetic and mechanical properties 7
Melting Point  Graph of melting point (Tm) vs size of particle (D)  Melting point of nanoparticles is below the melting point of bulk material Tm= TmBulk (1-1/D) 8
Optical Property  Size dependent optical properties of gold nanoparticles  This effect appears due to the interaction of electro- magnetic radiation with the electron cloud present on the surface of metal nanoparticles 9
Surface Plasmon Resonance  Surface Plasmon oscillations.  Large number of atoms present on the surface of nanoparticles contributes electron cloud which interacts with E-field of light and thus oscillates 10
Electronic Property  When the size enters nano level, electron motion is restricted to a smaller space, they don’t follow classical theory & restricts themselves from diffusion of valence and conduction band.  The energy gap between valence band and conduction bond (Kubo gap) becomes larger than thermal energy (KBT) and hence metallic nanoparticles become semiconductor further becomes an insulator 11
Other Properties  Magnetic Property: Bulk materials forms multiple magnetic domains, but nanoparticles form only a single magnetic domain thus could be used for super magnetism.  Bio-compatibility:  Electrical Properties: The metals that are good conductance behave as semiconductor at nano-level. 12
Property changes…  opaque substances become transparent (copper)  stable materials turn combustible (aluminum)  insoluble materials become soluble (gold)  Chemically inert becomes active (Gold) 13
Why different property at Nanoscale • High Surface to Volume ratio (Aspect ratio) : Because of this the nanoparticle become less stable .  Gravitational force: is not effective  Size comparable to wavelength of light: thus entire different optical properties like Surface Plasmon Resonance is exhibited.  Dangling bonds: 14
Surface to Volume Ratio  spherical particle,  surface area = 4πr2 and volume = 4/3 π r3  Sp= 4πr2σ/ (4/3)πr3ρ  Where, σ is surface area factor and ρ is volume factor  r→o , Sp→∞ 15
Quantum mechanics  Nanoparticles do not obey the laws of classical mechanics; instead they follow the principles of quantum mechanics.  Exhibits interesting shape dependence due to electronic motion in different dimensions. 16
Example of shape dependent property  Electronic tunneling phenomenon is observed for 0-D nanostructures which is the key concept used for building artificial atoms and devices like single electron transistors.  Electron can oscillate in two distinct ways in 1-D nanostructures under electromagnetic field, namely in longitudinal and transverse modes. The way electrons executes its motion alters their various properties and thus nano-rods and nano-tubes give rise to Surface Plasmon absorption peaks due to the two different types of electronic motion. 17
Nanoparticles as Smart Material:  Smart materials are the materials that respond favorably to change in temperature, pH, moisture or electromagnetic fields thus are extensively used as sensors and actuators.  Nanoparticles can also be used as advanced engineering materials which can withstand high temp, high impact, 18
Nano-composites  Light weight Nano composites can replace heavy metals in automobile industry to achieve high speed in vehicles  Nano-composites are actively used to enhance the efficiency of solar cells, and also in superconductor and super capacitors 19
Introduction to Nanotechnology
Norio Taniguchi  The term "nanotechnology" was defined by Tokyo Science University Professor Norio Taniguchi in a 1974 paper as follows: "'Nanotechnology' mainly consists of the processing, separation, consolidation, and deformation of materials by one atom or by one molecule." 21
Stabilization of Nanoparticles  Tendency to form agglomeration:  Stabilizing agent: usually accomplished by suitable passivating agents also called as capping agent. 22
Gibb’s Free Energy & Stability  As size of the nanoparticles decreases their surface energy increases.  Increase in the surface energy results in increase in the Gibb’s free energy.  According to the law of thermodynamics, every system always tries to attain minimum Gibb’s free energy  Therefore it loses its nanoness and exotic properties related to it. Hence it is very important to stabilize the nanoparticles against the aggregation. 23
24 Electrostatic Stabilization
Potential energy vs distance between the nanoparticles  Particles formed are surrounded by the electronic double layer of reactant ions on the surface of nanoparticles  Two forces: Van der Waals forces of attraction , and electrostatic force of repulsion due to the charged ions on the surface.  Stability of nanoparticles is dependent on the combined effect of these two forces.  Greater the thickness of the double layer, higher is the potential energy barrier & higher is stability 25
26 Different Capping agents used for Surface Modification & Stabilization
Surface Modification using Capping Agent  Electron rich ligands such as amines, thiols, phosphates, carboxylates used for capping of nanoparticles  Surface modifications like reactivity, Charge on the surface, specific gravity, nature of surface i.e. hydrophobicity induced in the nanoparticles with the help of different capping agents. 27
28 Stabilization by Steric interaction where Electrostatic Force of repulsion are weak
Steric Interaction for Stabilization  Nanoparticles dispersion in organic medium experiences less significant electrostatic effects and stability comes from steric interactions by adsorption of amphiphilic molecules.  The lead group of these molecules binds with metal nanoparticles surface while hydrocarbon chain prevents aggregation sterically as shown in figure.  Due to these steric interactions, the nanoparticles are found to be stable in the form of powder even after complete evaporation of solvent. 29
Choice of Capping Agent It determines:  Stability  Reactivity  Size and shape  e.g. Poly vinyl alcohol 30
Synthesis Techniques 1) Bottom-up technique 2) Top- down technique
32
Methodology  Adopted method is Chemical route of synthesis and Biosynthesis using plants  Prepared nanoparticles characterized using different characterization techniques  Antimicrobial activity  Synergetic effectiveness study  Use of synthesized NPs for dye degradation reaction  Use of synthesized NPs as potential catalyst in organic transformation reaction 33
PART II Biosynthesis Of Nanoparticles
Introduction to Nanotechnology
Why green synthesis?  To avoid production of unwanted/harmful by-products  For reliable and cost-effective build-ups  For production of nanoparticles at large-scale  3 R’s (Reduce, Recycle, Reuse)  Controlled morphologies  Bio-compatible products
Biosynthesis: • Production of chemical compounds from precursors in living organism. • Involves enzymes and energy sources. • some examples; photosynthesis, chemosynthesis, amino acid synthesis, nucleic acid synthesis, and ATP synthesis. • The biosynthesis method for production of nanoparticles have more effective applications than physical and chemical synthesis method, because this method is reliable, nontoxic, and eco-friendly.  Nanoparticles are biosynthesized when the microorganisms grab target ions from their environment and then turn the metal ions into the element metal through enzymes generated by the cell activities.  It can be classified into intracellular and extracellular synthesis according to the location where nanoparticles are formed.  The organisms used for synthesis of nanoparticles are bacteria, fungi, yeast.
Introduction to Nanotechnology
1. Bacteria:  Bacterial species have been widely utilized for commercial biotechnological applications such as bioremediation, genetic engineering, and bioleaching.  Bacteria possess the ability to reduce metal ions and are momentous candidates in nanoparticles preparation . For the preparation of metallic and other novel nanoparticles, a variety of bacterial species are utilized.  Prokaryotic bacteria and actinomycetes have been broadly employed for synthesizing metal/metal oxide nanoparticles. 2. Fungi:  Fungi-mediated biosynthesis of metal/metal oxide nanoparticles is also a very efficient process for the generation of monodispersed nanoparticles with well-defined morphologies.  They act as better biological agents for the preparation of metal and metal oxide nanoparticles, due to the presence of a variety of intracellular enzyme .  Competent fungi can synthesize larger amounts of nanoparticles compared to bacteria. Moreover, fungi have many merits over other organisms due to the presence of enzymes/proteins/reducing components on their cell surfaces.  The probable mechanism for the formation of the metallic nanoparticles is enzymatic reduction (reductase) in the cell wall or inside the fungal cell.
3. Yeasts:  Yeasts are single-celled microorganisms present in eukaryotic cells. A total of 1500 yeast species have been identified.  Successful synthesis of nanoparticles/nanomaterials via yeast has been reported by numerous research groups.  The biosynthesis of silver and gold nanoparticles by a silver-tolerant yeast strain and Saccharomyces cerevisiae broth has been reported. 4. Plants: • Plants have the potential to accumulate certain amounts of heavy metals in their diverse parts. Consequently, biosynthesis techniques employing plant extracts have gained increased consideration as a simple, efficient, cost effective and feasible methods as well as an excellent alternative means to conventional preparation methods for nanoparticle production. • There are various plants that can be utilized to reduce and stabilize the metallic nanoparticles in “one-pot” synthesis process. • Many researchers have employed green synthesis process for preparation of metal/metal oxide nanoparticles via plant leaf extracts to further explore their various applications.
Green synthesis of silver nanoparticles using Gongura leaf extract
PART III Uses of Nanoparticles
Ayurveda and Unani uses of nanoparticles :  In Sanskrit, Ayurveda means ‘ the science of life ’.  Ayurveda is the oldest form of Indian traditional system of medicine. The other traditional system of Indian medicine includes Unani and Siddha.  Ayurveda aims at strengthening the capacity of the body and improving immunity by using herbs and minerals in its medicines.  whereas Unani, which is the holistic system of medicine, is quite common throughout the India.  A section of Ayurveda deals with herbo-mineral preparations called Bhasma (ash) is known as Rasa Shastra (Vedic chemistry).
 The major therapeutic actions of Bhasma are their ability for Immunomodulation and anti-aging property (Rasayana) and ability to target drugs to the site.  Ayurvedic preparations are claimed to be nontoxic, absorbed readily, and biocompatible.  Bhasma is an important Ayurvedic formulation comprising mixture of herbs and metals.  Bhasma are nearer to nanocrystallite materials which are solid composed of crystallite with sizes less than 100 nm, at least in one dimension.  Ayurvedic metallic nanocrystallite or Bhasma have unique physicochemical properties such as biocompatibility and ease of surface fictionalization.
 The nanotechnology in Ayurvedic drugs have application in: 1. molecular detection 2. targeted delivery 3. biological imaging.  application of Nano-carriers for the delivery of Ayurvedic drugs can be a great initiative because such carriers are capable to cross the plasma membrane and deliver the drug in the desired concentration at the specific site of action. Integration of Ayurveda and nanotechnology may provide the best medicines to treat various life-threatening diseases.  Nanoparticles are used in various sensors such as Gas sensors, Chemical sensors, artificial tongue, humidity sensors etc
Attributes of Nanotechnology  Nanoparticles are used in solar cell devices  Nanoparticles are used in memory storage devices such as memristers  Nanoparticles are in super-capacitors to store electrical energy  Nanoparticles are in electrochromic materials  Nanoparticles are used in the area of veterinary and human medicine. Today we observe that efficiency of antibiotics against a pathogenic bacterium gets decrease after frequent uses. It is difficult to have new antibiotics. It has been observed that many nanoparticles especially silver nanoparticles show high antimicrobial activities.
PART IV Environmental Aspects Of Nanoparticles
POSITIVE IMPACT OF NMs Nanotechnology promises significant social, environmental, and financial benefits. Nanotechnology may ultimately be developed to help decrease the human footprint on the environment by providing more efficient and energy saving innovations.
NEGATIVE IMPACT OF NMs As the environmental impacts of NMs cannot be clearly diagnosed and there are too many variables to account for (e.g., NMs identification, low detection limits, and unknown environmental concentrations), it is very difficult to reach any conclusion about the ecological effects and environmental stability of NMs. Even a minor change in the chemical structure of NMs could radically change their properties, turning them into toxic compounds. According to the United States Environmental Protection Agency, “the toxicity of NMs is difficult to identify because they have unique chemical properties, high reactivity, and do not dissolve in liquid”
Analysis of Materials at Nanoscale  The nanomaterials are so small that they cannot be visualized by naked eyes.  The properties of materials at nanoscale depends upon size, shape, morphology, interatomic distance, electrostatic forece of attraction or repulsion, secondary bonds like van der waal’s interaction etc.  It is possible to determine the properties of the materials at nanoscale using advanced characterization techniques such as XRD, Scanning Electron Microscopy, Transmission Electron Microscopy, Zeta Potential etc.
Characterization Techniques  . The instruments used for analysis are of two types i.e. 1) spectroscopes and 2) microscopes.  A. Spectroscopy: It is a branch of science that deals with the interaction of electromagnetic radiations with the matter. Spectroscopy is the most powerful tool available for the study of atomic and molecular structure and is used in the analysis of a wide range of samples.  B. Microscopic Techniques  Microscopy is the technical field of using a microscope to view samples and objects that cannot be seen with the unaided eye. There are three well-known branches of microscopy; optical, electron, and scanning probe microscopy.
 Optical and electron microscopy involve the diffraction, reflection, and refraction of electromagnetic radiation/ electron beam interacting with the specimen and the subsequent collection of this scattered radiation or another signal to create an image. This process may be carried out by wide-field irradiation of the sample (e.g. Transmission Electron Microscope) or by scanning a fine beam over the sample (e.g. Scanning Electron Microscope).
Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) XRD X-Ray Diffraction Crystal structure, composition, crystallite size, XAS X-Ray Absorption Spectroscopy X-ray absorption co-efficient, chemical state of species, interatomic distances, Debye- Waller factors, and non- crystalline NPs
Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) SAXS Small Angle X-Ray Scattering Particle size, size distribution, growth kinetics XPS X-ray photoelectron Spectroscopy Electronic structure, elemental composition, oxidation states, ligand binding FT-IR Fouier Trasform Infrared Spectroscopy Surface composition, ligand binding NMR Nuclear Magnetic Resonance Spectroscopy Ligand density and arrangements, electronic core structure, atomic composition, the influence of ligands on NP shape, NP size BET Brunauer Emmett Teller Surface area
Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) TGA Thermogravimetric Analysis Mass and composition of stabilizers LEIS Low Energy Ion Scattering Thickness and chemical composition of self-assembled monolayers of NPs UV-Visible spectroscopy Ultra-violet Visible Spectroscopy Optical properties, size, concentration, and agglomeration state, hints at nanoparticles shape PL Spectroscopy Photoluminescence spectroscopy Optical properties, relation to structural features such as defects, size, composition, etc DLS Dynamic Light Scattering Hydrodynamic size, detection of agglomeration NTA Nanoparticle Tracking Analysis Nanoparticles size and their distribution DCA Direct Coupling Analysis Nanoparticles size and their distribution ICP-MS Inductively Coupled Plasma Mass Spectroscopy Elemental composition, size, size distribution, NP concentration
Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) SIMS ToF- SIMS,MALDI Sputtering Ion Mass Spectroscopy Chemical information on functional groups especially surface sensitivity, molecular orientation, and conformation, surface topography, MALDI for nanoparticle size VSM Vibrating Sample Magnetometer Magnetic properties of nanomaterials Contact Angle Contact Angle Determination of hydrophobic characters of thin films FMR Ferromagnetic Resonance Spectroscopy Nanoparticle size and distribution, shape, crystallographic imperfections, surface composition, M value, magnetic anisotropic constant, demagnetization fields XMCD X-Ray Magnetic Circular Dichroism Site symmetry and magnetic moments of transition metal ions in ferro and ferri magnetic materials element-specific
Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) CLSM Confocal Laser Scanning Microscope Imaging, ultrafine morphology BAM Brewster Angle Microscope Gas-liquid interface imaging APM Atomic Probe Microscopy Three Dimensional Imaging MFM Magnetic Force Microscopy Magnetic Material Analysis Low Energy Electron Diffraction Low Energy Electron Diffraction Surface/Adsorbate bonding
Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbrevi ation Characterization Techniques Main Information (Utility) AEM Auger Electron Microscopy Chemical Surface Analysis CFM Chemical Force Microscopy Chemical/Surface Analysis FIM Field Ion Microscopy Chemical Profile/ Atomic spacing UPS Ultraviolet Photoemission Spectroscopy Surface Analysis AAS Atomic Absorption Spectroscopy Chemical Analysis
Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) ICM Inductively Coupled Microscopy Elemental Analysis SANS Small Angle Neutran Scattering Surface Characterization CL Cthodoluminescence Characteristic Emission Nanocalorimetry Nanocalorimetry Latent Heat of Fusion Sears Method Sears Method Colloidal size, specific surface area FS Fluorescent Spectroscopy Elemental Analysis LSPR Localized Surface Plasmon Resonance Nanosized particle Analysis Rutherford Backscattering Rutherford Backscattering Quantitative Elemental Analysis TEM Transmission Electron Microscopy NP size, size monodispersity shape, aggregation state, detect and localize quantify nanoparticles in matrices, study growth kinetics HRTEM High-Resolution Transmission Electron Microscopy All information by conventional TEM and also on the crystal structure of a single particle. It is used to distinguish between monocrystalline, polycrystalline, and
Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviatio n Characterization Techniques Main Information (Utility) Liquid TEM Liquid Transmission Electron Microscopy Depict nanoparticle growth in real-time, study growth mechanism, single particle motion, and superlattice formation Cryo-TEM Cryo Transmission Electron Microscopy Study complex growth mechanisms, and aggregation pathways, good for molecular biology and colloidal chemistry to avoid the presence of artifacts or destroyed samples ED Electron Diffraction Crystal structure, lattice parameter, study order, and disorder transformation, long-range order parameters STEM Scanning Transmission Electron Microscopy Combined with HAADF, and EDX for morphology study, crystal structure, and elemental composition, Study the atomic structure of hetero-interface
Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) Aberration- corrected (STEM, TEM) Aberration corrected Scanning Transmission Electron Microscopy Atomic structure of NP clusters, especially bimetallic ones, as a function of composition, alloy, homogeneity, phase segregation EELS Electron Energy Loss Spectroscopy Type and quantity of atoms present, chemical states of atoms, collective interaction of atoms with neighbors, bulk plasma resonance Electron tomography Electron tomography Realistic 3D particle visualization, snapshots, video, and quantitative information down to atomic scale SEM-HRSEM, T-SE- EDX Scanning Electron Microscopy- High- Resolution Scanning Electron Microscope Morphology, dispersion of nanoparticles in cells and other matrices/ supports, precision in the lateral dimension of nanoparticles, quick examination-elemental composition
Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) EBSD Electron Backscattered Diffraction Microscopy Structure, crystal orientation, and phase of matrices in SEM. Examine microstructure, reveal texture, defects, grain morphology, deformation AFM Atomic Force Microscope Nanoparticle size and shape in 3D mode, evaluate the degree of covering of a surface with nanoparticle morphology, dispersion of nanoparticles in cell and other matrices/ supports, precision in the lateral dimension of nanoparticles, quick examination- elemental composition
Nanoscale Parameters Characterization Entity Characterized Possible Characterization Techniques Size ( structural properties) TEM, XRD, DLS, NTA, SAXS, HRTEM, SEM, AFM, EXAFM, FMR, DCS, ICP-MS, UV-Vis, MALDI, NMR, TRPS, EPLS, magnetic susceptibility Shape TEM, HRTEM, AFM, EPLS, FMR, 3D- tomography
Nanoscale Parameters Characterization Techniques Elemental chemical composition XRD, XPS, ICP-MS, ICP-OES, SEM-EDX, NMR, MFM, LEIS Crystal structure XRD, EXAFS, HRTEM, STEM, electron diffraction Size distribution DCS, DLS, SAXS, NTA, ICP-MS, FMR, DTA, TRPS, SEM, superparamagnetic relaxometry Magnetic properties SQUID, VSM, MFM, FMR, XMCD, magnetic susceptibility
Nanoscale Parameters Characterization Techniques Detection of Nanoparticles TEM, SEM, STEM, EBSD, magnetic susceptibility Structural defects HRTEM, EBSD Dispersion of nanoparticles in matrices SEM, AFM, TEM 3D visualization 3D topography, AFM, SEM Single-particle properties Sp-ICP-MS, UV-Vis, RMM-MEMS,PTA,DCS,TRPS Density DCS, RMM-MEMS
Nanoscale Parameters Characterization Techniques Agglomeration state Zeta potential, DLS, DCS, UV-Visible spectroscopy, SEM, Cryo-TEM, TEM Concentration ICP-MS, UV-Visible, RMM-MEMS, PTA, DCS, TRPS Surface charges Zeta potential, EPM Surface area, specific surface area BET, liquid NMR Ligand binding/ composition/ density/ arrangement/ mass, surface composition XPS, FTIR, NMR, SIMS, FMR, TGA, SANS Growth kinetics SAXS, NMR, TEM, cro- TEM, liquid-TEM Chemical state –oxidation state XAS, EELS, XPS, Mossbauer
Thank You

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Introduction to Nanotechnology

  • 1. Green sysnthesis of Metals and their Oxide Nanoparticles: Application for Environmental Remedation. Dr Rai Dhirendra Prasad Bihar Veterinary College, Patna, India Col Amit Sinha SPPU, Pune, India 1
  • 2. 2 PART I What Is Nanotechnology?
  • 3. “Nanotechnology is the art and science of manipulating matter at the nanoscale”
  • 4. Nanotechnology in Ancient Period  Ras-Ratnakar: described the formation of metallic nanoparticles about 5000 years ago Shodhan: purification Maran: killing the metallic properties  Alchemist- Aurum potable & Luna potable about 1570  Dr Samuel Hahnemann- Organon of medicines  Lycurgus Cup: 4th century AD 4
  • 5. History The idea of nanotechnology was born in December 29, 1959 when physicist “Richard Feynman” gave a lecture exploring the idea of building things at the atomic and molecular scale. He is regarded as Father of Nanotechnology and given the Famous statement “There is plenty of Room at the bottom” He imagined the entire Encyclopedia Britannica written on the head of a pin.
  • 6. Nanoparticles  "A particle with the size of the order of 1-nm to 100nm in any dimension and at least any one property different from that of bulk".  During the synthesis of nanoparticles, size of nanoparticles depends on the steochiometric ratio of metal ion to capping ligands concentration. 6
  • 7. Properties at nanoscale  Properties of nanoparticles: depend upon size, shape, stabilizing agent, method of preparation etc.  Changes in optical, thermal, electrical, electronic, magnetic and mechanical properties 7
  • 8. Melting Point  Graph of melting point (Tm) vs size of particle (D)  Melting point of nanoparticles is below the melting point of bulk material Tm= TmBulk (1-1/D) 8
  • 9. Optical Property  Size dependent optical properties of gold nanoparticles  This effect appears due to the interaction of electro- magnetic radiation with the electron cloud present on the surface of metal nanoparticles 9
  • 10. Surface Plasmon Resonance  Surface Plasmon oscillations.  Large number of atoms present on the surface of nanoparticles contributes electron cloud which interacts with E-field of light and thus oscillates 10
  • 11. Electronic Property  When the size enters nano level, electron motion is restricted to a smaller space, they don’t follow classical theory & restricts themselves from diffusion of valence and conduction band.  The energy gap between valence band and conduction bond (Kubo gap) becomes larger than thermal energy (KBT) and hence metallic nanoparticles become semiconductor further becomes an insulator 11
  • 12. Other Properties  Magnetic Property: Bulk materials forms multiple magnetic domains, but nanoparticles form only a single magnetic domain thus could be used for super magnetism.  Bio-compatibility:  Electrical Properties: The metals that are good conductance behave as semiconductor at nano-level. 12
  • 13. Property changes…  opaque substances become transparent (copper)  stable materials turn combustible (aluminum)  insoluble materials become soluble (gold)  Chemically inert becomes active (Gold) 13
  • 14. Why different property at Nanoscale • High Surface to Volume ratio (Aspect ratio) : Because of this the nanoparticle become less stable .  Gravitational force: is not effective  Size comparable to wavelength of light: thus entire different optical properties like Surface Plasmon Resonance is exhibited.  Dangling bonds: 14
  • 15. Surface to Volume Ratio  spherical particle,  surface area = 4πr2 and volume = 4/3 π r3  Sp= 4πr2σ/ (4/3)πr3ρ  Where, σ is surface area factor and ρ is volume factor  r→o , Sp→∞ 15
  • 16. Quantum mechanics  Nanoparticles do not obey the laws of classical mechanics; instead they follow the principles of quantum mechanics.  Exhibits interesting shape dependence due to electronic motion in different dimensions. 16
  • 17. Example of shape dependent property  Electronic tunneling phenomenon is observed for 0-D nanostructures which is the key concept used for building artificial atoms and devices like single electron transistors.  Electron can oscillate in two distinct ways in 1-D nanostructures under electromagnetic field, namely in longitudinal and transverse modes. The way electrons executes its motion alters their various properties and thus nano-rods and nano-tubes give rise to Surface Plasmon absorption peaks due to the two different types of electronic motion. 17
  • 18. Nanoparticles as Smart Material:  Smart materials are the materials that respond favorably to change in temperature, pH, moisture or electromagnetic fields thus are extensively used as sensors and actuators.  Nanoparticles can also be used as advanced engineering materials which can withstand high temp, high impact, 18
  • 19. Nano-composites  Light weight Nano composites can replace heavy metals in automobile industry to achieve high speed in vehicles  Nano-composites are actively used to enhance the efficiency of solar cells, and also in superconductor and super capacitors 19
  • 21. Norio Taniguchi  The term "nanotechnology" was defined by Tokyo Science University Professor Norio Taniguchi in a 1974 paper as follows: "'Nanotechnology' mainly consists of the processing, separation, consolidation, and deformation of materials by one atom or by one molecule." 21
  • 22. Stabilization of Nanoparticles  Tendency to form agglomeration:  Stabilizing agent: usually accomplished by suitable passivating agents also called as capping agent. 22
  • 23. Gibb’s Free Energy & Stability  As size of the nanoparticles decreases their surface energy increases.  Increase in the surface energy results in increase in the Gibb’s free energy.  According to the law of thermodynamics, every system always tries to attain minimum Gibb’s free energy  Therefore it loses its nanoness and exotic properties related to it. Hence it is very important to stabilize the nanoparticles against the aggregation. 23
  • 25. Potential energy vs distance between the nanoparticles  Particles formed are surrounded by the electronic double layer of reactant ions on the surface of nanoparticles  Two forces: Van der Waals forces of attraction , and electrostatic force of repulsion due to the charged ions on the surface.  Stability of nanoparticles is dependent on the combined effect of these two forces.  Greater the thickness of the double layer, higher is the potential energy barrier & higher is stability 25
  • 26. 26 Different Capping agents used for Surface Modification & Stabilization
  • 27. Surface Modification using Capping Agent  Electron rich ligands such as amines, thiols, phosphates, carboxylates used for capping of nanoparticles  Surface modifications like reactivity, Charge on the surface, specific gravity, nature of surface i.e. hydrophobicity induced in the nanoparticles with the help of different capping agents. 27
  • 28. 28 Stabilization by Steric interaction where Electrostatic Force of repulsion are weak
  • 29. Steric Interaction for Stabilization  Nanoparticles dispersion in organic medium experiences less significant electrostatic effects and stability comes from steric interactions by adsorption of amphiphilic molecules.  The lead group of these molecules binds with metal nanoparticles surface while hydrocarbon chain prevents aggregation sterically as shown in figure.  Due to these steric interactions, the nanoparticles are found to be stable in the form of powder even after complete evaporation of solvent. 29
  • 30. Choice of Capping Agent It determines:  Stability  Reactivity  Size and shape  e.g. Poly vinyl alcohol 30
  • 31. Synthesis Techniques 1) Bottom-up technique 2) Top- down technique
  • 32. 32
  • 33. Methodology  Adopted method is Chemical route of synthesis and Biosynthesis using plants  Prepared nanoparticles characterized using different characterization techniques  Antimicrobial activity  Synergetic effectiveness study  Use of synthesized NPs for dye degradation reaction  Use of synthesized NPs as potential catalyst in organic transformation reaction 33
  • 34. PART II Biosynthesis Of Nanoparticles
  • 36. Why green synthesis?  To avoid production of unwanted/harmful by-products  For reliable and cost-effective build-ups  For production of nanoparticles at large-scale  3 R’s (Reduce, Recycle, Reuse)  Controlled morphologies  Bio-compatible products
  • 37. Biosynthesis: • Production of chemical compounds from precursors in living organism. • Involves enzymes and energy sources. • some examples; photosynthesis, chemosynthesis, amino acid synthesis, nucleic acid synthesis, and ATP synthesis. • The biosynthesis method for production of nanoparticles have more effective applications than physical and chemical synthesis method, because this method is reliable, nontoxic, and eco-friendly.  Nanoparticles are biosynthesized when the microorganisms grab target ions from their environment and then turn the metal ions into the element metal through enzymes generated by the cell activities.  It can be classified into intracellular and extracellular synthesis according to the location where nanoparticles are formed.  The organisms used for synthesis of nanoparticles are bacteria, fungi, yeast.
  • 39. 1. Bacteria:  Bacterial species have been widely utilized for commercial biotechnological applications such as bioremediation, genetic engineering, and bioleaching.  Bacteria possess the ability to reduce metal ions and are momentous candidates in nanoparticles preparation . For the preparation of metallic and other novel nanoparticles, a variety of bacterial species are utilized.  Prokaryotic bacteria and actinomycetes have been broadly employed for synthesizing metal/metal oxide nanoparticles. 2. Fungi:  Fungi-mediated biosynthesis of metal/metal oxide nanoparticles is also a very efficient process for the generation of monodispersed nanoparticles with well-defined morphologies.  They act as better biological agents for the preparation of metal and metal oxide nanoparticles, due to the presence of a variety of intracellular enzyme .  Competent fungi can synthesize larger amounts of nanoparticles compared to bacteria. Moreover, fungi have many merits over other organisms due to the presence of enzymes/proteins/reducing components on their cell surfaces.  The probable mechanism for the formation of the metallic nanoparticles is enzymatic reduction (reductase) in the cell wall or inside the fungal cell.
  • 40. 3. Yeasts:  Yeasts are single-celled microorganisms present in eukaryotic cells. A total of 1500 yeast species have been identified.  Successful synthesis of nanoparticles/nanomaterials via yeast has been reported by numerous research groups.  The biosynthesis of silver and gold nanoparticles by a silver-tolerant yeast strain and Saccharomyces cerevisiae broth has been reported. 4. Plants: • Plants have the potential to accumulate certain amounts of heavy metals in their diverse parts. Consequently, biosynthesis techniques employing plant extracts have gained increased consideration as a simple, efficient, cost effective and feasible methods as well as an excellent alternative means to conventional preparation methods for nanoparticle production. • There are various plants that can be utilized to reduce and stabilize the metallic nanoparticles in “one-pot” synthesis process. • Many researchers have employed green synthesis process for preparation of metal/metal oxide nanoparticles via plant leaf extracts to further explore their various applications.
  • 41. Green synthesis of silver nanoparticles using Gongura leaf extract
  • 42. PART III Uses of Nanoparticles
  • 43. Ayurveda and Unani uses of nanoparticles :  In Sanskrit, Ayurveda means ‘ the science of life ’.  Ayurveda is the oldest form of Indian traditional system of medicine. The other traditional system of Indian medicine includes Unani and Siddha.  Ayurveda aims at strengthening the capacity of the body and improving immunity by using herbs and minerals in its medicines.  whereas Unani, which is the holistic system of medicine, is quite common throughout the India.  A section of Ayurveda deals with herbo-mineral preparations called Bhasma (ash) is known as Rasa Shastra (Vedic chemistry).
  • 44.  The major therapeutic actions of Bhasma are their ability for Immunomodulation and anti-aging property (Rasayana) and ability to target drugs to the site.  Ayurvedic preparations are claimed to be nontoxic, absorbed readily, and biocompatible.  Bhasma is an important Ayurvedic formulation comprising mixture of herbs and metals.  Bhasma are nearer to nanocrystallite materials which are solid composed of crystallite with sizes less than 100 nm, at least in one dimension.  Ayurvedic metallic nanocrystallite or Bhasma have unique physicochemical properties such as biocompatibility and ease of surface fictionalization.
  • 45.  The nanotechnology in Ayurvedic drugs have application in: 1. molecular detection 2. targeted delivery 3. biological imaging.  application of Nano-carriers for the delivery of Ayurvedic drugs can be a great initiative because such carriers are capable to cross the plasma membrane and deliver the drug in the desired concentration at the specific site of action. Integration of Ayurveda and nanotechnology may provide the best medicines to treat various life-threatening diseases.  Nanoparticles are used in various sensors such as Gas sensors, Chemical sensors, artificial tongue, humidity sensors etc
  • 46. Attributes of Nanotechnology  Nanoparticles are used in solar cell devices  Nanoparticles are used in memory storage devices such as memristers  Nanoparticles are in super-capacitors to store electrical energy  Nanoparticles are in electrochromic materials  Nanoparticles are used in the area of veterinary and human medicine. Today we observe that efficiency of antibiotics against a pathogenic bacterium gets decrease after frequent uses. It is difficult to have new antibiotics. It has been observed that many nanoparticles especially silver nanoparticles show high antimicrobial activities.
  • 47. PART IV Environmental Aspects Of Nanoparticles
  • 48. POSITIVE IMPACT OF NMs Nanotechnology promises significant social, environmental, and financial benefits. Nanotechnology may ultimately be developed to help decrease the human footprint on the environment by providing more efficient and energy saving innovations.
  • 49. NEGATIVE IMPACT OF NMs As the environmental impacts of NMs cannot be clearly diagnosed and there are too many variables to account for (e.g., NMs identification, low detection limits, and unknown environmental concentrations), it is very difficult to reach any conclusion about the ecological effects and environmental stability of NMs. Even a minor change in the chemical structure of NMs could radically change their properties, turning them into toxic compounds. According to the United States Environmental Protection Agency, “the toxicity of NMs is difficult to identify because they have unique chemical properties, high reactivity, and do not dissolve in liquid”
  • 50. Analysis of Materials at Nanoscale  The nanomaterials are so small that they cannot be visualized by naked eyes.  The properties of materials at nanoscale depends upon size, shape, morphology, interatomic distance, electrostatic forece of attraction or repulsion, secondary bonds like van der waal’s interaction etc.  It is possible to determine the properties of the materials at nanoscale using advanced characterization techniques such as XRD, Scanning Electron Microscopy, Transmission Electron Microscopy, Zeta Potential etc.
  • 51. Characterization Techniques  . The instruments used for analysis are of two types i.e. 1) spectroscopes and 2) microscopes.  A. Spectroscopy: It is a branch of science that deals with the interaction of electromagnetic radiations with the matter. Spectroscopy is the most powerful tool available for the study of atomic and molecular structure and is used in the analysis of a wide range of samples.  B. Microscopic Techniques  Microscopy is the technical field of using a microscope to view samples and objects that cannot be seen with the unaided eye. There are three well-known branches of microscopy; optical, electron, and scanning probe microscopy.
  • 52.  Optical and electron microscopy involve the diffraction, reflection, and refraction of electromagnetic radiation/ electron beam interacting with the specimen and the subsequent collection of this scattered radiation or another signal to create an image. This process may be carried out by wide-field irradiation of the sample (e.g. Transmission Electron Microscope) or by scanning a fine beam over the sample (e.g. Scanning Electron Microscope).
  • 53. Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) XRD X-Ray Diffraction Crystal structure, composition, crystallite size, XAS X-Ray Absorption Spectroscopy X-ray absorption co-efficient, chemical state of species, interatomic distances, Debye- Waller factors, and non- crystalline NPs
  • 54. Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) SAXS Small Angle X-Ray Scattering Particle size, size distribution, growth kinetics XPS X-ray photoelectron Spectroscopy Electronic structure, elemental composition, oxidation states, ligand binding FT-IR Fouier Trasform Infrared Spectroscopy Surface composition, ligand binding NMR Nuclear Magnetic Resonance Spectroscopy Ligand density and arrangements, electronic core structure, atomic composition, the influence of ligands on NP shape, NP size BET Brunauer Emmett Teller Surface area
  • 55. Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) TGA Thermogravimetric Analysis Mass and composition of stabilizers LEIS Low Energy Ion Scattering Thickness and chemical composition of self-assembled monolayers of NPs UV-Visible spectroscopy Ultra-violet Visible Spectroscopy Optical properties, size, concentration, and agglomeration state, hints at nanoparticles shape PL Spectroscopy Photoluminescence spectroscopy Optical properties, relation to structural features such as defects, size, composition, etc DLS Dynamic Light Scattering Hydrodynamic size, detection of agglomeration NTA Nanoparticle Tracking Analysis Nanoparticles size and their distribution DCA Direct Coupling Analysis Nanoparticles size and their distribution ICP-MS Inductively Coupled Plasma Mass Spectroscopy Elemental composition, size, size distribution, NP concentration
  • 56. Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) SIMS ToF- SIMS,MALDI Sputtering Ion Mass Spectroscopy Chemical information on functional groups especially surface sensitivity, molecular orientation, and conformation, surface topography, MALDI for nanoparticle size VSM Vibrating Sample Magnetometer Magnetic properties of nanomaterials Contact Angle Contact Angle Determination of hydrophobic characters of thin films FMR Ferromagnetic Resonance Spectroscopy Nanoparticle size and distribution, shape, crystallographic imperfections, surface composition, M value, magnetic anisotropic constant, demagnetization fields XMCD X-Ray Magnetic Circular Dichroism Site symmetry and magnetic moments of transition metal ions in ferro and ferri magnetic materials element-specific
  • 57. Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) CLSM Confocal Laser Scanning Microscope Imaging, ultrafine morphology BAM Brewster Angle Microscope Gas-liquid interface imaging APM Atomic Probe Microscopy Three Dimensional Imaging MFM Magnetic Force Microscopy Magnetic Material Analysis Low Energy Electron Diffraction Low Energy Electron Diffraction Surface/Adsorbate bonding
  • 58. Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbrevi ation Characterization Techniques Main Information (Utility) AEM Auger Electron Microscopy Chemical Surface Analysis CFM Chemical Force Microscopy Chemical/Surface Analysis FIM Field Ion Microscopy Chemical Profile/ Atomic spacing UPS Ultraviolet Photoemission Spectroscopy Surface Analysis AAS Atomic Absorption Spectroscopy Chemical Analysis
  • 59. Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) ICM Inductively Coupled Microscopy Elemental Analysis SANS Small Angle Neutran Scattering Surface Characterization CL Cthodoluminescence Characteristic Emission Nanocalorimetry Nanocalorimetry Latent Heat of Fusion Sears Method Sears Method Colloidal size, specific surface area FS Fluorescent Spectroscopy Elemental Analysis LSPR Localized Surface Plasmon Resonance Nanosized particle Analysis Rutherford Backscattering Rutherford Backscattering Quantitative Elemental Analysis TEM Transmission Electron Microscopy NP size, size monodispersity shape, aggregation state, detect and localize quantify nanoparticles in matrices, study growth kinetics HRTEM High-Resolution Transmission Electron Microscopy All information by conventional TEM and also on the crystal structure of a single particle. It is used to distinguish between monocrystalline, polycrystalline, and
  • 60. Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviatio n Characterization Techniques Main Information (Utility) Liquid TEM Liquid Transmission Electron Microscopy Depict nanoparticle growth in real-time, study growth mechanism, single particle motion, and superlattice formation Cryo-TEM Cryo Transmission Electron Microscopy Study complex growth mechanisms, and aggregation pathways, good for molecular biology and colloidal chemistry to avoid the presence of artifacts or destroyed samples ED Electron Diffraction Crystal structure, lattice parameter, study order, and disorder transformation, long-range order parameters STEM Scanning Transmission Electron Microscopy Combined with HAADF, and EDX for morphology study, crystal structure, and elemental composition, Study the atomic structure of hetero-interface
  • 61. Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) Aberration- corrected (STEM, TEM) Aberration corrected Scanning Transmission Electron Microscopy Atomic structure of NP clusters, especially bimetallic ones, as a function of composition, alloy, homogeneity, phase segregation EELS Electron Energy Loss Spectroscopy Type and quantity of atoms present, chemical states of atoms, collective interaction of atoms with neighbors, bulk plasma resonance Electron tomography Electron tomography Realistic 3D particle visualization, snapshots, video, and quantitative information down to atomic scale SEM-HRSEM, T-SE- EDX Scanning Electron Microscopy- High- Resolution Scanning Electron Microscope Morphology, dispersion of nanoparticles in cells and other matrices/ supports, precision in the lateral dimension of nanoparticles, quick examination-elemental composition
  • 62. Glimpses on experimental Techniques Used For Nanomaterial Characterization Abbreviation Characterization Techniques Main Information (Utility) EBSD Electron Backscattered Diffraction Microscopy Structure, crystal orientation, and phase of matrices in SEM. Examine microstructure, reveal texture, defects, grain morphology, deformation AFM Atomic Force Microscope Nanoparticle size and shape in 3D mode, evaluate the degree of covering of a surface with nanoparticle morphology, dispersion of nanoparticles in cell and other matrices/ supports, precision in the lateral dimension of nanoparticles, quick examination- elemental composition
  • 63. Nanoscale Parameters Characterization Entity Characterized Possible Characterization Techniques Size ( structural properties) TEM, XRD, DLS, NTA, SAXS, HRTEM, SEM, AFM, EXAFM, FMR, DCS, ICP-MS, UV-Vis, MALDI, NMR, TRPS, EPLS, magnetic susceptibility Shape TEM, HRTEM, AFM, EPLS, FMR, 3D- tomography
  • 64. Nanoscale Parameters Characterization Techniques Elemental chemical composition XRD, XPS, ICP-MS, ICP-OES, SEM-EDX, NMR, MFM, LEIS Crystal structure XRD, EXAFS, HRTEM, STEM, electron diffraction Size distribution DCS, DLS, SAXS, NTA, ICP-MS, FMR, DTA, TRPS, SEM, superparamagnetic relaxometry Magnetic properties SQUID, VSM, MFM, FMR, XMCD, magnetic susceptibility
  • 65. Nanoscale Parameters Characterization Techniques Detection of Nanoparticles TEM, SEM, STEM, EBSD, magnetic susceptibility Structural defects HRTEM, EBSD Dispersion of nanoparticles in matrices SEM, AFM, TEM 3D visualization 3D topography, AFM, SEM Single-particle properties Sp-ICP-MS, UV-Vis, RMM-MEMS,PTA,DCS,TRPS Density DCS, RMM-MEMS
  • 66. Nanoscale Parameters Characterization Techniques Agglomeration state Zeta potential, DLS, DCS, UV-Visible spectroscopy, SEM, Cryo-TEM, TEM Concentration ICP-MS, UV-Visible, RMM-MEMS, PTA, DCS, TRPS Surface charges Zeta potential, EPM Surface area, specific surface area BET, liquid NMR Ligand binding/ composition/ density/ arrangement/ mass, surface composition XPS, FTIR, NMR, SIMS, FMR, TGA, SANS Growth kinetics SAXS, NMR, TEM, cro- TEM, liquid-TEM Chemical state –oxidation state XAS, EELS, XPS, Mossbauer

Editor's Notes

  • #4: by definiton as you can see ”it’s the art of manipulating matter at the nanoscale level”
  • #21: Now this is a bit informative 3d chart, providing the size comparisons between different objects raised to the power of 10 meters. Here you can see, a 6 foot man is 1.62 meters or roughly around 2 billion nms tall. While on the other hand, a sample of a DNA molecule, as we have already seen in the previous slide, is approx. 2 nms long.