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In this module the application of TGA-FTIR for metal oxide nanoparticles is presented. This method is demonstrated on a sample of WO3-x nanorods synthesized via a solvothermal method.

Metal oxide nanoparticles

The binary compound of one or more oxygen atoms with at least one metal atom that forms a structure ≤100 nm is classified as metal oxide (MO x ) nanoparticle. MO x nanoparticles have exceptional physical and chemical properties (especially if they are smaller than 10 nm) that are strongly related to their dimensions and to their morphology. These enhanced features are due to the increased surface to volume ratio which has a strong impact on the measured binding energies. Based on theoretical models, binding or cohesive energy is inversely related to particle size with a linear relationship [link] .

E NP = E bulk [ 1 c r 1 ] size 12{E rSub { size 8{ ital "NP"} } =E rSub { size 8{ ital "bulk"} } cdot \[ 1 - c cdot r rSup { size 8{ - 1} } \] } {}

where E NP and E bulk is the binding energy of the nanoparticle and the bulk binding energy respectively, c is a material constant and r is the radius of the cluster. As seen from [link] , nanoparticles have lower binding energies than bulk material, which means lower electron cloud density and therefore more mobile electrons. This is one of the features that have been identified to contribute to a series of physical and chemical properties.

Synthesis of metal oxide nanoparticles

Since today, numerous synthetic methods have been developed with the most common ones presented in [link] . These methods have been successfully applied for the synthesis of a variety of materials with 0-D to 3-D complex structures. Among them, the solvothermal methods are by far the most popular ones due to their simplicity. Between the two classes of solvothermal methods, slow decomposition methods, usually called thermal decomposition methods, are preferred over the hot injection methods since they are less complicated, less dangerous and avoid the use of additional solvents.

Methods for synthesizing MO x nanoparticles
Method Characteristics Advantages Disadvantages
Solvothermal
  1. Slow decomposition
  2. Hot injection
  1. Slow heating of M-precursor in the presence of ligand/surfactant precursor
  2. Injection of M-precursor into solution at high Temp.
  1. Safe, easily carried out, variety of M-precursors to use
  2. Excellent control of particle distribution
  1. Poor control of nucleation/ growth stages – Particle size
  2. Hazardous, Reproducibility depends on individual
Template directed Use of organic molecules or preexistent nanoparticles as templates for directing nanoparticle formation High yield and high purity of nanoparticles Template removal in some cases causes particle deformation or loss
Sonochemical Ultrasound influence particle nucleation Mild synthesis conditions Limited applicability
Thermal evaporation Thermal evaporation of Metal oxides Monodisperse particle formation, excellent control in shape and structure Extremely high temperatures, and vacuum system is required
Gas phase catalytic growth Use of catalyst that serves as a preferential site for absorbing Metal reactants Excellent control in shape and structure Limited applicability

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Source:  OpenStax, Nanomaterials and nanotechnology. OpenStax CNX. May 07, 2014 Download for free at http://legacy.cnx.org/content/col10700/1.13
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