21UPHE01 Materials Science

UNIT-III: NONLINEAR OPTICAL AND NANOPHASE MATERIALS

Origin of optical nonlinearity - Basic theory of nonlinear optics – Harmonic generation- Optical mixing- classification of nonlinear optical materials and their applications. Nano
phase Material - Top-down & Bottom-up approach - synthesis- Ball milling method and Sol- Gel method physical properties with geometry –applications.

ONE MARK
1. In second harmonic generation, the frequency is ____________.
(a) Constant (b) Doubled
(c) Negative (d) All o f the above

2. In optical mixing, the sources of ___________ frequencies are mixed together

(a) Same (b) Different
(c) high (d) Low

3. Which of the following is not related to Kerr effects?

(a) Self-phase modulation (b) Cross-phase modulation
(c) Four-wave mixing (d) Stimulated Raman Scattering

4. The value of one nanometre is equal to______.

(a) 10-6m (b) 10-9m (c) 10-12m (d) 10-15m

5. ______ process is used to assemble atoms or molecules to form nanomaterials.

(a) Top down (b) Bottom up
(c) Ball mill (d) Condensation

6. Nanoparticles are obtained by breaking the bulk solids employing _______ method
(a) Top down (b) Bottom up
(c) Ball mill (d) Condensation

7. In mechanical grinding, hard materials are used to synthesis _______ materials

(a) Softer (b) harder
(c) magnetic (d) Glass

8. In which of the following atoms do not move from eachother?

(a) Sahpe memory alloys (b) Nano materials
(c) Dielectrics (d) Static materials

9. Which of the following is used to make both nano-particles and nano-powders?

(a) Chemical vapour deposition (b) Sol-gel technique
(c) Plasma arching (d) Electro deposition

10. Which method can be used to prepare iron nitriles nano-crystals using ammonia gas?
(a) Pulsed laser deposition (b) Sol-gel technique
(c) Electro deposition (d) Mechanical crushing

11. Which property of nanoparticles provides a driving force for diffusion?

(a) Optical Properties (b) High surface area to volume ratio
(c) Sintering (d) There is no such property

12. Nano crystalline materials synthesised by sol-gel technique results in a foam like structures
called ___________
(a) Gel (b) Aerosol (c) Foam (d) Aerogel
13. Which nanomaterial is used for cutting tools?

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(a) Fullerene (b) Aerogel
(c) Tungsten Carbide (d) Gold

14. What is the average particle size of ultra-fine grinders?

(a) 1 to 20 µm (b) 4 to 10 µm
(c) 5 to 200 µm (d) 50 to 100 µm

15. What does colloid mill produces?

(a) Wet and dry products (b) Emulsions and Solid dispersions
(c) Coarse and fine particles (d) Broad particles.

16. ____ is an open container usually cylindrical with uniform openings.

(a) Bowel (b) Screen
(c) Magnifier (d) Shredder

17. Ball mill is used for

(a) Crushing (b) Coarse grinding
(c) Fine grinding (d) Attrition

18. The Balls for ball mills are never made of

(a) Forged/cast steel (b) Lead
(c) Cast iron (d) Alloy steel

19. Carbon black is pulverised in a

(a) Hammer crusher (b) Ball mill
(c) Roll crusher (d) Gyratory crusher

20. Sol-gel method is ________ approach.

(a) Bottom up (b) Up bottom
(c) Top down (d) Down top

21. The sol-gel is a __________ of solid particle.

(a) Sublimation (b) Melting
(c) Colloidal suspension (d) Cool down

22. Sol-gel method is ________ chemical process.

(a) Dry (b) Wet
(c) Semi liquid (d) Semi solid

23. One of the advantages of sol-gel method is able to get uniform and _________ powder.
(a) Micro size (b) Large size
(c) Nano size (d) Small size

24. Sol-gel method can produce __________ systems.

(a) Uniform multi component
(b) Non uniform multi component
(c) Multi component
(d) Non uniform multi component

25. What’s the procedure in Top-down fabrication method?

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(a) nano-particles -> powder -> bulk
(b) powder -> bulk – > nano-particles
(c) bulk -> powder – > nano-particles
(d) nano-particle – > bulk -> powder

26. The chemical reaction taking place in the sol gel process is _______ and _______.
(a) Hydrolysis, Condensation (b) Evaporation, Reduction
(c) Hydrolysis, Conduction (d) Hydrolysis, Evaporation.
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NON-LINEAR OPTICS:
Definition:
Nonlinear Optics (NLO) is the study of the interaction of intense electromagnetic field with
materials to produce modified field, which is different from the input field, both in amplitude
(frequency) and phase.
In nonlinear optics the modification of the optical properties of a material system is made by
the light. That too only the laser light is sufficiently intense to modify the optical properties of a
material system.
Reason:
We know that the light is a part of electro magnetic spectrum. According to the electro optic
effects, when the light is pass through a material it changes the properties of the medium, (such as
refractive index) but it depends on the strength of the electromagnetic wave.
For example, if ordinary light (low intensity) passes through the material, it cannot change
the properties of the material i.e., here, the nonlinear activity is absent. Instead if the high intensity
light (laser) passes through the material it changes the properties of the material that means the
nonlinear optical activity is present. Consequently, the intensity of the light generated at the
second harmonic frequency tends to increase as the square of the intensity of the applied laser
light.
Bire fringence:
When light passes through a material the incident ray splits into two rays viz, one of same
wavelength and the other of different wavelength. This phenonmenon is called as double
refraction (or) Bire fringence. This effect is observed in NLO materials.
Examples :
(i) Second-harmonic generation
(ii) Optical mixing
(iii) Self focussing effects
(iv) Raman and Rayleigh scattering, etc.
Basic theory of nonlinear optics: HARMONIC GENERATION:
Definition:
Second harmonic generation represents the generation of new frequencies with the help of
the crystals such as quartz, potassium-dyhydro phosphate (KDP), etc.
Explanation:
Let us consider a material media in which the light is passed through it. We know that light
consists of both electric and magnetic field associated with it. These electric field associated with
the light will distort the atoms and molecules in the material to form oscillating dipoles.
The induced electric dipole is due to the displacement of electron cloud with respect to the
centre of the positive nucleus of an atom. This phenomenon is called electric polarisation (P).
Relation between P and E for ordinary light (linear medium): When light of low intensity (i.e.,

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ordinary light) is passed through dielectric medium (i.e., glass), the electric field has smaller
amplitude and the oscillation of dipoles can follow the field exactly.
Hence the relation between the electric field E and polarisation vector P can be written as,
P=ε 0 χ 0 E
where χ 0 - Electric field susceptibility
ε 0 - Permittivity of the medium
Relation between P and E for LASER beam (Non-linear medium):
When light of higher intensity (i.e. laser) is passed through dielectric medium, the electric
field has larger amplitude and the oscillation of dipoles are distorted. Therefore, some nonlinearity
is observed between P and E and hence the second harmonic generation is observed.
Thus, the polarisation vector can be written as,
P=ε 0 ( χ 0 E+ χ 1 E2 + χ 2 E3 + χ 3 E4 + …) …(1)
where, χ 0 - Linear susceptibility
χ 1 , χ 2, χ 3 - Non linear (higher order) susceptibilities
The higher order non linear susceptibilities are very small when compared to linear
susceptibilities. But the higher order susceptibilities produce so many new optical phenomina.
We know the oscillating electric field on a medium is,
E=E0 cos ωt …(2)
Substituting equation (2) in equation (1), we get
P=ε 0 ( χ 0 E0 cos ωt + χ 1 E02 cos2 ωt + χ 2 E03 cos3 ωt+ χ 3 E 04 cos 4 ωt+ …)
2 2 3 3 4 4
P=ε 0 χ 0 E 0 cos ωt +ε 0 χ 1 E0 cos ωt+ ε 0 χ 2 E 0 cos ωt+ ε 0 χ 3 E 0 cos ωt+ …
2 1+cos 2ωt 3 cos 3 ωt+ 3cos ωt
We know cos ωt = , cos ωt =
2 4

∴ P=ε 0 χ 0 E 0 cos ωt +ε 0 χ 1 E02 ( 1+ cos2 2 ωt )+ ε χ E ( cos 3 ωt +34 cos ωt )+…

0 2 0
3

ε 0 χ 1 E 02 ε 0 χ 1 E 02 cos 2 ωt ε 0 χ 2 E03 cos 3 ωt 3 3

P=ε 0 χ 0 E 0 cos ωt + + + + ε 0 χ 2 E 0 cos ωt+ …
2 2 4 4
Rearranging we get,
1
( 3 1
) 1
P= ε 0 χ 1 E02 + ε 0 E 0 cos ωt χ 0 + χ 2 E02 + ε 0 χ 1 E02 cos 2 ωt + ε 0 χ 2 E 03 cos 3 ωt
2 4 2 4
…(3)

I II III IV
Referring equation (3), the first term represents the dc field across the medium which has less
importance (since it doesn't have cos ωt term). The second term represents the external polarisation
which is called as first (or) fundamental harmonic susceptibility (since it has cos ωt ), the third term
represents the oscillating dipoles, which oscillates at a frequency 2 ω and hence called second
harmonic of polarisation. The fourth term which has cos 3 ωt is called the third harmonic of
polarisation etc.
When the first term and the third term is added we can get the term called optical
rectification. The frequency dependent polarisation is shown in Fig.(i).

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Experimental evidence:
The observation of second harmonic generation by quartz slab is illustrated Fig.(ii). A ruby
laser beam (𝜆 = 6493 Å) with average power of the order of 10 kW is focussed on a quartz slab. The
transmitted light then was passed through a filter which cuts off the red light and allows uv light
to pass through. The emerging light was incident on a photocell. Radiation with wavelength 𝜆 =
3471 Å and the power of the order of 1 mW was observed in the transmitted light.

Fig.(ii): Second Harmonic Generations

Optical Mixing:
When two coherent light sources of frequencies ω 1 and ω 2 are passed through a nonlinear
material, the mixing of the two light sources takes place and is known as optical mixing. When
two electromagnetic waves (E1 and E2) are mixed through the optical mixing process, it produces a
third wave Ep known as plasma. Therefore, the total electric field generated in the material due to
the transmission of optical light beam is
E=E1 cos ω1 t+ E 2 cos ω2 t …(4)
Substituting this in eqn.(1) becomes
P=ε 0 χ 0 ( E1 cos ω 1 t + E2 cos ω2 t)+ε 0 χ 1 (E 1 cos ω1 t + E2 cos ω 2 t)2
¿ ε 0 χ 0 ( E1 cos ω1 t+ E 2 cos ω 2 t )+ ε 0 χ 1 ¿ ….(5)
In Eq.(5), the second term is a function of angular frequency 2ω 1 and 2ω 2.
Using the trigonometric relation
2 cos α cos β=cos (α + β)+cos (α −β)
We can express the last term as
2 ε 0 χ 1 E 1 E2 cos ω 1 t cos ω2 t=ε 0 χ 1 E1 E 2 [ cos (ω 1+ ω2 )t +cos( ω1−ω2 )t ] …(6)
Eqn.(6) clearly shows that the frequencies ω 1, ω 2, 2 ω1, 2 ω2 , ω 1+ ω2 and ω 1−ω 2 are the new
waves generated. One can generate optical waves with different frequencies using the optical
arrangements. When a nonlinear material is used for optical wave generation, it generates optical
waves with different frequencies. This process is known as optical mixing. The resultant waves are
classified into two categories namely, up conversion and down conversion. The up conversion
waves are produced when the two input frequencies, i.e., ω 1 and ω 2, are summed(ω 1+ ω2 ¿. On the
other hand, the down conversion waves are produced due to the difference in the two input
signals, i.e., (ω ¿ ¿ 1−ω 2)¿.

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Examples of nonlinear materials used for the production of up conversion waves are
Potassium Dihydrogen Phosphate (KDP) and Ammonium dihydrogen phosphate (ADP), while
LiNbO3 and quartz are used for down conversion waves.
Classification of Nonlinear Optical Materials:
Generally, nonlinear materials are classified into two categories namely, molecular and bulk
materials. In molecular materials, the basic molecular units are classically bonded and interact
with bulk through Van der Waals interaction. As a result, the molecular material produces
nonlinear optical properties. The nonlinear arrangements of molecular sites determine the
nonlinear response of the material. The response of the material is used to define the nonlinear
coefficients. The nonlinear coefficients of materials are known as hyper polarisabilities. The
nonlinear property of materials occurs at molecular level and hence, the molecules are assembled
based on the requirement of nonlinear properties.
In bulk materials, the nonlinear properties mainly depend on the response of electrons which
are not associated with any individual sites. The nonlinear responses of bulk materials are
explained by the effects of band structure and the response of electrons.
Generally, when a light beam is passed through an optical material, the intensity and
frequency of the input and output lights are not related by a simple proportionality constant. The
above nonlinear property of the materials generates an additional harmonics or overtones in its
original light frequency. Based on the nonlinear properties of the materials, it is classified as
passive and active materials.
Passive Materials:
The passive materials are used to produce passive optical effects. In passive optical effects,
nonlinear effects are produced in a material without imposing their characteristic internal
resonance frequencies on to the incident beam of light. In the above process, the material acts as a
catalyst. Examples for passive optical effects are harmonic generations, frequency mixing, optical
reflection and self-focusing of light.
Active Materials:
In active materials, the characteristic resonance frequencies of the materials are imposed on
to an incident beam of light. This effect is known as active nonlinear effect. The materials which
exhibit this property are known as active materials. Examples of the optical nonlinear effects are
two photon absorption, and stimulated Raman, Rayleigh and Brillouin scattering. The passive
optical effects and the propagation of nonlinear materials, like polarisation, frequency doubling or
tripling, optical mixing, optical phase configuration, optical rectification and phase matching.
Applications of Nonlinear Optical Materials:
The nonlinear optical materials are gaining importance in designing materials and devices
due to their nonlinear optical properties. They find wide application almost in all fields of science
and technology such as optical devices, storage of data, etc. Following are some of the applications
of nonlinear optical materials.
(1) Computers:
It is used for information processing and image processing.
(2) Optical Communication:
(i) The optical bistability and optical solutions are the key process for the elements. It is used in
optical computing and long-distance fibre communications.
(ii) It is used for applications like frequency distribution or tripling of laser light, optical mixing
and telecommunication.
(iii) It is used to do radio frequency mixing; heterodyning and modulation are not at optical
frequencies employing laser beams.

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(iv) An effective coupling of light into fibre bundle using hexagonal arrays is fabricated using
phase grating.
(v) Optical phase configuration is used to achieve real-time aberration corrections in image
processing.
(3) Electronics:
Organic molecules are used as optical and electro-optical switching in photonics
applications.
Nano phase Material:
Definition:
Nanophase materials are newly developed materials with grain size at the nanometer range (
−9
10 m ), i.e., in the order of 1 – 100 nm. The particle size in a nano material is 1 nm. They are simply
called nanomaterials.
Synthesis of Nanomaterials:
The methods for the synthesis of nanomaterials are broadly classified into two ways.
(i) Top-down process (ii) Bottom-up process

(i) Top-down process:

In this process, the bulk materials are broken into nano sized particle as shown in fig.(i).

Fig.(i): Synthesis from bulk materials

Top-down process is an example of solid-state processing of materials.
Example: Mechanical alloying, Ball milling.
(ii) Bottom-up process:
In this process, nano materials are produced by building of atom by a atom as shown in fig.
(ii).

Fig.(ii): Synthesis from individual atoms

Example: Chemical Vapour Deposition.
Ball-Milling:
Principle:
In ball milling, Small hard balls are allowed to rotate inside a container (drum) and then it is
made to fall on a solid with high force to crush the solid into nano crystal.
Construction and working
The hardened steel or tungsten carbide balls are put in a container as shown in fig.(a) along

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with powder of particles (< 50 μm) of a desired material. The container is closed with tight lids.

Fig.(a): A Schematic diagram of ball mill vessel

When the container is rotating around the central axis, the material is forced to press against
the walls. The milling balls impart energy on collision and produce smaller grain size of nano
particle (fig.b).

Fig.(b): Principle of Ball Milling

Ball milling is also known as Mechanical alloying crushing.
Advantages:
Following are the advantages of ball-milling:
(1) It is used to obtain nano-structured materials at low temperature.
(2) It is a very cost effective and eco-friendly technique.
(3) It is possible to obtain large quantities of nanostructured materials.
The selection of materials of the balls plays an important role. Generally, a harder material
will be selected to synthesize the softer materials. For example, α -alumina and zirconia are used
widely as a ball for synthesizing the nanomaterials in view of their high grinding resistance
values. The relationship between the hardness and grinding resistance is shown in Fig.(c).

Fig.(c)The relationship between the micro hardness and grinding resistance

The main advantage of this method is the scaling up to tonnage quantity of materials for
wider applications. The disadvantage of this method is the contaminations of milling media and or
atmosphere and is restrictive for the production of nonmetal oxides. The nonmetal oxides require
an inert medium for milling and vacuum or glove box to handle the powder particles.
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Applications
(i) This method is preferred mainly in the preparation of elemental and metal oxide nano
crystals like Co, Cr, Al-Fe, Ag-Fe and iron.
(ii) A variety of intermetallic compounds of nickel and aluminum can be formed.
(iii) The ball mill is key equipment for regrinding. It is widely used for the preparation of cement,
the silicate product., new type building materials, fire - proof materials, chemical fertilizer, black
and non- ferrous metal, glass ceramics, etc.
SOL-GEL METHOD:
The sol gel process is a wet-chemical technique, i.e., chemical solution deposition technique
used for the production of high purity and homogeneous nanomaterials, particularly metal oxide
nanoparticles. The starting material from a chemical solution leads to the formation of colloidal
suspensions known as sol.
Then, the sol evolves towards the formation of an inorganic network containing a liquid
phase called gel. The removal of the liquid phase from sol yields the gel. The particle size and
shape are controlled by the sol/gel transitions. The thermal treatment (firing/calcinations) of the
gel leads to further polycondensation and enhances the mechanical properties of the products, i.e.,
oxide nanoparticles.
The precursors for synthesising the colloids are metal alkoxides and metal chlorides. The
starting material is processed with water or dilute acid in an alkaline solvent. The material
undergoes a hydrolysis and polycondensation reaction which leads to the formation of colloids.
The colloid system composed of solid particles dispersed in a solvent contains particles of size
from 1 nm to 1 mm. The sol is then evolved to form an inorganic network containing liquid phase
(gel). The schematic representation of the synthesis of nanoparticles using the sol gel method is
shown in Fig.

Fig. Schematic representations of sol gel synthesis of nano particles

The sol can be further processed to obtain the substrate in a film, either by dip coating or spin
coating, or cast into a container with desired shape or powders by calcinations. The chemical
reaction which takes place in the sol gel metal alkoxides M(OR) 2 during the hydrolysis process and
condensation is given above.
The sol gel method is an interesting, cheap and low temperature technique which is used to
produce a range of nanoparticles with controlled chemical compositions. One can produce the
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aero gel, a highly porous material like glass and glass ceramics, at a very low temperature by
controlling the process parameters. The sol gel derived nano particles finds wide spread
applications in various fields like optics, electronics, energy, space, bio sensors and drug delivery.
Properties of Nanophase Particles:
Physical properties: Variation of physical properties with geometry:
Let us study the geometrical arrangement of atoms and how their stability changes with size.
Starting from the bulk, the first effect of reducing the particle size is to create more surface
sites. This in turn changes surface pressure and interparticle spacing. This effect is explained in fig.
(a) for Cun particles.

Fig.(a): Interatomic distance in Cun as a function of grain size

(i) Interparticle spacing decreases with decrease in grain size for metal clusters. For example
in copper, it decreases from 2.52 (cluster size.50Ả) to 2.23A (Cu dimner)
The change in interparticle spacing and large surface to the volume ratio in particles have a
combined effect on material properties. Therefore, the nanophase materials have very high
strength and super hardness.
Because of the cluster of grains, the nanophase materials mostly free from dislocations and
stronger than conventional metals.
(ii) Melting point reduces with decrease in cluster size
The melting point of gold in nano phase (Aun) varies as a function of particle size (fig.b).
The melting point decreases from 1200 K to 800 K when the particle size decreases from 300
Ả to 20 Ả.

Fig.(b): Melting point of small Au paurtielee

(iii) Ionisation potential changes with cluster size of the nanograins
The variations in interparticle spacing and geometry will also result in the variation of
electronic properties The electronic bands in metals become narrower when the size is reduced
from bulk which changes the value of ionisation potential.
Fig.(c) shows the ionisation potential and reactivity of Fe n clusters as a function of size.
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Lonisation potentials are higher at small sizes than that for the bulk and show marked fluctuations
as a function of size.

Fig.(c): Ionisation potential and reactivity of Fe n clusters as a function of size

(iv) The large surface to volume ratio, the variations in geometry and the electronic structure
have a strong effect on catalytic properties.
As an example, the reactivity of small clusters has been found to vary by higher orders of
magnitude when the cluster size is changed by only a few atoms.
Applications of Nanophase Materials:
Nanoparticles are "the small particles with a big future". Because of their extremely small
particle size, they have extremely large specific surface area. Hence, they are chemically very
active. They are stronger and more ductile. Their electronic states are quite different from those of
bulk.
In dispersed state nanoparticles are used as fillers, paints, magnetic recording media,
ferrofluids, drugs, phosphors, rocket propellant, fuel additives etc.
In consolidate state nanoparticles are used as catalysts, electrodes of solar cells and fuel cells,
sensors, adsorbents, synthetic bone, self-cleaning glass etc.
In ordered assembly form nanoparticles are used as quantum electronic devices, photonic
crystals, DNA chips, biosensors etc.
In very dense phase nanoparticles are used in synthesis of flexible/dense ceramics and
insulators, harder metals etc.
Some of the detailed applications of nanomaterials are given below.
1. Materials Technology
 We can synthesis harder metals having hardness 5 times higher than normal metals using
nanoparticles.
 Flexible/dense ceramics and insulators have started replacing metals.
 Stronger, lighter, wear resistant, tougher and flame retardant polymers are synthesized
with nanoparticles as fillers. They are used in replacement of body parts and metals (bio-
materials).
 We can produce unusual colour paints using nanoparticles since nanoparticles exhibit
entirely different optical properties
 Smart magnetic fluids are used as vacuum seals, viscous dampers, cooling fluids, magnetic
separators etc.
 Nanometallic colloids are used as film precursors
 Useful as magneto-resistance spin valves.

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 Nanophase materials are used in nanoelectronic devices such as nanotransistors, ceramic
capacitors for energy storage, noise filters and stabilisers. The special features of these
devices include smaller sizes and reduced power losses.
 ZnO thermistors are used in thermal-protection and current-controlling devices.
2. Information Technology:
 Nanoparticles are used for data storage.
 Quantum electronic devices have started replacing bulk conventional devices.
 Nano dimensional photonic crystals are used in chemical/optical computers.
 Nanophase materials are used to produce very tiny permanent magnets of high energy
products.
 Hence, they are used in high-density magnetic recording.
 Magnetic devices made of Cu-Fe alloy are used in RAM, READ/WRITE heads and sensors.
 Quantum dots, quantum wells and quantum wires mainly produced from semiconductor
nanomaterials. Hence, they are used in computer storage (memory) devices.
3. Biomedicals:
 Biosensitive nanoparticles are used for tagging of DNA and DNA chips.
 Controlled drug delivery is possible using nanotechnology. Diffusion of medicine through
nanoporous polymer reservoir as per the requirement is very useful in controlling the
disease.
 Nanostructured ceramics readily interact with bone cells and hence finds applications as an
implant material.
4. Energy storage:
 Since the hydrogen absorbing capability increases with decrease of size of nanoparticles,
nanoparticles of Ni, Pd and Pt are useful in hydrogen storage devices.
 Useful in magnetic refrigeration
 Metal nanoparticles are very useful in fabrication of ionic batteries.
5. Optical devices:
 Nanomaterials are used in making efficient semiconductor laser and CD's.
 Nanoparticulate zinc oxide is used to manufacture effective Sunscreens.
 Nanoparticles are used in the coatings for eye glasses to protect from scratch or breakage.
6. Transmission lines:
Nanophase materials are used in the fabrication of signal processing elements such as filters,
delay lines, switches etc.
7. Nanomicro-Electro Mechanical Systems (Nano MEMS) have direct implications on integrated
circuits, optical switches, pressure sensors and mass sensors.
8. Molecular Nano-Technology (MNT) is aimed to develop robotic machines, called assemblers
on a molecular scale, molecular-size power sources and batteries.
9. Underwater nanosensor networks are used to detect the movement of ships in an efficient
manner with faster response. They can also detect chemical, biological or radiological materials in
cargo containers.

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