ENGINEERING MATERIALS

COURSE CODE : 16EM42B

By

Shilpa G D
 Syllabus

UNIT-III
Thin Film Electronic Materials :
• Techniques for Preparation of Thin Films
• Thin Film Conducting Materials
• Thin Film Resistors
• Transparent and Conductive Thin Films
• Thin Film Magnetic Materials

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 Thin Films
Thin films, a microscopically thin layer of material deposited onto a
substrate, could be Conductive, Semi-conductive or Dielectric .

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 Thin Films
 Most engineering materials (usually called bulk materials) have
fixed properties like electrical resistivity, optical opacity, etc.
 Bulk materials have fixed properties and hence their applications
are limited. When the thickness is reduced, beyond certain limits
these properties show a drastic change

 This is called size effect and this adds flexibility in designing

devices for a particular application

 Thin film possess attractive properties and therefore can have

versatile applications.
• Devices with thin films occupy less space
• Their fabrication requires less materials, hence inexpensive.

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 PVD- Evaporation
Thermal Evaporation
Principle: The material to be deposited is placed in a filament or
boat which is resistively heated by passing a high current and the
vapour is allowed to condense on the substrate.

Heating elements : tungsten boats, C, Molybdenum, Composite

ceramics
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Advantages
• High film deposition rates
• Relative simple
• Cheap equipment

Limitations:
Limited to evaporation of metals with
relatively melting points (below 1500oC)
such as Al and Zn

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 Electron beam Evaporation
 Used for metals, ceramics (oxides and nitrides).

 Fast deposition.

 Deposition rates as high as 50 microns per second

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 Deposition rates can be controlled, as per the requirement,
from very low to very high (few Angstroms to several Microns)
– hence this process has potential industrial applications like
thin-multilayerd optical coatings to thick hard coatings (Ex:
Optical Filters, Hard Coatings, Wear-resistant thermal barrier
coatings for Aerospace, Electronics, Defence, etc.).

 Better film-adhesion due to higher energy of the evaporated

material .

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 Sputtering
• PRINCIPLE: Ejection of atoms from a material by
the bombardment of high energetic particles.
 The ”energetic particles” may be ions, neutral atoms, neutrons,
electrons or protons.
 Ions - easily accelerated using electric field – hence most
sputtering applications are performed using ions.
 Ar + e- Ar+ + 2e-

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 Features
• Sputtering yield: The average number of atoms
ejected from the target per incident ion. (0.1-10)

• It Depends on
 Ion incident angle
 Energy of the ion
 Masses of the ion and target atoms
 Surface binding energy of atoms in the target.

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Advantages of sputtering over evaporation:
• Wider choice of materials.
• Better adhesion to substrate.
• Films can be deposited over large wafer (process can be scaled)
• Sputter yield = #of atoms removed per incident ion
• Deposition rate is proportional to yield for a given plasma
energy

Disadvantages:
• High cost of equipment.
• Substrate heating due to electron (secondary) bombardment.
• Slow deposition rate. (1 atomic layer/sec).

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 DC Diode Sputtering

 Superior adhesion
 Good crystalline structure
 Target must be electrically
conductive.

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 Magnetron Sputtering
Sputtering Targets

Magnetron

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 Magnetron Sputtering
A physical phenomenon involving
The creation of plasma by discharge of neutral
gas such as Argon.

 For ion sputtering, the source material is put

on the cathode (target); for sputter
deposition, the substrates to be coated on
the anode.

 The target, at a high negative potential is

bombarded with positive argon ions
created in a (high density) plasma.

 Condensed on to substrate placed at the

anode.

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 Magnetron Sputtering
• For Dielectrics/insulators
• Advantages
– Electron Confinement
– High ionization
– Low pressure sputtering
– High purity of the films
• Disadvantages
 Non uniform erosion
 Less target utilization

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 Molecular Beam Epitaxy
• Used to develop epitaxial films with atomic thickness on to single
crystal substrates.
• Advantage: Reflection High Energy Electron Diffraction (RHEED)
is used for monitoring of growth process.

Process: The word ‘beam’ means the evaporated atoms do not interact
with each other or with other vacuum chamber gases until they reach
the wafer.
• Ultra pure elements are heated in separate knudsen/effusion cells
until they begin to slowly sublimate.

Epitaxial growth: Epitaxial growth takes place due to the interaction

of molecular or atomic beams on a surface of a heated crystalline
substrate.
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• The substrate is heated to the necessary temperature.

• Atoms on a clean surface are free to move until finding correct

position in the crystal lattice to bond.

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 Pulsed Laser Deposition (PLD)
 Used for high quality thin films
• e.g., transition metal oxides, nitrides, superconducting
materials such as YBa2Cu3O7-y (yttrium barium copper oxide)

 Ease of operation and reproducibility.

 Films do not require post-deposition annealing
 Processing variables
• laser energy,
• laser pulse repetition rate,
• substrate temperature
• oxygen background pressure.

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 PLD

Layer fabrication
• Laser beam focus on the target

• Emission of the so-called

plasma plume

• Condensation of the plasma

atoms on the substrate’s surface

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( a ) 2D layer- by-layer growth
( b ) 3D island growth
( c ) layer-by-layer followed by an island growth
( d ) step-flow growth

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 Chemical Methods
1. Sol gel : Wet chemical technique.
Used in synthesis of ceramics, polymers and other
nanostructured materials.

Sol: Sol is liquid. Continuous phase is liquid

Dispersed phase is solid
Gel: A gel is a wet solid like material in which a solid network
of interconnected nanostructures spans the volume of a liquid
medium.

Continuous phase – Solid network

Dispersed phase –liquid.
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 Sol-gel

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 Sol-gel films

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 Reactions in Sol-gel

• Hydrolysis stage
- Alkoxide (OR) groups are replaced with hydroxyl groups
(OH)
Si-OR + H2O —> Si-OH + ROH.
• Condensation of two –OH or –OH with –OR groups to produce
M-O-M bonds and water
Si-OH + RO-Si --> Si-O-Si + ROH.

• The overall reaction can be written as:

Si(OR)4 + 2H2O —> SiO2 + 4ROH

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 2. Electroplating

Used for Conduction films of gold and copper

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 Factor affects property of the film

• Electrolyte composition

• pH

• Temperature and agitation

• Potential applied between the electrodes

• Current density

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 Chemical vapour deposition
• Reactant gases introduced in the chamber, chemical
reactions occur on wafer surface leading to the
deposition of a solid film.
• E.g. APCVD, LPCVD, PECVD, most commonly
used for dielectrics and Si.

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CVD steps:
• Introduce reactive gases to the chamber.
• Activate gases (decomposition) by heat or plasma.
• Gas absorption by substrate surface .
• Reaction take place on substrate surface, film
firmed.
• Transport of volatile byproducts away form
substrate.
• Exhaust waste

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• CVD is an important technique for producing
various functional thin films in semiconductor
and electronic industry

III-V and II-VI

compound semiconductors,
C, B, Si, borides, carbides,
nitrides, oxides,
silicides, sulfides, and also
many metallic and non-
metallic elements.

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 Some of reaction steps in CVD

• RF/Heat Energy is used for CVD reactions

• Plasma Enhanced CVD (PECVD) deposition

occurs at low temperature (since electrical energy
is used for chemical reactions)

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 RF PECVD System

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Chemical vapor deposition (CVD) systems

Atmospheric cold-wall system

used for deposition of epitaxial
silicon.
(SiCl4 + 2H2  Si + 4HCl)

Low pressure hot-wall system

used for deposition of
polycrystalline and amorphous
films, such as poly-silicon and
silicon dioxide.
Figure 9-4
37
 CVD advantages and disadvantages
(as compared to physical vapor deposition)

Advantages:
• High growth rates possible, good reproducibility.
• Can deposit materials which are hard to evaporate.
• Can grow epitaxial films.
• Generally better film quality, more conformal step coverage
(see image below).
Disadvantages:
• High process temperatures.
• Complex processes, toxic and corrosive gasses.
• Film may not be pure (hydrogen incorporation…).

38
• Metal-organic chemical vapour deposition (MOCVD)
is a type of CVD that utilizes metal-organic
precursors

• Initially metal-carbon precursor used for deposition

but later metal-oxygen, metal-nitrogen are also used

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 Thin film conducting materials
Thin film conductors are widely used as interconnectors,
electrodes for thin film resistors and capacitors and welding
regions in electrical and electronic devices.

Basic requirements for thin film conducting materials are

 High Conductivity
 Good Adhesion to the underlying substrate
 Good compatibility with other materials
 Compatible to photolithographic and other processes

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Types of thin film conducting materials

Elemental thin films - fabricated using a single

metallic element (Al)

Multi layered thin films – layer may have 2 or more

metallic constitutes (Cr-Au, Ti-Pd-Au, Ti-Cu-Ni-Au)

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 A. Copper Cu
• Good electrical and thermal conductivity.
• High strength
• Excellent solderability.
• High resistance to fatigue
• Deposition Method: CVD, Thermal Evaporation, sputtering or
electrochemical plating

Problems: Poor adhesion to most dielectric substrates.

Solution: Inter-layers composed of Al, Cr, Nb or Ti can be used to
enhance the adhesion in order to achieve desired mechanical
bonding.
Add small amounts of alloying elements such as Cr and Ti
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 b. Aluminium
• Lower conductivity than Cu
• Its alloys have good adhesion property to the
dielectric substrates.
• Good corrosion resistance in atmosphere and in many
chemicals and solutions.
• Deposition Method: Vacuum Evaporation

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 Au and Ag
 Au
• High electrical conductivity
• Corrosion resistant
• Environmental stability
• Deposition Method: evaporation or sputtering
• Inter layers of Ti or Cr are used to improve the adhesion.
• Used as top layer to protect other metallic layers.

 Ag
• Good conductivity
• Deposition Method: evaporation or Electro chemical
deposition
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Cr-Au and NiCr-Au
• widely used multi-layered conducting thin films.
• Cr and NiCr films are used to improve the interfacial
adhesion
• Au film is the conducting film.
• At elevated temperatures, inter-diffusion between
these two sub-layers may occur, leading to the
formation of undesired compounds or structural
defects, and then resulting in increased electrical
resistance and decreased surface property, reliability,
and stability.
• In comparison with Cr- Au system, NiCr-Au system
has a lower inter-diffusion probability.
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Ti-Pd(Pt)-Au
• Better resistance stability under humid conditions
compared with NiCr-Au system.
• Excellent corrosion resistance since Ti has superior self-
passivation ability under most atmospheric conditions.
• The Pd or Pt layer sandwiched between the bottom Ti
layer (to improve interfacial bonding) and
• The top Au layer : Inhibit the inter-diffusion
• Ti, Pd, Pt, and Au layers can be prepared by evaporation
or sputtering techniques.

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FeCrAl – Cu - Au
• Widely used as end contacts for thin film resistors,
interconnectors and welding joints.

• When compared with NiCr-Au thin films

• FeCrAl-Cu-Au films have better interfacial bonding

strength, solderability and stability.

• Inter-diffusion between FeCrAl and Cu layers could still

happen when the temperature of heat treatment is high.

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 Comparison of Thin Film Conducting
Materials
S.No Material Specifications

1 Cu  Good electrical conductivity Poor adhesion to most

 Thermal conductivity dielectric substrates.
 High strength Inter-layers composed of Al,
 High resistance to fatigue Cr, Nb, or Ti had been used
 Excellent solderability to enhance the adhesion

2 Al  Acceptable degree of
adhesion
 Good corrosion resistance
3 Au  High electrical conductivity Ti or Cr used as intermediate
 Excellent corrosion layer for adhesion
resistance
 Environmental stability

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 4 Ag Excellent conductivity Mainly used as contacts

5 Cr-Au and most widely used multi- Inter -diffusion between

NiCr-Au layered layer occur at High temp
conducting thin films NiCr-Au less Inter –
Cr and NiCr used as diffusion than NiCr
adhesive layer

6 Ti-Pd(Pt)-Au  better resistance stability Au layer used to reduce

under humid conditions inter diffusion b/w Ti &
 excellent corrosion Pd(or Pt)
resistance

7 FeCrAl-Cu-Au End contacts for thin film  better interfacial

resistors, bonding strength
 Solderability
 stability

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 Thin Film Resistors
• 40-50% of components in circuits

• Requirements

Low temperature coefficient of resistance (TCR)

Low voltage coefficient of resistance (VCR)

Sufficient stability.
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 Thin Film Resistors
• A thin layer of resistor material deposited onto a suitable substrate
(e.g., silicon, GaAs, or Al203).
• The deposition technique: Sputtering.
• The resistance value of a thin film resistor is given by the
relation

Rs - the sheet resistance of the film,

l - the length
w - width of the resistor.

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• Three major design principles of discrete thin film resistors,
including:
a. CHIP-type
b. MELF-type
c. Leaded type

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 Design Types

a) CHIP-type b)MELF-type c) Leaded Type Metal electrode

leadless face
(MELF)

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 Thin Film Resistors
S.N Materi Specifications
o al
1 Ni-Cr  Alloy composition of  TCR(-ve) for higher Cr
80:20%
 TCR control achieved by Au, Al and
 110 to 300 μΩ⋅cm. O2 as dopants
 Unstable under high humidity
 silicon monoxide and polyimide
used to increase the stability
 DC or RF magnetron sputtering
2 Cu-Ni  resistivity below 50  34 and 56 at.% Ni, show zero TCR
μΩ⋅cm
3 Cr  good adhesive strength  Resistivity is better than Ni-Cr
to substrate  TCRs are not as good as Ni-Cr

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4 Ta(Tantalum) TCR (-ve) transparency in the visible
wide range of resistivity (10- and IR range of 400-800
1000 μΩ-cm) nm, high durability, superior
high stability corrosion
highly prone to contamination resistance, and excellent
while deposition mechanical protection
5 Ta-Al •Amorphous Ta-Al film Inter -diffusion between
resistors layer occur at High temp
•Ta:Al(1:1) NiCr-Au less Inter –
•high resistivity diffusion than NiCr
•good thermal stability

6 Tantalum •High resistivity tantalum oxynitride films

nitride •Low temperature coefficient deposited using sputtering
of resistance (TCR) with Oxygen gases
•Ta2N more stable than TaN

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7 Cermet •ceramic-metal composites
•Cr-Si-O is insulating SiO2
matrix in which Cr
•Cr(80%),SiO(20%) at
550 μΩ⋅cm.
•103 to 105 μΩ⋅cm by
varying Composition of Cr
& SiO

8 RuO2 The films show positive Thin films of RuO2

TCR in a wide temperature on SiO2/Si shows TCR (-
region from 4.2 to 300 K. ve)

The realization of both negative and positive TCRs of the film

made it feasible for zero TCR resistor applications

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 Transparent and Conductive Thin Films

• Optical transparency

• Electrical conduction

• Extremely thin films of metals such as Ag, Au or

Cu can be transparent

• For E.g., Glass with Ag coatings used in Windows

for thermal cooling

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• Transparent conducting oxides (TCOs) Wide -
bandgap oxide semiconductors.
For e.g., Cd oxide (CdO), In2O3

• CdO is fabricated using sputtering of Cd metal

after incomplete thermal oxidation
In CdO oxide used to lends free charge carriers
• SnO2 + In2O3:Sn indium tin oxide or
ITO
Many e.g., for TCOs=> Cd2SnO4, CdSnO3,
CdSb2O6, CdIn2O4, ZnO, ZnSnO3, Zn2SnO4,
Zn2In2O5, MgIn2O4, GaInO3 and In4Sn3O12

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 Figure of merit for TCOs
• FOM =
Incident light energy

Reflection

Thin Film
• Sheet Resistance Transmission
• t= Thickness of the film
• T = Total visible transmission
•
The larger is the
R=total visible reflectance value of σ/α the
better is the
performance of
the TCO films.
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 Tin oxide (SnO2)
• SnO2 doped with F or Sb  energy-efficient windows

F:SnO2 deposited from SnCl2 precursors

• Direct Bang Gap 4.0 eV, Indirect Bang Gap 2.6 eV.

• Resistivity is on the order of 6 x10-4 Ω⋅cm,

• Mobility is 20 cm2/V⋅s,

• Carrier concentration of 5–8×1020 cm-3.

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• Tin oxide is less cost compare to ITO even though
electrical conductivity is poor than later

• Deposited by spray pyrolysis from the chlorides

• Photovoltaic applications such as heterojunctions

solar cell based on SnO2

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 Indium tin oxide (ITO)
•
40 atoms and
two non-
equivalent cation
sites

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• 3 Types
1. Crystalline ITO (c-ITO)

2. amorphous ITO (a-ITO)

3. amorphous IZO (a-IZO)

• DC or RF magnetron sputtering deposition

ITO sintered In2O3 + 3–10 wt.% SnO2
IZO sintered In2O3 + 7–10 wt.% ZnO

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• Crystalline ITO deposited onto heated substrates (250–
350 °C) offers relatively low resistivity's (1–3×10-4 ⋅cm)

• Both a-ITO and a-IZO films have slightly inferior

electrical transport properties compared with c-ITO

ITO/IZO
(For E.g., ITO (40 nm)
Thin metallic film To decrease the
(E.g., Ag (15 nm)& ref index n ~2) Resistivity(E.g reduce
ITO/IZO factor of ~20)
(E.g., ITO (40 nm))

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 Zinc oxide (ZnO)

• Undoped state ZnO High Resistivity

• Doping with Al, In or Ga increase its conductivity.

• Al-doped ZnO (AZO) require high degree since Al high

affinity with oxygen(it become Al203 than ZnO)

• Ga is less reactive better suited to doping with ZnO

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• bond length of Ga - O (0.192 nm) < Zn - O (0.197
nm)
So the lattice defects minimal while doping

• Al and Ga-doped ZnO (AZO or GZO) resistivity in

the order of 10-4 Ω⋅cm
• Deposition techniques:
Vacuum arc plasma evaporation (VAPE)
Metal organic molecular beam deposition (MOMBD)
Metal organic chemical vapour deposition (MOCVD)
Magnetron sputtering.

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• AZO films with a lower resistivity of the order of 10-5
Ω⋅cm have been prepared by PLD.

• AZO/ GZO Features

resistivity of 2–3×10-4 Ω⋅cm,

refractive index(n)~2.0,

Transmittance avg >85% (Deposition temp at ~200°C.0

• Low cost, high chemical and thermal stability

• Disadvantage: Zn is more chemically active in an

oxidizing atmosphere
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 Application of TCO
• Window layers of solar cells
• Front electrodes in flat panel displays
• Electromagnetic shielding of CRT in video display
terminals
• Electrochromic (EC) materials in rear view mirrors of
automobiles
• Touch -sensitive control panels
• Defrosting windows in refrigerators and airplanes

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• Invisible security circuits
• Gas sensors, biosensors
• Organic light emitting diodes (OLED)
• Polymer light emitting diodes (PLED)

• Some of New Applications:

high-refractive index waveguide overlays for sensors
and telecommunication applications
Holographic recording media
write-once read-many-times memory chips (WORM)
Electronic ink and etc.

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 Thin Film Magnetic Materials
• Soft magnetic thin films:
• Magnetic recording heads  Soft magnetic
thin films

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 The basic requirements
• High magnetic saturation (BS >> 1Tesla);

• Low coercivity for low hysteresis loss (Hc < 80 A/m)

Coercivity the resistance of a magnetic material to changes
in magnetization

• Optimal anisotropy field (Hk) for high permeability (μ)

• Zero or near zero magnetostriction (λ) for reduced domain noise

and head instability

magnetostrictionchange their shape or dimensions during the

process of magnetization.
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• High-electrical resistivity (ρ) for low eddy
current loss
– eddy current a localized electric current induced
in a conductor by a varying magnetic field

• Well-defined uniaxial anisotropy for domain

structure control

• Good thermal stability, excellent corrosion and

wear resistance.

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 Soft magnetic thin films categories

Micro /Nano-
Crystalline Amorphous
crystalline

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 Crystalline soft magnetic films
• Ni-Fe alloy (Permalloy) is one of the typical crystalline
alloys

• Ni80Fe20 alloy has been used for thin film inductive head

• Since NiFe has coercivity (Hc) of magnetic recording

media , So high Saturation magnetic flux density (Bs) is
required

• Fe-A1-Si (Sendust) and Fe-Ga-Si-Ru have higher Bs

(1.3T) Constructed as metal-in-gap (MIG) type VCR
heads

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 Micro-/nano-crystalline soft magnetic
films
• Improve the saturation flux density of soft magnetic films 
high Bs

• Films are prepared by electrodeposition

• CoFe with Bs = 1.8–1.9 T

• CoNiFe with Bs = 1.6–1.8 T

• FeN based films and NiFe/CoFeN/NiFe (Sputtered) 1.4-1.9

T and 2.4 T

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• Electrochemical deposition is preferred for CoNiFe due
to simplicity and cost-effectiveness

• Co65Ni12Fe23(with grain diameters of 10 to 20 nm)

Bs 2T

• DisAdv of electrodeposited films more susceptible to

corrosion than PVD

• iron-based alloys(Fe-M-X) M is a transition metal from

group III-V & X is C, N or O deposited using sputtering

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Advantage of Ion-based-Alloy using Sputtering

• improved corrosion resistance

• high resistivity
• High thermal stability,

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 How data is stored in hard disk

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 Giant Magnetoresistive Film – why is
it useful?
• Discovery and application of the GMR phenomenon
is responsible for the ubiquitous availability of
economical, high density information storage in our
society.

• Compact 160 GB Mp3 players and 1-2 TB hard

drives, now widely available, owe their existence to
GMR and subsequent related advances.

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• GMR is the change in electrical resistance in
response to an applied magnetic field

• The application of a magnetic field to a Fe/Cr

multilayer resulted in a significant reduction of
the electrical resistance of the multilayer

• Electrical Resistance decreases by around 10-80%

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 Discovery of GMR
Fert and Grünberg
• Discovered by independently by Professor Albert Fert of
Université Paris-Sud in France and Professor Peter Grünberg
of Forschungszentrum in Jülich, Germany.

• System:
– a thin layer of nonmagnetic material sandwiched
between two layers of magnetic material.

• Right: a Fe-Cr-Fe trilayer used in Grünberg’s original

experiment.

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 Granular GMR
• An effect that occurs in solid precipitates of a magnetic
material in a non-magnetic matrix.

• Matrices of copper containing cobalt granules. The reason for

this is that copper and cobalt are immiscible, and so it is
possible to create the solid precipitate by rapidly cooling a
molten mixture of copper and cobalt.

• Ex: Fe-Ag, Co- Ag.

• Preparation: Evaporation, Sputtering, ion implantation

• GMR effect varies with concentration, size, and morphology

of magnetic granules.

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 Multilayer GMR
• NM of thickness ~1nm, Cr, Cu, Ag, Au etc (non
magnetic transition metal)

Deposition
PVD
E-Beam evaporation
Laser ablation
sputtering

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 Applications of GMR

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