Ceramic Materials I: Asst - Prof. Dr. Ayşe KALEMTAŞ

CERAMIC
MATERIALS I
Asst. Prof. Dr. Ayşe KALEMTAŞ
Office Hours: Wenesday, 09:30-10:30 am.
akalemtas@mu.edu.tr, akalemtas@gmail.com, Phone: 211 19 17

Metallurgical and Materials Engineering Department
Powder Preparation Methods
Common Chemical Powder Preparation Methods for Ceramics
Method Advantages Disadvantage

Solid-state reaction
 Decomposition, reaction between solids Simple apparatus Agglomerated powder
Inexpensive Limited homogeneity for
multicomponent powders
Liquid solutions
 Precipitation or coprecipitation; solvent  High purity, fine particle  Expensive, poor for non-oxides,
vaporization (spray drying, spray pyrolysis, size, composition control, powder agglomeration commonly a
freeze drying); gel routes (sol-gel, Pechini, chemical homogeneity problem
citrate gel, glycine nitrate)
 Non-aqueous liquid reaction  High purity, fine particle  Limited to non-oxides
size
Vapour phase reaction
 Gas-solid reaction  Commonly inexpensive  Commonly low purity, expensive
for coarse particle size for fine powders
 Gas-liquid reaction  High purity, fine particle  Expensive, limited applicability

size
 Reaction between gases  High purity, fine particle  Expensive for non-oxides,
size, inexpensive for agglomeration commonly a
oxides problem
Vapour Phase Reactions
Comparison of the coating processes.

Development of vapour deposition technology

Chemical Vapor Deposition
The industrial exploitation of CVD could be traced back to a patent literature by
de Lodyguine in 1893 [1] who had deposited W onto carbon lamp filaments
through the reduction of WCl6 by H2. Around this period, the CVD process was
developed as an economically viable industrial process in the field of extraction
and pyrometallurgy for the production of high purity refractory metals such as Ti,
Ni, Zr and Ta.
Chemical Vapour Deposition (CVD) of films and coatings involve the chemical
reactions of gaseous reactants on or near the vicinity of a heated substrate
surface.
This atomistic deposition method can provide highly pure materials with structural
control at atomic or nanometer scale level.
Moreover, it can produce single layer, multilayer, composite, nanostructured, and

functionally graded coating materials with well controlled dimension and unique
structure at low processing temperatures.


Chemical Vapor Deposition - Advantages
Although CVD is a complex chemical system, it has the following distinctive
advantages:
(a) The capability of producing highly dense and pure materials.

(b) Produces uniform films with good reproducibility and adhesion at reasonably
high deposition rates.
(c) CVD is a non-line-of-sight process with good throwing power. Therefore, it can
be used to uniformly coat complex shaped components and deposit films with good
conformal coverage. Such distinctive feature outweighs the PVD process.
(d) It has the ability to control crystal structure, surface morphology and orientation
of the CVD products by controlling the CVD process parameters.



In CVD, powders and microcrystalline products are prepared from reactants in
the vapor phase, then can be deposited on a substrate to form single crystal films
for devices.
• Volatiles starting materials are heated to form vapors, then mixed at a suitable
temperature and transported to the substrate by carrier gas.
• Typical starting materials include hydrides, halides, and organometallic

compounds, since these tend to be volatile.
• When an organometallic precursor is used, it is called MOCVD (Metal Organic

Chemical Vapor Deposition).


CVD is used to grow a thin layer of advanced materials on the surface of a
substrate
Applications: Integrated circuits, optoelectronic devices and sensors, catalysts,

micromachines, and fine metal and ceramic powders, protective coatings

Fundamental Chemical Vapor Deposition Processes

Chemical Vapor Deposition (CVD) Reactions




Chemical Vapor Deposition (CVD) Reactor Types
• Chemical Vapor Deposition (CVD)
• Metal Organic CVD (MO-CVD)
• Atmospheric pressure CVD (AP-CVD)
• Low-pressure CVD (LP-CVD)
• Ultrahigh vacuum CVD (UHV-CVD)
• Aerosol assisted CVD (AA-CVD)
• Direct liquid injection CVD (DLICVD)
• Microwave plasma-assisted CVD (MP-CVD)
• Plasma-Enhanced CVD (PE-CVD)
• Remote plasma-enhanced CVD (RPE-CVD)
• Atomic layer CVD (ALCVD)
• Combustion Chemical Vapor Deposition (CCVD)
• Hot wire CVD (HWCVD)
• Hybrid Physical-Chemical Vapor Deposition (HPCVD)
• Rapid thermal CVD (RTCVD)
• Vapor phase epitaxy (VPE)

Chemical Vapor Deposition (CVD) Reactor Types

Applications of CVD

Applications of CVD

Advantages and Limitations of CVD

Physical vapor deposition (PVD)
Physical Vapor Deposition (PVD) is a collective set of processes used to deposit thin layers of material,
typically in the range of few nanometers to several micrometers. PVD processes are environmentally friendly
vacuum deposition techniques consisting of three fundamental steps :
Vaporization of the material from a solid source assisted by high temperature vacuum or gaseous plasma.
Transportation of the vapor in vacuum or partial vacuum to the substrate surface. Condensation onto the
substrate to generate thin films.
Different PVD technologies utilize the same three fundamental steps but differ in the methods used to generate
and deposit material. The two most common PVD processes are thermal evaporation and sputtering. Thermal
evaporation is a deposition technique that relies on vaporization of source material by heating the material
using appropriate methods in vacuum. Sputtering is a plasma-assisted technique that creates a vapor from the
source target through bombardment with accelerated gaseous ions (typically Argon). In both evaporation and
sputtering, the resulting vapor phase is subsequently deposited onto the desired substrate through a
condensation mechanism.
Deposited films can span a range of chemical compositions based on the source material(s). Further
compositions are accessible through reactive deposition processes. Relevant examples include co-deposition
from multiple sources, reaction during the transportation stage by introducing a reactive gas (nitrogen, oxygen
or simple hydrocarbon containing the desired reactant), and post-deposition modification through thermal or
mechanical processing.

• Physical vapor deposition (PVD) refers to a family of
processes in which a material is converted to its vapor
phase in a vacuum chamber and condensed onto a
substrate surface as a thin film.
• PVD can be used to produce coatings of a wide variety of
materials:
• metals
• alloys
• ceramics
• glasses
• semiconductors
• polymers
• All PVD processes consist of the following steps:

 synthesis of coating vapor,
 vapor transport to the substrate,
 condensation of vapors onto the substrate surface to
form a thin film.
• These steps are carried out inside a vacuum chamber, so
evacuation of the chamber always precedes the PVD
process.

• The two most common PVD processes are:
• evaporation
• sputtering
• For evaporation, the background pressure in the vacuum
chamber is typically ~10-6 Torr (~10-4 Pa) or lower.
• In order to evaporate a material, it must be heated to a
temperature at which its vapor pressure is 10-3 Torr or
higher.
• E.g., aluminum must be heated to 1000 C or more.

General features
 absence of chemical reaction during the deposition process;
relatively low temperatures (250 … 600ºC) in comparison


with chemical vapour deposition (CVD) processes;
 electric [and magnetic] field is applied;
the variety of PVD technologies can be classified into three

types: evaporation, sputtering and arc evaporation.


• The two most common PVD processes are:
• evaporation
• sputtering
• For sputtering, the background pressure in the vacuum
chamber is typically 10-3 to 10-2 Torr (~1 Pa).
• In sputtering, the source material is usually in the form of a
sheet or plate, called a target.
• Sputtering is achieved by bombarding the target with
energetic ions, typically Ar+.
• Atoms on the surface of the target are dislodged by this
bombardment and fly off .
• These atoms then impinge on the substrate, resulting in
deposition of a thin film.
• The physical vapor deposition technique is based on the formation of vapor of
the material to be deposited as a thin film. The material in solid form is either
heated until evaporation (thermal evaporation) or sputtered by ions
(sputtering). In the last case, ions are generated by a plasma discharge usually
within an inert gas (argon). It is also possible to bombard the sample with an
ion beam from an external ion source. This allows to vary the energy and
intensity of ions reaching the target surface.

PVD Applications
PVD is used in a variety of applications, including fabrication of microelectronic
devices, interconnects, battery and fuel cell electrodes, diffusion barriers, optical
and conductive coatings, and surface modifications

CVD vs. PVD
• Chemical Vapor Deposition (CVD) relies

on chemical reactions between reactants
in the gas phase and/or on the substrate
surface.
• Physical Vapor Deposition (PVD) is a
thermal evaporation driven or energy
driven process.

THE END
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CERAMIC

Office Hours: Wenesday, 09:30-10:30 am.

akalemtas@mu.edu.tr, akalemtas@gmail.com, Phone: 211 19 17

Method Advantages Disadvantage

 Gas-liquid reaction  High purity, fine particle  Expensive, limited applicability

Comparison of the coating processes.

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Moreover, it can produce single layer, multilayer, composite, nanostructured, and

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

(a) The capability of producing highly dense and pure materials.

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

• Typical starting materials include hydrides, halides, and organometallic

• When an organometallic precursor is used, it is called MOCVD (Metal Organic

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Applications: Integrated circuits, optoelectronic devices and sensors, catalysts,

Asst. Prof. Dr. Ayşe KALEMTAŞ

Fundamental Chemical Vapor Deposition Processes

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

• All PVD processes consist of the following steps:

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

relatively low temperatures (250 … 600ºC) in comparison

with chemical vapour deposition (CVD) processes;

 electric [and magnetic] field is applied;

the variety of PVD technologies can be classified into three

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

Asst. Prof. Dr. Ayşe KALEMTAŞ

• Chemical Vapor Deposition (CVD) relies

Asst. Prof. Dr. Ayşe KALEMTAŞ

Thanks for your kind

Asst. Prof. Dr. Ayşe KALEMTAŞ

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