REPORT ON PCSIR

(Pakistan Council of Scientific and Industrial Research)

Mainly

PITMEAM (PAKISTAN INSTITUTE OF TECHNOLOGY FOR MINERALS

AND ADVANCED ENGINEERING MATERIALS)
&

MPRC (MINERAL PROCESSING RESEARCH CENTER)

SUBMITTED TO:
MR. SYED MAHMOOD ALI SHAH
SUBMITTED BY:
M. HAROON AFZAL

ROLL NO. 12
B.S(HONS) 6th SEMESTER
INSTITUTE OF GEOLOGY

PUNJAB UNIVERSITY LAHORE

 REPORT ON THE PCSIR,

LAHORE,PAKISTAN.
By

Muhammad Haroon Afzal

Institute of Geology, 6th semester, University of the Punjab, Lahore, Pakistan.

INTRODUCTION:
A study tour of Geochemistry organised by our CR Mr. Moazzam Abbas under instructions of our
incharge Mr. S.M.A. Shah to PCSIR (Pakistan Council For Scientific And Industrial Research) on Thursday,
January 13,2011. PCSIR is best institution for resarch work in Pakistan as it has some precious
equipments not found in other ones. PCSIR Lahore is situated on Ferozpur Road near Muslim Town Mor,
Lahore. We reached there at 10 am and visited two blocks, named MPRC and PITMAEM.

PITMAEM (PAKISTAN INSTITUTE OF TECHNOLOGY FOR MINERALS AND ADVANCED

ENGINEERING MATERIALS):

It is a double story building with well equipped labs containing number of machines namely as

 Optical Emission Spectrometry lab

 Sample Preparation lab
 Non destructive Testing Lab
 Coating Lab
 Biomaterial Center
 X-ray fluorescence (XRF) lab
 Thermal analysis Lab

MPRC (MINERAL PROCESSING RESEARCH CENTER):

Here we learned the processes of ore minerals enrichments, different techniques like

 Jaw Crusher,
 Hammer Crusher,
 Ball mill,
 Rod mill,
 Shaking Table
 Flotation etc.
 MINERAL PROCESSING RESEARCH CENTER

Mineral Processing:
Mineral processing, also known as mineral dressing or ore dressing, is the process of separating
commercially valuable minerals from their ores.

Unit Operations:
Mineral processing can involve three general types of unit operation:

1. Comminution – particle size reduction.

2. Concentration by taking advantage of physical and surface chemical properties.
3. Dewatering – solid/liquid separation.

Comminution:
Comminution is particle size reduction of materials. Comminution may be carried out on either dry materials
or slurries. Crushing and grinding are the two primary comminution processes. Crushing is normally carried
out on "run-of-mine"ore, while grinding (normally carried out after crushing) may be conducted on dry or
slurried material.

1. Crushing:
A crusher is a machine designed to reduce large rocks into smaller rocks, gravel, or rock dust. Crushers
may be used to reduce the size, or change the form, of waste materials so they can be more easily
disposed of or recycled or to reduce the size of a solid mix of raw materials (as in rock ore), so that pieces
of different composition can be differentiated.

Crushing is the process of transferring a force amplified by mechanical advantage through a material made
of molecules that bond together more strongly, and resist deformation more, than those in the material
being crushed do.
Crushing devices hold material between two parallel or tangent solid surfaces, and apply sufficient force to
bring the surfaces together to generate enough energy within the material being crushed so that its
molecules separate from (fracturing), or change alignment in relation to (deformation), each other.

Jaw Crusher:
A jaw or toggle crusher consists of a set of vertical jaws, one jaw being fixed and the other being moved
back and forth relative to it by a cam or pitman mechanism. The jaws are farther apart at the top than at the
bottom, forming a tapered chute so that the material is crushed progressively smaller and smaller as it
travels downward until it is small enough to escape from the bottom opening. The movement of the jaw can
be quite small, since complete crushing is not performed in one stroke. The inertia required to crush the
material is provided by a weighted flywheel that moves a shaft creating an eccentric motion that causes the
closing of the gap.

Jaw Crusher

Single and double toggle jaw crushers are constructed of heavy duty fabricated plate frames with
reinforcing ribs throughout. The crushers components are of high strength design to accept high power
draw. Manganese steel is used for both fixed and movable jaw faces. Heavy flywheels allow crushing
peaks on tough materials. Double Toggle jaw crushers may feature hydraulic toggle adjusting mechanisms.

Hammer Crusher:
The hammer crusher is one of the main equipment for intermediate and fine crushing the brittle materials
with less than intermediate such as limestone coal and other used in metallurgy, building material, chemical
and water - power industry, with a feature of big crushing ratio and even product graininess.

Hammer Crusher
2. Grinding
In this process stage, the crushed material can be further disintegrated in a cylinder mill, which is a
cylindrical container built to varying length-to-diameter ratios, mounted with the axis substantially horizontal,
and partially filled with grinding bodies ( e.g., flint stones, iron or steel balls) that are caused to tumble,
under the influence of gravity, by revolving the container.

Ball mill:
A ball mill, a type of grinder is a cylindrical device used in grinding (or mixing) materials like ores,
chemicals, ceramic raw materials and paints. Ball mills rotate around a horizontal axis, partially filled with
the material to be ground plus the grinding medium. Different materials are used as media, including
ceramic balls, flint pebbles and stainless steel balls. An internal cascading effect reduces the material to a
fine powder.

Ball mill

Ball mills are used extensively in the Mechanical alloying process[1] in which they are not only used for
grinding but for cold welding as well, with the purpose of producing alloys from powders.

The ball mill is a key piece of equipment for grinding crushed materials, and it is widely used in production
lines for powders such as including cement, silicates, refractory material, fertilizer, glass ceramics, etc. as
well as for ore dressing of both ferrous non-ferrous metals. The ball mill can grind various ores and other
materials either wet or dry. There are two kinds of ball mill, grate type and overfall type due to different
ways of discharging material. There are many types of grinding media suitable for use in a ball mill, each
material having its own specific properties and advantages. Key properties of grinding media are size,
density, hardness, and composition.

Rod mill:
Rod mills are very similar to ball mills, except they use long rods for grinding media. The rods grind the ore
by tumbling within the the mill, similar to the grinding balls in a ball mill. To prevent the conditions leading to
rod charge tangling, the length to diameter ratio is maintained at 1.4 to 1.6. Rod mills accept feed up to
about 50 mm (2 in.) and produce a product in the size range of 3000 to 270 mm (–4 to –35 mesh). Grinding
action is by line contact between the rods extending the length of the mill. Rods tumble and spin in roughly
parallel alignment simulating a series of roll crushers. This results in preferential grinding of coarse material
and minimizes production of slimes.

Rod mill

Rod mills normally carry 35 to 65% rod charge by volume. The limits on charge level are (1) keeping the
feed end trunnion open so that feed will get into the mill, and (2) keeping the rod charge low so rods will not
work their way into discharge openings where they can cause rod tangling.

Concentration:
Concentration involves the separation of valuable minerals from the other raw materials received from the
grinding mill. In large-scale operations this is accomplished by taking advantage of the different properties
of the minerals to be separated. These properties can be colour (optical sorting), density (gravity
separation), magnetic or electric (magnetic and electrostatic separation), and physicochemical (flotation
separation).

1. Gravity separation:
Historically the earliest method used, particles can be classified based on their specific gravity. Air is the
main fluid medium used for the process.

Gravity separation methods fall into three broad categories: dense-medium separation, in which the
particles are immersed in a bath containing a medium of intermediate density, so that some particles float
and others sink; separation in vertical currents, such that advantage is taken of differing rates of settlement,
as typified by jigging; and separation in streaming currents, or 'thin film sizing' as for example on a shaking
table or spiral separator. A flat, rectangular surface that can be tilted and shaken about the long axis and
has horizontal riffles for imposing restraint in removing minerals from classified sand. Also known as
shaking table.

Shaking table

Gravity concentration on inclined planes is carried out on shaking tables, which can be smoothed or
grooved and which are vibrated back and forth at right angles to the flow of water. As the pulp flows down
the incline, the ground material is stratified into heavy and light layers in the water; in addition, under the
influence of the vibration, the particles are separated in the impact direction. Shaking tables are often used
for concentrating finely grained ores of tin, tungsten, niobium, and tantalum.

1. Flotation separation:
Flotation is the most widely used method for the concentration of fine-grained minerals. It takes advantage
of the different physicochemical surface properties of minerals—in particular, their wettability, which can be
a natural property or one artificially changed by chemical reagents.
By altering the hydrophobic (water-repelling) or hydrophilic (water-attracting) conditions of their surfaces,
mineral particles suspended in water can be induced to adhere to air bubbles passing through a flotation
cell or to remain in the pulp. The air bubbles pass to the upper surface of the pulp and form a froth, which,
together with the attached hydrophobic minerals, can be removed. The tailings, containing the hydrophilic
minerals, can be removed from the bottom of the cell.

Flotation separation
Flotation makes possible the processing of complex intergrown ores containing copper, lead, zinc, and
pyrite into separate concentrates and tailings—an impossible task with gravity, magnetic, or electric
separation methods. In the past, these metals were recoverable only with expensive metallurgical
processes.

3. Magnetic separation:
Minerals such as ilmenite and magnetite are naturally magnetic, and so can be separated from non-
magnetic particles using strong magnets. There are a number of different processes that can be used.
These include HGMS, HIMS and LIMS. The HIMS and HGMS are differentiated as the HGMS separators
are a batch process while the HIMS are a continuous process. These two processes are typically used for
paramagnetic particles while the LIMS are used for ferromagnetic particles.

Magnetic separation is based on the differing degrees of attraction exerted on various minerals by magnetic
fields. Success requires that the feed particles fall within a special size spectrum (0.1 to 1 millimetre). With
good results, strongly magnetic minerals such as magnetite, franklinite, and pyrrhotite can be removed from
gangue minerals by low-intensity magnetic separators. High-intensity devices can separate oxide iron ores
such as limonite and siderite as well as iron-bearing manganese, titanium, and tungsten ores and iron-
bearing silicates.

Dewatering:
Dewatering is an important process in mineral processing. The purpose of dewatering is to remove water
contained in particles. This is done for a number of reasons, specifically, to enable ore handling and
concentrates to be transported easily, allow further processing to occur and to dispose of the gangue. The
water removed from dewatering can be recycled through a mineral processing plant. The main processes
that are used in dewatering include dewatering screens, sedimentation, filtering, and thermal drying. These
processes increase in difficulty and cost as the particle size decreases.

Filtration:
Filtration is the separation of a suspension into a solid filter cake and a liquid filtrate by passing it through a
permeable filtering material. Important factors in this process are the properties of the suspension ( e.g.,
size distribution, concentration), the properties of the filtering materials ( e.g., the width and shape of pores),
and the forces applied to the suspension. Filtration is carried out in gravity filters (screens, dewatering
bins), in centrifugal filters (screen centrifuges), in vacuum filters (drum cell filters, disk filters), or in pressure
filters (filter presses). Such devices make it possible to produce filter cakes containing 8 to 15 percent
moisture.

Thickening:
In the process of thickening (also called sedimentation), the solids in a suspension settle under the
influence of gravity in a tank and form a thick pulp. This pulp, and the clear liquid at the top of the tank, can
be removed continuously or intermittently. In comparison with filtration, thickening offers the advantage of
low operation costs; on the other hand, it has the disadvantage of leaving a higher moisture content in the
pulp. For this reason, the dewatering of pulps containing fine particles often involves a combination of
thickening and filtration. The thickening of finely grained pulps is often aided by the use of flocculating
agents.

Drying
The removal of water from solid materials by thermal drying plays a significant role in modern mineral
processing. A great number of dryer types are available. Convection dryers, employing a flow of hot
combustion gases to remove moisture from a pulp stream, are the most common. To this type belong
rotary drum, conveyor, and fluidized-bed dryers.
 PITMAEM

PAKISTAN INSTITUTE OF TECHNOLOGY FOR MINERALS

AND ADVANCED ENGINEERING MATERIALS
Lab. #01 Optical Emission Spectrometry

Optical Emission Spectrometer:

Optical emission spectrometry using Arc/Spark excitation is the reference technique for rapid, elemental
analysis of solid metallic samples.

Lab. #02 Sample Preparation

General Sample Preparation have following steps:

1. Sectioning – typically abrasive cutting

2. Mounting (optional)

3. Coarse grinding

4. Fine grinding

5. Coarse polishing – 6 micron diamond paste or 6 micron and 1 micron diamond. Rotate sample
counter to the wheel rotation. Wash after each step under running water and rinse with alcohol.

6. Fine polishing – 0.3 and 0.05 micron alumina Slurry.

Sample Mounting:
Small specimens generally require mounting so that the specimen is supported in a stable medium for
grinding and polishing. The medium chosen can be either a cold curing resin or a hot mounting compound.

1. Hot Mounting:
When preparation requirements include less expensive, uniform size and shape, and short processing
times, hot mounting (hot compression mounting) is ideal. Hot mounting takes place under pressure in a
mounting press, where the specimen is placed in a cylinder together with the appropriate mounting resin.

A temperature of up to 200ºC, and a pressure of up to 50kN are then applied during the embedding of the
specimen.
 2. Cold Mounting:
Cold mounting or embedding is when a resin is mixed with a hardener (or accelerator) to provide the
mounting compound, and then the polymerization process take place to form the block. In some cases, this
process gives-off heat. However this heat generation can be controlled by the use of ice or cool air blow
setting. Cold mounting compounds are preferred for specimens that are sensitive to the heat or
pressure, which applies during the hot mounting process.

Grinding the Sample

1. Coarse Grinding:
Grinding can be achieved in a variety of ways, using a variety of abrasives. Fixed abrasive surfaces are
available using diamond or cubic boron nitride (CBN) abrasives. The method used to bind the abrasives to
the wheel affects the grinding characteristics, the harder or more rigid the bonding medium, the more
aggressive the grinding action of the surface. Therefore metal bonded fixed abrasive wheels are the most
aggressive grinding surfaces, whereas resin bonded wheels are less aggressive.

2. Fine Grinding:

Silicon Carbide (SiC) paper is the traditional method used for fine grinding and is adequate when used
properly. SiC paper blunts quickly and therefore should be discarded after a short period of grinding in
order to maintain efficient 'stock' removal.  Grinding on a surface that has blunt abrasives causes a great
deal of surface damage by smearing, 'burnishing' and local heating.

Polishing
1. Preliminary Polishing:
Diamond polishing compounds or slurries are good for preliminary stages for most materials. Polishing is a
similar action to grinding, accept that the supporting medium used to hold the abrasive is capable far
greater 'shock absorbency' i.e. the ability of the medium to allow the abrasive to move to some degree and
conform to the surface aspirates of the specimen.  Thus different polishing surface materials have differing
characteristics: soft cloths allow the greatest shock absorbency and therefore allow for gentle polishing with
little damage associated.  However soft cloths allow the abrasive to abrade different areas at different rates,
giving rise to 'relief'.  

2. Final Polishing:
Final polishing should not be prolonged, but just sufficient to achieve the desired surface finish without
causing excessive relief.

Colloidal Silica is a chemo-mechanical polish, i.e., it combines the effect of mechanical polishing with
etching.  

Etching:
Directly polished surfaces are improved by etching.  Additionally, etching delineates the grain structure,
which is of obvious benefit.  However, etching may attack a second phase preferentially, or attack grain
boundaries excessively.  Caution should be exercised when choosing and using etches.  Materials that are
difficult to polish may benefit from repeated etching and repolishing. Using special acid or alkali resistant
cloths,  it is also possible to add dilute etchants to the polishing wheel during polishing.   This can be
effective,  but can be difficult to control.  Some experience is required.  Any etchant that is used must
dissolve the specimen surface in an even manner, and not leave behind any oxide or reaction product
layers.  Such layers can completely suppress diffraction.  

Electrolytic Polishing and etching:

Electrolytic preparation uses an electrolytic reaction cell containing a liquid electrolyte with two electrodes:
an anode and cathode. The sample to be polished/etched forms the anode. The electrodes are connected
to an external power supply and voltage applied to cause reaction within the cell.
 

Factors controlling etching/polishing characteristics include:

1. Electrolyte composition
2. Electrolyte temperature
3. Electrolyte stirring
4. Area to be polished/etched (current density)
5. Voltage

Zoom Microscope:
Zoom microscopes can greatly enhance the ability of a researcher to record his findings by allowing the
alteration of an image size from the microscope to a video monitor.

Lab. #03 Non destructive Testing Lab

Brinell scale:
The Brinell scale characterizes the indentation hardness of materials through the scale of penetration of an
indenter, loaded on a material test-piece. It is one of several definitions of hardness in materials science.

Brinell Hard Tester

Proposed by Swedish engineer Johan August Brinell in 1900, it was the first widely used and standardised
hardness test in engineering and metallurgy. The large size of indentation and possible damage to test-
piece limits its usefulness.

The typical test uses a 10 millimetres (0.39 in) diameter steel ball as an indenter with a 3,000 kgf (29 kN;
6,600 lbf) force. For softer materials, a smaller force is used; for harder materials, a tungsten carbide ball is
substituted for the steel ball. The indentation is measured and hardness calculated as:

Material Hardness
Softwood (e.g., pine) 1.6 HBS 10/100
Hardwood 2.6–7.0 HBS 1.6 10/100
Aluminium 15 HB
Copper 35 HB
Mild steel 120 HB
18-8 (304) stainless steel annealed 200 HB[4]
Glass 1550 HB
Hardened tool steel 1500–1900 HB
Rhenium diboride 4600 HB
 Lab. #04 Radiographic Lab

Ultrasonic Testing:
Ultrasonic methods use beams of sound waves (vibrations) of short wavelength and high frequency,
transmitted from a probe and detected by the same or other probes. Usually, pulsed beams of ultrasound
are used and in the simplest instruments a single probe, hand held, is placed on the specimen surface. An
oscilloscope display with a time base shows the time it takes for an ultrasonic pulse to travel to a reflector
(a flaw, the back surface or other free surface) in terms of distance traveled across the oscilloscope screen.
The height of the reflected pulse is related to the flaw size as seen from the transmitter probe. The
relationship of flaw size, distance and reflectivity are complex, and a considerable skill is required to
interpret the display. Complex mutiprobe systems are also used with mechanical probe movement and
digitization of signals, followed by computer interpretation are developing rapidly.

Ultrasonic examinations are performed for the detection and sizing of internal defects, flaws or
discontinuities in piping, castings, forgings, weldments or other components. Exact sizing techniques have
been developed to detect and monitor progressive cracking in a variety of equipment.

Dye Penetrant Testing:

This method employs a penetrating liquid, which is applied over the surface of the component and enters
the discontinuity or crack. Subsequently, after the excess penetrant has been cleared from the surface, the
penetrant exudes or is drawn back out of the crack is observed. Liquid penetrant testing can sbe applied to
any non-porous clean material, metallic or non-metallic, but is unsuitable for dirty or very rough surfaces.
Penetrants can contain a dye to make the indication visible under white light, or a fluorescent material that
fluoresces under suitable ultra-violet light. Fluorescent penetrants are usually used when the maximum flaw
sensitivity is required. Cracks as narrow as 150 nanometers can be detected.

Magnetic Particle Testing:

The Magnetic Particle Inspection method of Non-Destructive testing is a method for locating surface and
sub-surface discontinuities in ferromagnetic material. It depends for its operation on the face that when the
material or part under test is magnetized, discontinuities that lie in a direction generally transverse to the
direction of the magnetic field, will cause a leakage field, and therefore, the presence of the discontinuity, is
detected by use of finely divided ferromagnetic particles applied over the surface, some of these particles
being gathered and held by the leakage field, this magnetically held collection of particles forms an outline
of the discontinuity and indicates its location, size, shape and extent.

Dry magnetic particle examinations and wet fluorescent magnetic particle examinations are performed on
ferromagnetic materials to detect surface and slight subsurface discontinuities. Specialized wet fluorescent
magnetic particle techniques are available for black light internal examinations of equipment through
borescopes.

Eddy Current Testing (ET):

Eddy current testing is a rapid and accurate technique used to detect discontinuities in tubing, heat
exchangers, condensers, wires, plates, etc. Eddy current testing is also performed for alloy separation and
for the determination of treatment conditions. The location of repair welds, girth welds and seam welds may
also be detected on ground machined surfaces .

Lab. #05 Coating Lab

Physical Vapor Deposition (PVD):

Physical Vapor Deposition, or PVD, is a term used to describe a family of coating processes. The most
common of these PVD coating processes are evaporation (typically using cathodic arc or electron beam
sources), and sputtering (using magnetic enhanced sources or "magnetrons", cylindrical or hollow cathode
sources). All of these processes occur in vacuum at working pressure (typically 10-2 to 10-4 mbar) and
generally involve bombardment of the substrate to be coated with energetic positively charged ions during
the coating process to promote high density. Additionally, reactive gases such as nitrogen, acetylene or
oxygen may be introduced into the vacuum chamber during metal deposition to create various compound
coating compositions. The result is a very strong bond between the coating and the tooling substrate and
tailored physical, structural and tribological properties of the film.

In addition to our standard TitankoteT PVD processes, we also provide several proprietary PVD coating
processes to meet our customers' needs. Each of these processes represents a family of specific PVD
coating compositions (TiN, TiCN, etc) that are processed in order to benefit specific applications.

The term physical vapor deposition appears originally in the 1966 book Vapor Deposition by CF Powell, JH
Oxley and JM Blocher Jr, but Michael Faraday was using PVD to deposit coatings as far back as 1838.

Variants of PVD include, in order of increasing novelty:

Cathodic Arc Deposition: In which a high power arc discharged at the target material blasts away some into
highly ionized vapor.

Electron beam physical vapor deposition: In which the material to be deposited is heated to a high vapor
pressure by electron bombardment in "high" vacuum.
Evaporative deposition: In which the material to be deposited is heated to a high vapor pressure by
electrically resistive heating in "low" vacuum.

Pulsed laser deposition: In which a high power laser ablates material from the target into a vapor.

Sputter deposition: In which a glow plasma discharge (usually localized around the "target" by a magnet)
bombards the material sputtering some away as a vapor.

PVD is used in the manufacture of items including semiconductor devices, aluminized PET film for balloons
and snack bags, and coated cutting tools for metalworking. Besides PVD tools for fabrication special
smaller tools mainly for scientific purposes have been developed. They mainly serve the purpose of
extreme thin films like atomic layers and are used mostly for small substrates. A good example are mini e-
beam evaporators which can deposit monolayers of virtually all materials with melting points up to 3500°C.

Some of the techniques used to measure the physical properties of PVD coatings are:

Calo tester: coating thickness test

Nanoindentation: hardness test for thin-film coatings

Pin on disc tester: wear and friction coefficient test

Scratch tester: coating adhesion test

How Does Physical Vapour Deposition Work?
PVD processes are carried out under vacuum conditions. The process involved four steps:

1. Evaporation
2. Transportation
3. Reaction
4. Deposition

Evaporation:

During this stage, a target, consisting of the material to be deposited is bombarded by a high ebergy source
suchg as a beam of electrons or ions. This dislodges atoms from the surface of the target, ‘vaporising’
them.

Transport:

This process simply consists of the movement of ‘vaporised’ atoms from the target to the substrate to be
coated and will generally be a straight line affair.

Reaction

In some cases coatings will consist of metal oxides, nitrides, carbides and other such materials. In these
cases, the target will consist of the metal. The atoms of metal will then react with the appropriate gas during
the transport stage. For the above examples, the reactive gases may be oxygen, nitrogen and methane. In
instances where the coating consists of the target material alone, this step would not be part of the process.

Deposition

This is the process of coating build up on the substrate surface. Depeding on the actual process, some
reactions between target materials and the reactive gases may also take place at the substrate surface
simultaneously with the deposition process.

What are PVD Coatings Used For?

PVD coatings are deposited for numerous reasons. Some of the main ones are:

1. Improved hardness and wear resistance

2. Reduced friction
3. Improved oxidation resistance

The use of such coatings is aimed at improving efficiency through improved performance and longer
component life. They may also allow coated components to operate in environments that the uncoated
component would not otherwise have been able to perform.
Advantages of the Physical Vapour Deposition Process:
1. Materials can be deposited with improved properties compared to the substrate material
2. Almost any type of inorganic material can be used as well as some kinds of organic materials
3. The process is more environmentally friendly than processes such as electroplating

Disadvantages of the Physical Vapour Deposition Process:

1. It is a line of sight technique meaning that it is extremely difficult to coat undercuts and similar
surface features
2. High capital cost
3. Some processes operate at high vacuums and temperatures requiring skilled operators
4. Processes requiring large amounts of heat require appropriate cooling systems
5. The rate of coating deposition is usually quite slow

Applications:

As mentioned previously, PVD coatings are generally used to improve hardness, wear
resistance and oxidation resistance. Thus, such coatings use in a wide range of applications
such as:
1. Aerospace
2. Automotive
3. Surgical/Medical
4. Dies and moulds for all manner of material processing
5. Cutting tools
6. Fire arms

Titankote™ C(TiN) Coated Milling Cutters Titankote™ C5 (TiCN) Coated

Punches
Titankote™ C2-SL (AlTiN-CrN) Coated Aluminum Die-Casting Cavities Titankote™C5B

Titankote™ C7 (TiAlSiCN) Coated

BallnoseInserts

Lab. #06 Biomaterial Center

Hydroxyapatite (Ca10(PO4)6(OH)2):
Hydroxyapatite is chemically similar to the mineral component of bones and hard tissues in mammals. It is
one of few materials that are classed as bioactive, meaning that it will support bone ingrowth and
osseointegration when used in orthopaedic, dental and maxillofacial applications.The chemical nature of
hydroxyapatite lends itself to substitution, meaning that it is not uncommon for non-stoichiometric
hydroxyapatites to exist. The most common substitutions involve carbonate, fluoride and chloride
substitutions for hydroxyl groups, while defects can also exist resulting in deficient hydroxyapatites.

Properties
The ability to integrate in bone structures and support bone ingrowth, without breaking down or dissolving
(i.e it is bioactive).

Hydroxyapatite is a thermally unstable compound, decomposing at temperature from about 800-1200°C

depending on its stoichiometry (see above).

Generally speaking dense hydroxyapatite does not have the mechanical strength to enable it to succeed in
long term load bearing applications.

Applications
Bioceramic Coatings

Coatings of hydroxyapatite are often applied to metallic implants (most commonly titanium/titanium alloys
and stainless steels) to alter the surface properties. In this manner the body sees hydroxyapatite-type
material which it is happy to accept. Without the coating the body would see a foreign body and work in
such a way as to isolate it from surrounding tissues. To date, the only commercially accepted method of
applying hydroxyapatite coatings to metallic implants is plasma spraying.

Bone Fillers

Hydroxyapatite may be employed in forms such as powders, porous blocks or beads to fill bone defects or
voids. These may arise when large sections of bone have had to be removed (e.g. bone cancers) or when
bone augmentations are required (e.g maxillofacial reconstructions or dental applications). The bone filler
will provide a scaffold and encourage the rapid filling of the void by naturally forming bone and provides an
alternative to bone grafts. It will also become part of the bone structure and will reduce healing times
compared to the situation, if no bone filler was used.

Lab. #07 X-ray fluorescence (XRF)

X-ray fluorescence (XRF)

X-ray fluorescence (XRF) is the emission of characteristic "secondary" (or fluorescent) X-rays from a
material that has been excited by bombarding with high-energy X-rays or gamma rays. The phenomenon is
widely used for elemental analysis and chemical analysis, particularly in the investigation of metals, glass,
ceramics and building materials, and for research in geochemistry, forensic science and archaeology.
Energy dispersive spectrometry
In energy dispersive spectrometers (EDX or EDS), the detector allows the determination of the energy of
the photon when it is detected. Detectors historically have been based on silicon semiconductors, in the
form of lithium-drifted silicon crystals, or high-purity silicon wafers.

Schematic arrangement of EDX spectrometer

Wavelength dispersive spectrometry

In wavelength dispersive spectrometers (WDX or WDS), the photons are separated by diffraction on a
single crystal before being detected. Although wavelength dispersive spectrometers are occasionally used
to scan a wide range of wavelengths, producing a spectrum plot as in EDS, they are usually set up to make
measurements only at the wavelength of the emission lines of the elements of interest.

Schematic arrangement of wavelength dispersive spectrometer

Densitometer:
A densitometer is a device that measures the degree of darkness (the optical density) of a photographic or
semitransparent material or of a reflecting surface. The densitometer is basically a light source aimed at a
photoelectric cell.

Heiland Densitometer TRDZ 1

It determines the density of a sample placed between the light source and the photoelectric cell from
differences in the readings. Modern densitometers have the same components, but also have electronic
integrated circuitry for better reading. There are two types:

1. Transmission densitometers that measure transparent materials

2. Reflection densitometers that measure light reflected from a surface.

Densitometers are used for:

1. Measuring color saturation by print professionals

2. Calibrating printing equipment
3. Making adjustments so outputs are consistent with the colors desired in the finished products.

Lab#08 Thermal analysis Lab

Differential Scanning Calorimetry:

Differential scanning calorimetry or DSC is a thermoanalytical technique in which the difference in the
amount of heat required to increase the temperature of a sample and reference is measured as a function
of temperature. Both the sample and reference are maintained at nearly the same temperature throughout
the experiment. Generally, the temperature program for a DSC analysis is designed such that the sample
holder temperature increases linearly as a function of time. The reference sample should have a well-
defined heat capacity over the range of temperatures to be scanned.
The technique was developed by E.S. Watson and M.J. O'Neill in 1960, and introduced commercially at
the 1963 Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy. The term DSC was
coined to describe this instrument which measures energy directly and allows precise measurements of
heat capacity.

DSC Curve

A schematic DSC curve demonstrating the appearance of several common features

Applications
Differential scanning calorimetry can be used :

1. To observe fusion and crystallization

2. To measure the glass transition temperatures Tg.
3. To study oxidation, as well as other chemical reactions.

Glass transitions may occur as the temperature of an amorphous solid is increased. These transitions
appear as a step in the baseline of the recorded DSC signal. This is due to the sample undergoing a
change in heat capacity; no formal phase change occurs.

As the temperature increases, an amorphous solid will become less viscous. At some point the molecules
may obtain enough freedom of motion to spontaneously arrange themselves into a crystalline form. This is
known as the crystallization temperature (Tc). This transition from amorphous solid to crystalline solid is an
exothermic process, and results in a peak in the DSC signal. As the temperature increases the sample
eventually reaches its melting temperature ( Tm). The melting process results in an endothermic peak in the
DSC curve. The ability to determine transition temperatures and enthalpies makes DSC a valuable tool in
producing phase diagrams for various chemical systems.

Dilatometer
A dilatometer is a scientific instrument that measures volume changes caused by a physical or chemical
process. A familiar application of a dilatometer is the mercury-in-glass thermometer, in which the change in
volume of the liquid column is read from a graduated scale. Because mercury has a fairly constant rate of
expansion over normal temperature ranges, the volume changes are directly related to temperature.

A simple structure of a dilatometer

Applications
Dilatometers have been used in the fabrication of metallic alloys, compressed and sintered refractory
compounds, glasses, ceramic products, composite materials, and plastics.

Dilatometry is also used to monitor the progress of chemical reactions, particularly those displaying a
substantial molar volume change (e.g., polymerisation). A specific example is the rate of phase changes.

Another common application of a dilatometer is the measurement of thermal expansion.

Laser Particle Analysis:

Laser Diffraction
Laser diffraction based particle size analysis relies on the fact that particles passing through a laser beam
will scatter light at an angle that is directly related to their size. As particle size decreases, the observed
scattering angle increases logarithmically. Scattering intensity is also dependent on particle size,
diminishing with particle volume. Large particles therefore scatter light at narrow angles with high intensity
whereas small particles scatter at wider angles but with low intensity.

Light scattering patterns observed for a large particle

(upper part) and a smaller particle (lower part).
It is this behaviour that instruments based on the technique of laser diffraction exploit in order to determine
particle size.
A typical system consists of:

1. A laser, to provide a source of coherent

2. Intense light of fixed wavelength
3. A series of detectors to measure the light pattern produced over a wide range of angles

Some kind of sample presentation system to ensure that material under test passes through the laser beam
as a homogeneous stream of particles in a known, reproducible state of dispersion.

The dynamic range of the measurement is directly related to the angular range of the scattering
measurement, with modern instruments making measurements from around 0.02 degrees through to
beyond 140 degrees (figure 3). The wavelength of light used for the measurements is also important, with
smaller wavelengths (e.g. blue light sources) providing improved sensitivity to sub-micron particles.

Fig. 3: Typical laser diffraction instrument layout.

Scanning Electron Microscope

A scanning electron microscope (SEM) is a type of electron
microscope that images a sample by scanning it with a high-
energy beam of electrons in a raster scan pattern. The
electrons interact with the atoms that make up the sample
producing signals that contain information about the
sample's surface topography, composition, and other
properties such as electrical conductivity.

The types of signals produced by an SEM include :

1. Secondary electrons,
2. Back-scattered electrons (BSE)
3. Characteristic X-rays,
 4. Light (cathodoluminescence),
5. Specimen current and transmitted electrons.

Secondary electron:
Secondary electron detectors are common in all SEMs, but it is rare that a single machine would have
detectors for all possible signals. The signals result from interactions of the electron beam with atoms at or
near the surface of the sample. In the most common or standard detection mode, secondary electron
imaging or SEI, the SEM can produce very high-resolution images of a sample surface, revealing details
about less than 1 to 5 nm in size. Due to the very narrow electron beam, SEM micrographs have a large
depth of field yielding a characteristic three-dimensional appearance useful for understanding the surface
structure of a sample. This is exemplified by the micrograph of pollen shown to the right.

Back-scattered electrons (BSE):

Back-scattered electrons (BSE) are beam electrons that are reflected from the sample by elastic scattering.
BSE are often used in analytical SEM along with the spectra made from the characteristic X-rays. Because
the intensity of the BSE signal is strongly related to the atomic number (Z) of the specimen, BSE images
can provide information about the distribution of different elements in the sample. For the same reason,
BSE imaging can image colloidal gold immuno-labels of 5 or 10 nm diameter which would otherwise be
difficult or impossible to detect in secondary electron images in biological specimens

Characteristic X-rays.
Characteristic X-rays are emitted when the electron beam removes an inner shell electron from the sample,
causing a higher energy electron to fill the shell and release energy. These characteristic X-rays are used
to identify the composition and measure the abundance of elements in the sample

Magnification
A wide range of magnifications is possible, from about 10 times (about equivalent to that of a powerful
hand-lens) to more than 500,000 times, about 250 times the magnification limit of the best light
microscopes
 Schematic SEM

Tribometer:

A tribometer is an instrument that measures tribological quantities,

such as coefficient of friction, friction force, and wear volume, between
two surfaces in contact. It was invented by the 18th century Dutch
scientist Musschenbroek

Static Friction Tribometer

A tribotester is the general name given to a machine or device used to perform tests and simulations of
wear, friction and lubrication which are the subject of the study of tribology. Often tribotesters are extremely
specific in their function and are fabricated by manufacturers who desire to test and analyze the long-term
performance of their products. An example is that of orthopedic implant manufactures who have spent
considerable sums of money to develop tribotesters that accurately reproduce the motions and forces that
occur in human hip joints so that they can perform accelerated wear tests of their products.

Surface Profilometer

Profilometer is a measuring instrument used to measure a surface's

profile, in order to quantify its roughness. Vertical resolution is usually
in the nanometre level, though lateral resolution is usually poorer .

While the historical notion of a profilometer was a device similar to a

phonograph that measures a surface as the surface is moved relative
to the contact profilometer's stylus, this notion is changing along with
the emergence of numerous non-contact profilometery techniques.