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LIST OF EXPERIMENTS

Sr. Page
No NAME OF EXPERIMENTS
No

1 Examination and testing of Mullite (3Al2O 3 .2SiO2 ) and (Fe) powder. 2

(a) The compaction of MgO powder.


(b) The compaction of a mixture of different concentration of
Mullite and MgO powders. 7
2 AND
(c) Sintering of compacted MgO and mixture of Mullite and MgO powders.

3 Powder processing and preparation of TiO2 and Fe powders. 13

Sintering of compacted mixtureTiO2 and Fe powders. 15


4

Liquid phase sintering of BaCO3-MgO System. 17


5

6 (a) The compaction of a mixture of Silica and FeO powders.


AND 21
(b) Sintering of compacted mixture of Silica and FeO powders.

(a) Compaction of cast iron powder. 25


7 (b) Sintering of Compacted Cast Iron
(c) Compaction of a mixture of Cast Iron and Silica powders.
(d) Sintering of compacted mixture of silica and cast iron powders.

1
EXPERIMENT NO.1
Examination and testing of mullite (3Al2O 3 .2SiO2 ) and (Fe) powder.
1.1 Objective:
The objective of this experiment is to familiarize the student about the simple examination and
testing techniques of powders and getting the properties of powder and their effect on the
processing characteristics.

1.2 Introduction:
The processing characteristics of a powder are related to its particle and bulk characteristics. Testing can
be of a restricted nature, involving only such simple test as microscopic examination, flow bulk density
and sieving tests etc.

Mullite is a rare silicate mineral of post clay genesis. Mullite has no charge balancing cations present.

1.3 Applications of mullite:


1) Mullite is used as the refractory applications like the lining of furnaces.
2) It is also used in electrode parts.
3) It is used as a kiln furniture.
4) bricks for the glass industry.

Iron powder is formed as a whole from several other iron particles. The particle sizes vary anywhere from
20-200 mu.m. The iron properties differ depending on the production method and history of a specific
iron powder.
1.4 Applications of Iron Powder:
1) Iron powder is used as automobile parts.
2) It is used in a different engine parts. such cam shaft pulley crank shaft pulley, pulley Crank,
bearing Valve seat
3) 3) It is also used in a different seats and door parts, Seat lifter cam set, door mirror plate clutch,
Striker, Slider.
4) It is used in transmission parts.
5) Steering parts, suspension, and brake parts
6) Machine parts, Hand Warmers, High strength/wear-resistant parts,
a. Magnetic materials
1.5 Apparatus used:
1) Mullite powder
2) Iron powder
3) Weighting balance
4) Filter paper
5) Gloss sintered paper
6) Test tube(5cm3,10cm3)
7) 100ml Measuring cylinders
8) Mask
9) Printing paper

2
1.6 Procedure:
Examination and testing of powders (mullite &iron) and Perform following tests on mullite and
iron powder provided to you.
1. Visual test
2. Tactile test
3. Adhesion test
4. Flow test
5. Packing test
6. Sedimentation test

1. Sieve analysis:
Carefully examine the particle dimensions. We done Sieve Analysis by just taking two sieves having
mesh no 100, 53 and an pan having zero mesh number sieves taking from,

Model:
ASTM E11

Observation and Calculation:

Mulite powder:
Page Weight =2.6g

Page + powder weight=17.6g

Final powder weight=15g

Iron powder:
Page weight = 2.6g

Page+ powder weight=7.6g Figure1.1: Sieve analysis (ASTM E 11)


Final powder weight=5g

3
Observation and Calculation
Mullite powder Iron powder

Sr. no Mesh size Weight Sr. no Mesh size Weight


retained retained
( micron) (micron)

1 100 1.6g 1 100 0.01g

2 53 2.6g
2 53 0.9g
3 0 10.6g

Weight 0.8g 3 0 3.9g

Loss Weight loss 0.19g

2. Tactile Test:

Rub a sample of powder between finger and thumb; if gritty the powder is possibly of sieve size, for a
flour-like smooth quality the powder is composed of particle finer than 10 micron diameter. Note any
adhesion of powder to the finger, which suggest a fine, flour-like powder.

Observation and Calculation:

Mullite powder Iron powder

As Adhesion of powder to the finger happened so As Adhesion of powder to the finger happened so
the powder is fine, flour-like. the powder is fine, flour-like.

3. Adhesion Test:
Three types of papers are used,(filter paper ,gloss finished paper and printing paper).pour a small
portion of powder on each paper and remove the powder by up-ending the paper if powder stick in
each paper it means that, the powder mesh size is smaller than paper mesh size. If powder flow, it
means that powder mesh size is larger than paper mesh size. Some powder will flow and some will
not.

4
Observation and Calculation
Mullite powder Iron power

Paper Paper size Powder Paper Paper size Powder


used retained used retained
(Micron ) (Micron )

Filter 100 12-13% Filter 100 35-40%


paper paper

Gloss 5 2.5% Gloss 5 1.8%


paper paper

Printing 20-40 40-50% Printing 20-40 25-30%


paper paper

4. Flow Test:
Pour the powder into the test tube. Tapping the tube for few second then see the powder after tapping.

Observation and Calculation:


Mullite powder Iron powder

Flow is a bit wave-like so it shows that the particles Flow is a bit wave like so it shows that most of the
are fine in the powder particles are fine in the powder

5. Packing Test:
Firstly weighted of the test tube. Fill the2/3rd of test tube with a sample of powder. Note the height of the
powder. Also measure the mass of the powder. Tapping the test tube in 1 min. Note the decrease or
increase in volume on tapping. Again note the mass of the powder. And calculate the density.

5
Observation and Calculation:
Mullite powder Iron powder

Tube weight=4.8g Tube weight=4.8g


Tube +powder weight=7.5g Tube +powder weight=9g
Powder weight=2.7g Powder weight=4.2g
Initial height=4.3cm Initial height=1.7cm
Final height=2.7cm (after tapping) Final height=1.1cm (after tapping)
=4.3-2.7cm =1.7-1.1cm
=1.6cm =0.6cm
Result compaction (%) Result compaction (%)
=(1.6/4.3)*100 = (0.6/1.7)*100
=37.20% =35.3%

Sr. .no Packing density Sr. no Packing density


Group 1 38.47% Group1 36.2%
Group 2 41% Group 2 39%
Group 3 33.33%
Group 3 30.1%
Group 4 29.98%
Group 4 36.83%
Group 5 37.20%
Group5 35.3%

Average 35.996%
Average 35. 486%

Sedimentation Test: Fill the tube with 5ml water then add same amount of water into it. Then calculate
the time of settling.

Observation and Calculation:


Mullite powder Iron powder
Sr. no Mullite powder settling Iron powder settling time
time (sec) (sec)
1 10.5 sec 11.5sec
2 11.9 sec 11.5sec
3 10.5sec 9sec
Average 10.8sec 10.6sec
1.7 Result: Mullite (3Al2O 3 .2SiO2 ) and (Fe) powders are performed by different tests and obtained
very fine and flour-like properties.

6
EXPERIMENT NO.2
(a) The compaction of MgO powder.
(a) 2.1 Objective:
The objective of this experiment is to get the green density of powders and their effect on the processing
characteristics.

(a) 2.2 Introduction:


Magnesium oxide is hygroscopic, resulting in the uptake and retention of moisture under certain humidity
and temperature conditions. Magnesia or magnesium oxide is an alkaline earth metal oxide. The majority
of magnesium oxide produced today is obtained from the calcinations of naturally occurring minerals.
Magnetite, MgCO3, is being the most common.

(a) 2.3 Applications of MgO:


1) MgO more suited to refractory applications.
2) Fused MgO is used for a variety of refractory and electrical applications.
3) MgO powder is widely used as a filling for electrical heating elements for applications in
contact with air or liquid

(a) 2.4 Characteristics of MgO:

1) Moisture Penetration.
2) Dielectric Strength (Although the dielectric strength of magnesium oxide insulation
decreases with temperature),
3) Insulation Resistance (The insulation resistance of magnesium oxide decreases with
increasing temperatures)
4) Unlike most electrical insulations, magnesium oxide has a relatively high thermal
conductivity.
5) The power factor of magnesium oxide insulation is very low compared to that of most
electrical cable insulations.

(a) 2.5 Apparatus Used:


1. MgO powder
2. Core die
3. Gloves
4. Mask
5. Vernier calipers
6. Weight balance
7. Hydraulic press

Figure 2.1: Core dies (1.3cm dia)

7
(a) 2.6 Procedure:

First we took total weight 1.2g powder and weighted it. Now
put this powder in the core die along with spacer. Then in
Hydraulic Press, we have to place the core die on the middle of
the bench and push the powder into the core die to compact it.
Now by handle move the bottom bench towards upper bench.10,
000-15,000 Psi pressure applied on the plunger to move
downwards into the die and compact the powder. After sometimes
we come out the core die from hydraulic press and then opened
the core die thus we can easily saw compact powder. Now we are
using the handle slowly and carefully because compact can be
damage if it strikes with the supporting plate. We weighted it
again. And find the diameter and height of the pellet by using
vernier calipers. And calculate its volume change and then
calculate the compact density.

Compact Density = Mass/Volume

Figure 2.2: Hydraulic press (carver)

(a) 2.7 Observation and Calculation: ( MgO Powder )

Weight of sample 1.2g


Diameter of sample (d) 1.3cm
Height of sample (h) o.6cm
Radius of sample (r) 0.65cm

Volume (V) = πr2h r=d/2


= 3.1415*(0.65cm)2 *0.6cm

=0.976 cm3

Green density=mass/volume
=1.2g/0.976cm3

Green density =1.229g/cm3

8
(b) The compaction of a mixture of different concentration of mullite and MgO
powders.
(b) 2.1Introduction of Mono Mill:

The mono mill performs mixing by continually revolving the large


plate and rotating the container. To further improve the mixing
efficiency, grinding media can be added into the containers.

Speed of rotation of the container can be adjusted along with the


proper control of time for the rotation periods. Which can be
referred as rotation speed which is in the rotation per min.rpm?

(b) 2.2 Apparatus used:

1. Mullite and MgO powder

2. Mono mill machine and Balls

3. Weight balance and vernier calipers

4. Hydraulic press (carver) (b) Figure 2.1: Mono Mill

(b) 2.2 Procedure


First we took powders of MgO and mullite of three different compositions and weighted it. We took
them and mixed in the mono mill one by one and to make three sample of MgO and mullite mixture. For
two samples, we used 28 balls and rpm 250 are applied for 2 to 3min and for third sample, we used 4
balls and rpm 150 are applied for 3 min. We successfully mixed the powders and three samples mixture
container different composition of MgO and mullite powders contain. Now put these three samples one
by one in the steel sleeve having pellet injector and the core die along with spacer. Then in Hydraulic
Press, we have to place the core die on the middle of the bench and push the powder into the core die to
compact it. Now by handle move the bottom bench towards upper bench.10,000-15000 Psi pressure
applied on the plunger to move downwards into the die and compact the powder. After sometimes we
come out the core die from hydraulic press and then opened the core die thus we can easily saw compact
powder. Now we are using the handle slowly and carefully because compact can be damage if it strikes
with the supporting plate. We weighted it again. And find the diameter and height of the pellet by using
vernier calipers. And calculate its volume change and then calculate the compact density. Volume (V) =
πr2h. And then calculate the compact density

Green Density = Mass/Volume

9
(b) 2.3 Observation and Calculation:
Serial Initial weight Final Diameter Radius Height Volume Green
number G weight of sample of of of Density
G sample sample sample of
(r2) sample
1 MgO+Mullite 0.9 g 1.3 cm 0.65 cm 0.3 cm 0.398 2.26
(0.2g+0.8g) cm3 g/cm3
1grams
2 Mgo+Mullite 1.2 g 1.3 cm 0.65 cm 0.4 cm 0.53 cm3 2.26
(0.2g+1.0g) g/cm3
1.2grams
3 MgO+Mullite 1.3 g 1.3 cm 0.65 cm 0.5 cm 0.66 cm3 1.97
(0.2g+1.2g) g/cm3
1.4grams

2.4 Result:
The green density of Mgo is 1.229g/cm3 and the green density of a mixture of different concentration of
MgO and Mullite powders are 1,2, and 3 samples 2.26g/cm3,2.26g/cm3 and 1.97g/cm3 respectively.

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(c) Sintering of compacted MgO and mixture of mullite and MgO powders.
(c) 2.1 Objective:
The objective of sintering to find out the sintered density of MgO and mixture of mullite and MgO
powders.

(c) 2.2 Introduction:


Sintering is the process of compacting and forming a solid mass of material by heat or pressure without
melting it to the point of liquefaction. Sintering happens naturally in mineral deposits or as a
manufacturing process use with metals ceramics plastics, and other materials. The atoms in the materials
diffuse across the boundaries of the particles, fusing the particles together and creating one solid piece.
Because the sintering temperature does not have to reach the melting point of the material, sintering is
often chosen as the shaping process for materials with extremely high melting points

(c) 2.3 Properties:


Sintering is effective when the process reduces the porosity
and enhances properties such as strength, electrical
conductivity, translucency and thermal conductivity. It may
be useful to increase its strength but keep its gas absorbency
constant as in filters or catalyst.

(c) 2.4 Application:


Sintering is one of the final stage of ceramics and it is used
to increase the strength of the compacted materials.

( c) 2.5 Apparatus Used:


1. Compacted MgO powder
2. Compacted mixture powders
3. Gloves and mask
4. Tongs
5. Vernier calipers
6. Weight balnce
7. Muffle furnace (Nabertherm)
(c) Figure 2.1: muffle furnace (Nebertherm)

(c) 2.6 Procedure:

Green compacted samples or pellets are placed in muffle furnace for sintering. We give different
sintering time to each samples which are to be sintered The MgO pellets are heated at 1250oc for
30mint as sintering time
and given a soaking time 30 mints and 1g mixture of MgO+Mullite Powder is heated at 1250oc for 1
hour as sintering time.1.2g mixture of MgO+Mullite powder are heated at 1250oc for 2 hours as
sintering time and then calculate its density.1.4g mixture of MgO+Mulllite Powder is heated at
1250oc for 3 hours as sintering time. We weighted it again after sintering and find out the diameter

11
and height of pellets by vernier caliper. Finally, calculate the volume and compact density of sintered
pellets

(c ) 2.7 Observation and Calculation:

Serial Compact Sintered


number density Density

G1 1.74g/cm3 1.76g/cm3

G2 1.8g/cm3 1.75g/cm3

G3 1.8g/cm3 1.94g/cm3

G4 1.84g/cm3 0.796g/cm3

G5 1.884g/cm3

G5-1 2.26g/cm3

G5-2 2.26g/cm3

G5-3 1.97g/cm3

2.6 Result:
Green density of MgO powder is 1.884g/cm3 and green density of a mixture of different concentration of
three samples are 2.26g/cm3, 2.26g/cm3and 1.97g/cm3 and sintered density cannot be find out because all
samples are firmly stick with the steel plate and broken so therefore sintered density cannot be obtained.

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EXPERIMENT NO. 3
Powder processing and preparation of TiO2 and Fe powders
3.1 Objective:
The objective of this experiment is to determine the green density of TiO2+Fe powders and properties.

3.2 Introduction:

Titanium oxide (TiO2) is used as a bright white pigment for paint; it is a use in the food industry as a
coloring, in sunscreens and cosmetics, used in other industrial. While, iron powder is used as automobile
parts, engine parts, and seat and door parts, transmission parts. Manufacture of printing ink, self-cleaning
ceramics and glass, coating, etc. Making of cosmetic products such as sunscreen creams, whitening
creams, morning and night creams, skin milks, etc. Used in the paper industry. Iron powder: is formed as
a whole from several other iron particles. The particle sizes vary anywhere from 20-200 mu.m. The iron
properties differ depending on the production method and history of a specific iron powder. Iron powder
are used as automobile parts. It is used in a different
engine parts. such cam shaft pulley crank shaft pulley,
pulley Crank, bearing. It is also used in a different seats
and door parts, Seat lifter cam set, Door mirror plate
clutch, Striker, Slider It is used in transmission parts.
Steering parts, suspension, and brake parts Machine parts,
Hand Warmers, High strength/wear-resistant parts.
Magnetic materials.
3.3 Apparatus Used:
1. TiO2 power
2. Fe powder
3. Weight balance
4. Vernier calipers
5. Gloves
6. Mask
7. Hydraulic press

Figure3.1: Core Die (13cm dia) Figure3.2: Hydraulic press (carver)

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3.4 Procedure:
First we took total weight 1.5g powder in which 70% (1.05g) titanium oxide (TiO2), and 30 % (0.45g) Fe
and weighted it. We successfully mixed the powders by hand for 20 mints. Now put this mixture of
powder in the core die along with spacer. Then in Hydraulic Press, we have to place the core die on the
middle of the bench and push the powder into the core die to compact it. Now by handle move the bottom
bench towards upper bench.15, 000 to 20,000 Psi pressure applied on the plunger to move downwards
into the die and compact the powder. We check the sleeve after sometime again and again. After
sometimes we came out the core die from hydraulic press and then opened the core die thus we can easily
saw compact powder. Now we are using the handle slowly and carefully because compact can be damage
if it strikes with the supporting plate. We weighted it again. And find the diameter and height of the pellet
by using vernier calipers. And calculate its volume change and then

Calculate the compact density.

3.5 Observation and Calculation:


Serial Initial Final Diameter Radius of Height of Volume Green
number weight weight of sample sample sample of sample Density
(g) ( g) ( r2) of sample

1 1.5g 1.5g 1.3cm 0.65 0.44cm 0.589 cm3 2.54g/cm3


cm
2 1.1g 1.1g 1.3cm 0.65 0.286cm 0.379 2.9g/cm3
cm cm3
3 2.17g/cm3
(pure 1.2g 1.2g 1.3cm 0.65 0.417 0.553
MgO) cm cm3

3.6 Result:
Green density and preparation of TiO2 and Fe powders are 1 and 2 samples 2.54g/cm3 and 2.9g/cm3
respectively. And green density of pure MgO is 2.17g/cm3

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EXPERIMENT NO.4
Sintering of compacted mixtureTiO2 and Fe powders.
4.1 Objective:
The objective of sintering to find out the sintered density of a mixture of TiO2 and Fe powders.

4.2 Introduction:
Sintering is the process of compacting solid mass of material by heat without melting it to the point of
liquefaction. Sintering happens naturally in mineral deposits or as a manufacturing process used
with metals, ceramics, plastics and other materials. The atoms in the materials diffuse across the
boundaries of the particles, fusing the particles together and creating one solid piece. Because the
sintering temperature does not have to reach the melting point of the material.
4.3 Properties:
Sintering is effective when the process reduces the porosity and
enhances properties such as strength, electrical conductivity,
translucency and thermal conductivity. It may be useful to
increase its strength but keep its gas absorbency constant as in
filters or catalyst.

4.4 Application:
Sintering is one of the final stages of ceramics and it is used to
increase the strength of the compacted materials.

4.5 Apparatus Used


1. Compacted mixture powders(TiO2+Fe)
2. Gloves
3. Tongs
4. Vernier calipers
5. Weight balance
6. Muffle furnace

Figure 4.1: Muffle furnace (Nebertherm)

4.6 Procedure:

Green compacted samples or pellets are placed in muffle furnace for sintering. The pellets are heated at
1050◦c for 90 mints to each sample which is to be sintered and given a same soaking time 90 mints. We
weighted it again after sintering and find out the diameter and height of pellets by vernier caliper. Finally,
calculate the volume and sintered density of sintered pellets.

15
4.7 Observation and Calculation:

Sample Initial Final Volume Green Sintered


Number Weight Weight of density Density
Before After Sample
sintering sintering
1 1.5g 1.7g 0.589 cm3 2.54 2.5462g/cm3
g/cm3
2 1.1g 1.2g 0.379 2.9 2.201g/cm3
cm3 g/cm3
3 1.2g 1.1g 0.553 2.17 1.986g/cm3
(Pure cm3 g/cm3
MgO)

Figure 4.2: Microstructure of pure MgO (200 x)

16
EXPERIMENT NO. 5
Liquid phase sintering of BaCO3-MgO System.
5.1 Objective:
The objective of this experiment is to compare the compaction properties (e.ge densification, green
density and %age porosity) of BaCO3 +MgO system and sintered properties (e.g. densification sintered
density and %age porosity) of different compositions.

5.2 Introduction:
In liquid phase sintering a mixture of two or more powders is sintered at a temperature below the melting
point of the high-melting constituent but above that of the low-melting constituent. In liquid phase
sintering, densification takes place under the effect of surface tension (low surface tension, better wetting
properties). Particle is rapidly drawn together and air is expelled. Resultant liquid phase can be
disappeared by diffusion or by peritectic reaction.

Liquid phase sintering is characterized by a rapid change in properties and densification, removal of
porosity quickly completed. Materials produced by the process of liquid phase sintering are referred to as
the high density (low porosity) materials. It must not be thought that all liquid phase sintered materials are
dense, as porosity may be extremely difficult to remove and diffusion may be slow in complex alloys.
This is particularly so if coarse sized pores are present in the as pressed state and the liquid content at
temperature is of a minor proportion. In this case the effect of surface tension is reduced and porosity will
remain after sintering is complete. Liquid phase sintering applies to pre-mixed powders. If the constituent
are mixed properly, the behavior on sintering depend on the wetting properties of the two metals.

Mechanism of liquid phase sintering, it can be explained by


three overlapping action.

(1) The liquid phase allows rearrangement and rapid


shrinkage of the solid materials.
(2) Dissolution and re-precipitation occurs with
densification.
(3) Coalescence occurs when the liquid phase disappears.

5.3 Apparatus Used:

1. Powder of BaCO3 and MgO


2. Glass beakers of 100ml volume

3. Solvent binder

4. Heating furnace with max. Temperature 1200◦C

5.4 Procedure:
Prepare 5 sample of BaCO3+MgO powder of 1.5g each,

(i) MgO =1.3g +BaCO3=0.2g


(ii) MgO=1.1g +BaCO3=0.4g
(iii) MgO=0.9g +BaCO3 =0.6g Figure 5.1: Hydraulic press (Carver)

17
(iv) And powder mixture (ii) are divided into two subsample S1 and S2
(v) And powder mixture (iii) are divided into two subsample S3 and S4

Calculate the theoretical volume of MgO and BaCO3 powders by using the formula of Volume (V)
πr2h =mass/density. Density of BaCO3=4.2g/cm3, MgO=3.6g/cm3.Calculate the theoretical densities
of each (i), (ii), and (iii) powder mixtures and also calculate the theoretical density of (ii) subsample
of S1 and S2 and (iii) subsample of S1 and S2. Add a amount of 4-5 drops of solvent (ethanol) into each
powder mixtures to aid in compaction. Mix thoroughly with the help of stainless steel rod so that
sample powders should be completely mixed.

Cold compaction:
Clean all part of die with the help of ethanol. Lubricate the inner walls of die orifice with 2% ethanol. Use
10,000-15,000 psi load for all samples. Apply pressure and maintain for 10 sec. Remove the pellets from
die and reweight the pellets. Measure the green densities of these pellets. Calculate densification of these
pellets (densification=green density/theoretical density). Calculate the %age porosity of green compacts.
(%age porosity=1-green density/actual density). Compare the green density, densification, and %age of
porosity of MgO+BaCO3 samples.

Liquid phase sintering:


Place the sample pellets into the furnace. Select sintering cycle in such a way that first hold at 150◦c for
10 min, second hold at 450◦c for 15 min and third hold at 850◦c for 25 min and finally furnace cooled.
And draw a graph between temperature and time. Take out the sintered pellets from the furnace with the
help of tongs. Calculate and compare the sintered densities, %age porosity and densification of sintered
pellets

18
5.5 Compaction:
Observation and calculation:
Load (10,000-15,000)

Diameter of die =1.3cm

Area of die =1.32cm2

Figure 5.1: Muffle furnace (Nebertherm)

Mass Pressure Dia of Height Vol.of Green Theoretical %age Densification


Pellets of Psi pellets of pellets density density of
pellets Cm pellets cm3 g/cm3 g/cm3 porosity
G Cm

i 1.5 10,000- 1.3 0.759 1.00740 1.48 3.679 59.77 0.4023


15,000

ii 0.7 10,000- 1.3 0.315 o.418 1.67 3.761 55.59 0.4440


S1 15,000

iii 0.897 10,000- 1.3 0.356 0.4725 1.693 3.761 54.98 0.4501
S2 15,000

iv 0.9 10,000- 1.3 0.329 0.4366 2.06 3.847 46.45 0.5355


S3 15,000

V
S4 0.6 10,000 0.214 0.2840 2.418 3.846 37.12 0.6287
-15,000

19
5.6 Liquid phase sintering:
Mass of Pressure Dia of Height Vol.of Sintered Theoretical %age Densification
Pellet pellet Psi pellets of pellets density density of
G Cm pellets g/cm3 g/cm3 porosity
Cm

i 1.164g NIL 1.3 0.795 1.05 1.109 3.685 69.90 0.3014

ii 0.538 NIL 1.264 0.349 0.4384 1.226 3.761 67.40 0.3259


s1

iii 0.604 NIL 1.286 0.357 0.4636 1.304 3.761 65.32 0.3463
s2

0.679 NIL 1.283 0.33 0.4356 1.55 3.847 59.70 0.4052


Iv
S3

V 0.5078 NIL 1.284 0.261 1.157 0.4385 3.847 88.61 0.1140


S4

5.7 Result:
The compaction of BaCO3-MgOsystem and find out the green density, theoretical density, %age porosity
and densification. Sintering of Liquid phase sintering of BaCO3-MgO System and find out the all samples
of sintered density, theoretical density, %age of porosity and densification.

20
EXPERIMENT NO.6
(a) Compaction of silica and FeO powders.
(a) 6.1 Objective:
The objective of this experiment is to get the green density of powders and their effect on the processing
characteristics.

(a) 6.2 Introduction:


Silicon dioxide also known as silica and with the chemical formula of SiO2 and most commonly found in
nature as quartz and in many parts of the world, silica is the major constituent of sand. Silica is one of the
most complex and most abundant families of materials, existing as a compound of several minerals and as
synthetic product. Notable examples include fused quartz fumed silica, silica gel and aero gels. It is used
in structural materials, microelectronics (as an electrical insulator), and as components in the food and
pharmaceutical industries. Iron oxides are widespread in nature, play an important role in many
geological and biological processes, and are widely used by humans, e.g., as iron ores pigments
catalysts in termite and hemoglobin. Common rust is a form of iron (III) oxides. Iron oxides are
widely used as inexpensive, durable pigments in
paints, coatings and colored concretes. Colors
commonly available are in the "earthy" end of the
yellow/orange/red/brown/black range. When used as
a food coloring

(a) 6.3 Apparatus used:


1) Silica and Fe powders
2) Core die
3) Carver Hydraulic press
4) Spacer
5) plunger
6) Vernier calipers
7) Gloves

(a) Figure 6.2: Hydraulic press (Carver)


(a) Figure 6.1: Core Die (1.3cm dia)

21
(a) 6.7 Procedure:
First we took total weight 1.5g powder in which 1g silica (SiO2) and 0.5g FeO and weighted it. We
successfully mixed the powders by hand for 5 mints. Now put this mixture of powder in the core die
along with spacer. Then in Hydraulic Press, we have to place the core die on the middle of the bench and
push the powder into the core die to compact it. Now by handle move the bottom bench towards upper
bench.10,000 Psi pressure applied on the plunger to move downwards into the die and compact the
powder. After sometimes we come out the core die from hydraulic press and then opened the core die
thus we can easily saw compact powder. Now we are using the handle slowly and carefully because
compact can be damage if it strikes with the supporting plate. We weighted it again. And find the
diameter and height of the pellet by using vernier calipers. And calculate its volume change and then
calculate the compact density.

(a) 6.8 Observation and Calculation:


Weight of sample 1.5g (1g silica+ 0.5g FeO)
Diameter of sample (d) 1.3cm
Height of sample (h) 0.401cm
Radius of sample (r) 0.65cm

Volume (V) = πr2h r=d/2

= 3.1415*(0.65cm)2 *0.401cm

=0.5322 cm3

Green density=mass/volume
=1.5g/0.5322cm3

Green density =2.8g/cm3

(a) 6.9 Result:


Green density of 2.8g/ cm3 of silica and FeO are obtained.

22
(b) Sintering of compacted mixture SiO2 and FeO powders
(b) 6.1 Objective:
The objective of sintering to find out the density of a mixture of TiO2 and FeO powders.

(b) 6.2 Introduction:


Sintering is the process of compacting solid mass of material by heat without melting it to the point of
liquefaction. Sintering happens naturally in mineral deposits or as a manufacturing process used
with metals, ceramics, plastics and other materials. The atoms in the materials diffuse across the
boundaries of the particles, fusing the particles together and creating one solid piece. Because the
sintering temperature does not have to reach the melting point of the material.

(b) 6.3 Properties:


Sintering is effective when the process reduces the porosity and enhances properties such as strength,
electrical conductivity, translucency and thermal conductivity. It may be useful to increase its strength
but keep its gas absorbency constant as in filters or catalyst.

(b) 6.4 Application:


Sintering is one of the final stage of ceramics and it is
used to increase the strength of the compacted materials.

(b) 6.5 Apparatus required:


1. Compacted mixture powders(TiO2+Fe)
2. Gloves
3. Tongs
4. Vernier calipers
5. Weight balance
6. Muffle furnace( Nabertherm)
7. Mask

(b) Figure 6.1: Muffle furnace (Nebertherm)

(b) 6.6 Procedure:


Green compacted samples or pellets are placed in muffle furnace for sintering. The pellets are heated at
950◦c for 120 mints to each sample which is to be sintered and given a same soaking time 120 mints. We
weighted it again after sintering and find out the diameter and height of pellets by vernier caliper. Finally,
calculate the volume and compact density of sintered pellets.

23
(b) 6.7 Observation and Calculation:
Weight of sample 1.72g
Diameter of sample (d) 1.381cm
Height of sample (h) 0.43cm
Radius of sample (r) 0.6905cm

Volume (V) = πr2h r=d/2

= 3.1415*(0.6905cm)2 *0.43cm

= 0.6440cm3

sintered density=mass/volume
=1.72g/0.6440cm3

sintered density =2.6g/cm3

(b) 6.8 Result:


Sintered density of silica and FeO 2.6g/cm3 are obtained at temperature 950◦c.

24
Experiment No.7
Compaction of cast iron powder.
7.1 Objective:
The objective of this experiment is to get the green density of powders and their effect on the processing
characteristics.

7.2 Introduction:
Cast irons are basically iron-carbon alloys having carbon between 2.11% and 6.67%. Eutectic reaction
takes place during solidification. Alloys having Carbon between 2.11% and 4.3% are called hypo-eutectic
cast irons. The alloy Containing 4.3% C is called eutectic cast iron, and the alloys containing
between4.3% and 6.67% carbon are called hyper-eutectic cast irons. The cast ability is the best of a
eutectic alloys. The industrial cast irons have carbon normally in the range of 2.11% to 4.0%, along with
other elements like silicon, manganese, sulphur phosphorus in substantial amounts. Higher carbon content
makes them more brittle. Cast irons are brittle, and cannot be forged, rolled, drawn etc. but can only be
‘cast’ into desired shape and size by pouring the molten alloy of desired composition into a mould of
desired shape and allowing it to solidify. As casting is the only and exclusively suitable process to shape
these alloys, so called cast irons. Its usefulness derives from its relatively low melting temperature. The
alloy constituents affect its color when fractured. White cast iron has carbide impurities which allow
cracks to pass straight through. Grey cast iron has graphite flakes which deflect a passing crack and
initiate countless new cracks as the material breaks. Ductile cast iron has spherical graphite "nodules"
which stop the crack from further progressing.

(a) 7.3 Compacted cast iron:


The formation of compacted iron depends on the chemical composition, section thickness and the process
used for production. Normally, 10-20% of the spheroidal graphite may be present, which requires C.E.V.
of 4.00, and flake graphite should be avoided. In one of the production methods, nitrogen (—0.015%) is
added to liquid alloy in ladle by adding nitride Ferro-manganese (80% Mn, 4% N, rest Fe). This method
gives non-uniformity of structure and unsoundness in castings. In another method, an alloy (4-5% Mg,
8.5-10.5% Ti, 4-5.5% Ca, 1-1.5% Al, 0.2-0,5% Ce, 48-52% Si, rest Fe) in amounts 0.6-1.6% is added, as
additions are made to produce S.G. iron. Sulphur content of iron should not be more than 0.035%. This
method is section-sensitive as spheroids get formed in thin sections. The compacted graphite permits
strength. Stiffness and ductility that exceeds those of gray iron.

7.4 Properties of compacted cast iron:


1. Compacted cast iron to retain good damping capacity,
and thermal conductivity.
2. Its resistance to crazing, tracking and distortion is
superior to both S.G. iron and gray iron. As the shrinkage
during casting is less than in S.G. iron.
3. This cast iron having inferior mechanical properties hut
similar production costs as S.G. Iron has limited
replacement potential to S.G. iron parts. However,
because of greater strength and toughness, it can replace
more expensive alloyed gray cast irons. Figure 7.1: Core Die (1.3cm dia)

7.5 Apparatus used

25
1. Cast iron power
2. Weight balance
3. Vernier calipers
4. Gloves
5. Mask
6. Hydraulic press

(a) 7.7 Procedure


First we took total weight 2g cast iron powder and weighted it. Now
put this powder in the core die along with spacer. Then in Hydraulic
Press, we have to place the core die on the middle of the bench and
push the powder into the core die to compact it. Now by handle move
the bottom bench towards upper bench.10, 000-15,000psi pressure
applied on the plunger to move downwards into the die and
compact the powder. After sometimes we come out the core die from
hydraulic press and then opened the core die thus we can easily saw
compact powder. Now we are using the handle slowly and carefully
because compact can be damage if it strikes with the supporting plate.
We weighted it again. And find the diameter and height of the pellet by
using vernier calipers. And calculate its volume change and then
calculate the compact density.

Figure 7.2: Hydraulic press (Carver)


7.8 Observation and Calculation:
Weight of sample 2g
Diameter of sample (d) 1.3cm
Height of sample (h) 0.437cm
Radius of sample (r) 0.65cm

Volume (V) = πr2h r=d/2

= 3.1415*(0.65cm)2 *0.437cm

=0.58002 cm3

Green density=mass/volume
=2g/0.58002cm3

Green density =3.44g/cm3

7.9 Result. Green density of cast iron 3.44g/cm3 are obtained.

26
(b) Sintering of Compacted Cast Iron
(b) 7.1 Objective:
The objective of sintering to find out the sintered density of cast iron.

(b) 7.2 Introduction:


Sintering is the process of compacting and forming a solid mass of material by heat or pressure without
melting it to the point of liquefaction. Sintering happens naturally in mineral deposits or as a
manufacturing process use with metals ceramics plastics, and other materials. The atoms in the materials
diffuse across the boundaries of the particles, fusing the particles together and creating one solid piece.
Because the sintering temperature does not have to reach the melting point of the material, sintering is
often chosen as the shaping process for materials with extremely high melting points

(b) 7.3 Properties:


Sintering is effective when the process reduces the porosity and
enhances properties such as strength, electrical conductivity,
translucency and thermal conductivity. It may be useful to
increase its strength but keep its gas absorbency constant as in
filters or catalyst.

(b) 7.4 Application:


Sintering is one of the final stage of ceramics and it is used to
increase the strength of the compacted materials.

( b) 7.5 Apparatus Used:


8. Compacted MgO powder
9. Compacted mixture powders
10. Gloves and mask
11. Tongs
12. Vernier calipers (b) Figure 7.1: muffle furnace (Nebertherm)
13. Weight balnce
14. Muffle furnace

(b) 7.6 Procedure


Green compacted samples or pellets are placed in muffle furnace for sintering. The pellets are heated at
950◦c for 120 mints to each sample which is to be sintered and given a same soaking time 120 mints. We
weighted it again after sintering and find out the diameter and height of pellets by vernier caliper. Finally,
calc

(b) 7.7 Observation and Calculation:


Weight of sample 2.55g
Diameter of sample (d) 1.3cm
Height of sample (h) 0.5cm
Radius of sample (r) 0.65cm

27
Volume (V) = πr2h r=d/2

= 3.1415*(0.65cm)2 *0.5cm

= 0.663641cm3

sintered density=mass/volume
=2.55g/0.663641cm3

sintered density =3.8g/cm3

(b) 7.9 Result. Sintered density of cast iron 3.84g/cm3 are obtained.

28
(c) Compaction of a mixture of Cast Iron and Silica powders.

(c) 7.1 Objective:


The objective of this experiment is to determine the green density of SiO2+Cast Iron powders and
properties.

(c) 7.2 Introduction:


The formation of compacted iron depends on the chemical composition, section thickness. And the
process used for production. Normally, 10-20% of the spheroidal graphite may be present. In one of the
production methods, nitrogen (—0.015%) is added to liquid alloy in ladle by adding nitride Ferro-
manganese (80% Mn, 4% N, rest Fe). This method gives non-uniformity of structure and unsoundness in
castings. In another method, an alloy (4-5% Mg, 8.5-10.5% Ti, 4-5.5% Ca, 1-1.5% Al, 0.2-0,5% Co, 48-
52% Si, rest Fe) in amounts 0.6-1.6% is added, as additions are made to produce S.G. iron. Sulphur
content of iron should not be more than 0.035%. The compacted graphite permits strength, Stiffness and
ductility that exceed those of gray iron. Compacted cast iron to retain good damping capacity, and
thermal conductivity. Its resistance to crazing, tracking and distortion is superior to both S.G. iron and
gray iron. As the shrinkage during casting is less than in S.G. iron. This cast iron having inferior
mechanical properties hut similar production costs as S.G. Iron has limited replacement potential to S.G.
iron parts. However, because of greater strength and toughness, it can replace more expensive alloyed
gray cast irons. Silicon dioxide also known as silica and with the chemical formula of SiO2 and most
commonly found in nature as quartz and in many parts of the world, silica is the major constituent
of sand. Silica is one of the most complex and most abundant families of materials, existing as a
compound of several minerals and as synthetic product. Notable examples include fused quartz fumed
silica, silica gel and aero gels. It is used in structural materials, microelectronics (as an electrical
insulator), and as components in the food and pharmaceutical industries. They are used in Structural used
Precursor to glass, Food and pharmaceutical applications, in cosmetics, its useful for its light-diffusing
properties, Can be used as a glass fiber for fiberglass.

(c) 7.3 Apparatus used:


1. Silica and Cast iron powders

2. Mono mill machine and Balls

3. Weight balance and vernier calipers

4. Hydraulic press (carver)

5. Sieve analysis

6. Mask

(c) 7.4 Procedure:


First we took small amount of silica in sieve analysis and given a 10 min. for analysis. Then we took a
5.2g cast iron and 2 g silica in the mono mill and mixed them . For five samples, we used 4-5 balls and
100rpm speed are applied for 15 min. after successfully mixed the powders we took different weight of
five samples Now put these five samples one by one in the core die along with spacer. Then in Hydraulic
Press, we have to place the core die on the middle of the bench and push the powder into the core die to

29
compact it. Now by handle move the bottom bench towards
upper bench.10,000-15000 Psi pressure applied on the plunger to
move downwards into the die and compact the powder. After
sometimes we come out the core die from hydraulic press and
then opened the core die thus we can easily saw compact
powder. Now we are using the handle slowly and carefully
because compact can be damage if it strikes with the supporting
plate. We weighted it again. And find the diameter and height of
the pellet by using vernier calipers. And calculate its volume
change and then calculate the compact density. Volume (V) =
πr2h. And then calculate the compact density

Green Density = Mass/Volume

Figure7.2: Hydraulic press (Carver)


(c) 7.5 Observation and Calculation:

Serial Initial Final Diameter Radius of Height of Volume of Green


number weight weight of sample sample sample sample Density of
(g) (g ) ( r 2) sample

1.3cm 0.31cm 0.4114cm3


1 1.2g 1.2g 0.65 cm 2.9g/cm3

1.3cm
2 1.58g 1.58g 0.65 cm 0.54cm 0.7163cm3 2.20g/cm3

3 1.57g 1.57g 1.3cm 0.65 cm 0.52cm 0.6901cm3 2.27g/cm3

4 1.61g 1.61g 1.3cm 0.65cm 0.51cm 0.6791cm3 2.37g/cm3

5 1.64g 1.64g 1.3cm 0.65cm 0.53cm 0.7037cm3 2.33g/cm3

30
(d) Sintering of compacted mixture of silica and cast iron powders.
(d) 7.1 Objective:
The objective of sintering to find out the sintered density of a mixture of silica and cast iron powders.

(d) 7.2 Introduction:


Sintering is the process of compacting solid mass of material by heat without melting it to the point of
liquefaction. Sintering happens naturally in mineral deposits or as a manufacturing process used
with metals, ceramics, plastics and other materials. The atoms in the materials diffuse across the
boundaries of the particles, fusing the particles together and creating one solid piece. Because the
sintering temperature does not have to reach the melting point of the material.
(d) 7.3 Properties:
Sintering is effective when the process reduces the porosity and enhances properties such as strength,
electrical conductivity, translucency and thermal conductivity. It may be useful to increase its strength
but keep its gas absorbency constant as in filters or catalyst.

(d)7.4 Application:
Sintering is one of the final stages of ceramics and it is used
to increase the strength of the compacted materials.

(d) 7.5 Apparatus Used


7. Compacted mixture powders(silica+ cast iron)
8. Gloves
9. Tongs
10. Vernier calipers
11. Weight balance
12. Muffle furnace
13. Mono Mill

Figure 7.1: Muffle furnace (Nebertherm)


(d) 7.6 Procedure
Green compacted samples or pellets are placed in muffle furnace for sintering. The pellets are heated at
900◦c for 120 mints to each sample which is to be sintered and given a same soaking time120 mints. We
weighted it again after sintering and find out the diameter and height of pellets by vernier caliper. Finally,
calculate the volume and sintered density of sintered pellets.

31
(d) 7.7 Observation and Calculation:
Serial Initial Final Diameter Radius of Height of Volume of Sintered
number weight weight of sample sample sample sample Density of
(g) ( g) ( r 2) sample

1 1.2g 1.01g 1.3cm 0.65 cm 0.5cm 0.6636cm3 1.52g/cm3

2 1.58g 1.57g 1.3cm 0.65 cm 0.5cm 0.6636cm3 2.36g/cm3

3 1.57g 1.56g 1.3cm 0.65 cm 0.5cm 0.6636cm3 2.35g/cm3

4 1.61g 1.63g 1.3cm 0.65cm 0.5cm 0.6636cm3 2.45g/cm3

5 1.64g 1.65g 1.3cm 0.65cm 0.5cm 0.6636cm3 2.47g/cm3

(d) 7.7 Result


Green density and sintered density of silica and cast iron powders are obtained.

32

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