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Laboratory 1: Production and Testing 

of Ceramic Bars 
 
 
Prepared for 
 
Dr. Xueyuan Nie 
 
 
 
 

 
 
 
 

Faisal SIDDIQUI 
Student ID 101963673 
th
4  year Candidate for BASc. Mechanical Engineering 
Department of Mechanical Automotive and Materials Engineering
Table of Contents
Abstract:.......................................................................................................................... 2
Summary:........................................................................................................................ 2
Survey of literature: ........................................................................................................ 3
Experimental Procedures: ............................................................................................... 4
Experimental Results: ..................................................................................................... 6
Part A: ......................................................................................................................... 6
Part B: ......................................................................................................................... 6
Part C: ......................................................................................................................... 7
Part D: ......................................................................................................................... 8
Part E:.......................................................................................................................... 9
Discussion:.................................................................................................................... 10
Conclusion: ................................................................................................................... 11
Recommendations:........................................................................................................ 12
References:.................................................................................................................... 12
Appendix:...................................................................................................................... 12
Calculations: ............................................................................................................. 12
Tables and Charts...................................................................................................... 14

List of Figures
Figure 1: Early Shrinkage Data for Slip Casting Ceramics ................................................ 6
Figure 2: Subsequent Shrinkage Data for Slip Casting Ceramics for Bars 1-9 .................. 7
Figure 3: Shrinkage from Firing at different temperatures................................................. 8
Figure 4: Fracture Loads vs firing temperatures................................................................. 9

List of Tables

Table 1: Shrinkage (%) from Firing................................................................................... 7


Table 2: Fracture Loads for each bar from each group and their averages......................... 8
Table A - 1: Dimensions and Shrinkages for Drying and Firing Stages .......................... 14
Table A - 2: X-ray Diffractions and Microstructures of bars at different temperatures ... 15
Abstract:
The objective of this experiment is to recognize the basic steps in the production of clay
containing ceramic materials by slip casting and to evaluate their mechanical properties.
This experiment was conducted to firstly, see the effect of acid and base addition to slip
(clay particles which are suspended in liquid). Secondly, using slip casting to make a
certain number of bars and examine the dimensional changes occurring in the bars during
drying and to find a relationship between the shrinkage vs. drying time. Thirdly, to
produce ceramics by firing the preformed green body or green ware to fabricate a
permanent piece and examine its shrinkage vs. firing temperature. Fourthly, to determine
the mechanical properties of the bars by the fracture loads of the bars using a three point
bend test and therefore find a relationship between the fracture loads vs. the firing
temperatures. And finally, to examine the x-ray diffraction and microstructure of the
fractured surfaces and correlate the two.

Summary:
The purpose of doing the experiment was to become familiar with the ceramic materials,
its preparation and examining its mechanical properties and finally to analyze its
microstructure. This is an important experiment due to the fact that this experiment meets
all of the necessary objectives. In the study of materials engineering it is very important
to become familiar with ceramics preparation and its various properties due to the fact
that a lot of objects in our daily life are made from ceramics.

Firstly ceramic preparation method demonstrated in this experiment is slip casting. This
is one of many different methods of ceramic preparation. This method of ceramic
preparation is advantageous for forming thin-walled and complex shapes of uniform
thickness. Slip casting is especially economical for development parts and short
production runs. Therefore this experiment is one of the cheapest to perform.

Secondly this experiment helps us determine the shrinkage during the drying and firing
stages and correlate the shrinkage with drying time and firing temperatures. This helps us
understand the necessary time and temperature required for ceramic production.

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Finally with the aid of this experiment we can examine the fracture strength and the
microstructure of the ceramic materials that were produced by slip casting with drying
and firing, to understand the relationship between the microstructure characteristics and
fracture strength and time and temperature used during drying and firing stages.

Survey of literature:
Slip casting is a method of casting by which usually takes place at room temperature and
the ceramic particles which are suspended in liquid are cast into a porous mould. The
viscosity of this suspension can be lowered with the addition of deflocculates (e.g.
NaOH). A lower viscosity suspension is required to start the slip casting process. Also the
viscosity of the particles in the suspension can be increased and made more rigid by the
addition of acids (e.g. HCl). The addition of HCl lowers the ph and polarizes the
suspension. This causes the edges and the faces of the suspended particles to have
opposite charges and they attract each other and become increasingly viscous.

After the low viscosity slip is cast into a cavity mould the next step is drying. In this step
the excess water is driven off the cast part and as a result the cast part attains considerable
strength which can be enhanced by firing. The purpose of drying ceramics is to remove
water from the plastic ceramic body before it is fired at higher temperatures. Generally,
drying to remove water is carried out at or below 100ºC and can take as long as 24
hrs for a large ceramic part.

During firing additional amount of water is driven off the cast part and permanent bonds
develop by reactions among the components of clay. Firing/Sintering can occur in the
presence or absence of a liquid phase (e.g. a liquid phase is formed during the drying
process). The firing process results in the transformation of a porous compact into a
dense, coherent product.

Ceramic materials in green condition contain many small pores leading to low strengths.
As the firing process proceeds, larger particles are formed at the expense of the smaller
ones. As the particles get larger with the time of sintering, the porosity of the compacts

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decreases and gives rise to high strength. The high strength material formed is also brittle
and unsuitable for applications requiring resistance to mechanical and thermal stresses.

General References
Ceramics laboratory 1 handout: Production and testing of ceramic bars.
Chapter 3 Lecture Slides: Processing of ceramics.

Experimental Procedures:
¾ Put some well mixed commercial clay slip in a beaker.
¾ Lower the pH of the slip by slowly adding 3% HCl solution while stirring. Note
the relative viscosity as the pH drops.
¾ Raise the pH of the solution by slowly adding sodium silicate with stirring. Note
the relative change in the viscosity as the pH rises.
¾ Explain the changes in viscosity in terms of the structure of kaolinite and the
changes that occur when the pH is changed.
¾ Measure the dimensions of the cavities in the moulds. Keep track of the cavity
sizes by mould number and cavity number.
¾ Slip cast a number of bars by pouring clay slip into the plaster of Paris moulds.
Make sure to top up the moulds with slip as water is absorbed. This is necessary
to avoid the formation of hollow topped bars.
¾ When the bars are solid enough, remove them from the mould and measure their
dimensions (width, length, and depth). Keep track of which bar came from which
mould and cavity. While the bars are in this green state, an identification number
can be scribed on one end of each bar.
¾ Re-measure the bars at 24 hour intervals until the next laboratory session.
¾ Calculate the volume shrinkage for each set of measurements for each bar, using
the cavity sizes in the moulds as the starting sizes.
¾ Plot a graph of the shrinkage of the bars versus the drying time.
¾ Retain three bars in their unfired, green condition. These will be tested to give the
breaking load for the green ware.
¾ Of the remaining bars, put nine in furnace one, six in furnace two, and nine in
furnace three.
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¾ Turn the furnaces on, set the temperature to 200°C, and allow the furnaces to reach
the set temperature. Once the furnaces have reach 200°C hold this temperature for
thirty minutes. At the end of this time remove three bars from furnace three.
¾ Raise the set temperature on the furnaces to 600°C. When this temperature has
been reached, hold the bars for thirty minutes. At the end of this time remove three
bars from furnace three.
¾ Raise the set temperatures of the furnaces to the temperatures in the following table
and hold the bars at each temperature for thirty minutes. After each thirty minute
period, remove three samples from the indicated furnace. For the 1100°C, 1150°C,
and 1200°C temperatures do not remove the bars from the furnaces. Instead at the
end of the thirty minute hold, turn off the furnaces and allow the temperature to fall
below 1000°C before opening the furnace doors.
¾ After the bars have cooled to room temperature, re-measure the dimensions of the
bars. Determine if any shrinkage has occurred during firing. Use the last set of
measurements from the drying stage as the reference. Plot the shrinkage versus the
firing temperature.
¾ Use the three point bend test apparatus on the Instron universal test machine to find
the fracture load for each bar. Average the three values for each temperature
condition to give the fracture load for that condition.
¾ Do not put the fractured ends of the bars back together as the fracture surfaces will
be investigated in the following section of the laboratory.
¾ Plot the fracture loads versus the firing temperatures.
¾ Tour the scanning electron microscope and x-ray diffraction laboratories.
¾ Typical microstructure and x-ray results will be distributed.
¾ Analyze the above results and correlate them.

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Experimental Results:
Part A:
¾ Relative viscosity increased with the fall in pH as the 3% HCl solution was added.
¾ Relative viscosity dropped and the slip became more viscous with the addition of
sodium silicate with stirring.
¾ When suspended in a weak acid solution (e.g. HCl pH = 4 – 6) the flake like
kaolinite particles have positive charges at their edges and negative charges on
their faces. Such a configuration develops coulombic attraction which results in
flocculation as a result of edge to face attraction between particles. At pH 6 or
higher (e.g. addition of sodium silicate), the positive edge charges disappear and
viscosity drops.

Part B:
¾ See volume shrinkage of bars in the Appendix Table A1. Calculation is shown in
the Appendix as well.

Early Shrinkage Data for Slip Casting Ceram ics

10

8
Average Shrinkage (%)

0
0 5 10 15 20 25 30
Tim e (Hours)

Early Shrinkage Data

Figure 1: Early Shrinkage Data for Slip Casting Ceramics

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Subsequent Shrinkage Data for Slip Casting Ceramics for Bars 1-9

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12

10
Average Shrinkage (%)

0
0 20 40 60 80 100 120 140 160 180
Time (Hours)

Bar 1 Bar 2 Bar 3 Bar 4 Bar 5 Bar 6 Bar 7 Bar 8 Bar 9

Figure 2: Subsequent Shrinkage Data for Slip Casting Ceramics for Bars 1-9

Part C:
The bars shrunk as they were fired. New dimensions and shrinkage data can be found in
the Appendix Table A-1. Calculation are also in Appendix. Shrinkage values (%)
tabulated here.
Table 1: Shrinkage (%) from Firing
Shrinkage from
o
Firing Tem.( C) Sample No. Firing (%)
25 1 0.689654739
200 2 -0.603445413
600 3 -1.815400159
800 4 0.715899232
1000 5 3.025286771
1050 6 3.064253013
1100 7 3.962576034
1150 8 8.001779567
1200 9 18.91325573

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Shrinkage from Firing at different temperatures

20

15
Shrinkage from Firing (%)

10

0
25 200 600 800 1000 1050 1100 1150 1200

-5
Firing Temperature (ºC)

Shrinkage from Firing

Figure 3: Shrinkage from Firing at different temperatures

Part D:
Table 2: Fracture Loads for each bar from each group and their averages
Sample Load (lb)
Firing Tem.(oC) No. A B C Average
25 1 6 12 11 9.666666667
200 2 7 12 20 13
600 3 14 16 26 18.66666667
800 4 21 28 48 32.33333333
1000 5 119 182 30 110.3333333
1050 6 115 126 30 90.33333333
1100 7 62 61 188 103.6666667
1150 8 107 160 316 194.3333333
1200 9 162 234 468 288

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Tem perature vs Load Strength

350

300

250
Strength (lb)

200

150

100

50

0
0 200 400 600 800 1000 1200 1400
Temperature (ºC)

Temperature vs Strength

Figure 4: Fracture Loads vs firing temperatures

Part E:
Microstructure and X-ray diffraction patterns are tabulated in Table A-2 in the appendix.

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Discussion:
From the experiment it was found that adding an acid such as HCl to a slip suspension
increased the viscosity of the slip whereas adding a base such as deflocculents (eg.
NaOH, Na2SiO3,) lowered the viscosity of the slip. When suspended in a weak acid
solution (pH = 4 – 6) the flake like kaolinite particles have positive charges at their edges
and negative charges on their faces. Such a configuration develops coulombic attraction
which results in flocculation as a result of edge to face attraction between particles
(Figure 1). At pH 6 or higher, the positive edge charges disappear. Consequently the
edge to face attraction disappears and the kaolinite particles become well dispersed in the
water.(deflocculation).

Secondly after the bars were cast from the slip suspension and dried it was found that the
bars in general attained a significant amount of shrinkage with the number of hours they
were dried. This is shown in table A-1.

Thirdly it was also found that as the preformed green body ceramic bars were fired the
shrinkage of the bars in general was proportional to the level of firing temperatures. In
other words at higher temperatures the bars shrunk a greater amount. This is shown in
table 1 and table A-1.

Fourthly, after careful examination of the fracture loads from the three point bend test, it
was found that the fracture loads were directly proportional to the firing temperatures. In
other words bars which were fired at higher temperatures demonstrated a greater fracture
load. This is shown in table 2.

Finally, after examining the x-ray diffraction and microstructure it was found that green
bar from room temperature and other bars which were fired at lower temperature
demonstrated a greater amount of porosity and voids compared to that of the bars which
were fired at higher temperatures. There were some exceptions of the above statement at
certain temperatures. The microstructure and corresponding x-ray diffractions are shown
in table A-2.

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Conclusion:
The purpose of this experiment was to recognize the basic steps in the production of clay
containing ceramic materials by slip casting and to evaluate their mechanical properties.
From this experiment we learned a several important characteristics of slip, slip casting,
drying and firing and the corresponding x-ray and microstructure.

It was observed that the viscosity of the slip increases with the addition of acidic
substances such as HCl at pH 4-6. At pH 6 and above the slip becomes non viscous and
suitable for casting.

From the drying stage it was found that most of the shrinkage occurred during the first 24
hours and then the shrinkage amount remained almost constant as evident from figure 1
and 2. The average shrinkage was around 3% at 2 hours after casting and 9% at 24 hours
after casting.

It was also found that the bars shrunk a greater amount as a result of firing temperature.
The shrinkage from firing at 25ºC was around 0.7% and was around 19% at 1200ºC as
evident from table 1.

Another finding was that the fracture loads were seen to increase as directly proportional
as the firing temperature. From table 2 it was seen that at room temperature the green bar
had an average fracture load of 9.66lb compared with 288lb at 1200ºC.

Finally after examining the microstructure we found that from room temperature to
around 600ºC, the microstructure remained almost similar and as a result the fracture
loads were fairly constant. There was a slight improvement of fracture load at 800ºC due
to a microstructure which was slightly nonporous compared to the lower temperatures. At
1000ºC the bar achieved a local peak in strength compared to 1050 and 1100ºC. This
could be contributed to at 1050 and 1100ºC the due to grain growth the microstructure of
1050 and 1100ºC was coarser than that of 1000ºC. Finally at 1150ºC the bonds solidified
and pores and voids started to disappear and strength was improved. At 1200ºC most of
the pores and voids disappeared and the structure achieved maximum strength.
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Recommendations:
In our results we found some negative shrinkage values which is likely to be a measuring
error. It was found that we did not measure the bars at the same location every time and
due to the bar having a non uniform cross sectional area that gave a misleading reading.

In the future therefore, it is recommended that the party conducting experiment mark a
location on the bar where all the measurements will be taken from.

References:
Ceramics laboratory 1 handout: Production and testing of ceramic bars.
Chapter 3 Lecture Slides: Processing of ceramics.

Appendix:

Calculations:
Average Loads (P) at different Temperatures
6 + 12 + 11
PT = Room = = 9.67lb
3
7 + 12 + 20
PT = 200°C = = 13lb
3
14 + 16 + 26
PT =600°C = = 18.67lb
3
21 + 28 + 48
PT =800°C = = 32.33lb
3
119 + 182 + 30
PT =1000°C = = 110.33lb
3
115 + 126 + 30
PT =1050°C = = 90.33lb
3
62 + 61 + 188
PT =1100°C = = 103.67lb
3
107 + 160 + 316
PT =1150°C = = 194.33lb
3
162 + 234 + 468
PT =1200°C = = 288lb
3

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The calculation for Bar 1 is shown. Each bar is calculated in the similar fashion

Original: Jan 30, 4pm. Time = 24 hours:


So = L × W = 97.4 × 21.37 = 2081.438mm 2
S − So 2081.438 − 2081.438
Shrinkage = − =− = 0%
So 2081.438

Jan 31, 1pm. Time = 45 hours:


S = L × W = 92.54 × 20.5 = 1897.07 mm 2
S − So 1897.07 − 2081.438
Shrinkage = − =− = 8.86%
So 2081.438

Feb 1, 11:30am. Time = 67.5 hours:


S = L × W = 92.42 × 20.26 = 1872.429mm 2
S − So 1872.429 − 2081.438
Shrinkage = − =− = 10.04%
So 2081.438

Feb 4, 1:15pm. Time = 117.25 hours:


S = L × W = 92.4 × 20.5 = 1894.2mm 2
S − So 1894.2 − 2081.438
Shrinkage = − =− = 9.00%
So 2081.438

Feb 5, 2:05pm. Time = 142.08 hours:


S = L × W = 92.58 × 20.82 = 1927.516mm 2
S − So 1927.516 − 2081.438
Shrinkage = − =− = 7.40%
So 2081.438

Feb 6, 2:40pm. Time = 166.66 hours:


S = L × W = 92.57 × 20.61 = 1907.868mm 2
S − So 1907.868 − 2081.438
Shrinkage = − =− = 8.34%
So 2081.438

Firing Shrinkage Feb 13:


So = 1907.868mm 2 from Feb 6, 2:40pm.
S = L × W = 92.2 × 20.55 = 1894.71mm 2
S − So 1894.71 − 1907.868
Shrinkage = − =− = 0.689%
So 1907.868
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Tables and Charts
Table A - 1: Dimensions and Shrinkages for Drying and Firing Stages

Group: C Drying Firing


DATE Original Jan.31 Feb. 1 Feb.4 Feb.5 Feb.6 Feb.13 color
TIME 4pm 1pm 11:30am 1:15pm 2:05pm 2:40pm
L 97.4 92.54 92.42 92.4 92.58 92.57 92.2
W 21.37 20.5 20.26 20.5 20.82 20.61 20.55
S 2081.438 1897.07 1872.429 1894.2 1927.516 1907.868 1894.71
1 SHRINKAGE 0 8.857722 10.04156 8.995608 7.395003 8.338961 0.689655 brown
L 95.16 90.33 90.21 90.08 90.2 90.72 90.96
W 21.36 20.82 20.77 21.02 20.98 20.71 20.78
S 2032.6176 1880.671 1873.662 1893.482 1892.396 1878.811 1890.149
2 SHRINKAGE 0 7.475435 7.820256 6.845164 6.898573 7.566913 -0.60345 brown
L 98.45 93.78 93.12 93.58 93.7 93.78 93.45
W 22.18 21.13 20.81 21.43 21.83 21.15 21.61
S 2183.621 1981.571 1937.827 2005.419 2045.471 1983.447 2019.455
3 SHRINKAGE 0 9.252961 11.25625 8.16083 6.326647 9.167067 -1.8154 light grey
L 98.19 93.56 93 93.25 93.21 93.26 93.49
W 21.56 20.87 20.78 21.44 21.46 20.83 20.63
S 2116.9764 1952.597 1932.54 1999.28 2000.287 1942.606 1928.699
4 SHRINKAGE 0 7.76481 8.712256 5.559646 5.512097 8.236776 0.715899 white
L 98.08 93.41 92.94 93.29 93.35 93.39 91.96
W 22.33 21.03 20.92 21.22 21.18 21.09 20.77
S 2190.1264 1964.412 1944.305 1979.614 1977.153 1969.595 1910.009
5 SHRINKAGE 0 10.30599 11.22408 9.611893 9.724252 10.06934 3.025287 white
L 98.35 94.12 93.81 94.03 93.91 93.85 92.27
W 21.74 20.79 20.77 21.14 21.13 20.65 20.36
S 2138.129 1956.755 1948.434 1987.794 1984.318 1938.003 1878.617
6 SHRINKAGE 0 8.482846 8.872023 7.031138 7.193705 9.359889 3.064253 white
L 98.03 93.87 93.78 94.04 94.09 93.9 91.87
W 21.48 21.17 20.6 21.45 21.71 21.19 20.8
S 2105.6844 1987.228 1931.868 2017.158 2042.694 1989.741 1910.896
7 SHRINKAGE 0 5.625558 8.254627 4.204163 2.99145 5.50621 3.962576 white
L 97.66 93.29 92.99 92.84 92.92 92.89 88.42
W 22.43 21.08 20.86 20.98 20.84 20.89 20.19
S 2190.5138 1966.553 1939.771 1947.783 1936.453 1940.472 1785.2
8 SHRINKAGE 0 10.22411 11.44674 11.08099 11.59824 11.41475 8.00178 yellow
L 97.43 92.99 92.69 92.68 92.75 92.77 85.8
W 22.29 20.99 20.88 20.99 21.02 20.85 18.28
S 2171.7147 1951.86 1935.367 1945.353 1949.605 1934.255 1568.424
9 SHRINKAGE 0 10.12355 10.88299 10.42317 10.22739 10.93423 18.91326 yellow

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Table A - 2: X-ray Diffractions and Microstructures of bars at different temperatures

Green

600

500
X - ra y C o u n t in c p s

400

300

200

100

0
5 10 15 20 25 30 35 40 45 50
X-ray Diffraction Angle in Degrees Two Theta for Copper Radiation

200

800
700
X - ra y C o u n t in c p s

600
500
400
300
200
100
0
5 10 15 20 25 30 35 40 45 50
X-ray Diffraction Angle in Degrees Two Theta for Copper Radiation

600

1400
1200
X - ra y C o u n t in c p s

1000
800
600
400
200
0
5 10 15 20 25 30 35 40 45 50
X-ray Diffraction Angle in Degrees Two Theta for Copper Radiation

15
800

700
600
X - ra y C o u n t in c p s

500
400
300
200
100
0
5 10 15 20 25 30 35 40 45 50
X-ray Diffraction Angle in Degrees Two Theta for Copper Radiation

1000

600

500
X - ra y C o u n t in c p s

400

300

200

100

0
5 10 15 20 25 30 35 40 45 50
X-ray Diffraction Angle in Degrees Two Theta for Copper Radiation

1050

600

500
X - ra y C o u n t in c p s

400

300

200

100

0
5 10 15 20 25 30 35 40 45 50
X-ray Diffraction Angle in Degrees Two Theta for Copper Radiation

16
1100

450
400
X - ra y C o u n t in c p s

350
300
250
200
150
100
50
0
5 10 15 20 25 30 35 40 45 50
X-ray Diffraction Angle in Degrees Two Theta for Copper Radiation

1150

300

250
X - ra y C o u n t in c p s

200

150

100

50

0
5 10 15 20 25 30 35 40 45 50
X-ray Diffraction Angle in Degrees Two Theta for Copper Radiation

1200

350
300
X - ra y C o u n t in c p s

250
200
150
100
50
0
5 10 15 20 25 30 35 40 45 50
X-ray Diffraction Angle in Degrees Two Theta for Copper Radiation

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