EXP.

NO: L3/S1/02

CHARACTERIZATION OF SINTERED CERAMICS

INSTRUCTED BY: MR. WEERASOORIYA P.R.P. MEMBERS: 1. 2. 3. 4. 5. 6. 7. 8. RAJAPAKSE R.A.S.N. RANASINGHE P.V.S.K. RUPASINGHE P.S.P. SANDARUWAN A.W.H.O. SENDANAYAKE D.D.I. SENEVIRATHNE H.V.H.H. THILAWALA K.G.N. THUSHYANTHAN T.

NAME: COURSE: INDEX NO: GROUP:

RUPASINGHE P.S.P. MATERIALS ENGINEERING 080431T D

DATE OF PER: DATE OF SUB:

TITLE: CHARACTERIZATION OF SINTERED (FIRED) CERAMICS INTRODUCTION Ceramics can be basically divided into two categories; traditional ceramics and advanced ceramics. Traditional ceramics are closely related to materials that have been developed since the earliest times whilst advanced ceramics are those which have been developed in the recent past. Ceramics with certain properties can only be used for specific purposes; i.e. the properties of a given ceramic determine its possible applications. Therefore, obtaining knowledge of its properties after sintering is extremely important. The properties determined in this experiment are shrinkage, absorption and porosity. THEORY Shrinkage Shrinkage is the percentage decrease in dimensions during firing. Therefore, Shrinkage = (Unfired diameter Fired diameter) 100 Dry weight Water Absorption Water absorption after firing at a specified nominal temperature is the weight percentage of water absorbed by a test piece, when soaked under a vacuum. Therefore, Water absorption = (Soaked weight Dry weight) 100 Dry weight Porosity Porosity is the percentage of pores in a given sample. If, W1 - weight of a fired disk W3 - weight of the sample when freely suspended, but fully immersed in water. W2 - weight of the sample after water impregnation, then Porosity = (W2 W1) 100 (W2 W3) METHOD The required amount of calcined clay was weighed and placed in a steel mould to obtain a uniform depth. The upper die was inserted and pressure was applied by hand to expel air and give an initial compaction to the clay. The assembled die was placed centrally between the plates of the hydraulic and a compaction pressure was applied. The pressure was maintained for about 10 seconds. The ample (disk) was removed and the sample was marked using a sharp scriber. 3 samples each for shrinkage, water absorption and porosity measurements were made. The test discs were placed for firing with their scribed mark facing upwards on a refractory batt covered with a thin uniform layer of calcined alumina and insert into the kiln. After reaching the firing temperature, the disk was soaked for 2 hours and then cooled in the furnace. The discs were removed from the kiln after cooling, and any adhering alumina was brushed off and placed in a dessicator. The diameter of the first set of fired discs was measured with a micrometer.

The second set of fired discs was weighed to 0.001g. Then they were put into a small beaker and the beaker was filled with water until all the discs were fully submerged. Then the water was boiled for 5 hours while making sure that the specimens were fully submerged all the time. Then the samples were removed and soaked for an additional 24 hours. After that the specimens were removed from water and then lightly wiped and placed immediately onto a balance pan. The soaked weight was recorded to 0.001g. The third sets of fired discs were weighed to 0.001g and then the samples were boiled for 5 hours and soaked for an additional 24 hours while the specimens were fully immersed in water. The sample was weighed while freely suspended but fully immersed in water to 0.001g. The specimens were removed from water and then lightly wiped and placed immediately onto a balance pan. The weight after water impregnation was recorded to 0.001g.

CALCULATIONS Shrinkage Sample Unfired diameter /mm

25.13 25.1 25.14

Mean unfired diameter / mm

25.12333333 25.13333333 24.54666667 25.16666667

Fired diameter/mm

mean fired diameter / mm

22.12666667 22.15333333 22.13333333 22.14333333

Shrinkage /%
11.927823 11.856764 9.8316133 12.013245

S1 S2 S3 S4

22.1 22.14 22.14 22.17

22.16 22.16 22.14 22.12

22.12 22.16 22.12 22.14

25.12 25.14 25.14 25.21 23.22 25.21 25.17 25.16 25.17

For S1 Mean unfired diameter = (25.13 + 25.1 +25.14)/3 = 25.1233 Mean fired diameter = (22.1 + 22.16 + 22.12) /3 = 22.1266 Shrinkage = (25.1233 - 22.1266) / 25.1233 * 100 = 11.9278 Water Absorption Sample S1 S2 S3 S4 Dry weight/g Wet weight/g 5.384 2.93 3.6459 2.99 Water absorption / % 14.31915724 38.56415324 16.5828362

2.563 2.6312 2.5647

Water absorption = (2.93-2.563)/2.563*100 = 14.31915 Porosity Sample S1 S2 S3 S4 Dry weight/g 2.4423 2.5831 2.3942 2.5718 Wet weight/g 2.6 3.6869 3.6649 3.6464 immersed weight/g 1.4802 2.1469 2.114 2.1075 Porosity / % 14.08287194 71.67532468 81.93307112 69.82909871

RESULTS Sample S1 S2 S3 S4 Shrinkage / %

11.927823 11.856764 9.8316133 12.013245

Water absorption /% 14.31915724 38.56415324 16.5828362

Porosity / % 14.08287194 71.67532468 81.93307112 69.82909871

DISCUSSION Many properties of a sintered ceramic are strongly dependent on the pore shape and distribution. For example, the presence of pores decreases the area which the applied load affects and they also acts as stress concentrators. Experimentally, it has been found that the strength of porous ceramics decrease exponentially with the porosity. It has also been discovered that the presence of pores can be helpful under stresses (such as those induced by thermal shock) as they tend to obstruct the propagation of cracks so that only surface checking is obtained and not complete fracture. The porosity has an affect on the transfer of heat. The contribution to heat transfer by small pores will be lesser than the contribution to heat transfer made by larger pores at high temperatures. As a result the pore size is an important microstructural feature determining heat transfer properties at high temperatures. The electron and optical microscopes can be used when determining the pore size, pore shape and the connectivity of pores. When using the optical microscopes, the reflected light technique which was first used for metals is used widely. However for slices or thin sections, the transmitted light method can be used but this technique is gradually becoming unpopular. Other than the above methods X-ray diffraction can also be used. The electron microscopes are fast becoming a useful tool in the examination of very fine detail. The scanning electron microscope which works by a reflection process combines high magnification with great depth of field giving a good three dimensional structure of the material.

Due to the presence of surface pores, the true density is given by, true = M / (V Vs Vc) Where M is the mass of the object, V is the bulk volume, Vs is the volume of the surface pores, Vc is the volume of the closed pores. However, due to the presence of surface pores it is impossible to measure the true density of the sample using Archimedes law as the basis. Therefore, the determination of the true density can be done by grinding part of the specimen down to powder particles which are sufficiently small as to have no porosity within them, and then by determining the powder density. There are several errors which could affect the accuracy of the results obtained by the practical. One such error is the damaging of the unfired sample whilst measuring its diameter. When the jaws of the Vernier Caliper is placed firmly on the surface on an unfired sample, it (the sample) tends to get damaged resulting in wrong measurements. Marking the samples using a sharp scribe will also affect the accuracy of the sample as the amount of material removed may differ from sample to sample resulting in differing weights. Such an action may also affect the porosity of the sample as there is a tendency for some pores within the sample to become surface pores. Other than the above

mentioned errors, the other possible errors are the errors that occurred during the measurement of the weight of the calcined clay, errors that occur during the measurement of weights for calculation of porosity and water absorption etc. CONCLUSION According to the results obtained above, in measuring porosity the samples used roughly contained pores about 1/3 of its total volume. However it should be noted that the values obtained are not accurate as they do not represent the true porosity. The shrinkage of the three samples is very small, especially that of sample no 1. and in water absorption, the weight of the water absorbed amounts to about 1/5-1/4 by weight of the samples, REFERENCES Budworth, W. D., An introduction to ceramics, Pergamon Press, 1970, 155-157p.