1 Ceramic Crucibles At least 20,000 years ago clay materials were shaped into figurines and then hardened by baking in a fire. About 10,000 years ago humans began to form utilitarian vessel out of clay and harden them in a fire. Baking clay alters both its chemical composition, structure, and properties. A kiln fired ceramic is genuinely a different substance from clay, one that does not occur in nature. The clay you will use in this experiment is an earthenware clay called kaolin that consists primarily of water and the mineral kaolinite. The water provides the “plasticity” that allows you to shape the clay. To turn clay into ceramics requires heating through three distinct phases. The first phase does not require a kiln at all (temperatures below 100˚C) and involves merely the evaporation of the water of plasticity to give a dry clay that retains its shape. This state however is not useful as pottery because if you add water to the “leather dry” clay, it will soften and lose its shape (however, it can be still re-worked into a different shape). Thus, this first phase is reversible. The second and third phase of ceramic formation require temperatures that can only be obtained in a kiln. When your piece is fired in the kiln irreversible changes take place in its chemical structure. Although the dry kaolinite has no water molecules in it per se, it loses water by combining some of the oxygen and hydrogen atoms to form water. The water released is really just a by-product as the kaolinite is converted into mullite and silica: 3 Al2Si2O5(OH)4 kaolinite → 3 Al2O3•2SiO2 + 4 SiO2 + 6 H2O mullite silica water The crystalline structure of kaolinite shows two layers: a silica layer and an alumina layer with additional hydroxyl groups (–OH) attached to the aluminum atoms. Mullite is a complex material that comes in many forms. For simplicity, we show it here as a 3:2 aluminum silicate. Kaolin that has been fired to 1000˚C is said to be calcined, which means to expel by-products, typically water or carbon dioxide, during roasting with strong heat. The calcinations binds the two “slippery” layers of kaolinite into one rigid material. Thus, in phase two we have carried out a chemical reaction that turned clay into stone. The transformation to pottery is not yet complete. In stage three we fire the ceramics to the vitrification temperature. To vitrify means to melt and turn into a glass-like substance. The melting point of mullite (1920˚C, ~3500˚F) and silica (1650˚C, ~3000˚F) are too high to be attained in ancient kilns, and the even the modern one used in this experiment. It is not the mullite or silica that melts, but rather the impurities in the kaolinite. One such impurity is called “grog” and includes materials sand (again SiO2) and/or crushed pottery that give the ceramic internal strength. Grog also gives earthenware ceramics a rough surface. Certain kinds of clay, like porcelain clay, have little or no grog. Grog also do not melt at kiln temperatures. However, kaolin is actually a mixture of kaolinite and ball clay, an earthy material that contains impurities like iron oxide that give it color. The impurities in earthenware clay vitrify at about 900˚C (~1650˚F), while those of porcelain clay vitrify at 1300˚C (~2375˚F). When the impurities melt they soak into the crystal lattice of mullite and silica. When the ceramic cools the impurities coat the minerals, making the ceramic impervious to cooking fire (260˚C, 500˚F). The earliest ceramic vessels were presumably formed by hand-shaping lumps of clay or snakes (ropes) of clay. With the invention of the potter’s wheel, a lump of clay placed at the center of a spinning disk could more evenly and smooth formed to give a more uniform product. The vessel you will make does not involve the familiar potter’s wheel, but will instead be molded by hand. FYEC 175 Crucible 2 Time Management This experiment will be spread out over several days. On day 1 you will make your crucibles – at least four of them. Make the lids first let them dry for as long as possible. Ideally you should wait 4 to 5 hours, but you don’t have that long, so try to let them dry for up to an hour. Then make your lids. We will let them dry until the next class (day 3). They will be weighed, then fired and ready for you in the next class (day 5). Overview • • • • • • Hand form crucibles Dry crucibles Form lids on dried crucibles Weigh crucibles Fire crucibles Re-weigh crucibles A. Shaping the wet (plastic) clay into a “pinch pot” Materials low fire earthenware clay beaker 1. Before you start have a bowl or beaker of water ready. paper drying board Note: If you work clay with dry hands, it is likely to crack. 2. Procure a 6 cm x 6 cm x 6 cm lump of earthenware clay (white or red) from your instructor. 3. Place a piece of regular 8.5" x 11" paper on your bench. This will be your work surface. Hint – because the clay is sticky, it is easier to turn clay on paper than on clay on the bench. 4. Place the lump of clay onto the work surface and press your thumb into the middle to create a dimple. 5. Rotate the clay and continue to work deeper into the pot until wall of the crucible begin to take shape. Hint – if your hand or the clay starts to get dry, wet your fingers in a bowl of water. 6. Be sure to stop every once and a while to check the shape of the pot. Strive to for wall of uniform thickness (~ 8 mm) as you rotate the pot. The pot should be conical or parabolic in shape: rounded at the bottom and sloping upward and outward on the sides. Hint – You success at this operation depends on your ability to stop and analyze the developing shape and make necessary corrections. 7. Once you are satisfied with the shape of the bowl, start to for the base. To begin gently pinch just below the bottom of the bowl. 8. Flare the base to the pot will have a will, firm base to stand on. Hint – A common mistake at the point is form the pedestal off-center resulting in a pot that tips. Be sure to check and correct as you go. 9. Make any final adjustments to the shape of the crucible. Again your goal is uniformity and symmetry. FYEC 175 Crucible 3 10. When you are satisfied with the shape place the pot on the paper and hold a knife blade against the pot at a constant height and turn the pot to mark a line that indicates a uniform height. Then gently cut the clay until even all the way round. 11. Make 3 more crucibles. 12. Scratch you initials and a unique number unique on the bottom of the pedestals. 13. Place your crucibles on a board to dry for an hour or so. B. Final shaping and making the lid 1. Procure a fresh lump of clay about 2 cm x 6 cm x 6 cm. 2. Either by hand or with a rolling pin, roll the clay flat to a thickness of about 8 mm. 3. Place your partially dried crucible upside down on the flattened lid. Use a knife to cut a round circle that is larger than your crucible by 1 cm all the way around. 4. Turn your crucible right side up and set it on its pedestal. Gently press the soft lid into the harden crucible until the lid has a rim that folds over the edge of the crucible. The lid will look like a shallow dish. Gentle – if you press too hard you will deform the crucible. 6. Turn the crucible and lid over again so the crucible is again resting on the upside-down lid. Gently remove the crucible from the lid and set it right side up. 7. Make lids for your other crucibles. Hint – Each crucible has its own unique shape and therefore its own unique lid. Don’t get them mixed up. 8. Label each lid with your initials and the number that matches the one on the pedestal. 9. Transfer the crucibles to a board. Let them dry until next class. C. Weighing crucible 1. Weigh each crucible and record the weight in your lab notebook. 2. Turn in your crucible and lids for firing. D. Firing your crucible 1. Your crucible will be fired for you in an electric kiln to cone 05 (1063˚C, 1945˚F). Your fired crucible is now bone dry and called “bisque” or “bisqueware”. FYEC 175 Crucible 4 2. Record the weight of the fired crucibles. 3. Calculate the amount of water lost from each crucible (as a percentage), and then average the values. Questions – How much water was lost? If your clay were pure, dry kaolinite, how much water should be lost? Adapted from Caveman Chemistry by Kevin M. Dunn (Universal Press, 2003, p. 60) FYEC 175 Crucible
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