Crucible

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A modern crucible used in the production of silicon ingots via the Czochralski process Czochralski method used crucible 1.jpg
A modern crucible used in the production of silicon ingots via the Czochralski process

A crucible is a ceramic or metal container in which metals or other substances may be melted or subjected to very high temperatures. While crucibles were historically usually made from clay, [1] they can be made from any material that withstands temperatures high enough to melt or otherwise alter its contents.

Contents

History

Typology and chronology

The form of the crucible has varied through time, with designs reflecting the process for which they are used, as well as regional variation. The earliest crucible forms derive from the sixth/fifth millennium B.C. in Eastern Europe and Iran. [2]

Chalcolithic

Crucibles used for copper smelting were generally wide shallow vessels made from clay that lacks refractory properties which is similar to the types of clay used in other ceramics of the time. [3] During the Chalcolithic period, crucibles were heated from the top by using blowpipes. [4] Ceramic crucibles from this time had slight modifications to their designs such as handles, knobs or pouring spouts [5] allowing them to be more easily handled and poured. Early examples of this practice can be seen in Feinan, Jordan. [4] These crucibles have added handles to allow for better manipulation, however, due to the poor preservation of the crucibles there is no evidence of a pouring spout. The main purpose of the crucible during this period was to keep the ore in the area where the heat was concentrated to separate it from impurities before shaping. [6]

A crucible furnace dating to 2300–1900 BC for bronze casting has been found at a religious precinct of Kerma. [7]

Iron Age

The use of crucibles in the Iron Age remains very similar to that of the Bronze Age with copper and tin smelting being used to produce bronze. The Iron Age crucible designs remain the same as the Bronze Age.[ citation needed ]

The Roman period shows technical innovations, with crucibles for new methods used to produce new alloys. The smelting and melting process also changed with both the heating technique and the crucible design. The crucible changed into rounded or pointed bottom vessels with a more conical shape; these were heated from below, unlike prehistoric types which were irregular in shape and were heated from above. These designs gave greater stability within the charcoal. [8] These crucibles in some cases have thinner walls and have more refractory properties. [9]

During the Roman period a new process of metalworking started, cementation, used in the production of brass. This process involves the combination of a metal and a gas to produce an alloy. [10] Brass is made by mixing solid copper metal with zinc oxide or carbonate which comes in the form of calamine or smithsonite. [11] This is heated to about 900 °C, the zinc oxide vaporizes into a gas, and the zinc gas bonds with the molten copper. [12] This reaction has to take place in a part-closed or closed container otherwise the zinc vapor would escape before it can react with the copper. Cementation crucibles, therefore, have a lid or cap which limits the amount of gas loss from the crucible. The crucible design is similar to the smelting and melting crucibles of the period utilizing the same material as the smelting and melting crucibles. The conical shape and smallmouth allowed the lid to be added. These small crucibles are seen in Colonia Ulpia Trajana (modern-day Xanten), Germany, where the crucibles are around 4 cm in size, however, these are small examples. [13] There are examples of larger vessels such as cooking pots and amphorae being used for cementation to process larger amounts of brass; since the reaction takes place at low temperatures lower fired ceramics could be used. [6] The ceramic vessels which are used are important as the vessel must be able to lose gas through the walls otherwise the pressure would break the vessel. Cementation vessels are mass-produced due to crucibles having to be broken open to remove the brass once the reaction has finished as in most cases the lid would have baked hard to the vessel or the brass might have adhered to the vessel walls.

Medieval period

Smelting and melting of copper and its alloys such as leaded bronze were smelted in crucibles similar to those of the Roman period which have thinner walls and flat bases to sit within the furnaces. The technology for this type of smelting started to change at the end of the Medieval period with the introduction of new tempering material for the ceramic crucibles. Some of these copper alloy crucibles were used in the making of bells. Bell foundry crucibles had to be larger at about 60 cm. [14] These later medieval crucibles were a more mass-produced product.

The cementation process, which was lost from the end of the Roman to the early Medieval period, continued in the same way with brass. Brass production increased during the medieval period due to a better understanding of the technology behind it. Furthermore, the process for carrying out cementation for brass did not change greatly until the 19th century. [15]

However, during this period a vast and highly important technological innovation happened using the cementation process, the production of crucible steel. Steel production using iron and carbon works similarly to brass, with the iron metal being mixed with carbon to produce steel. The first examples of cementation steel are wootz steel from India, [16] where the crucibles were filled with good quality low-carbon wrought iron and carbon in the form of organics such as leaves, wood, etc. However, no charcoal was used within the crucible. These early crucibles would only produce a small amount of steel as they would have to be broken once the process has finished.

By the late Medieval period, steel production had moved from India to modern-day Uzbekistan where new materials were being used in the production of steel crucibles, for example, Mullite crucibles were introduced. [17] These were sandy clay crucibles which had been formed around a fabric tube. [17] These crucibles were used in the same way as other cementation vessels but with a hole in the top of the vessel to allow pressure to escape.

Post-Medieval

At the end of the Medieval Era and into the Post-Medieval Era, new types of crucible designs and processes started. Smelting and melting crucibles types started to become more limited in designs which are produced by a few specialists. The main types used during the Post Medieval period are the Hessian crucibles which were made in the Hesse region in Germany. These are triangular vessels made on a wheel or within a mold using high alumina clay and tempered with pure quartz sand. [18] Furthermore, another specialized crucible which was made at the same time was that of a graphite crucible from southern Germany. These had a very similar design to that of the triangular crucibles from Hesse but they also occur in conical forms. These crucibles were traded all across Europe and the New World.

The refining of methods during the Medieval and Post-Medieval periods led to the invention of the cupel which resembles a small egg cup, made of ceramic or bone ash which was used to separate base metals from noble metals. This process is known as cupellation. Cupellation started long before the Post Medieval period, however, the first vessels made to carry out this process started in the 16th Century. [19] Another vessel used for the same process is a scorifier which is similar to a cupel but slightly larger and removes the lead and leaves the noble metals behind. Cupels and scorifiers were mass-produced as after each reduction the vessels would have absorbed all of the lead and become fully saturated. These vessels were also used in the process of metallurgical assay where the noble metals are removed from a coin or a weight of metal to determine the amount of the noble metals within the object.

Modern-day uses

Crucibles used in Czochralski method Czochralski method crucibles.jpg
Crucibles used in Czochralski method
Melting gold in a graphite crucible Melting crucible.jpg
Melting gold in a graphite crucible
Three crucibles used by Thomas Edison Menlo Lab Cruicibles.jpg
Three crucibles used by Thomas Edison

Crucible is used in the laboratory to contain chemical compounds when heated to extremely high temperatures. Crucibles are available in several sizes and typically come with a correspondingly-sized lid. When heated over a flame, the crucible is often held inside a pipeclay triangle which itself is held on top of a tripod.

Crucibles and their covers are made of high temperature-resistant materials, usually porcelain, alumina or an inert metal. One of the earliest uses of platinum was to make crucibles. Ceramics such as alumina, zirconia, and especially magnesia will tolerate the highest temperatures. More recently, metals such as nickel and zirconium have been used. The lids are typically loose-fitting to allow gases to escape during the heating of a sample inside. Crucibles and their lids can come in high form and low form shapes and in various sizes, but rather small 10 to 15 ml size porcelain crucibles are commonly used for gravimetric chemical analysis. These small-size crucibles and their covers made of porcelain are quite cheap when sold in quantity to laboratories, and the crucibles are sometimes disposed of after use in precise quantitative chemical analysis. There is usually a large mark-up when they are sold individually in hobby shops.

In the area of chemical analysis, crucibles are used in quantitative gravimetric chemical analysis (analysis by measuring mass of an analyte or its derivative). Common crucible use may be as follows. A residue or precipitate in a chemical analysis method can be collected or filtered from some sample or solution on special "ashless" filter paper. The crucible and lid to be used are pre-weighed very accurately on an analytical balance. After some possible washing and/or pre-drying of this filtrate, the residue on the filter paper can be placed in the crucible and fired (heated at very high temperature) until all the volatiles and moisture are driven out of the sample residue in the crucible. The "ashless" filter paper is completely burned up in this process. The crucible with the sample and lid is allowed to cool in a desiccator. The crucible and lid with the sample inside are weighed very accurately again only after it has completely cooled to room temperature (higher temperature would cause air currents around the balance giving inaccurate results). The mass of the empty, pre-weighed crucible and lid is subtracted from this result to yield the mass of the completely dried residue in the crucible.

A crucible with a bottom perforated with small holes which are designed specifically for use in filtration, especially for gravimetric analysis as just described, is called a Gooch crucible after its inventor, Frank Austin Gooch.

For completely accurate results, the crucible is handled with clean tongs because fingerprints can add a weighable mass to the crucible. Porcelain crucibles are hygroscopic, i. e. they absorb a bit of weighable moisture from the air. For this reason, the porcelain crucible and lid is also pre-fired (pre-heating to high temperature) to constant mass before the pre-weighing. This determines the mass of the completely dry crucible and lid. At least two firings, coolings, and weighings resulting in exactly the same mass are needed to confirm the constant (completely dry) mass of the crucible and lid and similarly again for the crucible, lid, and sample residue inside. Since the mass of every crucible and lid is different, the pre-firing/pre-weighing must be done for every new crucible/lid used. The desiccator contains desiccant to absorb moisture from the air inside, so the air inside will be completely dry.

See also

Related Research Articles

Alloy Mixture or metallic solid solution composed of two or more elements

An alloy is an admixture of metals, or a metal combined with one or more other elements. For example, combining the metallic elements gold and copper produces red gold, gold and silver becomes white gold, and silver combined with copper produces sterling silver. Combining iron with non-metallic carbon or silicon produces alloys called steel or silicon steel. The resulting mixture forms a substance with properties that often differ from those of the pure metals, such as increased strength or hardness. Unlike other substances that may contain metallic bases but do not behave as metals, such as aluminium oxide (sapphire), beryllium aluminium silicate (emerald) or sodium chloride (salt), an alloy will retain all the properties of a metal in the resulting material, such as electrical conductivity, ductility, opacity, and luster. Alloys are used in a wide variety of applications, from the steel alloys, used in everything from buildings to automobiles to surgical tools, to exotic titanium alloys used in the aerospace industry, to beryllium-copper alloys for non-sparking tools. In some cases, a combination of metals may reduce the overall cost of the material while preserving important properties. In other cases, the combination of metals imparts synergistic properties to the constituent metal elements such as corrosion resistance or mechanical strength. Examples of alloys are steel, solder, brass, pewter, duralumin, bronze, and amalgams.

Brass Alloy of copper and zinc

Brass is an alloy of copper and zinc, in proportions which can be varied to achieve varying mechanical, electrical, and chemical properties. It is a substitutional alloy: atoms of the two constituents may replace each other within the same crystal structure.

Metallurgy Domain of materials science that studies the physical and chemical behavior of metals

Metallurgy is a domain of materials science and engineering that studies the physical and chemical behavior of metallic elements, their inter-metallic compounds, and their mixtures, which are called alloys. Metallurgy encompasses both the science and the technology of metals; that is, the way in which science is applied to the production of metals, and the engineering of metal components used in products for both consumers and manufacturers. Metallurgy is distinct from the craft of metalworking. Metalworking relies on metallurgy in a similar manner to how medicine relies on medical science for technical advancement. A specialist practitioner of metallurgy is known as a metallurgist.

Slag Glass-like by-product left over after a desired metal has been separated from its raw ore

Slag is the glass-like by-product left over after a desired metal has been separated from its raw ore. Slag is usually a mixture of metal oxides and silicon dioxide. However, slags can contain metal sulfides and elemental metals. While slags are generally used to remove waste in metal smelting, they can also serve other purposes, such as assisting in the temperature control of the smelting, and minimizing any re-oxidation of the final liquid metal product before the molten metal is removed from the furnace and used to make solid metal. In some smelting processes, such as ilmenite smelting to produce titanium dioxide, the slag is the valuable product instead of the metal.

Crucible steel Type of steel

Crucible steel is steel made by melting pig iron, iron, and sometimes steel, often along with sand, glass, ashes, and other fluxes, in a crucible. In ancient times steel and iron were impossible to melt using charcoal or coal fires, which could not produce temperatures high enough. However, pig iron, having a higher carbon content and thus a lower melting point, could be melted, and by soaking wrought iron or steel in the liquid pig-iron for a long time, the carbon content of the pig iron could be reduced as it slowly diffused into the iron. Crucible steel of this type was produced in South and Central Asia during the medieval era. This generally produced a very hard steel, but also a composite steel that was inhomogeneous, consisting of a very high-carbon steel and a lower-carbon steel. This often resulted in an intricate pattern when the steel was forged, filed or polished, with possibly the most well-known examples coming from the wootz steel used in Damascus swords. The steel was often much higher in carbon content and in quality in comparison with other methods of steel production of the time because of the use of fluxes.

Cementation process

The cementation process is an obsolete technology for making steel by carburization of iron. Unlike modern steelmaking, it increased the amount of carbon in the iron. It was apparently developed before the 17th century. Derwentcote Steel Furnace, built in 1720, is the earliest surviving example of a cementation furnace. Another example in the UK is the cementation furnace in Doncaster Street, Sheffield.

Reverberatory furnace metallurgical furnace

A reverberatory furnace is a metallurgical or process furnace that isolates the material being processed from contact with the fuel, but not from contact with combustion gases. The term reverberation is used here in a generic sense of rebounding or reflecting, not in the acoustic sense of echoing.

Cupellation

Cupellation is a refining process in metallurgy where ores or alloyed metals are treated under very high temperatures and have controlled operations to separate noble metals, like gold and silver, from base metals, like lead, copper, zinc, arsenic, antimony, or bismuth, present in the ore. The process is based on the principle that precious metals do not oxidise or react chemically, unlike the base metals, so when they are heated at high temperatures, the precious metals remain apart, and the others react, forming slags or other compounds.

History of metallurgy in the Indian subcontinent

The history of metallurgy in the Indian subcontinent began prior to the 3rd millennium BCE and continued well into the British Raj. Metals and related concepts were mentioned in various early Vedic age texts. The Rigveda already uses the Sanskrit term Ayas(आयस) (metal). The Indian cultural and commercial contacts with the Near East and the Greco-Roman world enabled an exchange of metallurgic sciences. With the advent of the Mughals, foreign Mughal Empire further improved the established tradition of metallurgy and metal working in India.

Foundry

A foundry is a factory that produces metal castings. Metals are cast into shapes by melting them into a liquid, pouring the metal into a mold, and removing the mold material after the metal has solidified as it cools. The most common metals processed are aluminium and cast iron. However, other metals, such as bronze, brass, steel, magnesium, and zinc, are also used to produce castings in foundries. In this process, parts of desired shapes and sizes can be formed.

Spelter

Spelter is a zinc–lead alloy that ages to resemble bronze, but is softer and has a lower melting point. The name can also refer to a copper–zinc alloy used for brazing, or to pure zinc.

Arsenical bronze

Arsenical bronze is an alloy in which arsenic, as opposed to or in addition to tin or other constituent metals, is added to copper to make bronze. The use of arsenic with copper, either as the secondary constituent or with another component such as tin, results in a stronger final product and better casting behavior.

Ferrous metallurgy

Ferrous metallurgy, the metallurgy of iron and its alloys, began in prehistory. The earliest surviving iron artifacts, from the 4th millennium BC in Egypt, were made from meteoritic iron-nickel. It is not known when or where the smelting of iron from ores began, but by the end of the 2nd millennium BC iron was being produced from iron ores from at least Greece to India, and in Sub-Saharan Africa. The use of wrought iron was known by the 1st millennium BC, and its spread defined the Iron Age. During the medieval period, smiths in Europe found a way of producing wrought iron from cast iron using finery forges. All these processes required charcoal as fuel.

Zinc smelting is the process of converting zinc concentrates into pure zinc. Zinc smelting has historically been more difficult than the smelting of other metals, e.g. iron, because in contrast, zinc has a low boiling point. At temperatures typically used for smelting metals, zinc is a gas that will escape from a furnace with the flue gas and be lost, unless specific measures are taken to prevent it.

Metals and metal working had been known to the people of modern Italy since the Bronze Age. By 53 BC, Rome had expanded to control an immense expanse of the Mediterranean. This included Italy and its islands, Spain, Macedonia, Africa, Asia Minor, Syria and Greece; by the end of the Emperor Trajan's reign, the Roman Empire had grown further to encompass parts of Britain, Egypt, all of modern Germany west of the Rhine, Dacia, Noricum, Judea, Armenia, Illyria, and Thrace. As the empire grew, so did its need for metals.

Gold parting

Gold parting is the separating of gold from silver. Gold and silver are often extracted from the same ores and are chemically similar and therefore hard to separate. Over the centuries special means of separation have been invented.

Ancient iron production refers to iron working in times from prehistory to the early Middle Ages where knowledge of production processes is derived from archaeological investigation. Slag, the byproduct of iron-working processes such as smelting or smithing, is left at the iron-working site rather than being moved away with the product. It also weathers well and hence it is readily available for study. The size, shape, chemical composition and microstructure of slag are determined by features of the iron-working processes used at the time of its formation.

Experimental archaeometallurgy is a subset of experimental archaeology that specifically involves past metallurgical processes most commonly involving the replication of copper and iron objects as well as testing the methodology behind the production of ancient metals and metal objects. Metals and elements used primarily as alloying materials, such as tin, lead, and arsenic, are also a part of experimental research.

Conservation and restoration of copper-based objects

The conservation and restoration of copper and copper-alloy objects is the preservation and protection of objects of historical and personal value made from copper or copper alloy. When applied to items of cultural heritage, this activity is generally undertaken by a conservator-restorer.

Non-ferrous extractive metallurgy metallurgy process

Non-ferrous extractive metallurgy is one of the two branches of extractive metallurgy which pertains to the processes of reducing valuable, non-iron metals from ores or raw material. Metals like zinc, copper, lead, aluminium as well as rare and noble metals are of particular interest in this field, while the more common metal, iron, is considered a major impurity. Like ferrous extraction, non-ferrous extraction primarily focuses on the economic optimization of extraction processes in separating qualitatively and quantitatively marketable metals from its impurities (gangue).

References

  1. Percy, John. Natural Refractory Materials Employed in the Construction of Crucibles, Retorts, Forunaces &c. Metallurgy. London: W. Clowes and Sons, 1861. 208–09. Print.
  2. Pigott, Vincent C. "The Neolithic (C.A 7500–5500 B.C) and Caltholithic (C.A 5500–3200 B.C) Periods." The Archaeometallurgy of the Asian Old World. Philadelphia: UPenn Museum of Archaeology, 1999. 73–74. Google Scholar. Web.
  3. Rehren T. & Thornton C. P, 2009, A truly refractory crucible from fourth millennium Tepe Hissar, Northeast Iran, Journal of Archaeological Science, Vol. 36, pp2700–2712
  4. 1 2 Hauptmann A., 2003, Developments in copper Metallurgy During the Fourth and Third Millennia B.C. at Feinan, Jordan, P. Craddock & J. Lang, Eds, Mining and Metal Production Through the Ages, British Museum Press, London, pp93–100
  5. Bayley & Rehren 2007: p 47
  6. 1 2 Rehren Th., 2003, Crucibles as Reaction Vessels in Ancient Metallurgy, Ed in P. Craddock & J. Lang, Mining and Metal Production Through the Ages, British Museum Press, London pp207–215
  7. Childs, T. and Killick, D. 1993. Indigenous African metallurgy: nature and culture. Annual Review of Anthropology, 22: 317–37.
  8. Bayley & Rehren 2007: p 49
  9. Tylecote 1976: p 20
  10. Zwicker et al. 1985: p 107
  11. Rehren 2003: p 209
  12. Rehren 1999: p 1085
  13. Rehren Th., 1999, Small Size, Large Scale Roman brass Production in Germania Inferior, Journal of Archaeological Science, Vol. 26, pp 1083–1087
  14. Tylecote 1976: p 73
  15. Craddock P., 1995, Early Metal Mining and Production, Edinburgh University Press Ltd, Edinburgh
  16. Craddock 1995: p 276
  17. 1 2 Rehren, Th. and Papakhristu, O., 2000, Cutting Edge Technology – The Ferghana Process of Medieval crucible steel Smelting, Metalla, Bochum, 7(2) pp55–69
  18. Martinon-Torres M. & Rehren Th., 2009, Post-Medieval crucible Production and Distribution: A Study of Materials and Materialities, Archaeometry Vol.51 No.1 pp49–74
  19. Rehren 2003: p 208

Bibliography

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  6. Rehren T. & Thornton C. P, 2009, A truly refractory crucible from fourth millennium Tepe Hissar, Northeast Iran, Journal of Archaeological Science, Vol. 36, pp2700–2712
  7. Rehren Th., 1999, Small Size, Large Scale Roman brass Production in Germania Inferior, Journal of Archaeological Science, Vol. 26, pp 1083–1087
  8. Rehren Th., 2003, Crucibles as Reaction Vessels in Ancient Metallurgy, Ed in P. Craddock & J. Lang, Mining and Metal Production Through the Ages, British Museum Press, London pp207–215
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