Understanding the Walloon method of iron refining: archaeological and archaeometric experiments, phase 1
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Published
Nov 9, 2021
Abstract
The Walloon method of refining pig (cast) iron is one of the first extensions of the blast furnace process, which appears between the 14th and 16th centuries in northern Europe. This study investigates the production capacity of Walloon refining and in particular its handling of high-phosphorus pig iron through a series of experiments. A Walloon hearth was built to refine high-phosphorus pig iron, using data on the refining process found in archaeological sources and historical documents fro m the 18th century onwards. The chemical composition and the structure of the metals and slag produced during refining have been determined. A similar yield to those mentioned in historical sources has been obtained. These experiments suggest specific techniques enabling high-phosphorus pig iron to be refined efficiently. Finally,the results point out the importance of the metal-slag reaction phase in obtaining a carbon-free and phosphorus-free material.
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References
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Arribet-Deroin D 2010, ‘Une industrie normande au début du procédé indirect (1450-1600) : la sidérurgie du pays de Bray et l’usine à fer de Glinet’, in M Arnoux and A-M Flambard-Héricher (eds),
La Normandie dans l’économie européenne (XIIe-XVIIe siècle) (Caen), 119-137.
Awty B G 2006, ‘The elusive Walloon finery forges of Liège’, Historical Metallurgy 40(2), 129-137.
Awty B G 2007, ‘The development and dissemination of the walloon method of ironworking’, Technology and Culture 48, 783-803.
Bedwin O R 1978, ‘The excavation of a late sixteenth/early seventeenth century gun-casting furnace at Maynard’s Gate, Crowborough, East Sussex, 1975-76’, Sussex Archaeological
Collections 116, 163-178.
Bedwin O R, 1980, ‘The excavation of a late sixteenth-century blast furnace at Batsford, Herstmonceux, East Sussex, 1978’, Post-Medieval Archaeology 14, 89-112.
Belhoste J-F 2001, ‘Mutations techniques et filières marchandes dans la sidérurgie alpine entre le XIIIe et le XVIe siècle’, in P Braunstein (ed), La sidérurgie alpine en Italie (XIIe-XVIIe siècle) (Rome), 515-624.
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Bouchu E and Courtivon G 1774, ‘Art des forges et fourneaux à fer, description des arts et métiers faites ou approuvées par MM. de l’Académie royale des sciences de Paris’, Description des arts et métiers, vol 2. available on cnum.cnam.fr
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Dillmann P, Arribet-Deroin D, Vega E and Benoit P 2007. ‘Early modern cast iron and iron at Glinet’, in I-M P Jensen and U Öhman (eds), Norberg-Nora, 700 years of ironmaking (Stockholm: Jernkontorets Bergshistorika Rapporter H78), 99-106.
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Dillmann P and L’Héritier M 2007, ‘Slag inclusion analyses for studying ferrous alloys employed in French medieval buildings: supply of materials and diffusion of smelting processes’, Journal of Archaeological Science 34, 1810-1823.
Dumas J B 1833, Traité de Chimie Appliquée aux Arts (Paris).
Durand-Charre M 2003, La microstructure des aciers et des fontes (Paris).
Hellot J (ed) 1966, ‘Cahier G’, Bibliothèque Municipale de Caen In-4° 171.
Im J, Morita K and Sano N 1996, ‘Phosphorus distribution between CaO-SiO2-FeO slags and carbon-saturated iron at 1573 K’, Iron and Steel Institute of Japan International 36, 517-521.
Le Coze J 2008, ‘Histoires de fontes. Les descriptions du XVIIIe siècle. Partie II: Sur les diverses conceptions de l’affinage des fontes au bas foyer’, Comptes Rendus Chimie 11, 1584-1603.
Lechevallier G, Dillmann P, Benoit P and Fluzin P 2000, ‘L’affinage wallon des fontes phosphoreuses, approche expérimentale et historique’, in P Benoit and P Fluzin (eds), Arts du feu et production artisanale (Antibes), 171-182.
Litz J, Rahmel A and Schorr M 1988, ‘Selective carbide oxidation and internal nitridation of the Ni-Base Superalloys IN 738 LC and IN 939 in Air’, Oxidation of Metals 30(1/2), 95-105.
Mackenzie R J and Whiteman JA 2006, ‘ Why pay more? An archaeometallurgical investigation of 19th-century Swedish wrought iron and Sheffield blister steel’, Historical Metallurgy
40, 138-149.
Philibert J, Vignes A, Brechet Y and Combrade P 1998, Métallurgie du minerai au matériau (Paris).
Piaskowsky J 1989, ‘Phosphorous in iron ore and slag and in bloomery iron’, Archaeomaterials 3, 47-59.
Stewart J W, Charles J A and Wallach E R 2001, ‘Iron-Phosphorus-Carbon system part III - Metallography of low carbon iron - phosphorus alloys’, Materials Science and Technology 16, 291-303.
Tylecote R F 1992, A history of metallurgy (London).
Vega E, Dillmann P and Fluzin P 2002, ‘Contribution à l’étude du fer phosphoreux en sidérurgie ancienne’, Revue d’Archéométrie 26, 197-208.
Weber J P 1997, Marsolle : un complexe sidérurgique du XVIe siècle en terre de Mirwart (Luxembourg).
Williams A 2003, ‘Biringuccio and the metallurgy of Italian armour’, Archaeometallurgy in Europe (Milan), 143-151.
Arribet-Deroin D 2001, ‘Fondre le fer en gueuses au XVIe siècle. Le haut fourneau de Glinet en pays de Bray (Normandie)’, Archéologie, Paris I Sorbonne (Paris).
Arribet-Deroin D 2010, ‘Une industrie normande au début du procédé indirect (1450-1600) : la sidérurgie du pays de Bray et l’usine à fer de Glinet’, in M Arnoux and A-M Flambard-Héricher (eds),
La Normandie dans l’économie européenne (XIIe-XVIIe siècle) (Caen), 119-137.
Awty B G 2006, ‘The elusive Walloon finery forges of Liège’, Historical Metallurgy 40(2), 129-137.
Awty B G 2007, ‘The development and dissemination of the walloon method of ironworking’, Technology and Culture 48, 783-803.
Bedwin O R 1978, ‘The excavation of a late sixteenth/early seventeenth century gun-casting furnace at Maynard’s Gate, Crowborough, East Sussex, 1975-76’, Sussex Archaeological
Collections 116, 163-178.
Bedwin O R, 1980, ‘The excavation of a late sixteenth-century blast furnace at Batsford, Herstmonceux, East Sussex, 1978’, Post-Medieval Archaeology 14, 89-112.
Belhoste J-F 2001, ‘Mutations techniques et filières marchandes dans la sidérurgie alpine entre le XIIIe et le XVIe siècle’, in P Braunstein (ed), La sidérurgie alpine en Italie (XIIe-XVIIe siècle) (Rome), 515-624.
Belhoste J-F, Lecherbonnier Y, Arnoux M, Arribet D, Awty B G and Rioult M 1991, La métallurgie normande XIIe-XVIIe siècles. La révolution du haut fourneau Inventaire Général SPADEM (Paris).
Belhoste J-F and Léon P 1996, ‘Naissance d’une sidérurgie moderne aux confins du Berry (fin du XIVe - XVe siècles), Mélanges Jean-Yves Ribault’, Cahiers d’Archéologie et d’Histoire du Berry, hors-série, 45-52.
Birembaut A and Tuillier G 1966, ‘Une source inédite : les cahiers du chimiste Jean Hellot (1685-1766)’, Annales ESC 21, 357-364.
Biringuccio V 1540, La Pirotechnia, (ed Smith C S and M T Gnudi 1990, New York).
Booker H, Kunrath A O and Hepworth M T 1997, ‘Experimental determination of ternary diagram of the Ti-Cr-C system’, Acta Materialia 45(4), 1625-1632.
Bouchu E and Courtivon G 1774, ‘Art des forges et fourneaux à fer, description des arts et métiers faites ou approuvées par MM. de l’Académie royale des sciences de Paris’, Description des arts et métiers, vol 2. available on cnum.cnam.fr
Bourbon N 1529, ‘ Vandoperani, campani, epigrammata’, Laurent Hyllaire (Lyon). available on gallica.bnf.fr
Buchwald V F 2008, Iron, steel and cast iron before Bessemer (Copenhagen).
Cantelaube J and Verna C 2000, ‘Les forges à la génoise dans les Pyrénées ariégeoises au XVIe siècle: quel transfert d’innovation?’, in C Cucini Tizzoni and M Tizzoni (eds), Il ferro nelle Alpi (Breno), 152-163.
Crew P and Williams M 1986, ‘Early iron production in north west Wales’, Medieval iron in society II (Stockholm: Jernkontorets Bergshistorika Rapporter H39), 20-30.
Crossley D 1972, ‘A sixteenth-century Wealden blast furnace: A report on excavations at Panningridge, Sussex, 1964-1970’, Post-Medieval Archaeology 6, 42-68.
Crossley D 1975a, ‘Cannon-manufacture at Pippingford, Sussex: The excavation of two iron furnaces of c 1717’, Post-Medieval Archaeology 9, 1-37.
Crossley D 1975b, Sidney Ironworks Accounts, 1541-1573 (London: Camden 4th series vol 15).
d’Angenoust and de Wendel 1769, ‘Mémoire sur les forges et les fourneaux du Berry et du Nivernais, Le marteau Pilon’, Histoire de la Métallurgie Nivernaise 5, 1993, 19-26.
Den Ouden A 1981, ‘ The production of wrought iron in finery hearths. Part I: the finery process and its development’, Historical Metallurgy 15, 63-87.
Diderot D and d’Alembert J 1751, Encyclopédie ou dictionnaire raisonné des sciences des arts et des métiers (Paris).
Dillmann P, Arribet-Deroin D, Vega E and Benoit P 2007. ‘Early modern cast iron and iron at Glinet’, in I-M P Jensen and U Öhman (eds), Norberg-Nora, 700 years of ironmaking (Stockholm: Jernkontorets Bergshistorika Rapporter H78), 99-106.
Dillmann P, Fluzin P and Chevallier P 2002. ‘Determination of ironmaking processes using synchrotron microprobe’, in E Jerem and K T Biro (eds), Archaeometry 98: Proceedings of the 31st symposium, Budapest (Oxford: BAR IS 1043), 327-334.
Dillmann P, Hilare-Perez L and Verna C 2010 in press, ‘L’acier en Europe avant Bessemer Introduction’, in P Dillmann, L Hilare-Perez and C Verna (eds), Actes du colloque (Paris 2005) (Toulouse).
Dillmann P and L’Héritier M 2007, ‘Slag inclusion analyses for studying ferrous alloys employed in French medieval buildings: supply of materials and diffusion of smelting processes’, Journal of Archaeological Science 34, 1810-1823.
Dumas J B 1833, Traité de Chimie Appliquée aux Arts (Paris).
Durand-Charre M 2003, La microstructure des aciers et des fontes (Paris).
Hellot J (ed) 1966, ‘Cahier G’, Bibliothèque Municipale de Caen In-4° 171.
Im J, Morita K and Sano N 1996, ‘Phosphorus distribution between CaO-SiO2-FeO slags and carbon-saturated iron at 1573 K’, Iron and Steel Institute of Japan International 36, 517-521.
Le Coze J 2008, ‘Histoires de fontes. Les descriptions du XVIIIe siècle. Partie II: Sur les diverses conceptions de l’affinage des fontes au bas foyer’, Comptes Rendus Chimie 11, 1584-1603.
Lechevallier G, Dillmann P, Benoit P and Fluzin P 2000, ‘L’affinage wallon des fontes phosphoreuses, approche expérimentale et historique’, in P Benoit and P Fluzin (eds), Arts du feu et production artisanale (Antibes), 171-182.
Litz J, Rahmel A and Schorr M 1988, ‘Selective carbide oxidation and internal nitridation of the Ni-Base Superalloys IN 738 LC and IN 939 in Air’, Oxidation of Metals 30(1/2), 95-105.
Mackenzie R J and Whiteman JA 2006, ‘ Why pay more? An archaeometallurgical investigation of 19th-century Swedish wrought iron and Sheffield blister steel’, Historical Metallurgy
40, 138-149.
Philibert J, Vignes A, Brechet Y and Combrade P 1998, Métallurgie du minerai au matériau (Paris).
Piaskowsky J 1989, ‘Phosphorous in iron ore and slag and in bloomery iron’, Archaeomaterials 3, 47-59.
Stewart J W, Charles J A and Wallach E R 2001, ‘Iron-Phosphorus-Carbon system part III - Metallography of low carbon iron - phosphorus alloys’, Materials Science and Technology 16, 291-303.
Tylecote R F 1992, A history of metallurgy (London).
Vega E, Dillmann P and Fluzin P 2002, ‘Contribution à l’étude du fer phosphoreux en sidérurgie ancienne’, Revue d’Archéométrie 26, 197-208.
Weber J P 1997, Marsolle : un complexe sidérurgique du XVIe siècle en terre de Mirwart (Luxembourg).
Williams A 2003, ‘Biringuccio and the metallurgy of Italian armour’, Archaeometallurgy in Europe (Milan), 143-151.
How to Cite
Dillmann, P., Perez, A., Vega, E., Arribet-Deroin, D., & Aranda, R. (2021). Understanding the Walloon method of iron refining: archaeological and archaeometric experiments, phase 1. Historical Metallurgy, 46(1), 19-31. https://www.hmsjournal.org/index.php/home/article/view/123
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How to Cite
Dillmann, P., Perez, A., Vega, E., Arribet-Deroin, D., & Aranda, R. (2021). Understanding the Walloon method of iron refining: archaeological and archaeometric experiments, phase 1. Historical Metallurgy, 46(1), 19-31. https://www.hmsjournal.org/index.php/home/article/view/123