Laboratory of Process Metallurgy ANNUAL REPORT 2003

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1 3 DEPARTMENT OF PROCESS AND ENVIRONMENTAL ENGINEERING Laboratory of Process Metallurgy Editor: BERITH ZINOVJEV UNIVERSITY OF OULU LABORATORY OF PROCESS METALLURGY P.O. BOX 4300 FIN UNIVERSITY OF OULU OULU UNIVERSITY PRESS OULU 2004

2 4 PREFACE The year 2003 was the 11th calendar year in the history of our unit. However, it was only five years ago that we obtained the status of a Laboratory of Process Metallurgy and our new premises. When looking at the situation today, I can only note with gratitude and appreciation the magnitude of the achievement of our staff. From a modest beginning we have been able to develop a well-functioning teaching and research unit for the Department of Process and Environmental Engineering. Our department has defined its own mission and vision. The goals of the Laboratory of Process Metallurgy are in line with the department s aspirations. Our aim is to be awarded the status of High-quality Education Unit and Centre of Excellence in the near future. In the field of teaching we have already reached the goal of High-Quality-Unit-of-Education as the status has been awarded to our unit for the next three years starting from the year The work done for the latter goal by both the department and the Chair of Process Metallurgy was massive and took several years. The year 2003 was dedicated to the drafting of the application. Our pedagogical development work goes on, boosted by a pedagogical development team consisting of the laboratory teaching staff and student representatives from every year of study. In addition, pedagogical development and planning takes place on a regular basis at departmental level. In 2003 our University initiated work for the implementation of the new two-cycle degree system. Our laboratory has also assumed an active role in the effort of the department to promote the training of post-graduate researchers. The research done at our laboratory during this year has been financed primarily by the technology programmes of metallurgical industry (the National Technology Agency of Finland). The share of external funding in the financing of the research of our laboratory has been significant. Only 25 % of the total budget of the laboratory has been allocated by the University. As a result, our research work has assumed a strong applied quality compatible with the requirements of

3 5 neighbouring industry. Our co-operation with Rautaruukki and Outokumpu has continued to be successful and mutually beneficial in the fields of both education and research. An increasing number of research reports are being published in international journals or presented at conferences. We are now better known in the world. The challenges met by our laboratory technology have been substantial: Using the construction skills of our own workshop staff and the ideas of our own researchers, we have managed to develop high-temperature research equipment on a small budget. This work is still progressing successfully. Our financial administration has been in firm hands and about 30 people have been working at our premises during the past year. As evidence of the productivity of the year, the graduation of 12 Masters of Science in Technology must be mentioned. During its 11-year existence ( ), our laboratory has produced a total of 76 M.Sc.(Tech.) degrees, 11 Lic.Sc. (Tech.) degrees, as well as one D.Sc.(Tech.) degree. The employment rate among the degree holders has been high. The operative management of our activities has been the responsibility of our laboratory management group: Teaching: Eetu Heikkinen, Lic.Sc.(Tech.), Senior Assistant, Research: Timo Fabritius, Lic.Sc.(Tech.), Professor, Technics: Riku Mattila, M.Sc.(Tech.), Financial Administration: Berith Zinovjev, Project Secretary; and I, the undersigned as Chairman. I wish to extend my warmest thanks for the successful year 2003 to all of the above mentioned people, and through them, to the whole laboratory staff. Jouko Härkki Professor Head of the laboratory

4 6 TABLE OF CONTENTS Page PREFACE 4 TABLE OF CONTENTS 6 1 LABORATORY STAFF AND STUDENTS 8 2 EDUCATIONAL ACTIVITIES University Courses Held by the Laboratory Metallurgical Processes Metallurgical Thermodynamics Theory of Pyrometallurgical Processes Laboratory Working Casting and Solidification Construction Materials of High Temperature Processes Steel Industry s Challenges 14 3 RESEARCH ACTIVITIES Reduction metallurgy Development of the Steel Belt Sintering Technology for Ferroalloys PANAMA Coke OPTIDUST II MMX CO2H Refining metallurgy TASK AHA Inclusion Control INGROS TTJV Electromagnetic Forces in Melts The Lifespan of Refractory Lining and the Properties of the Slag in Steelmaking Converter, KOVUKE 28

5 7 Page 4 RESEARCH DEVICES AND ANALYTIC INSTRUMENTS High Temperature Devices The simultaneous DTA-TGA TGA High Temperature Viscosimeter Finger Test Device Optical Dilatometer Gradient Furnace Pressure Furnace Alkali Test Others Watermodels Coulter Omnisorp 360 cx Computational Fluid Dynamics Software Thermodynamic Calculation Programmes Gas Chromatograph Microscopes Materialographic Surface Preparation of Solid Materials Other Available Facilities 35 5 PUBLICATIONS Papers Conferences and Symposiums Reports Annuals and Final Reports 39 6 THESIS Licenciate in Technology Theses Diploma Engineer Theses (Master of Science in Technology) 40 7 CONFERENCE VISITS Nordic Symposium for Young Scientists 43 8 CONTACT INFORMATION 45

6 8 1 LABORATORY STAFF AND STUDENTS Academic Staff Härkki, Jouko Taskinen, Pekka Seppänen, Matti Heinänen, Kyösti Jonsson, Lage D.Sc.(Tech), Professor, Head of the Laboratory D.Sc.(Tech), Docent in thermodynamics, Outokumpu Research Oy, Pori D.Sc.(Tech), Docent in process metallurgy, Rautaruukki Steel, Raahe D. Phil. (Geol Min), Docent in mineralogy, Rautaruukki Steel, Raahe D.Sc.(Tech), Docent in macro modelling, Luleå, Sweden Heikkinen, Eetu-Pekka Lic.(Tech), Senior Assistant Heino, Jyrki Lic. (Tech), Senior Assistant , Assistant Paananen, Timo M.Sc.(Tech), Assistant, Kokkonen, Tommi Makkonen, Hannu Mattila, Riku Tanskanen, Pekka Virtanen, Esa Angerman, Mikko Ikäheimonen, Topi Karhumaa, Teemu Teachers from Industry Hooli, Paavo Päätalo, Mika Co-lecturers: M.Sc.(Chem), Part-time teacher M.Sc.(Geol Min), Part-time teacher M.Sc.(Tech), Part-time teacher M.Sc.(Geol Min), Part-time teacher M.Sc.(Tech), Part-time teacher Student, Part-time teacher Student, Part-time teacher Student, Part-time teacher M.Sc. (Tech), Part-time teacher, Outokumpu Stainless, Tornio M.Sc. (Tech), Part-time teacher, Outokumpu Stainless, Tornio Researchers from the laboratory, Rautaruukki Steel and Outokumpu Stainless

7 9 Researchers Angerman, Mikko Erkkilä, Helena Fabritius, Timo Gornostayev, Stanislav S. Harju, Markus Heikkinen, Eetu-Pekka Hekkala, Lauri Huttunen, Satu Höynälä, Arto Kallio, Kimmo Luomala, Matti Makkonen, Hannu Mattila, Olli Mattila, Riku Mure, Petri Paananen, Timo Petäjäjärvi, Marko Talonen, Anna-Maija Tang, Yong Tanskanen, Pekka Virtanen, Esa Student, Project Manager M.Sc. (Tech), MGS, Project Manager Lic. (Tech), Special Researcher, Research Manager, Acting professor Ph.D. M.Sc. (Math) Lic. (Tech), Project Manager M.Sc. (Math) M.Sc. (Chem), GSCE M.Sc. (Phys), Project Manager M.Sc. (Tech), Project Manager, GSCE M.Sc. (Tech), Project Manager, GSCE, Acting Special Researcher M.Sc. (Geol Min), Project Manager M.Sc. (Tech), Project Manager M.Sc. (Tech) M.Sc. (Tech) M.Sc. (Tech) M.Sc. (Tech) M.Sc. (Chem) Dr. (Tech) M.Sc. (Geol Min), Project Manager M.Sc. (Tech)

8 10 Research Assistants Hekkala, Lauri Ikäheimonen, Topi Karhumaa, Teemu Kivilompolo, Laura Kokkonen, Tommi Kurkinen, Petri Kyllönen, Toni Kärnä, Aki Leinonen, Virpi Linnala, Kati Luoto, Tuula Petäjäjärvi, Marko Pöyhtäri, Samuli Sippola, Jukka Virtanen, Esa Student Student Student Student M.Sc. (Chem) Student Student Student Student Student Student Student Student Student Student Diploma Thesis Workers Hannula, Petri Hekkala, Lauri Isokääntä, Jani Kaijalainen, Antti Karjalainen, Eveliina Kärnä, Aki Leinonen, Virpi Luoto, Pasi Mure, Petri Mäenpää, Jani Petäjäjärvi, Marko Suikkanen, Pasi Tikka, Janne Virtanen, Esa

9 11 Technical Staff Kokkonen, Tommi Mattila, Riku Penttinen, Jorma Sarkkinen, Jorma Virkkala, Jouko M.Sc. (Chem), Research Assistant M.Sc.(Tech), Laboratory Manager Special Laboratory Technician, part-time Special Laboratory Technician Laboratory Technician Administration Zinovjev, Berith Heikkinen, Kaisa Project Secretary, Financial Administration Secretary, Web-master, part time Postgraduate Students Erkkilä, Helena Fabritius, Timo Heikkinen Eetu-Pekka Heino, Jyrki Hekkala, Lauri Hiltunen, Rita Huttunen, Satu (in GSCE) Kallio, Kimmo (in GSCE) Kokkonen, Tommi Luomala, Matti (in GSCE) Makkonen, Hannu Mattila, Olli (in GSCE) Mattila, Riku Niemi, Tommi Paananen, Timo Petäjäjärvi, Marko Tanskanen, Pekka Virtanen, Esa New students from Haimi Timo Halonen Lauri Junttila Satu Jääskeläinen Kari Luukkonen Antti Niskanen Samuli Närhi Lauri Prokkola Elina Pätsi Pauli

10 12 2 EDUCATIONAL ACTIVITIES Eetu-Pekka Heikkinen The primary goal of the Laboratory of Process Metallurgy is to educate people with master s and doctoral degrees (M.Sc.Eng. and D.Sc.Tech.) into the service of metallurgical industry. As a part of the department of process and environmental engineering, the laboratory also organizes its education in a way that serves the educational objectives of the whole department at the same time. Because of this it is not the laboratory s only goal to teach people to understand the metallurgical processes of iron, steel and ferroalloys production as thoroughly as possible. It is equally as important is to give students different viewpoints and perspectives to the phenomena and problems concerning metallurgical processes as well as other challenges which a freshly graduated M.Sc.Eng. may encounter in his or her future career. This means that the students have the abilities to understand, model and control the phenomena inside the processes no matter what the process in question is. In the past year the main emphasis of the educational development has been focused on the preliminary planning of the two-phase degree in engineering which will take place in The opinions and expectations of the students as well as the industrial partners have been taken into consideration from the very beginning of this planning. The education and the organised planning of the education were rewarded in 2003 when The Finnish Higher Education Evaluation Council suggested that the department of process and environmental engineering will be credited as a national High-quality Education Unit for the years UNIVERSITY COURSES HELD BY THE LABORATORY Metallurgical processes Metallurgical processes is the laboratory s only course which is directed at all the students of process engineering; not just the metallurgists. The aim of the course is to teach students the fundamentals of metallurgical unit operations and metal production in Finland as well as the basics of thermodynamics and its applications in metallurgy. Some environmental aspects are considered, too. Although the emphasis of the laboratory s education is on the production of iron, steel and ferroalloys, the production of other metals (e.g. copper, nickel, zinc and aluminium) is also considered during this course. The course is carried out with lectures, exercises and an industrial excursion which in 2003 was directed at Outokumpu Stainless Oy s steel works in Tornio. The course

11 13 was lectured by assistant Timo Paananen (M.Sc.Eng.) and part-time teacher Teemu Karhumaa. Additional lectures were held by professors Jouko Härkki (D.Sc.Tech.) and Timo Fabritius (Tech.Lic.) as well as researcher Jyrki Heino (Tech.Lic.) Metallurgical Thermodynamics The aim of the course is to equip the students with tools that are needed while examining the phenomena inside metallurgical processes in the forthcoming courses. After this course the students are required to have a sufficient knowledge of physical chemistry for thermodynamic calculations which involve gas and liquid (slag and metal) phases. The most important topics are thermodynamics of solutions, phase diagrams and the use of commercial software in thermodynamic equilibria calculations. The course was lectured in as well as in by senior assistant Eetu-Pekka Heikkinen (Tech.Lic.) and part-time teacher Topi Ikäheimonen. Jukka Vatanen and Matti Seppänen from Rautaruukki appeared as visiting lecturers Theory of Pyrometallurgical Processes During this course the phenomena inside the pyrometallurgical processes are considered using thermodynamics, kinetics, heat transfer, mass transfer and fluid dynamics. The purpose of education is not only to teach metallurgy, but also develop students ability to present their ideas and opinions both literally and verbally. The course is carried out with lectures and seminars. The course was lectured in 2003 by professor Jouko Härkki (D.Sc.Tech.) and researchers from the laboratory; e.g. Timo Fabritius (Tech. Lic.), Timo Paananen (M.Sc.Eng.) and Pekka Tanskanen (M.Sc. Geol.Min.) Laboratory Working The purpose of the course is to teach students how experimental laboratory scale research is carried out by using the experimental equipment at the university and industry s research centers. In addition to this, some safety aspects are considered during the lectures. The course was lectured in 2003 by research assistants Esa Virtanen (M.Sc.Eng) and Tommi Kokkonen (M.Sc.Chem.) as well as chief engineer Riku Mattila (M.Sc. Eng.). The exercises were supervised by researcher Timo Paananen (M.Sc.Eng.) and

12 14 researcher Esa Virtanen. This course also contained two industrial excursions which were directed at Rautaruukki s and Outokumpu s stainless steel works in Raahe and Tornio Casting and Solidification The aim of the course is to equip students with the ability to study casting and solidification using both phenomenon- and process-based viewpoints. The contents of this course have been updated and kept close to practice due to skilled lecturers from the industry. In 2003 the course was lectured by Paavo Hooli (M.Sc.Eng.) and Mika Päätalo (M.Sc.Eng.) from Outokumpu Stainless Oy Construction Materials of High Temperature Processes This course is focused on ceramic refractory and insulation materials and their use as construction materials in metallurgy and other high temperature processes. The aim of the course is to present different kind of refractory materials, their physical and chemical properties as well as interaction mechanisms between refractories and metallurgical melts (slagand metal). The course was lectured in 2003 by researcher Hannu Makkonen (M.Sc.Geol.Min.) and professor Jouko Härkki (D.Sc.Tech.). Additional lectures were held by senior assistant Eetu-Pekka Heikkinen (Tech. Lic.) Steel Industry s Challenges The aim of the last course of metallurgy is to represent metallurgical processes and industry as a part of a larger economic-technical environment in which environmental aspects are also considered. The contents features e.g. main ideas of technology roadmaps, challenges of metallurgical research and development, review of development state of alternative metallurgical processes, steel industry s effects on the enviroment and visions of future business environment of the steel industry. In 2003 the course was coordinated by professor Jouko Härkki (D.Sc.Tech.) and lectured by several lecturers from the laboratory and industry. The profitability calculation exercises were supervised in 2003 by docent Matti Seppänen (D.Sc.Tech.) from Rautaruukki. The use of visiting lecturers ensures that the contents of the course are always updated and close to practice.

13 15 3 RESEARCH ACTIVITIES Timo Fabritius Based on the strategy of the Laboratory of Process Metallurgy we have focused our research activities on iron and steelmaking processes, including carbon steelmaking, as well as stainless steelmaking unit operations. The importance of high temperature chemistry of recycling and waste treatments has increased as a form of new research projects. Furthermore, we are looking for new possibilities into breakthroughs or spinoffs with utilizing electro magnetic forces in different metallurgical unit operations. The finishing of TEKES s (National Technology Agency of Finland) technology programme Frontiers of Metallurgy ( ) has shown an accretion of arrangements of new research proposals with the industry. A remarkable amount of external financing of the laboratory came from the technology programme Frontiers of Metallurgy as part of three projects during Developing and building of research devices and analytical instruments for laboratory experiments was furthermore one of the most important investment targets. The biggest and most important investment during year 2003 was DSC-MS (Differential Scanning Calorimeter with integrated Mass Spectrometer). The production of scientific publications was at a satisfactory level despite not having even one graduated doctor of technology during the last year. There were 12 graduated diploma engineers and one graduated licentiate of technology.

14 REDUCTION METALLURGY Modelling of Belt Sintering Process - Steel Belt Oxidation Models Project Manager: Timo Fabritius Researcher: Lauri Hekkala Research Assistant: Aki Kärnä and Virpi Leinonen This 3-year subcontract research project is a continuation project of Development of steel belt sintering technology for ferroalloys, which finished at the end of The aim of this project is to present a detailed mathematical model that calculates the gas flow, temperature and composition distribution in the bed of chromite pellets and the atmosphere. Many different reactions (oxidation of coke, oxidation and reduction of iron cations in chromite, reduction of carbonates etc.) in the chromite pellets set hard challenges for the relevant description of the sintering process. Computational fluid dynamics programme Fluent is used in the flow simulations. Sub-models are developed and implemented in the calculations to describe reactions. Lots of laboratory experiments (drying of pellets, specific heat and heat conductivity of pellets, oxidation of coke and chromite etc.) were done for validation of the mathematical sub-models. Study is focused on three main reactions: 1) drying of pellet, 2) oxidation and reduction behaviour of iron cations in chromite and 3) oxidation of coke. Picture 1. Oxidation of Coke in pellet at a temperature of 850 C

15 PANAMA Panama: Novel Analysis and Optimization of Blast Furnace Burden Materials for Cost-effective and High-iron Capacity Production. Project Manager: Pekka Tanskanen Researchers: Timo Paananen and Satu Huttunen PANAMA is a subcontract project ( ) for Rautaruukki Raahe Steel. Final target of this project is to develop a mineralogy-based optimisation method for iron burden materials to enable more stable and cost-effective blast furnace operation. The research includes determination of the mineralogical evolution of ferrous burden in solid state and formation and further evolution of liquid slags from the cohesive zone down to the final blast furnace slag. A special issue of the project is to characterise alkali capture of different solid mineral systems and the alkali retention capacity of different primary liquids. The alkali retention during the liquid evolution will be determined, as well. The research was realised as laboratory-scale experiments. Different iron burden materials were used in the mineralogical part of the research. Mineralogical evolution of the iron oxides and slag phases and the initial liquid formation were determined at certain equilibrium-state reduction conditions. Mechanisms of the mineralogical alkali capture was analysed for certain burden materials. The further evolution and properties of the liquid slags, as well as the alkali retention capacity was determined with synthetic slag systems. The research methods included chemical analysis, optical microscopy, TG, SEM, XRD, DTA, viscometer, optical dilatometer, and thermodynamic equilibrium calculation.

16 Coke Coke: The Behaviour and Properties of Coke in Blast Furnace and in Cupola Furnace Project Manager: Olli Mattila Researcher: Stanislav Gornostayev Research Assistant: Tommi Kokkonen This project was started on and ends The main target of this project is to increase coke production and improvement of cost-effectiveness of coke production and decrease the reducing agent (coke, oil) consumption in BF. Additional targets are to increase knowledge in Finland and in Northern countries in the field of coke structures and the behaviour of coke in BF and to develop methods to analyse coke behaviour straight from the process data. Laboratory of Process Metallurgy will study the structural changes of coke and the main factors causing those changes as the coke moves downwards in the BF process. An additional task is to study the behaviour of coke in contact with slag and metal e.g. how the mineral particles revealed to the surface of coke will be detached to slag. The project is divided in two parts. In the first part the behaviour of coke is studied in the conditions simulating BF conditions. The second part of this project will focus on coke-slag and coke-metal interaction. Two laboratories and two industrial partners are involved in the project: Laboratory of Process Metallurgy, Laboratory of Heat Engineering, Rautaruukki Oyj and Paroc Group Oyj respectively. Coke research in Sweden is monitored through Jernkontoret s meetings.

17 Picture 2. Developed Blast Furnace Gas Phase Simulator. 19

18 OPTIDUST II OPTIDUST II - Environmentally Friendly Utilization of Dusts, Sludge, Scraps and Skulls of Raahe and Koverhar Steel Plants in Hot Metal Production Project Manager: Hannu Makkonen Researchers: Hannu Makkonen, Eetu-Pekka Heikkinen The project started on 1st of January 2002 and will be concluded on 31st of December OPTIDUST was a preliminary project, in which Rautaruukki Group s and SKJ companies recycling questions and aims were analyzed in order to establish a 3-year industrial project. Sufficient results were obtained to continue with the second phase of the project now named as OPTIDUST II. The target is to evaluate and choose the most feasible and ecological recycling and utilization technique for Fundia Koverhar s and Rautaruukki Steel s problematic and unexploitable dusts, sludge, skulls, scrap fines and scales. The information obtained will be used as a basis for an industrial designing and selection project to increase Rautaruukki s hot metal production. The project has used reduction trials of laboratory scale for the waste materials to assess the efficiency of certain recycling techniques in e.g. Zn removal. The products of the reduction tests have been analyzed chemically, physically and mineralogically in order to evaluate if the products can be utilized in iron production. The next step will be smelting tests. The reduced materials will be smelted in an induction furnace and metal and slag will be analyzed. Thermodynamic calculations complement the evaluation of different recycling methods. The harmful components (Zn, Pb, Na, K, Sn, Cd, As) were emphasized in the calculations. Furthermore, the project will collect data about cupola furnaces and rotary hearth furnaces, which are used for waste recycling. Partners in the project are National Technology Agency of Finland, Rautaruukki Group, SKJ Companies and Technical Research Centre of Finland.

19 MMX Project Manager: Mikko Angerman Researcher: Markus Harju Partners: University of Oulu, Lab. of Process Metallurgy Helsinki University of Technology, Lab. of Metallurgy Rautaruukki Group MMX project s objectives were to create a systematic method and a tool to compare process route alternatives for integrated iron and steelmaking. Duration of the whole project: Results: A novel, user-friendly simulation tool software, Factory, was produced successfully. Factory turned out to be distinguishingly flexible and is enabling plant level simulations for a variety of different process industries like any metals production, chemical industry, construction material manufacturing, energy production and pulp and paper industry. Factory s flexibility results from totally open, clear text-like and user editable calculation content. Hence Factory is easily adaptable to new application areas. Factory simulations can be carried out to e.g. calculate mass and energy balances and financial performance of selected processes, the whole plant or several plants. Also assessments of environmental friendliness with emission levels are available. Factory is useful in testing ideas for enhancing process integration too. More information about the current state of Factory is available on the internet at:

20 CO2H2 Project Manager: Mikko Angerman Researchers: Markus Harju, Jukka Sippola, Paul Fedory Partners: University of Oulu, Lab. of Process Metallurgy University of Oulu, Lab. of Control Engineering University of Oulu, Lab. of Heat and Mass Transfer Åbo Akademi, Avd. för Värmeteknik The project s objectives are to study the feasibility of present technology to achieve closed gas loop or highly circulated gas flows in process industry and power generation. The aim is to build up knowledge to participate in international research activities on the field. Study includes principles of gas reforming and upgrading, assessments of applicable technology and it s controllability, economical performance and effect to overall CO2 and other GHG (green house gas) emissions balance. Results: Factory simulation tool developed in the PYOMET research project MMX is being modified to enable required studies in CO2H2-project. Metallurgical knowledge and thermodynamics about the targeted processes are collected, analysed and reported to project partners. More information about the current state of Factory is available on the Internet at: REFINING METALLURGY TASK TASK: Effective Blowing Practice for AOD-Converter Project Manager: Timo Fabritius Researcher: Petri Mure Research Assistant: Petri Kurkinen The aim for the project TASK is to develop techniques to achieve as efficient blowing practice as possible for the 150-ton AOD converter. The project was already started

21 23 in the middle of 2001 and it will be continued till the end of June The implementation of an efficient blowing practice in the AOD needs that a large amount of gases can be blown into the steel melt in an intense but also controlled way. To achieve this, the facts having an effect on gas blowing and on its behaviour on steel melt has to be carefully known. One important phenomenon for the usability of the vessel is an oscillation of the melt bath. Oscillation does not have a direct effect on the efficiency of the process but enough strong oscillations may have a destructive effect on constructions of the AOD. During 2003 theory of the vibration of the AOD vessel during gas injection, including the model experiments and the industrial tests with AOD in Outokumpu Stainless Oy s Tornio Works, were announced. Picture 3. Intensity of vibrations with new and worn-out refractory lining of AOD.

22 AHA Controlling of Atmosphere in the AOD-converter (AHA) Project Manager: Timo Fabritius Researcher: Yong Tang, Esa Virtanen The purpose of the project was to control optimally dissolution and desorption of nitrogen in steel melt at AOD and to develop the present nitrogen model of AOD for less argon consumption. The study divided into three parts: 1) thermodynamic equilibrium calculation of nitrogen dissolution into the steel, 2) literature survey of kinetics of nitrogen absorption and desorption and 3) CFD-simulation (Fluent) of gas flows into the upper part of AOD and simulation of submerged gas injection. Based on the literature survey and thermodynamic calculation two new blowing practices for AOD were developed. According to the industrial tests, the consumption of argon decreased 20% -30% depending on the blowing practice in low carbon grade production. In new practices, desorption of nitrogen is mainly carried out during process stages where the amounts of surface-active elements (oxygen and sulphur) in the steel melt are low. The effects of geometrical parameters (distance between cone and hood, cone diameter and cone angle) and process parameters (gauge pressure, gas flow rate, gas composition and temperature) on the dissolution of nitrogen from atmosphere to the melt during reduction stage explained by using Picture 4. The computing domain, (a) the upper part is included, (b) only the water bath is selected as the computing domain and the free surface is treated as a flat plane.

23 25 CFD-model (Fluent). Furthermore, a preliminary model of submerged gas injection for simulating sidewall blowing in AOD was generated. As a result of increased knowledge three international papers, three conference presentations and six other reports were written during the project. The project was financed by TEKES (National Technology Agency of Finland) and Outokumpu Stainless Oy. The duration time of the project was about two years and it finished at the end of Inclusion Control Inclusion Control: Inclusion Engineering for Better Quality Project Manager: Helena Erkkilä and Eetu-Pekka Heikkinen ( ) Researcher: Eetu-Pekka Heikkinen Partners: Rautaruukki, Fundia Wire, HUT, VTT, Outokumpu Stainless, Imatra Steel and TEKES. The project began as a follow-up to the Oxide metallurgy ( ) and TEVITE ( ) projects at the beginning of 2002 and lasted until the end of The main objective of the project was to develop and to apply thermodynamic equilibrium calculations in predicting and controlling the inclusion composition of steel during the ladle treatments and continuous casting. The interest of research at the University of Oulu has been focused on the estimation of inclusion formation and reactions with steel using both thermodynamic calculation software and laboratory-scale experiments whereas the academic and industrial partners have concentrated on the development of thermodynamic-kinetic software for the inclusion formation calculation and applications to the process and product development.

24 INGROS INGROS: Inclusion Engineering and Grain Size Control of Steels Project Manager: Helena Erkkilä till 15th September, Funding by Nordisk Industrifond The project was started on 1st of January 2001 and ended on 31st of December The main idea behind this project was to establish the required basis for a formal collaboration between the Norwegian Ferroalloy industry (Elkem, ASA; SINTEF Materialteknologi & NTNU) and the steel industry in Sweden (Ovako Steel AB; AB Sandvik Steel & KTH) and Finland (Rautaruukki Oyj; Fundia Wire Oy Ab & HUT). This was accomplished by initiating an innovation project on inclusion engineering and grain size control of steel along with a network project to promote the education and training of students and researchers with a multidisciplinary background within the field. Part project of the Laboratory of Process Metallurgy included thermodynamic equilibrium calculations for certain ferroalloys in different circumstances. Calculations were carried out using FactSage software. According to the examination, the agreement was good between the thermodynamic calculations and experiments, which were made in Helsinki University of Technology (HUT) TTJV TTJV: Mould Powders for High Casting Speeds Project Manager: Kimmo Kallio Researcher: Marko Petäjäjärvi TTJV is a 3-year project which started on 1st of May 2001 and will end on 31st of May The project is part of the national technology programme Frontiers in Metallurgy and is financed by Rautaruukki Oyj, Outokumpu Stainless Oy and TEKES (National Technology Agency of Finland). The purpose of the project is to obtain better knowledge about mould powders and to achieve higher casting speeds and flawless surface quality in the steel industry. With higher casting speeds cleaner and better surface quality steels needs to be produced. The steel output can be increased with higher casting speeds but, at the same time, the surface quality is reduced. The aim is to achieve higher casting speed

25 27 and better surface quality by optimization of the mould powder composition. Mould powder is added automatically or manually on the surface of the molten steel where it melts. The liquid slag infiltrates into the mould/strand channel and lubricates the gap. Most of the first liquid enters the channel, freezes against the water-cooled copper mould and forms a solid slag film. This slag film (Picture 5.) controls horizontal heat transfer by both the thickness and nature of the solid slag layer. On the basis of the laboratory (DTA-TGA, XRD, XRF, SEM-EDS, HT-viscosimeter, etc.) and industrial scale experiments a better mould powder composition will be developed, at first to peritectic steel grade. Picture 5. Solid slag layer from continuous casting mould (thickness ~2 mm, mould side at the bottom) Electromagnetic Forces in Melts Project Manager: Arto Höynälä The project started on 1st of April 2003 and it will end on 30th of April The utilizing of electromagnetic forces in processing of metal melts (for example manufacturing of aluminium products) is well-known technology in the world. The aim of this project is to study the utilization and transfer of this existing knowledge and technology to steelmaking process development. Increasing of knowledge advances through the following milestones: 1) how electromagnetic forces influence the steel melt system, 2) what physical and chemical phenomena happens during electromagnetic inclusion removal and how it can be intensified and 3) what kind of electromagnetic and electric phenomena happens in SEN (submerged entry nozzle) during casting of steel.

26 The Lifespan of Refractory Lining and the Properties of the Slag in Steelmaking Converter, KOVUKE Project Manager: Matti Luomala Research Assistant: Teemu Karhumaa The project started on the 1st of October 2003 and will be concluded on the 30th of June Multiple goals have been set for the project; 1) to extend significantly the lifespan of refractory linings of Rautaruukki s converter vessels, 2) to ensure workable bottom stirring for the whole campaign length, and 3) to find out optimal slag composition for slag splashing operation. Versatile means will be applied in order to achieve the above-mentioned targets; laboratory experiments, optical dilatometer, viscosimeter, thermodynamic equilibrium calculations etc. KOVUKE is funded by the National Technology Agency of Finland and Rautaruukki Oyj. Additional partners in the project are Outokumpu Stainless Oy and Bet-Ker Oy.

27 29 4 RESEARCH DEVICES AND ANALYTIC INSTRUMENTS 4.1 HIGH TEMPERATURE DEVICES The simultaneous DSC-TGA-MS The simultaneous thermal analyzer (STA) is a Netzsch 409 PC Luxx and the mass spectrometer (MS) is a Netzsch QMS 403 Aëolos. Mass changes (thermogravimetry, TGA), characteristic temperatures and enthalpy changes (differential scanning calorimetry, DSC) and mass-specific characterization of the decomposition gases can be determined on one sample in one measurement. The furnaces maximum temperature is 1550 C and a maximum sample weight is 18 g. The maximum sensitivity of TGA is 2 µg. Mass range of MS is: amu. The device was purchased in Picture 6. The simultaneous DSC-TGA-MS

28 The simultaneous DTA-TGA The model of the device is TA- Instruments SDT It measures both differential temperature and mass changes in a material as a function of temperature and time in a controlled atmosphere. The furnaces maximum temperature is 1500 C and a maximum sample weight is 200 mg. The sensitivity of TGA is 0,1µg and DTA sensitivity is 0,001 C. The device was purchased in TGA The device measures weight changes in a material as a function of temperature and time in a controlled atmosphere. Flow Control - Brooks mass flow meter 5858S CO2 0-2 l /min accuracy ± 0.01 l /min - Brooks mass flow meter 5858S CO 0-10 l /min accuracy ± 0.05 l /min Picture 7. The homemade TGA.

29 31 Balances - Mettler-toledo AG204, sensitivity 0,1mg, max weight is 210 g. Purchased Denver TL 4102D, sensitivity is 0,01g, max weight is 4100 g. Purchased Denver APX200, sensitivity is 0,1mg, max weight is 200 g. Purchased Furnaces - The homemade furnace s maximum working temperature is 1400 C. The inside diameter of the working tube is 25 mm. This is equipped with LAND lancom series II CO,CO2,O2 gas analyzer. - The SiC furnace s maximum working temperature is 1500 C. The inside diameter of the working tube is 30 mm. -The Entech ETF / 18-V furnace s working tube inside diameter is 105 mm and it s maximum working temperature is 1800 C. It was purchased in High Temperature Viscosimeter The device measures viscosities of slag and melts as a function of temperature and time in a controlled atmosphere. The model of viscotester is Haake VT 550 and it was purchased in The furnace is Carbolite PVT 18/75/350 and its maximum temperature is 1750 C. The furnace was purchased in Finger Test Device The measurement method is to rotate the refractory material piece finger with a constant speed in a slag or metal and then measure the corrosion rate and analyze the infiltration. The IKA eurostar power control visc is an adjustable rotator device whose speed can be altered between r/min. The furnace is Lenton CSC 17/ 90/250 and its maximum temperature is 1700 C. The furnace was purchased in Optical Dilatometer The device indicates a materials dimension changes as a function of temperature and time in a controlled atmosphere. With the device a sessile drop contact angle and all the parameters for surface tension calculations can be determined. The tai-

30 32 lor-made programme Dakota calculates automatically the sample area and all the other parameters. Cameras The B&W Camera is an AD C660 1/3 ccd 768 x 494 pixels, the lens is a Dyotar DY135. The colour Camera is a Canon DM-MV1 digital video camera. Furnaces The SiC furnace s maximum working temperature is 1550 C. The inside diameter of the working tube is 30 mm. A sample is made from powder, then pressed into the cylinder, 4 mm in diameter and the sample plate is usually sawn into 4 mm thick 10 mm x 10 mm sq uares. NaberSupertherm HT08/18 furnace s maximum working temperature is 1750 C Gradient Furnace The device is an Entech ETF 75/17V. It is a double chamber tube furnace, whose tubes are 200 mm in height. The maximum temperature of the furnace is 1750 C. The tubes inside diameter is 200 mm or 75 mm. The purpose of the furnace is to measure material properties in a constantly controlled temperature gradient. It was purchased in Pressure Furnace The maximum pressure of the furnace is 10 bar and the temperature 1500 C. The inner pipe diameter is 90 mm. The furnace was purchased in Alkali Test The tester measures alkali effects on minerals. The inner diameter of the steel tube is 90 mm and the maximum temperature is 1150 C. It was purchased in 2000.

31 OTHERS Watermodels The models visualize phenomenon taking place inside a converter / ladle, like steel / slag flow during a blowing session and wear and tear of refractory materials. The watermodels were purchased between Coulter Omnisorp 360 cx The gas sorption analyzer measures a surface area of a sample and determinates the pore size distribution. The Omnisorp is a continuous volumetric method, used to determine the adsorption and desorption isotherms. The pore size distribution peaks can be separated in a scale as little as 2 Ångström. The pore size distribution range is from 3 to 2000 Ångströms. The surface area value down to 3m2/gm resolution is better than 2 %. The device was purchased in 1997 in co-operation with the other laboratories Computational Fluid Dynamics Software The Phoenics software is for gas and liquid flow model. The Femlab software on Matlab is for simple model tasks and the Fluent software is for more complicated models within a project Thermodynamic Calculation Programmes HSC, Chemsage, Fact Sage programmes are for thermodynamic equilibrium calculations Gas Chromatograph The device is Agilent 6890 plus a thermal conductivity detector. The carrier gas is helium. The device was purchased in 2001.

32 Microscopes An Olympus polarizing microscope BX51P and an Olympus research stereomicroscope SZX9 with DP-12 camera and DP-software. The microscopes were purchased in Materialographic Surface Preparation of Solid Materials The device is for preparing materialographic samples for microscopic examination. We use diamond cutting and cold mounting. The Struers Epovac vacuum impregnation equipment is used for mounting and impregnation of porous specimens and for gluing specimens for thin sections to glass slides. Grinding and polishing is done with a Struers LaboForce-1 at speed of 8 rpm and a LabPol-1 - single speed machine, 250 rpm with MD or SiC consumables. The ready samples go through ultrasonic cleaning before inspection and use. The device was purchased in 2002.

33 OTHER AVAILABLE FACILITIES Within the University of Oulu: Institution of Electron Optics (EOL): The EOL facilities are based on the use of seven instruments: Energy Filtered Transmission Electron Microscope EFTEM, Scanning Electron Microscope SEM, Field Emission Scanning Electron Microscope FESEM, Scanning Transmission Electron Microscope STEM, Electron Probe Microanalyzer EPMA, X-Ray Diffractometer XRD and X-Ray Fluorescence Spectrometer XRF. They provide three basic kinds of information: images, chemical analyses and crystal structures. Trace Element Laboratory: Plasma atomic emission spectrometry (DCP-AES, ICP- AES) and plasma mass spectrometry (ICP-MS). This equipment provides chemical analyses of difficult samples. At Rautaruukki Steel in Raahe: There is for example XRF, XRD, optical emission spectrometer (OES) and SEM. At AvestaPolarit in Tornio Works: There is for example XRF, OES and SEM.

34 36 5 PUBLICATIONS PAPERS Fabritius, Timo; Mure, Petri & Härkki, Jouko: Determination of the Minimum and Operational Gas Flow Rates for Sidewall Blowing in the AOD-converter. - ISIJ International, 2003, vol. 43, nro 8, pp Tang, Yong; Laine, Jarmo; Fabritius, Timo & Härkki, Jouko: Modelling of the Gas Flow and its Influence on the Scale Accumulation in the Steel Slab Pusher-type Reheating Furnace. - ISIJ International, 2003, vol. 43, nro 9, pp Heikkinen, Eetu-Pekka: Kierrätyksen asiantuntijoita koolla Luulajassa. - Vuoriteollisuus, 2003, nro 3, s Jaako, Juha & Heikkinen, Eetu-Pekka: Prosessi- ja ympäristötekniikan osasto - koulutuksen laatuyksikkö. - Vuoriteollisuus, 2003, nro 1, s. 32. Mure, Petri & Zinovjev, Berith Nuorten metallurgitutkijoiden symposiumi. - Vuoriteollisuus, 2003, nro 3, s Paananen, Timo; Heinänen, K. & Härkki, Jouko Degradation of Iron Oxide Caused by Alumina During Reduction from Magnetite. - ISIJ International, 2003, vol. 43, nro 5, pp Gornostayev, Stanislav & Mutanen, T.: Platinum-group Minerals in Chromitites of the Akanvaara Deposit, Northern Finland and in their Processing Products. - Minerals Engineering, 2003, vol. 16, nro 11, pp

35 CONFERENCES AND SYMPOSIUMS Angerman, M.; Harju, M; Sippola, J. & Pöyhtäri, S: Alternative Processes and Plant Simulation Made Easy, ISS Tech 2003 Conference, , Indianapolis, IN, USA, p. 7. Heikkinen, Eetu-Pekka; Makkonen, Hannu; Heikkinen, J. & Seppänen, M.: Computational Study of the Formation of Zn, Pb, Sn, Cd and Alkali Compounds While Recycling the Integrated Steel Work Rejects. - 2nd Nordic Iron and Steel Waste Recycling Day, , Luleå, Sweden, Mimer pp Angerman, Mikko; Harju, Markus; Pöyhtäri, Samuli & Sippola, Jukka: Flexible Simulation Tool for Process Industry. - Nordic Symposium for Young Scientists, Production Metallurgy for Iron, Steel and Ferroalloys, June 2003, Oulu, Finland pp Fabritius, Timo; Mure, Petri & Härkki, Jouko: Modelling of the AOD Bath Oscillation. - Nordic Symposium for Young Scientists, Production Metallurgy for Iron, Steel and Ferroalloys, June 2003, Oulu, Finland. Pohto pp Heikkinen, Eetu-Pekka; Kokkonen, Tommi & Mattila Riku: Chemical Wear of the Steel Ladle Slagline Due to Sequential Contact with Molten Steel and Ladle Slag. - Nordic Symposium for Young Scientists, Production Metallurgy for Iron, Steel and Ferroalloys, June 2003, Oulu, Finland pp Tang, Yong; Fabritius, Timo & Härkki, Jouko: Air Entrapment and Gas Escape Caused by the Unsteady Suction Ability in the Ventilation Hood of AOD at the Reduction Stage. - Nordic Symposium for Young Scientists, Production Metallurgy for Iron, Steel and Ferroalloys, June 2003, Oulu, Finland pp. 16. Angerman, M.; Harju, M.; Pöyhtäri, S. & Sippola, J.: User-Friendly Tool for Simulating Alternative Production Routes in Iron and Steelmaking, Metec Congress 03 3rd ICSTI Conference, , Düsseldorf, Saksa, pp. 5.

36 38 Tang, Yong; Fabritius, Timo & Härkki, Jouko Investigation of Air Entrapment into an Argon Oxygen Decarburization Converter at the Reduction Stage. - Csiro, 3rd International Conference on CFD. Melbourne, Australia pp REPORTS Gornostayev, Stanislav: Mineralogical Research on Chromitites of the Akanvaara Deposit and Products of their Processing with Emphasis on PGM/PGE. - University of Oulu, Department of Process and Environmental Engineering. Report nro p. Ikäheimonen, Topi; Heikkinen, Eetu-Pekka & Fabritius, Timo Typen liukoisuus sulaan ruostumattomaan teräkseen. Termodynaaminen tarkastelu. - University of Oulu, Department of Process and Environmental Engineering. Report nro 290. Oulu, s. Heino, Jyrki Harjavalta ja Outokummun kuparitehdas vuosina Lähimenneisyyden metallurgis- ja ympäristöhistoriallinen katsaus. - University of Oulu, Department of Process and Environmental Engineering. Report nro 291. Oulu, s. Aho, Jani; Leinonen, Virpi; Kyllönen, Toni; Fabritius, Timo & Härkki, Jouko Kirjallisuusselvitys typen absorptiota ja desorptiosta. - University of Oulu, Department of Process and Environmental Engineering. Report nro 292. Oulu, s. Tang, Yong; Fabritius, Timo & Härkki, Jouko Modelling of Air Entrapment into the AOD by FLUENT University of Oulu, Department of Process and Environmental Engineering. Report nro 293. Oulu, p. Heikkinen, Eetu-Pekka; Makkonen, Hannu; Heikkinen, J. & Seppänen, M. Terästuotannossa muodostuvien hienorakeisten poisteiden sisältämien haitta-aineiden vaikutus materiaalien kierrätettävyyteen. Termodynaaminen tarkastelu. - University of Oulu, Department of Process and Environmental Engineering. Report nro 294. Oulu, s.

37 39 Virtanen, Esa; Fabritius, Timo & Härkki, Jouko Terässulan lämmönnousu AOD:ssä korkeilla Si-pitoisuuksilla. - University of Oulu, Department of Process and Environmental Engineering. Report nro 300. Oulu, Oulun yliopisto s. Tang, Yong; Fabritius, Timo & Härkki, Jouko Bottom Gas Injection into the AOD Bath at the Reduction Stage. - University of Oulu, Department of Process and Environmental Engineering. Report nro 301. Oulu, p. Lin, R.; Jahnsen, U.; Widner, S.; Bürgler,T.; Lectard, É.; Sert, D.; Mannila, P.; Heinänen, K.; et al.;tanskanen, Pekka; Huttunen, Satu; Kallio, Sauli & Härkki, Jouko Investigations of Chlorine and Alkali Behaviour in the Blast Furnace and Optimisation of Blast Furnace Slag with Respect to Alkali Retention Capacity. - Technical Steel Research. Report nro EUR Belgium, European commission p. 5.4 ANNUALS AND FINAL REPORTS Petäjäjärvi, Marko (editor) University of Oulu. Laboratory of Process Metallurgy, Department of Process and Environmental Engineering, Annual Report 2002, Oulu 2003, University of Oulu. 51 p.

38 40 6 THESIS 6.1 LICENCIATE IN TECHNOLOGY THESES Erkkilä Helena Modelling of Non-metallic Inclusion Composition of Steel by Thermodynamic Equilibrium Calculations and a Solidification Model 6.2 DIPLOMA ENGINEER THESES (MASTER OF SCIENCE IN TECHNOLOGY) Hannula, Petri Surface Quality of Copper and Copper Alloy Slabs Isokääntä, Jani Optimizing the Heat Treatment and Improving the Mechanical Properties of a High Strength Ductile Iron Kaijalainen, Antti Optimizing of Aluminium, Calcium and Boron alloys with Stainless Steel Karjalainen, Eveliina Production of Low-carbon Aluminium Killed Strip Steel with Low Inclusion Content Leinonen, Mervi The Modelling and Optimization of Desulphurization of Hot Metal Luoto, Pasi Hot Strip Rolling Simulation by Crown426 Simulation

39 41 Mure, Petri The Effect of Sidewall Blowing on Melt Flows, Mixing and Oscillation of Melt Bath in a 150 ton AOD-Converter Mäenpää, Jani Preparation and Uses of Nickel and Cobalt Salts and the Manufacturing from them of Metallic Powders Petäjäjärvi, Marko Increase of Casting Speed with Peritectic Steel Grades at Rautaruukki Steel s Curved Continuous Casting Machines Suikkanen, Pasi Effect of Sinter Mix Segregation to Properties of Sinter as a Function of Bed Height Tikka, Janne Effects of Oxygen Lance Height and Nozzle Wear on the Dynamic Pressure at the Molten Metal Surface in the Boff Process Virtanen, Esa Top Lance Practice in CRK and AOD-Converter

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