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Authors = Semiramis Friedrich ORCID = 0000-0002-4078-0799

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19 pages, 7635 KiB  
Article
Hydrogen Reduction of Tellurium Oxide in a Rotary Kiln, Initial Approaches for a Sustainable Process
by Hanwen Chung, Semiramis Friedrich, Mengqi Qu and Bernd Friedrich
Crystals 2025, 15(5), 478; https://doi.org/10.3390/cryst15050478 - 18 May 2025
Viewed by 541
Abstract
In the recycling of semiconductor materials like Bi2Te3 or CdTe, TeO2 may form as a by-product that can be directly reduced to recover metallic Te. The hydrogen reduction of TeO2 offers an eco-friendly alternative to conventional carbothermic reduction [...] Read more.
In the recycling of semiconductor materials like Bi2Te3 or CdTe, TeO2 may form as a by-product that can be directly reduced to recover metallic Te. The hydrogen reduction of TeO2 offers an eco-friendly alternative to conventional carbothermic reduction by avoiding CO by-products. This study investigates the reduction of 99.99 wt.% purity level TeO2 using hydrogen in an oscillating kiln furnace (200–800 °C, 2–7 h), with phase composition and microstructure analysed via XRD and SEM. Results demonstrate conversions of up to 89% (solid–gas) and 100% (liquid–gas), revealing that kinetics dominate over thermodynamics in controlling reaction progress. The work proposes a reaction mechanism based on morphological evolution observed in SEM images, suggesting that further parameter optimisation could enhance scalability. As the first lab-scale demonstration of hydrogen-assisted TeO2 reduction, this study establishes a preliminary process window (temperature/time) and underscores the potential for industrial adoption. Future work should verify the proposed mechanism and refine operational parameters to maximize efficiency. Full article
(This article belongs to the Special Issue II-VI and III-V Semiconductors for Optoelectronic Devices)
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11 pages, 2731 KiB  
Article
Static Crystallization, an Alternative Methodology for Synthesis of High-Purity Aluminum
by Michaela Gotenbruck, Danilo C. Curtolo, Semiramis Friedrich, Clemens J. Müller, Nico Rademacher and Bernd Friedrich
Metals 2023, 13(2), 280; https://doi.org/10.3390/met13020280 - 31 Jan 2023
Cited by 1 | Viewed by 2592
Abstract
Due to its outstanding properties and wide range of applications, high-purity to ultra-high-purity aluminum represents a strategic material for meeting the future challenges of the 21st century. The purification of aluminum towards higher purity levels is usually performed via a combination of three-layer [...] Read more.
Due to its outstanding properties and wide range of applications, high-purity to ultra-high-purity aluminum represents a strategic material for meeting the future challenges of the 21st century. The purification of aluminum towards higher purity levels is usually performed via a combination of three-layer electrolytic refining and fractional crystallization using zone-melting processes. New methods and processes are being researched in the search for more time-saving and less costly options. Metal refining using static crystallization represents one of these new, alternative processes. This work investigated the feasibility of metal refining by means of a static crystallization furnace using aluminum as an example metal. In particular, the effects of the temperature gradient and the cooling rate on the reduction factor of the impurities iron (Fe), silicon (Si), and lead (Pb) were investigated. In addition, the effects of the process parameters on the grain structure formed were investigated, and correlations to the resulting purity level were made. Full article
(This article belongs to the Special Issue Separation and Purification of Metals)
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17 pages, 3763 KiB  
Article
The Effectiveness of Cooled-Finger and Vacuum Distillation Processes in View of the Removal of Fe, Si and Zn from Aluminium
by Michaela Gotenbruck, Danilo C. Curtolo, Semiramis Friedrich and Bernd Friedrich
Metals 2022, 12(12), 2027; https://doi.org/10.3390/met12122027 - 25 Nov 2022
Cited by 6 | Viewed by 3358
Abstract
The increasing demand for ultra-high purity aluminum for technological applications has led to the improvement of refining methods in recent decades. To achieve ultra-purity levels (>5N), the common industrial way is to firstly purify aluminum from 2N8 up to 4N8 via three-layer electrolysis, [...] Read more.
The increasing demand for ultra-high purity aluminum for technological applications has led to the improvement of refining methods in recent decades. To achieve ultra-purity levels (>5N), the common industrial way is to firstly purify aluminum from 2N8 up to 4N8 via three-layer electrolysis, followed by fractional crystallization (usually zone melting). Since both of these methods are very cost- and time-intensive, this paper aims at providing other alternatives of purification. For this purpose, here, the purification of some selected impurities through cooled-finger fractional crystallization method and vacuum distillation have been the focus of this investigation. Both processes are more environmentally friendly than three-layer electrolysis and require less time than zone melting. In this paper, both methods were explored for the aluminum purification. Moreover, the effect of process parameters on the purification efficiency of iron, zinc, and silicon has been investigated. At the end, the effectiveness of the two processes was compared and advantages and disadvantages were summarized. The results showed that the cooling finger process effectively removed iron and silicon impurities, but the removal efficiency of zinc was low. The vacuum distillation process successfully removes zinc in the first stage of distillation. Iron and silicon removal requires additional distillation stages to achieve lower impurity levels. Full article
(This article belongs to the Special Issue Separation and Purification of Metals)
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22 pages, 5262 KiB  
Review
High- and Ultra-High-Purity Aluminum, a Review on Technical Production Methodologies
by Danilo C. Curtolo, Neng Xiong, Semiramis Friedrich and Bernd Friedrich
Metals 2021, 11(9), 1407; https://doi.org/10.3390/met11091407 - 6 Sep 2021
Cited by 41 | Viewed by 14859
Abstract
Aluminum and aluminum-based alloys have been used for many years. In view of the increase in material purity requirements of advanced technology products, research regarding high-purity aluminum has gained significant attention in recent years. In this review, we seek to describe the fundamental [...] Read more.
Aluminum and aluminum-based alloys have been used for many years. In view of the increase in material purity requirements of advanced technology products, research regarding high-purity aluminum has gained significant attention in recent years. In this review, we seek to describe the fundamental purification principles and the mechanisms of various segregation techniques used to produce high-purity aluminum. Moreover, we aim to provide an overview of high-purity aluminum production, with particular emphasis on: (a) principles on how to produce high-purity aluminum by layer- and suspension-based segregation methods; (b) discussion of various influencing process parameters for each technique, including three-layer electrolysis, vacuum distillation, organic electrolysis, suspension-based segregation, zone melting, Pechiney, Cooled Finger, and directional solidification; as well as (c) investigations of fundamental working principles of various segregation methods and corresponding reported end-purification for the production of HP-Al. Eventually, the end-reported product purity, and advantages and disadvantages of various purification methods and technologies are summarized. By analyzing and comparing the characteristics of different methods, we put forward suggestions for realizing efficient and environmentally friendly production of high-purity aluminum in the future. Full article
(This article belongs to the Section Extractive Metallurgy)
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11 pages, 1714 KiB  
Article
The Influence of Initial Purity Level on the Refining Efficiency of Aluminum via Zone Refining
by Xiaoxin Zhang, Semiramis Friedrich and Bernd Friedrich
Metals 2021, 11(2), 201; https://doi.org/10.3390/met11020201 - 22 Jan 2021
Cited by 2 | Viewed by 2614
Abstract
Zone refining is a well-known technique, usually using pure initial materials to produce high purity metals. However, the effectiveness of zone refining in the purification of different purity levels of metals as well as its feasibility for use as a recycling technique for [...] Read more.
Zone refining is a well-known technique, usually using pure initial materials to produce high purity metals. However, the effectiveness of zone refining in the purification of different purity levels of metals as well as its feasibility for use as a recycling technique for low quality metals are rarely investigated. In this work, conducted at IME/RWTH Aachen University, three kinds of Al with different purities, i.e., three-layer electrolysis (4N), commercial pure (2N8) and recycled Al (1N7), were put on focus to address the above-mentioned issue. The experiments were conducted with an optimized zone length combination at the moving rate of 1.2 mm/min for five zone passes. The results showed that the 4N pure initial Al was improved to 5N5 after five passes, much higher than the results for commercial pure- or recycled Al, where less than 50% reduction of total impurities was achieved. Full article
(This article belongs to the Special Issue 10th Anniversary of Metals: Metallurgy and Metal Technology)
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15 pages, 18014 KiB  
Article
Numerical and Experimental Investigation of Germanium Refining via Fractional Crystallization Based Innovative Rotary Cooling Device
by Danilo C. Curtolo, Semiramis Friedrich, Michael Noack and Bernd Friedrich
Metals 2020, 10(7), 973; https://doi.org/10.3390/met10070973 - 18 Jul 2020
Cited by 4 | Viewed by 4206
Abstract
This paper focuses on the principle study and application of a fractional crystallization methodology using a rotating and internally gas cooled crystallizer (so called cooled finger, developed at IME/RWTH Aachen) first applied to the refining of germanium. For this purpose, a series of [...] Read more.
This paper focuses on the principle study and application of a fractional crystallization methodology using a rotating and internally gas cooled crystallizer (so called cooled finger, developed at IME/RWTH Aachen) first applied to the refining of germanium. For this purpose, a series of experimental trials were performed using a model metal—Aluminum—to gather the temperature profile needed for the numerical simulation that provides an initial process window used for the purification of germanium in a vacuum resistance furnace. The results of the simulation showed good agreement with the experimental results and the conducted trials based on that process window enabled the single step purification of germanium from an initial purity of 98.8% up to 99.9%. Full article
(This article belongs to the Special Issue 10th Anniversary of Metals: Metallurgy and Metal Technology)
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12 pages, 1620 KiB  
Review
Refining Principles and Technical Methodologies to Produce Ultra-Pure Magnesium for High-Tech Applications
by Seifeldin R. Mohamed, Semiramis Friedrich and Bernd Friedrich
Metals 2019, 9(1), 85; https://doi.org/10.3390/met9010085 - 15 Jan 2019
Cited by 32 | Viewed by 6320
Abstract
During the last decade, magnesium-based medical implants have become the focal point of a large number of scientific studies due to their perceived favorable properties. Implants manufactured from magnesium alloys are not only biocompatible and biodegradable, but they are also the answer to [...] Read more.
During the last decade, magnesium-based medical implants have become the focal point of a large number of scientific studies due to their perceived favorable properties. Implants manufactured from magnesium alloys are not only biocompatible and biodegradable, but they are also the answer to problems associated with other materials like stress shielding (Ti alloys) and low mechanical stability (polymers). Magnesium has also been a metal of interest in another field. By offering superior technical and economic features in comparison to lithium, it has received significant attention in recent years as a potential battery anode alternative. Natural abundancy, low cost, environmental friendliness, large volumetric capacity, and enhanced operational safety are among the reasons that magnesium anodes are the next breakthrough in battery development. Unfortunately, commercial production of such implants and primary and secondary cells has been hindered due to magnesium’s low corrosion resistance. Corrosion investigations have shown that this inferior quality is a direct result of the presence of certain impurities in metallic magnesium such as iron, copper, cobalt, and nickel, even at the lowest levels of concentration. Magnesium’s sensitivity to corrosion is an obstacle for its usage not only in biomedical implants and batteries, but also in the automotive/aerospace industries. Therefore, investigations focusing on magnesium refinement with the goal of producing high and ultra-high purity magnesium suitable for such demanding applications are imperative. In this paper, vacuum distillation fundamentals and techniques are thoroughly reviewed as the main refining principles for magnesium. Full article
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12 pages, 8255 KiB  
Article
Characterization and Interpretation of the Aluminum Zone Refining through Infrared Thermographic Analysis
by Xiaoxin Zhang, Semiramis Friedrich and Bernd Friedrich
Materials 2018, 11(10), 2039; https://doi.org/10.3390/ma11102039 - 19 Oct 2018
Cited by 5 | Viewed by 3808
Abstract
High purity metals are nowadays increasingly in demand to serve in electronic, photovoltaic, and target materials industries. The zone refining process is the most common way to achieve high purity in the final step of metal purification. Zone length and crystal growth rate [...] Read more.
High purity metals are nowadays increasingly in demand to serve in electronic, photovoltaic, and target materials industries. The zone refining process is the most common way to achieve high purity in the final step of metal purification. Zone length and crystal growth rate are the main parameters that control the zone refining process. To determine these values, information about temperature profiles in the molten zone is necessary due to its direct correlation with these values. As the determination of this profile is not practically achievable in the present, the novel approach of applying an infrared (IR) camera during the zone refining of 2N8 aluminum is the focus of the investigation in this work. The whole temperature profile of the region near the molten zone was recorded by IR camera during the entire running process. The zone length and the crystal growth rate at each thermographic image shooting moment were successfully extracted by thermographic analysis. Results showed that both factors varied significantly, which is in contrast to the assumption in literature about their stability while running under constant input power and heater movement velocity, though noticeable purification took place in all of these experiments. However, the impurity concentration during refinement fluctuated remarkably. This was well-demonstrated by the tendency of variation in crystal growth rate attained in this work. These results provide a better understanding of the mechanisms of zone refining with an inductive heater and contributes to the optimization of the process. Full article
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13 pages, 6638 KiB  
Article
Realization of the Zone Length Measurement during Zone Refining Process via Implementation of an Infrared Camera
by Danilo C. Curtolo, Xiaoxin Zhang, Martin J. R. Rojas, Semiramis Friedrich and Bernd Friedrich
Appl. Sci. 2018, 8(6), 875; https://doi.org/10.3390/app8060875 - 25 May 2018
Cited by 9 | Viewed by 8231
Abstract
Zone refining, as the currently most common industrial process to attain ultrapure metals, is influenced by a variety of factors. One of these parameters, the so-called “zone length”, affects not only the ultimate concentration distribution of impurities, but also the rate at which [...] Read more.
Zone refining, as the currently most common industrial process to attain ultrapure metals, is influenced by a variety of factors. One of these parameters, the so-called “zone length”, affects not only the ultimate concentration distribution of impurities, but also the rate at which this distribution is approached. This important parameter has however neither been investigated experimentally, nor ever varied for the purpose of optimization. This lack of detections may be due to the difficult temperature measurement of a moving molten area in a vacuum system, of which the zone refining methodology is comprised. Up to now, numerical simulation as a combination of complex mathematical calculations, as well as many assumptions has been the only way to reveal it. This paper aims to propose an experimental method to accurately measure the molten zone length and to extract helpful information on the thermal gradient, temperature profile and real growth rate in the zone refining of an exemplary metal, in this case aluminum. This thermographic method is based on the measurement of the molten surface temperature via an infrared camera, as well as further data analysis through the mathematical software MATLAB. The obtained results show great correlation with the visual observations of zone length and provide helpful information to determine the thermal gradient and real growth rate during the whole process. The investigations in this paper approved the application of an infrared camera for this purpose as a promising technique to automatically control the zone length during a zone refining process. Full article
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12 pages, 3337 KiB  
Article
Definition of a First Process Window for Purification of Aluminum via “Cooled Finger” Crystallization Technique
by Danilo C. Curtolo, Semiramis Friedrich, Dominic Bellin, Gargi S. Nayak and Bernd Friedrich
Metals 2017, 7(9), 341; https://doi.org/10.3390/met7090341 - 1 Sep 2017
Cited by 24 | Viewed by 6619
Abstract
Aluminum ultra-purification is commonly realized through a combination of three-layer electrolytic refining and fractional crystallization, mostly using zone melting. In order to achieve a purity over 6N with the aid of zone melting, many passes have to be performed, taking several days to [...] Read more.
Aluminum ultra-purification is commonly realized through a combination of three-layer electrolytic refining and fractional crystallization, mostly using zone melting. In order to achieve a purity over 6N with the aid of zone melting, many passes have to be performed, taking several days to be accomplished. This paper focuses on a fractional crystallization methodology using a rotating and internally gas cooled crystallizer (“cooled finger”), based on a Japanese patent from the 1980s, about which no scientific investigation or publication has yet been found. This paper focuses on the impact of process conditions (mainly cooling gas flow and rotation velocity) on the growth rate of the crystallized material as well as on the reduction factor of the impurities Fe, Si, Pb, and Zn in aluminum in relationship to their initial concentration and their interaction in a multi-component system. This technique can be considered as a promising alternative for purification of aluminum as well as other metallic systems. Full article
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