Artykuł przedstawia przegląd rozwoju strategii i metod używanych w badaniach na temat stopów o wysokiej entropii. Jest to nowa grupa materiałów, która może być scharakteryzowana poprzez nowoczesne podejście do kompozycji stopowych. Podczas, gdy w tradycyjnych stopach można wyróżnić jeden lub dwa podstawowe elementy, których stężenie jest bardzo wysokie w stosunku do innych pierwiastków stopowych, w stopach o wysokiej entropii pięć lub więcej pierwiastków stopowych dodaje się w równych lub prawie równych proporcjach. Od dawna uważano, że ten rodzaj kompozycji doprowadzi do kruchej konglomeracji związków międzymetalicznych, ale stwierdzono, że wysoka entropia losowych stałych roztworów może je uprzywilejowywać względem innych uporządkowanych, fazowych lub międzymetalicznych związków, prowadząc do prostej jednofazowej struktury. To odkrycie stworzyło nowe, ogromne możliwości projektowania nowych materiałów, ale także konieczność przyjrzenia się istniejącym metodologiom rozwoju stopów.
EN
Paper presents a review of development strategies and methods used in research on high entropy alloys. This is a new group of materials which can be characterised by novel approach to alloy composition. Whereas in traditional alloys we can distinguish one or two base elements whose concentration is very high in relation to other alloying elements, in high entropy alloys five or more alloying elements are added in equal or near equal proportions. It has been long thought that this type of composition will lead to brittle conglomeration of intermetallics, but it was found that high entropy of random solid solutions can preferentiate them over other, ordered, phases or intermetallic compounds leading to simple single phase structure. This discovery created new and vast possibilities for designing new materials, but also necessitated revision of existing methodologies for alloy development.
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The paper presents an attempt to estimate the difference in the intensity of the curing process of a polyester resin: without any filler and filled with fragmented glass fabric. Curing of the resin samples was carried out at room temperature. The temperature-time course of the process and gel time were recorded for each sample. On the basis of the obtained results and the conducted observations, it was found that filling the resin with fragmented glass fabric caused a decrease in the peak temperature of the curing process and increased the time of reaching this temperature. These effects were found to intensify with an increase in filler weight (inhibitory effect of the filler). A slightly longer gelation time was also found for the filled resin in comparison to the unfilled one. The observed effects indicate an increase in the thermal insulation of the curing mass along with an increase in filler content. They also indicate that the presence of fibers leads to stabilization (improvement of repeatability) of the resin curing process. The work is a continuation of earlier work aimed at experimental evaluation of the behavior of curing resins, which in turn will help to systematize the practical knowledge in this field. Thus, it finally meets the expectations of users and processors of curable resins.
PL
Zaprezentowano próbę oszacowanie różnicy w intensywności procesu sieciowania żywicy poliestrowej bez żadnego napełniacza oraz napełnionej rozdrobnioną tkaniną szklaną. Utwardzanie próbek żywicy prowadzono w temperaturze pokojowej i rejestrowano przebieg temperaturowo-czasowy procesu oraz czas żelowania. Na podstawie uzyskanych wyników i poczynionych obserwacji stwierdzono, że napełnienie żywicy rozdrobnioną tkaniną szklaną spowodowało zmniejszenie temperatury szczytu procesu utwardzania oraz wydłużyło czas osiągania tej temperatury. Stwierdzono postępowanie tych efektów ze zwiększeniem masy napełniacza (inhibicyjne działanie napełniacza). Dla żywicy napełnionej stwierdzono też nieznaczne wydłużenie czasu żelowania. Zaobserwowane efekty wskazują na zwiększenie izolacyjności termicznej sieciującej masy wraz ze wzrostem zawartości napełniacza. Wskazują też, że obecność włókien prowadzi do stabilizacji (poprawy powtarzalności) procesu sieciowania żywicy. Praca jest kontynuacją wcześniejszych prac, mających na celu eksperymentalną ocenę zachowania się utwardzanej żywicy, co z kolei pomoże usystematyzować praktyczną wiedzę w tym zakresie i wyjść naprzeciw oczekiwaniom użytkowników oraz przetwórców żywic utwardzalnych.
Paper presents the results of ATD and DSC analysis of two superalloys used in casting of aircraft engine parts. The main aim of the research was to obtain the solidification parameters, especially Tsol and Tliq, knowledge of which is important for proper selection of casting and heat treatment parameters. Assessment of the metallurgical quality (presence of impurities) of the feed ingots is also a very important step in production of castings. It was found that some of the feed ingots delivered by the superalloy producers are contaminated by oxides located in shrinkage defects. The ATD analysis allows for quite precise interpretation of first stages of solidification at which solid phases with low values of latent heat of solidification are formed from the liquid. Using DSC analysis it is possible to measure precisely the heat values accompanying the phase changes during cooling and heating which, with knowledge of phase composition, permits to calculate the enthalpy of formation of specific phases like γ or γ′.
Paper presents the results of research on modified surface grain refinement method used in investment casting of hollow, thin-walled parts made of nickel based superalloys. In the current technology, the refining inoculant is applied to the surface of the wax pattern and then, it is transferred to the ceramic mould surface during dewaxing. Because of its chemical activity the inoculant may react with the liquid metal which can cause defects on the external surface of the cast part. The method proposed in the paper aims to reduce the risk of external surface defects by applying the grain refiner only to the ceramic core which shapes the internal surface of the hollow casting. In case of thin-walled parts the grain refinement effect is visible throughout the thickness of the walls. The method is meant to be used when internal surface finish is less important, like for example, aircraft engine turbine blades, where the hollowing of the cast is mainly used to lower the weight and aid in cooling during operation.
The paper presents the results of analysis of creep behaviour in short term creep tests of cast MAR-247 nickel-based superalloy samples made using various modification techniques and heat treatment. The accelerated creep tests were performed under temperature of 982 °C and the axial stresses of σ = 150 MPa (variant I) and 200 MPa (variant II). The creep behaviour was analysed based on: creep durability (creep rupture life), steady-state creep rate and morphological parameters of macro- and microstructure. It was observed that the grain size determines the creep durability in case of test conditions used in variant I, durability of coarse-grained samples was significantly higher.
The paper presents the results concerning impact of modification (volume and surface techniques), pouring temperature and mould temperature on stereological parameters of macrostructure in IN713C castings made using post-production scrap. The ability to adjust the grain size is one of the main issues in the manufacturing of different nickel superalloy castings used in aircraft engines. By increasing the grain size one can increase the mechanical properties, like diffusion creep resistance, in higher temperatures. The fine grained castings. on the other hand, have higher mechanical properties in lower temperatures and higher resistance to thermal fatigue. The test moulds used in this study, supplied by Pratt and Whitney Rzeszow, are ordinarily used to cast the samples for tensile stress testing. Volume modification was carried out using the patented filter containing cobalt aluminate. The macrostructure was described using the number of grains per mm2, mean grain surface area and shape index. Obtained results show strong relationship between the modification technique, pouring temperature and grain size. There was no significant impact of mould temperature on macrostructure.
The paper presents the results of research on the determination of the effect of pouring temperature on the macrostructure of the castings subjected to complex (surface and volume) modification and double filtration. Tested castings were made of post-production scrap (gating system parts) of IN-713C superalloy. Tests included the evaluation of the number of grains per 1 mm2, mean grain surface area, shape factor and tensile strength. Casting temperature below 1470 °C positively influenced the modification effect. The grains were finer and the mechanical properties increased, especially for castings with thicker walls. On the other hand, manufacture of thin walled castings of high quality require pouring temperature above 1480 °C.
In current casting technology of cored, thin walled castings, the modifying coating is applied on the surface of wax pattern and, after the removal of the wax, is transferred to inner mould surface. This way the modification leading to grain refinement occur on the surface of the casting. In thin walled castings the modification effect can also be seen on the other (external) side of the casting. Proper reproduction of details in thin walled castings require high pouring temperature which intensify the chemical reactions on the mould – molten metal interface. This may lead to degradation of the surface of the castings. The core modification process is thought to circumvent this problem. The modifying coating is applied to the surface of the core. The degradation of internal surface of the casting is less relevant. The most important factor in this technology is “trough” modification – obtaining fine grained structure on the surface opposite to the surface reproduced by the core.
Paper presents the assessment of impact of heat treatment on durability in low-cycle fatigue conditions (under constant load) in castings made using post-production scrap of MAR-247 and IN-713C superalloys. Castings were obtained using modification and filtration methods. Additionally, casting made of MAR-247 were subjected to heat treatment consisting of solution treatment and subsequent aging. During low-cycle fatigue test the cyclic creep process were observed. It was demonstrated that the fine-grained samples have significantly higher durability in test conditions and , at the same time, lower values of plastic deformation to rupture Δ□pl. It has been also proven that durability of fine-grained MAR-247 samples can be further raised by about 60% using aforementioned heat treatment.
The study assesses the impact of surface and bulk modification and filtration during pouring on a durability under accelerated creep conditions of casts made of IN-713C and MAR-247 nickel superalloys scrap used for manufacturing of aircraft engine parts. The impact of solutionizing (1185°C/2 h) with subsequent ageing (870°C/20 h) on the creep resistance of a casting made from MAR-247 coarse-grained superalloy was also examined. Morphological structure parameters were determined with the use of Met-Ilo software. Macrostructure analysis of casts showed very significant impact of surface modification treatment. Creep test results clearly showed that coarse grained samples of IN-713C and MAR-247 superalloys have higher creep resistance. Moreover alloy MAR-247 had higher creep durability after heat treatment compared to as-cast state.
PL
W pracy przeprowadzono ocenę wpływu zabiegów modyfikacji powierzchniowej i objętościowej oraz filtracji podczas zalewania form na trwałość w warunkach przyspieszonego pełzania odlewów wykonanych z odpadów poprodukcyjnych nadstopów niklu IN-713C i MAR-247 stosowanych na łopatki turbin silników lotniczych. Analizie poddano również wpływ operacji przesycania (1185°C/20 h) z następnym starzeniem (870°C/20 h) na trwałość pełzaniowa odlewu wytworzonego z stopu MAR-247 o strukturze gruboziarnistej. Badania makrostruktury wykonanych odlewów wykazały bardzo istotny wpływ zabiegu modyfikowania powierzchniowego. Stosując program Met-Ilo określono istotne z punktu widzenia trwałości parametry morfologiczne struktury. Próby pełzania wskazuje, że nadstopy IN-713C i MAR-247 charakteryzujace się wiekszym makroziarnem wykazywały dłuższy czas do zerwania próbki. Ponadto próbki stopu MAR-247 poddane obróbce cieplnej wykazują większą odporność na pełzanie niż próbki w stanie lanym.
Paper presents the results of evaluation of heat resistance and specific heat capacity of MAR-M-200, MAR-M-247 and Rene 80 nickel superalloys. Heat resistance was evaluated using cyclic method. Every cycle included heating in 1100°C for 23 hours and cooling for 1hour in air. Microstructure of the scale was observed using electron microscope. Specific heat capacity was measured using DSC calorimeter. It was found that under conditions of cyclically changing temperature alloy MAR-M-247 exhibits highest heat resistance. Formed oxide scale is heterophasic mixture of alloying elements, under which an internal oxidation zone was present. MAR-M-200 alloy has higher specific heat capacity compared to MAR-M-247. For tested alloys in the temperature range from 550°C to 800°C precipitation processes (γ′, γ′′) are probably occurring, resulting in a sudden increase in the observed heat capacity.
This paper presents the results of measurements of liquid metal fluidity and linear shrinkage of nickel alloy IN-713C in vacuum induction melting furnace Balzers VSG-2. Because of limited volume of the furnace chamber special models for technological trials were fluidity of hypoeutectic silumin, however in case of nickel superalloy the mould cavity was completely filled in each test because of high required pouring temperature. Positive results were obtained from the modified spiral test for all alloys used in the research. Relationship between the linear shrinkage for the test rod and a specific indicator of contraction defined on a spiral was observed.
The paper presents the results of research on the impact of impurities in the feed ingots (master heat) on the precipitation of impurities in the ATD thermal analysis probe castings. This impurities occur mostly inside shrinkage cavities and in interdendritic space. Additionally, insufficient filtration of liquid alloy during pouring promotes the transfer of impurities into the casting. The technology of melting superalloys in vacuum furnace prevents the removal of slag from the surface of molten metal. Because of that, the effective method of quality assessment of feed ingots in order to evaluate the existence of impurities is needed. The effectiveness of ATD analysis in evaluation of purity of feed ingots was researched. In addition the similarities of non-metallic inclusions in feed ingots and in castings were observed.
The paper presents a research results concerning impact of volume modification (ceramic filter containning cobalt aluminate and hafnium powder) and simultaneous surface and volume modification on solidification and stereological parameters of macrostructure of castings made from post-production scrap of nickel superalloy IN-713C. Research included investigation of the influence of chemical composition on the temperature Tliq i Tsol and evaluation of following macrostructure parameters: the number of grains per mm2, average grain area and shape coefficient. Results indicate high influence of carbon content on Tliq. Macrostructure of sample castings indicate positive effect of surface and volume modification, however impact of surface modification is more pronounced.
The paper presents the results of studies to determine the effect of complex surface and bulk modification and double filtration during mould pouring on the stereological parameters of macrostructure and mechanical properties of castings made from the post-production waste IN-713C and the MAR-247 nickel alloys. The evaluation covered the number of grains per 1mm2 of the sample surface area, the average area of grains and the shape index, hardness HB, tensile strength and resistance to high temperature creep. The results indicate the possibility of controlling the stereological parameters of macrostructure through application of several variants of the modification, controlling in this way also different low- and high-temperature properties. The positive effect of double filtration of the alloy during mould pouring on the metallurgical quality and mechanical properties of castings has also been emphasized.
The paper presents the results of evaluation of the metallurgical quality of master heat ingots and of the identification of non-metallic inclusions (oxides of Al., Zr, Hf, Cr, etc.), which have been found in the shrinkage cavities formed in these ingots. The inclusions penetrate into the liquid alloy, and on pouring of mould are transferred to the casting, especially when the filtering system is not sufficiently effective. The specific nature of the melting process of nickel and cobalt alloys, carried out in vacuum induction furnaces, excludes the possibility of alloy refining and slag removal from the melt surface. Therefore, to improve the quality of castings (parts of aircraft engines), it is so important to evaluate the quality of ingots before charging them into the crucible of an induction furnace. It has been proved that one of the methods for rapid quality evaluation is an ATD analysis of the sample solidification process, where samples are taken from different areas of the master heat ingot. The evaluation is based on a set of parameters plotted on the graph of the dT/dt derivative curve during the last stage of the solidification process in a range from TEut to Tsol.
W artykule przedstawiono wyniki badań wpływu parametrów odlewania i intensywności stygnięcia na wybrane cechy morfologiczne mikrostruktury odlewu ze stopu AlSi10Mg. Ocenie poddano podstawowe parametry morfologiczne oraz granicę plastyczności R0,2. Wyniki rzeczywiste porównano z rezultatem symulacji komputerowej. Do symulacji krzepnięcia odlewu, w masie formierskiej o zróżnicowanej osnowie, wykorzystano nowo opracowany moduł programu MAGMASoft o nazwie MAGMAnon-ferrous, udostępniony do testów Instytutowi Odlewnictwa w Krakowie.
EN
The paper presents results of studies into influence of casting conditions and intensity of cooling down on selected morphological features of microstructure of AlSi10Mg alloy cast. Basic morphological parameters as well as yield point R0,2 were evaluated. The actual results were compared to the results of computer simulation. For simulation of solidification of the cast in moulding sand of diversified matrix a new module of MAGMASoft program, called MAGMAnon-ferrous, was used. In the result of segregation and diffusion on crystallization front, properties related to the local changes in composition of the alloy become modified. The program performs real-time analysis of those phenomena and corrects the data according to the current situation in a specific part of the cast and according to the thermophysical parameters of the alloy.
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The paper presents the results of studies on the effect of combined surface and bulk modifications on the macrostructure of castings made from remelted, post-production IN-713C, IN-100 and MAR-247 waste alloys. Surface modification was carried out by applying onto the wax pattern surface, a coating containing zirconium silicate and cobalt aluminate. Bulk modification was carried out when the cast liquid alloy was passed through a special ceramic filter containing, among others, cobalt aluminate. The nanoparticles of cobalt, acting as crystallisation nuclei, are the product of a modifier reaction (CoAl2O4 inoculant) with the chemically active constituents of the nickel alloys and with the additional filter components in the form of Al and Ti powders. The filters were placed in the mould pouring basin. The beneficial effect of combined modification on the macrostructure (equiaxial crystals) and mechanical properties was stated. The effect of the active constituents present in the nickel alloys and in the filter material was confirmed. A particularly strong refining effect on the macrostructure of equiaxial crystals was obtained in the MAR-247 alloy, which contained the strongest chemically active additives of Hf, Ta and Nb. A hypothetical model of the surface and bulk modification was developed. A strong influence of the alloy pouring temperature on the modification effect was reported. Modification was most effective when the pouring temperature did not exceed 1440°C.
PL
Zamieszczono wyniki badań wpływu łącznego modyfikowania powierzchniowego i objętościowego na makrostrukturę odlewów wykonanych po przetopie odpadów poprodukcyjnych ze stopów IN-713C, IN-100 i MAR-247. Modyfikację powierzchniową zrealizowano poprzez naniesienie na model woskowy powłoki zawierającej krzemian cyrkonu i glinian kobaltu. Modyfikację objętościową zrealizowano podczas odlewania ciekłego stopu przez specjalne filtry ceramiczne, zawierające między innymi glinian kobaltu. Nanocząstki kobaltu, pełniące rolę zarodków krystalizacji, są produktem reakcji modyfikatora (inoculant CoAl2O4) z aktywnymi chemicznie składnikami stopów niklu oraz dodatkowymi składnikami filtrów w postaci proszków Al i Ti. Filtry umieszczono w zbiorniku wlewowym formy. Stwierdzono korzystny wpływ łączonej modyfikacji na makrostrukturę (kryształy równoosiowe) i właściwości mechaniczne. Potwierdzono oddziaływanie aktywnych składników obecnych w stopach niklu i materiale filtrów. Szczególnie silny efekt rozdrobnienia makrostruktury kryształów równoosiowych uzyskano dla stopu MAR-247, który zawiera najbardziej aktywne chemicznie dodatki Hf, Ta i Nb. Opracowano hipotetyczny model modyfikacji powierzchniowej i objętościowej. Stwierdzono istotny wpływ temperatury odlewania stopu na efekt modyfikowania. Efekt modyfikowania jest szczególnie widoczny przy temperaturze odlewania poniżej 1440°C.
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The study describes thermal-chemical interactions that take place in the molten nickel alloy-ceramic mould system, where the mould is either coated with a modifying coating ('blue' mould) or is not ('white' mould). The ceramic mould based on zirconium silicate was made by investment process at the WSK Rzeszów Foundry. The main component of the modifying coating was cobalt aluminate CoAl2O4 added in an amount of 10%. Thermodynamic calculations indicated the possibility of chemical reactions taking place between the chemically active nickel alloy constituents (Al, Ti, Hf, Ta and Nb) and the components of a ceramic mould and modifying coating. The result of such interactions is the risk of the formation of cracks on the surface of mould and molten metal penetration into these cracks, combined with the formation of casting defects, like burns-on, pitting, etc., as proved by extensive X-ray microanalysis. Changes of chemical composition in the surface layer of castings were also reported.
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The work includes studies to determine the significance of the effect of selected technological parameters of moulding and casting conditions on the macrostructure of IN-713C cast nickel alloy. Two-level, fractional 24-1 experiment was carried out, requiring eight experiments. The evaluation covered the number of grains per 1mm2 of the sample surface, the average grain surface area, and the shape index. Macrostructure of test castings indicates a positive effect of combined surface and bulk inoculation treatment, with the effect of surface inoculation prevailing as regards its importance. Statistically significant effect on the number and surface of grains have in descending order: surface modification, bulk modification and temperature of alloy pouring.
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