UDC/UDK 669.18 Original scientific article/Izvirni znanstveni članek ISSN 1580-2949 MTAEC9, 41(3)139(2007) MODELLING OF THE SOLIDIFICATION PROCESS AND THE CHEMICAL HETEROGENEITY OF A 26NiCrMoV115 STEEL INGOT MODELIRANJE PROCESA STRJEVANJA IN KEMIČNE HETEROGENOSTI INGOTA IZ JEKLA 26NiCrMoV115 Martin Balcar1, Rudolf Železný1, Ludvík Martínek1, Pavel Fila1, Jií Bažan2 1ŽAS, a. s., Strojírenská 6, 591 71 Ždár nad Sázavou, Czech Republic 2University VŠB - TU Ostrava, FMMI, 17. listopadu 15, 708 33 Ostrava, Czech Republic martin.balcarŽzdas.cz Prejem rokopisa – received: 2006-08-29; sprejem za objavo - accepted for publication: 2006-12-12 Steel making at ŽDAS, a.s. using secondary metallurgy technology makes it possible to produce liquid metal with high levels of metallurgical cleanliness. During the casting and subsequent cooling of forging ingots, the steel solidification takes place. Directional material solidification, grain size, chemical heterogeneity and discontinuities can have a negative effect on the products’ final properties. The comparison of the chemical composition based on a numerical calculation with the heterogeneity of the real ingot has proven the possibility of using MAGMA software to model the casting and solidification of ingots for open-die forgings made from 26NiCrMoV115 steel. Key words: forging ingot, solidification, heterogeneity, modelling of segregations Za uporabo tehnologije sekundarne metalurgije se v ŽDAS izdeluje tekoče jeklo z veliko metalurško čistostjo. Med ulivanjem in ohlajanjem kovaških ingotov se izvrši strjevanje. Usmerjeno strjevanje, velikost zrn, kemična heterogenost in diskontinuitete lahko negativno vplivajo na lastnosti končnega proizvoda. Primerjava kemične sestave z numeričnim izračunom heterogenosti realnega ingota je dokazala možnost uporabe softvera MAGMA za modeliranje ulivanja in strjevanja ingotov za prosto kovanje izjekla26NiCrMoV115. Ključne besede: kovaški ingot, strjevanje, heterogenost, modeliranje segregacij 1 INTRODUCTION The manufacture of steel forgings for the rotary parts of gas turbines requires an adherence to exactly defined forming and heat-treatment rules. A prerequisite for the successful production of highly stressed machine parts is a high-quality initial blank or ingot. The use of MAGMA software to model the ingot casting and solidification, to forecast the internal quality and the segregation of basic alloying elements and to compare the theoretical prerequisites with practical results makes it possible to evaluate the possibility of also using software for other types of numerical simulation related to the processing of ingots. The evaluation of the chemical heterogeneity of the forging ingot of type 8K8.4 cast at ŽAS, a.s. from 26NiCrMoV115 steel demonstrated the requirements for an isotropic structure and mechanical properties of the steel forging are met. 2 MODELLING OF THE INGOT CASTING AND THE SOLIDIFICATION PROCESS Using the MAGMA software a simulation of the casting and solidification of the 8K8.4 forging ingot in 30NiCrMoV steel with the chemical composition shown in Table 1 was carried out. The results of the numerical modelling of the ingot solidification process in the form of the location of the solidus temperature for different solidification times are shown in Figure 1. A graphical visualisation of the time Figure 1: Development of the solidus temperature range depending on time Slika 1: Časovna evolucija razpona solidusne temperature Materiali in tehnologije / Materials and technology 41 (2007) 3, 139-144 139 M. BALCAR ET AL.: MODELLING OF THE SOLIDIFICATION PROCESS ... Table 1: Chemical composition of steel as per the MAGMA software Tabela 1: Kemična sestava jekla za softver MAGMA MAGMA C Mn Si P S Cr Ni Cu Mo V Al w/% 30NiCrMoV 0.30 - - 0.025 0.006 1.40 3.00 - 0.40 - Figure 2: Stay of the melt in the phase boundary between the liquidus and solidus temperatures Slika 2: Zadržanje taline na fazni meji med likvidusno in solidusno temperaturo zones when the temperature of the molten steel changes through the phase between the liquidus and solidus lines is shown in Figure 2. The final phase of the solidification process is intended for an immediate share of 100 % solid phase. 1 Along with the numerical simulation of the ingot casting and the solidification, calculations of the segregation and unmixing of the basic alloying and tramp elements were also carried out. Significant concentration changes throughout the steel ingot’s cross-section were only noted for elements with greater content. The concentration distribution of some elements is shown in Figures 3 and 4. It is obvious that the degree of segregation increases from the ingot surface towards the axial part. The concentration of the elements was deduced from the concentration ranges in Figures 3 and 4 and arranged in an ascending order, with numbers from 0 to X, according to the local level of concentration. By summing the local content of all the elements the values in Table 2 were obtained showing the relative segregation degree according to the location of the analyses points in Figure 5. Table 2: Relative segregation degree Tabela 2: Relativna stopnja segregacije Sample 1 2 3 H 18 8 0 S 14 9 4 P 7 8 4 Carbon Chromium Nickel Figure 3: Concentration of some elements in the central vertical section of the ingot Slika 3: Koncentracija nekaterih elementov na pokončnem prerezu skozi sredino ingota Molybdenum 140 Materiali in tehnologije / Materials and technology 41 (2007) 3, 139–144 M. BALCAR ET AL.: MODELLING OF THE SOLIDIFICATION PROCESS ... C Concentration w/% Č ¦ 0.3188 0.3149 0.3110 0.3071 0.3031 0.2902 0.2953 0.2914 0.2875 0.2836 0.2707 0.2757 0.2718 0.2679 0.2640 3.050 3.040 3.031 3.021 3.012 3.002 2.993 2.984 2.974 2.965 2.955 2.946 Cross-section view below the ingot top Figure 4: Concentration of some elements in the cross-section, view below the ingot top Slika 4: Koncentracija nekaterih elementov na prerezu pod glavo ingota Table 3: Chemical composition of steel - final melt test Tabela 3: Kemična sestava jekla, končna analiza šarže 0.3864 0.3845 0.3827 Melt analyse C Mn Si P S Cr Ni Cu Mo V Al As Sn Sb Ca w/% µg/g 30NiCrMoV 0.29 0.21 0.01 0.004 0.006 1.69 2.88 0.01 0.41 0.12 0.009 30 <5 <5 4 The highest values of the positive segregation correspond to the ingot part marked with the index H1. Compared with the other sampling points, all the elements attain the maximum concentration here. The lowest concentrations of the analysed elements were found in H3 and events S3 and P3. 3 PRODUCTION PROCESSING AND SAMPLING METHOD Within the scope of the experimental work, the 26NiCrMoV115 steel melt with the chemical composition in Table 3 was made at ŽAS, a.s. The molten Figure 5: Steel ingot dividing and sampling diagram Slika 5: Razdelitev ingota in skica odvzema vzorcev Materiali in tehnologije / Materials and technology 41 (2007) 3, 139-144 141 M. BALCAR ET AL.: MODELLING OF THE SOLIDIFICATION PROCESS ... metal was bottom cast in the mould of the 8K8.4 to form an ingot with a mass of approximately 8 tonnes.3 The solidification and the cooling of the ingot to ambient temperature took place in the mould. In order to facilitate the manipulation after the fettling, the ingot was divided into three parts using a cutting machine, as shown in Figure 5. Figure 5 shows the sampling points for the specimens taken for analysis from parts below the top, from the middle and from the bottom of the ingot. 4 CHEMICAL COMPOSITION OF THE INGOT IN THE MONITORED ZONES The samples H1, H2, H3 were cut out from the body part below the ingot top, the samples S1, S2, S3 from the middle part and the samples P1, P2 and P3 from the ingot’s bottom part. All the samples were submitted for chemical analyses in the laboratory of ISPAT NOVÁ HUT, a.s. and the contents of several elements were determined.4 The chemical compositions of the samples, shown in Table 4, only include the elements present in sufficient Table 4: Chemical composition of samples taken throughout the ingot cross-section Tabela 4: Kemična analiza vzorcev, izrezanih iz prereza ingota Sample K H1 H2 H3 C 0,29 0,315 0,292 0,294 Mn 0,21 0,21 0,20 0,20 P 0,004 0,004 0,005 0,004 S 0,006 0,006 0,005 0,006 Cr 1,69 1,67 1,63 1,63 Ni 2,66 2.88 2,80 2,83 Mo 0,41 0,449 0,381 0,405 V 0,12 0,127 0,111 0,117 Al 0,009 0,010 0,010 0,011 Sample K S1 S2 S3 C 0,29 0,298 0,289 0,290 Mn 0,21 0,20 0,20 0,20 P 0,004 0,003 0,004 0,004 S 0,006 0,005 0,007 0,006 Cr 1,69 1,62 1,63 1,63 Ni 2,83 2,77 2,82 2,80 Mo 0,41 0,381 0,398 0,396 V 0,12 0,111 0,116 0,116 Al 0,009 0,010 0,010 0,011 Sample K P1 P2 P3 C 0,29 0.289 0,289 0,282 Mn 0,21 0,20 0,20 0,20 P 0,004 0.004 0,005 0,004 S 0,006 0,006 0,006 0,006 Cr 1,69 1,62 1,64 1,61 Ni 2,es 2,82 2,83 2,77 Mo 0,41 0,403 0,415 0,409 V 0,12 0,116 0,121 0,117 Al 0,009 0,010 0,010 O,O10 concentrations with respect to the detection limits of the analytical device. If the concentrations of the elements from Table 4 are arranged in ascending order, with evaluation points from 0 to X according to the increasing content, a sum for all the elements indicating the relative segregation degree in Table 5 is obtained. Table 5: Relative segregation degree Tabela 5: Relativna stopnja segregacije Sample 1 2 3 H 27 8 18 S 7 11 9 P 10 19 9 In the zone corresponding to the ingot part marked with H1 the highest positive segregations occur. In this area most elements show a significant unmixing. Compared with other sampling points, carbon, chromium, nickel, molybdenum and vanadium attain the maximum segregation; the lowest concentrations of the elements analysed were found in the S1 and also in the S3 and P3 zones. 5 ELEMENT HETEROGENEITY MEASUREMENT The chemical heterogeneity of the steel samples was determined at VTÚO Brno using a method previously reported 5. For the energy-dispersion (ED) X-ray microanalysis a JEOL JXA8600/KEVEX Delta V Sesame microscope was used. The analyses were performed for elements with a content higher than the detection limit for the ED microanalysis. For each analysed element the content was determined for 101 points. The analysed elements were vanadium, chromium, manganese, iron, nickel and molybdenum. For each point analyses, the program also determined some basic statistical parameters: XS mean value SX standard deviation Min minimum value IHet heterogeneity index IHet = SX/XS Max maximum value Is segregation index Is = Max/XS The results are shown in Table 6. For the evaluation of the chemical heterogeneity the maximum point content for each element was considered and obtained along a measured line of 1000 µm for each sample. The dimensionless parameter known as the segregation index (Is) was determined as the relationship between the maximum concentration and the average concentration in the given section (Is = Max/XS). The results are shown in Table 7. 142 Materiali in tehnologije / Materials and technology 41 (2007) 3, 139-144 M. BALCAR ET AL.: MODELLING OF THE SOLIDIFICATION PROCESS ... Table 6: Basic statistics of samples and elements Tabela 6: Osnovna statistika vzorcev in elementov Table 7: IHet and Is indexes Tabela 7: Indeks IHet in Is H H1 H2 H3 XS SX Min Max XS SX Min Max XS SX Min Max v 0.077 0.000 - -3 0.065 0.044 0.000 0.173 - . 66 0.052 0.000 -¦-", Cr 1.723 0.447 ¦ ¦" 3.119 1.535 0.370 3.079 1.464 0.287 ¦ . : m Mn '85 0.095 0.000 ¦ 6 0.146 0.105 0.000 0.400 ¦ 30 0.084 0.000 0.370 Fe 94.72 0.84 91.48 9631 ¦•• Yi 0.56 Ü82 9. ,0 95.34 0.48 94.02 96 37 Ni 2.967 0.305 2.301 3.791 2 8;;3 0 26: 2.091 3.331 2.866 0.274 2.031 3.611 Mo 0.406 *!j 0.037 i .687 0.239 V- 0.000 0 6:;; 0.185 0.106 0.000 0.547 S S 1 S 2 S3 xs SX Min Max xs sx Min Max xs SX Min Max V 0096 0146 0000 1223 0067 0040 0000 0173 0084 0052 0000 0.213 Cr 1.561 0.477 <¦:¦- 3.119 1.507 0.248 1.119 Ě.559 1.566 0.239 0.969 39 Mu 0.114 O.ü.Č 0.000 0.360 0.Ü8.* dr. i 0.000 0.330 0.147 0.115 0.000 0.410 Fe 95.19 1.13 91 38 9641 95.25 0.39 94.19 96.04 95.18 0.49 93.54 96.07 Ni 2.729 0.271 2.151 3.551 2.918 0.227 2.351 3.501 2.780 0.264 2.121 3.561 Mo 0.313 0.391 O.Oi io 1.787 0.173 .; 09( 0.8: i7 0.427 0.241 0.132 0.3: i7 0.797 P P1 P2 P3 XS SX Hin Max XS SX Min Max XS SX Min Max V 0.108 0.076 0.000 0.343 0 085 0.048 0.000 0.193 0.071 0.050 0.000 0.213 Cr 1.693 0.481 1.049 3.579 1.603 0.577 1.079 5.129 1.499 0.451 0.829 3.129 Mu 0.221 0.129 0.000 0480 0.242 0.137 0.000 0.530 0.095 0.083 0.000 - ¦!-'¦ Fe 9479 0.92 90.42 96 f 95.13 0.70 91.05 36 i: 95.26 0.59 ,,;- 96.31 Ni 2.824 0.283 2.151 3.441 ,688 0.250 2.111 3.261 2.851 0.270 2.331 3.451 Mo 0 370 a;. : V 3.147 0 202 0.113 0.017 , 547 , 225 0.140 V: 0.647 H H1 H2 H3 Ina 1, Ira 1, Ira 1, V 0.802 6.177 B.B77 2.662 8.788 3.379 Cr 0.259 1.810 8.241 2.006 8.196 1.550 Mn 1.118 4.235 8.719 2.740 1.B5B 4.625 Fe 0.009 1.017 0.006 1.012 B.B05 1.011 Ni 0.103 1.278 B.1BB 1.242 B.B96 1.260 Mo 8.663 4.155 8.565 2.791 8.573 2.957 S S1 S2 S3 Ira I. Ira I. Ira I. v 1.521 12.740 B.597 2.582 B.619 2.536 ű 0.306 1.998 8.165 1.698 8.153 1.494 Mi. 8.842 3.153 1.023 4.368 8.782 2.789 Fe 0.012 1.013 B.0B4 1.008 B.B05 1.009 Ni 8.899 1.301 8.078 1.200 B.B95 1.281 Mo 1.249 5.709 8.555 2.468 B.548 3.307 P P1 P2 P3 Ira I. Ira I. Ira I. V 8.784 3.176 8.565 2.271 8.704 3.000 Cr 8.284 2.114 B.36B 3.200 8.301 2.087 Mn 8.584 2.172 8.566 2.190 8.874 3.474 Fe B.B1B 1.016 B.0B7 1.011 B.B06 1.011 Ni 8.188 1.213 8.893 1.213 B.B95 1.210 Mo 1.827 8.505 B.559 4.193 8.619 2.863 Table 8: Maximum and minimum segregation indexes Tabela 8: Največji in najmanjši indeksi segregacije Table 9: Mass distribution of segregation indexes Tabela 9: Razdelitev indeksov segregacije po masi Maxima Minima H1 H2 H3 H1 H2 H3 S1 S2 S3 S1 S2 S3 P1 P2 P3 P1 P2 P3 1 0 1 0 0 0 2 0 0 0 3 1 1 1 0 1 1 0 In order to make it easier to understand, the segregation index for the analysed elements is arranged so that it emphasizes the maximum and minimum segregation index. According to the position of the samples in the ingot, the following indexes were determined. The distribution of the values of the maximum and minimum segregation indexes of the elements shows that it is not possible to decide unambiguously in which ingot part the highest and/or lowest segregation intensity occurs. If we assign the same weight to the highest and/or the lowest segregation index of each element (six analysed elements with a mass of 1/6), the distribution of the maximum and/or minimum segregation indexes of the elements, the data in Table 8, are obtained. Materiali in tehnologije / Materials and technology 41 (2007) 3, 139–144 143 M. BALCAR ET AL.: MODELLING OF THE SOLIDIFICATION PROCESS ... Table 10: Limit values of the segregation indexes related to the elements Tabela 10: Mejne vrednosti za indekse segregacije za elemente Maxima H1 H2 H3 S1 S2 S3 P1 P2 P3 Fe Mn V Ni Mo Cr Minima H1 H2 H3 S1 S2 S3 P1 P2 P3 Fe Ni Mo Cr Mn V These data show that the highest segregation index is obtained in the ingot axis area, where a fraction of 4/6 of cases falls on the vertical column of samples H1-S1-P1 The smallest segregation index is found for samples from the S2 ingot position. In terms of the fraction 3/6 it means S2 takes half of all cases. The fraction 2/3 of cases falls on the column H2, S2 and P2. The minimum fraction 1/6 of the lowest measured values of the segregation indexes falls on the vertical columns H1-S1-P1 and H3-S3-P3, while in the column H1–S1-P1 the weight of occurrence of the elements with the maximum heterogeneity index is 2/3. It can be concluded that the highest unmixing tendency is expected in the ingot axis - column 1. The lowest unmixing tendency can be expected at the surface of the ingot - column 3. The segregation behaviour of the elements Cr and Mn is different, as shown in Table 9. The smallest measured segregation indexes are found for the ingot areas H2, S2 and P2. However, there are also two exceptions to this rule, again the elements are Cr and Mn. Sequence according to the highest segregation index: Table 11: Sequence of segregation indexes Tabela 11: Sekvence indeksov segregacije Segregation V Mo Mn Cr Ni Fe Index 12.74 8.51 4.63 3.20 1.30 1.02 Sequence of elements according to the lowest segregation index: Segrgeation Mo V Mn Cr Ni Fe Index 2.47 2.27 2.17 1.49 1.20 1.01 Both sequences are almost identical, i.e., Mo, V, Mn, Cr, Ni and Fe and only two elements, molybdenum and vanadium, exchange their places in the sequence. In both sequences the elements V, Mo and Mn are in the first three places and the sequence is ended by the elements Cr, Ni and Fe. The reciprocal value of the segregation index k č 1/Is represents, as a first approximation, the effective distribution coefficient of the element6. 6 CONCLUSION The relatively good agreement of the results of the measurements and the simulations of the maximum and minimum segregation index sequence indicate the same tendencies during the solidification and cooling of a steel ingot with a given chemical composition. On the basis of the measurements it can be concluded that this tendency depends on the real value of the effective distribution coefficient of the elements. It is also possible to conclude on the basis of the measurements that, of the external parameters, the parameter referred to as the local solidification time plays an important role, i.e., the time when the particular measured area of the sample stays between the solidus and liquidus temperatures. The use of the MAGMA software to model the ingot casting and solidification process and to predict the behaviour of the basic alloying elements confirms the relative agreement between the theoretical predictions and the practical results. The determination of the chemical heterogeneity of the forging ingot type 8K8.4 of 26NiCrMoV115 steel will contribute to an explanation of the causes of possible occurrence of structural anisotropy of the steel in connection with the end-use properties. ACKNOWLEDGEMENTS The investigations were performed within the EUREKA programme of the E!3192 ENSTEEL project, identification number 1P04EO169. The project was funded partially with the financial support of the Ministry of Education, Youth and Sport of the Czech Republic 7 LITERATURE 1 Martínek, L., Balcar, M., Bažan, J. et al.: Optimization of casting and solidification with respect to the ingot structure and homogeneity. Progress report from the solution of the EUREKA E!3192 ENSTEEL project, identification number 1P04OE169, 2005, 69 p. 2 Martínek, L., Balcar, M. Železný, R.: Optimization of casting and solidification with respect to the ingot structure and homogeneity. Annex No. 4: Numerical simulation outputs and selected quality parameters of the ingot. Progress report form the solution of the EUREKA E!3192 ENSTEEL project, identification number 1P04OE169, 2005, 97 p. 3 Martínek, L., Balcar, M. et al.: Production of components from high-clean steels for power equipment. Progress report on the solution of the EUREKA E!3192 ENSTEEL project, 2004, 117 p. 4 Metallurgical and chemical laboratories ISPAT NOVÁ HUT a.s., Test report, 2004 5 Bažan, J. et al.: Comparison of influence of the contemporary, single and combined processes of extra-furnace metallurgy and casting on the end-use properties and expensiveness of high-grade steels. /Opposed final report of the grant project GAČR 106/01/0365/. VŠB - TU Ostrava, 2003, 68 p. 6 Rek, A., Stránský, K.: Element heterogeneity in the 26NiCrMoV115 steel samples from the 8 t ingot. VTÚO Brno, 2004, 35 p. 144 Materiali in tehnologije / Materials and technology 41 (2007) 3, 139-144