Sinterizazio-atmosferaren eragina M graduko (ASP 30 ... - Euskara
Sinterizazio-atmosferaren eragina M graduko (ASP 30 ... - Euskara Sinterizazio-atmosferaren eragina M graduko (ASP 30 ... - Euskara
AVOIDING GRAIN GROWTH DURING THE SUPERSOLIDUS SINTERING OF HIGH SPEED STEELS J .I. SAN MARTIN, S .JAUREGI, LURRUTIBEASKOA, V.MARTÍNEZ, R.PALMA AND J .J.URCOLA CENTRO DE ESTUDIOS E INVESTIGACIONES TÉCNICAS DE GUIPÚZCOA (CEIT) ESCUELA SUPERIOR DE INGENIEROS INDUSTRIALES DE SAN SEBASTIÁN SAN SEBASTIÁN, (GUIPÚZCOA), BASQUE COUNTRY, SPAIN . KEY WORDS : High Speed Steel, Grain Size, Supersolidus Sintering, ABSTRACT Grain growth during supersolidus sintering of high speed tool steels in vacuum and in an atmosphere composed of N2-H2-CH4 has been investigated . An increase of temperature above the optimum for sintering (minimum temperature at which the theoretical density is reached) in vacuum causes a significant increase in the grain size, due to the dissolution of carbides and the increased amount of the liquid phase. On the other hand, oversintering in the N2-H2-CH4 atmosphere, although increasing the amount of liquid phase, results in only a small increase in the grain size . This different behaviour can be explained in terms of the formation, by reaction with the atmosphere, of very fine vanadium carbonitrides (< 1µm), which are very stable and do not dissolve even at high temperatures . This effect, responsible for better mechanical properties of high speed steels oversintered in the N2-H2-CH4 atmosphere, in comparison with vacuum, can be explained in terms of the Zener drag exerted by the fine and stable carbonitrides . INTRODUCTION It is widely known that oversintering, in vacuum, of high speed steels causes an accelerated austenite grain growth (1), also resulting in the formation of eutectic carbides during cooling (2), with the subsequent impairment of the mechanical properties (3) . In recent years investigations carried out at CEIT have shown that this grain growth during oversintering can be avoided when an atmosphere composed of N2-H2-CH4 is used (4) . In the present work a detailed analysis of the microstructural changes taking place during sintering in this atmosphere, and their effect on grain growth during the oversintering, have been carried out .
EXPERIMENTAL PROCEDURE Vacuum annealed, water atomized T42, T15 and Px30 powders were bought from Powdrex Limited, Tonbridge, U .K. The compositions of the powders provided by the manufacturer are given in Table I . Additions of 0 .2 weight % of elemental carbon in the form of graphite, 15 µm mean size, were made in some cases . TABLE 1.- Chemical Analyses of As-Received Steel Powders . Weight Percent . C Si Cr a (PPm) Compacts of 16 mm diameter were cold compacted uniaxially at a pressure of 500 MPa, the walls being lubricated . These compacts were sintered either in a flowing atmosphere composed of 90 volume %N2-9%H2-1%CH4 or in vacuum, better than 5 Pa during the sintering . Density after sintering was normally evaluated through the Archimedes method (5), although for some samples this was calculated using the weight and the geometrical dimensions after grinding the sintered specimen to a cylinder . Transverse sections were mechanically polished . After etching with 5% Nital these were observed under an optical microscope in order to measure the austenite grain size, using the mean linear intercept length technique . A minimum of 600 grains was measured . The amount of retained austenite was also determined by X-ray diffraction techniques (6) . Quantitative metallography techniques were used to measure the volume fraction and the distribution of primary carbides and/or carbonitrides . RESULTS AND DISCUSSION Co V Cu Mn Mo Ni p S W PX30 1 .33 0 .31 4 .28 488 8 .7 3 .32 0 .08 0 .23 5 .14 0 .29 0 .024 0 .015 6 .63 T42 1 .43 0 .28 4 .18 478 9 .44 2 .94 0 .10 0 .21 3 .22 0 .12 0 .024 0 .013 8 .89 T15 1 .64 0 .25 4.37 757 4 .99 4 .70 0 .11 0 .24 0 .56 0 .13 0 .023 0 .019 12 .40 The variation of austenite grain size with the deviation of temperature from the optimum for sintering is shown in figure 1 for the three steels with and without the addition of free carbon . It is apparent that for vacuum sintering grain growth results rapidly at temperatures higher than the optimum (positive deviation), but the grain size increases only very slowly above the optimum sintering temperature for gas sintered steels. Grain growth is very similar for the three steels when sintered under the same conditions . Figure 2(a) shows the microstructure of a specimen vacuum sintered at the optimum temperature . The presence of the products of decomposition of austenite is clearly seen mainly surrounding the primary carbides and inside the original grains of austenite . Some retained austenite is also present . The primary carbides are mainly MC and M6C . The carbides in the grain boundaries are fundamentaly massive type MC (> 4 gm ) . For atmosphere sintering (figure 2(b)), the incorporation of nitrogen into the steel produces some important modifications to the microstructure . Firstly a significant increase in retained austenite is observed and secondly the MC type carbides change to MX carbonitrides of smaller size, as shown in figure 3 .
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EXPERIMENTAL PROCEDURE<br />
Vacuum annealed, water atomized T42, T15 and Px<strong>30</strong> powders were bought from Powdrex<br />
Limited, Tonbridge, U .K. The compositions of the powders provided by the manufacturer are<br />
given in Table I . Additions of 0 .2 weight % of elemental carbon in the form of graphite, 15 µm<br />
mean size, were made in some cases .<br />
TABLE 1.- Chemical Analyses of As-Received Steel Powders . Weight Percent .<br />
C Si Cr a<br />
(PPm)<br />
Compacts of 16 mm diameter were cold compacted uniaxially at a pressure of 500 MPa, the<br />
walls being lubricated . These compacts were sintered either in a flowing atmosphere composed of<br />
90 volume %N2-9%H2-1%CH4 or in vacuum, better than 5 Pa during the sintering . Density after<br />
sintering was normally evaluated through the Archimedes method (5), although for some samples<br />
this was calculated using the weight and the geometrical dimensions after grinding the sintered<br />
specimen to a cylinder .<br />
Transverse sections were mechanically polished . After etching with 5% Nital these were<br />
observed under an optical microscope in order to measure the austenite grain size, using the mean<br />
linear intercept length technique . A minimum of 600 grains was measured . The amount of retained<br />
austenite was also determined by X-ray diffraction techniques (6) . Quantitative metallography<br />
techniques were used to measure the volume fraction and the distribution of primary carbides<br />
and/or carbonitrides .<br />
RESULTS AND DISCUSSION<br />
Co V Cu Mn Mo Ni p S W<br />
PX<strong>30</strong> 1 .33 0 .31 4 .28 488 8 .7 3 .32 0 .08 0 .23 5 .14 0 .29 0 .024 0 .015 6 .63<br />
T42 1 .43 0 .28 4 .18 478 9 .44 2 .94 0 .10 0 .21 3 .22 0 .12 0 .024 0 .013 8 .89<br />
T15 1 .64 0 .25 4.37 757 4 .99 4 .70 0 .11 0 .24 0 .56 0 .13 0 .023 0 .019 12 .40<br />
The variation of austenite grain size with the deviation of temperature from the optimum for<br />
sintering is shown in figure 1 for the three steels with and without the addition of free carbon . It is<br />
apparent that for vacuum sintering grain growth results rapidly at temperatures higher than the<br />
optimum (positive deviation), but the grain size increases only very slowly above the optimum<br />
sintering temperature for gas sintered steels. Grain growth is very similar for the three steels when<br />
sintered under the same conditions .<br />
Figure 2(a) shows the microstructure of a specimen vacuum sintered at the optimum<br />
temperature . The presence of the products of decomposition of austenite is clearly seen mainly<br />
surrounding the primary carbides and inside the original grains of austenite . Some retained<br />
austenite is also present . The primary carbides are mainly MC and M6C . The carbides in the<br />
grain boundaries are fundamentaly massive type MC (> 4 gm ) . For atmosphere sintering (figure<br />
2(b)), the incorporation of nitrogen into the steel produces some important modifications to the<br />
microstructure . Firstly a significant increase in retained austenite is observed and secondly the MC<br />
type carbides change to MX carbonitrides of smaller size, as shown in figure 3 .