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PHASE TRANSFORMATIONS DURING TEMPERING OF QUENCHED Fe--N ALLOYS M. V. Belous, Yu. N. Moskalenko, and V. G. Permyakov UDC 620.181:669.1'786 The addition of nitrogen to steels is of practical interest due to the development of surface hardening procedures and also from the standpoint of replacing several scarce alloying elements by alloying with nitrogen. Nitrogen is similar to carbon, and therefore similar changes in the strueture and properties can be expected after quenching of austenite and temperIng of martensite with nitrogen. These changes are of considerable theoretical and practical interest. Iron--nitrogen alloys with 0.3-2.05% N were prepared by nitriding samples obtained by pressing and sintering iron powder (0.02% C, 0.014% S, 0.016% P) in hydrogen atl000~ Nitriding was conducted at 550 ~ in ammonia. The quantity of nitrogen in the samples was controlled by the processing time and the degree of dissociation of ammonia. The phase composition of the alloys was determined by x-ray and magnetic analysis. It was found that the alloys consist of ferrite with nitrogen and the 7' nitride, Fe4N. The e phase formed in some cases was eliminated by removal of a surface layer. The alloys were quenched from tem- peratures ensuring homogeneous austenite. The martensite contained 0.5-2.05% N. The quenched samples consisting of martensite with nitrogen and retained austenite were tempered at 100-600 ~ (50 ~ Intervals) for 1 h and cooled in air. The tempered samples were subjected to x-ray analysis. Some of the samples were tempered at constant temperature and with heating in a dilatometer and differen- tial magnetometer in saturating fields. According to the x-ray analysis, tempering at 150 ~ results in the formation of high-nitrogen phase with a tetragonal lattice, with c/a larger than for the original martensite. Temper martensite with a low degree of tetragonality occurred along with this phase after 10w-temperature tempering of the Fe--N alloys. It is probable that the formation of high-nitrogen phase during low-tem- perature tempering is due to ordering in the arrangement of nitrogen ions in the pores of the bcc lattice of iron. Similar results were obtained in [1, 2] for tempered martensite with carbon in several high-manga- nese and high-nickel steels. The increase in the tetragonality of the martensite with carbon at room tem- perature as compared with the quenched condition at negative temperatures is associated with ordering of interstitial atoms. Ordering occurs at all temperatures In the first stage of tempering (20-180 ~ of the quenched Fe--N alloys. It accelerates with increasing tempering temperatures. The coercive force increases at the same time (~40% as compared withthe quenched condition), the intensity of magnetization decreases (by 20% for the alloy with 2% N), and the electrical resistivity decreases ~30% (see Fig. 1). The results of the mag- netometric analysis indicate that the reduction of the magnetization can be explained if the composition of the nitride phase formed during low-temperature tempering matches formula Fel6N2 and the specific magnetization is equal to 110-130 G-cm3/g [3]. No e phase is formed in low-temperature tempering, which is confirmed by the magnetization graphs, on which no Curie temperature was observed for e nitrides. After tempering at 200-300 ~ (second stage) the resistivity is somewhat lower than after low-tempera- ture tempering, the magnetization increases sharply, and the coercive force decreases. The dilatometric analysis showed a reduction in the volume of the sample (0.15% for the alloy with 1.5% N), accompanied by a considerable thermal effect (3 cal/g for the alloy with 1.9% N). According to the structural analysis, the volume effect must be considered outside the rebuilding of the crystal lattice of the lowFtemperature nitride VAev Polytechnical Institute. Translated from Metallovedenie i Termicheskaya Obrabotka Metallov, No. 3, pp. 28-30, March, 1974. Consultants Bureau, a division of Plenum Publishing Corporation, 227 g'est 17th Street, New York, N. Y. I0011. No part of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying, microfilming, recording or otherwise, without written permission of the gr~blisher. ,4 copy of this article is available from the publisher for $15.00. 225

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  • PHASE TRANSFORMATIONS DURING TEMPERING

    OF QUENCHED Fe- -N ALLOYS

    M. V. Be lous , Yu . N. Moska lenko , and V. G. Permyakov

    UDC 620.181:669.1'786

    The addition of nitrogen to steels is of practical interest due to the deve lopment of surface hardening procedures and also f rom the standpoint of replacing several scarce alloying e lements by alloying with nitrogen. Nitrogen is s imilar to carbon, and therefore s imi lar changes in the strueture and propert ies can be expected after quench ing of austenite and temper Ing of martens i te with nitrogen. These changes are of considerable theoretical and practical interest.

    Iron--nitrogen alloys with 0.3-2.05% N were prepared by nitriding samples obtained by press ing and sintering iron powder (0.02% C, 0 .014% S, 0 .016% P) in hydrogen at l000~ Nitriding was conducted at 550 ~ in ammonia . The quantity of nitrogen in the samples was control led by the process ing t ime and the degree of dissociation of ammonia . The phase compos i t ion of the alloys was determined by x - ray and magnet ic analysis. It was found that the alloys consist of ferrite with nitrogen and the 7' nitride, Fe4N. The e phase fo rmed in some cases was el iminated by remova l of a surface layer. The alloys were quenched f rom tem- peratures ensur ing homogeneous austenite. The martens i te contained 0.5-2.05% N.

    The quenched samples consisting of martensi te with nitrogen and retained austenite were tempered at 100-600 ~ (50 ~ Intervals) for 1 h and cooled in air. The tempered samples were subjected to x - ray analysis. Some of the samples were tempered at constant temperature and with heating in a di latometer and differen- tial magnetometer in saturat ing fields. According to the x - ray analysis, tempering at 150 ~ results in the formation of high-nitrogen phase with a tetragonal lattice, with c /a larger than for the original martensite. Temper martensite with a low degree of tetragonality occurred along with this phase after 10w-temperature tempering of the Fe--N alloys. It is probable that the formation of high-nitrogen phase during low-tem- perature temper ing is due to order ing in the arrangement of nitrogen ions in the pores of the bcc lattice of iron. Similar resul ts were obtained in [1, 2] for tempered martensi te with carbon in several h igh-manga- nese and high-nickel steels. The increase in the tetragonality of the martensi te with carbon at room tem- perature as compared with the quenched condition at negative temperatures is associated with ordering of interst i t ia l atoms.

    Ordering occurs at al l temperatures In the f i rs t stage of tempering (20-180 ~ of the quenched Fe--N alloys. It acce lerates with increasing tempering temperatures . The coercive force increases at the same time (~40% as compared withthe quenched condition), the intensity of magnetization decreases (by 20% for the al loy with 2% N), and the electr ical res ist iv i ty decreases ~30% (see Fig. 1). The results of the mag- netometr ic analysis indicate that the reduction of the magnetization can be explained if the composition of the nitride phase formed during low-temperature tempering matches formula Fel6N2 and the specific magnetization is equal to 110-130 G-cm3/g [3]. No e phase is formed in low-temperature tempering, which is conf irmed by the magnetization graphs, on which no Curie temperature was observed for e nitr ides.

    After tempering at 200-300 ~ (second stage) the res ist iv i ty is somewhat lower than after low-tempera- ture tempering, the magnetization increases sharply, and the coercive force decreases. The di latometric analysis showed a reduction in the volume of the sample (0.15% for the alloy with 1.5% N), accompanied by a considerable thermal effect (3 ca l /g for the alloy with 1.9% N). According to the structural analysis, the volume effect must be considered outside the rebuilding of the crysta l lattice of the lowFtemperature nitride

    VAev Polytechnical Institute. Translated f rom Metallovedenie i Termicheskaya Obrabotka Metallov, No. 3, pp. 28-30, March, 1974.

    9 Consultants Bureau, a division of Plenum Publishing Corporation, 227 g'est 17th Street, New York, N. Y. I0011. No part of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying, microfilming, recording or otherwise, without written permission of the gr~blisher. ,4 copy of this article is available from the publisher for $15.00.

    225

  • Hc, Oe Hc, Oe 1

    C

    t.o

    E

    ?

    / /

    cm O,6O

    r~

    o, Jo

    IUO 200 JUg ZllO JUU 'tuO '~C '~ Tempering temperature a b

    Fig. i. Change in physical propert ies with temper ing of quenched Fe + 1% N. a) First stage of temper ing; b) second stage, i) Coerc ive force; 2) magnet i za - tion intensity; 3) electrical resistivity; 4) di latometric curve dur ing temper ing; 5) calor imetr ic curve during tempering. I, 3) I sothermal temper ing for I h; 2, 4, 5) continuous heating at rate of 3-4~

    phase Fe I6N 2 into the T' Fe4N phase. This is conf i rmed by the quantitative analysis of the vo lume effect, taking account of the specific vo lume of the phase participating in the transformation. F rom the results reported in [3], the increase in magnet izat ion in the second stage of temper ing is due to the superposit ion of two effects -- decompos i t ion of retained austenite with nitrogen and the Fe I6N 2 -~ Fe4N transformation.

    In the third stage of temper ing (300-550 ~ the t ransformat ions associated with a change in the phase compos i t ion of the Fe - -N alloys do not occur. The increase in the temper ing temperature leads to a reduc- tion in the width of interference lInes of the a and T' phases and to changes in the coercive force and hard- ness, s imilar to those in carbon steels.

    CONCLUSIONS

    It was found that temper ing processes are similar in quenched steel and nitrided iron -- in the first stage of temper ing (20-180 ~ the martensi te with nitrogen t ransforms, with format ion of metastable F I6N 2 and temper martensite; in the second stage (180-300 ~ the retained austenite decomposes and the Fe I6N 2 --" Fe4N transformat ion occurs; in the third stage (300-550 ~ the number of lattice defects decreases and the Fe4N particles coalesce. After quenching and temper ing at 550-600 ~ the alloy consists of a ferrite--nitride mixture of the type of temper sorbite in carbon steel.

    I.

    2.

    3.

    L ITERATURE C ITED

    L. I. Lysak and Ya. N. Vovk, "Format ion of phase with a cubic lattice dur ing quench ing of steels, " Fiz. Metal. Metal loved., i_99, 5, 669-705 (1965). Yu. L. Al 'shevskii and G. V. Kurdyumov, "The crystal lattice of martensi te in manganese steels, " Fiz. Metal. Metal loved., 25, i, 172-174 (1968). M. V. Belous, Yu. N. Moska lenko, and V. G. Permyakov , "Phase t ransformat ions dur ing temper ing of quenched alloys in the Fe - -N system, " Fiz. Metal. Metal loved., 28, 5, 894-902 (1969).

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