recrystallization of electrolytic iron

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RECRYSTALLIZATION OF ELECTROLYTIC IRON V. G. Dazhin, V. A. Kurdyumov, and Yu. D. KonTkov UDC 669-17-174:669.177 We investigated the reerystallization process in electrolytic iron of differing initial hardness (after electrolysis) in a wide temperature range. Copper samples were plated with iron from an electrolyte of 500 g/liter FeC12.4H20 , pH = 1.5-1.6. At 82-85~ and a current density of 5, 10, 20, 30, and 50 A/din 2 we obtained deposits with a hardness HV of 150, 250, 330, 410, and 490. Recrystallization annealing was con- ducted in a neutral atmosphere at 600, 700, 800, and 900~ for 0.5 h. As the result of subsequent metallo- graphic analysis we obtained a recrystallization diagram (Fig. 1). The initial recrystallization temperature was determined from the appearance of the first nuclei of recrystallized grains during annealing at temper- atures of 500-900~ (20 ~ intervals). The results obtained (Fig. 1) confirm the data [1] on the fact that the initial reerystallization temper- ature of electrolytic iron is above that of pyrometallurgical iron. The main reason for the increase of the initial recrystallization temperature is the saturation of the metal with products of the pyrolysis of hydrox- ides, the decomposition of which occurs at temperatures up to 500~ and is accompanied by the formation of a solid solution of oxygen in iron and oxygen-containing inclusions. Hydrogen pins dislocations only in heat- ing to 300~ [2], and therefore its effect on the recrystallization of electrolytic iron is negligible. Harder coatings, deposited under nonequilibirum conditions, have a stressed structure with strong dislocation fields. Recrystallization should occur with a low activation energy, although it can be seen from Fig. 1 that with an increase in initial hardness of electrolytic iron the initial recrystallization temperature increases. This is due to the increase in its impurity concentration. The concentration of oxygen entering into the composition of these impurities was determined by the vacuum fusion method (Fig. 2). An increase in the concentration of impurity atoms in the form of Cottrell atmospheres has an effect on the initial recrystallization temperature only at small total impurity concentrations. In electrolytic iron the effect of oxygen is apparent only at substantial concentrations (Fig. 2). It can be assumed that oxygen ,o ~ 0,25 / mm 0,20 10- 120 80 / 0.10 .= o,os .j, c.-. /00 200 300 ~00 I/Y Fig. 1 Fig. 2 Fig. 1. Diagram of reerystallization of electrolytic iron. ----) Initial reerystallization temperature. Fig. 2. Effect of oxygen content of electrolytic iron on the orig- inal hardness. Khabarovsk Polyteehnieal Institute. Translated from Metallovedenie i Termicheskaya Obrabotka Metallov, No. 1, pp. 79-80, January, 1970. Consl~lt<mts [3ureau, a division of Plenum Publishing Corporation, 227 II;'est 17th Street~ Neu, Yorh:~ N. Y. I0011. .'~ll rights reserved. T[~is article cannot be reproduced for any purpose whatsoever without permission of the publisher. :l copy of this article is aL, ailable from the publisher for $I5.00. 81

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Page 1: Recrystallization of electrolytic iron

RECRYSTALLIZATION OF ELECTROLYTIC IRON

V. G. Dazhin, V. A. Kurdyumov, a n d Y u . D. K o n T k o v

UDC 669-17-174:669.177

We investigated the reerys ta l l iza t ion p rocess in electrolyt ic iron of differing initial hardness (after e lect rolysis) in a wide tempera ture range. Copper samples were plated with iron from an electrolyte of 500 g / l i t e r FeC12.4H20 , pH = 1.5-1.6. At 82-85~ and a current density of 5, 10, 20, 30, and 50 A /d in 2 we obtained deposits with a hardness HV of 150, 250, 330, 410, and 490. Recrysta l l iza t ion annealing was con- ducted in a neutral a tmosphere at 600, 700, 800, and 900~ for 0.5 h. As the result of subsequent meta l lo- graphic analysis we obtained a recrys ta l l iza t ion diagram (Fig. 1). The initial recrys ta l l iza t ion tempera ture was determined f rom the appearance of the f irst nuclei of r ec rys ta l l i zed grains during annealing at t emper - atures of 500-900~ (20 ~ intervals) .

The resul ts obtained (Fig. 1) confirm the data [1] on the fact that the initial reerys ta l l iza t ion t e m p e r - ature of electrolyt ic iron is above that of pyrometal lurgical iron. The main reason for the increase of the initial recrys ta l l iza t ion tempera ture is the saturat ion of the metal with products of the pyrolys is of hydrox- ides, the decomposit ion of which occurs at t empera tures up to 500~ and is accompanied by the formation of a solid solution of oxygen in iron and oxygen-containing inclusions. Hydrogen pins dislocations only in heat - ing to 300~ [2], and therefore its effect on the recrys ta l l iza t ion of electrolyt ic iron is negligible.

Harder coatings, deposited under nonequilibirum conditions, have a s t r e s sed s t ruc ture with s trong dislocation fields. Recrys ta l l iza t ion should occur with a low activation energy, although it can be seen from Fig. 1 that with an increase in initial hardness of electrolyt ic iron the initial recrys ta l l iza t ion t empera tu re increases . This is due to the increase in its impuri ty concentration. The concentrat ion of oxygen entering into the composit ion of these impuri t ies was determined by the vacuum fusion method (Fig. 2).

An increase in the concentrat ion of impuri ty atoms in the form of Cottrell a tmospheres has an effect on the initial recrys ta l l i za t ion tempera ture only at small total impurity concentrat ions. In e lectrolyt ic iron the effect of oxygen is apparent only at substantial concentrat ions (Fig. 2). It can be assumed that oxygen

,o ~ 0,25 / mm 0,20 10- 120

80 / 0.10

.= o, os . j , c.-.

/00 200 300 ~00 I/Y

Fig. 1 Fig. 2

Fig. 1. Diagram of reerys ta l l iza t ion of e lectrolyt ic iron. - - - - ) Initial reerys ta l l iza t ion tempera ture .

Fig. 2. Effect of oxygen content of electrolyt ic iron on the o r ig - inal hardness .

Khabarovsk Polyteehnieal Institute. Transla ted from Metallovedenie i Termicheskaya Obrabotka Metallov, No. 1, pp. 79-80, January, 1970.

�9 Consl~lt<mts [3ureau, a division of Plenum Publishing Corporation, 227 II;'est 17th Street~ Neu, Yorh:~ N. Y. I0011. .'~ll rights reserved. T[~is article cannot be reproduced for any purpose whatsoever without permission of the publisher. :l copy of this article is aL, ailable from the publisher for $I5.00.

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Page 2: Recrystallization of electrolytic iron

Fig. 3. The beginning of r ec rys ta l l i za t ion of coatings with an initial ha rdnes s of HV 150 (a) and HV 490 (b). (•

a toms favor the fo rmat ion of Suzuki a tmosphe re s , which is par t i a l ly conf i rmed by the fa i r ly slow the rma l act ivat ion of the r ec rys t a l l i za t ion p r o c e s s [3]. Rais ing the annealing t e m p e r a t u r e i nc reases the grain s ize , probably due to the fact that the ra te of grain growth exceeds the fo rmat ion ra te of r ec rys t a ! l i za t ion nuclei at higher t e m p e r a t u r e s .

It can be seen f rom Fig. 1 that soft coatings fo rmed in r ec rys t a l l i za t ion have re la t ive ly fine gra ins . Evidently, with re la t ive ly smal l impur i ty concentra t ions and low dislocat ion dens i t ies the the rmodynamic conditions in different sect ions of the coating become fa i r ly uni form. This induces the format ion of a l a rge number of r ec rys ta l l i za t ion nuclei (Fig. 3). In coatings of high initial ha rdness the conditions for f o r m a - tion of r ec rys t a l l i za t ion nuclei occur f i r s t in p laces with re la t ive ly high excess energ ies , i .e . , at the bound- a r i e s of c racks and l a rge inclusions (Fig. 3). The impor tance of the la t te r in the r ec rys t a l l i za t ion of e l ec - t rolyt ic i ron can be compared with the role of twins in pyrometa l lu rg ica l meta ls [4]. The fo rmat ion of r e - c rys ta l l iza t ion nuclei in ha rde r coatings occurs at e levated t e m p e r a t u r e s , where the number of adsorbed impur i t i es in the gra in boundar ies d e c r e a s e s [5, 6], and t he re fo re the growth ra te of r e c ry s t a l l i z ed gra ins will be higher than in soft coatings and the gra ins will be l a rge r .

It is in te res t ing to note that secondary annealing of r e c ry s t a l l i z ed samples at h igher t e m p e r a t u r e s in- c r e a s e s the gra in s ize , which indicates the collecting r ec rys t a l l i za t ion p r o c e s s in e lec t ro ly t ic iron.

C O N C L U S I O N S

1. An inc rea se of the initial r ec rys t a l l i za t ion t e m p e r a t u r e of e lec t ro ly t ic iron as compared with p y r o - meta l lu rg ica l i ron is due to the la rge amount of oxygen and oxygen-containing impur i t i e s in the meta l , which pin dis locat ions and inhibit the fo rmat ion of r ee rys ta l l i za t ion nuclei.

2. With increas ing initial ha rdness of the coating the initial r ee rys t a l l i za t ion t e m p e r a t u r e and the gra in s ize inc rease .

1.

2. 3. 4.

5.

6.

L I T E R A T U R E C I T E D

Yu. N. Pe t rov et al . , Fiz . Metal. i Metalloved. , 22, No. 5 (1966). V. A. Yagunova and K. V. Popov, Fiz. Metal. i Metal loved. , 12, No. 2 (1961). S. S. Gorel ik, Recrys ta l l i za t ion of Metals and Alloys [in Russian] , Meta l lurgiya , Moscow (1967). L. N. Lar ikov, in: The Phys ica l Bas is of the Strength and Ductil i ty of Metals [in Russian] , Me ta l lu r - gizdat, Moscow (1963}. V. I. Arkharov , Fiz. Metal . i Metal loved. , 12, No. 1 (1961). L. N. Aleksandrov and A. N. Kogan, Fiz. Metal. i Metal loved. , 23, No. 4 (1967).

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