ISSN 0031-918X, The Physics of Metals and Metallography, 2008, Vol. 105, No. 4, pp. 409419.

Pleiades Publishing, Ltd., 2008. Original Russian Text V.P. Pilyugin, T.M. Gapontseva, T.I. Chashchukhina, L.M. Voronova, L.I. Shchinova, M.V. Degtyarev, 2008, published in Fizika Metallov i Metallovedenie, 2008, Vol. 105, No. 4, pp. 438448.

STRENGTH AND PLASTICITY

Evolution of the Structure and Hardness of Nickel upon Cold and Low-Temperature Deformation under Pressure
V. P. Pilyugin, T. M. Gapontseva, T. I. Chashchukhina, L. M. Voronova, L. I. Shchinova, and M. V. Degtyarev
Institute of Metal Physics, Ural Division, Russian Academy of Sciences, ul. S. Kovalevskoi 18, Ekaterinburg, 620041 Russia
Received March 12, 2007; in nal form, July 7, 2007

AbstractThe effect of the deformation temperature ensuring different mobility of dislocations on the change of stages of the structural state of single-crystal nickel has been studied. It has been shown that the deformation temperature affects the type of arising boundaries and the degree of deformation that corresponds to the transition of the material to a new structural state. The formation of microtwins and deformation bands in the structure at the liquid-nitrogen temperature not only retards the formation of a homogeneous submicrocrystalline structure but also leads to a lesser strain hardening. PACS numbers: 62.20.Fe, 81.40.Lm DOI: 10.1134/S0031918X08040157

INTRODUCTION The ways of the development of the orientation instability of the single-crystal structure which transforms it into a polycrystalline aggregate are determined by the mobility of dislocations. The dislocation mobility can be reduced by two methods: by decreasing stacking-fault energy (SFE) upon alloying and by decreasing deformation temperature. The rst method, which was realized in [1], is connected with investigating materials of different chemical composition. The second method makes it possible to perform the investigation on one and the same material and, hence, seems to be more preferable [2]. There exist two approaches to the estimation of the type of structure formed upon deformation. The rst approach is based on the direct measurement of misorientation angles of neighboring structure elements and allows one to determine, to a certain accuracy, the fraction of high- and low-angle boundaries. The drawbacks of this method are in that, rst, the classication of the boundaries is performed arbitrarily, irrespective of their type, using, for example, the magnitude of the misorientation angle (say, whether this angle is more or less than 15, as in [3]); but, second, even the knowledge of the fraction of boundaries of one or another type does not enable one to predict the kinetics of grain growth upon heating, and the percentage ratio itself can depend on the examined area of a sample. The other approach is statistical. It is based on an analysis of the dependence of hardness of the material under consideration on the degree of deformation [4]. Although this approach yields no data on the quantitative relation of different-type boundaries, it shows degrees of

deformation leading to a changeover of the stages of the structural state. Since in this case the entire area of a large number of samples deformed using both the same angle and different angles of the anvil rotation is investigated, this approach lacks the drawbacks of the rst method. The determination of the conditions of transition to the stage of a homogeneous submicrocrystalline structure is of great practical importance, since this transition is associated with a fundamental change in the kinetics of primary recrystallization [5] and, as a consequence, with a signicant enhancement in thermal stability of the ultradispersed structure [6]. The rst studies of structural changes in nickel upon cold and low-temperature deformation by shear under pressure were performed in [1, 2]. It was shown that the mechanisms of structure formation change with changing deformation temperature. In [2], the low-temperature deformation was performed in order to obtain ner grains upon recrystallization than in the same material deformed at room temperature. The result, however, proved to be opposite. One of the factors responsible for this result was the nonuniform structure formed upon low-temperature deformation. Neither the degree of deformation which can provide a homogeneous submicrocrystalline structure, nor any other quantitative characteristics of the stage nature of structural development were established in [1, 2]. The purpose of this work was to study the effect of the deformation temperature on the hardness of nickel and on the various stages of the development of its structure.

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EXPERIMENTAL A single crystal of nickel of purity 99.98% was deformed by the method of shear under pressure using Bridgman anvils at 80 and 290 K. The temperature was measured by a thermocouple attached to the xed anvil. Before deformation, the specimens had a diameter of 7 mm and a thickness of 0.3 mm. The specimen surface was parallel to a plane {111}. The average calculated pressure was 5 GPa. The angle of the anvil rotation was varied from 45 to 10 rev (10 rev = 360 10). To obtain the radial distribution of hardness in the specimens, measurements were conducted on a PMT-3 testing device at a load of 0.5 N. The degree of deformation was calculated with allowance for the upsetting, which depended on the angle of the anvil rotation and distance to the specimen center [4]. When constructing the dependence of the hardness, its values obtained on different specimens were averaged in intervals of logarithmic deformation e = 0.2. The microstructure was studied by transmission electron microscopy. The distance from the specimen center to the region under consideration was estimated with an accuracy of 0.2 mm. The sizes of structure elementsdislocation cells and microcrystalliteswere determined in bright-eld and dark-eld images in a reection of the {111} type from the results of more than 400 measurements, which ensured an error of less than 10% [7]. Statistical processing of the results was performed using a STATISTICA program. RESULTS Figure 1 displays the hardness dependence of nickel deformed at 290 and 80 K on the square root of logarithmic deformation. The bends in the dependence, according to [8], correspond to changes in structural states.
H, GPa 6

3 e1/2

Fig. 1. Hardness of nickel deformed by shear under pressure at T = 290 K (solid circles) and T = 80 K (open squares).

In a deformation range of 1 < e < 9, three stages of changes in the hardness (transitions from the rst stage to the second and from the second stage to the third occur at e12 = 3 and e23 = 5.3, respectively) are observed at Tdef = 290 K and two stages (e12 = 3.4) at Tdef = 80 K. In this case, the hardness of nickel deformed to e 7 at room temperature proves to be greater than that after deformation to the same degree at the liquid-nitrogen temperature. At a higher degree of deformation the relation between the hardnesses values changes to the reverse. Each stage is characterized by a certain hardness-enhancement coefcient. At the rst stage, the coefcient is relatively small at both 290 and 80 K: k1290 = 0.4 and k180 = 0.2 GPa per unit logarithmic deformation. At the second stage, on the contrary, its values are high: k2290 k280 0.6. At the third stage, at 290 K, the hardness grows only weakly with increasing degree of deformation: k3290 = 0.06. At 80 K, as was already noted, no third stage is observed (Fig. 1). The electron-microscopic investigation made it possible to establish the type of structure at each of the stages found. At room temperature, in the rst stage of the H = f (e0.5) dependence observed in Fig. 1, a weakly misoriented cellular structure is formed (see Figs. 2a, 2b). An azimuthal spreading of reections in electron diffraction patterns and a gradually changing contrast in dark-eld electron-microscopic images are characteristic of such a structure. Since prior to deformation the nickel single crystal examined contained no high-angle boundaries, at this stage only low-angle dislocation boundaries of deformation origin (i.e., single-type boundaries) are present. With increasing deformation, the cell boundaries become narrower and the cell size decreases. The rst microcrystallites (structure elements separated from the surrounding matrix by highangle boundaries and containing virtually no dislocations [1]) appear after deformation to e = 3 (second stage in Fig. 1). These microcrystallites are characterized by a sharp change in the diffraction contrast at their boundaries in the dark-eld images and yield isolated pointlike reections in a microdiffraction pattern [1, 4]. This stage is characterized by the presence of differenttype boundaries in the structure (Fig. 2c). With increasing deformation, the fraction of microcrystallites in the structure grows, while the fraction of cells decreases; and in the third stage, at e > 5.3, a structure consisting only of microcrystalliteshomogeneous submicrocrystalline (SMC) structureis formed (Fig. 2d). At this stage, microcrystallites whose internal volume is divided into fragments by low-angle dislocation boundaries are observed (Fig. 2d). With decreasing deformation temperature, as is known, the critical shear stress grows and diffusional processes slow down. This decreases the mobility of dislocations and, in spite of some growth of the SFE (in nickel, according to [9], when the temperature is reduced from room temperature to 77 K, the magnetic
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411

(a)

0.3 m

(b)

0.3 m

(c)

0.3 m (d)

0.3 m

Fig. 2. Microstructure of nickel deformed at 290 K: (a, b) e = 0.5, (c) 3.3, (d) 5.6; and (b, c, d) dark-eld images in a reection of the {111} type.

component of SFE increases), retards the formation of a cellular structure [2, 10]. As a result, at 80 K conditions for deformation by the twinning mechanism are ensured. At the initial stages of low-temperature deformation (rst stage in Fig. 1), microtwins are observed along with a cellular structure (Fig. 3). In Figs. 3a3c, bright-eld and dark-eld images of a twin in the structure of nickel deformed to e = 1.5 are presented and the twinning plane (111) is determined. An increase in the low-temperature deformation to e = 2.5 led to an enhancement in the density of twins and their mutual intersection (Fig. 3d). A structure in the form of packets of alternating bands (Figs. 4a, 4b) characterized by high-angle mutual misorientations occupies a considerable fraction of the volume. Within each band, the orientation changes only a little. In the literature, regions of a banded structure in which the orientation changes only slightly are called deformation bands [11] and if their thickness is smaller than 1 m, they are called microbands [12]. Thus, under conditions of a reduced mobility of dislocations, the deformation at 80 K, unlike the deformation at room temperature, gives rise already at the rst stage (according to Fig. 1) to both low-angle and highangle boundaries. The rst microcrystallites at 80 K appear at a somewhat higher degree of deformation (the
THE PHYSICS OF METALS AND METALLOGRAPHY

onset of the second stage, e = 3.4) than at room temperature. At the second stage, microbands become fragmented (Figs. 4c, 4d), and regions of a submicrocrystalline structure are formed with increasing deformation (Figs. 4e, 4f). However, the microcrystallites do not become the only structural constituent up to e = 8, and no transition to a homogeneous SMC structure is observed. The structure remains inhomogeneous and consists of nitely misoriented microcrystallites and microband fragments close in size to them, with a continuously alternating misorientation within one band (Fig. 4f). Thus, at 80 K both the rst and second stages are stages with a mixed structure. It should be noted that the change of stages can remain unnoticed in this case if it is determined from the misorientation spectrum since at both these stages both low-angle and high-angle boundaries are observed. Figure 5 displays the size distribution of the elements of the nickel structure (dislocation cells, fragments of microbands, and microcrystallites) upon deformation at the stages of mixed and SMC structures; the corresponding characteristics of the distribution are given in Table 1. In this work, at the stage of cellular structure no distribution was constructed and no average size of the elements was determined. It is seen that at room temperature, already at the beginning of the
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(a)

0.5 m

(b)

0.5 m

333tw 113tw 511 113tw 551tw 311 331tw 440tw 131 111tw 220tw 662tw 440 000tw 220 442tw (110) 553tw 000 222tw 333tw 371 113tw 131 151 (c)

(d)

1 m

[114] || [110]tw
Fig. 3. Microstructure of nickel deformed at 80 K: (ac) e = 1.5; (d) 2.5; (b) dark-eld image of the twin with a twinning plane {111} in a reection of {331} type; (c) microdiffraction pattern with a superimposed key pattern; and (d) dark-eld image in a reection of the {111} type.

stage of mixed structure, the sizes of the elements comprising it prove to be predominantly smaller than 1 m (Fig. 5a). With increasing deformation, their further reduction occurs (Fig. 5b). At the stage of the SMC structure, on the contrary, an increased deformation does not lead to a marked change in the distribution histogram (Figs. 5c, 5d). At the liquid-nitrogen temperature, the structure observed at the beginning of the second stage is more inhomogeneous than at room temperature. The elongated structure elements stemmed from the fragmentation of microbands form an isolated peak (of about 1%) in the distribution histograms in a range of large sizes (Fig. 5e). At the second stage (Fig. 1) the low-temperature deformation results in such a renement of structure elements (Figs. 5e5h) that already at e = 6.7 their size proves to be smaller than that reached at the third stage of deformation (5.3 < e < 9.3) at room temperature. The uniformity of the renement of structure elements upon deformation can be estimated using the coefcient of variation of their linear dimensionsa ratio of the root-mean-square deviation to the average size of elements (Table 1). After room-temperature deformation, the value of the variation coefcient is about 0.50.7, which indicates a high degree of structural homogeneity [13]. Deformation at 80 K in the

interval of 4.0 < e < 5.3 led to the variation coefcient ranging from 1.3 to 1.0, which is characteristic of a structure formed by elements nonuniform in size [13]. With increasing deformation at 80 K, the variation coefcient drops to 0.50.6, i.e., the structure becomes uniform in size of its elements. Figure 6 shows the variation of the average size of structure elements with increasing deformation. It is seen that these dependences correlate with the behavior of hardness (see Fig. 1). The bend in the dependence at T = 290 K corresponds to e = 4.8. This value is close to e23 = 5.3 found from the graph of hardness at which a transition of the structure to the third stage takes place. It should be emphasized that the degree of deformation corresponding to the bend in Fig. 1 was determined statistically reliably, using numerous specimens, whereas the bend in Fig. 6 is determined much less exactly. At 80 K, the dependence of the average size of structure elements on the logarithmic deformation was determined only for the second stage. This dependence is linear and has no inections. The coefcient of renement of structure elements at the second stage (stage of mixed structure), irrespecref tive of the deformation temperature, is k2 80 K k2 290 K 0.15 m per unit logarithmic deformation. A
ref

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(a)

0.5 m

(b)

0.5 m

(c)

0.1 m (d) 0.1 m

(e)

0.1 m

(f)

0.1 m

Fig. 4. Microstructure of nickel deformed at 80 K: (a, b) e = 0.5, (c, d) 5.3, (e) 5.5, (f) 6.7; and (b, d, f) dark-eld images in a reection of the {111} type.

change in the average size of elements of the SMC structure at the third stage is very insignicant and is characterized by a renement coefcient k3ref = 0.004 m per unit logarithmic deformation. DISCUSSION A decrease in the deformation temperature to 80 K brought about a reduced mobility of dislocations and hampered dynamic recovery. With the unaltered mechanism of deformation via dislocation slip, the deformation-temperature lowering must cause a faster growth of hardness. Data in Fig. 1, however, demonstrate the contrary result: a twofold drop in the hardness-enhancement coefcient at this stage (rst stage in Fig. 1). The hampered dislocation slip increases the probability of twinning [2, 14]. According to literature data [12, 15,
THE PHYSICS OF METALS AND METALLOGRAPHY

16], the localization of deformation and the appearance of deformation bands is accompanied by cessation of strain hardening. For this reason, a slower enhancement in the hardness of nickel upon low-temperature deformation at the rst stage (see Fig. 1) can be connected with both the formation of banded structures (Figs. 4a, 4b) and the activation of a new deformation mechanismvia twinning (Fig. 3). The absolute values of hardness in this case likewise proved to be smaller (large sizes of elements of the arising structure corresponded to smaller values of hardness). Besides, this stage at the low temperature turned out to be of longer duration (to e = 3.4 and 3.0 at 80 and 290 K, respectively). This can indicate a higher efciency of twinning as a relaxation process. At the same time, the transition to a new mechanism of deformationrotational modesat the second stage
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0.5

1.0

1.5 (b)

2.0 0

4 (f)

0.5

1.0

1.5 (c)

2.0 0

0.5

1.0

1.5 (g)

2.0

0.5

1.0

1.5 (d)

2.0 0

0.5

1.0

1.5 (h)

2.0

0.5

1.0

1.5

2.0 0 d, m

0.5

1.0

1.5

2.0

Fig. 5. The size-distribution histograms of structure elements for nickel deformed at (ad) 290 K and (eh) 80 K: (a) e = 3.3, (b) 5.0, (c) 5.6, (d) 9.3, (e) 4.4, (f) 5.3, (g) 5.5, and (h) 6.7.

(Fig. 1) at 80 K occurred in the material with a larger size of crystallites (Fig. 5). This stage at both deformation temperatures is characterized by the highest rate of growth of hardness and renement of structure elements. The corresponding coefcients vary only slightly with deformation temperature. At room temperature, the next stagestage of submicrocrystalline structureis achieved in nickel at a relatively small deformation of e = 5.3 (see Fig. 1). Earlier, when investigating iron and structural steels [4], it was found that the transition from the stage of mixed structure to the stage of SMC structure can be accompanied by both increase and decrease in the coef-

cients of enhancement in hardness and of renement of structure elements. In nickel at the stage of an SMC structure, there are observed weak tendencies for an enhancement in hardness, a renement of structure elements, and an increase in their size uniformity (Figs. 1, 5, 6 and Table 1) characterized by very small values of the above coefcients and a small decrease in the coefcient of variation of linear dimensions. Whether or not the observed change in the SMC structure of nickel upon deformation is signicant or it does not exceed an experimental error can be established with the help of recrystallization, as this was done in [17, 18]. However,
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EVOLUTION OF THE STRUCTURE AND HARDNESS OF NICKEL Table 1. Characteristics of the size distribution of structure elements Tdef , K 290 Type of structure Mixed e 3.3 3.8 5 5.6 9.3 9.6 9.9 4.4 5.3 5.5 6.7 dav , m 0.40 0.30 0.13 0.14 0.12 0.13 0.13 0.35 0.25 0.10 0.08 dprob , m 0.18 0.13 0.07 0.08 0.07 0.08 0.08 0.22 0.07 0.04 0.03 dmax , m 1.3 1.1 0.57 0.57 0.48 0.44 0.38 4.6 1.4 0.25 0.23 , m 0.26 0.17 0.08 0.08 0.07 0.06 0.06 0.44 0.23 0.05 0.04 K 0.7 0.6 0.6 0.6 0.6 0.5 0.5 1.3 1.0 0.5 0.5

415

SMC

80

Mixed

this problem will be the subject of an independent investigation. Upon low-temperature deformation of nickel, the second stage continues at least to e = 7.3 and the transition to the stage of SMC structure has not been conrmed statistically. The fragmentation developed in microbands and microtwins leads to their gradual destruction. Nevertheless, up to the extremely large degrees of low-temperature deformation reached in this work, there are retained regions of structure in which microcrystallites along a certain direction exhibit close orientation (Fig. 4f). At this stage, no new deformation bands were found. According to the theoretical concepts, twinning can be one of the possible mechanisms of nanostructural evolution upon plastic deformation. Upon a renement of nanograins, the twinning is hampered. Nevertheless, the formation of semicoherent and coherent twins is possible in grains of 100 and 10 nm in size, respectively [19]. In this work, no formation of microtwins was found either at the second stage at 80 K, when the rotational mechanism of deformation begins to operate, or throughout deformation at room temperature, which is contradictory to the theoretical model [19]. The dependence that shows the variation of the hardness upon low-temperature deformation also can be represented as a three-stage one (Fig. 1). In this case, the e12 value increases to four and the third stage begins at e23 = 7.3. The hardness-enhancement coefcient increases to k280 K = 0.74 GPa per unit logarithmic deformation. However, the establishment of the third stage is not justied statistically, since it was performed using only two experimental points. The unambiguous solution to the problem of reaching the third stage calls for an additional study of specimens deformed at 80 K to higher degrees (e > 7), which meets with considerable methodical difculties. A signicant role in the structure formation in nickel deformed at room temperature apparently belongs to
THE PHYSICS OF METALS AND METALLOGRAPHY

dynamic recovery, which leads to both annihilation of dislocations and formation of their equilibrium congurations. The formation of regular dislocation congurations initiates the appearance of misoriented cellular structures [1, 10, 20] and results in strengthening of the material. On the other hand, the inevitable annihilation of dislocations of unlike signs reduces their total density and results in softening. When, due to these competing processes, the density of structure-forming dislocations (which are retained in the structure after termination of loading [21]) remains unaltered and, because of this, structure parameters and properties of the material under consideration likewise remain unchanged, we deal with the steady-state stage of dynamic recovery. This stage corresponds to the stage of steady-state deformation with a strain-hardening coefcient approaching zero [1]. A similar situation is observed in nickel at the stage of SMC structure. In microcrystallites, dislocation boundaries are formed, with the result that the misorientation of neighboring
d, m 0.6

0.4

0.2

10 e

Fig. 6. Dependence of the average structure-element size on the degree of deformation at 290 (solid circles) and 80 K (open squares). Vol. 105 No. 4 2008

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(a)

0.1 m (b)

0.1 m (c)

0.1 m

Fig. 7. A change in the contrast in the nickel single crystal deformed to e = 9.3 at 290 K. The inclination of a goniometer: 5 from (a) to (b); and 5 from (b) to (c).

parts of the microcrystallite can reach 10 (Fig. 7). An increased deformation does not lead to renement of the microcrystallites. Low-angle boundaries inside microcrystallites were also observed in iron of purity 99.97% at the stage of the SMC structure, an increased deformation at this stage was accompanied by renement of the microcrystallites. Distinctions in the behavior of the SMC structure between nickel and iron upon deformation can be connected with different mobility of dislocations. Under comparable temperatureforce conditions, the mobility of dislocations in nickel, according to data reported in the monograph [22], is higher by seven orders of magnitude than in iron (the velocities of motion are on the order of 104 and 103 cm/s, respectively). From this it may be concluded that in iron, due to rotational modes of deformation, these low-angle twist boundaries of low mobility [23] transform into high-angle boundaries and in such a fashion a renement of microcrystallites takes place [4]. In nickel at the stage of SMC structure, mobile tilt dislocation boundaries [23] inside the microcrystallites are formed and disappear continuously, and almost no renement of the microcrystallites occurs for this reason. The hampering of recovery at 80 K results in the continuation of renement of structure elements upon deformation to e > 5.3. In this case, their dimensional uniformity characterized by such indices as the coefcient of variation of linear dimensions and the ratio of the maximum size to the average size increases. However, there is retained a structural inhomogeneity caused by the presence of different-type boundaries (dislocations boundaries of cells and microbands, twin boundaries, and nonequilibrium high-angle boundaries

of microcrystallites), although different structure elements have sizes of the same order of magnitude. A comparison of Figs. 2d and 4d shows that the observed structure elements have close sizes. In the size-distribution histograms of structure elements corresponding to these treatments (Figs. 5c and 5f), it is seen that in both structures a considerable number of elements on the order of 0.1 m in size are present. However, the microdiffraction patterns differ strongly. Figure 2d displays an SMC structure that consists of microcrystallites characterized by mutual discrete (nite) misorientations. The point reections in the microdiffraction pattern are located so closely to one another that the diaphragm captures instantaneously several reections. For this reason, in the dark-eld image (Fig. 2d) almost each of the observed microcrystallites exhibits its particular orientation. Figure 4d shows a mixed-type structure formed in a region occupied by diffraction microbands. The structure elements observed in Fig. 4d have the same orientation and are bright in one and the same reection. In other words, since some sets of elements of this structure yield only one reection, the number of reections is small. Thus, distinctions between the microdiffraction patterns depend not only on the structure-element size but also on the type of structure that in this case is determined by the deformation temperature. By analogy with boundaries of initial martensite laths in the SMC structure of deformed packet martensite [4], the boundaries of microbands produce a small mutual misorientation of microcrystallites within microbands which is retained to ultimately large deformations reached in this work. Apparently, it is precisely this factor that can be responsible for the anomalous grain growth upon subsequent annealing.
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417 0.5 d, m 1

As a result of this inhomogeneity, the nickel specimens deformed to e 7 at room and low temperature demonstrate different behavior upon heating [2]. In this work, it was assumed that the formation of coarser recrystallized grains after low-temperature deformation is connected with a hampered formation of recrystallization centers immediately in the course of deformation and with a high driving force of recrystallization owing to a high stored energy of deformation. The results of this work show that an insufcient mutual misorientation of structure elements that were formed within one deformation band can also be responsible for the formation of coarse recrystallized grains. In [24], the formation in the quenched 20G2R steel of closely oriented microcrystallites within the initial martensite lath caused, upon subsequent heating, their growth by the coalescence mechanism, rapid coarsening of some grains, and signicant variations in grain size. The effects of the deformation temperature on the dependence of hardness on the structure-element size was also investigated. This dependence is usually described by the HallPetch-type equation: H = H 0 + kd .
m

0.1 1.5 ln(H 0.75) 1.0 0.5 0 3

0 lnd

Fig. 8. Dependence of the hardness of nickel on the structure-element size at T = 290 (solid circles) and T = 80 K (open squares).

value of H0 = 0.75 GPa corresponding to the hardness of the initial single-crystal nickel. Combining two groups of data obtained at different deformation temperatures led, at a given exponent, to a high value of H0 in Eq. (2) and at a given H0, to a high value of m in Eq. (5). It may be supposed that such a combination of the two groups of data is incorrect. Indeed, it is seen in Fig. 8 that the points corresponding to deformation at room temperature and at the liquidnitrogen temperature are located higher and lower, respectively, than the dependence obtained, and, hence, the dependences for each temperature (Table 2) were constructed individually. The two approaches led to the same corresponding values of the angular coefcient k which in Eq. (1) characterizes the barrier effect of boundaries [10]. The highest coefcient k is obtained in Eqs. (3) and (6). It is known that the nature of boundaries depends primarily on the temperature of their formation; the higher the temperature, the more effectively the boundaries resist to plastic ow and the larger the coefcient k [21, 29]. In the case of room-temperature deformation at a given H0, the value of the parameter m is closer to the value characteristic of the equilibrium granular structure (Eq. (6)). The fact that for low-temperature deformation the value of H0 (Eq. (4)) proved to be smaller than that for 290 K is difcult to explain and may mean that it is illegal to a priori assume the exponent to be equal to 0.5 in the structure with high nonequilibrium
Table 2. Approximating functions for nickel deformed at different temperatures T, K H = f(d0.5) ln(H H0) = f(lnd)

(1)

Two approaches to the calculation of parameters of Eq. (1) exist in literature. According to one of these approaches, the SMC structure formed upon large deformation is similar to a usually grained structure [25]. Based on this supposition, the exponent in Eq. (1) is taken to be m = 0.5 [25, 26]. The other approach stems from the fact that the deformed structure is not granular and the exponent, depending on the fraction of high-angle boundaries and degree of their equilibrium state, can vary from m = 0.5 to 1.0 [8, 10, 27, 28]. In this case, at a given H0 the parameters k and m are found from the linear dependence of ln(H H0) on lnd. The dependences obtained in accordance with these concepts are presented in Fig. 8 and Table 2. It should be noted that these dependences were based on the values of hardness obtained on concrete specimens in the region in which the structure was studied and the sizes of its elements were determined rather than on the averaged values of hardness shown in Fig. 1. Since upon the transition from stage to stage it is only the deformation mechanism that changes (from dislocation slip to rotational modes), while the structure-forming process remains unaltered, it was assumed that for nickel, as well as for pure iron studied in [28], the parameters of Eq. (1) remain unaltered when the stage of mixed structure transforms into the stage of an SMC structure. For this reason, the data on the room-temperature deformation at the stages of mixed and SMC structure was not separated, and the dependence for 80 K corresponds only to the stage of mixed structure. In Eqs. (2)(4) (Table 2) the exponent was taken to be equal to 0.5. Equations (5)(7) are obtained at a
THE PHYSICS OF METALS AND METALLOGRAPHY

Combined H = 1.00 + 1.2d0.5 (2) H = 0.75 + 1.2d0.54 (5) 290 K H = 0.77 + 1.5d0.5 (3) H = 0.75 + 1.5d0.51 (6) 80 K H = 0.66 + 1.1d0.5 (4) H = 0.75 + 1.1d0.52 (7)
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boundaries. Earlier, we established in [28] that good agreement of the analytical dependence with the experimental results (within the error of their determination) is obtained when the exponent is rounded off with an accuracy to the second decimal place. CONCLUSIONS (1) The degrees of deformation leading to transitions between various stages of the structural state in nickel deformed by shear under pressure at 290 and 80 K were determined. It was conrmed that the deformation temperature signicantly affects the mechanism of the structure formation of single-crystal nickel. At room temperature, the formation of a submicrocrystalline structure occurs through the formation and renement of a cellular dislocation structure with a subsequent transition to high-angle misorientations as a result of rotational modes of deformation. In early stages of deformation at the liquid-nitrogen temperature, along with a cellular structure, high-angle misorientations are formed owing to microtwinning and deformation localization at the boundaries of deformation microbands. (2) The formation of microtwins and microbands in nickel at a temperature of 80 K brings about, at the initial stages of deformation, the retardation of growth of microhardness and, with the continuation of deformation, retards the formation of a homogeneous submicrocrystalline structure. (3) Activation of dynamic recovery in the course of deformation at room temperature in the stage of the SMC structure hampers the growth of hardness and renement of microcrystallites. (4) The formation of microbands and twinning upon deformation result in the fact that, at equal sizes of structure elements, nickel deformed at the liquid-nitrogen temperature has a lower hardness than after deformation at room temperature. ACKNOWLEDGMENTS This work was supported by the Russian Foundation for Leading Scientic Schools (project no. NSh5965.2006.3) and by the Program No. 9 of the Presidium of the Russian Academy of Sciences Substance under Extreme Conditions. The electron-microscopic investigation was performed at the Center of Electron Microscopy of the Institute of Metal Physics (Ural Division, Russian Academy of Sciences). REFERENCES
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