Formation Pattern

of Ridging of Cr and

Related

to the

Banded

Segregation Sheet*

C on Ferritic

Stainless

Steel

By Keijiro SUZUKI,** Shozaburo

ASAMI*** and Kaxuyoshi

SUZUKI***

Synopsis Ridging phenomenonis a surface defect undesirablefor deep drawing applications of ferritic stainless steels. Stripe pattern is frequently observed parallel to the rolling direction and appears as narrow banded areas when the strip or sheet of these steels is severely etched. In the present paper, correlation of the ridging and the stripe pattern was discussed, and the origin of the stripe pattern was examined in 18 % Cr stainless steel sheet. It is shown that there is a close resemblancebetween the stripe pattern and the ridging in terms of the periodicity, the directional characteristics, and the nature of the macro- and microscopic structural compound. The stripe pattern has its origin in the hot rolling stage when partition of Cr and C in a and r phase proceeds. Debris of r particles is retainedwith depletionof Cr in the elongated form in thefinal product. Local variation of Cr content results in the development the stripe pattern. of

I.

Introduction Ferritic stainless steels, in particular 18 % Cr steels, are widely used in furniture, household appliance, and automotive parts as cheap alternatives for their Ni-bearing counterparts. Because of such decorative applications, the surface appearance of articles formed from the sheet steels is an important factor for evaluating the material performance. There is a serious drawback to the use of 18 % Cr stainless steel sheets for deep drawing applications to suffer ridging or roping phenomena on the surface of the drawn parts. Ridging is considered to be unsightly surface defect in the form of corrugations resulting from stretching operation, and removal by grinding or polishing increases the production cost. A number of studies have been carried out on the mechanisms of ridging and it has been a subject of several patents on the methods to eliminate or to reduce ridging phenomena. Ridging is known to have the following characteristics. (1) Appearance of ridging is related to the development columnar structure during solidification of the steel ingots-3) and the distribution of martensite4,5)or ferrite band6) forming banded structure in the hot rolled sheet. (2) Ridging is considered as an anisotropic plastic flow caused by a combination of high r-valued {l1l} and low r-valued {100} orientations in the recrystallization textures4-13) of final products. (3) Ridging is reduced by refinement of ferrite grains with addition of Ti or Nb to fix carbon in the form of carbide and to promote extensive nucleation of recrystallized grains.l4)
. **

So far mechanisms of ridging have been thought on the basis of combinations and distributions of particular crystallographic orientations. However, ridging has been observed remarkably on a low carbon 18 % Cr stainless steel sheet prepared to have a crystallographic orientation of exclusively very sharp {l1l} <112> and a fine grain structure of the order of several microns.l5) This combination of the texture and the grain structure is favorable for elimination of ridging from the conventional viewpoint. Therefore, main factors of ridging are considered to be not limited to the grain size and crystallographic orientation. In this connection, stripe pattern appear parallel to the rolling direction on the surface of 18 % Cr stainless steel sheets which were subjected to chemical etching. The relation between the stripe pattern caused by corrosion and ridging, and the origin of stripe pattern have been discussed in terms of the inhomogeneities of recrystallization textures in the sheets.5,10,12) However, the origin of inhomogeneities parallel to the rolling direction. So, the present authors consider that the difference of corrosivity to form the stripe pattern occurs by the segregation Cr and C, because, obviously from the phase diagram of Fe-0.05%C-Cr system, 18 % Cr stainless steel has an (a+r) two-phase region in the hot rolling stage. In this paper, the stripe pattern produced by corrosion was observed on the surface of 18 % Cr stainless steel products in the conventional process in details to get a correlation between the ridging and the stripe pattern. The origin of stripe pattern was discussed in terms of the difference of corrosivity produced by the partition of elements in (cc two-phase structure formed +r) during hot rolling. II. Experimental Method and Result Starting material was a commercial semi-product of JIS type SUS430 processed by annealing, and pickling. The thickness of the sheets is 3.6 mm and the chemical composition is shown in Table 1. 1. Ridging Final products of cold-rolled 18 % Cr stainless steel sheets, skinpass-rolled after bright annealing (BA)

vrlginaiiy pu oiisnea in 1 etsu-io-rragane, u. ~i y i I), ooo, in Japanese. iingiisn version receivea July o, 1 'oh. ) 15o3 ii j Formerly Faculty of Engineering , The University of Tokyo. Now at Kogakuin-Daigaku Senmon Gakko, Nishi Shinjuku, Shinj ukuku, Tokyo 160. * ** Research and Development Center , Takasago Tekko Co., Ltd., Shingashi, Itabashi-ku, Tokyo 175.

Research

Article

(731)

(732)

Transactions

ISIJ,

Vol.

23,

1983

Table

1.

Chemical

composition

of

steel

used.

(wt%)

Fig.

1.

Surface on Photo.

profiles 1.

of the

temper

rolled

sheets

shown

Photo.

1.

Distortion of reflection image of a straight line caused by surface corrugation due to ridging after temper rolling of bright annealed 18 % Cr stainless steel sheet products.

or annealing and pickling (AP), have excellent surface luster. However, when a black straight line drawn on a white paper was reflected by a stainless steel sheet, the reflected image is distorted by existence of ridging on the sheet. Distortion of reflected image in the commercial SP (finished by skinpass-rolling) products of SUS430 is shown in Photo. 1 for severe ridging in (a), moderate ridging in (b), in comparison with non ridging in SUS304 product. Beautiful appearance is damaged when the reflected image is distorted by the severe ridging as in the case of Photo. 1(a), while it is preserved in the case of Photo. 1(b) or (c). The intervals of distortions were nearly equal for the severe and the moderate ridging as shown Ira and Irb in Photos. 1(a) and (b). Figure 1 shows the irregularity of surface in each stainless steel sheet measured with the roughness meter by scanning vertical to the rolling direction. The surface profile of SUS304 which is free from ridging and produces the straight image is as shown in Fig. 1(c). The surface profiles of SUS430 are corrugated with a wave length of about 1 mm (illustrated as Iwa and Iwb) as shown in Figs. 1(a) and (b). The height of wave was 0.4 p for the severe and 0.2 p for the moderate ridging. Close agreement was obtained between the intervals (Iw) or heights of wave

Photo.

2.

Appearance cup. tions the

of ridging L and and

on

the

wall in the

of a deep respective

drawn posiof disc.

Locations parallel sheet with

T are

vertical to the

to the center

rolling of the

direction blank

regard

and the intervals (Ir) of distortions of reflected image as shown in Photo. 1 in conformity with visual inspection. Thus, it is considered that the waves as shown in Figs. 1(a) and (b) distort the reflected images. The ridging was observed in hot- and cold-rolled 18 % Cr stainless steel sheets and also in materials as treated with BA or AP. The ridging was also observed on the wall and flange of deep drawn cylindrical cup as shown in Photo 2. Ridging occurs all around the wall of a deep drawn cup, always running parallel to the rolling direction of the sheet as shown in Photo. 2. The ridges appear bright because of abrasion during drawing operation. The enlarged images and surface profiles of ridging in Photo. 3 for particular locations L and T which are in the respective positions parallel and vertical to the longitudinal direction of the sheet with respect to the center of the blank disc. The amplitude of the macroroughness due to ridging is about 12 p in the location L and between about 7.5 ii and 4 with gradual decrease from the

Transactions

ISIJ, Vol.

23,

1983

(733)

1C:

Period cup 3.

of ridging

on the deep drawn

Photo. Enlarged

views

at the location their

L and

in Photo. 2 and surface profiles.

corresponding

flange to the top in the location T. The period of the ridges, shown as 'ca and I~bin Photo. 3, is about 1.0 to 1.5 mm independent of the locations and nearly equal to that of the surface corrugation after tensile deformation shown in Fig. 1. In the present experience, quantitative determination of the surface profile of ridging was made by scanning a surface roughness-meter on the tensile specimen strained 20 %. The patch of the profilometric measurement is always vertical to the rolling direction of the sheet. 2. Stripe Pattern Stripe pattern was revealed on the surface of final product, as shown in Photo. 4 in the increasing order of magnification, by etching with aqueous solution of 30 % nitric and 3 % hydrofluoric acid for 2 min at 80 C. The product was processed by two cycles of cold rolling with reduction of 50 % and annealing at 800 C for 10 min as a simulation of the conventional production. The stripe pattern appears as an alternation of bright and dark etched bands with a width of about 1.0 to 1.5 mm at a low magnification (Photo. 4(a)). The macroscopic dark band was found to consist of an aggregate of microscopic fine bands with a width of 20 to 200 ,um at a higher magnification (Photos. 4(b) and (c)). The macro- and microscopic bands are to be designated as types A and B patterns hereafter. Transition from bright to dark area in the type B pattern is fairly clear and often passes through grain interior. The stripe pattern is also observed in the as hot or as cold-rolled sheet by electrolyzing in 30 % nitric acid aqueous solution or 10 % phosphoric aqueous solution. 3. Stripe Pattern and Ridging In order to correlate the stripe pattern with ridging phenomena, tensile specimens were etched in nitric fluoride aqueous solution at 80 % before tensile testing. Sampling procedure was shown in Fig. 2: two types

Photo

4.

Macroscopic stripe pattern (type A) consists of an aggregate of microscopic stripe pattern (type B).

of specimens were prepared to set the tensile direction parallel or vertical to the rolling direction and two points were marked 10 mm apart on a line vertical to the rolling direction of each specimen for duplica-

Research

Article

(734)

Transactions

ISIJ, Vol.

23,

1983

Fig . 2.

Procedure

of sampling

for tensile

specimens.

tion of the profilometric scanning before and after tensile deformation. The stripe pattern was shown in Photos. 5(a) and 6(a) for two types of specimens. Ridging occurs parallel to the rolling direction independent of the tensile direction after straining up to 20 %. By phase-contrast microscopic observation of the ridges, the macroscopic ridges (denoted by type A in Photos. 5(b) and 6(b)) were found to consist of microscopic ridges (denoted by type B in Photos. 5(b) and 6(b)). As shown in Photos. 5(c) and 6(c), average amplitude of the ridges of type A is about 9.4 j,i and 5.0 p for tensile deformation parallel and vertical to the rolling direction respectively, which is consistent with ranking of ridging by visual inspection. The microscopic ridges of type B have an amplitude of about 4.0 p for the longitudinal and about 3.0 e for the transverse deformation. Period of the ridges is about 1.0 to 1.5 mm for type A (Ita) and about 0.1 to 0.3 mm for type B (Itb) independent of the tensile direction. Appearance and surface profile after tensile deformation are essentially the same to those of the temper-rolled sheet (Fig. 1) and the deep drawn cup (Photo. 3). Thus it is shown that there is a close resemblance between the stripe pattern and the ridging in terms of the periodicity, the directional characteristics, and the macro- and microscopic structural compound.

Photo.

5.

Correlation of the stripe pattern with the macro(type A)- and micro-(type B)-roughness due to ridging formed in longitudinal deformation.

Photo.

6.

Correlation and verse

of

the

stripe due

pattern to ridgin

with g formed

the in

macrotrans-

microroughness deformation.

Transactions

ISI1, Vol.

23,

1983

(735)

4.

Partition of Alloying Elements betweena and r Phases As evident from the phase diagram of Fe-Cr alloy in Fig. 3, the present material has two phase structure of a and r in the temperature range of 95O1 350 C. In order to study partition of alloying elements between the two phases, the hot-rolled sheet was heated up to 1 300 C for 2 hr and quenched into water. The microstructure of the quenched sample was revealed by etching in picric acid-hydrochloric acidalcohol solution as shown in the upper part of Photo. 7. Differentiation of the two phases was made by means of hardness measurement with micro Vickers tester (500 g). The hard phase, designed to be aM, has a hardness Ho=565 and the soft phase, a, Ho= 145. The chemical composition of each phase was analyzed by linear scanning mode with EPMA. Enrichment of C and Fe and depletion of Cr in the aM phase are confirmed as shown in the lower part of Photo. 7 and the left column of Table 2.

Since the as-quenched specimen could not be successfully cold rolled owing to the presence of the hard aM phase, the specimen was annealed at 800 C for 10 min for further processing. Photograph 8 shows structural changes of a hot-rolled sheet after heating at 1 300 C followed by quenching and annealing at 800 C. Heating at 1 300 C destroys the stripe pattern formed in hot-rolled sheet and produces coarse a+aM structure. Annealing at 800 C
Table 2. Structures specimen at and each chemical experimental compositions process. of

Fig. 3.

Phase diagram of Fe-0.05%C Bungard et al.ls)).

-Cr

alloy

(after K.

Photo.

7.

Microstructure chart of linear

after analysis

quenching by EPMA.

from

1 300 C and
Photo. 8. Microstructural changes with processing.

Research

Article

(736)

Transactions

ISIJ, Vol. 23, 1983

induce no substantial changes in microstructure. However, it lowers the hardness of aM phase down to Hv=245 and reduces the resistance to corrosion to be etched much more darkly. The tempered aM phase is to be denoted as aM hereafter. Partition of Cr and C between the phases is hardly homogenized as shown hi the middle column of Table 2. Microstructural and Compositional Changes in Cold Rolling and Annealing Stage The hot-rolled and annealed specimen was processed by a series of cold reduction with 50 % and annealing at 800 C for 10 min in two stages. Microstructural changes in the processing are shown in Photo. 9. Starting microstructure consists of bright etched a and dark a'Mphase. After the first stage of cold rolling and annealing, c particles remain without decomposition only to be elongated in the cold rolling direction (Photo. 9(b)). In the final product debris of a' particles is observed aligning parallels to the rolling direction. The debris will be tentatively designated a2 and the matrix of recrystallized structure al. Average hardness of a1 and a2 phase is Hv=138 and 176, respectively. The chemical composition of each phase was analyzed with EPMA by linear scanning along a line indicated on Photo. 10 and shown in the right column of Table 2. III. Discussion Stripe pattern is formed parallel to the rolling direction because of local difference in corrosivity by etching a cold-rolled and annealed product of 18 % Cr stainless steel. The period of dark and bright etched bands in the stripe pattern is well coincident with that of the macroroughness due to ridging. This suggests a close corelation between the stripe pattern and the ridging phenomenon. Therefore it is attempted to study the stripe pattern for its origin of the local difference of corrosivity and the directional characteristics. Origin of the stripe pattern has been discussed in the previous reports5,1o,12)mainly in terms of the local variation of orientation relevant to the ridging formation. The difference in orientation has been considered to originate from the macro-band of ferrite6~ or martensite5~ formed in the hot rolling stage or from the columnar structure developed during solidification.'-3) In the present observation, however, the boundary of microscopic stripe pattern which divides the dark and bright bands often crosses grain interior. This suggests another possibility of the difference in corrosivity besides orientation. It is well known that the resistance to corrosion of ferritic stainless steels differs in accordance with the Cr content. In 18 % Cr stainless steel partition of Cr and C between a phase and r phase proceeds in the a+7' two phase region between 950 C and 1 350 C as evident from the phase diagram of Fe-0.05%C-Cr alloy.16,1'~ Conventional hot rolling procedure involves heating to and rolling in the two phase region. Therefore it 5.

`V/ Photo. 9.

1aL41J1 ~Jl..l,Vlll.4U{.bV \iVlu LVlllll~ changes in cold rollin

11l.4

1L111,.11110

Microstructural

g and

annealing.

Photo.

10.

Linear annealed

analysis

of c hemical

composition

in the

final

specimen.

is probable to arise local variation of Cr content which leads to the difference in corrosivity, as a consequence of partition of alloying elements in the hot rolling stage. A dual phase structure of a and aM was produced, when a hot rolled sheet was quenched from the two phase region. The hard aM particles with a hardness

Transactions

ISIJ,

Vol.

23,

1983

(737)

In the conventional process the transformation products of r are ferrite and chromium carbide. The difference of the nature of transformation product from the conventional process may not affect the essential points of the present results, however, it remains a further problem for study. Conclusion The stripe pattern which appears on the surface of 18 % Cr stainless steel sheet product parallel to the rolling direction by chemical etching is correlated with the characteristics of ridging phenomena. (1) The period of dark and bright etched bands in the stripe pattern is coincident with that of the macroroughness due to ridging. (2) The stripe pattern is formed by the difference in corrosivity caused by local depletion of Cr. (3) Partition of Cr and C occurs in the hot rolling stage. The debris of r particle remains in the final product to be elongated parallel to the rolling direction and susceptible to corrosion attack owing to the poor Cr content.
REFERENCES
Fig. 4. A model for of processing

Iv.

formation of stripe pattern in the 18 % Cr stainless steel sheet.

of Hv 565 are enriched in C, suggesting a martensitic transformation product of r. Tempering of the quenched sample reduces the hardness and the resistance to corrosion of the aM particles. 18 % Cr stainless steel sheet for deep drawing application is usually processed by a series of cold rolling and annealing in two stages. The debris of aM particles in hot rolled sheet still remains in the final annealed product. The adverse partition of Cr and C which is formed in the hot rolling stage and inherited in the product induces a local difference in passivity in a corrosive atmosphere.18_20) The transformation product of r phase poor in Cr and rich in C is more susceptible to corrosion than the matrix, which leads to the formation of the stripe pattern. A model for development of the stripe pattern running parallel to the rolling direction is schematically shown in Fig. 4. The particles of r phase are formed in the slab heated in the two phase temperature region, elongated parallel to the rolling direction in hot rolling and transformed into aggregates of aM particles. The aM particles are further elongated by cold rolling to be a2 particles. The a2 particles is responsible for the microscopic stripe pattern of type B.

1) K. Kawahara : J. Japan Inst. Metals, 38 (1974), 440. 2) K. Kawahara : J. Japan Inst. Metals, 38 (1974), 731. 3) K. Kawahara : J. Japan Inst. Metals., 38 (1974), 1059. 4) M. Arakawa, K. Shimizu, T. Sawatani and K. Ooka : Tetsu-to-Hagane, 58 (1972), 5480. 5) H. Miyaji and S. Watanabe: J. Japan Inst. Metals, 39 (1975), 194. 6) N. Ohashi : J. Japan Inst. Metals, 31 (1967), 549. 7) I. Gokyu, K. Suzuki and S. Ino: J. Japan Inst. Metals, 34 (1970), 516. 8) I. Gokyu, K. Suzuki, S. Ino and K. Shimizu : J. Japan Inst. Metals, 34 (1970), 520. 9) M. Hamazaki, I. Gokyu and S. Okamura: J. Japan Inst. Metals, 33 (1969), 1017. 10) M. Hamazaki, I. Gokyu and S. Okamura: J. Japan Inst. Metals, 34 (1970), 569. 11) H. Takechi, H. Kato, T. Sunami and T. Nakayama : J. Japan Inst. Metals, 31 (1967), 717. 12) H. C. Chao: Met. Trans., ASM, 60 (1967), 37. 13) H. C. Chao : Met. Trans., 4 (1973), 1183. 14) T. Thompson and J. L. Lamont: Proc. Elect. Fur., 19 (1961), 70. 15) K. Suzuki : TTetsu-to-Hagane, (1976), 5226. 62 16) K. Bungard, E. Kunze and E. Horn: Arch. Eisenhuttenw., 29 (1958), 193. 17) T. Sawatani and K. Shitani : Tetsu-to-Hagane, 55 (1969), 1255. 18) H. P. Leckie and H. H. Uhlig: J. Electrochem Soc., 113 (1966), 1261. 19) N. G. Green and M. G. Fontana: Corrosion, 15 (1959), 25 t. 20) G. Wranglen: Corros. Sci., 9 (1969), 585.