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Heat Treatment and Thermo-Mechanical Treatment to Modify Carbide Banding

in AISI 440C Steel: A Case Study

Article in Metallography Microstructure and Analysis · March 2016

DOI: 10.1007/s13632-016-0266-0

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 Heat Treatment and Thermo-Mechanical Treatment to Modify
Carbide Banding in AISI 440C Steel: A Case Study
By
S. Chenna Krishna, K. Thomas Tharian, K. V. A. Chakravarthi, Abhay
Kumar Jha, Bhanu Pant

Citation: S. Chenna Krishna, K. Thomas Tharian, K. V. A. Chakravarthi, Abhay Kumar

Jha, Bhanu Pant. Heat Treatment and Thermo-Mechanical Treatment to Modify Carbide
Banding in AISI 440C Steel : A Case Study. Metallogr. Microstruct. Anal. 5, 108–115
(2016).

Full text available at: http://link.springer.com/article/10.1007%2Fs13632-016-0266-0

1
 Heat Treatment and Thermo-Mechanical Treatment to Modify Carbide
Banding in AISI 440C steel: A Case Study
*S. Chenna Krishna1, K. Thomas Tharian2, K.V.A. Chakravarthi1, Abhay Kumar Jha1, Bhanu Pant1
1
Materials and Mechanical Entity, Vikram Sarabhai Space Centre, Trivandrum-695022, India
2
Materials and Mechanical Entity, Liquid Propulsion Systems Centre, Valiamala-695011, India
*[email protected], phone number: +0471-2563582, fax number: +0471-2705048.

Abstract

In the present case study, simple heat treatment and thermo-mechanical treatment (TMT) are suggested

to salvage AISI 440C steel bars with carbide banding. Optical microscopy, scanning electron microscopy,

and hardness measurement were employed to characterize the steel before and after treatments. The

experimental results indicate that carbide refinement and uniform distribution of carbides can be achieved

by TMT. The hardness of the steel after TMT was higher than 58 HRC in hardened (H1050), cryo-treated

(C-80), and tempered (T180) conditions. This TMT cycle was implemented to produce one batch of rings

free of carbide banding for outer race of ball bearings.

Keywords: AISI 440C steel, carbide banding, thermo mechanical treatment, heat treatment

1. Introduction carbon (0.9-1.1wt %) content of the steel results in

Steels with carbon content in the range of 0.8-1.1 a hard martensite matrix with carbides whereas

wt% were historically used for bearings [1]. 52100 chromium (17 wt %) content imparts corrosion

steel is one such steel extensively being used for resistance [3,4]. Carbides provide improved wear

bearings covering a wide range of industrial resistance, inhibit grain growth and are responsible

applications. However, its application is limited by for the development of desired properties after

poor corrosion resistance due lower content of heat treatment [1,3]. One of the major

chromium [2]. 440C is a high carbon martensitic metallurgical problems reported in the literature for

stainless steel with high hardness of 58-60 HRC such high-carbon steels is carbide banding [2,5]. A

coupled with good corrosion resistance. The high- banded structure can be defined as a segregated

2
structure of approximately parallel bands of two treatment and thermo-mechanical treatment were

different phases aligned in the working direction performed. Specimen cut from the bars were heat

[5,6]. Carbide banding was reported to adversely treated in the temperature range of 900-1150 °C

affect the performance of bearings [7]. The with an interval of 50 °C for a holding time of 1 h

deleterious effect of carbide banding include followed by oil quenching. A tube furnace with an

reduced wear resistance; hard spot and cracking on accuracy of ±10°C was employed to heat treat the

quenching along the carbide bands; reduction in samples. 135 mm diameter ×70 mm height piece

fatigue resistance and premature failure of bearings was subjected to thermo-mechanical treatment in

[5,7]. Parker et al. [8] reported that fatigue life of the temperature range of 1080-950 °C using a

rolling element made from AMS 5749 reduced by 500 T hydraulic press. The piece was subjected to a

four times due to carbide banding. The source and combination of upsetting and drawing operations

essential steps through which carbide banding under flat dies. Samples cut from the thermo-

develop is well documented in the literature [10- mechanically treated work piece were subjected to

14]. However, generalized heat treatment cycles heat treatment cycles shown in Fig. 1. The heat

and thermo-mechanical treatments are not treated and TMT specimens were characterized for

available to salvage the carbide banding. microstructure and hardness. Rockwell hardness

Therefore, an effort has been made to design tester was used to measure hardness in ‘C’ scale.

simple heat treatment and thermo-mechanical An average of six measurements is reported in the

treatment to reduce the carbide banding keeping in paper. Conventional and color metallography was

view production of outer race of bearings. performed to identify the carbides in the steel. Five

2. Experimental procedure etchants used in the study are listed in Table 2.

The steel used in the present study was melted in a Light microscope was used to record the images in

vacuum induction melting (VIM) furnace. Refining dark field and bright field modes. Scanning electron

was done by electro-slag remelting (ESR) followed microscopy was employed to characterize the

by vacuum arc remelting (VAR). The chemical carbides. Samples for optical and scanning electron

composition of the steel in wt % is given in Table 1. microscopy were prepared by conventional

The cast ingot was homogenized at 1100 °C for 12 polishing techniques using different grades of

h and then forged to bars. Forged bars showed emery papers, alumina, and diamond paste. Image

carbide banding and to salvage them, heat analysis software (ImageJ) was used to measure
3
the volume fraction of carbides. Nevertheless, it is rather difficult to differentiate

3. Results and Discussion the carbides using single etchant. Therefore,

3.1 Material different etchants listed in Table 2 were used in

Fig. 2 shows the microstructure of the 135 mm this work. The optical micrographs obtained in the

diameter 440C steel bar in the longitudinal bright and dark field using different etchants are

direction. The optical micrograph clearly shows shown in Fig. 3. Etchant-1 reveals large carbides

carbide bands that appear as bright arrays in dark (M7C3) as dark particles and fine carbides (M23C6)

martensite matrix as shown in Fig. 2. The bands appear as gray particles in bright field (BF) as

mainly consist of primary and secondary carbides shown in Fig. 3a. In dark field (DF), the large and

[6]. The two possible sources of carbides are; (i) fine carbides appear as bright particles in dark

primary carbides (M23C6, MC and M7C3) which form martensite matrix (Fig. 3b). Carbides were

directly from liquid in the inter-dendritic region and selectively etched by etchant-2, large M7C3

(ii) secondary carbides (Mo2C and M23C6) which carbides were fully darkened whereas M23C6

form of solid state reactions [6]. The large primary carbides were dark outlined as indicated by arrows

carbides from the melt do not dissolve at the (Fig. 3c). The same was clear from DF image with

forging temperature and get aligned during drawing bright carbides in dark matrix as shown in Fig. 3d.

operation leading to the formation of bands. The grain structure and carbides could be clearly

However, the severity of banding depends on the revealed using etchant-3. The grain boundaries

size of cast ingot, cast microstructure, and amount and light green carbide bands were visible in BF as

of hot working [6-7]. The volume fraction of the shown in Fig. 3e. On the other hand, M7C3 and

carbides in the bands was measured to be M23C6 appeared as brown and golden-yellow

10.50 %. particles, respectively in DF as shown in Fig. 3f.

3.2 Metallography 3.2.2 Scanning Electron Microscopy (SEM)

3.2.1 Color Metallography The SEM micrograph and corresponding energy

The main constituents of the steel hardened at dispersive X-ray spectroscopy (EDS) spectra from

1050°C from Fe-Cr-C phase diagram (17%Cr the matrix and carbides of the 440C steel in

Isopleth) are austenite, M7C3, and M23C6 [5]. The hardened condition are shown in Fig. 4. SEM

microstructure after quenching consists of micrograph shows morphologically two types of

martensite, retained austenite, and carbides. carbides: large primary carbides and fine secondary
4
carbides in the martensite matrix (Fig. 3a). The EDS with reduction in severity on increase of

spectra of the matrix , large and fine carbides temperature as shown in Fig. 5b-5e. This change in

obtained from spots indicated by letters ‘M’, ‘P’, and microstructure can be explained with the aid of Fe-

‘S’, respectively in the Fig. 4(a) are shown in Fig. Cr-C ternary phase diagram. From the isothermal

4(b)-4(d). The EDS spectrum and quantitative section of phase diagram at 1000 and 1100 °C, the

analysis from ‘M’ show that the spectrum pertains typical content (wt %) of the C and Cr in the

to that of matrix as shown in Fig. 4(b). On the martensite matrix after quenching is 0.3 % and

other hand, spectra from the spot ‘P’ and ‘S’ 11.7 %, and 0.5 % and 13.2 %, respectively [15].

showed prominent peaks of Cr and Fe along with This increase in the carbon and chromium content

Mo peaks as shown in Fig. 4(c) and 4(d), in the matrix will lead to lower volume fraction of

respectively. From the quantitative analysis results, the carbides. In the similar way, volume fraction of

it is suggested that large primary carbides are carbide is further expected to decrease at

(Fe,Cr,Mo)7C3 carbides and fine carbides are temperature above 1050 °C due to dissolution of

(Fe,Cr,Mo)23C6 carbides M7C3 carbides [16]. The typical temperature range

3.3 Heat Treatment for dissolution of M23C6 and M7C3 carbides is 950-

Fig. 5 shows the effect of heat treatment on the 1050 °C and 1050-1150 °C, respectively [16]. The

microstructure (etchant-4) of the 440C steel in the observations made here agree with trend reported

temperature range of 900-1150 °C for holding time for change in volume fraction of carbides with

of 1 h followed by oil quenching. At 900 °C, the temperature in a medium carbon stainless steel

micrograph showed severe carbide banding with (AISI 420). The carbide density was reported as

thick bands as shown in Fig. 5a. With the increase 184 and 14 carbide per mm2 at 1050 and 1150 °C,

in the temperature, the severity of the banding respectively [16]. Even though, severity of banding

reduced to minimum at 1150 °C as shown in Fig. decreases at higher temperature (1050-1150 °C), it

5f. The volume fraction of carbides within the has adverse effect on the prior austenite grain size

bands determined by image analysis was 14 % and and retained austenite. The austenite grain size and

7 % at 900 and 1150 °C, respectively. At 1050 °C retained austenite increase at high temperatures

the volume fraction of carbides was measured to be [7,16]. In addition, quenching from high

10.5 %. In the temperature range of 950-1100 °C temperature sometimes even makes components

the transformation of carbide banding was gradual prone to quench cracks [7].
5
3.4 Thermo-mechanical treatment (TMT) high carbon steels is improper selection of hot

Considering the problems associated with high working operations [7]. In present case, cast billet

temperature heat treatment, thermo-mechanical (350 mm diameter) after homogenization is

treatment (TMT) was performed on a cut piece of subjected to hot working to break the cast

135 mm diameter x 70 mm height. Fig. 6 shows structure and refine the grain size. The

the schematic of TMT cycle employed with a homogenized billet was forged (drawing) from 350

combination of upsetting and drawing operations. mm diameter to 135 mm diameter in the multiple

Work piece was soaked at 1080 °C for sufficient steps. During this process, the large primary

time and subjected to upsetting operation. carbides got aligned and resulted in carbide

Upsetting was performed by reducing the height of banding. Intermediate upsetting would have been

the work piece from 70 to 40 mm (Ø 135 to Ø 195 an ideal choice for fragmentation of large carbides

mm). This was followed by drawing, where the and uniform distribution of carbides. The

height of the work piece was increased from 40 to envisaged use of these 440C was manufacture of

57 mm (Ø 135 to Ø 195 mm). The microstructure ball bearings which includes fabrication of outer

of the TMT work piece in transverse and race, inner race and balls. For the reasons listed

longitudinal direction is shown in Fig. 7. In earlier, 440Csteel with carbide banding cannot be

transverse direction at lower magnification, the used for aerospace applications. As a salvage

microstructure appears to be free of carbide action, keeping in view the fabrication of inner and

banding with uniform distribution of carbides as outer race which involves ring rolling, a simple

shown in Fig. 7a. At higher magnification, operation was inducted into the production

fragmentation of large primary carbides was process. The operation involves upsetting and

observed as indicated by arrows (Fig. 7b). drawing as per the schematic shown in Fig. 6,

Similarly, microstructure in the longitudinal prior to piercing and ring rolling. This combination

direction showed uniform distribution of fine will ensure the fragmentation of the large primary

carbides and fragmentation of large primary carbides which are main constituents of bands. It

carbides as illustrated in Fig. 7c and 7d, also aids in better distribution of fine secondary

respectively. It is interesting to note that after TMT carbides. In this manner, one batch of rings (outer

microstructure in both directions is free of carbide diameter 165 mm X inner diameter 135 mm X

banding. One of the reasons for carbide banding in height 30 mm) were produced to manufacture
6
outer race of bearing which showed better microstructure free of carbide banding and (ii)

distribution of carbides compared to forged bars as minimum hardness of 58 HRC can be achieved by

illustrated in Fig. 8. The microstructure in incorporation of simple thermo-mechanical

transverse and longitudinal direction of the ring treatment cycle.

was free of carbide banding with fragmented 4. Conclusions

carbides as shown in Fig. 8a-8d. Heat treatment and thermo-mechanical treatment

Response to heat treatment was also performed on were employed to salvage the AISI 440C steel bars

TMT samples. Fig. 9 shows the hardness of the with carbide banding. Through the limited studies,

steel after different heat treatment cycles. The heat a simple thermo-mechanical treatment was

treatment cycle for steel consists of hardening, cryo proposed which involves upsetting and drawing

treatment, and tempering. Except high temperature operations to modify the carbide banding in 440C

tempered (HTT) sample (H1050+C-80+T550), steel bars. This treatment was successfully inducted

other samples showed hardness higher than or into the production process and one batch of rings

equal to 58 HRC. The lower hardness in HTT free of carbide banding was manufactured.

sample may be attributed to higher volume fraction Acknowledgement

of austenite due to formation of reverted austenite The authors would like to express sincere gratitude

[17]. The minimum hardness requirement for the to the Dr. K. Sivan Director, VSSC for his kind

steel in hardened and tempered condition is 58 permission to publish this work.

HRC. To summarize, both the requirements: (i)

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steels for bearing applications. Journal of Materials Engineering and Performance.

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5. Hetzner DW, Van Geertruyden W. Crystallography and metallography of carbides in high alloy

steels. Materials Characterization. 2008;59(7):825-41.

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Materials Engineering and Performance. 2000;9(3):286-96.

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John M. Beswick (editor) 1419 (2002): 27-46.

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fatigue life of AMS 5749." NASA-TP-2189 (1983):1–14.

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prevention. 2010;10(5):351-7.

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HY-100 steel. Metallurgical and Materials Transactions A. 2000;31(13):995-1005.

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Materials Transactions B. 2003;34(6):781-92.

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 17. Krishna, S. C., Gangwar, N. K., Jha, A. K., Pant, B., & George, K. M. Effect of Heat Treatment

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List of Tables

Table 1: Chemical composition of the steel

C Cr Mo Mn Ni Si S P Fe Element

0.98 17.2 0.62 0.25 0.02 0.3 0.002 0.003 Bal Wt%

Table 2: List of etchants used in the study

Sl. No Etchant Method

1. 1 g CrO3 and 100 mL H2O (Chromic acid) Electrolytic etch: 2-3 V, 30°C, 30 s

2. 10 g Picric acid, 5 drops HCl, 100 mL Ethanol Immersion: 15-60 s, 30°C

or Methanol

3. 10 g Ammonium persulfate, 100 mL H2O Electrolytic etch: 6 V, 30°C, 20 s

4. 8 cc HNO3 + 92 cc Ethyl alcohol (8 % Nital) Immersion: 10-15 s, 30°C

5. 5 g Picric acid + 100 cc Ethyl alcohol (5 % Immersion: 15-20 s, 30°C

Picral)

9
List of Figures

Fig. 1: Heat treatments performed on the thermo-mechanically treated samples

Fig. 2: Optical Micrographs of the steel (135 mm diameter bar) showing the carbide band (etchant – 5 %
Picral)

10
Fig. 3: Optical micrographs of the steel etched with different etchants (a) etchant-1 (bright field); (b)
etchant-1 (dark field); (c) etchant-2 (bright field); (d) etchant-2 (dark field); (e) etchant-3 (bright field) ;
(f) etchant-3 (dark field)

11
Fig. 4: SEM micrograph and corresponding EDS spectrum of the steel in hardened condition (a) SEM
micrograph; (b) EDS spectrum of the matrix ‘M’ in Fig. 3(a); (c) EDS spectrum of particle ‘P’ in Fig. 3(b);
(d) EDS spectrum of particle ‘S’ in Fig. 3(a).

Fig. 5: Optical micrographs of steel subjected to different heat treatment (a) 900 °C; (b) 950 °C; (c)
1000 °C; (d) 1050 °C; (e) 1100 °C and 1150 °C (etchant – 8 % Nital)

12
Fig. 6: Schematic of thermo-mechanical treatment cycle employed

Fig. 7: Optical micrographs of the steel after TMT (a) Longitudinal (lower magnification); (b) Longitudinal
(higher magnification); (c) Transverse (lower magnification) and (d) Transverse (higher magnification),
Arrow pointing fragmented primary carbides (etchant – 8 % Nital)

13
Fig. 8: Microstructure of the steel ring (OD 165 mm X ID 135 mm X Height 30 mm) in transverse and
longitudinal direction: (a) transverse direction (lower magnification), (b) transverse direction (higher
magnification), (c) longitudinal direction (lower magnification), and (d) longitudinal direction (higher
magnification) (etchant – 5 % Picral)

14
 Fig. 9: Hardness of the thermo-mechanically treated samples in different heat treatment conditions

15

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