2012 American Transactions on Engineering & Applied Sciences.

2011 American Transactions on Engineering & Applied Sciences

American Transactions on Engineering & Applied Sciences

Influence of Carbon in Iron on Characteristics of Surface Modification by EDM in Liquid Nitrogen

a*

Department of Industrial Engineering Faculty of Engineering, Thammasat University, THAILAND Department of Mechanical Engineering Faculty of Engineering, Nagaoka University of Technology, JAPAN
b

ARTICLEINFO
Article history: Received 23 August 2011 Received in revised form 23 September 2011 Accepted 26 September 2011 Available online 26 September 2011

A B S T RA C T

Keywords: EDM, Surface modification Titanium nitride, Liquid nitrogen.

Many surface modification technologies have been proposed and carried out practically by CVD, PVD et.al. Carbonized layer has been made using EDM method. In this paper, to make the nitride layer by EDM some new trials were carried out using a titanium electrode in liquid nitrogen. Experiments were carried out on carbon steel (S45C), pure iron and cast iron. TiN can be obtained on EDMed surface. Moreover, TiCN can be found on cast iron and steel (S45C) by XRD investigation. To confirm the fabrication mechanisms of modified layer on the steel, the following experimental factors were investigated by EDS. 2012 American Transactions on Engineering & Applied Sciences.

1. Introduction
Many surface modification technologies have been proposed and carried out practically by CVD, PVD et.al. Surface modification by EDM have been succeeded to make the modified layer
*Corresponding author (A.Muttamara). Tel/Fax: +66-2-5643001 Ext.3189. E-mail address: [email protected] 2012 American Transactions on Engineering & Applied Sciences. Volume 1 No.1 ISSN 2229-1652 eISSN 2229-1660 Online available at http://TUENGR.COM/ATEAS/V01/41-55.pdf

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i.e. TiC, Si, WC etc. on the work piece by EDM method (N.Saito et.al.,1993). In this method, the carbon element that is supplied from the dissolution phenomena of working oil during discharges reacts with the electrode element of Titanium. When the compacted powder body used as an electrode, TiC products piled up easily on the steel surface. On the other hand, the surface modified TiN can be achieved with titanium electrode in liquid nitrogen. (Muttamara et al.,2002). Biing Hwa Yan et al., 2005, carried out EDM in urea solution in water with Ti electrode and obtained TiN machined surface. It is interesting that carbon come off by reverse diffusion from the workpiece to the recast layer (Marash et al., 1965). Therefore, the surface modified TiN and TiCN layers have attracted interest for workpiece materials which have high carbon content such as carbon steel and cast iron. Although hardness of TiN layer is lower than TiC layer but friction co-efficiency of TiN layer is quite stable and quite low. In this paper, a new modification method of nitride modified layer on steels by EDM in liquid nitrogen using a titanium electrode is proposed.

2. Experimentalprocedure
Figure 1 shows the illustrated experimental set up. The machining was carried out in liquid nitrogen on carbon-steel (S45C), pure iron and cast iron. Cylindrical Ti solid was applied as an electrode. Table 2 shows chemical composition of S45C. Table 3 shows chemical composition of pure iron and cast iron. The discharge waveforms were observed with a current monitor to analyze the discharge phenomena on this machining.

Control circuit
Electrical power source

Current Detector Oscilloscope Vessel Ti electrode Liquid Nitrogen

Ground

Workpiece

Figure 1: Experimental Set up for EDM in liquid nitrogen.

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Apiwat Muttamara, and Yasushi Fukuzawa

Table 1 : Properties - PVD coating Datasheet. Coating Material TiN TiC TiCN Gold Grey Blue Gray Perple Good general purpose High hardness High hardness, good wear resistance, enhanced toughness Colour Key Characteristics Hardness (Vickers) 2300 3500+ 3000 Maximum Working Temperature 600C TBD 400C Friction Coef
(on dry steel)

0.4 >0.1 0.4

Table 2 : Chemical composition of S45C (mass%) C 0.45 Si 0.2 Mn 0.77 P 0.17 S 0.25 Fe Bal.

Table 3 : Chemical composition of pure iron and cast iron (%) Workpiece Pure iron Cast Iron C (%) <0.005 2.11-4.5 Si (%) 0 3.5 Fe Bal. Bal.

Table 4 : The experiment conditions Parameters Polarity (Electrode) Current (A) On-time (s) Duty factor (%)
Open circuit voltage, ui (V)

Values
10, 47 32,512 11,50 220 40 500

Water pressure (kg/cm2) Spindle speed (rpm)

*Corresponding author (A.Muttamara). Tel/Fax: +66-2-5643001 Ext.3189. E-mail address: [email protected] 2012 American Transactions on Engineering & Applied Sciences. Volume 1 No.1 ISSN 2229-1652 eISSN 2229-1660 Online available at http://TUENGR.COM/ATEAS/V01/41-55.pdf

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The machining characteristics are estimated in terms of surface roughness, Vickers hardness, surface layer thickness, X-ray diffraction pattern, EPMA and EDS analysis. The machining conditions are shown in Table 4. The special vessel was designed by polystyrene material for the machining in the liquid nitrogen.

3. Resultsanddiscussions
At room temperature, liquid nitrogen holds as a boiling state in the vessel. It is known that when the discharge occurs in boiled working medium, the machining phenomena are affected by the bubble generation and the a few discharges contribute to the machining state. Further, exploding the vapor bubble and causing the molten metal to difficult be expelled from the workpiece so that only piling process occurs without machining process. To investigate the pulse discharges in liquid nitrogen, discharge waveforms were observed. Figure 2 shows the discharge waveforms in liquid nitrogen. The detailed waveforms were indicated as A` and A line in Figure 2, are shown in Figure 3. The experiments of EDM were performed on the surface of S45C. Machining conditions were as follows: negative polarity, ie=10A, te=32s, D.F.=50%. There are 4 types waveforms: (a) normal, (b) short, (c) concentrate, (d) short eliminated current. Due to liquid nitrogen holds as a boiling state, therefore EDMed in liquid nitrogen requires a time to break down into ionic (charged) fragments, allowing an electrical current to pass from electrode to workpiece. This region was named as an ignition delay time. Many shorts and concentrate discharges occurred in this process. It can be explained that the sludge was made by the gathering debris phenomena in the gap space during the short circuit and piled on the machined surface during ignition delay time. When the electrode touches the workpiece through the sludge, the concentration of discharge pulse and short circuit occurs. It assumed that the surface modified layer was fabricated by these special discharge phenomena. When short occurs in EDM, it tends to continue long time such as several 100ms from several 10ms. To solve the problem, our EDM system automatically lunches eliminate current to the process (Goto A.et al.,1998). As Figure shows, during off-time it is checked whether gap is short, next pulse is eliminated.

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Apiwat Muttamara, and Yasushi Fukuzawa

Ignition delay time Voltage 80V 0V

A A

Eliminate current Current 1 0 Time 0.5ms/div Figure 2: Discharge waveforms in liquid nitrogen. Discharge voltage (ue)= 15V Voltage 80V. 0V.
A

Short

Concentrate Normal
A

Current

10 0A 50 s/div

Figure 3: Normal discharge and concentrate discharge in period A` A.

3.1 Effectofelectrodepolarity
On the normal EDM, the positive (+) electrode polarity is chosen for the machining (Janmanee P. and Muttamara A.,2011). On the contrary, the negative polarity (-) often uses for the modified technology (N.Saito et.al.,1993), (Muttamara et al.,2004), and also machines for insulating ceramic materials (Muttamara et al.,2009-2010). These experiments were done under the

*Corresponding author (A.Muttamara). Tel/Fax: +66-2-5643001 Ext.3189. E-mail address: [email protected] 2012 American Transactions on Engineering & Applied Sciences. Volume 1 No.1 ISSN 2229-1652 eISSN 2229-1660 Online available at http://TUENGR.COM/ATEAS/V01/41-55.pdf

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following machining conditions: ie=10A, te=32s, D.F.=11.1% with Ti solid electrode of5mm. Figure 4 shows the shape of electrical discharge marks from a single pulse electrical discharge experiment in which all other conditions are identical, and only the polarities are changed.

a) Positive

b) Negative

Figure 4: Single crater created by a) positive and b) negative polarity. It can be seen that in the case of negative polarity, large amounts of the melted electrode implant to the workpiece. In comparison, in case of positive, a relatively clean surface crater is formed. Judging from the result, the negative polarity was selected.

3.2 EDMonS45C
To study characteristics of modified layer, the cross sectional of nitride product modified layer on S45C was observed by laser microscope and EPMA analysis. Figure 5 (a),(b) and (c) show the cross sectional EDMed surface by laser microscope, EPMA map analysis and EPMA line analysis of cross sectional EDMed surface, respectively. The golden colored layer could be observed on the machined surface. The characteristics of the modified layer were investigated by the micro-hardness Vickers using a load of 10gf and the EPMA analysis. Figure 6 shows micro-hardness distribution on the cross section of modified layers with solid and semi-sintered. (ie=10A., te=32s, D.F.=11.11%). On the machining of Ti solid electrode, there were three areas: (1) nearest surface region, 0-50 m, the hardness reached to 1300HV that corresponded almost to the same value of other report (table 3.1), (2) thermal affected region, 50-100 m: similar hardness of martensite structure of 800HV, (3) original substrate region: over 100 m. On the contrary, the hardness of region (1) became the same value, 800HV at region (2) on the machining of semi-sintered electrode. 46
Apiwat Muttamara, and Yasushi Fukuzawa

EPMA analysis of Ti, N and C, was carried out on the cross sectional modified surface. The distribution of Ti and N element was divided to three regions same as Figure 5. The distribution of Ti and N element was detected from region (1) to (2). It indicated that the region composed with the thermal affected structure of substrate and the diffused TiN products. In the (1) and (2) region, the higher carbon element was observed than matrix regardless no supplying source around discharge circumstances. Because carbon was observed on the modified layer on S45C. It was thought that carbon come off by reverse diffusion (Barash et al.,1965). Line analysis Area Modified layer

40

a) Modified layer on S45C in liquid nitrogen

b) EPMA Map analysis Modified layer on S45C in liquid nitrogen continue Figure 5 on next page
*Corresponding author (A.Muttamara). Tel/Fax: +66-2-5643001 Ext.3189. E-mail address: [email protected] 2012 American Transactions on Engineering & Applied Sciences. Volume 1 No.1 ISSN 2229-1652 eISSN 2229-1660 Online available at http://TUENGR.COM/ATEAS/V01/41-55.pdf

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Int (Count) Ti N 1600 240 C 40

T N

Modified layer

800

120

20

C
0

Distance from top surface (m) c) EPMA Line analysis

50

100

150

250

Figure 5: Cross sectional image of TiN layer on S45C by a) Laser Microscope b) EPMA Map analysis c) EPMA Line analysis.

Modified layer Hardness (HV)

50

100

150

200

Distance from top surface (m) Figure 6 : Relationship between micro-hardness Vickers against the cross section of modified layer on S45C.

3.3 EDMonPureiron
Pure Iron does not contain carbon (less than 0.005%). The concentration of substances on the cross section of modified surface on pure iron were carried out with Ti solid. Figure 7 shows cross sectional SEM of EDMed surface on pure iron compared with EPMA results. Figure 8 shows the sectional micro-hardness measurements of modified surface. The thickness of modified layer is 100 m as same as the modified layer on S45C. From the sectional micro-hardness result, 48
Apiwat Muttamara, and Yasushi Fukuzawa

hardness of modified surface is 600-800 HV. The hardness of modified layer on Fe is lower than that on S45C. This is considered that carbon in the material of S45C affect to the compound of modified layer.
Int (Count) Ti 600 300 N 800 400 C 20 10 N

Ti

Modified layer

100 m Line analysis a) SEM of TiN layer on pure iron

0 100 200

Distance from top surface (m)

b) EPMA Line Analysis

Figure 7: Cross sectional TiN layer on Fe a) SEM and b) EPMA Line Analysis

1000

Modified layer

Hardness (HV)

800 600 400 200 0

100

200

300

400

500

Distance from top surface (m) Figure 8: Micro-hardness distribution (EDM Conditions; ie=47A, te=256s, D.F.= 11.1%).

3.4 EDMoncastiron
Cast iron was used to confirm (reverse) diffusion of carbon. In this experiment, discharge current (ie)=47A, discharge duration (te)=256s, (D.F.)=11.11%, were selected for EDMed condition. Figure 9 shows cross sectional SEM of EDMed surface on cast iron compared with EPMA results. Figure 10 shows the sectional micro-hardness measurements of modified surface.
*Corresponding author (A.Muttamara). Tel/Fax: +66-2-5643001 Ext.3189. E-mail address: [email protected] 2012 American Transactions on Engineering & Applied Sciences. Volume 1 No.1 ISSN 2229-1652 eISSN 2229-1660 Online available at http://TUENGR.COM/ATEAS/V01/41-55.pdf

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Int (Count) Ti 600 300 N C

800 20 400 10

Ti

Modified layer

N 100 200

100 m Line analysis a) SEM of TiN layer on cast iron

Distance from top surface (m)

b) EPMA Line Analysis

Figure 9: Cross sectional TiN layer on cast iron a) SEM and b) EPMA Line Analysis

Modified layer
1000

Hardness (HV)

800 600 400 200

100

200

300

400

500

Distance from top surface (m) Figure 10: Micro-hardness distribution (EDM Conditions; ie=47A, te=256s, D.F.= 11.1%)

The C and N elements concentrations are measured on the modified layer, distance of the generation of C and N elements are 250 m of modified layer as can seen from the Figure 9. First, it should be noticed that system experiment was decarburizing. So carbon on modified layer should come from the precipitated graphite in the cast iron. However, we cannot see clearly on EDS result of carbon. Etching was done on cross section surface of cast iron as shown in Figure 11.

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Apiwat Muttamara, and Yasushi Fukuzawa

(1)

HAZ

(2)

(1)

(2)

20 m

20 m

Figure 11: SEM micrographs of etched cross section surface of cast iron The low part represents the base material, the central part in the curve mark represents the base material that effect from heat affected zone (HAZ), and carbon diffused zone. The modified layer was generated irregularly. The dendritic parts in substrate are graphite exist in the form of flakes. It is pointed out that some areas inside close line carbon are depressed. The large scale of structure
*Corresponding author (A.Muttamara). Tel/Fax: +66-2-5643001 Ext.3189. E-mail address: [email protected] 2012 American Transactions on Engineering & Applied Sciences. Volume 1 No.1 ISSN 2229-1652 eISSN 2229-1660 Online available at http://TUENGR.COM/ATEAS/V01/41-55.pdf

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under modified surface is shown in Figure 11 (a) Also the structure of normal graphite in cast iron is shown in Figure 11 (b). The presences of graphite in HAZ (a) are different from normal content (b). Therefore, it is considered that precipitated carbon diffuses by discharges or the changing of structure of case iron.
Micro hardness (HV) 2000 1500 1000 50 Modified layer HAZ + Diffused zone Matrix

200

400

600

800

Depth Depth below surface (m) below surface (mm)

Figure 12: Section hardness of machined surface before and after annealing To investigate effect of carbon and HAZ on the hardness, the hardness was evaluated on cross sectional of cast iron. Figure 12 shows the sectional hardness measurement of modified surface on cast iron. It can be considered that the machined surface is covered with TiN and TiCN layer. The hardness of modified layer is about 1450 Hv. On HAZ region, the hardness decreases gradually according to the distance from the surface. It reaches to the hardness of matrix cast iron through that of requenched region. Some hardness regions on HAZ are below the hardness of matrix region, it is considered that the coming off of carbon effects to the hardness of that region. HAZ.

3.5 Xraydiffraction(XRD)analysis
As mentioned above, the some modified layer could be adhered on the work piece by EDM in liquid nitrogen. To confirm the layer composition X ray-diffraction (XRD) pattern was investigated for the EDMed surface with Ti solid electrode. Figure 13 shows the result of XRD on EDMed surface on S45C compared with EDMed surface on pure iron and cast iron. The peak of TiN and TiCN are very near. From the EPMA results and the hardness results, it indicates that the EDMed surface on S45C and cast iron are composed of TiN and TiCN. On the other hand, only TiN layer was observed on the EDMed surface of pure iron. 52

Apiwat Muttamara, and Yasushi Fukuzawa

(CPS)

1000 500
TiCN TiN
30

Fe TiCN TiN TiN TiCN Fe

Fe

TiN TiN
80

Diffraction angle 2 (Cu K)

a) EDMed surface on S45C

1000 1
TiN

CPS)

Fe Fe Fe

500

TiN

TiN

TiN TiN

30

Diffraction angle 2 (Cu K)

40

50

60

70

80

b) EDMed surface on pure iron

1000 500

TiCN TiN TiCN TiN

Fe Fe TiN Fe TiCN TiN TiN

30

40

50

60

70

80

Diffraction angle 2 (Cu K)

c) EDMed surface on cast iron Figure 13: X-ray diffraction patterns obtained from the EDMed layer in liquid nitrogen by solid Ti on a) S45C , b) pure iron and c) cast iron.

*Corresponding author (A.Muttamara). Tel/Fax: +66-2-5643001 Ext.3189. E-mail address: [email protected] 2012 American Transactions on Engineering & Applied Sciences. Volume 1 No.1 ISSN 2229-1652 eISSN 2229-1660 Online available at http://TUENGR.COM/ATEAS/V01/41-55.pdf

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4. Conclusion
A new EDM surface modification method was tried in liquid nitrogen on S45C steel in various conditions. The results were summarized as follows: (1) In liquid nitrogen, machining process is not obtained, but the TiN products adhere on the work piece. (2) Ti and N element diffused from nearest surface to the thermal affected zone. (3) Discharge causes carbon migration from deeper layers of the substrate. (4) TiCN modified layer could be generated on carbon steel and cast iron because carbon from substrate diffused to modified layer and reacted with nitride product of modified layer.

5. Acknowledgement
The authors are grateful to Faculty of Engineering, Thammasat University, the National Research Council of Thailand (NRCT), the Thailand Research Fund (TRF) and the National Research University Project of Thailand Office of Higher Education Commission for the research funds and T. Klaykaow for carrying out this work.

6. References
Barash, M.M.(1965). Effect of EDM on the surface properties of tool and die steels. Metals engineering quarterly, 5, (4), 48-51. Biing H.Y., Tsai H.C., Huang F. Y. (2005).The effect in EDM of a dielectric of a urea solution in water on modifying the surface of titanium. International Journal of Machine Tools and Manufacture, 45, (2), 194-200. Fredriksson G., and Hogmark S., (1995). Influence of dielectric temperature in EDM of hot worked tool steel. Surface Engineering, 11, (4), 324330. Goto A., T. Magara, T. Moro, H. Miyake, N. Saito, N. Mohri.(1997). Formation of hard layer on metallic material by EDM. Proceedings of the ISEM-12, 271278. Goto, A., Yuzawa, T., Magara, T., and Kobayashi, K. (1998). Study on Deterioration of Machining Performance by EDMed Sludge and its Prevention. IJEM, 3,1-6. Mohri N., Fukusima Y., Fukuzawa Y., Tani T., and. Saito N.(2003). Layer Generation Process on Work-piece in Electrical Discharge Machining, Annals of the CIRP, 52(1),161-164. Mohri, N., Saito, N., and Tsunekawa, Y. (1993). Metal Surface Modification by EDM with Composite Electrode. Annals of the CIRP, 42, (1) 219-222. 54
Apiwat Muttamara, and Yasushi Fukuzawa

Muttamara A., Fukuzawa Y., Mohri N., and Tani T. (2009). Effect of electrode Materials on EDM of Alumina. Journal of Materials Processing Technology, 209, 2545-2552. Muttamara A., Janmanee P., and Fukuzawa Y.(2010). A Study of MicroEDM on Silicon Nitride Using Electrode Materials. International Transaction Journal of Engineering, Management, & Applied Sciences & Technologies. 1(1), 1-7. Janmanee P., and Muttamara A.(2011). A Study of hole drilling on Stainless Steel AISI 431 by EDM Using Brass Tube Electrode. International Transaction Journal of Engineering, Management, & Applied Sciences & Technologies. 2(4), 471-481. Muttamara A., Fukuzawa Y., and Mohri N.(2002). A New Surface Modification Technology on Steel using EDM, Journal of Australian Ceramic Society (38), 2,125-129.

Dr.Apiwat Muttamara is an Assistant Professor of Department of Industrial Engineering at Thammasat University. He received his B.Eng. from Kasetsart University and the D.Eng. in Materials Science from Nagaoka University of Technology, Japan. Dr. Muttamara is interested involve Electrical Discharge Machining of insulating materials. Yasushi FUKUZAWA is Professor of Material Science and Engineering group in Department of Mechanical Engineering at Nagaoka University of Technology, Japan. Prof. Dr. Fukuzawas fields are material processing and treatment.

Peer Review: This article has been internationally peer-reviewed and accepted for publication according to the guidelines given at the journals website.

*Corresponding author (A.Muttamara). Tel/Fax: +66-2-5643001 Ext.3189. E-mail address: [email protected] 2012 American Transactions on Engineering & Applied Sciences. Volume 1 No.1 ISSN 2229-1652 eISSN 2229-1660 Online available at http://TUENGR.COM/ATEAS/V01/41-55.pdf

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