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Synthesis and Characterization of Titanium and Titanium Nitride Deposition on High Speed Steel Substrate
Available online at www.sciencedirect.com
ScienceDirect Materials Today: Proceedings 18 (2019) 5416–5420
www.materialstoday.com/proceedings
ICMPC-2019
Synthesis and Characterization of Titanium and Titanium Nitride Deposition on High Speed Steel Substrate M.R. Kumara,*, C.K. Beheraa, S. Mohana, S. Aichb a b
Dept of Metallurgical Engg, IIT (BHU),Varanasi -221005,India Dept of Metallurgical engg,IIT Kharagpur, W.B.-721302,India
Abstract In the present study, titanium and titanium nitride are deposited on the high speed steel at ambient temperature and the tribological behavior is investigated. The deposited high speed steels are characterized by different experimental techniques. scanning-electron microscopy (SEM) is used for film morphology and fractured cross-section examination. However, Profilometer is used for measuring the film thickness and roughness. Nano-indentation is used to extract the intrinsic hardness and youngs modulus evaluation. Ball on-disc sliding test under dry condition at ambient temperature is employed for tribological properties of deposited high speed steels. The test results indicate the improvement in the hardness of titanium nitride deposited high speed steel as compared to other deposition leads to improvement in the tribological properties. The tribological properties have been correlated with the hardness and the morphology of the worn surfaces. © 2019 Elsevier Ltd. All rights reserved. Selection and peer-review under responsibility of the 9th International Conference of Materials Processing and Characterization, ICMPC-2019 Keywords: Tool steel; magnetron sputtering; wear; Roughness;
1. Main text Surface engineering involves modification of surface microstructure and composition by applying controlled amount of energy and/or matter. Elements are added to meet the required properties by forming alloys, stable or metastable phases or even layers. Optimum performance in engineering components often require differential properties between the surface and the bulk e.g. high hardness in the case of cutting tool, which is achieved by engineering or tailoring the surface microstructure and/or composition. Coated cutting tools tend to retain a greater life proportion of the bulk tool material. * Corresponding author. Tel.: +91 542 2369346; fax: +91 542 2369478. E-mail address: [email protected]
2214-7853 © 2019 Elsevier Ltd. All rights reserved. Selection and peer-review under responsibility of the 9th International Conference of Materials Processing and Characterization, ICMPC-2019
M.R. Kumar/ Materials Today: Proceedings 18 (2019) 5416–5420
5417
A possible reason for this could be due to the presence of the coating; at the tool-chip interface the coating suppresses high temperature generation, this leads to reductions in dissolution wear. As a result of machining, large portions of the tool are retained because there are mechanically robust regions [1]. This is not the case for uncoated tools because at high temperatures it encourages dissolution wear. This leads to the formation of mechanically and physically weaker area, which become prone to chipping. [2, 3]. Because conserving scarce material resources are the main needs of modern tool industry. Achieving of these demands and reducing the use of hazardous lubricants are just some examples. High hardness and temperature strength, chemical stability and high toughness are demanded by coatings. For reducing friction and wear, the tool surface has to form stable compounds at the contact interface. It is impossible to combine all these properties together in a single conventional tool material. 2. Experiment The experiments included in the present work can be broadly classified as surface coatings of high speed steel (HSS) using Magnetron sputtering unit at different process parameters, microstructural study of the coated steel surface, study on the micro hardness, phase analyses, and the wear behavior of the coated steel surface. In this study a commercial high-speed steel (HSS), SS-CRM NO.487/1 was chosen as substrates as shown in below Fig 1 (a-b). 2.1 Sample prepration The specimen was first cut into a few slices of optimum size of thickness around 1mm with EDM (electric discharge machine). Initially the small pieces of different substrates were mechanical polished using Belt grinder to remove the oxide layer from the surface followed by 240, 320, and 600 grit silicon carbide grinding papers on Buehler polishing Machine with continuous flow of water on the silicon carbide grit papers .The second stage of polishing involved using 6μm and 9μm Diamond paste with Meta-D fluid on Trident cloths. 2.2 Magnetron sputtering The HSS substrates were ultrasonically cleaned with acetone and ethanol before charging inside the deposition chamber. Then system is evacuated to below 5.6 × 10− 6 Pa and raise the temperature. During experiment highpurity argon gas was introduced into the chamber. 3. Results and discussion 3.1 Profilometry study The mentioned sputtering system is equipped with a turbo-molecular pump and a high-performance rotary backing pump to maintain desirable vacuum in the chamber as shown in below Fig 2 (a-b) ,Fig 3 (a-b) and Fig 4 (a-b) Fig 5 (a-b) and Table 1.
(a)
(b)
Fig. 1 Coating thickness profile of sputtered titanium and titanium nitride on HSS steel at; (a) Ti at Room temperature, (b) TiN at Room temperature.
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M.R. Kumar et al. / Materials Today: Proceedings 18 (2019) 5416–5420
(a) (b) Fig. 2 Coating roughness profile of sputtered titanium on HSS steel (a)Ti at Room temperature (b) TiN at Room temperature.
3.1 Scanning electron microscope
Fig. 3 Scanning electron micrographs of top surfaces of coated samples at different temperature (a) at Room temperature (b)Titanium nitride Coated at room temperature.(mag.5.00Kx)
M.R. Kumar/ Materials Today: Proceedings 18 (2019) 5416–5420
5419
Table1: Nano hardness and youngs modulus of coated sample Mechanical Properties
Ti at room temp.
TiN at room temp.
Hardness (Gpa)
0.56
4.86
Youngs modulus (Gpa)
4.64
124.67
Fig. 4 (a) Ti coated sample at room temperature
(b) TiN Coated sample at room temperature
Fig. 5 Scanning electron micrograph of worn out surface of (a)Ti Coated at Room temperature and (b)TiN coated at Room temperature (mag.5.00Kx)
From profilometry it has observed that coating thickness is more in case of titanium than titanium nitride while coating roughness is lower in case of titanium deposition [4].SEM reveals that titanium coated shows spherical particles but in titanium nitride particles elongated due to nitrogen particles at interstitial sites. From wear test it has observed that coefficient of friction is very small in case of nitride coating and more in case of titanium coated sample[5]. which reveals that titanium nitride has better wear resistance property. But from SEM of worn out surface nitride layer shows some irregularity like jagged edges and cracks while in case of titanium it was not found [6]. 4. Conclusions Titanium Nitride improved hardness and wear resistance property than titanium coated sample. From worn out surface these observations found that titanium nitride coating is brittle in nature, which provide the scope to explore how to overcome the brittleness of the coating. References [1] [2]
M.J. Jacksona, G.M. Robinson, J.S. Morrell, “machining M42 tool steel using nano structured coated cutting tools”, Achievements in materials and manufacturing engg, vol. 23, pp 83-86 , 2007 S.A. Barnett,A.Madan,I.Kim,and K.Martin,”stability of nano materials thick layer in hard coating”, E-MRS Bulletin, vol. 28,pp. 169-172, 2003.
5420 [3] [4] [5]
[6]
M.R. Kumar et al. / Materials Today: Proceedings 18 (2019) 5416–5420
S.J. Bull and A.M Jones,”multilayer coating for improved performance”, surface coating technology,vol. 78, pp. 173-175,1996. L.A. Dobrzański a, E. Jonda a, K. Lukaszkowicz a, K. Labisz a, A. Klimpel ,Surface modification of the X40CrMoV5-1 steel by laser alloying and PVD coatings deposition,27(2008)179-182. B. Subramania, R. Ananthakumar, Akira Kobayashi, M. Jayachandran, Surface modification of 316L stainless steel with magnetron sputtered TiN/VN nanoscale multilayers for bio implant applications, J Mater Sci: Mater Med, 23 (2012) 329–338. 6 . D.H. Jeong, F. Gonzalez*, G. Palumbo*, K.T. Aust and U. Erb, the effect of grain size on the wear properties Of electrodeposited nanocrystalline nickel Coatings Scripta mater. 44 (2001) 493–499.
ScienceDirect Materials Today: Proceedings 18 (2019) 5416–5420
www.materialstoday.com/proceedings
ICMPC-2019
Synthesis and Characterization of Titanium and Titanium Nitride Deposition on High Speed Steel Substrate M.R. Kumara,*, C.K. Beheraa, S. Mohana, S. Aichb a b
Dept of Metallurgical Engg, IIT (BHU),Varanasi -221005,India Dept of Metallurgical engg,IIT Kharagpur, W.B.-721302,India
Abstract In the present study, titanium and titanium nitride are deposited on the high speed steel at ambient temperature and the tribological behavior is investigated. The deposited high speed steels are characterized by different experimental techniques. scanning-electron microscopy (SEM) is used for film morphology and fractured cross-section examination. However, Profilometer is used for measuring the film thickness and roughness. Nano-indentation is used to extract the intrinsic hardness and youngs modulus evaluation. Ball on-disc sliding test under dry condition at ambient temperature is employed for tribological properties of deposited high speed steels. The test results indicate the improvement in the hardness of titanium nitride deposited high speed steel as compared to other deposition leads to improvement in the tribological properties. The tribological properties have been correlated with the hardness and the morphology of the worn surfaces. © 2019 Elsevier Ltd. All rights reserved. Selection and peer-review under responsibility of the 9th International Conference of Materials Processing and Characterization, ICMPC-2019 Keywords: Tool steel; magnetron sputtering; wear; Roughness;
1. Main text Surface engineering involves modification of surface microstructure and composition by applying controlled amount of energy and/or matter. Elements are added to meet the required properties by forming alloys, stable or metastable phases or even layers. Optimum performance in engineering components often require differential properties between the surface and the bulk e.g. high hardness in the case of cutting tool, which is achieved by engineering or tailoring the surface microstructure and/or composition. Coated cutting tools tend to retain a greater life proportion of the bulk tool material. * Corresponding author. Tel.: +91 542 2369346; fax: +91 542 2369478. E-mail address: [email protected]
2214-7853 © 2019 Elsevier Ltd. All rights reserved. Selection and peer-review under responsibility of the 9th International Conference of Materials Processing and Characterization, ICMPC-2019
M.R. Kumar/ Materials Today: Proceedings 18 (2019) 5416–5420
5417
A possible reason for this could be due to the presence of the coating; at the tool-chip interface the coating suppresses high temperature generation, this leads to reductions in dissolution wear. As a result of machining, large portions of the tool are retained because there are mechanically robust regions [1]. This is not the case for uncoated tools because at high temperatures it encourages dissolution wear. This leads to the formation of mechanically and physically weaker area, which become prone to chipping. [2, 3]. Because conserving scarce material resources are the main needs of modern tool industry. Achieving of these demands and reducing the use of hazardous lubricants are just some examples. High hardness and temperature strength, chemical stability and high toughness are demanded by coatings. For reducing friction and wear, the tool surface has to form stable compounds at the contact interface. It is impossible to combine all these properties together in a single conventional tool material. 2. Experiment The experiments included in the present work can be broadly classified as surface coatings of high speed steel (HSS) using Magnetron sputtering unit at different process parameters, microstructural study of the coated steel surface, study on the micro hardness, phase analyses, and the wear behavior of the coated steel surface. In this study a commercial high-speed steel (HSS), SS-CRM NO.487/1 was chosen as substrates as shown in below Fig 1 (a-b). 2.1 Sample prepration The specimen was first cut into a few slices of optimum size of thickness around 1mm with EDM (electric discharge machine). Initially the small pieces of different substrates were mechanical polished using Belt grinder to remove the oxide layer from the surface followed by 240, 320, and 600 grit silicon carbide grinding papers on Buehler polishing Machine with continuous flow of water on the silicon carbide grit papers .The second stage of polishing involved using 6μm and 9μm Diamond paste with Meta-D fluid on Trident cloths. 2.2 Magnetron sputtering The HSS substrates were ultrasonically cleaned with acetone and ethanol before charging inside the deposition chamber. Then system is evacuated to below 5.6 × 10− 6 Pa and raise the temperature. During experiment highpurity argon gas was introduced into the chamber. 3. Results and discussion 3.1 Profilometry study The mentioned sputtering system is equipped with a turbo-molecular pump and a high-performance rotary backing pump to maintain desirable vacuum in the chamber as shown in below Fig 2 (a-b) ,Fig 3 (a-b) and Fig 4 (a-b) Fig 5 (a-b) and Table 1.
(a)
(b)
Fig. 1 Coating thickness profile of sputtered titanium and titanium nitride on HSS steel at; (a) Ti at Room temperature, (b) TiN at Room temperature.
5418
M.R. Kumar et al. / Materials Today: Proceedings 18 (2019) 5416–5420
(a) (b) Fig. 2 Coating roughness profile of sputtered titanium on HSS steel (a)Ti at Room temperature (b) TiN at Room temperature.
3.1 Scanning electron microscope
Fig. 3 Scanning electron micrographs of top surfaces of coated samples at different temperature (a) at Room temperature (b)Titanium nitride Coated at room temperature.(mag.5.00Kx)
M.R. Kumar/ Materials Today: Proceedings 18 (2019) 5416–5420
5419
Table1: Nano hardness and youngs modulus of coated sample Mechanical Properties
Ti at room temp.
TiN at room temp.
Hardness (Gpa)
0.56
4.86
Youngs modulus (Gpa)
4.64
124.67
Fig. 4 (a) Ti coated sample at room temperature
(b) TiN Coated sample at room temperature
Fig. 5 Scanning electron micrograph of worn out surface of (a)Ti Coated at Room temperature and (b)TiN coated at Room temperature (mag.5.00Kx)
From profilometry it has observed that coating thickness is more in case of titanium than titanium nitride while coating roughness is lower in case of titanium deposition [4].SEM reveals that titanium coated shows spherical particles but in titanium nitride particles elongated due to nitrogen particles at interstitial sites. From wear test it has observed that coefficient of friction is very small in case of nitride coating and more in case of titanium coated sample[5]. which reveals that titanium nitride has better wear resistance property. But from SEM of worn out surface nitride layer shows some irregularity like jagged edges and cracks while in case of titanium it was not found [6]. 4. Conclusions Titanium Nitride improved hardness and wear resistance property than titanium coated sample. From worn out surface these observations found that titanium nitride coating is brittle in nature, which provide the scope to explore how to overcome the brittleness of the coating. References [1] [2]
M.J. Jacksona, G.M. Robinson, J.S. Morrell, “machining M42 tool steel using nano structured coated cutting tools”, Achievements in materials and manufacturing engg, vol. 23, pp 83-86 , 2007 S.A. Barnett,A.Madan,I.Kim,and K.Martin,”stability of nano materials thick layer in hard coating”, E-MRS Bulletin, vol. 28,pp. 169-172, 2003.
5420 [3] [4] [5]
[6]
M.R. Kumar et al. / Materials Today: Proceedings 18 (2019) 5416–5420
S.J. Bull and A.M Jones,”multilayer coating for improved performance”, surface coating technology,vol. 78, pp. 173-175,1996. L.A. Dobrzański a, E. Jonda a, K. Lukaszkowicz a, K. Labisz a, A. Klimpel ,Surface modification of the X40CrMoV5-1 steel by laser alloying and PVD coatings deposition,27(2008)179-182. B. Subramania, R. Ananthakumar, Akira Kobayashi, M. Jayachandran, Surface modification of 316L stainless steel with magnetron sputtered TiN/VN nanoscale multilayers for bio implant applications, J Mater Sci: Mater Med, 23 (2012) 329–338. 6 . D.H. Jeong, F. Gonzalez*, G. Palumbo*, K.T. Aust and U. Erb, the effect of grain size on the wear properties Of electrodeposited nanocrystalline nickel Coatings Scripta mater. 44 (2001) 493–499.