Influence of methane flow ratios on the structural and mechanical properties of Ti doped diamond-like carbon films

doi:10.21203/rs.3.rs-2820001/v1

Diamond-like carbon films with Ti dopant (Ti-DLC) are synthesized by reactive magnetron sputtering using a pure Ti metal target. This study determines the effect of methane flow ratios [R_m=CH₄/(Ar + CH₄), ranging from 4 to 12%] on the surface morphology, microstructure, mechanical properties and cermet cutting tool inserts features of Ti-DLC films. The GIXRD diffraction spectrum for Ti-DLC film depicts an amorphous structure. There are peaks for nano-crystalline TiC at 2θ values of 35.88^o, 41.52^o and 60.14^o, which respectively correspond to the (111), (200) and (220) planes of the face centered cubic structure. The characteristic binding energy of C 1s, Ti 2p and O 1s for Ti-DLC film is determined using a high-resolution XPS spectra. Increasing R_m flow ratio (reducing Ti metal doping) increases the intensity of the Raman spectrum because there is an increased sp²-C (sp²/sp³ ratio) site fraction for DLC components. The experimental results show that the hardness of the DLC film increases from 11.07 GPa to 14.76 GPa as the R_m flow ratio is increased from 4% to 12%. The adhesive strength of the Ti-DLC film coating is measured using a scratch test and shows that the film adheres well to the substrate. The Ti-DLC films are coated onto cutter inserts for the dry milling of an Inconel 718 workpiece and the results show that all coated tools have a significantly longer tool life than uncoated tools.

Diamond-like carbon

sputtering

methane ratios

milling performance

Diamond-like carbon (DLC) is a carbonaceous material that is composed of SP²- and SP³- bonded carbon atoms, which are respectively configured as in graphite and diamond [1]. The ratio of sp²/sp³ has a significant effect on the mechanical features of DLC films. The ratio of these components is adjusted to optimize the DLC film properties to increase the field of applications [2]. DLC thin film coatings feature high hardness, high wear resistance, a low coefficient of friction, excellent anti-corrosive behavior and good bio-compatibility and antibacterial activity [3]. DLC films are used as protective coatings for electrical devices, cutting tools and dies, medical components and biological implants [4].

Many techniques are used to prepare DLC films. Reactive magnetron sputtering is used to synthesize DLC films because it is inexpensive, allows easy control of the elemental composition and produces a uniform film [5]. Doping with metallic or non-metallic elements (Si, Al, Ti, W, and N, etc.) is used to reduce residual internal stress and to increase the adhesive strength of DLC films [6]. Chen et al. [7] used reactive sputtering to synthesize Ti-doped DLC films whose properties were controlled by fabrication parameters. The results show that the coated tool inserts have less flank wear and the workpiece has fewer surface defects, so cutting performance is increased. Wu et al. [8] reported F and Si co-doped DLC films prepared by reactive magnetron sputtering, using a SiC crystal target and a source gas that is a mixture of trifluromethane and Ar. Studies show that the input power affects the structure and mechanical properties of DLC films. Xu et al. [9] reported Ti/Al Co doped DLC films that were synthesized using a hybrid ion beam system. The doped Ti forms a TiC carbide bond structure in the amorphous carbon matrix and the doped Al element exists in an oxide state, not a metallic state. Therefore, the co-doping of Ti/Al elements into DLC film significantly improves the mechanical properties and corrosion resistance. Zhang et al. [10] fabricated Ti-DLC films using a magnetron sputtering system. TiC bonds form as the Ti concentration reaches 4.43 at.% and the surface roughness increases as the Ti concentration increases. A Ti-DLC film containing 17.13 at.% Ti element has excellent adhesive strength and micro-hardness.

This study produces a Ti-DLC/Ti buffer bi‑layer film that is grown using reactive direct current (DC) magnetron sputtering. A pure Ti metal target and an argon and methane gas mixture are used. The content of Ti metal in the film is controlled using the methane flow ratio [R_m = CH₄/(CH₄ + Ar)%]. The structural features, elemental composition, mechanical properties and the behavior of cutting tool inserts that are coated with the film are determined. The dry milling mode of a nickel-based superalloy (Inconel 718, which is a hard-to-cut material [11]) is performed using tools that are coated in a Ti-DLC film. The film and prolongs the service life of the coated tools.

Composite Ti-DLC/Ti buffer bi-layer coatings were deposited onto cermet cutting tool inserts (TNMG-160404R-UM T1200A, Sumitomo, for dry milling) and glass substrate (for structural analysis) using reactive DC magnetron sputtering with a working pressure of 1.4 × 10^− 3 Pa. A pure Ti metal target (99.99%, 76 mm in diameter) and a mixture of high purity (99.99%) Ar plasma and CH₄ reaction gas were used. The R_m flow ratio varied from 4 to 12%. DLC films were doped with elemental Ti using DC power of 180 Watts, substrate temperature of 200^oC, substrate bias of − 50 V and coating time of 25 min. A Ti buffer layer (thickness of ~ 178 nm) was deposited using DC power of 180 Watts and coating time of 6 min. The deposition conditions for Ti-DLC films with a Ti buffer layer are listed in Table 1. Substrates (glass and tool inserts) were ultrasonically cleaned in isopropanol, rinsed with deionized water and dried under nitrogen. Prior to coating, the target was pre-sputtered for 15 min to remove any contamination.

The morphological characteristics and cross-sections of films were determined using atomic force microscopy (PSIA-XE-100, AFM) and field emission scanning electron microscopy (SEM 6500 F) respectively. Energy dispersive X-ray spectroscopy (EDS) was used for semi-quantitative analysis of elemental concentrations in the film. Raman scattering spectroscopy (Horiba iHR550) was used to characterize the carbon-based structure of DLC films. High-resolution transmission electron microscopy (TEM, FEI Tecnai F20) was utilized to determine the microstructure of Ti-DLC film. The phase structure of the films is characterized using X-ray diffraction (GIXRD, D8A25) with a grazing incidence angle of 2°. X-ray photoelectron spectroscopy (XPS, VG ESCA Scientific Theta Probe) was used for analyzing the bonding state and the structural composition of Ti-DLC films [12]. The composition depth distribution of elements in DLC films is determined using secondary ion mass spectrometry imaging (ION-TOF, Germany).

The mechanical features of the Ti-DLC/Ti buffer bi-layer coatings were measured at room temperature using a nano-indenter (ASMEC UNAT) with a load of 8 mN. To determine the adhesive performance of the coated film, the cracking features were determined using a scratch test (JLST022). Milling operations produce complex geometric surfaces so this determines the effect of a Ti-DLC/Ti buffer bi-layer on coated cermet tool inserts using a conventional milling machine, without coolant, and using an Inconel 718 superalloy workpiece. The mechanical features and the chemical elemental composition of the Inconel 718 are detailed in a previous study [13]. A cutting tool with a single tooth was used for milling with milling cutter face of 50 mm in diameter, depth of cut of 1.0 mm, a spindle speed of 300 rpm and feed rate of 0.04 mm/rev. The milling performance was characterized by measuring the flank wear on the tool insert and the surface roughness of the machined workpiece (Inconel 718, width and length 22 mm and 24 mm, respectively). Flank wear and surface roughness (Ra, µm) were measured using SEM and a profilometer (Mitutoyo, Suftest-402), respectively. All dry milling operation tests were repeated four times and their values were averaged for analysis.

Table 1

Experimental conditions for the deposition of Ti-DLC film coatings and for coatings with a Ti buffer layer.
	Ti buffer layer	Ti doped DLC coating
Substrate	cermet cutting inserts (TNMG-160404R-UM T1200A), glass and stainless steel
Gas	Ar (99.99%)
Metal target	Ti (99.99%)
Base pressure	6.2×10^–4 Pa
Working pressure	1.4×10^–3 Pa
Substrate temperature	200^oC
Substrate bias	– 50 V
Substrate-to-target distance	80 mm
Substrate rotate speed	20 rpm
Total gas flow	30 sccm
DC power	180 Watt
Deposition time	6 min (thickness of 178 nm)	25 min (various thickness)
R_m%= CH₄/(Ar + CH₄)	0	4. 6, 8, 10, 12%

3.1 Characterization of the Ti- DLC films

The use of a metal buffer layer between the DLC film and the substrate significantly reduces the internal stress and increases the adhesion of the DLC film [14]. The Ti buffer layer (~ 178 nm thick) was grown by sputtering, using a DC power of Ti target, a DC power of 180 Watt and a deposition time of 6 min. Figure 1 shows that the surface AFM and cross-sectional SEM morphology of the Ti-DLC/Ti buffer bi-layer film are relative to R_m flow ratio. The DLC films exhibit a smooth particular structure with a relatively small surface roughness (Ra = 6.99 ~ 8.80 nm). The film is dense and uniform in structure, with no delamination or peeling after coating, and it is perfectly bonded to the substrate. The growth rate is calculated by dividing the DLC film thickness by the 25 min deposition time. The growth rate for Ti-DLC films decreases from 23.24 nm min^–1 (581 nm thick) to 16.52 nm min^–1 (413 nm thick) when the R_m flow ratio is increased from 4–12%.

Ti atoms are sputtered and incorporated into the film, which contains carbon. If the methane flow rate is increased, the surface of the Ti target becomes covered with carbonaceous material due to target poisoning [15] so the Ti concentration and the growth rate for the DLC film decreases. In the right parts of Fig. 1, the cross-sectional SEM morphology shows correlation between the thickness of the film and the R_m flow ratio. As the R_m flow ratio is 4%, 6%, 8%, 10% and 12%, the thickness of the films is 581, 569, 514, 484 and 413 nm, respectively. This result show that the thickness of the film decreases while the R_m flow ratio increases. This depicts Ti atoms become more difficult to be sputtered because the carbon coating has been coated on the Ti target during sputtering. This result was also demonstrated by Wang et al. [16].

The C, Ti and O content in the Ti-DLC films is shown in Table 2 as a function of the R_m flow ratio. As R_m increases, the carbon concentration increases from 48.62 at.% to 58.63 at.%, the Ti concentration decreases from 37.23 at.% to 28.21 at.% and the O concentration ranges from 13.16 at.% to 14.15 at.%. The doped Ti element bonds with carbon to form a Ti-C structure. As the R_m flow ratio increases, the proportion of carbide bonds decreases and the proportion of carbon bonds increases. The Ti content of the DLC film is controlled by adjusting the R_m flow ratio. This is also demonstrated in the study by Cao et al. [17].

Table 2

Element concentration of a Ti-DLC film coating as a function of R_m flow ratio.
R_m	Element composition (atomic %)
R_m	C	Ti	O	Totals
4%	48.62	37.23	14.15	100
6%	51.83	34.45	13.72	100
8%	53.46	32.47	14.07	100
10%	56.73	30.07	13.20	100
12%	58.63	28.21	13.16	100

Figure 2 shows the GIXRD diffraction spectrum for a Ti-DLC film coating for various R_m flow ratios. There are no diffraction peaks for the carbon and diamond phase, so the Ti-DLC film is amorphous. There are peaks for nano-crystalline TiC at values for 2θ of 35.88^o, 41.52^o and 60.14^o, which respectively correspond to the (111), (200) and (220) planes [JCPDS No.89-3828] of the face centered cubic (FCC) structure. The peaks for the (200) and (220) planes are relatively weak. This is in agreement with the results of the study by Gayathri et al. [18]. The preference for orientation in the (111) plane is attributed to the surface energy [19]. As the R_m flow ratio is increased from 4 to 12%, the position of the (111) peak shifts towards a lower diffraction angle of 35.88^o to 35.12°. The microstructure of Ti-DLC using TEM is shown in Fig. 3. Typical amorphous/nanocrystalline composite carbon structure embedded in DLC matrix. The electron diffraction pattern of a selected area (Fig. 3a) shows crystalline diffraction rings that correspond to (111), (200) and (220) crystal planes of TiC, indicating the presence of a polycrystalline structure. This is in agreement with the GIXRD diffraction results. The interplanar distance calculated from the inverse fast Fourier transform (FFT) resulted in 0.223 nm (Fig. 3b inset 1) and 0.246 nm (Fig. 3b inset 2), which corresponds to (200) and (113) planes.

The grains size in the films is calculated using the full width at half maximum (FWHM) and the Scherrer equation [20]. The 2θ, FWHM and grain size for Ti-DLC (111) plane that are grown using various R_m flow ratios, corresponding to Fig. 2 are shown in Table 3. The grain size of the Ti-DLC (111) plane is among 13.63 nm to 15.66 nm, 2θ is 35.120 ~ 35.882 degree, and FWHM is 0.533 to 0.612. The incorporation of carbon into the interstitial spaces of the FCC TiC lattice results in lattice distortion and compressive stress inside the film, as demonstrated by the shift in the TiC (111) XRD peak to a lower angle. Figure 4 shows the SIMS depth profile for a Ti-DLC film coating for a R_m flow ratio of 4%. The distribution of Ti and C elements is uniform throughout the depth of the film.

Table 3

The 2θ, FWHM and grain size for Ti-DLC (111) films that are grown using various R_m flow ratios, corresponding to Fig. 2.
R_m	2θ (degree)	FWHM	Grain size (nm)
4%	35.882	0.545	15.32
6%	35.676	0.610	13.68
8%	35.696	0.533	15.66
10%	35.541	0.612	13.63
12%	35.120	0.547	15.23

High-resolution XPS spectroscopy is used to determine the bond state structure and the elemental composition information of Ti-DLC films. The XPS spectra for characteristic binding energies for C 1s, Ti 2p and O 1s for Ti-DLC film coatings with a R_m flow ratio of 4%, are shown in Fig. 5. The O 1s signal is observed in the DLC films, probably there is a residual atmosphere in the chamber or because the sample is oxidized in air [21]. The C 1s spectra in Fig. 5 (a) has a main peak und at ~ 283.4 eV (C-C/C-H bonds, amorphous carbon), which is typical of DLC film structure. There is a major peak ~ 280.4 eV and a weak peak at ~ 287.3 eV, which respectively correspond to C-Ti (Ti carbide components) and C = O (carbide bonds). The peaks at around 280.4 eV are due to C-Ti components. This shows that C atoms interact with doped Ti atoms to form a nanocrystalline TiC structure [22]. The Ti 2p spectrum in Fig. 5 (b) has peaks at ~ 453.7 eV and ~ 459.8 eV, which respectively correspond to the Ti 2p_3/2 and Ti 2p_1/2 peaks for the Ti-C bond structures (TiC state) [23]. The binding energies at around 457.2 eV and 462.9 eV are respectively attributed to Ti 2p_3/2 and Ti 2p_1/2 for the Ti-O (TiO₂ structure). Moreover, in the interval between the Ti-C peak and the Ti-O peak, there are two weak peaks near 454.8 eV (Ti 2p_3/2) and 461.6 eV (Ti 2p_1/2), which are denoted as Ti-X. These peaks consist of TiC_x (x < 1) and TiO_x (or TiC_xO_y) [24]. The O 1s spectrum in Fig. 5 (c) has binding energies at around 527.9 eV, 528.6 eV, 530.2 eV and 531.6 eV that are respectively associated with O-Ti, O-Ti^*, O = C and O-C bonding. This result is consistent with the study by Zhang et al. [25].

Raman spectroscopy is used to determine the DLC carbon bonding state in the C-C phase structure [26]. Figure 6 shows the Raman spectra for a Ti-DLC that is deposited using various R_m flow ratios. The Raman spectrum has an asymmetrically dispersed, curved spectrum with peaks between 1000 and 1800 cm^− 1, which is typical for a DLC structure. The D peak has a smaller shoulder (disordered, indicated C-C sp² bonding), which is associated with carbon disorder, due to breathing patterns for those sp² carbon bonds that are only in aromatic rings. The G peak at 1560 ~ 1680 cm^− 1 (suggested C-C sp³ bonding) is attributed to the C-C stretching patterns of sp² atoms in aromatic rings and carbon chains [27]. Figure 6 shows that increasing the R_m flow ratio (reducing Ti metal doping) increases the intensity of the Raman spectrum, because there is an increase in sp²-C (sp²/sp³ ratio) site fraction of DLC components [28]. These results are in agreement with those of the study by Guo et al. [29], which showed that increasing the metal doping decreases the intensity of the Raman spectrum for a DLC film, because the proportion of centrosymmetric structures (such as TiC) increases, which hinders Raman excitation.

The position of the G peak and the I_D/I_G ratio are used to characterize the sp²/sp³ bonding ratio for the DLC structure [1, 17, 30]. The G peak position and the I_D/I_G ratios are shown in Table 4. As the R_m flow ratio is increased from 4–12%, the I_D/I_G ratio increases from 0.757 to 0.919 and the G peak position ranges from 1562.56 to 1576.23 cm^− 1. Similar results were obtained by Dai et al. [28], which showed that as the C₂H₂ fraction increases, the G peak position shifts to higher wavenumbers and the value of the I_D/I_G ratio also increases, so there is in an increase in the sp²/sp³ ratio. If the R_m flow ratio is relatively low (the doping concentrations of Ti increases), the sp²/sp³ ratio for the DLC film decreases and the structural phase of the coating is carbide nanocomposite Ti-DLC. Further increasing the R_m flow ratio causes the structure to transformed into an amorphous carbon-based Ti-DLC coating [28].

Table 4 The ratio of I_D/I_G and the position of the G peak for Ti-DLC films as a function of the R_m flow ratio.

R_m	I_D	I_G	I_D/I_G	G peak position
4%	1747.24	1946.97	0.757	1562.56
6%	2712.98	3521.65	0.770	1576.08
8%	3636.29	4208.89	0.864	1571.53
10%	4494.26	5188.46	0.866	1576.23
12%	5317.22	5779.88	0.919	1567.72

3.2 Mechanical properties and cutting tool inserts features of Ti-DLC films

To determine the mechanical properties of the Ti-DLC films, the load-displacement curve is plotted using the results of nano-indentation tests, and the elastic modulus (E, GPa), hardness (H, GPa), and elastic recovery (%R_e) values are determined [31]. The %R_e represents the ability of a film to return to its original shape after indentation [32] and is defined as:

$$\% {R_e}=\frac{{{h_{\hbox{max} }} - {h_r}}}{{{h_{\hbox{max} }}}} \times 100\%$$

1

where h_max is the maximum indentation depth and h_r is the residual indentation depth. The indentation depth is less than 10% of the film's thickness to eliminate substrate effects. Four identical nano-indentation tests were performed on each sample. Table 5 lists the hardness (H), elastic modulus (E), H/E ratio H³/E² ratio and %R_e value for Ti-DLC films that are grown using various R_m flow ratios. The hardness increases from 11.07 GPa to 14.76 GPa as the R_m flow ratio is increased from 4–12%. The hardness of DLC coatings is directly related to the sp³-C fraction in the carbon matrix [15]. A higher H/E ratio and H³/E² ratio are respectively related to good resistance to elastic strain failure and resistance to plastic deformation. The results in Table 5 show that if the R_m flow ratio is increased to 12%, the maximum respective values for the H/E ratio, the H³/E² ratio and %R_e are 0.12, 0.22 and 62.47%. The formation of TiC carbide bonds is thought to be responsible for an increase in the elastic modulus so adjusting the doping content by adjusting the R_m flow ratio controls the H/E ratio, the H³/E² ratio and the %R_e value for the coating. These results are in agreement with those for the study by Dai et al. [6]. A high H/E, H³/E² ratio and R_e value are characteristic of good tribological features for a film coating [15].

Table 5 The H, E, H/E ratio H³/E² ratio, %R_e value for Ti-DLC films that are grown using various R_m flow ratios.

R_m	Hardness (H, GPa)	Elastic modulus (E, GPa)	H/E	H³/E²	h_max	h_r	Elastic recovery (%R_e)
4%	11.07 ± 0.32	125.3 ± 8.93	0.09	0.09	177.5	98.1	44.73
6%	13.30 ± 0.59	117.9 ± 7.72	0.11	0.17	175.7	96.9	44.85
8%	13.46 ± 0.58	118.0 ± 6.79	0.11	0.18	181.1	91.8	49.31
10%	14.63 ± 0.55	119.9 ± 6.82	0.12	0.22	154.1	58.6	61.97
12%	14.76 ± 0.61	120.6 ± 7.91	0.12	0.22	146.3	54.9	62.47

The adhesive strength of the film coating onto cermet cutting tool inserts is measured using a scratch test [33]. Typical crack modes quantify the critical load for failure [34]. To determine the failure characteristics for a DLC film coating, scratch tracking is used to test the adhesion of the film to the substrate. Figure 7 shows the scratch tracking, normal load and acoustic emission (AE) recordings for a Ti-DLC/Ti buffer bi‑layer film coating. The normal load on the diamond stylus is gradually increased from 500 mN (begin load) to 50 N (end load) at a loading rate of 49.5 N/min, using a scratch speed of 5 mm/min, with a total scratch length of 5 mm. The scratch adhesion critical normal loads L_C1 (first crack) and L_C2 (first peel) are respectively defined as the load that causes incipient cracking and initial adhesive failure [35]. The respective normal loads for L_C1 and L_C2 are about 37.5 N and 47.5 N. The corresponding AE signals are shown at about 3.7 mm (incipient crack) and 4.8 mm (initial peeling), so this film adheres well to the substrate.

Dry milling without a coolant reduces the environmental impact [36]. This study uses a cermet cutting insert that is coated with a Ti-DLC/Ti buffer bi‑layer film for the dry machining of an Inconel 718 superalloy workpiece (hard-to-cut material), as shown in Fig. 8. For uncoated tool inserts, the surface roughness and flank wear are Ra = 3.81 µm and 56.73 µm, respectively. For a Ti-DLC coated cutter insert, the R_m flow ratio increases from 4–12%, the surface roughness decreases from Ra = 3.31 to Ra = 1.96 µm and the flank wear is reduced from 47.55 to 30.81 µm. These experimental results are consistent with the results for the nano-indentation test. A Ti-DLC/Ti buffer bi‑layer coating on a cutter insert reduces surface roughness and flank wear. All coated tools have a significantly longer life than uncoated tools.

A Ti-DLC/Ti buffer bi‑layer is grown on cermet cutting tool inserts, stainless steel and glass. Using sputtering with a Ti metal target in an atmosphere that is a mixture of gases (Ar and methane) and methane flow ratios [R_m=CH₄/(CH₄ + Ar)] from 4–12%. The Ti doping content of DLC films is controlled by adjusting the R_m flow ratio. The formation peaks for nano-crystalline TiC occur at 2θ values of 35.88^o, 41.52^o and 60.14^o, which respectively correspond to the (111), (200) and (220) planes of the face centered cubic (FCC) structure. This is consistent with the TEM image results.

As the R_m flow ratio is increased from 4 to 12%, the position of the (111) peak shifts towards lower diffraction angles of 35.88^o to 35.12° and the Raman spectrum shows that the I_D/I_G ratio also increases from 0.757 to 0.919. If the R_m flow ratio is increased to 12%, the maximum respective values for the H/E ratio, H³/E² ratio and %R_e are about 0.12, 0.22 and 62.47%. A scratch test, shows that the film adheres well to the substrate. Dry milling of an Inconel 718 workpiece using cermet tool inserts that are coated with a DLC film shows that the film significantly reduces the surface roughness and flank wear.

Author contribution: Wei-Hsiang Lee and Yin-Tung Alber Sun conceptualization; Chih-Chung Hu, Bo-Yuan Wang and Ho Chang experimentation; Wei-Hsiang Lee and Yin-Tung Alber Sun characterization; Chih-Chung Hu, Bo-Yuan Wang and Ho Chang validation; Ho Chang and Chun-Yao Hsu analysis; Chun-Yao Hsu writing draft.

Acknowledgments: The authors gratefully acknowledge the support of the Ministry of Science and Technology of the Republic of China, Taiwan, through Grant nos. MOST 111-2637-E-262-002, MOST 111-2221-E-262-005 and NSTC 111-2622-E-262-002.

Funding: The authors gratefully acknowledge the support of the Ministry of Science and Technology of the Republic of China, Taiwan, through Grant nos. MOST 111-2637-E-262-002, MOST 111-2221-E-262-005 and NSTC 111-2622-E-262-002.

Data availability: All necessary data is shown in the figures and tables within the document. The raw data can be made available upon request.

Code availability: Not applicable.

Ethics approval: Not applicable.

Consent to participate: Not applicable.

Consent for publication: Not applicable.

Conflict of interest: The authors declare no competing interests.

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Influence of methane flow ratios on the structural and mechanical properties of Ti doped diamond-like carbon films

Status:

Journal Publication

Version 1

Abstract

Figures

1. Introduction

2. Experimental Procedure

3. Results And Discussion

3.1 Characterization of the Ti- DLC films

3.2 Mechanical properties and cutting tool inserts features of Ti-DLC films

4. Conclusions

Declarations

References

Status:

Journal Publication

Version 1