Diamond & Related Materials 100 (2019) 107588

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Diamond & Related Materials

journal homepage: www.elsevier.com/locate/diamond

Experimental investigation on chromium-diamond like carbon (Cr-DLC) T

coating through plasma enhanced chemical vapour deposition (PECVD) on
the nozzle needle surface
⁎ ⁎⁎
A. Muthurajaa, Shubham Naika, Dipen Kumar Rajakb, , Catalin I. Pruncuc,d,
a
Department of Mechanical Engineering, Sandip University, Nashik 422213, India
b
Department of Mechanical Engineering, Sandip Institute of Technology and Resesarch Centre, Nashik 422213, India
c
Mechanical Engineering, Imperial College London, Exhibition Rd., London SW7 2AZ, UK
d
Mechanical Engineering, School of Engineering, University of Birmingham, Birmingham B15 2TT, UK

A R T I C LE I N FO A B S T R A C T

Keywords: This study emphases the reduction of droplet defect in nozzle needle during the application of Cr-DLC coating on
Adhesion the substrate. The coatings were carried out in the highly sophisticated chamber with attached coating setup
Deposition under the vacuum atmosphere. The materials were assessed in terms of their adhesiveness, hardness, wear
Droplet defect resistance, and microstructural morphology. The dry wear test result reveals the appreciable outcome of nitrogen
Cr-DLC coating
(N2) flushing on quality of interfacial bonding. The indentation confirms the superior morphology of coated
N2
Needle
substrates but yet insufficient to resist crack propagation due to weak in adhesiveness of chromium (Cr) layer
PECVD under non-N2 flushing. Scanning electron microcopy (SEM) embedded with energy dispersive X-ray (EDX) was
deployed for analysis of cross-sectional coated of substrate. The statistical results claimed that the samples
rejection without N2 flushing was showed up to 1.2%. However, the results revealed that Cr-DLC coating with N2
flushing reduced droplet defect and gain remarkable performance over a wide range of samples. Consequently,
this novel methodology was employed to assess the coating performance by using a performance index based on
tribological properties.

1. Introduction operating temperatures to 300 °C), an increase in the mechanical and

thermal steadiness is required. Eventually, there, the common rail
Diamond-like carbon (DLC) coatings are commonly used for tribo- system became the ruling system since the constantly high pressure in
logical and thermal applications in automotive industries. DLC coating the rails allows for multiple injections which lead to enhancement of
possesses excellent mechanical, thermal, and tribological properties. In fuel economy. These coatings may well contribute to reducing the CO2
addition, they have greater physical properties due to its superior emissions, in turn, they lead to the development of environmentally
properties of hardness, thermal stability, low friction coefficient, and friendly systems [2]. The main characteristic of DLC is represented by
excellent wear resistance. DLC also provides a good diffusion barrier to the ratio between the sp3 and sp2 bonded carbon atoms and the hy-
moisture, gas and excellent properties which make the DLC coating drogen content. They can possess high hardness, low coefficients of
appropriate to be used for use in anti-wear field [1]. They are applied as friction against materials such as steel, and are chemically inert [3–5].
wear protection coatings for specific components such as modern diesel The adhesive strength may have superior bonding, which allows an
injection systems. Thin-film coatings, deposited with the help of plasma increase of the tribological characteristics [6,7]. Further, these coated
technology, are very hard and suitable as wear-resistant. Intense plasma surfaces promote a higher adhesive strength with an increased wear
cleaning and ion bombardment during deposition result in formation of resistance corroborated with superior mechanical properties, corrosion
excellent adhesion and high density films. Thin-films are highly suitable resistance and bioactivity [8,9]. However, to avoid any weakness on
for parts with low tolerances. The introduction of automotive coatings DLC adhesiveness during coating of steel substrate, the chromium layer
was started with the development of the high-pressure fuel injection was considered as an intermediate adhesive layer. It was deposited
pump. Due to increased injection pressures of up to 2500 bar (with between CeH and its substrate. To improve the quality of coating, a

⁎
Corresponding author.
⁎⁎
Correspondence to: C.I. Pruncu, Mechanical Engineering, Imperial College London, Exhibition Rd., London SW7 2AZ, UK.
E-mail addresses: [email protected] (D.K. Rajak), [email protected] (C.I. Pruncu).

https://doi.org/10.1016/j.diamond.2019.107588
Received 10 September 2019; Received in revised form 7 October 2019; Accepted 16 October 2019
Available online 20 October 2019
0925-9635/ © 2019 Published by Elsevier B.V.
A. Muthuraja, et al. Diamond & Related Materials 100 (2019) 107588

new methodology was developed for the selection of coating perfor- the table. Now, since the process is PECVD, the rotation of the table
mance by using a performance index. It was observed that Cr-DLC plays a very important role in the distribution of coating. The negative
coating shows better adhesion behavior with high carbon steel sub- bias voltage will be connected to the substrate table through the rota-
strate [10]. The CrN single layer and Cr-CrN multilayer coatings were tion feed by software controller (fully or semi-automatic). It is neces-
observed having no significant improvements in the tribological prop- sary to load the chamber with the highest possible number of substrates
erties as that of uncoated carbon fiber reinforced epoxy composites to minimize the coating cost per substrate, as taking into account that
using ball-on-disc testing. It is due to highest value of μ > 0.6 in dry all these substrates must be in compliance with the specification
contact between AISI 5210 steel and Al2O3. However, Cr-CrN multi- properties of the coating. Prior, the substrate is being loaded in the
layer coatings with DLC top layers may significantly improve the tri- loading fixture followed by the table; the fixtures are being cleaned
bological material properties. It allows obtaining maximum of sliding with the help of N2 gas, also known as N2 flushing. This process is
cycles, due to reduced shear forces with low-friction behavior of DLC- carried out at a pressure of 5 bar with the help of a flushing gun. The
steel system [11]. sole purpose of carrying out this process is to flush out the loose as well
Sui et al. [12] investigated the performance of a single and multi- as sticky carbon particles from the fixtures, which were deposited when
layer plasma which enables to enhance the chemical vapour deposition the previous batch was being coated. It ultimately causes the non-re-
(PECVD) process. It forms the CrN/DLC/Cr-DLC having superior ad- parable defect on the substrate called as droplet defect. Vacuum
hesive wear resistance as compared with the single CrN and DLC cleaning, post N2 flushing, is done on the entire loading fixture and the
coating. The investigation revealed that the multilayer coatings were table so as to suck the remaining loose particles of carbon. After these
superior in toughness. It is caused by the very fine-grained that is in processes, the table and fixture are ready to load the substrate for
contrast to the single layer coatings, which contain coarse-grained coating. Now, once the batch is loaded in the coating chamber, the first
structure. Also, multilayer PVD coatings provide high wear resistance step performed is the evacuation process, which is the vacuum forma-
and low friction coefficient. The friction coefficient of multilayer-coated tion process. The vacuum pressure maintained inside the chamber is of
surface is seven times lower as compared to single-layer coated surface the order of 10−4 millibar. This process is followed by the heating and
and shows as well as a reduction in the adhesive wear, of multi-layer cooling of the batch for 2.5 h. Once the cooling is done, the fully au-
coatings, under sliding test against ISI 440C steel [12]. The dominant tomated coating chamber does the leak rate test, to ensure the complete
adhesive behavior and thermal stability permits to increase the stress vacuum inside the chamber. Then is conducted the most important
corrosion resistance at interface due to its characteristics, lubricity of processes before coating deposition taking place, called the etching
DLC [1]. The PECVD-Si coatings on Ti substrate surface strongly ad- process. The etching process is done with the assistance of plasma
hered on the substrate and was noted having superior resistance to source, giving a line-of-sight effect for the argon (Ar) ions. The attrac-
delamination [13]. However, surface defects of delamination and dro- tion of the argon ions enforces etching of the biased substrates. The Ar
plet defect on the coating process are necessary to be understood. In flow rate is set around 35 sccm. Once the etching of the entire batch is
most cases, the type of coating process, thickness of coating, an ultra- done, chromium (Cr) deposition starts taking place on the substrates,
sonic vibration, spray flow rate and spray droplet size, a continuous since, it acts as an excellent adhesion agent between the high carbon
thin liquid film and substrate temperature was revealed to influence the steel and the carbon layer.
surface quality of the coating. The impingement of multiple droplets on This process is followed by transition-1 and transition-2 phases.
a substrate using a spray coating endorse that the spray process is Carbon (C) deposition starts through transition-1 phase, still having a
highly random and stochastic. There, a higher substrate temperature majority of Cr deposition. In transition-2 phase, the % of C is higher
provides a more uniform and defect-free coating forms [13]. The than transition-1 phase and % of Cr which is lower in this phase as
thickness of the coating was over 35 μm which led to delamination compared to transition-1. The sole purpose of these two transition
defects, over the coating surface, and the results showed that the de- phases is to progressively increase the deposition of C, followed by
position rate may drive the quality of deposition [14]. decreasing the deposition of Cr. Further, is conducted the final phase of
In the light of all above literature review and in order to overcome coating, called as C-deposition, in which purely C-coating is done on the
the current quality of coating, in this paper, Cr-DLC coatings were substrates, without the presence of Cr in. This entire coating process is
produced. It can develop a superior adhesion DLC multilayer on the carried out at a constant temperature of 150 °C and for a duration of 7 h.
nozzle needle made of high carbon steel that is used as base material, The deposition pressure is maintained in the range of 10–3 Pa. The Cr
commonly used for rail fuel injector. The injector has to assure the exact layer with a thickness of about 0.4 to 0.7 μm was deposited on the
fuel metering by tight closing of the nozzle valve and has to operate surface of substrates and followed by DLC coating at the above the Cr
with very high speed because of the multiple injections during an in- layer, with a thickness of about 1.7 to 2.2 μm. Fig. 1 shows the sche-
dividual cycle of the engine. The objective of this study was to in- matic representation of plasma enhanced chemical vapour deposition
vestigate whether the Cr-DLC dual layer coatings could reduce droplet (PECVD).
defect in nozzle needle and to increase the coating hardness.
2.2. Coating characterization
2. Experimental methods
In order to evaluate the adhesion quality, some disruptive tests were
2.1. Materials and coating deposition performed on the substrate samples. The strength of cohesiveness was
obtained by penetrating the surface with a diamond indenter on a
The high carbon steel substrate was chosen as a nozzle needle ma- macro scale. The macro indentations were performed on rockwell
terial (substrates) with a dimension of 42 mm in length. The substrates hardness tester (Make: ATMO rockwell hardness tester, Model: BRIO)
are arranged in a tray and cleaned in an ultrasonic cleaner containing which is used for evaluating the hardness of substrate material, Cr
cleaning agent as Isopar-H for 15 min. Yet, in the case of mass pro- layer, and DLC layer as well. The macro indentation was performed
duction, the manufacturing rate will be higher for fully loaded system. using a rockwell C hardness tester with a tip radius of 2 μm. Micro-
For that, a substrate rotation table is developed; where its base is abrasive wear test (calowear) using a simple ball catering method is
equipped with a vertical spindle distributed over the table cir- generally used in tribological experiments for quality assessment of
cumference. The design of the table allows forming a satellite table, superficial up to 100 μm thick coatings. The thickness of coated samples
where the epicyclical gear drive system is located on the circumference was measured by calowear abrasion tester (Make: CSM instruments). It
of base table. The vertical spindle with substrate holders is individually is a straight forward method to characterize the resistance to abrasion
driven by the planetary gears and is connected to a rotation axis under of a surface. The spherical ball of 30 mm diameter is kept on the guide

2
A. Muthuraja, et al. Diamond & Related Materials 100 (2019) 107588

Fig. 1. Schematic construction of PECVD sputtering process.

of the needle with the help of suitable fixture and then the ball is ro- 10.13 wt% Fe; spectrum 2 contains 50.23 wt% C, 42.94 wt% Cr and
tated over it with a speed of 800 rpm for a span of 25 s. There, a small 4.86 wt% Fe while spectrum 3 contain 24.93 wt% C, 59.15 wt% Cr and
drop of diamond slurry (0.5–1 μm) is put on the spherical ball. The SEM 10.16 wt% Fe, respectively. It was observed that white spots were found
and EDX analysis have been performed on the substrate to understand having more concentration of Cr particles and the grey surface having
the surface characteristics and compositions of the coated substrate. an accumulation of C particle on the surface as shown in the Fig. 3. The
The N2 flushing was performed before and after each batch of coating to occurrence of this type of defect may be due to the transition layer
provide a quality coating. where Cr percentage became lesser than C, as poor adhesiveness or
uneven coating on the substrate. Because, a single DLC coating may
have poor adhesion with the substrates, a Cr layer is added to achieve
3. Results and discussion better adhesiveness behavior with the steel substrate [1]. The presence
of Fe in a higher amount of 4 wt% could be related to delamination of
3.1. Morphology of coated sample coated particles. However, the deposition of particles was influenced by
rate of deposition and surface condition before coating. Therefore, the
The coating was done at the guide and seat of nozzle needle by Cr- N2 flushing is considered as potential route to reduce these defects and
DLC layers via PECVD technique. However, the deposited coating was maintain a proper flow rate of deposition.
considered to be dense and the uniform. The needle was examined after
coating using SEM morphology (Fig. 2).
It was observed that few white spots were agglomerated on the 3.2. Adhesive performance
surface. Those are defects generated due to the improper deposition
during transition layer after Cr deposition. Therefore, the rate of de- The adhesive performance was examined through indentation
position was considered to be an important parameter which can affect technique. Here, the hardness was obtained by conducting trials, on
the quality of deposition [13]. To understand the surface of white spots three coated substrates from four different batches, by indentation
were conducted chemical composition scanning using Energy-dis- using rockwell hardness tester as presented in Fig. 4. The adhesion trials
persive X-ray spectroscopy (EDX) (Fig. 3). The EDX analysis has re- made over the coating deposited without N2 flushing indicate that the
vealed that the spectrum 1 contains 24.70 wt% C, 59.11 wt% Cr and Cr-DLC coating do not perform very well, hence, it demonstrates low
resistance to crack formation as is shown in Fig. 4(b, c, d).
This observation made on the Cr layer can indicate the poor adhe-
siveness between Cr layer and C-layers when is associated to high value
of load which is responsible for the adhesive failures of coatings [15].
The indented image of Cr-layered samples revealed fine transverse
cracks in and around the indentation due to the high hardness and
brittle nature of carbon. The result revealed that the hardness was
around 60 ± 0.5 HRC. There was no significant difference of hardness,
between uncoated and coated substrates. Nevertheless, the Cr-DLC dual
layer coating had shown a superior indentation morphology (Fig. 4a).
The evaluation was performed on a scale from HF 1 (stated as very good
adhesion) to HF 6 (insufficient adhesion) in accordance to VDI 3198
[16]. The Fig. 4a shows the absence of delamination that is associated
to a strong interfacial bond. On the other hand, the identical type of
coating produced on similar substrate (Fig. 4b, c, and d) indicates very
poor adhesion and notable number of radial micro-cracks and delami-
nated [16–18]. Accordingly, it was noted that N2 flushing is playing a
Fig. 2. Droplet defect on the surface of coated nozzle and view of defected significant role and enable an increased adhesiveness of interfacial
portion using SEM morphology. bonding between Cr and its C substrate. In the as-deposited state, the

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A. Muthuraja, et al. Diamond & Related Materials 100 (2019) 107588

Fig. 3. SEM and EDX morphology showing the droplet defect on the surface of coated nozzle needle.

Fig. 4. Optical images presenting the failure patterns of the Cr-DLC coated nozzle needle after indentation: (a) with N2 flushing, (b, c and d) without N2 flushing.

4
A. Muthuraja, et al. Diamond & Related Materials 100 (2019) 107588

Fig. 5. The failure patterns on the Cr-DLC coatings deposited on high carbon steel after calowear test; with effective flow rate and with N2 flushing (upper left
picture); with uneven effective flow rate and without N2 flushing.

indentation results indicate values in range of HF 2 to HF 3 for system A

whereas an HF 4 for system B. They are both rated as acceptable ad-
hesion quality with the gradient system being slightly superior. By the
event of indentation, severe tensile stresses may be induced in the
azimuthal direction [16]. Due to this fact, the test cannot be treated as
fully reliable adhesion evaluation. Therefore, the results should be
considered with an appropriate degree of caution for Cr-layer thickness
measurement.

3.3. Cr-layer thickness measurement

The calowear test has been used to assess the tribological properties
up to 100 μm thick coatings. Fig. 5 shows the worn-out coated surface
after calowear test. Wornout surface was clearly visible, in the direction
of sliding, in the all test materials. Microcutting caused by the diamond
slurry, on the test surface, was observed but no asperity deformation
traces were observed. From the worn-out image, the thickness of Cr-
layer was detected as tcr = (D3 − D2) / 2 and C-layer, tc = (D1 − D2) /
2. It was observed that superior wear resistance is achieved in the case 2 µm
of effective flow rate and a proper N2 flushing. Fig. 5 shows severe wear
track due to weakness in the transition layer of the coated surface
[19,20,22–26]. It was revealed that the thin films exhibited a high Fig. 6. The cross-sectional view of Cr-DLC coated substrates.
friction coefficient. From these results, it is concluded that the wear
rates of DLC films are influenced by the counter material [21,27–29]. pull-out of hard particles were identified as the main mechanisms of the
The adhesiveness of Cr with DLC cause a lower friction behavior due to DLC coatings deposited on the as-sintered substrate [12,31].
superior bonding as presented in Fig. 5. The better quality of coating
has confirmed the superior adhesiveness between the Cr-C: H layers. It
provides as well as high tribological properties when is applied the 3.4. Effect of N2 flushing
nitrogen flushing. Similarly, were observed that the DLC specimen
shown a prominence in C]O and COOH bonds and better corrosion Fig. 7 shows the statistical analysis that has been performed for a
resistance as that of Nitrogen-doped DLC specimen [30]. period of 15 months. It indicates that the N2 flushing as being a sig-
The cross-sectional view was observed having a uniform thickness/ nificant route to overcome the adhesives problem and defective out-
quality of coating on the substrates. Fig. 6 shows the cross-sectional puts, which allows finally improving the quality of coated substrates.
view of Cr-DLC coated substrates. There, we can note slightly the The statistical data demonstrates that the defects rate achieved through
weakness occurred at the interface between the Cr-layer and substrate N2 flushing can be reduced to a minimum that is around 0.2% of re-
C:H. The insufficient bonding that describes this interface can be re- jection. However, the rejections without N2 flushing can be much
sponsible of premature failure in adhesiveness when submitted to heavy higher, up to 1.2%, and at the peak period when the requirement are
mass. The large portion of carbon coating on the Cr surface tends to higher (during months (March and October)), there, is a possibility to
have loose particles on the outside surface. The wear performance obtain even a more higher rejection rate. These observations clearly
achieved on the DLC films, deposited on sintered specimen, is close demonstrate the importance of N2 flushing as parameter index to obtain
related to an improvement on the adhesive strength. Adhesive wear and a superior coating quality.

5
A. Muthuraja, et al. Diamond & Related Materials 100 (2019) 107588

Fig. 7. The failure patterns on the Cr-DLC coatings deposited on high carbon steel after calowear test.

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