Journal of Ceramic Processing Research. Vol. 25, No. 1, pp.

79~84 (2024) J O U R N A L O F
(Received 7 November 2023, Received in revised form 8 December 2023, Accepted 11 December 2023)
https://doi.org/10.36410/jcpr.2024.25.1.79 Ceramic
Processing Research

Comparative study between hot isostatic pressing and pressure less sintering
for self-lubricating CuO/ZTA composites
K. Rajaa,*, M. Dhanabalb, Bipin Kumar Singhc and P. Ganeshanc
a
Department of Mechanical Engineering, Anna University Regional Campus Coimbatore, Coimbatore- 641046, Tamil Nadu, India
b
Department of Mechanical Engineering V.S.B. Engineering College, Karur – 639111, Tamil Nadu, India
c
Center for Augmented Intelligence and Design, Department of Mechanical Engineering, Sri Eshwar College of Engineering,
Coimbatore - 641202, Tamil Nadu, India

Self-lubricating composite, comprises of CuO/ZTA is developed for its application as cutting inserts. The powders of zirconia
toughened alumina (ZTA) is prepared through co-precipitation process, further mixed with MgO particles (act as sintering
aid) and CuO (provide self-lubrication) using mechanical assistance. After mixing the homogeneous composites are used
to fabricate the Inserts obeying powder metallurgy process sintered through Hot isostatic pressing (HIP) and cold press
technique. The sintered samples are cut to size using diamond wheel on tool grinder machine. The geometry of inserts are
maintained according the international (ISO) standard SNUN 120408. The mechanical characterizations of developed
inserts are carried out on mirror polished samples. Crack bridging and crack deflection are the influential phenomenon
on the fracture toughness, whereas impurity phases of CuO at grain boundary result in little decrement in hardness. After
mechanical characterization the inserts are used to machine AISI 4340 steel on conventional N-26 lathe. Flank wear after 5
min of machining for all inserts are calculated at fixed set of machining parameters to explore the performance of indigenously
developed inserts. The self-lubrication phenomenon showed its effect on tool life i.e. thin layer (Patchy layer) formation
increases the life of novel inserts.

Keywords: CuO/ ZTA, Self-lubrication, Machining, Flank wear.

Introduction for machining of grey cast iron probably takes place in

1930s but lack of knowledge on fabrication technologies
High precision at minimum machining costs always on ceramics, its commercial application was limited till
attract attention of industries due to critical link with 1970s [6]. Thanks to the invention of advanced ceramic
profit and quality of manufactured component. To composite that explored numerous of fabrication process
achieve high precision of components, cutting inserts that open the application of ceramic in every sector
plays vital role as it is responsible for conversion of raw most important as cutting inserts. The first commercial
material to finish product through chipping technology. ceramic tool was made up of HP aluminium oxide
The recent paradigm of Industry 4.0 indeed require reinforced with titanium carbide showed an excellent
prolong useful tool life at minimum cost, to omit result over traditional tools [7]. Further development
the auxiliary cost of machining incurred by coolants, in properties of ceramic by reinforcing some additives
grinding of tool, grinding worker, and handling time made these tool capable to machine the 60-63 Rc
to replace the tool at regular interval. Therefore, to with superior surface finish [8]. Furthermore, the
short out the auxiliary costs ceramic cutting tools are improvements in strength imparted through dispersion
highly acknowledged [1-3] that showed huge potential to techniques of additives lead to multifarious application
sustain in harsh environment with prolong tool life. The in every industry. Later Claussen, 1976 [9] and Gravie
high hardness, high mechanical properties, resistance to [10] explored the concept of toughening phenomenon
wear, fracture and chipping along with high hot hardness by dispersion of ZrO2 in alumina matrix acted as
are some ideal properties that all govern by ceramic revolutionary mechanism in the application of alumina
tool [3-5]. Furthermore, the application of ceramic tool ceramic as cutting tool. The developed composites is
to achieve mass production in manufacturing industries known as zirconia toughed alumina (ZTA) that have
is also possible. The advent of ceramic as cutting tool peculiar volume expansion properties responded with
critical shear strain value. The mechanism illustrated
that during transformation of tetragonal crystal structure
*Corresponding author:
Tel : +91 8110057539 (t) to monoclinic crystal structure (m) phase dispersed
E-mail: [email protected] zirconia particles expand their volume by ~3-4 percent

79
80 K. Raja, M. Dhanabal, Bipin Kumar Singh and P. Ganeshan

[11] result in exception high fracture toughness sector. The application of ceramics is also showed by
value. Recent inventions of hot pressing (HP), spark various researchers [24-26] that have huge potential to
plasma sintering, and microwave sintering technologies replace conventional systems in manufacturing sector.
provide high mechanical properties in-situ with simpler Hence, the study from above literature suggested
fabrication process, bring the ceramic components for huge potential of self-lubricating composites towards
real world application [12]. Increase in the demand its application as cutting inserts. Furthermore, the
of ceramic materials shouted another challenge of uniform microstructure maintained in the ceramic
inferior tribological properties, also applicable with the always play significant role in strength, or fracture
ceramic cutting tool. So, at start the said challenges are toughness, dependent on sintering mechanism. The
encountered by providing coating to the ceramic tools, efficient sintering process for CuO/MgO/ZTA is still
but these coating are effective only upto the film exist. inconclusive and direly require through investigation for
It was observed that after few minutes of machining the its effective application as cutting tool. Therefore, in this
problem again reached to initial state. To encounter such study two sintering process are carried out i.e. pressure
problem scientific community invented novel concept less sintering and hot isostatic pressing (HIP) to densify
i.e. reinforcing third phase material inside the matrix the composites for its application as cutting inserts.
that act as lubricant. The concepts have well worth The studies also reveal the machining performance of
and acted as a pioneer concept towards development developed inserts for machining of AISI 4340 steel. The
of self lubricating composites. After postulation of predominant physics that lies to improve and degrade
such concepts numerous of researches were dedicated the properties are also thoroughly discussed.
to develop self lubricating materials by doping the
hard matrix of ceramic with soft additives like CuO, Process Opted to Manufacture
Graphene, SiCp, CaF2, h-BN, MoS2 etc. [13-16]. In Self-Lubricating Inserts
this regard, Dey et al. [17] reinforced several metal
oxides of Cu, Ti, Mg, Zn, Mn inside the zirconia In ceramics preparation procedures play a vital effect
toughened alumina (ZTA) composites to improve on the end properties. Hence in this investigation all
the tribological properties. All developed composites the standards have been strictly followed in order to
showed improvement in tribological properties but develop the self-lubricating CuO/ZTA composite. In
highest improvement was noticed for Cu doped ZTA the aforementioned composite, copper oxide (CuO)
due to formation of CuO that result in formation of act as a lubricant, and zirconia toughened alumina
soft thin layer (patchy layer) at interface responsible (ZTA) as parent matrix. The requisite amounts of
for improvement in tribological properties. Xing et al. compounds i.e. 1.5 wt% CuO, remaining ZTA were
[18] developed self-lubricating composite by coating selected from earlier optimization work carried out by
with Ni-MoS2-Al2O3 particles using laser powder-bed the Co-authors [27]. In aforementioned research work
fusion (additive manufacturing technique)on high-speed the quantity of CuO was varied from 0.5 wt.% to 5
steel cutting tools (HSS). The novel tool showed an wt.% inside ZTA matrix. The functional as well as
improvement of 8.8-11.7% in co-efficient of friction mechanical properties for each sample were carried
(COF) whereas, reduction in cutting force and power out. The research showed 1.5 wt.% CuO doped ZTA
by 17.6-29.6% and 17.3-22.0% respectively, compared had minimum CoF as value of 0.24 also poses highest
with conventional HSS tool. Gupta et al. [19] explored fracture toughness and flexural strength with a little
the concept of textured tool that efficiently improved compromise in hardness. Furthermore, the composition
the useful tool life and minimizes the cutting force by of ZTA comprises alumina and yttria stabilized zirconia
incorporating self lubricating phenomenon. Parihar et al. in the ratio of 90 : 10 were maintained in all composites.
[20] used spark plasma sintering technique to develop In this investigation, at first ZTA was prepared using
self-lubricating cutting tool made up of functionally co-precipitation route considering all nitrate salts of
graded cemented tungsten carbide with solid lubricant. high purity more than 99%. The requisite amounts
The developed insert showed huge potential for dry of salts were properly mixed in distilled water using
machining suited for manufacturing industries for mass magnetic stirrer followed by drop wise mixing of 0.1
production. Fangyuan et al. [21] used laser cladding mol% ammonium nitrate through a burette. The mixing
technique to fabricate the cutting inserts of (TiBw was continued till the pH of solution not reached to
+TiCp)/Ti composite for application as cutting inserts. 9 maintaining the temperature of 70 ˚C. The selection
Tremendous improvement in plastic deformation was of nitrate salts for preparation of ZTA composites
observed with cladding technique consequences in is based on easy dissolving nature of nitrate ions in
high useful tool life. Recently, Singh et al. [22, 23] warm water that can remove out easily during filtration.
successfully developed CuO/MgO/ZTA self-lubricating Furthermore, the pH plays a vital role for complete
inserts to demonstrate its machining performance and formation of precipitate that decides the properties of
fracture mechanism for AISI 4340 steel. A huge developed composites. It is found that the complete
potential of such compsites is found in manufacturing formation of precipitates generally occurs at pH 9. So,
Comparative study between hot isostatic pressing and pressure less sintering for self-lubricating CuO/ZTA composites 81

in this experiment the composites were prepared by process were opted for better comparison and clear
maintaining the pH 9. Furthermore, the agglomeration of understanding behind the physics of sintering process.
particles during precipitation is avoided by maintaining
a temperature around 70 ˚C. The formed precipitate was Process opted for Morphological investigation
decant from water and pour into a filter unit where, The fully densified samples were selected for morpho

­
warm water are mixed to remove the nitrate ions present logical study using FESEM images. The images were
in the precipitate. After complete removal of nitrate ions, taken at same magnification for better comparison of
the jelly cakes of ZTA composites were kept in an grains formed after sintering. The phases present inside
oven for 12 h. The dried mass were crushed manually the matrix were evaluated through XRD technique in
and kept at 800 ˚C for calcination. The calcined ZTA the angle (2θ) lies between 20° and 70°.
powders were further used to mixed CuO and MgO
using powder metallurgy route. The powders of 1.5 wt.% Process opted for Mechanical properties investigation
CuO were thoroughly dispersed in alcoholic medium After phase evaluation the bulk density of polished
using probe sonicator. The dispersed powders were kept samples were evaluate through Archimedes principal.
in zirconia jar with requisite amount of ZTA powder The relative density i.e. ratio of bulk density to theoretical
under alcoholic medium. The alumina balls of different density were calculated for better understanding of
sizes (diameter 8, 10, 12 mm) were also placed inside densification. Furthermore, the mechanical properties
the zirconia jar to obtain better attrition effect during i.e. hardness and fracture toughness were evaluated on
milling. The jar was fully tightened and fixed on a Vickers testing machine. An average of ten reading for
planetary ball mill. The powders were milled for next hardness and five readings for the fracture toughness
12 h under a rotational speed of 360 rpm. The perfectly were consider to cite the value of hardness and fracture
milled powders were dried and calcined at 800 ˚C to toughness.
remove all impurities. The calcined powders were mixed
with PVA solution for granulation. After granulation the Process opted for Machinability investigation
powders were sintered using two processes the first one The perfectly shaped inserts as per SNUN 120408
is pressure less sintering and second one is hot isostatic were selected to evaluate the machining performance in
pressing (HIP) technique. In cold pressed technique the terms of flank wear during machining of AISI 4340 steel
requisite amount of powders were pressed at pressure on the conventional lathe. The tool signature maintain
of 500 MPa on a hydraulic press. The pressed samples on tool holder (made: NTK) as -6o, -6o, 6o, 6o, 15o,
were slowly removed from the die and kept in a ceramic 15o, and 0.8 mm. Piezoelectric dynamometer (make:
crucible. The samples were fully covered with alumina Kistler, model: 9272) fitted at tool post just below
powders for uniform distribution of heat and kept in a the tool holder was used to measure the cutting force.
HT furnace at a temperature of 1500 ˚C for half hour After every pass of machining the surface roughness of
as soaking time. In another process the developed CuO/ machined surface was measured thorough SURTRONIC
ZTA composites powders were pour into the graphite 25. Averages of ten readings were used to cite the
die for compaction and sintering at a pressure of 500 surface roughness. At last the flank wear after 5 min
MPa and temperature of 1500 ˚C using HIP technique. of machining was measured on the Tool Makers’
In this case also the heating time was maintained as Microscope. The parameter selected for machinability
half an hour. After sintering the samples were used evaluation were cutting speed as 300 m/min, depth of
for morphological characterization. After morphological cut as 1 mm and feed rate as 0.18 mm/sec based on
characterization the samples were thoroughly polished earlier investigation carried out by Singh et al. [28].
using silicon powder and diamond paste. After polishing
the samples were cut to size maintaining ISO SNUN Discussion on the Observed Results
120408 to develop the cutting insert for machining of
AISI 4340 steel. After imparting the shape and size the Analysis of Physical Properties
edges of inserts were beveled to impart strength. The The composites of ZTA/CuO are classified as self-
well finished inserts were again decomposed at 800 lubricating ceramics that have all necessary properties
˚C to reveal the stress developed during polishing and for prolong life. The composites fabricated through
imparting the shape. The heated inserts were used to powder metallurgy route in which earlier researchers [29]
machine AISI 4340 steel. revealed that CuO grain undergone liquid phase during
sintering operation. Furthermore, the research carried out
Experimental Investigation by Ran et al. [30] clearly demonstrated that the viscosity
flow of metal oxide was very low when reinforced
In this investigation three samples named as Z1 inside the YSZ or ZTA matrix. The flow restriction
for ZTA, Z2 for CuO/ZTA prepared through pressure maintained the homogeneous distribution of CuO inside
less sintering, and Z3 for CuO/ZTA prepared through the matrix after sintering, but restructuring of CuO grains
HIP technique. For every characterization the same could be possible. Hence, a comparative study between
82 K. Raja, M. Dhanabal, Bipin Kumar Singh and P. Ganeshan

Fig. 1. Final shapes and sizes of Cutting Inserts after Sintering.

pressureless sintering (conventional sintering) and hot

pressing technique during densification was investigated.
The images of all three samples Z1, Z2 and Z3 after
sintering are shown in Fig. 1. From images it can be
observed that the homogeneously structure with uniform
distribution of CuO grains is observed in case of Z3.
The XRD plot of Z1, Z2 and Z3 samples are shown
in Fig. 2. The homogeneous mixing of CuO inside
the matrix alongside low amount of CuO (beyond the
detection limit of XRD) make difficult to identify the
phases through XRD phase analysis.
The evaluated values of bulk density, hardness and
fracture toughness are shown in Fig. 3(a), (b) and (c).
From figure it can be observed that the bulk density
of Z2 samples i.e. pressure less sintering have lowest
density than Z2 and Z3 samples. Whereas, approximately Fig. 2. XRD plot of Z1, Z2 and Z3.
similar value of bulk density is observed for the Z2
and Z3 samples. The result is attributed to the uniform
grain sizes present inside the cluster which is high for but the value of hardness for Z2 and Z3 is lower than
Z3 samples. This may happen due to controlled pore Z1 sample. This result observed due to creation of
mobility rate that have huge impact on the grain growth impurity phases at the grain boundary by presence of
predominant in case of HIP sintering. The simultaneous CuO particles. The earlier researchers illustrate that the
action of pressure and temperature restrict the pores presence of CuO particle inside the cluster make Cu-
consequences in the uniform grain size. Whereas, in enrich phases at the grain boundary. The Cu-rich region
case of Z1 and Z2 samples abnormal grain growth is crates a weaker section in the cluster and can be easily
noticed due to uncontrolled capability of temperature deformed. The presence of such region exaggerated the
(i.e. temperature didn’t affect the pore mobility rate) to propagation of crack or larger deformation result in
restrain pore mobility rate. The results are in agreement lower value of hardness in the both Z2 and Z3 samples.
with earlier research carried out by Pratap et al. [31]. Interesting results are observed for Z2 and Z3
The investigation on hardness shown in Fig. 2(b) samples in which high fracture toughness is higher
also replicate the same results as observed for density, than parent matrix Z1. This result may be due to

Fig. 3. Mechanical properties i.e. bulk density, hardness and fracture toughness of Z1, Z2 and Z3 samples.
Comparative study between hot isostatic pressing and pressure less sintering for self-lubricating CuO/ZTA composites 83

formations of films at the interface during machining

consequences in the restriction of adhesive wear, that
also controls the flank wear.

Conclusion

Investigation successfully showed comparative study

between pressure less sintering and hot static pressing
to develop homogeneous CuO/ZTA composites. The
result shows slight decrement in mechanical properties
with incorporation of CuO particles inside the ZTA
matrix. A beneficial effect on the fracture toughness is
observed with the incorporation of CuO particles. The
machining result shows that inserts prepared through
HIP technique have high longer life compared to other
inserts. The uniform distribution of CuO particle formed
Fig. 4. Comparative result of flank wear after 5 min of machining.
a thin layer at the interface responsible for increase in
the tool life.
predominant behavior of crack bridging and crack
deflection phenomenon inside the cluster exaggerated
Acknowledgments
by presence of Cu-grains. The results are in agreement
The author like to thanks Principal and Director of Sri
with the Oh et al. [32] who demonstrated that the
Eshwar college of engineering for their supports. Also,
ductility of second phase grain inside hard matrix act
the authors thanks to the staff member of Department
as barrier for propagation of crack or shock the stress
of Mechanical Engineering staff (DST-Fist Sponsored
need to propagate the crack through plastic dissipation.
Department) for continuous support to carried out this
Furthermore, the dissipation of acoustic waves act as
work.
relief of stress required higher amount of energy for
crack propagation ultimately result in high value of
fracture toughness. Funding:
Fund received by DST-INDIA-FIST Program-2022
[TPN-83971] (SR/FST/College-/ 2022/ 1300).
Analysis of machining performance
The performance of any cutting inserts is entirely
dependent on the tool life which is changing with Conflicts of interest/Competing interests
materials properties. In this investigation, Z1, Z2 and No conflict between the authors.
Z3 composites are selected to fabricate the three cutting Availability of data and material
inserts. These inserts are tested on conventional lathe All data are presented in the manuscript
maintaining the ISO Standard 3685 for calculating
tool life illustrated by Kumar et al. [33]. Researchers Authors' contributions
demonstrated that when the average flank wear exceed K Raja: Formal analysis, Methodology, Supervision,
0.3 micron the tool is considered to be rejected. So, Dhanabal M: Validation, Visualization, Bipin Kumar
an optimized condition i.e. cutting speed of 300 m/ Singh: Experimentation, Validation, Visualization, P.
min, feed rate of 0.16 mm/min and depth of cut as 1 Ganeshan: Write-up, Visualization
mm based on the earlier research of Singh et al. [34]
are selected to evaluate the machining performance. References
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