metals

Article
Microstructure and Mechanical Properties of
Thixowelded AISI D2 Tool Steel
M. N. Mohammed 1, *, M. Z. Omar 2 , Salah Al-Zubaidi 3 , K. S. Alhawari 2 and M. A. Abdelgnei 2
1 Department of Engineering & Technology, Faculty of Information Sciences and Engineering,
Management & Science University, Selangor 40100, Malaysia
2 Department of Mechanical and Materials Engineering, Faculty of Engineering and Built Environment,
Universiti Kebangsaan Malaysia, Selangor 43600, Malaysia; zaidiomar@ukm.my (M.Z.O.);
alhawary.khaled@yahoo.com (K.S.A.); mnel_abdelgnei@yahoo.com (M.A.A.)
3 Department of Automated Manufacturing Engineering, Al-Khwarizmi college of Engineering,
University of Baghdad, Baghdad 10071, Iraq; salah_mfeng@yahoo.com
* Correspondence: mohammed.ukm@gmail.com; Tel.: +60-111-123-5993




Received: 9 March 2018; Accepted: 19 April 2018; Published: 4 May 2018


Abstract: Rigid perpetual joining of materials is one of the main demands in most of the
manufacturing and assembling industries. AISI D2 cold work tool steels is commonly known as
non-weldable metal that a high quality joint of this kind of material can be hardly achieved and almost
impossible by conventional welding. In this study, a novel thixowelding technology was proposed
for joining of AISI D2 tool steel. The effect of joining temperature, holding time and post-weld heat
treatment on microstructural features and mechanical properties were also investigated. Acceptable
joints without defect were achieved through the welding temperature of 1300 ◦ C, while the welding
at lower temperature resulted in a series of cracks across the entire joint that led to spontaneous
fracture after joining. Tensile test results showed that maximum joint tensile strength of 271 MPa was
achieved at 1300 ◦ C and 10 min holding time, which was 35% of that of D2 base metal. Meanwhile,
tensile strength of the joined parts after heat treatment showed a significant improvement over the
non-heat treated condition with 560 MPa, i.e., about 70% of that of the strength value of the D2 base
metal. This improvement in the tensile strength attributed to the dissolution of some amounts of
eutectic chromium carbides and changes in the microstructure of the matrix. The joints are fractured
at the diffusion zone, and the fracture exhibits a typical brittle characteristic. The present study
successfully confirmed that by avoiding dendritic microstructure, as often resulted from the fusion
welding, high joining quality components obtained in the semi-solid state. These results can be
obtained without complex or additional apparatuses that are used in traditional joining process.

Keywords: thixowelding; thixojoining; semisolid joining; cold-work tool steel

1. Introduction
Recently, AISI D2 tool steel get significant attention in the wide applications of industrial sector
owing to its attractive properties. Unfortunately, a high-quality joint of this type of material can be
hardly achieved and almost impossible by conventional welding methods owing to its high carbon and
alloying elements content with an enormous amount of carbides. The existing fusion welding technique
is the most commonly used process and has been widely practiced in industries. In this process, the
welding is used with preheating and post-weld heat treatment (PWHT) to avoid solidification cracking
and residual stresses that induced by the phase transformations throughout the welding. The most
critical part in the process is the heat affected zone (HAZ), which can be very hard and brittle, along
with susceptive to cracking if the tools are not heat-treated correctly.

Metals 2018, 8, 316; doi:10.3390/met8050316 www.mdpi.com/journal/metals

Metals 2018, 8, 316 2 of 16

In addition, fusion welding technologies are characterized by high temperature gradients that
results in high thermal stresses and a fast solidification, which lead to the occurrence of segregation
phenomena. Furthermore, the interface morphology is characteristically dendritic and the natural
progression of solidification commonly leads to interior structural defects, such as shrinkage porosities
and non-homogenous microstructure [1]. Therefore, an innovative route that can avoid the above
mentioned problems inherent in fusion welding is required. Thixojoining is a possible technique that
can weld the AISI D2 cold-work tool steel free from the above mentioned problems, as the process is
carried at the semisolid state where the mechanisms of solidification and heat flow are different from
other welding processes [2–4].
During the last 30 years, several authors have shown that the thixojoining process has the
potential to be used for a wide range of metal production processes. Notwithstanding some technical
and technological differences between the available semi-solid joining processes, they can be classified
into four categories: (1) joining metals by using semisolid slurries, (2) addition of functional features,
(3) semisolid stir joining, and (4) semisolid diffusion joining [2].
The first method involves the utilization of a thixotropic metal as filler applied into the joint
groove for the purpose of joining materials. This kind of joining has the distinctive advantage of
allowing a controlled flow during deposition process. Moreover, the applied temperatures and thermal
gradients are considered smaller if compared with fusion welding. Earlier research work in the 1990s
has demonstrated the feasibility of the process when Mendez and Brown used Sn-5 wt. % Pb as a filler
and applied it on the joint groove to join bars of Sn-15 wt. % Pb model alloy. The microstructure of
the joint cross-sectional area showed excellent metallurgical joining with the interface connection and
smooth and homogeneous welding between the bars and filler metal without defects or adverse effects
in the heating zone [5].
Other researchers have more investigations in the field of semisolid joining revealed the possibility
of producing prototype components by combining the forming operation with the simultaneous
insertion of additional components [6]. One special approach that takes advantage of the material’s
high flowability is the addition of functional features to a forged part. With this technology, it is
possible to shorten conventional process chains and to create a new generation of components. Kiuchi
et al. [6] studied the possibility of joining aluminum with aluminum and steel alloys. They found
that thixojoining of simple insert shape with bulk material is promising approach. With decreasing of
liquid fraction, there was increasing in joint strength. This clarifies the significant merits compared
with conventional casting due to formation of intermetallic compounds and diffusion between base
and insert materials. The big challenge of improvement this technique for other materials is accessible
inserting component in mushy matrix with destruction of joint geometry by remelting or deformation.
Further investigations in Semisolid stir joining (SSSJ) showed the applicability of this type of
joining process to improve and overcome the difficulties accompanied with current joining techniques
which were based on friction stir welding. Recently, there was trend toward carrying out a vacuum-free
SSSJ process that enables using low joining temperature when applied to a semisolid base or filler
metal. Hosseini et al. [7] have also carried out extensive experiments on semisolid stir joining (SSSJ)
for AZ91 alloy by using mechanical stirring and a Mg-25 wt. % Zn interlayer. The results showed the
significant effect of mechanical stirring rate on the joint-strength. This supposes that the formed oxide
layer has been disrupted due to stirring effect and consequently improve metallurgical bonds. They
claimed that this method can be used as an alternative joining for Mg-based alloys.
More investigations to achieve joint with high-quality globular structure were undertaken by
Mohammed et al. [8–10] in semisolid diffusion joining (SSDJ). Their research explored the possibilities
of joining semisolid AISI D2 tool steel with functional elements of the same material as well as with
other materials such as AISI 304 stainless steel by using a peculiar characteristic of the metals’ liquid
components. In their proposed method, when the interfaces of two metals are pasted together, the
liquid components present in both sides of these “semisolid metals” penetrate and diffuse through
the interface and then solidify together as one body. The experimental results showed that, the use of
Metals 2018, 8, 316 3 of 16

this technique can make homogeneous properties with high surface quality without any evidence of
porosity or microcracking.
The semisolid metal joining (SSMJ) process can be used for processing different net near net shape
components with complicated shape and geometries where other joining processes cannot be utilized
for many reasons such as: low melting temperature, poor mechanical properties, and insufficient
plastic deformation. Several applications have been considered based on this new joining method like
heating radiator components, car shock absorber, slider system components and roller way elements.
In addition, this joining technology can be used for joining craft glass and stones to plates and bars
with different shapes. The products can be utilized in decoration various wall plates and floor panels.
Furthermore, metal/glass joining products have great capabilities to add other functional properties to
materials to produce lubricated, corrosion-proof, antiwear or heatresistant items [2].
The thixojoining is new semi-solid-based process that should take their place among other joining
processes. Nevertheless, it takes little considerations by researcher and investigators. This new specific
area needs continuous studies and works to overcome the related problem and propose solutions
and suggestions especially for high grade alloys and materials. In this work, the thixowelding
process was applied to join AISI D2 cold work tool steels by using a direct partial remelting method
(DPRM) method. The objectives of the present research are to study the microstructure evolution and
mechanical properties of the joints under different welding conditions.

2. Experimental Section

2.1. Materials and Sample Preparation

AISI D2 cold-work tool steel used in this study which was supplied after a soft annealing process,
i.e., heating to 850 ◦ C followed by cooling at 10 ◦ C/h to 650 ◦ C and finally air cooling. The chemical
composition of the studied AISI D2 cold-work tool steel was determined by using X-ray fluorescence
(XRF) (S8 TIGER ECO, Bruker, Karlsruhe, Germany) as shown in Table 1. The base blank of AISI D2
was cut Ø 16× 100 mm while the length of the pin insert was 18 mm with diameter of 7 mm as shown
in Figure 1. Each specimen was disposed of rust and scale by submerging in pickling solution, washed
with acetone, and finally rinsed using distilled water.
The temperatures of liquidus and solidus, in addition to liquid fraction, were estimated by carrying
out differential scanning calorimetry test (DSC). Small pieces samples (less than 20 mg) were cut from
the as-received material for testing with The Netzsch-STA 449 F3 simultaneous thermogravimeter
(TGA-DSC) (STA 449F3, NETZSCH, Bavaria, Germany). The samples were heated at a rate of
10 ◦ C/min in nitrogen atmosphere to prevent oxidation. The common tangent procedure is adopted to
estimate the liquid fraction. Finding out the fraction of liquid was done by integrating of partial areas
under the heating curves as shown in Figure 2.

Table 1. Chemical composition of AISI D2 cold-work tool steel (in Weight Percent).

C Si Mn P S Cr Ni Mo W Cu V Fe
1.50 0.258 0.24 0.02 0.01 11.2 0.21 0.78 0.2 0.08 0.781 Balance
Metals 2018, 8, 316 4 of 16
Metals 2018, 8, x FOR PEER REVIEW 4 of 16

Metals 2018, 8, x FOR PEER REVIEW 4 of 16

16mm

16mm
AISI D2

AISI D2
7mm 100mm

7mm 100mm
AISI D2
AISI D2

20mm
20mm

Figure1.1.Schematic
Figure Schematicdrawing
drawingofofthe
theAISI
AISID2
D2parts
partscombination.
combination.
Figure 1. Schematic drawing of the AISI D2 parts combination.

0.187
0.187 100
100
90 90
0.137
0.137 80 80
Heat flow/(mW/mg)
Heat flow/(mW/mg)

70 70

Liquid fraction
Liquid fraction
0.087
0.087 60 60
50 50
0.037
0.037 40 40
30
30
-0.013 20
-0.013 DSC/(mW/mg) 20
DSC/(mW/mg) 10
Liquid fraction 10
-0.063 0
Liquid fraction
-0.063 1220 1240 1260 1280 1300 1320 1340 1360 1380 1400 1420 0
1220 1240 1260 1280Temperature
1300 1320 (°C)
1340 1360 1380 1400 1420
Temperature (°C)
FigureFigure 2. Liquid
2. Liquid fraction
fraction vs.vs. temperatureand
temperature and heating
heating flow
flowvsvstemperature curves
temperature of the
curves of AISI D2 tool
the AISI D2 tool
steel steel calculated
calculated by differential
by fraction
differential scanning calorimetry
scanning calorimetry (DSC).
(DSC).
Figure 2. Liquid vs. temperature and heating flow vs temperature curves of the AISI D2 tool
steel calculated by differential scanning calorimetry (DSC).
2.2. Thixo Welding Process
2.2. Thixo Welding Process
2.2.HighHigh
Thixo temperature
Welding Processcarbolite furnace was utilised to carry out the thixo welding of AISI D2 tool
temperature carbolite furnace was utilised to carry out the thixo welding of AISI D2 tool
steel as shown in Figure 3. The furnace is vertical type and protected with argon gas. The moment
asHigh
steel thatshown temperature
furnace inreached
Figure the3.carbolite
The furnace
furnace
pre-selected was utilised
is vertical
temperature type
(1250, to
and carry
andout
protected
1275, 1300the
with thixo
°C),argon welding wasoflowered
gas. The
the sample AISI D2that
moment tool
◦ C), the sample was lowered into
steel
furnace as shown
reached in
the Figure 3.
pre-selectedThe furnace
temperature is vertical
(1250, type
1275, and protected
1300 with
into the furnace by use chromehromel wire for 0, 5 and 10 min respectively then it was allowed to argon gas. The moment
that
the furnace
cool
furnace byreached
slowly at room
use the pre-selected
temperature
chromehromel wire temperature
as shown
for 0, and(1250,
in 5Figure 4. To
10 min 1275, and 1300
investigate
respectively °C), the
the influence
then sample
of
it was post was lowered
welding
allowed to cool
intoheat
slowly attreatment
the furnace
room on the
by usemicrostructure
temperature as shownand
chromehromel mechanical
inwire
Figurefor4.0,To5properties
and of the
10 min
investigate welded plates,
respectively
the influence ofspecimens
then it was
post were
allowed
welding heatto
coolheat
treatment treated
slowly at by
on the heating
room the specimens
temperature
microstructure to 850–900
andasmechanical
shown in °C followed
Figure
properties 4. Toby slowwelded
rates ofthe
ofinvestigate
the furnace coolingof
influence
plates, (22post
specimens °C/h),
welding
were heat
when aheating
steel cools tospecimens
650 °C, air cooling can be
◦ Cused to bring the steelrates
to room temperature. ◦ C/h),
heat treatment on the microstructure and mechanical properties of the welded plates, specimens were
treated by the to 850–900 followed by slow of furnace cooling (22
◦ C, air cooling can be used to bring the steel to room temperature.
heat treated
when by heating
a steel cools
2.3. Metallography
to 650the specimens to 850–900 °C followed by slow rates of furnace cooling (22 °C/h),
when a steel cools to 650 °C, air cooling can be used to bring the steel to room temperature.
The thixowelded joint samples were polished and then etched by using Villela reagent (1 g picric
2.3. Metallography
2.3.acid, 5 mL hydrochloric acid, and 95 mL ethyl alcohol) to reveal their microstructures. The
Metallography
The thixowelded joint samples were polished and then etched by using Villela reagent (1 g
microstructures of the joints were characterized by Optics microscopy (BX51-P, Olympus, Tokyo,
picricJapan),
acid,thixowelded
The 5scanning
mL hydrochloric acid, were
joint samples
electron and(SEM)
microscopy 95 mL(LEO
ethyl
polished andalcohol)
then
1455 to reveal
VP etched
SEM, their
by using
Zeiss, microstructures.
Villela
Oberkochen, reagent The
(1 g picric
Germany)
microstructures of the joints were characterized by Optics microscopy (BX51-P, Olympus,
acid, 5 mL hydrochloric acid, and 95 mL ethyl alcohol) to reveal their microstructures. The Tokyo, Japan),
microstructures of the joints were characterized by Optics microscopy (BX51-P, Olympus, Tokyo,
Japan), scanning electron microscopy (SEM) (LEO 1455 VP SEM, Zeiss, Oberkochen, Germany)
Metals 2018, 8, 316 5 of 16

Metals 2018,
2018,8,8,xxFOR
Metalselectron
scanning FOR PEER
PEERREVIEW
REVIEW
microscopy (SEM) (LEO 1455 VP SEM, Zeiss, Oberkochen, Germany) equipped 55 of
of 16
16 with

energy dispersive X-ray spectroscopy (EDX) (Oxford 7353, Oxford Instruments, Wiesbaden, Germany).
equipped
equipped with with energy
energy dispersive
dispersive X-ray
X-ray spectroscopy
spectroscopy (EDX)
(EDX) (Oxford
(Oxford 7353,7353, Oxford
Oxford Instruments,
Instruments,
X-rayWiesbaden,
diffractionGermany).
(XRD) (Bruker
Wiesbaden, Germany). X-ray
D8 Discover,
X-ray diffraction
diffraction (XRD)
Bruker,
(XRD) (Bruker
Karlsruhe,
(Bruker D8
Germany)
D8 Discover,
Discover, Bruker,
analyses
Bruker, Karlsruhe,
were carried out
Karlsruhe, Germany)
Germany)
to analyze
analyses the
analyses were phases
were carriedpresent
carried out
out toin the
to analyzesteel
analyze the specimen
the phases before
phases present
present in and
in the after
the steel the thixojoining.
steel specimen
specimen before It
before and also
aftergives
and after the an
the
thixojoining.
thixojoining. ItIt also
idea about the also gives
gives an
characteristics an idea
ofidea about
about the
joints and the characteristics
if characteristics of
there is any of joints
joints and
harmful and ifif there
phase there is
or is any
brittleany harmful
harmful phase
phase havephaseformed
or
duringor brittle
brittle phase
phase have
thixojoining. have formed
formed during
during thixojoining.
thixojoining.

2.4.
2.4. Test Test
2.4.of
Test of
of Mechanical
Mechanical
Mechanical Properties
Properties
Properties
The
The mechanical
mechanical
The mechanical characterization
characterization
characterization ofof the
ofthe joints
joints was
thejoints was measured
was measuredusing
measured using
using tensile
tensile strength
tensilestrength
strengthand hardness
andandhardness
hardness
tests.
tests.The
The tensile
tensile tests
tests were
were carried
carried out
outon
on using
using Zwick
Zwick universal
universal testing
testing
tests. The tensile tests were carried out on using Zwick universal testing machine (ProLine Z005/Z100, machine
machine (ProLine
(ProLine Z005/Z100,
Z005/Z100,
Zwick,
Zwick, Ulm, Germany)
Germany) with aa cross-head
cross-head speed
speed ofof 0.5
0.5 mm/min
mm/min at at room
room temperature
temperature according
according to
Zwick, Ulm, Ulm,
Germany) with witha cross-head speed of 0.5 mm/min at room temperature according to to
ASTM
ASTM
ASTM E8M E8M Standards.
Standards. The The fracture
fracture morphologies
morphologies of of failed
failed specimens
specimens were were then
then observed
observed by by
E8M Standards. The fracture morphologies of failed specimens were then observed by scanning electron
scanning
scanning electron
electron microscopy
microscopy (SEM). (SEM). Vickers
Vickers micro-hardness
micro-hardness testingtesting (FH5,
(FH5, Tinius
Tinius Olsen,
Olsen, Horsham,
Horsham,
microscopy
PA,
PA, USA)
(SEM).
USA) was
Vickers
was performed
performed on
micro-hardness
on the
the polished
testing
polished specimens
(FH5, of
specimens of
Tinius
the
Olsen, Horsham,
the transverse
transverse section
section of
PA, USA)
of joints
joints as
was
as well
performed
well as
as the
the
on the polished
base
base material specimens
material andand insert
insert toof the
to comparetransverse
compare the section
the phases
phases present of
present injoints
in the as well
the joint
joint and as
and the the base
the joining material
joining parameters
parameters onandoninsert
the to
the
base
compare metal.
basethemetal. The
The profiles
phases presentof
profiles inmicro-hardness
of micro-hardness
the joint and the were
were constructed
constructed
joining across
parametersacross the
thethe
on sample’s
sample’s horizontal
horizontal
base metal. Thesection
section
profiles of
of
of the
the D2
micro-hardness D2 tool
tool steel base
base metal,
metal, the
steelconstructed
were the weld
weld
across zone
thezone and
and the
sample’s insert
insert by
thehorizontal by using
using aa load
section load of
of 10
of the 10
D2gg for
for
tool30 ss along
30steel
along
basethe
the
metal,
lines
lines perpendicular
perpendicular to
to the
the joint
joint interface.
interface. Hardness
Hardness measurements
measurements were
were
the weld zone and the insert by using a load of 10 g for 30 s along the lines perpendicular to the joint carried
carried out
out by
by using
using Vickers
Vickers
micro-hardness
micro-hardness
interface. tester
tester FH5.
Hardness measurements FH5. were carried out by using Vickers micro-hardness tester FH5.

Argon
Argon In
In
Thermocouple
Thermocouple

Furnace
Furnace tube
tube

Sample
Sample

Heating
Heating element
element

Furnace
Furnace casing
casing
25mm
25mm
Steel
Steel cup
cup

Steel
Steel plate
plate
Argon
Argon Out
Out

Figure
Figure 3.3.3.
Figure Schematic drawing
drawingof
Schematicdrawing
Schematic ofthe
of thefurnace
the furnace
furnaceset-up.
set-up.
set-up.

Temp.
Temp. (°C)
(°C)

Process
Process Temp.
Temp. Semi
Semi solid
solid zone
zone
Holding
Holding time
time

Air
Air cooling
cooling

Time
Time (minutes)
(minutes)

Figure 4. Temperature profile of direct partial remelting experiment.

Metals 2018, 8, x FOR PEER REVIEW 6 of 16
Metals 2018, 8, 316 6 of 16
Figure 4. Temperature profile of direct partial remelting experiment.

3.
3. Results
Results and
and Discussion
Discussion

3.1. Microstructure
3.1. Microstructure and
and Joint
Joint Quality
Quality
The microstructure
The microstructure of as-received AISI
of as-received AISI D2D2 consists
consists of of ferritic
ferritic matrix
matrix parallel
parallel to to working
working direction
direction
in which different surplus of large-coarse and fine carbides
in which different surplus of large-coarse and fine carbides are distributed as shown in Figureare distributed as shown in Figure
5. The5.
The revealed microstructure refers to annealed tool steel [11] and
revealed microstructure refers to annealed tool steel [11] and indicates that the heat treatment was indicates that the heat treatment
was carried
carried out asout as recommended.
recommended. The optical
The optical microscopy microscopy
examinationexamination
performed performed
on the welded on the joints
welded at
joints at various conditions is shown in Figure 6. From the complete weld section at 1250 ◦ C heating
various conditions is shown in Figure 6. From the complete weld section at 1250 °C heating
temperature with
temperature with 0,0, 55 and
and 10 10 min
min holding
holding time,time, large
large gap
gap cancan been
been seen
seen andand bigbig cracks
cracks at at the
the joint
joint
interface can be observed. With the increase of welding temperature to 1275 ◦ C with 0 and 5 min
interface can be observed. With the increase of welding temperature to 1275 °C with 0 and 5 min
holding time,
holding time, aa series
seriesof ofcracks
cracksresulted
resultedand andthe theweldweldseam
seamcould could not
not bebe wellwell joined,
joined, as as shown
shown in
in Figure
Figure 6S4,S5.
6S4,S5. In In addition,
addition, bigbig fractures
fractures across
across thetheentire
entirejoint
jointwere
wereshown
shownwith with little
little and
and local
local
interactions
interactions were were lactated
lactated at at different
different zones
zones in in the interface resulting
the interface resulting in spontaneous fracture
in spontaneous fracture after
after
joining. However, when the holding time is adequate (10 min) the weldability is relatively good and
joining. However, when the holding time is adequate (10 min) the weldability is relatively good and
there
there is is no
no macroscopic
macroscopic voids voids and and fractures
fractures across
across the the entire
entire joint
joint which
which is is occupied
occupied by byeutectic
eutecticliquid,
liquid,
◦ C, strong
as shown in Figure 6S6. Meanwhile, by further increasing the welding temperature to 1300 °C, strong
as shown in Figure 6S6. Meanwhile, by further increasing the welding temperature to 1300
thixojoint
thixojoint can can bebe produced.
produced. Further,
Further, finefine and
and small
small boundary
boundary can can bebe observed
observed as as transition
transition zone zone
between two alloys. No presence of porosity and micro-cracking at this zone and the joint shape was
between two alloys. No presence of porosity and micro-cracking at this zone and the joint shape was
smooth and not corrugated, as shown in Figure 6S7–S9. The thixoweld joint was characterised by
smooth and not corrugated, as shown in Figure 6S7–S9. The thixoweld joint was characterised by
visible
visible full
full penetration
penetration that that indicate
indicate perfect
perfect thixojoning
thixojoning betweenbetween base base blank
blank and and the the insert
insert along
along thethe
bounding border. Higher amount of the interfacial reactions has been produced between two base
bounding border. Higher amount of the interfacial reactions has been produced between two base
metals
metals [12].
[12]. The
The structure
structure is is distinguished
distinguished by by two
two features
features that
that can
can bebe determined
determined by by grain
grain direction,
direction,
as
as illustrated
illustrated in in arrows
arrows direction
direction in in Figure
Figure 7. 7. The
The direction
direction of of the
the grains
grains are
are inin bands
bands in in the
the forming
forming
direction and as a single pin of AISI D2 was inserted perpendicular into a base blank of AISI D2
direction and as a single pin of AISI D2 was inserted perpendicular into a base blank of AISI D2 to
to
illustrate
illustrate two two distinct
distinct features.
features. The The interfacial
interfacial reactions
reactions during
during heating
heating have
have accelerated
accelerated the the diffusion
diffusion
of elements through the interface and propagated the eutectic liquid across the joined surfaces that
of elements through the interface and propagated the eutectic liquid across the joined surfaces that
resulted in good thixojoint of the interface at both side of steels.
resulted in good thixojoint of the interface at both side of steels.
Additionally,
Additionally, the the properties
properties of of the
the thixojoining
thixojoining can can be
be improved
improved by by subsequent
subsequentheat- heat-treatment.
treatment.
It is clearly visible that the changes in the microstructure patterns of the thixojoining occur after
It is clearly visible that the changes in the microstructure patterns of the thixojoining occur after the
the
heat treatment as shown in Figure 8. It is obviously to see that the primary distribution of grain
heat treatment as shown in Figure 8. It is obviously to see that the primary distribution of grain
boundary
boundary is is decreased
decreasedsubstantially
substantiallyand andsome
someamounts
amountsofofeutecticeutecticcarbides
carbides dissolve
dissolve in in
thethematrix.
matrix.It
means that the primary grain boundaries have distinctly pinning effect on growth of grain size in
It means that the primary grain boundaries have distinctly pinning effect on growth of grain size in the
the
heat
heat treated
treated condition
condition [12].
[12]. The
The heat
heat treated
treated structures
structures of of the
the thixojoined
thixojoined parts parts onlyonly show show improved
improved
contrast between solid and liquid phases, whereby the big solids appeared in little liquid matrix.
contrast between solid and liquid phases, whereby the big solids appeared in little liquid matrix.

Figure 5. Optical microstructure of as received AISI D2 tool steel.

Figure 5. Optical microstructure of as received AISI D2 tool steel.
Metals 2018, 8, 316 7 of 16
Metals 2018, 8, x FOR PEER REVIEW 7 of 16
Metals 2018, 8, x FOR PEER REVIEW 7 of 16

Figure 6. Microstructure of the thixojoined samples processed at different conditions: (S1) 1250 °C/0
Figure 6. Microstructure of the thixojoined samples processed at different conditions:
Figure 6. Microstructure
min, (S2) of the
1250 C/5 min, (S3) thixojoined
1250 samples
°C/10 min, processed
(S4) 1275 at (S5)
°C/0 min, different
1275 conditions: (S1)1275
°C/5 min, (S6) 1250°C/10
°C/0
(S1) 1250 C/0 min, (S2) 1250 C/5 min, (S3) 1250 ◦ C/10 min, (S4) 1275 ◦ C/0 min, (S5) 1275 ◦ C/5 min,
◦
min, (S2) 1250 C/5 min, (S3) 1250 °C/10 min, (S4) 1275 °C/0 min,
min, (S7) 1300 °C/0 min, (S8) 1300 °C/5 min, (S9) 1300 °C/10 min. (S5) 1275 °C/5 min, (S6) 1275 °C/10
(S6) 1275 ◦ C/10 min, (S7) 1300 ◦ C/0 min, (S8) 1300 ◦ C/5 min, (S9) 1300 ◦ C/10 min.
min, (S7) 1300 °C/0 min, (S8) 1300 °C/5 min, (S9) 1300 °C/10 min.

Figure 7. Microstructure of thixo-weld-joint of (a) base metal, (b) diffusion zone (c) insert, after
Figure
Figure 7. Microstructure
7.
subjecting
Microstructure of
to 1300 °C heating thixo-weld-joint
of thixo-weld-joint of
of (a)
(a) base
temperature for 10 min.
base metal,
metal, (b)
(b) diffusion
diffusion zone (c) insert,
zone (c) insert, after
after
◦ C heating temperature for 10 min.
subjecting to
subjecting to 1300
1300 °C heating temperature for 10 min.
Metals 2018, 8, 316 8 of 16
Metals 2018, 8, x FOR PEER REVIEW 8 of 16

Metals 2018, 8, x FOR PEER REVIEW 8 of 16

Figure
Figure 8.
8. Microstructure
Microstructure of
of thixojoint
thixojoint parts
parts after
after application
application of
of 1300
1300 °C
◦ C for
for 10
10 min
min and
and subjected
subjected to
to
heat
heat treatment.
treatment.
Figure 8. Microstructure of thixojoint parts after application of 1300 °C for 10 min and subjected to
The heat treatment. also examined using SEM in order to get a complete assessment if there is any
The samples
samples were were also examined using SEM in order to get a complete assessment if there is any
harmful or
harmful orThe brittle
brittle phasehave
phase have formed during thixojoining. Figure 9 shows the Scanning electron
samples were alsoformed
examined during
usingthixojoining.
SEM in order Figure
to get a 9complete
shows the Scanning
assessment electron
if there images
is any
images of
of theharmful the microstructures
or brittle of
microstructures phase
of the
have formed
the thixojoint thixojoint
partsduring
and the parts and
thixojoining.
EDS spectra the
Figure
EDS spectra corresponding
9 shows thetoScanning
corresponding electron
the analyzed to the
phases.
analyzed
While, imagesphases.
SEM-EDX of theWhile,
elementalSEM-EDX
microstructures
mapping ofelemental
the mapping
thixojoint
techniques techniques
partsalso
was the EDSwas
andperformed also
spectra
on performed
corresponding
both sides at theon toboththesides
periphery
at the periphery
analyzed of
phases. the joint
While, in
SEM-EDXorder to determine
elemental mappingthe composition
techniques was of the
also
of the joint in order to determine the composition of the region near the diffusion zone of the joined region
performed near
on the
both diffusion
sides
zone of
part, at the
asthe
shownjoined
periphery part, as10.
of the
in Figure shown
joint inin Figure
order
Regarding to 10. Regarding
todetermine
Figures 9the to Figures
andcomposition
10, the EDX 9 and
of 10, confirm
the region
results thenear
EDXthe results
theconfirm
diffusion
that contact
that
area was identical in microstructure, composition, and properties with the base and insert. Onand
the
zonecontact
of the area
joined was
part, identical
as shown in microstructure,
Figure 10. composition,
Regarding to Figures 9 and properties
10, the EDX with
results the base
confirm the
insert.that the
thecontact area was identical in microstructure, composition, thatand properties with the base and of
basis ofOn element basis of element
distribution, it distribution,
can be deduced it can
thatbethe
deduced
both sides atthe
theboth sides
periphery at
ofthe
theperiphery
joint display
the insert.
joint On the abasis
display of element
uniform and distribution,
homogeneous it can be deduced in that thestructure
both sidesdueat the periphery of
a uniform and homogeneous distribution in thedistribution
structure due the thermal diffusion thermal diffusion
driving force [12].
the joint display a uniform and homogeneous distribution in the structure due thermal diffusion
driving force
Alongdriving
with this[12]. Along with this result, it was observed that the intermetallic compounds were not
forceresult, it was
[12]. Along observed
with thatit the
this result, wasintermetallic
observed that compounds
the intermetallic were not incorporated
compounds were not into
incorporated into the joining region, providing further evidence
the joining region, providing further evidence of the reliability of this process. of the reliability of this process.
incorporated into the joining region, providing further evidence of the reliability of this process.

Figure 9. SEM micrographs of thixojoined part at 1300 °C with EDX of point (1) for base metal, (2) for
Figure 9. SEM micrographs of thixojoined part at 1300 ◦ C with EDX of point (1) for base metal, (2) for
diffusion area and (3) for insert.
diffusion
Figure area and
9. SEM (3) for insert.
micrographs of thixojoined part at 1300 °C with EDX of point (1) for base metal, (2) for
diffusion area and (3) for insert.
Metals 2018, 8, 316 9 of 16
Metals 2018, 8, x FOR PEER REVIEW 9 of 16

Figure10.
Figure 10.SEM-EDX
SEM-EDXelemental
elementalmapping
mappingofofthixojoined
thixojoinedpart
partatat1300
1300◦ C
°Cofofresults
resultsnear
nearjoint:
joint:(a)
(a)SEM
SEM
micrograph,(b)
micrograph, (b)Fe,
Fe,(c)
(c)Cr,
Cr,(d)
(d)C,C,(e)
(e)V,V,
(f)(f)
allall
fourfour elements.
elements.

X-raydiffraction
X-ray diffractiontest
testhas
hasbeenbeencarried
carriedout outforformore
morecharacterisation
characterisationofofthixojoint
thixojointasasdisplayed
displayedinin
Figure 11. The analysis of the diffraction patterns of as-received tool steel found
Figure 11. The analysis of the diffraction patterns of as-received tool steel found peaks corresponding peaks corresponding
totothe
theferrite
ferritephase
phaseandandiron-chromium
iron-chromiumcarbide carbide(M (MC7C).3).From
7 3
Fromthe theother
otherside,
side,thethethixoweld
thixoweldatat1300 1300◦ C°C
isischaracterised
characterised by by three
three peaks
peaks refer
refer to
toaustenite
austeniteand andferrite
ferritephases
phases ininaddition
addition to to
M7M C3 carbides. The
7 C3 carbides.
presence of austenite is primarily connected with the increasing of carbon
The presence of austenite is primarily connected with the increasing of carbon in the solid solution in the solid solution that
stabilizing
that the the
stabilizing austenite
austenite [13]. Higher
[13]. Higher contents
contents ofofthese
theseelements
elementshave have aa significant effect on
significant effect onthe
the
martensitetemperature
martensite temperature andand consequently
consequently the transformation
the transformation of austenite
of austenite to martensite
to martensite is very
is very difficult.
In addition, when relatively fast cooling from the solidus–liquidus range is applied there is relativelyis
difficult. In addition, when relatively fast cooling from the solidus–liquidus range is applied there
relatively
better better
stability forstability for thephase
the austenitic austenitic
at roomphase at room temperature
temperature [14]. [14].
Meanwhile, analysis of the XRD patterns of the joined
Meanwhile, analysis of the XRD patterns of the joined parts after post parts after postwelding
weldingheat heattreatment
treatment
condition revealed a change of the structure character over the non-heat treated condition asasshown
condition revealed a change of the structure character over the non-heat treated condition shown
ininFigure
Figure10.10. As
As can
canbebeobserved
observedthat, that,thethemicrostructures
microstructuresare arecomposed
composedofofdifferent differentamounts
amountsofof
retained austenite, martensite and chromium carbides. Retained
retained austenite, martensite and chromium carbides. Retained austenite was recognised using austenite was recognised using
crystallographic data for austenite, while martensite was recognised with data for ferrite because ofof
crystallographic data for austenite, while martensite was recognised with data for ferrite because
similarityininthe
similarity thecrystal
crystalstructure
structureand andslight
slightdifferences
differencesininlattice
latticeconstants.
constants.The Thedecomposition
decompositionofof
metastable austenite in the structure was probably caused by the
metastable austenite in the structure was probably caused by the changes of carbon content. changes of carbon content.TheThe
effectofofslow
effect slowcooling
coolinggive
giveriserisetotodissolution
dissolutionofofaalarge largenumber
numberofofcarbide
carbideparticles
particlescausing
causingininan an
augmentation of retained austenite after post welding heat treatment
augmentation of retained austenite after post welding heat treatment condition. During the thermal condition. During the thermal
exposure,carbon
exposure, carbon migrates
migrates andand diffused
diffused deeperdeeper
to thetograin
the boundaries
grain boundaries
while some whileamounts
some amounts
of eutecticof
eutectic chromium
chromium carbidesindissolve
carbides dissolve in the
the matrix. matrix.that
It means It means that thegrain
the primary primary grain boundaries
boundaries have
have distinctly
distinctly pinning effect on growth of grain size in the heat treated condition
pinning effect on growth of grain size in the heat treated condition [15]. Based on these findings, no [15]. Based on these
findings,
harmful orno harmful
brittle phaseorwasbrittle phase by
detected wasXRD detected
patternsby XRD
at thepatterns
thixoweld at the
zone thixoweld
and thesezone and these
observations
observations
were were in good
in good agreement with agreement with microstructure
microstructure examinations. examinations.
 Metals 2018, 8, 316 10 of 16
Metals 2018, 8, x FOR PEER REVIEW 10 of 16

Figure 11.11.
Figure XRD patterns
XRD forfor
patterns AISI D2-AISI
AISI D2D2
D2-AISI joining processed
joining atat
processed different
differentconditions.
conditions.

3.2.
3.2.Mechanical
MechanicalProperties
Properties

3.2.1.
3.2.1.Tensile
TensileTest
Testand
andFracture-surface
Fracture-surfaceInvestigation
Investigation
ForForthe
thetensile
tensilestrength,
strength,six sixsamples
sampleswere wereprepared
preparedusing usingdifferent
differentjoining
joiningparameters
parameters(the (thefirst
first
three
threespecimens
specimenswith with 1250
1250 °C ◦ C heating temperaturewas
heating temperature wasneglected).
neglected).It Itis is believed
believed that
that thethe supplied
supplied heat
heat
inputinput
not not providing
providing sufficient
sufficient diffusion
diffusion withinwithin
the the
joint joint interface
interface eveneven
when when thethe holding
holding time time
was
was long.
long. Typical
Typical stress-strain
stress-strain curvescurves
for for
the the different
different testtest conditions
conditions are are
shown shown in Figure
in Figure 12. With
12. With high
high thixowelding
thixowelding temperature,
temperature, the produced
the produced interface
interface is freeisfromfree voids
from and
voids anddue
pores pores due diffusion
to high to high
diffusion rates of different elements across this area. Consequently,
rates of different elements across this area. Consequently, when this high temperature accompany when this high temperature
accompany with long
with long holding holding
time, time, high
high tensile tensile
strength strength
could could beItachieved.
be achieved. is well knownIt is well
thatknown that the
the strength of a
strength of a joint primarily depends on the quality of its microstructure.
joint primarily depends on the quality of its microstructure. As can be observed, the tensile strength As can be observed, the
tensile
graphstrength
shows a graph relatively shows a relatively
identical shape of identical shapeheating
the applied of the temperature
applied heating to 1300temperature
◦ C at 0, 5 and to
1300 °C at
10 min to 0, 5 and
give 241 10
MPa,min253 to MPa
give 241
and MPa,
271 MPa 253respectively.
MPa and 271AMPa minimumrespectively. A minimum
tensile strength of 241tensile
MPa is
strength of 241 MPa is recorded for the applied heating◦ temperature of
recorded for the applied heating temperature of 1300 C at 0 min. At 5 min a slight increment in tensile 1300 °C at 0 min. At 5 min a
slight increment
strength in tensile
was recoded. strength was
Meanwhile, withrecoded. Meanwhile,
10 min. holding time with
there10 min.
was holding time
remarkable there wasin
improvement
remarkable improvement
tensile strength due to fact in tensile strengthrate
that diffusion dueisto fact that
highly diffusion
affected rateofistemperature
by both highly affected andby both
time for
ofnon-steady
temperature and time for non-steady state diffusion. The tensile value
state diffusion. The tensile value of the D2 as-supplied material (791 MPa) is more than two of the D2 as-supplied
material
times if(791 MPa) is
compared more
with thethan two timesvalue
as-thixojoind if compared with This
of 271 MPa. the as-thixojoind
is actually anvalue of 271result
interesting MPa. whichThis
iswas
actually an interesting result which was achieved by a process which
achieved by a process which is simpler than conventional processes. Meanwhile, tensile strength is simpler than conventional
processes.
of the joinedMeanwhile,
parts after tensile strengthheat
post welding of the joined parts
treatment after post
condition showedwelding heat treatment
a significant improvementcondition over
showed a significant
the non-heat treatedimprovement
condition which overisthe560non-heat
MPa, i.e.,treated
about condition which is
70% the strength 560 MPa,
value of D2 i.e.,
baseabout
metal.
70%
Thisthe strength value
improvement of D2 base
of strength metal. to
is linked Thissuchimprovement
factors as the ofsize,
strength is linkedand
distribution to such factors asof
dissolvement
the size, distribution
carbides, and dissolvement
relative proportions of austeniteof carbides, relativephases,
and martensite proportions of austenite
and grain size. This and martensiteis
explanation
phases, and grain size.
also corroborated This explanation
by microscopic studiesiswhich
also corroborated
resulted in improvedby microscopic
contrast studies
betweenwhich resulted
solid and liquid
inphases,
improved contrast between solid and liquid phases, whereby the big
whereby the big solids appeared in little liquid matrix where primary distribution of grainsolids appeared in little liquid
matrix
boundarywhere primary distribution
is decreased substantially of and
grainsomeboundary
amounts is decreased
of eutecticsubstantially
carbides dissolve and some
in theamounts
matrix.
of eutectic carbides dissolve in the matrix.
The mechanical properties of similar substrates will have an important effect on the joints
The mechanical
properties because the properties
temperature of similar
attained substrates will havemarkedly
by each substrate an important depends effect
onon thethe joints
properties
properties because the temperature attained by each substrate markedly depends on the properties
of the materials and on the selected joining parameters. According to the Arrhenius equation, an
Metals 2018, 8, 316 11 of 16

Metals
of the2018, 8, x FORand
materials PEERonREVIEW
the selected joining parameters. According to the Arrhenius equation, 11 ofan
16
increase in the temperature will occasion an exponential enhancement in the diffusivity of solute [16].
increase in the temperature
Consequently, will occasionfor
the heating temperature an the
exponential
materialenhancement in the diffusivity
will have a substantial impactofonsolute [16].
the joint
Consequently, the heating temperature for the material will have a substantial impact on
properties. Weak joint may be produced if heating temperature is set on low level, even though if it is the joint
properties.with
combined Weak joint
high may be
holding produced
time. if heating
This resulted temperaturediffusion
in inadequate is set onalong
low level, even though
the interface if it
because
is combined
the elements with high
do not haveholding
enoughtime. Thisto
energy resulted
migrateinand
inadequate diffusion
diffuse within along the
diffusion interface
transition because
zone.
the elements do not have enough energy to migrate and diffuse within diffusion transition zone.
D = D* exp (−Qd / RT)
D = D* exp (−Qd / RT) (1)(1)
where D
where D isisthethediffusivity,
diffusivity, D* D*is temperature-independent
is temperature-independent preexponential (m2/s), (m
preexponential Qd2 /s),
is theQdactivation
is the
energy for diffusion (J/mol or eV/atom), R is the gas constant (8.31 J/(mol·K)
activation energy for diffusion (J/mol or eV/atom), R is the gas constant (8.31 J/(mol·K) or or 8.62×10−5 eV/(atom·K))
and×T10
8.62 is−absolute
5 eV/(atom temperature
·K)) and T(K). is absolute temperature (K).
It is worth mentioning that
It is worth mentioning thatthe
thejoining
joiningstrength
strengthincreases
increaseswith
with the increase
the increaseof of
holding
holding time at the
time at
initial stage of the joining process due to the better coalescence of mating surfaces
the initial stage of the joining process due to the better coalescence of mating surfaces to ensures to ensures complete
diffusion diffusion
complete of atoms ofand atomsattains
and aattains
maximum strength
a maximum value [17].
strength valueIn[17].
general, in non-steady
In general, in non-steadystate
diffusion, the concentration of diffusion species is function of both of time and
state diffusion, the concentration of diffusion species is function of both of time and position (Fick’sposition (Fick’s second
law). Itlaw).
second is thus
It isexpected
thus expected with with
the aid of more
the aid of moresuitable holding
suitable holdingtime,
time,joints
jointswith
with highly desirable
highly desirable
microstructure can be obtained and in turn, highly reliable bonded joints
microstructure can be obtained and in turn, highly reliable bonded joints with good performance with good performance can
be anticipated. Moreover, holding time has an effect on the quantity of atomic
can be anticipated. Moreover, holding time has an effect on the quantity of atomic diffusion and the diffusion and the creep
of theofprotrusions
creep the protrusions (i.e.,(i.e.,
elemental
elementaldiffusion of the
diffusion joined
of the alloy
joined alloycan
canbebeimproved
improved by by increasing
increasing the the
holding time)
holding time) [17]. [17].
2
∂C/∂t==DD(∂(∂2C/∂x
∂C/∂t 2
C/∂x2)) (2)(2)
where ∂C/∂t
where ∂C/∂t is
is the
the change
change inin solute
solute concentration
concentration with
with time
time at
at aa given
given position
position inin the
the base
base metal,
metal,
whichcould
which couldprovide
providean an indication
indication of
of isothermal
isothermal solidification
solidification rate,
rate, and
and D
D is
is the
the diffusion
diffusion coefficient,
coefficient,
and ∂2C/∂x2
2 2 is the change in concentration gradient with distance.
and ∂ C/∂x is the change in concentration gradient with distance.

Figure 12. Typical stress-strain curves for the different test conditions.
Figure 12. Typical stress-strain curves for the different test conditions.

Figure 13 displays the SEM morphology of the thixojoint that achieved with various joining
conditions. Through observing the fracture surfaces created by the tensile test, it was found that the
fracture appearance of the welded joint at 1300 °C was not completely along the interface between
base metal and insert. The fractures were characterised by brittleness, where intergranular fracture
mode is illustrative. The fracture path, which is typically dimpled, is located around liquid-solid zone
Metals 2018, 8, 316 12 of 16

Figure 13 displays the SEM morphology of the thixojoint that achieved with various joining
conditions. Through observing the fracture surfaces created by the tensile test, it was found that the
fracture appearance of the welded joint at 1300 ◦ C was not completely along the interface between base
Metals 2018, 8, x FOR PEER REVIEW 12 of 16
metal and insert. The fractures were characterised by brittleness, where intergranular fracture mode
is illustrative.
and The fracture
grain boundary. path, which
The close-up of theisfracture
typically dimpled,
path revealsisa located
“cobbled” around liquid-solid
surface appearance, zone and
which
grain boundary.
could indicate that The close-up
during of the fracture
solidification path reveals
the fracture a “cobbled”
occurred throughsurface appearance,
the liquid which could
with the re-solidified
indicate that during solidification the fracture occurred through the liquid
grains then becoming exposed as “cobbles”, a phenomenon also seen in 7075 Al alloy [18]. with the re-solidified grains
The
then becoming
brittleness was exposed
a result ofascoarse
“cobbles”, a phenomenon
fracture with big solidalso seenthat
lump in 7075
referAltoalloy [18]. The
unbroken brittleness
structure. The
was
solidaγresult of coarsemainly
(Fe) particles, fracture with
with big solid
globular lump
shape, that refer to
surrounded byunbroken
the carbide structure.
networksThe solid
which is γ
a
(Fe) particles, mainly with globular shape, surrounded by the carbide networks
typical characteristic with respect to semi-solid microstructure of D2 tool steel. The fracture then which is a typical
characteristic
appears to havewithquickly
respectpropagated
to semi-solidalong
microstructure
the grain of D2 tool steel.
boundaries andThe
the fracture then appears to
weak liquidus–solidus
have quickly propagated along the grain boundaries and the weak liquidus–solidus
interface of the lumps [19]. From the results it is believed that there is a good metallurgical interface of the
joining at
interface; this kind of compound fracture mechanism means that the rupture is not along this
lumps [19]. From the results it is believed that there is a good metallurgical joining at interface; the
kind of compound fracture mechanism means that the rupture is not along the interface.
interface.

Figure 13. Fractured surface of welded joints of samples processed at various conditions: (S7) 1300
Figure 13. Fractured surface of welded joints of samples processed at various conditions:
°C/0 1300
(S7) min, ◦(S8)
C/01300
min,°C/5
(S8) min,
1300 (S9)
◦ C/51300
min,°C/10 min. ◦ C/10 min.
(S9) 1300

Figure 14 shows fractured surface of welded joints obtained after post welding heat treatment.
As canFigure 14 shows fractured
be understood from thissurface
figure,ofpost
welded joints
welding obtained
heat afterchanges
treatment post welding heat treatment.
the fracture mode to
As can be understood
predominantly from this
transgranular figure,with
fracture, postfewwelding heat treatment
intergranular changes
facets. On the fracture
the contrary, in themode to
tensile
predominantly transgranular fracture, with few intergranular facets. On the contrary,
test of the non treated condition, disbanding of the solid particles has occurred as well as several in the tensile
test of the non
microcracks treated
with nano condition,
wide which disbanding
are found of outthe
in solid particles
fracture hasStress
surface. occurred as well
applied on theas sample
several
microcracks
during with nano
the tensile tests wide
led towhich are foundofout
the formation bigincracks
fracture
outsurface.
of smallStress
poresapplied on thefractures
and in turn, sample
during the tensile tests led to the formation of big cracks out of small pores and
occurred when these cracks grew. It is worth mentioning that the main parameter responsible for the in turn, fractures
occurred
low when
ductility is these cracks
the grain grew. ItThe
boundary. is worth
liquid mentioning
phase appearancethat thein main
grain parameter
boundaries, responsible
results in
for the low ductility is the grain boundary. The liquid phase appearance in
formation of porosities after solidification, which reduces ductility. It is thus expected with the grain boundaries,
results in of
presence formation of porosities
grain boundary leadsafter solidification,
to long soft zones which
which reduces ductility. It is during
distort discriminatory thus expected
plastic
deformation [18,20]. It is attractive to note that post-joining heat treatment is one of the key
parameters for improving the mechanical properties of thixojoined parts (although this would have
cost-implications and could reduce the attractiveness of the process).
Metals 2018, 8, 316 13 of 16

with the presence of grain boundary leads to long soft zones which distort discriminatory during
plastic deformation [18,20]. It is attractive to note that post-joining heat treatment is one of the key
parameters for improving the mechanical properties of thixojoined parts (although this would have
cost-implications
Metals and could
2018, 8, x FOR PEER reduce the attractiveness of the process).
REVIEW 13 of 16

Figure 14. Fractured surface of welded joints after post welding heat treatment.
Figure 14. Fractured surface of welded joints after post welding heat treatment.

3.2.2. Hardness Measurements

3.2.2. Hardness Measurements
Micro-hardness profiles were obtained for the AISI D2 tool steel base metal, the weld zone and
Micro-hardness profiles were obtained for the AISI D2 tool steel base metal, the weld zone and
the insert by using a load of 10 g for 30 s. Figure 15 presents the micro-hardness profile against
the insert by using a load of 10 g for 30 s. Figure 15 presents the micro-hardness profile against
distance from the interface and illustrates the variations of the HV value along the lines perpendicular
distance from the interface and illustrates the variations of the HV value along the lines perpendicular
to the joint interface. The hardness measurement of the base metal, the weld zone and the insert is
to the joint interface. The hardness measurement of the base metal, the weld zone and the insert is
fluctuated in the range 350 Hv to 370 Hv. This indicated that the hardness value of the welded joints
fluctuated in the range 350 Hv to 370 Hv. This indicated that the hardness value of the welded joints
was almost similar to those of base metal and insert. This indicated that the hardness profile gives a
was almost similar to those of base metal and insert. This indicated that the hardness profile gives a
good impression of joint microstructure and the degree of homogenization, this looks very
good impression of joint microstructure and the degree of homogenization, this looks very promising.
promising. However, the thixoweld-joint of AISI D2 exhibits different hardness values if compare to
However, the thixoweld-joint of AISI D2 exhibits different hardness values if compare to as supplied
as supplied material. This exposure to thixojoining temperature also results in the phase change to
material. This exposure to thixojoining temperature also results in the phase change to metastable
metastable austenite. While the remaining interspaces are filled by precipitated eutectic carbides on
austenite. While the remaining interspaces are filled by precipitated eutectic carbides on the grain
the grain boundaries and in the lamellar network. As can be seen from this figure, almost the similar
boundaries and in the lamellar network. As can be seen from this figure, almost the similar trend is
trend is observed in the microhardness profiles of all samples. Figure 15 clarifies small decrement in
observed in the microhardness profiles of all samples. Figure 15 clarifies small decrement in hardness
hardness values at same temperature with high holding time. The behaviour may be attributing to
values at same temperature with high holding time. The behaviour may be attributing to grain growth
grain growth with increasing holding time during evolution of microstructures. [21,22]. These results
with increasing holding time during evolution of microstructures. [21,22]. These results evidenced that
evidenced that diffusion has occurred and weld zone micro-hardness was free from harmful or brittle
diffusion has occurred and weld zone micro-hardness was free from harmful or brittle phases. In the
phases. In the case of post welding heat treatment condition (S10), hardness measurements were
case of post welding heat treatment condition (S10), hardness measurements were somewhat higher
somewhat higher than for the non-heat treated samples. This higher hardness can be attributed to the
than for the non-heat treated samples. This higher hardness can be attributed to the some amounts of
some amounts of eutectic chromium carbides dissolve in matrix during slow cooling. It means that
eutectic chromium carbides dissolve in matrix during slow cooling. It means that the primary grain
the primary grain boundaries have distinctly pinning effect on growth of grain size in the heat treated
boundaries have distinctly pinning effect on growth of grain size in the heat treated condition [23]. In
condition [23]. In addition, the phase transformation is probably the reason of hardness increase to
addition, the phase transformation is probably the reason of hardness increase to the (490 Hv). This
the (490 Hv). This value is higher in comparison with material hardness in the initial state after
value is higher in comparison with material hardness in the initial state after thixojoining processing.
thixojoining processing. During the isothermal heat treatment at higher temperatures, particular
During the isothermal heat treatment at higher temperatures, particular decomposition of the austenite
decomposition of the austenite and ferrite phases to the martensitic phases was achieved and the
and ferrite phases to the martensitic phases was achieved and the carbides of chromium and retained
carbides of chromium and retained austenite were included in the structure, as shown in XRD
austenite were included in the structure, as shown in XRD analysis. In tool steels with high alloy
analysis. In tool steels with high alloy content, high hardenability may cause martensite to form
content, high hardenability may cause martensite to form during air cooling. Hardenability is the topic
during air cooling. Hardenability is the topic which relates alloying to the phase transformations that
which relates alloying to the phase transformations that occur on cooling [24].
occur on cooling [24].
Metals 2018, 8, 316 14 of 16
Metals 2018, 8, x FOR PEER REVIEW 14 of 16

600

500
Micro-hardness HV 0.2
400

300

200 S7
S8
100 S9
S10
0
-4 -3 -2 -1 0 1 2 3 4
Distance from joined interface (mm)

Figure 15.
Figure 15. Hardness
Hardnessdistributions
distributionsofofD2–D2
D2–D2 tool steel
tool thixowelded
steel thixowelded joints at various
joints conditions:
at various (S7)
conditions:
13001300
(S7) °C/0◦ C/0
min,min,
(S8) (S8)
13001300
°C/5◦ C/5
min, min,
(S9) (S9)
13001300
°C/10 min, min,
◦ C/10 (S10)(S10)
13001300
°C/10 min +min
◦ C/10 post welding
+ post heat
welding
treatment.
heat treatment.

4. Conclusions
4. Conclusions
The novel
The novel thixojoining
thixojoining process
process of
of AISI
AISI D2D2 similar
similar tool
tool steel
steel was
was carried
carried out
out by
by using
using the
the direct
direct
partial re-melting
partial re-melting technique,
technique, and
and this
this was
was investigated
investigated through
through this
this research.
research. The
The effect
effect of
of joining
joining
temperature, holding
temperature, holding time
time and
and post-weld
post-weld heat
heat treatment
treatment onon microstructural
microstructural characteristics
characteristics and
and
mechanicalproperties
mechanical propertiesofofAISI
AISID2
D2 tool
tool steel
steel joints
joints have
have beenbeen studied.
studied. TheThe summarised
summarised conclusions
conclusions can
canlisted
be be listed as below:
as below:

1.1. Adequate
Adequate and and defectless
defectless thixoweld-joint
thixoweld-joint werewere successfully
successfully produced
produced with with thixowelding
thixowelding
temperature of 1300 °C,
◦ while lower welding temperature
temperature of 1300 C, while lower welding temperature caused a series of crackscaused a series of cracks across the
across
entire
the joint
entire resulting
joint resulting in in
spontaneous
spontaneous fracture
fractureafter
afterjoining.
joining.While
Whilepostpost weld
weld heat treatment,
heat treatment,
resulted in
resulted in improved
improved contrast
contrast between
between solid
solid and
and liquid
liquid phases,
phases, whereby
whereby the the big
big solids
solids appeared
appeared
in little liquid matrix where primary distribution of grain boundary is
in little liquid matrix where primary distribution of grain boundary is decreased substantiallydecreased substantially
and some
and some amounts
amounts of of eutectic
eutectic carbides
carbides dissolve
dissolve inin the
the matrix.
matrix.
2.2. According to the X-ray line scan analyses across the
According to the X-ray line scan analyses across the joint interface joint interface confirms
confirms aa uniform
uniform elemental
elemental
distribution in
distribution in the
the structure
structure while
while the
the X-ray
X-ray diffraction
diffraction pattern
pattern ofof the
the thixowelded
thixowelded areaarea was
was free
free
from any brittle or harmful
from any brittle or harmful phases. phases.
3.3. Maximum
Maximum tensile tensile streghth
streghth of of 271
271 MPa
MPa was
was achieved
achieved at at 1300
1300 ◦°C and 10
C and 10 min
min holding
holding time,
time, which
which
was 35%
was 35%that thatof of
D2D2basebase metal.
metal. Meanwhile,
Meanwhile, tensiletensile
strengthstrength of theparts
of the joined joined parts
after heat after heat
condition
condition showed a significant improvement over the non-heat treated
showed a significant improvement over the non-heat treated condition which was 560 MPa, i.e., condition which was 560
MPa, i.e., about 70% that of as received AISI
about 70% that of as received AISI D2 tool steel base metal.D2 tool steel base metal.
4.4. The fracture
The fracture of of joints
joints was
was located
located along
along the
the interface
interface between
between basebase metal
metal and
and insert
insert with
with typical
typical
brittle characteristics (intergranular). Meanwhile, the joints after heat condition
brittle characteristics (intergranular). Meanwhile, the joints after heat condition are fractured at are fractured at
the diffusion
the diffusion zone,zone, and
and the
the fracture
fracture exhibits
exhibits typical
typical brittle
brittlecharacteristic
characteristic(tranasgranular).
(tranasgranular).
5. The hardness measurement of the base metal, the weld zone and the insert is fluctuated in the
5. The hardness measurement of the base metal, the weld zone and the insert is fluctuated in the
range of 350 Hv to 370 Hv. This indicated that the hardness value of the welded joints was
range of 350 Hv to 370 Hv. This indicated that the hardness value of the welded joints was almost
almost similar to those of base metal and insert. While the hardness measurements of the
similar to those of base metal and insert. While the hardness measurements of the (thixojoining
(thixojoining + heat treated) condition (490 Hv) was somewhat higher than for the non-heat
+ heat treated) condition (490 Hv) was somewhat higher than for the non-heat treated samples.
treated samples. This is more related to the phase transformation (austenite and ferrite phases
This is more related to the phase transformation (austenite and ferrite phases to the martensitic
to the martensitic phases). Moreover, some amounts of eutectic chromium carbides dissolve in
phases). Moreover, some amounts of eutectic chromium carbides dissolve in the matrix.
the matrix.

Acknowledgments: The authors would like to thank Universiti Kebangsaan Malaysia (UKM) and the ministry of
Higher Education (MoHE), Malaysia, for the financial support under Research Grants AP-2012-014.
Metals 2018, 8, 316 15 of 16

Author Contributions: M.N.A. and M.Z.O. conceived and designed the experiments; M.N.A. performed the
experiments; M.N.A., M.Z.O., S.A.-Z., K.S.A., M.A.A. analyzed the data; M.N.A. wrote the paper. All authors
discussed the result and contributed to the final manuscript.
Conflicts of Interest: The authors declare no conflict of interest.

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