ESSENCE - International Journal for Environmental Rehabilitation and Conservation

Kotach et al./Vol. VII [2] 2016/39 - 45

Volume VII: No. 2 2016 [39 – 45] [ISSN 0975 - 6272]
[www.essence-journal.com]

Influence of deep cryogenic treatment on the mechanical properties of AISI-

H11 Hot Die Steel

Katoch, Sanjeev1; Sehgal, Rakesh2 and Singh, Vishal

Received: August 17, 2016  Accepted: November 28, 2016  Online: December 31, 2016

Keywords: Hot die steel | Cryogenic

Abstract
treatment | Tools and Dies | Tool steels |
One of the latest processes which have Carbides; Hardness
shown its potential to enhance the Introduction
mechanical properties of material is
Morphology of microstructure plays vital
cryogenic treatment. Cryogenic treatment
role in the mechanical properties and service
affects the bulk properties of the material at
life of tools and dies. Nowadays deep
the crystal level. In the present study
cryogenic treatment is applied on tools and
influence of deep cryogenic treatment on hot
dies to enhance their mechanical properties,
die steel grade AISI H11 is investigated
and this treatment exhibits the encouraging
experimentally. DCT has been performed at -
effects on various tool and die materials.
154°C for 6, 21, and 36 hours and tempered
Cryogenic treatment affects the bulk
for 2hours at 600°C. The mechanical
properties as well as surface properties of the
properties obtained after DCT have been
materials and hence its effects are permanent.
characterized with a distinction to understand
AISI H11 HDS is one of the grades of
the influence of cryogenic treatment vis-à-vis
Chromium hot die steel family which is used
vacuum heat treatment and tempering on the
as tools and dies for die casting of aluminum,
hardness and toughness. The results show
zinc and magnesium; and as forging dies,
that cryogenic treated samples ATC1 (36) T
punches and piercers. These hot works
have 7, 38 and 57% higher toughness than
applications require high toughness, shock
ATC1 (21), ATC1 (6) T, and A3T
resistance and red hot hardness. This grade
respectively while ATC1 (21) T treated
faces strong challenges such as wear
samples have 2.8, 0.4 and 5.8% higher
resistance along-with toughness. Researchers
hardness than A3T, ATC1 (6) T and ATC1
have cited the usefulness of cryogenic
(36) T samples, respectively.
treatment on the modification of
For Correspondence: microstructure, homogeneity of crystal
1
Centre for Material Science and Engineering, National structure and mechanical properties of
Institute of Technology, Hamirpur-177005 (H.P.), India
2
materials. Cryogenic treatment improves the
Department of Mechanical Engineering, National Institute
of Technology, Hamirpur-177005 (H.P.), India micro hardness value, enhances the number
Email: katochsanjeev@gmail.com of secondary carbides and improves dry
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 Kotach et al./Vol. VII [2] 2016/39 - 45
sliding wear behavior in comparison to
vacuum treated samples of hot die steel grade
AISI H13. Modification of microstructure
and improvement in the mechanical
properties of AISI H13 hot die steel has been
reported by the cryogenic treatment. The aim
of present experimental work is to study the
effect of different cryogenic treatments on
hardness, impact strength and microstructure
of HDS AISI-H11.
Material and Methodology
Hot die steel, grade AISI- H11; in
spheroidized annealed condition was selected
for experimental study and its chemical
composition analyzed with optical spark
emission Spectrometer (Model: DV6, Make:
Baird, USA), following ASTM E 415-2014
standard is as follows (wt.%): 0.37,C;0.91,Si;
0.31, Mn; 5.32,Cr ; 1.31, Mo; 0.34, V; 0.014,
P; 0.007 S; balance –Fe. Material chemical
composition conforms to HDS AISI-
H11.Prismatic blocks of dimensions
6.35x6.35x9 mm were extracted from
spheroidized annealed 16 mm round bars for
hardness and metallographic study and
Prismatic sample (10x10x55mm) were
extracted in the longitudinal direction for
Charpy impact testing as per ASTM E23-07.
Heat Treatment
Vacuum heat treatment of machined samples
was carried out in horizontal front loading
electrical heated vacuum furnace, (Make
Hind High Vacuum, Bangalore, India,
Capacity: 600x600x900mm), at process
parameters; austenization temperature:
1040°C, Vacuum maintained: 10-2 mbar,
soaking time at austenization temperature:
30minutes and quenching at gas pressure of
5bar with Nitrogen gas to room temperature.
Table 1 provides the details of sample
treatment conditions. After quenching
samples were taken out from the furnace and
divided in to two groups namely A3T:
vacuum heat treated and three times
tempered for 2 hours, C1: vacuum heat
treated plus cryogenic treated at -154°C for
varied soak time 6, 21, and 36 hours and
tempered for 2hours. A3T group samples of
HDS H11 were tempered at 550, 570 and
600°C respectively for 2 hours, coded as
A3T, in Box type electrical heated furnace,
Capacity: 300Kg, Temperature range up to
750°C. C1group samples were deep
cryogenic treated at -154 for varied soak time
6, 21and 36 hours with pre and post
tempering at two different temperatures.
S .No. Nomenclature Depiction of treatment
1. A 3T VFA = 1040° C, ST = 30 Minute,
Nitrogen gas quench, quench pressure =
5bar, Three T = 550°C, 570°C, 600°C
respectively for 2 hours .
2. A T C1(6)T VFA = 1040°C, ST = 30 Minute,
Nitrogen gas quench, Quench pressure =
5bar, T = 550°C for 2 hours, C1, ST = 6
hours, T = 600°C for 2 hours.
3. AT C1(21)T VFA = 1040°C, ST = 30 Minute,
Nitrogen gas quench, Quench pressure =
5bar, T = 550°C for 2 hours, C1, ST =
21 hours, T = 600°C for 2 hours.
4. AT C1(36)T VFA = 1040°C, ST = 30 Minute,
Nitrogen gas quench, Quench pressure =
5bar, T=550°C for 2 hours, C1, ST = 36
hours, T= 600°C for 2 hours.
Number in parentheses shows the soaking times in hours at
cryogenic temperature.
Table 1: Heat Treatment Sequence Followed for
HDS H11
Cryogenic treatment was done at -154°C in
a Computerized controlled cryogenic
processor with tempering facility up to
200°C (Make: Primero Enserve, Chennai,
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India). Slow cooling rate (1°C/Min) from
ambient to deep cryogenic treatment soak
temperature (-154°C) and a slow heating rate
(1°C/Min) from cryogenic treatment
temperature to ambient temperature were
applied.
Hardness Test
Micro hardness value was measured on
Micro Vicker hardness tester, model: MVK-
H2, make: Akashi, Japan, by following
ASTM standards E384-08a [9]. Indentation
load applied in hardness test was 1000gf
(9.8N) with dwell time of 15 second. Five
hardness readings were taken at different
points to estimate the average value of
hardness for each sample.
molds were prepared with Cold setting
resins, grinding of molds were done with
silicon carbide emery paper of grit size 120,
200, 600, 800, 1000, 1600, 2000, 3000 and
fine polished using diamond slurry, particle
size 6micron,with white kerosene oil as a
suspension media on rotating velvet cloth.
Polished specimen were etched with 3%
Nital (97%Nitric Acid + 3% Ethanol) and
dried in hot air. A3T and C1 group’s
specimens micro structural features were
studied under the field emission scanning
electron microscope model: Quanta FEG450
make: FEI, Holland. SEM microstructure
images of C1 and A3T group samples are
shown in “Figure 4” and “Figure 5”.

Charpy Impact Testing Results And Discussion

The relative toughness of materials was Hardness Test

measured with the Charpy V-notch impact Micro hardness value (HV 1 ) were obtained
test. This test was performed on calibrated for A3T, A T C1 (6) T, A T C1 (21) T, and A
Impact test machine, least count: 2J, Model: T C1 (36) T AISI H11 HDS at five equally
IT-30, Make: FIE, India, as per ASTM spaced points along the diagonal length of
standards designation E23-07a [8]. each specimen. Table 2 depicts the results of
Environment conditions during the test were: mean micro-hardness value (measured at five
temperature: 24.5°C and relative humidity different locations in the samples) along-with
RH 54%. Sample surface roughness and V- standard deviation and standard error of
notch dimension were kept precisely as per mean.
standard E23 and verified using Surface Mean Micro-
Treatment Standard SE of
hardness
Roughness tester, (Model:SJ201P, Make: Condition Deviation Mean
(HV 1 )
Mitutoyo, Japan), Profile Projector (Make:
A3T 446 4.415 1.974
Mitutoyo, Japan) and V-notch template
ATC1(6)T 456.2 2.863 1.280
respectively. The value of Charpy impact
ATC1(21)T 458.6 5.366 2.4
strength was measured using three Charpy
ATC1(36)T 436 4.472 2
impact tests for conventional and varied
Table 2: Results of mean micro-hardness
cryogenic treatment samples. of conventionally and varied
Microsturctural Analysis cryogenic treated samples of
HDS AISI H11
Samples for micro structural analysis were
The mean micro-hardness value of CHT and
prepared as per ASTM standards designation
DCT samples are shown in the Fig.1.
E3-01(Reapproved 2007) [10]. Specimen
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 Kotach et al./Vol. VII [2] 2016/39 - 45

ATC1(21)T treated sample have significantly increasing soaking time at the cryogenic
higher micro- hardness, which is around temperature and to have best mechanical
2.8% higher than the A3T sample and also properties optimum holding time is 36 hours
highest in the C1, DCT sample which are in case of D2 Cold work steel for deep
around 0.4 and 5.8% higher than the cryogenic treatment. Amini et al. also
ATC1(6)T, ATC1(36)T, respectively. The showed the decrease in hardness of
results demonstrate that the DCT influences 80CrMo12 5 cold work tool steel and
the micro-hardness of the samples in predicted that 48 hours holding time is
comparison to the A3T samples; the observed optimum to have best hardness value in this
micro-hardness value for treatment C1 tool steel grade.
increases up to 21 hour soaking time and then Charpy Impact strength
shows decrease in micro-hardness with Results of toughness (CVN) for A3T and
further increase in soaks time at DCT i.e. 36 varied DCT treated sample of HDS AISI H-
hours soaking. 11 are shown in Table 3 which depicts the
500

450 446
456.2 458.6
436
results of mean value of three samples for
400 each treatment group along-with standard
Micro Vicker Hardness (HV1)

350
deviation and standard error of mean.
300

250 Mean Charpy

Treatment Standard SE of
200 Impact strength
Condition Deviation Mean
150 (J)
100
A3T 18.6 1.154 0.66
50

0 ATC1(6)T 27.3 1.154 0.66

A3T ATC1(6)T ATC1(21)T ATC1(36)T
Treatment Conditions ATC1(21)T 21.3 1.154 0.66

Figure 1: Micro-hardness of conventional and varied ATC1(36)T 29.3 2.309 1.33

cryogenic treated HDS AISI - H11
Table 3: Results of Charpy impact
In the earlier studies Das et al., Gill et al., strength of conventionally and
Koneshlou et al. and Amini et al. concluded varied cryogenic treated samples
of HDS AISI H11
that increase in the micro-hardness is due to
the elimination of retained austenite, more The trend of toughness of A3T and varied
homogeneous carbide distribution and higher DCT samples are shown in the Figure 2.
degree of carbide distribution. Figure1 also ATC1 (36) T treated samples have
depicts that there is increase in the micro- significantly higher toughness, which is
hardness up to the soaking time of 21 hours around 57% higher than the A3T sample and
in C1 treatment. But in case of 36 hours also highest in the C1 sample. Enhancement
soaking time there is decrease in the micro- in toughness observed in case of ATC1 (36)
hardness as compared to the A3T and T is around 7 and 38% higher than the other
decrease was approximately 2% in case of DCT samples viz. ATC1 (6) T and ATC1
C1 treatment. This result corroborates the (36) T respectively. DCT sample shows the
finding of Das et al. who concluded that remarkable improvement in the toughness
there is reduction in the hardness value with over the A3T sample and enhancement is
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approximately 46, 14 and 32% for the

treatment group viz. ATC1 (6) T, ATC1 (21)
T and ATC2 (36) T respectively. This result
is in line with earlier findings of li et al. [14]
that shows that DCT treated AISI H13
samples have the higher toughness due to the
modification of microstructure with DCT.
30
29 (b)
27

25
21
Charpy Impact Strength (J)

20 19

15

10

0
A3T ATC1(6)T ATC1(21)T ATC1(36)T
Treatment Conditions (c)
Figure 2: Charpy impact strength of conventional and
varied cryogenic treated HDS AISI - H11

To have the better understanding of the

influence of varied cryogenic treatments vis-
à-vis resulted variation of micro structural
constituents on the fracture toughness, the
fractographs analysis was carried out with the
help of field emission scanning electron (d)
microscope (FESEM). Figure 3 (a) illustrates Figure 3: Field emission scanning electron microscope
fractographs of a conventional treated sample (FESEM) fractographs of fracture surfaces of different
(A3T), Figure 3 (b) , (c) and (d) represents treatments: (a) A3T, (b) ATC1(6)T, (c) ATC1(21)T and (d)
ATC1(36)T HDS AISI - H11.
fractographs of varied cryogenic treated
FESEM fractographs of conventional treated
samples ATC1(6)T2, ATC1(21)T2 and
sample (A3T) shows cleavage facets in
ATC1(36)T2 respectively.
Charpy impact strength of conventional and
microcracks appearing along the cleavage
plane. In case of varied cryogenic treated
samples dimples of various sizes and small
zone of microvoid coalescence are evidenced
on the grain facets and interfaces.
Microstructure
(a) Cryogenic treated FESEM Micrograph
shown in “Figure 4” indicates more density
and even distribution of precipitated
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secondary carbides in comparison to A3T
sample as shown in “Figure 5”. Number of
secondary carbides increases after the
cryogenic treatment and morphology of
secondary carbide in A3T and C1 group
samples are noticeably different. Results of
this study are in concurrence with previous
studies, that reported the enhancement of
number of secondary carbides, responsible
Figure 4: FESEM Image of Cryogenic treated (C1) sample.
Figure 5: FESEM Image of A3T sample.
for the strengthening of matrix and load
bearing capacity of tools and dies.
Conclusion
The effect of different DCT on the static
mechanical prosperities and microstructure of
HDS AISI H11 are investigated. The major
conclusions of this research study are:
• The micro hardness of DCT samples C1
increases in comparison to the vacuum heat
treated samples A3T. Micro Vicker
hardness of C1 treated samples increases up
to 21 hour soaking time and then decreases
with further increase in duration of soaks
time at DCT (i.e. 36 hours soaking).
• Toughness strength (CVN) increases in
DCT with longer soak time. There is 57%
higher Toughness (CVN) in case of ATC1
(36) T sample than the A3T sample and is
also highest in the C1 group sample.
Enhancement in toughness observed in case
of ATC1 (36) T is around 7 and 38% higher
than the other DCT samples viz. ATC1 (6)
T and ATC1 (36) T respectively.
• 21 hours soaking times at DCT (-154°C),
enhances the number of carbides
precipitations and formation of very fine
needle type carbides.
Acknowledgment
The authors gratefully acknowledge the
authorities of National Institute of
Technology, Hamirpur (H.P) for providing
FESEM characterization lab facilities;
Institute of Auto Parts and Hand tools
Technology, Ludhiana for extending
facilities under the expert supervision for
spectroscopic analysis, micro-indentation
test, vacuum heat treatment, Charpy impact
testing and cryogenic treatment facility
required for the study.
NOMENCLATURE
CHT : Conventional Heat Treatment
C1 : Cryogenic Treatment at -154°C
CVN : Charpy V- Notch Impact Strength
DCT : Deep Cryogenic Treatment
HDS : Hot Die Steel
SCT : Shallow Cryogenic Treatment
ST : Soak time
VFA : Vacuum Furnace Austenization
T : Tempering
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