materials

Article
Mechanical Properties, Short Time Creep, and Fatigue
of an Austenitic Steel
Josip Brnic 1, *, Goran Turkalj 1 , Marko Canadija 1 , Domagoj Lanc 1 , Sanjin Krscanski 1 ,
Marino Brcic 1 , Qiang Li 2 and Jitai Niu 2,3
1 Department of Engineering Mechanics, Faculty of Engineering, University of Rijeka, Rijeka 51000, Croatia;
turkalj@riteh.hr (G.T.); markoc@riteh.hr (M.C.); dlanc@riteh.hr (D.L.); sanjink@riteh.hr (S.K.);
mbrcic@riteh.hr (M.B.)
2 School of Material Science and Engineering, Henan Polytechnic University, Jiaozuo 454003, China;
liqiangdoc@163.com (Q.L.); niujitai@163.com (J.N.)
3 School of Material Science and Engineering, Harbin Institute of Technology, Harbin 150001, China
* Correspondence: brnic@riteh.hr; Tel.: +385-51-651-491; Fax: +385-51-651-490

Academic Editor: Richard Thackray

Received: 26 February 2016; Accepted: 15 April 2016; Published: 20 April 2016

Abstract: The correct choice of a material in the process of structural design is the most important
task. This study deals with determining and analyzing the mechanical properties of the material,
and the material resistance to short-time creep and fatigue. The material under consideration in
this investigation is austenitic stainless steel X6CrNiTi18-10. The results presenting ultimate tensile
strength and 0.2 offset yield strength at room and elevated temperatures are displayed in the form of
engineering stress-strain diagrams. Besides, the creep behavior of the steel is presented in the form of
creep curves. The material is consequently considered to be creep resistant at temperatures of 400 C
and 500 C when subjected to a stress which is less than 0.9 of the yield strength at the mentioned
temperatures. Even when the applied stress at a temperature of 600 C is less than 0.5 of the yield
strength, the steel may be considered as resistant to creep. Cyclic tensile fatigue tests were carried
out at stress ratio R = 0.25 using a servo-pulser machine and the results were recorded. The analysis
shows that the stress level of 434.33 MPa can be adopted as a fatigue limit. The impact energy was
also determined and the fracture toughness assessed.

Keywords: mechanical properties; creep test; fatigue; austenitic stainless steel

1. Introduction
The structure is usually designed both in accordance with the purpose for the use intended
and with favorable material selection. Service life conditions are determined by the purpose of the
structure and accordingly the properties of the material have to comply with these conditions. It is
known that material properties are tied in with the material chemical composition, the processing
path, and the resulting microstructure. The properties depending on the microstructure are called
structuresensitive properties, for example, yield strength, hardness, etc., [1]. A material selection
process for structural design includes issues such as strength, stiffness, weight, etc., as mentioned in
Ref. [2]. The designing process has to include an efficient selection of materials and it is conducted
under the assumption that the engineering material does not contain any failures. Furthermore,
the proper use of the structure ensures that no failure will occur in it during its service life [3].
Any engineering structure (or structural element) needs to be shaped. This means that the material is
subjected to processes (called manufacture) that include forming (i.e., forging, casting), joining (i.e.,
welding), material removal (i.e., machining) and the finishing process [4]. In all the applied processes
mentioned, i.e., in designing, manufacturing, service life conditions and maintenance, various failure

Materials 2016, 9, 298; doi:10.3390/ma9040298 www.mdpi.com/journal/materials

Materials 2016, 9, 298 2 of 19

modes may occur. In engineering practice, many failures can occur and any failure has a cause of its
origin and the mode of its representation. The analysis of failure provides an answer to how and why
an engineering component has failed, and in this sense such a discipline becomes a very powerful tool
in modern structural design [5]. Common causes of failures are usually mentioned such as pre-existing
defects (for example pre-existing cracks), defects initiating from imperfections, but also categories
such as design errors, misuse, inadequate maintenance, assembly error, etc. In engineering practice
a lot of failure modes have been observed, for example, force induced elastic deformation, creep,
yielding, buckling, fatigue, fracture, corrosion, thermal shock, etc., [6]. Creep is mentioned as one of
the possible failure modes and in this investigation the short-time creep resistance of the considered
material will be examined. Creep as a thermally activated phenomenon is usually defined as time
dependent behavior of the material where at constant stress (load) the strain continuously increases [7].
Its occurrence is appreciable at temperatures above 0.4 Tm, where Tm is the melting temperature [8].
This behavior of the metallic material is usually displayed in the form of a curve consisting of three
stages (I-transient creep, II-steadystate creep, III-accelerating creep). Material properties, the features
of its machinability as well as numerical analysis of the structure made of the considered material
belong to the most important information about both material and structure. In this sense, it is also
recommended to get an insight into some investigations not only made by the authors of this work but
also by other authors [923]. The possibility of the use of the finite element method in the shear stress
analysis of the structure made of any of the mentioned materials is presented in [24]. The main task of
the research presented in this paper is to determine the properties of the materials so as to provide
the relevant information about the structure and behavior of the material under certain conditions
of exploitation.
In addition, a brief overview of recently published papers relating to steel X6CrNiTi18-10 is
presented. The material damage and the microhardness variations of X6CrNiTi18-10 were analyzed in
order to determine the incubation period, performing the tests at different cavitation conditions
in a cavitation chamber [25]. Since the low-cycle fatigue damage evolution in the metastable
austenitic steel causes a deformation induced phase transformation from austenite to martensite, the
microstructure changes in the pre-crack stage were investigated [26]. In Ref. [27] the surface integrity
of some materials, including X6CrNiTi18-10, was quantified by means of 2D and 3D surface roughness
parameters, strain-hardening effects and associated residual stresses. Furthermore, the phase formation
and annealing behavior are described after nitrogen PIII (Plasma immersion ion implantation) in two
austenitic stainless steels, 1.4541 (X6CrNiTi18-10) and 1.4571 (X6CrNiMoTi17122), differing only
in the Mo content, [28]. In Ref. [29] a viscoplastic constitutive model is developed based on the
results of uniaxial tensile tests on some austenitic stainless steels, also including AISI 321. In Ref. [30]
the hot workability of AISI 304 and 321 austenitic stainless steels were compared through single-hit
Gleeble simulated thermomechanical processing between 800 C and 1200 C (the strain rate varies
between 0.001 s1 and 5 s1 ). An optimizing deep drilling parameter based on the Taguchi method
for minimizing surface roughness was considered in Ref. [31], while the influence of nitriding time on
the microstructure and microhardness of AISI 321 austenite stainless steel was investigated in Ref. [32].
The microstructural character of dissimilar welds between Incoloy 800H and 321 Stainless Steel was
discussed in Ref. [33]. In Ref. [34] the effect of low temperature nitriding on the fatigue behavior of
a titanium stabilized AISI 321 grade austenitic stainless steel is presented.

2. Information Concerning the Material, Equipment, Specimens, Test Procedures, and Standards
The material considered in this research is X6CrNiTi18-10 steel, delivered as 18 mm soft annealed
round bar. The added titanium content helps in preventing chromium carbide precipitation when
exposed to high temperatures, which may occur on account of wrong applications or may be generated
from the welding process. The material retains good strength and is treated as very resistant to
oxidation and intergranular corrosion in dry service conditions up to 850 C. Its maximum service
temperature can be significantly reduced in a hot atmosphere due to corrosive compounds such as
Materials 2016, 9, 298 3 of 19

water and sulfur compounds. However, the grade 321 possesses good creep strength. This steel is
known as heat resistant steel and austenitic corrosion resistant steel. In accordance with the commonly
used definition of steel as an alloy of iron and carbon (<2%) with or without the addition of other
alloying elements, Table 1 presents the chemical composition of the considered steel.

Table 1. Material chemical composition: X6CrNiTi18-10 steel.

Material: X6CrNiTi18-10
Designation
Steel name Steel number (Mat. No; W. Nr; Mat. Code)
EN 10088-3-2014/DIN 17440:
X6CrNiTi18-10; AISI 321; ASTM A249 1.4541
(321) UNS S32100; BS: 321S51.
Chemical composition of considered material Mass (%)
C Si Mn P S Cr Ni V
0.0176 0.436 1.44 0.0209 0.0174 16.95 9.263 0.204
Mo Cu Al Ti Pb Sn Co W Rest
0.241 0.548 0.0208 0.266 0.006 0.0443 0.1 0.107 70.318

The basic properties of steel depend on the chemical composition, resulting microstructure,
the state, form, and dimensions of the finished product. This means that processing as a means
to development and control of the microstructure as well as heat treatment are of significance for
achieving the required material properties. The properties (for example: yield strength, hardness) that
depend on the microstructure are called structure-sensitive properties. The general properties of this
material are: good corrosion resistance, medium values of mechanical properties, average forgeability,
poor machinability, excellent weldability (TIG, MAG, Arc, laser beam, and submerged arc welding,
except gas welding). Core X6CrNiTi18-10 steel is titanium-stabilized steel with improved intergranular
corrosion resistance and may be used in an extended temperature range. With respect to well-balanced
material properties, it is suitable for many applications and can be used at elevated temperatures.
As regards processing, it can be said that it is suitable for machining (but not automated), hammer
and die forging, cold forming, but it is not suitable for polishing, etc. However, due to formation of
titanium carbo-nitrides, its machinability differs from other low carbon stainless steels with titanium
free variants. Its main applications are in: the automotive industry, the chemical industry (chemical
processing equipment), building and construction industries, food and beverage industries, and
aviation and aerospace industries (used for aircraft parts, such as exhaust systems), jet engine parts,
weld equipment, power station constructions, furnace heat treated parts, oil refiners, as well as general
use in mechanical engineering. Due to its vibration fatigue resistance, application is quite extensive
in the aircraft industry, where operating temperatures are higher than 400 C and where corrosive
conditions are not too severe. Concerning its special property, it is usually stated to be suitable for
continuous exposure to high temperatures up to 850 C in an oxidizing atmosphere (750 C containing
sulfur). Its optimal fabrication and mechanical properties are achieved after solution annealing
(temperature range: from 1075 C to 1125 C) followed by rapid cooling (air or water).
Equipment used in these investigations can be divided into equipment used to perform uniaxial
tests at room and high temperatures and equipment used to determine impact energy. The former was
the (Zwick/Roell) 400 kN capacity materials testing machine for uniaxial tests, while the latter was
the Charpy impact machine. Also, if the uniaxial test was performed at room temperature then the
macro extensometer was used whereas for high temperature tests high temperature extensometer and
furnace (900 C/Mytech) were used.
Specimens used in uniaxial tests to determine engineering stress-strain diagrams and in creep
testing were machined from 18 mm steel rod.
The diameter of the specimen in its central part is 5 mm.
Materials 2016, 9, 298 4 of 19

The geometry of each specimen used in the uniaxial test (room and high temperature) was defined
according to that specified in ASTM: E 8M-15a, and its ends were threaded to match the holders of the
testing
Materialsmachine,
Materials 2016, 298Figure 1.
2016,9,9,298 4 4ofof1919

Figure
Figure1.1.Specimens
Specimensgeometrytensile
geometrytensiletest.
test.
Figure 1. Specimens geometrytensile test.

Test
Testprocedure
procedureand andstandards
standardsininaccordance
accordancewith
withwhich
whichuniaxial
uniaxialtests
testswere
werecarried
carriedout
outare
areasas
Test procedure
follows. and standards in accordance with which uniaxial tests were carriedatout are
follows. Tensile
Tensile tests
tests related
related toto determination
determination ofof engineering
engineering stress-strain
stress-strain diagrams
diagrams at roomroom
as follows.
temperature Tensile tests related to determination of engineering stress-strain diagrams at room
temperaturewerewereperformed
performedaccording
accordingtotoASTM:
ASTM:EE8M-15a,
8M-15a,while
whilethose
thoserelated
relatedtotohigh
hightemperatures
temperatures
temperature
were were performed according to ASTM: E 8M-15a, while those related to high temperatures
wereperformed
performedininaccordance
accordancewith withASTM:
ASTM:E21-09
E21-09standard
standard[35].
[35].Creep
Creeptesting
testingwaswascarried
carriedoutout
were performed ASTM:
according in accordance with ASTM: E21-09 standardwere[35]. Creep outtesting was carried out
accordingtotothe
the ASTM:EE139-11 139-11standard
standard[35].
[35].Charpy
Charpytests
tests werecarried
carried outaccording
accordingtotoASTM:
ASTM:
according
E23-12c to the ASTM: E 139-11 standard [35]. Charpy tests were carried out according towith ASTM:
E23-12cstandard
standardandandspecimens
specimensused usedininthese
thesetests
testswere
werealso
alsomanufactured
manufacturedininaccordance
accordance withthe the
E23-12c
same standard and specimens used in these tests werebe also manufactured in accordance with the
samestandards.
standards.AllAllofofthe
thementioned
mentionedstandards
standardscancanalso
also befound
foundininthe
theAnnual
AnnualBook,
Book,Ref.
Ref.[35].
[35].
same standards. All of the mentioned standards can also be found in the Annual Book, Ref. [35].
3.3.Test
TestResults
Resultsand
andDiscussion
Discussion
3. Test Results and Discussion
3.1.
3.1.Mechanical
3.1. Properties-Engineering
MechanicalProperties-Engineering
Mechanical Stress-Strain
Properties-EngineeringStress-Strain Diagrams
Stress-StrainDiagrams
Diagrams
Engineering stress-strain
Engineeringstress-strain
Engineering diagrams
stress-straindiagrams
diagramswerewere obtained
wereobtained
obtainedby by performing
byperforming uniaxial
performinguniaxial tests
uniaxialtests atatroom
testsat room and
roomand high
andhigh
high
temperatures.
temperatures. AA minimum
minimum ofoffive
fivetests
tests was
was performed
performed for
for each
each test
testtemperature.
temperature.
temperatures. A minimum of five tests was performed for each test temperature. Since engineering Since
Since engineering
engineering
stress-strain
stress-strain diagrams
stress-straindiagrams carried
diagramscarried
carried out
out atatat
out the
thethe considered
considered
considered temperature
temperature
temperature dodo
do
notnot
not differ
differ
differ fromfrom
from each
each each other
other
other atatall,
at all, all,
or
aoror aavery
very little,little,
very only only
little, one
onediagram
onlydiagram
one diagram
is shown isisshown
shown
for eachforfor each
each
of the ofofthe
consideredtheconsidered
considered
temperatures temperatures
temperatures (the
(thefirst
(the first conducted first
conducted
conducted test),
test), Figure
Figure 2.
2.On
On the
the basis
basis of
of experimental
experimental investigations,
investigations, the
the
test), Figure 2. On the basis of experimental investigations, the ultimate tensile strength and yield ultimate
ultimate tensile
tensile strength
strength
and
andyield
strength yield strength
are said to are
strength aresaid
saidto
decrease todecrease
with decrease with
an increasewithinan
an increase
increaseinintemperature,
temperature, temperature,
except except
exceptatataaof
at a temperature temperature
temperature
250 C where ofof
250
250C
these C where
wherethese
properties these properties
properties
increase increase
a little.increaseaalittle.
little.

(a)
(a) (b)
(b)
Figure
Figure2.2.Engineering
Engineeringstress-strain
stress-straindiagrams
diagramsatatroom
roomandandhigh
hightemperatures:
temperatures:X6CrNiTi18-10
X6CrNiTi18-10steel.
steel.
Figure 2. Engineering stress-strain diagrams at room and high temperatures: X6CrNiTi18-10 steel.
(a)
(a)Stress-strain
Stress-straindiagrams:
diagrams:2020C
Ctoto800
800C;
C;(b)
(b)Stress-strain
Stress-straindiagrams:
diagrams:150
150C
Cto
to550
550C.
C.
(a) Stress-strain diagrams: 20 C to 800 C; (b) Stress-strain diagrams: 150 C to 550 C.
The
Themodulus
modulusofofelasticity
elasticitycontinuously
continuouslydecreases
decreaseswith
withan anincrease
increaseinintemperature.
temperature.Also,Also,from
from
the engineering stress-strain diagram, it is visible that strains at 300 C, 400 C, and 500 Cthe
the The modulus
engineering of elasticity
stress-strain continuously
diagram, it isdecreases
visible with
that an increase
strains at in
300 temperature.
C, 400 C, Also,
and 500from
C are
are
engineering stress-strain diagram, it is visible that strains at 300 C, 400 C, and 500 C are somewhat
somewhat
somewhatreduced
reducedinincomparison
comparisonwith withthetheones
onesatathigher
highertemperatures.
temperatures.On Onthethebasis
basisofofengineering
engineering
stress-strain
stress-straindiagrams
diagramsititisisvisible
visiblethat
thatstrains
strainsatat300
300C,
C,400
400C Cand
and500500CCare
aresomewhat
somewhatreduced
reducedinin
comparison
comparisonwith withthose
thoseatathigher
highertemperatures.
temperatures.As Asaaconsequence
consequenceofofdynamic
dynamicstrainstrainaging,
aging,which
whichisis
treated
treatedasashardening
hardeningphenomenon,
phenomenon,ininthe thestress-strain
stress-straincurves
curvessomesomeeffects
effectscan
canarise.
arise.Serrations
Serrationsininthe
the
stress-strain curves are the most visible effects of dynamic strain aging. When this effect
stress-strain curves are the most visible effects of dynamic strain aging. When this effect is not seen is not seen
other
othereffects
effectscan
canbe
bepresent.
present.Usually,
Usually,ififserrations
serrationsare arenot
notseen,
seen,dynamic
dynamicstrain
strainaging
agingcan
canbebemarked
marked
Materials 2016, 9, 298 5 of 19

reduced in comparison with the ones at higher temperatures. On the basis of engineering stress-strain
diagrams it is visible that strains at 300 C, 400 C and 500 C are somewhat reduced in comparison
with those at higher temperatures. As a consequence of dynamic strain aging, which is treated as
hardening phenomenon, in the stress-strain curves some effects can arise. Serrations in the stress-strain
curves are the most visible effects of dynamic strain aging. When this effect is not seen other effects
can be present. Usually, if serrations are not seen, dynamic strain aging can be marked by lower strain
rateMaterials 2016, 9, 298
sensitivity. 5 of 19
Also, dynamic strain aging causes a minimum variation of ductility with temperature,
a plateau
by lower in strain
strengthrateas well as aAlso,
sensitivity. peakdynamic
in workstrain
hardening.
aging causes a minimum variation of ductility
with temperature, a plateau in strength as well as a peak in work hardening.
3.1.1. Graphical Representation of the Temperature Dependency of Mechanical Properties
3.1.1. Graphical Representation
Experimentally determined of the Temperature
mechanical Dependency
properties such as of Mechanical
ultimate Properties
tensile strength, yield strength
(0.2 offset yield strength),
Experimentally modulus
determined of elasticity,
mechanical and elongation
properties are displayed
such as ultimate in Figure
tensile strength, 3 using
yield
strength
special (0.2 offset
characters (, yield strength), modulus
). Approximation of elasticity,
curves relatedand elongation
to the are displayed
same properties are in Figure 3 using
presented
using
solid special characters
or dashed lines. These (, ).approximation
Approximation curves
curves related
relating to to
thethe
same propertiesproperties
mentioned are presented
describe
using solid or dashed lines. These approximation curves relating to the mentioned
their experimentally obtained values with greater or lower accuracy. To determine the accuracy of properties
describe their experimentally obtained values with 2greater or lower accuracy. To determine the
approximation, the coefficient of determination (R ) is used as a measure of accordance between
accuracy of approximation, the coefficient of determination (R2) is used as a measure of accordance
experimentally obtained results and polynomial approximation and serves as a statistic that gives
between experimentally obtained results and polynomial approximation and serves as a statistic that
information on the fit of a model [36].
gives information on the fit of a model [36].

m (T ) 3.34066 10 9 T 4 8.38792 10 6 T 3 6.09445 10 3 T 2 1.88466 T 642.468

t (T ) 5.2065 10 10 T 4 5.15185 10 7 T 3 4.95939 10 4 T 2 2.74578 10 1 T 76.1836

0.2 (T ) 1.05807 109 T 4 5.06733 107 T 3 1.37419 103 T 2 6.13642 101T 402.068

(a)

E (T ) 5.45165 107 T 3 5.066 104 T 2 2.49019 101T 229.624

(b)

Figure 3. Cont.
Materials 2016, 9, 298 6 of 19

Materials 2016, 9, 298 6 of 19

Materials 2016, 9, 298 6 of 19

(T ) 5.988941010T 4 1.08478106T 3 8.0243104T 2 2.63097 101T 92.6016

t (T ) 5.2065 1010 T104 45.15185 1076T 33 4.95939 41024 T 2 2.74578 101T 76.1836
(T ) 5.9889410 T 1.0847810 T 8.024310 T 2.63097 101T 92.6016
t (T ) 5.2065 1010 T 4 5.15185 107 T 3 (c)
4.95939 104 T 2 2.74578 101T 76.1836

Figure 3. Dependence of mechanical properties(c)on temperature: X6CrNiTi18-10 steel. (a) Ultimate

tensile strength (m) and 0.2 offset yield strength (0.2) versus temperature; (b) The modulus of
Figure 3. Dependence
Figure 3. Dependenceofofmechanical propertiesonontemperature:
mechanical properties temperature: X6CrNiTi18-10
X6CrNiTi18-10 steel.steel. (a) Ultimate
(a) Ultimate
elasticity (E) versus temperature; (c) Total elongation (t) and reduction in the area () versus
tensile
tensile strength
strength (m( m) and
) and 0.2 0.2 offset
offset yield
yield strength
strength (0.2() 0.2 ) versus
versus temperature;
temperature; (b)(b)
TheThe modulus
modulus of
of elasticity
temperature.
elasticity (E) versus temperature; (c) Total elongation (t) and reduction in the area () versus
(E) versus temperature; (c) Total elongation (t ) and reduction in the area () versus temperature.
temperature.
3.1.2. Descriptive Error Bars-Mechanical Properties
3.1.2. Descriptive Error Bars-Mechanical Properties
3.1.2. Descriptive Error Bars-Mechanical Properties
The structure operating under certain environmental conditions is to be subjected to certain
loads.The isstructure
ItThe structure
also operating
necessary operating under certain
under acertain
to choose environmental
environmental
material conditions
conditions
whose properties toisbetothe
is meet
will be structure
subjected
subjected to certain
to certain
service life
loads.
loads.It isIt also
is necessary
also necessary to
to choose
choose a
a material
material whose
whose properties
properties willwill
meetmeet
the
requirements, i.e., the ones based on known material properties so that the behavior of the structure the structure
structure service service
life life
requirements,
requirements, i.e., the
i.e., theones
onesbased
based on known
on known material
material properties
properties so
so thatthat the behavior
the behavior
can be predicted. Besides, very important aspects, e.g., the accuracy of the experimental results and of theof the structure
structure
can can
theirbe be predicted.
predicted.
interpretation,
Besides,very
Besides, very important
arise from the
important aspects,
aspects,
experimental
e.g.,
e.g.,
data.
the accuracy
In the accuracy
accordance
of the
of experimental
with the experimental
this,
resultsresults
several uniaxial
and and
tensile
their interpretation,
their regarding
interpretation, arise from
arise fromof the
the experimental
experimental data.
data.In accordance
In accordance with this, several
with this, uniaxial
several tensile
uniaxial tensile
tests
tests regarding
determination
determinationof
ultimate
ofultimate
tensile
ultimate tensile
strength
strength
were
were
performed.
performed.
In
In the
the
so
so
called
called descriptive
descriptive
tests
error regarding
bars, determination
Figure 4, 4,anananalysis tensile strength were performed. In the so called descriptive
error bars, Figure analysis ofof ultimate tensilestrength
ultimate tensile strength is shown
is shown wherewhere
rangerange (R)standard
(R) and and standard
error bars,
deviation Figure
(SD) 4,
areare an
used. analysis of ultimate tensile strength is shown where range (R) and standard
deviation (SD) used.TheThestandard deviationwas
standard deviation wascalculated
calculated as given
as given in Ref.
in Ref. [37]. [37].
deviation (SD) are used. The standard deviation was calculated as given in Ref. [37].

Figure 4. Cont.
Materials 2016, 9, 298 7 of 19
Materials 2016, 9, 298 7 of 19

Figure 4. Descriptive error bars: Ultimate tensile strength of steel X6CrNiTi18-10. (The small triangles
Figure 4. Descriptive error bars: Ultimate tensile strength of steel X6CrNiTi18-10. (The small triangles
are experimental data points (test results), while R = range; SD = standard deviation; i = a number of
are experimental data points (test results), while R = range; SD = standard deviation; i = a number of
the test, n = the total number of tests).
the test, n = the total number of tests).

g xi x 2
f i pxi xq2
f
(1)
SD
n 1
e i
SD (1)
n1
(1), xxii isisthe
In Equation (1), theindividual
individual data
data of the considered
consideredproperty
propertyatateach test, xx isisthe
eachtest, the mean
mean
value
value of
of the
the considered
considered property,
property,calculated
calculatedas:
as:
xi
x
n
x (2)
x ni
i
(2)
i
In Equation (2), n is the total number of the tests/experiments (at each test one data of the
In Equation (2), n is the total number of the tests/experiments (at each test one data of the
considered property is obtained). In this consideration there are: xi = (m,i ; 0.2,i ); x (m ; 0.2 );
1...n. property is obtained). In this consideration there are: xi = ( m , i ; 0.2,i ); x ( m; 0.2 );
iconsidered
i 1 ...n .
3.2. Determining the Resistance of Material to Creep
3.2. Determining the Resistance of Material to Creep
3.2.1. Short-Time Creep Tests
3.2.1.To
Short-Time
assess the Creep Testscreep behavior of the considered material or to predict its creep resistance,
short-time
several uniaxial short-time creep tests were carried out. Data defining creep tests as well as material
To assess the short-time creep behavior of the considered material or to predict its creep
creep responses are shown in Figures 58. In these investigations short-time creep behavior was
resistance, several uniaxial short-time creep tests were carried out. Data defining creep tests as well
considered since most materials can be subjected to such temperature conditions (occurrence of high
as material creep responses are shown in Figures 58. In these investigations short-time creep
behavior was considered since most materials can be subjected to such temperature conditions
(occurrence of high temperature due to error in cooling, hazard, fire, etc.). Only some of the special
Materials 2016, 9, 298 8 of 19

Materials
Materials2016,
2016,9, 298 88ofof19
Materials 2016,
temperature 9,9,
due
298
298 to error in cooling, hazard, fire, etc.). Only some of the special materials are intended
19
8 of 19

to be usedare
materials
materials inintended
are structures
intendedto todesigned
be
beused
usedin for
in long term
structures
structures operation
designed
designed for at high
forlong
long termtemperatures.
term operation
operationat In
athigh long
high term creep
temperatures.
temperatures.
materials are intended to be used in structures designed for long term operation at high temperatures.
processes,
In
Inlong
longterm
termhowever,
creep special equipment
creepprocesses,
processes, however,
however,specialfor creep
special processfor
equipment
equipment monitoring
forcreep
creepprocess is tomonitoring
process be used. In
monitoring isisthese
to
tobe tests,
beused.
used.
In long term creep processes, however, special equipment for creep process monitoring is to be used.
stress
In
In levels
these
these are
tests,
tests, selected
stress
stress levels in
levels accordance
are
are selected
selected with
in
in the
accordance0.2
accordance offset
with
withyield
the
the strength
0.2
0.2 offset
offset previously
yield
yield strengthdetermined
strength previously
previouslyat
In these tests, stress levels are selected in accordance with the 0.2 offset yield strength previously
determined
determinedat
the considered atthe
theconsidered
consideredtemperature
temperature (fortemperature(for
example: (forexample:
253.6 example:253.6
MPa is 253.6MPa
equivalent MPais
to 0.2 equivalent
equivalentto
offset yield to0.2
0.2offset
strengthoffsetyield
for this
determined at the considered
C). temperature (for example: 253.6 MPa isis equivalent to 0.2 offset yield
yield
strength
material
strengthforfor
at this
400
forthis material
thismaterial
materialat at 400
at400 C).
400C).
C).
strength

Figure
Figure5. Creep
Creepbehavior
behaviorof
ofsteel
steelX6CrNiTi18-10 atatthe temperature of 400
400C.
Figure
Figure 5.5.Creep
5. Creep behavior
behavior of
of steel
steel X6CrNiTi18-10at
X6CrNiTi18-10
X6CrNiTi18-10 thetemperature
at the
the temperatureof
temperature of400
of 400 C.
C.
C.

Figure
Figure6. Creep
Creepbehavior
behaviorof
ofsteel
steelX6CrNiTi18-10 atataatemperature of 500
500C.
Figure 6.6.Creep behavior of steel X6CrNiTi18-10at
X6CrNiTi18-10 temperatureof
at aa temperature
temperature of500
of 500 C.
C.
C.

Figure
Figure7. Creep
Creepbehavior
behaviorof
ofsteel
steelX6CrNiTi18-10
X6CrNiTi18-10at
ataaatemperature
temperatureof
of600
600C.
Figure 7.7.Creep
Figure 7. Creep behavior of
behavior of steel
steel X6CrNiTi18-10
X6CrNiTi18-10 at
at temperature
a temperature of
of 600
600
C.
C.
C.
Materials 2016, 9, 298 9 of 19
Materials 2016, 9, 298 9 of 19

Figure 8. Creep
Figure 8. Creep behavior of steel
behavior of steel X6CrNiTi18-10
X6CrNiTi18-10 at
at aa temperature
temperature of
of 700
700 C.
C.

In accordance with the short-time creep tests, steel X6CrNiTi18-10 is considered to be creep
In accordance
resistant with the
at temperatures short-time
of 400 creep
C and 500 Ctests,
when steel X6CrNiTi18-10
the stress is considered
level does not exceed 0.9 to be creep
of the yield
resistant
strength at the mentioned temperatures. Also, this steel may be treated as creep resistantofatthea
at temperatures of 400 C and 500 C when the stress level does not exceed 0.9
yield strengthofat600
temperature the mentioned temperatures.
C if the applied Also, not
stress does this exceed
steel may
0.5 be
oftreated as creep
the yield resistant
strength at
at this
atemperature.
temperature Inof 600 C if the applied stress does not exceed 0.5 of the yield strength at this temperature.
addition, even at temperatures of 700 C this material may be treated as creep
this material may be treated as creep resistant when the
In addition,
resistant wheneven
theatapplied
temperatures of 700
stress does notCexceed 30% of the yield strength.
applied stress does not exceed 30% of the yield strength.
3.2.2. Creep Test Modeling
3.2.2. Creep Test Modeling
To perform a creep test, appropriate but usually expensive equipment is indispensable.
To perform a creep test, appropriate but usually expensive equipment is indispensable. Although
Although the creep test shows deformation behavior of the material realistically, sometimes it is
the creep test shows deformation behavior of the material realistically, sometimes it is possible, based
possible, based on known data of the behavior from similar conditions, to predict the creep behavior
on known data of the behavior from similar conditions, to predict the creep behavior for the prescribed
for the prescribed conditions. This prediction can be done using similar analytical methods or
conditions. This prediction can be done using similar analytical methods or rheological models that are
rheological models that are used to model/simulate real creep processes. In the following part there
used to model/simulate real creep processes. In the following part there are two rheological models
are two rheological models and one analytical method (formula) proposed to be used in creep
and one analytical method (formula) proposed to be used in creep modeling. All of the proposed
modeling. All of the proposed tools can be used for modeling the first and second creep stages. Well
tools can be used for modeling the first and second creep stages. Well known rheological models are
known rheological models are the Burgers model and the Standard linear solid model (SLS). The
the Burgers model and the Standard linear solid model (SLS). The Burgers model is represented in
Burgers model is represented in Refs. [20,38]:
Refs. [20,38]:
1 1 t
1 1 pE2 {1 qt t
ptq
E
1 E 2

1e
t E1 E2 1 e E2 1 t 2
`
`
2
(3)
(3)
In Equation (3) there are: (t)-strain, -stress, E1 -modulus of elasticity, t-time, all related to
In Equation
considered (3) there
creep curve, while E2 ,(t)-strain,
are: 1 , and 2 are-stress, E1-modulus
parameters whose of valueselasticity, t-time, allonrelated
are determined the basisto
considered creep curve, while , , and are parameters whose values
of equality of the discussed creep curve and Equation (3). The Standard linear solid model (SLS) is are determined on the
basis of equality
represented Refs.of[22,39]:
the discussed creep curve and Equation (3). The Standard linear solid model (SLS)
is represented Refs. [22,39]: E E t
1 1 1 2 q
ptq ` e pE1E`E
E 2t (4)
E1 E1 `1E2 E11 E1 1 E22
t e (4)
In Equation (4) there are: (t)-strain, E E E
1 t-time,
1 -stress, 2 EE11 ,E2 , and are parameters whose values
are determined on the basis of equality of the discussed creep curve and Equation (4).
In Equation (4) there are: (t)-strain, -stress, t-time, E1, E2, and are parameters whose values
An analytical formula to model/simulate creep behavior is proposed in Refs. [11,12,22]:
are determined on the basis of equality of the discussed creep curve and Equation (4).
An analytical formula to model/simulate creepbehavior is proposed in Refs. [11,12,22]:
ptq D T p tr (5)
t D T p t r (5)
In Equation (5) there are: T-temperature, -stress, t-time and D, p and r are parameters which
are toInbeEquation
determined. All of
(5) there theT-temperature,
are: -stress,(3)(5)
mentioned Equations t-timecan
andbeD,
used forrthree
p and different types
are parameters of
which
modelling, namely, for:All of the mentioned Equations (3)(5) can be used for three different types of
are to be determined.
modelling, namely, for:
 Material: X6CrNiTi18-10 steel
Application of Equation (6c) = (, T , t ) D (T ) T p (T ) t r (T )
Constant temperature T
400 500 600 700
(C)
Constant stress level x 0.9 x = 0.70.9 x 0.5 x 0.3
Materials 2016, 9, 298 x .
(MPa) = 376 214275 150 63 10 of 19
Time (min) 1200
Parameters
D(T ) 6.150138108T 3 1.1354401104T 2 6.7433968102T 11.784261
Analytical Equation (5) ptq ptq, const, T const (6a)
p(T) 7.7811369107T3 1.6357754103T 2 1.0613631T 213.60664
8 3
r(T) 7.751213
ptq 10tq
p, const104T2 7.1958106102T 12.690118
T, T1.3200375 (6b)

ptq p, T, tq (6c)
In general, all of the above mentioned models for simulating creep behavior are considered to
The first type ofHowever,
be satisfactory. modeling,anEquation
analytical(6a),
formula is proposed
denotes as the of
the modeling best
onemodel.
exactlyWhen rheological
defined creep curve
models are considered, then the Burgers model seems to be more suitable for the creep
that is described by the defined creep temperature and the defined stress level at this temperature. processes The
where the dominated creep phase is the steady-state phase, while for creep process with dominated
last type of modeling, Equation (6c), is the most useful and applicable one. Namely, this modeling
transient phase (more expressed parabolic shape), the SLS model is considered to be more suitable.
covers an entire range of stress levels and temperature levels for the considered time range. In Table 2,
Also, it needs to be said that any of the used models are more suitable when only a particular curve
data relating
is selectedtotocreep modelling are presented, while creep modelling curves are presented in Figure 9.
be modeled.

Figure 9. Experimental and modeled creep curves: steel X6CrNiTi18-10. Modeling was performed
Figure 9. Experimental and modeled creep curves: steel X6CrNiTi18-10. Modeling was performed
using Equation (5) by applying the principle 6c.
using Equation (5) by applying the principle 6c.

Table 2. Creep modeling data: X6CrNiTi18-10 steel.

Material: X6CrNiTi18-10 steel

Application of Equation (6c) = p, T, tq DpTqT ppTq trpTq
Constant
400 500 600 700
temperature T ( C)
Constant stress level x 0.9 x = 0.70.9 x 0.5 x 0.3
pMPaq = x 0.2 376 214275 150 63
Time (min) 1200
Analytical Equation Parameters
(5)
DpTq 6.150138 108 T 3
1.1354401 104 T 2 ` 6.7433968 102 T 11.784261
ppTq 7.7811369 10 T 3 1.6357754 103 T 2 ` 1.0613631 T 213.60664
7

rpTq 7.751213 108 T 3 ` 1.3200375 104 T 2 7.1958106 102 T ` 12.690118

In general, all of the above mentioned models for simulating creep behavior are considered to be
satisfactory. However, an analytical formula is proposed as the best model. When rheological models
are considered, then the Burgers model seems to be more suitable for the creep processes where the
dominated creep phase is the steady-state phase, while for creep process with dominated transient
phase (more expressed parabolic shape), the SLS model is considered to be more suitable. Also, it
needs to be said that any of the used models are more suitable when only a particular curve is selected
to be modeled.
Materials 2016, 9, 298 11 of 19

3.3. Correlation between Charpy V-Notch Impact Energy and Fracture Toughness
Materials 2016, 9, 298 11 of 19
Undoubtedly fracture toughness is one of the most important material properties used to design
3.3. Correlation
structure against between Charpy
fracture. V-Notch
Fracture Impact Energy
toughness and Fracture
is a parameter thatToughness
defines material resistance to crack
extension [40], and itfracture
Undoubtedly represents a critical
toughness is one value
of theofmost
the stress
importantintensity
materialfactor K), designated
(SIF orused
properties to design
KIc . Designation
as structure K
against fracture. Fracture toughness is a parameter that defines material resistance to crackby
Ic indicates that this is a minimum value of fracture toughness determined
using a specimen
extension [40], and thatit meets the plane
represents strain
a critical value conditions
of the stress and besides,
intensity is tensile
factor (SIF orloaded (first mode).
K), designated as
Fracture toughness is stated
KIc. Designation indicatesto be a subject
that this is aconcerned
minimum with valuepredicting
of fracturefailure
toughness mode, especiallyby
determined one
containing crack-likethat
using a specimen defects
meets[41].
the In engineering
plane practice,and
strain conditions fracture
besides, toughness
is tensilecan be experimentally
loaded (first mode).
Fracture toughness
determined by a number is stated to be a tests
of standard subject concerned
[42]. However, with predicting related
experiments failure mode, especially one of
to the measurement
containing
fracture crack-like
toughness are defects [41]. Infor
not intended engineering
materialspractice, fracture
that behave toughness
plastically. In can
thisbe experimentally
case, the J-integral
(or,determined
for example, by aCTOD)
numberasofastandard
fracturetests [42]. However,
parameter is fairlyexperiments
appropriate. related
On the to the measurement
other hand, to avoidof
fracture toughness are not intended for materials that behave plastically.
problems such as complicated manufacturing of the specimen, differences between the crack in the real In this case, the J-integral
(or, for and
structure, example, CTOD) as a fracture
the manufactured crack onparameter
the specimen,is fairly appropriate.
other On the other
methods existing hand, to
for fracture avoid
toughness
problems such as complicated manufacturing of the specimen, differences
assessment are used. One of these such methods is the determination of the Charpy impact energy. between the crack in the
real structure,
Correlation betweenand the
theCharpy
manufactured
impact crack
energy onandthefracture
specimen, other methods
toughness was reviewedexistinginfor fracture
Refs. [43,44].
toughness assessment are used. One of these such methods is the determination of the Charpy impact
In these investigations the Charpy test was used to assess the fracture toughness. The specimens were
energy. Correlation between the Charpy impact energy and fracture toughness was reviewed in Refs.
machined from the material rod (longitudinal direction). The formula used to assess fracture toughness
[43,44]. In these investigations the Charpy test was used to assess the fracture toughness. The
is based on the measured Charpy V-notch impact energy, i.e., it is a well-known Roberts-Newton
specimens were machined from the material rod (longitudinal direction). The formula used to assess
formula that is independent of the temperature:
fracture toughness is based on the measured Charpy V-notch impact energy, i.e., it is a well-known
Roberts-Newton formula that is independent of the temperature:
KIc 8.47 pCVNq0.63 (7)
KIc = 8.47 (CVN)0.63 (7)
However, although this formula can be applied independently of the temperature, the CVN
However, although this formula can be applied independently of the temperature, the CVN
impact energy is inserted in it in accordance with the obtained result at the considered temperature.
impact energy is inserted in it in accordance with the obtained result at the considered temperature.
TheThegeometry
geometry ofof
the
thespecimens
specimensused usedin inthese
these investigations
investigations is is shown
shownininFigureFigure10a. 10a.Experimentally
Experimentally
obtained
obtained results
resultsofof
the
theCharpy
CharpyV-notch
V-notchimpact
impact energy
energy and and the
thecalculated
calculatedvalues valuesofoffracture
fracture toughness
toughness
areare
presented in Figure 10b. Note: Specimen (10 10 55 mm 3 ) is manufactured from a rod in such
presented in Figure 10b. Note: Specimen (10 10 55 mm ) is manufactured from a rod in such
3

waywaythat itsits
that largest
largestdimension
dimension(55 (55mm)
mm)coincides
coincides withwith the
the length
length of of the
therod.
rod.

(a)

Figure 10. Cont.

Materials 2016, 9, 298 12 of 19
Materials 2016, 9, 298 12 of 19

CVN(T) 8.2587104 T 2 2.63111101T 210.123

K Ic (T ) 1.02339103 T 2 3.28979101T 163.636
CVN = Charpy V-notch impact energy (measured, presented as an average value based on
three tests), KIc = fracture toughness (calculated).
(b)

Figure 10. Charpy V-notch specimen and impact energy determination. (a) Specimens geometry-
Figure 10. Charpy V-notch specimen and impact energy determination. (a) Specimens geometry-
Charpy V-notch impact energy determination; (b) Charpy V-notch energy (CVN); and calculated
Charpy V-notch impact energy determination; (b) Charpy V-notch energy (CVN); and calculated
fracture toughness (KIc) versus temperature.
fracture toughness (KIc ) versus temperature.

3.4. Fatigue Testing of Tensile Stressed Specimens

3.4. Fatigue Testing of Tensile Stressed Specimens
3.4.1. General Consideration
3.4.1. General Consideration
As engineering structures are frequently subjected to different loadings, it is surely of interest to
As engineering
investigate structures
the resistance of theare frequently
material subjected
to failure to differentloadings.
at the mentioned loadings, it known
It is is surely of when
that interest
to ainvestigate the resistance of the material to failure at the mentioned loadings.
material is subjected to a repeated load (cyclic load), fatigue failure may result in fracture of the It is known that
when a material
considered is subjected
engineering to a repeated
element at a stressload level
(cyclic load),
that fatiguelower
is much failure maythe
than result in fracture
fracture stress of
thecorresponding
considered engineering
to a monotonic element at aload.
tensile stress level may
Fatigue that isbe much
defined lower
as thethan the fracture
process of damage stress
corresponding to a monotonic tensile load. Fatigue may be defined
accumulation due to cyclic loading [45]. The main task for the designer dealing with a structure as the process of damage
accumulation
design subjected due toto cyclic loading
repeated load is [45]. The main
to ensure task for the
the required designer
structure dealing
service with a structure
life. Fatigue design
design subjected
criteria are based to on
repeated
known load
fatigueis to
lifeensure
modelsthe required structure
in accordance with theservice
required life. Fatigueofdesign
durability the
structure.
criteria These on
are based models
known are:fatigue
stress-life
lifemodel,
modelsdeformation-life
in accordance model with the andrequired
crack-propagation
durability rate of the
model. In
structure. this models
These paper a are:
stress-life model
stress-life is applied.
model, In these investigations
deformation-life the specimens were
model and crack-propagation rate
subjected
model. to paper
In this tensileastresses at the
stress-life modelprescribed stressInratio
is applied. theseand the cyclic loading
investigations processes were
the specimens were carried
subjected
to out in accordance
tensile stresses atwiththe the sinusoidal
prescribed law.ratio
stress The abscissa
and the(the number
cyclic loadingof cycles (N) towere
processes failure) is usually
carried out in
accordance with the sinusoidal law. The abscissa (the number of cycles (N) to failure)stress
plotted on a logarithmic scale, while the ordinate (cyclic maximum stress, or cyclic mean or
is usually
stress amplitude) is plotted on a linear scale or on a logarithmic scale.
plotted on a logarithmic scale, while the ordinate (cyclic maximum stress, or cyclic mean stress Fatigue can be considered in or
the cases of tensile loading (or another type of load) for unnotched (smooth) or notched specimens.
stress amplitude) is plotted on a linear scale or on a logarithmic scale. Fatigue can be considered in
However, attention should be paid to ensure that the test specimen is compatible with the testing
the cases of tensile loading (or another type of load) for unnotched (smooth) or notched specimens.
structure generating test data. The geometry (including dimensions) of the specimen as well as the
However, attention should be paid to ensure that the test specimen is compatible with the testing
testing procedure are recommended by standard (ASME standard, ISO standard). Each fatigue test
structure generating test data. The geometry (including dimensions) of the specimen as well as the
performed at the prescribed fatigue stress and at the prescribed stress ratio generates one point in the
testing procedure are recommended by standard (ASME standard, ISO standard). Each fatigue test
S-N system. Usually several fatigue tests are performed for the same fatigue stress level since a scatter
performed
related toatthethe prescribed
number fatigue
of cycles stressexists.
to failure and atOn thetheprescribed
basis of thestress ratio test
recorded generates
data the oneS-Npoint in the
system,
S-N system. Usually several fatigue
or S-N diagram (also called S-N curve, tests are performed for the same fatigue stress level
curve or fatigue life) is created and it represents thesince a scatter
related to the number of cycles to failure exists. On the basis of the recorded test data the S-N system,
Materials 2016, 9, 298 13 of 19

or S-N diagram (also called S-N curve, Wohler curve or fatigue life) is created and it represents the
applied fatigue stresses versus the number of cycles to failure for the considered material and for the
prescribed stress ratio. A. Wohler, a German scientist [46] carried out numerous tests using smooth
and notched specimens
Materials 2016, 9, 298 taken from railway axles. When regardless of the number of cycles 13 ofthe
19 test
specimen remains unbroken (i.e., without the occurrence of failure) at the prescribed conditions of the
applied fatigue stresses versus the number of cycles to failure for the considered material and for the
test, the fatigue limit has been reached, and the stress associated with this limit is called the fatigue limit
prescribed stress ratio. A. , a German scientist [46] carried out numerous tests using smooth
(endurance limit) [3,47,48]. This in fact means that there is a theoretical level of stress for the prescribed
and notched specimens taken from railway axles. When regardless of the number of cycles the test
stressspecimen
ratio belowremains which the material
unbroken will not
(i.e., without thefail for any number
occurrence of failure) ofatcycles. The S-N conditions
the prescribed diagram consists
of
of twothe test, the fatigue limit has been reached, and the stress associated with this limit is called the life)
parts (areas) of which the first area belongs to the finite fatigue region (finite fatigue and the
fatigue
second one
limit that belongs
(endurance limit)to[3,47,48].
the infiniteThisfatigue regimethat
in fact means (life).
thereIf both parts are level
is a theoretical presented in linear
of stress for the form,
then prescribed
the diagram contains
stress the inclined
ratio below which and the horizontal
the material will notline. fail Namely, in this case
for any number the infinite
of cycles. The S-N part of
diagram
the S-N curveconsists
(infinite of fatigue
two parts (areas)becomes
region) of which the first areahorizontal.
practically belongs to the This finite fatigue
is valid region
for (finite with
a material
fatigue
clearly life) and
expresses the second
fatigue limit. one that belongs
By contrast, thetoS-Nthecurve
infinite may fatigue
haveregime
a shape (life).
thatIf corresponds
both parts areto the
presented in linear form, then the diagram contains the inclined
material without clear fatigue limit. In the standards as well as in literature in general, and the horizontal line. Namely, in
a proposition
this case the infinite part of the S-N curve (infinite fatigue region) becomes practically horizontal. This
related to the performing of the fatigue test and also for fatigue limit determination can be found.
is valid for a material with clearly expresses fatigue limit. By contrast, the S-N curve may have a shape
For steel alloys, as fatigue limit, the number of the cycles at which the specimen remains unbroken,
that corresponds to the material without clear fatigue limit. In the standards as well as in literature
is usually adopted in an amount of to 7 cycles. Some engineering components are subjected to low
10the
in general, a proposition related performing of the fatigue test and also for fatigue limit
stresses relative tocan
determination thebematerial
found. For ultimate tensile
steel alloys, strength
as fatigue buttheatnumber
limit, a very of large number
the cycles of cycles
at which the and
that due to long
specimen service
remains life and/or
unbroken, high frequency
is usually adopted inload. So, high
an amount of cycle fatigue
107 cycles. Some(HCF) is treated as
engineering
crackcomponents
growth phenomenon
are subjectedrelated to lowto the previously
stresses relative tomentioned
the materialstressedultimatecomponents.
tensile strength Inbut
anyatcase,
a in
very large number of cycles and that due to long service life and/or
engineering practice the influence of HCF exerted on the life of the component is to be eliminated or high frequency load. So, high
cycletofatigue
reduced a minimum. (HCF) is If treated
testing as crack growth
procedures phenomenon
require 109 cycles, related
it maytobe thesaid
previously
that these mentioned
cases belong
stressed components. In any case, in engineering practice the
to the so called ultra-high cycle fatigue regime (UHCF). Some factors such as surface finish, influence of HCF exerted on the lifeapplied
of
the component is to be eliminated or reduced to a minimum. If testing procedures require 109 cycles,
loading conditions, deviations in specimen alignment, etc., cause scatter in fatigue data. A group of
it may be said that these cases belong to the so called ultra-high cycle fatigue regime (UHCF). Some
methods also exists that provides a means to deal with the scatter fatigue data and in this sense provide
factors such as surface finish, applied loading conditions, deviations in specimen alignment, etc.,
an estimate for median
cause scatter in fatiguefatigue
data.strength
A group at of the considered
methods also existsnumber of cycles.a To
that provides meansthe to
mentioned
deal with group
the of
methods (tools)
scatter fatigue theredatamay andbeincounted:
this sense provide an S-N
conventional tests,for
estimate advanced
median statistical methods,
fatigue strength quantal
at the
response tests, and
considered number accelerated
of cycles.stress
To thetests [45]. Within
mentioned group theseof methodsgroups therethere
(tools) are several
may be methods:
counted: for
example, methods
conventional such
S-N as advanced
tests, the Staircase method,
statistical Two-point
methods, quantal responseetc.
method, which
tests, and belong to the
accelerated quantal
stress
tests [45].
response testsWithin
(regarded these as groups
a group thereofare several methods:
methods). Conversely,for example,
fatigue methods
limit issuchoften as considered
the Staircase to be
method,
a material Two-point method, etc. which belong to the quantal response tests (regarded as a group of
property.
methods). Conversely, fatigue limit is often considered to be a material property.
3.4.2. Fatigue Testing
3.4.2. Fatigue Testing
In the case presented in this paper, fatigue tests of cyclic tensile stressed specimens were carried
In the case presented in this paper, fatigue tests of cyclic tensile stressed specimens were carried
out in accordance with the standard ISO 12107:2012 (2012) [49], at the prescribed stress ratio of R = 0.25
out in accordance with the standard ISO 12107:2012 (2012) [49], at the prescribed stress ratio of
and at
R room
= 0.25 temperature. The geometry
and at room temperature. The of the specimen
geometry is shownisinshown
of the specimen Figurein11 while11test
Figure results
while test data
as well as fatigue limit are presented in Figure 12.
results data as well as fatigue limit are presented in Figure 12.

Figure 11. Specimens geometry-fatigue test.

Figure 11. Specimens geometry-fatigue test.
Materials 2016, 9, 298 14 of 19
Materials 2016, 9, 298 14 of 19

Figure 12. Fatigue tests (at room temperature and stress ratio R = 0.25) for X6CrNiTi18-10 steel:
Figure 12. Fatigue tests (at room temperature and stress ratio R = 0.25) for X6CrNiTi18-10 steel:
maximum stress versus number of cycles to failure ( = no failure, = failure), approximated S-N
maximum stress versus number of cycles to failure (# = no failure,  = failure), approximated S-N
curve (line) in fatigue limit region (\) and fatigue limit (endurance limit) in fatigue infinite region ().
curve (line) in fatigue limit region (z) and fatigue limit (endurance limit) in fatigue infinite region ().

Fatigue testing started in such a way that the first tests were at the stress level (600 MPa) near
Fatigue
the tensile testing (608
strength started in such
MPa) of thea way that
tested the firstAfterwards
material. tests were atthese
the stress level (600
specimens wereMPa)
testednear
by
the tensile strength (608 MPa) of the tested material. Afterwards these specimens
decreasing stress regime. A number of 10 million cycles was selected as the desired number of cycles were tested by
decreasing stress regime. A number of 10 million cycles was selected as the desired
at which the specimen remains unbroken. In general, at the considered stress level some specimens number of cycles
at which
may the specimen
be expected remains(failed)
to be broken unbroken.
whileInsome
general, at the
others mayconsidered
not. Namely,stress
inlevel
somesome
casesspecimens
there is a
runout where the time to failure exceeds that available for the test (censoring). As is visible,there
may be expected to be broken (failed) while some others may not. Namely, in some cases is
in this
a runout where the time to failure exceeds that available for the test (censoring). As is
stress-life model, the entire procedure of fatigue testing included 21 tests of which seven tests belongvisible, in this
stress-life
to model,method
the staircase the entire procedure
(modified of fatigue
staircase testing
method) included
used 21 tests
for fatigue of which
limit seven testsInbelong
determination. finite
fatigue life the approximated curve (line) is determined without taking into account runouts. finite
to the staircase method (modified staircase method) used for fatigue limit determination. In
fatigue life the approximated curve (line) is determined without taking into account runouts.
3.4.3. Fatigue Limit Calculation
3.4.3. Fatigue Limit Calculation
The fatigue limit (endurance limit) or so called fatigue strength in the infinite fatigue life range
The fatigue limit (endurance limit) or so called fatigue strength in the infinite fatigue life range
can be estimated in accordance with the modified staircase method and in Figure 12 it is presented
can be estimated in accordance with the modified staircase method and in Figure 12 it is presented by
by the horizontal line. Specimens were tested under decreasing stress regime. In Table 3 data related
the horizontal line. Specimens were tested under decreasing stress regime. In Table 3 data related to
to failed and not-failed specimens for analysis in the modified Staircase method are presented.
failed and not-failed specimens for analysis in the modified Staircase method are presented. Fatigue
Fatigue data used in the modified Staircase method analysis are completed from fatigue testing. Data
data used in the modified Staircase method analysis are completed from fatigue testing. Data are
are presented using the following designations: specimens failed () or not-failed () for the
presented using the following designations: specimens failed () or not-failed (#) for the appropriate
appropriate stress levels at a certain number of cycles. In this sense, fatigue stress levels applied are:
stress levels at a certain number of cycles. In this sense, fatigue stress levels applied are: 450 MPa (as
450 MPa (as , the last stress level from the finite fatigue life, hence it is visible that all of the
2 , the last stress level from the finite fatigue life, hence it is visible that all of the specimens failed),
specimens failed), 440 MPa (as , first stress level at which the first and last specimens occur that
440 MPa (as 1 , first stress level at which the first and last specimens occur that are not-failed among
are not-failed among one that failed), 430 MPa (as , stress level at which specimen not-failed). It is
one that failed), 430 MPa (as 0 , stress level at which specimen not-failed). It is worth pointing out
worth pointing out that the highest level of the stress was and it coincides with the lowest stress
that the highest level of the stress was 2 and it coincides with the lowest stress measured in the finite
measured in the finite fatigue regime. Let, in general, the magnitude of stress be designated as
fatigue regime. Let, in general, the magnitude of stress be designated as i (MPa) related to the
(MPa) related to the specific i-th level of testing, and the number of failure events as fi related to
specific i-th level of testing, and the number of failure events as fi related to the same specific
the same specific (considered) stress level. As observed, each stress level (430, 440, 450) increases to
(considered) stress level. As observed, each stress level (430, 440, 450) increases to the previous one in
the previous one in stress intensity which is equal to the stress step, d = 10 MPa. Table 4 presents an
stress intensity which is equal to the stress step, d = 10 MPa. Table 4 presents an analysis of the staircase
analysis of the staircase data needed for the derivation of constants. Furthermore, the mentioned
data needed for the derivation of constants. Furthermore, the mentioned constants are needed for the
constants are needed for the fatigue limit calculation, Table 5.
fatigue limit calculation, Table 5.
Materials 2016, 9, 298 15 of 19

Table 3. Data for modified staircase method related to failed () and not-failed (#) specimens.

Number of Specimen
Stress i MPa
1 2 3 4 5 6 7
450
440 # #
430 #

Table 4. Data analysis for modified staircase method.

Stress i (MPa) Level of Stress i fi if i i2 f i

450 2 3 6 12
440 1 1 1 1
430 0
0 0 0
4 7 13

Table 5. Calculation of the constants A, B, C, D in accordance with ISO standard.

Formula Material: X6CrNiTi18-10

A i fi 7
2
B i fi 13
C fi 4
2
D BCA
C 2 0.1875

The lower limit of fatigue strength in infinite fatigue life (i.e., fatigue limit, endurance limit) is
defined as (in accordance with ISO standard):

f pP, 1q y kpP,1,do f q y (8)

In this Equation there are: The mean fatigue strength

A 1
y 0 ` d (9)
C 2

where d is stress step-The coefficient for the one sided tolerance limit for a normal distribution kpP,1,q.
The estimated standard deviation of the fatigue strength

y 1.62 d pD ` 0.029q . (10)

In accordance with the standard recommendation of n 1 6 where n is the number of

items in a considered group. Consecutively, for a desired probability of P 10% and a confidence
level p1 q = 90%, in accordance with the table B1 (ISO), it follows: kpP,1,q = kp0.1;0.9;6q 2.333.
In accordance with Equations (9) and (10), it is:

A 1 7 1
y 0 ` dp q 430 ` 10p q 442.5 MPa (11)
C 2 4 2
or this can be obtained as:
430 ` 440 ` 450 ` 440 ` 450 ` 440 ` 450
y 442.8 (12)
7
y 1.62 d pD ` 0.029q 1.62 10 p0.1875 ` 0.029q 3.5 MPa (13)
Materials 2016, 9, 298 16 of 19

Finally, the fatigue limit is:

f p0.1;0.9;6q y kpP,1,q y 442.5 2.333 3.5 434.33 MPa (14)

Similar investigations related to fatigue of X6CrNiTi18-10 steel have not been found in the
literature so far.
Materials 2016,However,
9, 298 many materials have been tested for fatigue as well as phenomena
16 of 19 that
occur with fatigue such as those considered in [50].
Similar investigations related to fatigue of X6CrNiTi18-10 steel have not been found in the
literature so far. However, many materials have been tested for fatigue as well as phenomena that
3.5. Basic Analysis of the Microstructure
occur with fatigue such as those considered in [50].
As is well known, material properties depend on the chemical composition, processing path,
3.5. Basic Analysis of the Microstructure
and microstructure. For the considered steel and its composition, some of properties depend on
As is well known,
the microstructure. The properties material properties
that depend depend on the
on the chemical composition,
microstructure are calledprocessing path,
structure sensitive
properties (for example, yield strength, hardness). Cold or hot rolling, for example, is thethe
and microstructure. For the considered steel and its composition, some of properties depend on means to
microstructure. The properties that depend on the microstructure are called structure sensitive
develop and control the microstructure. Since the microstructure can be changed when the material
properties (for example, yield strength, hardness). Cold or hot rolling, for example, is the means to
is exposed to high
develop temperature,
and control three specimens
the microstructure. Since the exposed to different
microstructure temperature
can be changed when theconditions
material were
examined. The first
is exposed to highspecimen is referred
temperature, to as delivered
three specimens material,
exposed to different and the other
temperature twowere
conditions specimens
with reference
examined.toThecreep
first conditions carriedtoout
specimen is referred at different
as delivered temperatures
material, and the other and
twodifferent
specimensstress
with levels.
reference
The former creeptotest
creep
was conditions carried
carried out out at
at 500 C,different
153 MPa, temperatures
1200 min and and the
different
latterstress
one atlevels.
700 The
C, 63 MPa,
former creep test was carried out at 500 C, 153 MPa, 1200 min and the latter one at 700 C, 63 MPa,
1200 min. Optical micrographs of the examined specimens are shown in Figure 13.
1200 min. Optical micrographs of the examined specimens are shown in Figure 13.

(a) (b)

(c) (d)

(e) (f)
Figure 13. X6CrNiTi18-10 steel: optical micrographs, aqua regia. (a) As-received material (austenitic
Figure 13. X6CrNiTi18-10
stainless steel:
steel, annealed bar),optical micrographs,
the cross-section of the aqua regia.
specimen, (a)(b)
500; As-received
As receivedmaterial (austenitic
material, the
stainless
longitudinal-section of the specimen, 500; (c) After performing the creep process at 500 C/153material,
steel, annealed bar), the cross-section of the specimen, 500; (b) As received
the longitudinal-section of the specimen,
MPa/1200 min, the cross-section 500; 500;
of the specimen, (c) After performing
(d) After performingthethe creep process
creep process at 500 C/
at 500
C/153 MPa/1200 min, the longitudinal-section of the specimen, 500; (e) After performing
153 MPa/1200 min, the cross-section of the specimen, 500; (d) After performing the creep process at the creep
process at 700 C/63 MPa/1200 min, the cross-section of the specimen, 1000; (f) After the creep process
500 C/153 MPa/1200 min, the longitudinal-section of the specimen, 500; (e) After performing the
performed at 700 C/63 MPa/1200 min, the longitudinal-section of the specimen, 1000.
creep process at 700 C/63 MPa/1200 min, the cross-section of the specimen, 1000; (f) After the creep
process performed at 700 C/63 MPa/1200 min, the longitudinal-section of the specimen, 1000.
Materials 2016, 9, 298 17 of 19

On the basis of the given micrographs, it can be said as follows. The basic microstructure (main
phase/main structure) of as-received material is austenite characterized by polygonal austenite grains,
Figure 13a,b. Also, there is a mixture of austenite and ferrite. A lot of impurity exists in the material
and this is distributed in the form of non-uniform black particles. In between there are twin grains.
Considering the longitudinal section, it can be concluded that the slip line and twin crystals are
included in the austenite. The ferrite has been stretched and that suggests that the material has suffered
some plastic deformation in the longitudinal direction. In the case of the specimen that was previously
subjected to creep (500 C/153 MPa/1200 min), Figure 13c,d, the temperature of the creep process
was not so high but the stress level was high and the austenite grains were increased. It is shown that
not only slip lines increase after creep deformation, but the ferrite content increases as well. Some
ferrite precipitated from the austenite which indicated that the stability of the austenite of this material
was not good enough. At the same time a higher number of twin grains occurs which have better
polygonal shapes. Also, the formation of holes due to the diffusion of failures in the crystal lattice
is noticed. As regards the case presented in Figure 13e,f; that is, when the specimen was previously
subjected to creep (700 C/63 MPa/1200 min), since the temperature increases, although the stress
level was low the temperature increased, the grains are increased and the number of twin grains
also increases. In this case, the influence of high temperature on the deformation process is apparent.
Some recrystallized grains can be found, which indicates that this material starts to recrystallize at
a temperature of 700 C.

4. Conclusions
The results of this research present very good information for designers involved in design of
structures made of steel X6CrNiTi18-10. The obtained results relating to tensile strength and yield
strength show that this material has good ultimate tensile strength and yield strength not only at
room temperature but also at high temperatures as is apparent from Table 2. Furthermore, the steel is
creep resistant over a wide range of temperatures and stress levels, as can be seen from Figures 58.
Also, after carrying out the tests, the fatigue limit of the cyclic tensile stressed steel at a stress ratio of
R = 0.25 can be adopted in an amount of 434.33 MPa. Finally, the steel is characterized by an impact
energy obtained with the Charpy impact machine in an amount of 176 J/20 C from which a fracture
?
toughness of 220 MPa m was calculated.

Acknowledgments: This work was supported by the Croatian Science Foundation under the project 6876 and it
is also partially supported by the University of Rijeka within a project 13.09.1.1.01. Microstructure analysis was
made by Jitai Niu and Qiang Li from School of Materials Science, Henan Polytechnic University, Jiaozuo, China,
while some additional explanations in this field were done by Roman Sturm from the Faculty of Mechanical
Engineering, University of Ljubljana.
Author Contributions: Josip Brnic performed the experiments, analyzed the data, and wrote the paper;
Goran Turkalj analyzed the fatigue data; Marko Canadija analyzed the creep and tensile data; Domagoj Lanc
performed the fatigue test; Sanjin Krcanski analyzed the creep; Marino Brcic analyzed the tensile test data;
Qiang Li and Jitai Niu peformed the microstructure tests and analysis.
Conflicts of Interest: The authors declare no conflict of interest.

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