Z. Kristallogr. Suppl. 27 (2008) 89-96 / DOI 10.1524/zksu.2008.

0012 89
© by Oldenbourg Wissenschaftsverlag, München

Stress and hardness in surface layers of

shot-peened steels
J. Drahokoupil1,2,*, N. Ganev2, M. eranský1, P. Bohá1,
R. tvrtlík1,3, M. Stranyánek1,3
1
Institute of Physics of the ASCR, v. v. i., Na Slovance 2, 182 21 Prague 8, Czech Republic
2
Faculty of Nuclear Sciences and Physical Engineering, Czech Technical University, Troja-
nova 13, 120 00, Prague 2, Czech Republic
3
Joint Laboratory of Optics of Palacky University and Institute of Physics of the ASCR,
v.v.i., 17. listopadu 50, 772 07 Olomouc, Czech Republic
*
jandrahokoupil@seznam.cz

Keywords: microstrain, hardness, macroscopic stress, shot peening, steels

Abstract. The main goal of the research is to study gradients of stresses and hardness in
surface layer after shot peening and to look for correlations between these quantities, and this
way to contribute to understanding of the onset of residual stress formation in engineering
materials. X-ray diffraction was applied as a main technique for microscopic and macro-
scopic residual stress determination. Combination of X-ray diffraction with electrolytic pol-
ishing enables to study the depth profile of aforesaid quantities. Indentation on polished cross
sections was used to study hardness depth profiles. It could be state that the shot peening
produce the compressive macrostresses and the depth of the compressive layer is primarily
influenced by intensity of blasting.

1. Introduction
Shot peening process consists of the controlled bombardment of the metal surface by spheri-
cal shot including steel shot, steel and stainless steel pieces of wire, ceramic or glass
beads [1]. The shots may be driven by a high velocity stream of air or liquid or by mechani-
cal device in which the shots are fed into a rotating wheel and thrown at the desired velocity.
The treatment causes plastic flow of the surface layers, thereby inducing surface compressive
stresses, change of microstructure and may cause phase transformation in the surface layers.
Although shot peening have been used widely in machined industry for a long time, it is still
in the focus of interest of scientists and technologists [1]. The mechanism of the creation of
compressive residual stress by shot peening has been recently clarified by Kobayashi et al. in
[2] and a lot of papers dealing with the improvement of fatigue life of products caused by
this treatment is still appearing [3 - 6]. Ultrasonic shot peening method is successfully used
for generation of a nanostructured surface layer, i.e. surface nanocrystalisation of steels [7 -
8].

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X-ray diffraction is widely used as the best developed experimental method of quantifying
residual stresses. When the beneficial effect of imposed compressive residual stresses by shot
peening is evaluated, usually only depth distribution of macroscopic (first kind) ones is taken
into account [1, 9, 10]. The unique ability of X-ray diffraction methods to determine both
the macroscopic residual stress and mean value of micro-strain and crystalline size in the
irradiated volume is not commonly applied for complete characterization of degree of severe
plastic deformation imposed into the surface layer affected by the shots´ stream. The diffrac-
tion line broadening caused by micro-strains and crystallite size reduction is taken into ac-
count by Prevéy in [11], where only the mutual effect (diffraction peak width) is considered
and evaluated with connection with the cold work.
The aim of the paper is to present a complete X-ray diffraction study of the depth profile of
real structure of shot-peened steel surfaces revealing courses of macroscopic stresses as well
as of micro-strains. Comparative indentation study can enable to highlight advantages and
lacks of method used. The broad range of selected samples includes common steels, tool
steel and high alloyed steel as well.

2. Samples
The set of analysed samples (50 x 50 x 5 mm3) was prepared from five steels: carbon steel to
the heat treatment and surface quenching SN 12 050 (A), Mn-Cr steel to the cementation
SN 14 220 (B), refractory Cr-Mo-V steel SN 17 134 (C), tool low-alloyed Mn-Cr-V steel
for the cold working SN 19 313 (D), and high speed heavy duty Mo-W-Cr steel SN 19
852 (E). Summary of main alloying elements in steels is in Tab. 1.The samples were shot-
peened by using two different intensities of blasting specified by using Almen test [12] as 0.2
mmA (samples signed by number 11) and 0.4 mmA (samples signed by number 13).
Equally, the chosen intensity of the shot peening are minimum and maximum usually used in
engineering practice. In order to analyse the stress gradients beneath the samples surface the
layers of material was gradually removed by electrolytic polishing. A STRUERS device
Lectro-Pol-5 was used. The indentation measurements were performed on polished cross
sections (10 x 5 mm2), which were cut off from the central part of the samples. Prior to shot
peening the samples were annealed (stress-relieved) in Ar at 550 °C for 2 hours.

3.Table
Used1.methods
The chemical composition (only major alloying elements) of investigated steels.

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3. Used methods
3.1 X-ray diffraction
The measurement was performed on an -goniometer Siemens with Cr-K radiation. The
line {211} of -Fe phase was measured. Nine different tilts angles ( ) from 0° to 63° were
used. The sin2 method was used for determination of macroscopic residual stress [13]. The
X-ray elastic constants ½ s2 = 5.95·10-6 MPa-1, – s1 = 1.325·10-6 MPa-1 were used in stress
calculations. The single line Voigt function method was applied for corrections of instrumen-
tal broadening (Fe powder standard was measured for all nine inclination) and determination
of microstrains and crystallite size (the data are not presented here) [14]. The microstress
micro was calculated from microstrains e using Hooke’s law ( = e E) [15] with the Young
modulus E211 = 216 GPa to be comparable with macroscopic residual stress macro. The
Young modulus represents the average of two values from E211 computed in accordance with
two extreme interaction models - Reuss and Voigt [13] for X-ray elastic constants calcula-
tion.
In order to obtain depth profiles of X-ray diffraction characteristics, the surface layers were
removed by a LectroPol–5 device for electrolytic polishing. The cooling system maintains
the temperature in the range of 15 – 25 °C.

3.2 Indentation
The DSI (depth sensing indentation) curves were obtained by apparatus NanoTestTM NT600
equipped with diamond Berkovich indenter. Each sample was indented in several different
points at each given distance from edge of treated surface. Maximal load was 50 mN; load-
ing/unloading time was 20 s; dwell time at maximal load was 10 s. The improper curves
(shifted, deformed, etc.) were excluded from calculations. Despite it each point in graphs is
an average value from minimal three measurements. Indentation hardness was calculated
according to the Oliver-Pharr method [16] which uses the unloading part of the DSI curve.

4. Results and discussions

4.1 X-ray diffraction
The samples were measured in two perpendicular directions. For reasons of clarity the aver-
age values for these perpendicular directions are used there. Ascertainment that shot peening
is symmetrical treatment [12], give us the competence for the mentioned averaging. The
single line Voigt function method [14] offer values of particle size D and microstrain e (or
micro) for each of the tilt angles , i.e. for sin2 = 0, 0.1, 0.2, … 0.8. The individual values
depend on gradients, orientation of diffracting planes (angle ), and inaccuracy of used pro-
cedures. In order to compare these data with macroscopic residual stress, the values for all
tilts and also for two perpendicular directions were averaged.
Figures 1 show the depth profiles of macro and micro stresses for all samples. The shot peen-
ing caused symmetrical both macroscopic and microscopic residual stresses. The macro-
scopic stresses are compressive.
The depth profile of microscopic stresses has nearly the same hyperbolic decreasing tenden-
cies. The surface values differentiate both among steels and intensities of blasting. All micro-

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scopic stresses are decreasing to zero with increasing depth aside the refractory steel (C)
which reaches the lowest value ca 100 MPa. This non-zero value is not evocated by shot
peening and likely to have the origin in mass content of alloying elements. The depth profiles
of macroscopic stresses show larger differences in the influenced depth than microscopic
stresses.

800 macro A13 800 macro B13

macro A11 macro B11
micro A13 micro B13
400 400
micro A11 micro B11
σ [MPa]

σ [MPa]
0 0
0 0,2 0,4 0,6 z [mm] 0,8 0 0,2 0,4 0,6 z [mm] 0,8

-400 -400

Carbon steel Mn -Cr steel

-800 -800

800 macro C13 800 macro D13

macro C11 macro D11
micro C13 micro D13
400 400
micro C11 micro D11
σ [MPa]
σ [MPa]

0 0
0 0,2 0,4 0,6 z [mm] 0,8 0 0,2 0,4 0,6 z [mm] 0,8

-400 -400

Refractory steel Tool steel

-800 -800

800 macro E13

macro E11
Figure 1. Depth profiles of macro and micro
micro E13
400 stresses for two intensity of blasting (11-low,
micro E11
σ [MPa]

13-high) for all materials A, …, E. The stan-

0
dard deviations are approximately ± 30 MPa.
0 0,2 0,4 0,6 z [mm] 0,8

-400

High speed steel

-800

The maximum values of macroscopic compressive stresses due to both the intensities (0.2
mmA – marked 11; 0.4 mmA - marked 13) applied are not different with respect to the ex-
perimental error. They reach the values of ~ 400 MPa for materials A, B, D and ~ 550 MPa
for materials C, E. The last two materials have greater strength limits than materials A, B, D
[17]. They have also higher hardness than remaining three steels. It could be as a conse-

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Z. Kristallogr. Suppl. 27 (2008) 93

quence of higher alloying, namely by chromium (Tab. 1). Thus, the magnitude of the com-
pressive stress is primarily a function of the mechanical properties of the material.
The depth of the compressive layer is influenced primarily by intensity of shot peening,
broadly speaking: approximately it is 0.2 mm for intensity of peening 0.2 mmA and 0.4 mm
for intensity of peening 0.4 mmA. The widest affected zone has Mn-Cr steel (B) where the
affected depths are approximately 0.3 and 0.5 respectively. The depth profiles of stresses are
for all materials very similar. The most different is for the refractory steel (C) which has the
widest zone of large macroscopic deformations near the surface but the depth of affected
zone is smallest among all the observed materials. These two observations show to small
deformation transfer ability. This finding is also in agreement with the lowest ductility found
out in previous work [17]. Moreover the more intensively blasted sample (C13) has the
maximum values of macroscopic stress in the depth of 0.08 mm (about 100 MPa larger com-
pressive stress than the surface value). Presumably it is a result of the main role of plastic
deformation.
4.2 Indentation
3,5 3,5
3,0 3,0 Mn-Cr steel
2,5 2,5
H [GPa] .

H [GPa] .

2,0 2,0
1,5 Carbon steel 1,5
1,0 A11 1,0 B11
0,5 A13 0,5 B13 z[mm]
z[mm]
0,0 0,0
0 0,1 0,2 0,3 0,4 0,5 0 0,1 0,2 0,3 0,4 0,5

4,5 4,0
4,0 3,5
Tool steel
3,5 3,0
3,0
H [GPa] .

H [GPa] .

Refractory steel 2,5

2,5
2,0
2,0
1,5 1,5
C11 1,0 D11
1,0
C13 z[mm] z[mm]
0,5 0,5 D13
0,0 0,0
0 0,1 0,2 0,3 0,4 0,5 0 0,1 0,2 0,3 0,4 0,5

4,5
4,0 High speed steel
3,5 Figure 2. Depth profiles of hardness for
3,0
H [GPa] .

two intensity of blasting (11-low, 13-high).

2,5 The standard deviations are approximately
2,0
± 0.2 GPa.
1,5
E11
1,0
0,5 E13 z[mm]
0,0
0 0,1 0,2 0,3 0,4 0,5

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Figures 2 show hardness depth profiles of corresponding samples investigated by XRD. The
carbon steel (A) and refractory steel (C) do not show any distinct hardened zone. Some gra-
dients of hardness can be observed only in material B, D, E. The peening process improved
surface hardness of these steels on the average for about 0.8 GPa. The hardened zone is
about 0.25 mm for both intensities of blasting. Parameters of the shot peening process have
little effect on the magnitude of the hardness being primarily a function of the mechanical
properties of the material. Nevertheless, hardness stays roughly directly proportional to
macro stress.
The hardness was locally non-uniform on the studied samples, thus indentations applied on
various places, although in the same distance from surface, lead to different results of hard-
ness. The residual impressions in material after indentation were about 7 m in diameter. The
differences in hardness may by caused by inhomogeneties in the material and also by anisot-
ropy of elastic constants. And so, the study of hardness gradients is difficult due to these
inhomogeneties.
4.3 Relations between stresses and hardness
The figure 3 is parametrical plot between macro and micro stresses where on the axis x are
plotted microscopic residual stresses micro and on the axis y are plotted macroscopic residual
stresses macro. Since dependences for both intensities of blasting are for all materials very
similar (whereas the curves for both intensities do not differ much from one another for the
same material) and on the curves for different materials are shifted each other, it can be
stated that the relations between macro and micro stress depend primarily on the material
characteristics independently of intensity of peening. Thus, dependencies for only two mate-
rials (B, C) are plotted as limiting curves for the remaining materials (A, D, E).
The horizontal parts of the curves correspond to the zones where macroscopic stresses reach
their maximum but microscopic stresses not yet. This occurred close to the samples surfaces.
The vertical parts of the curves correspond to the zones where macroscopic stresses change
rapidly as microscopic change slowly. This happened in the depths where the effect of blast-
ing vanishes (0.1 – 0.5 mm). Compare these statements with figures 1.

200 4,0
100 micro
σ [MPa]
0
3,5
-100 0 200 400 600 800 1000
H [GPa]
[MPa].

3,0 B11
-200 B11 B13
B13 2,5 D11
macro

-300 Mn-Cr steel C11 D13

σ

-400 C13 E11

2,0
-500 Refractory steel E13
-600 1,5 macro
σ [MPa]
-700 -600 -400 -200 0
Figure 3. Parametric plot of macrostress vs. Figure 4. Parametric plot of macrostress vs.
microstress for materials B and C. hardness for materials B, D, and E.

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These experiments imply that relationships between macroscopic and microscopic stresses
are independent on intensity of blasting for the particular material. Hence, knowledge of this
dependence for a given material would enable to evaluate macro stresses from micro stresses
and vice versa.
As mentioned afore, only materials B, D, and E show some distinct gradients of hardness.
Figure 4 shows parametric plots of hardness H and macrostresses for these three materials.
The values of macrostresses were extrapolated to the depth where hardness was measured.
The curves are like linear lines where greater hardness corresponds to greater compressive
residual macroscopic stresses. Similar relationship we presented elsewhere [18]. It is shown
that material characteristics are more dominant than the intensity of shot peening - curves for
different intensity of blasting are closer one to another than for different materials. In addi-
tion, the figure also shows influence of compressive stress on increase of hardness as re-
ported for sputtered films as well [19].

5. Conclusions
The shot peening caused symmetrical both macroscopic and microscopic residual stress
depth distributions. The macroscopic stresses are compressive and they reach the maximum
surface value between - 400 and - 550 MPa. Depth profiles of particular types of stresses for
all five investigated steels are similar. The former shows larger differences in course, the
latter in surface value depending on both, material and intensity of blasting. The relationship
between macroscopic and microscopic stresses is independent on intensity of blasting for the
particular material. Hence, knowledge of this dependence for a given material would enable
to evaluate macro stresses from micro stresses and vice versa.
Parameters of the shot peening process have only a little effect on the magnitude of the com-
pressive macrostress induced which is primarily a function of the mechanical properties of
the material. Subsurface range of this stress depends on intensity of the process; broadly
speaking: it is approximately 0.2 mm for intensity of peening 0.2 mmA and 0.4 mm for in-
tensity of peening 0.4 mmA.
Surface hardening by shot peening was observed namely for Mn-Cr steel (B), tool low-
alloyed Mn-Cr-V steel (D), and high speed heavy duty Mo-W-Cr steel (E); on the average for
about 0.8 GPa. Small hardening showed remaining two steels: carbon steel (A) and refrac-
tory Cr-Mo-V steel (C). Like linear dependence was found between macrostresses and hard-
ness in subsurface region.
The indentation is a less sensitive method than X-ray diffraction. Surface roughness influ-
ences measurements for small indents. Deviations of results of the indentation are also
greater because of a large influence of the surroundings of the indentation place (various
grains, grain boundary, precipitate). On the other hand, namely the micro hardness in a larger
depth indicates, that the investigated steels are considerable different. This is not clearly
manifested by the residual stresses estimated by X-ray diffraction. The intensity of the shot
peening has a less influence on the micro hardness, than on the results of X-ray diffraction
measurements.

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Acknowledgements. The research was supported by the Project No 106/07/0805 of the

Czech Science Foundation, by the Project MSM 6840770021 of the Ministry of Education,
Youth and Sports of the Czech Republic.

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