materials

Article
The Number of Subgrain Boundaries in the Airfoils of
Heat-Treated Single-Crystalline Turbine Blades
Jacek Krawczyk 1, * , Włodzimierz Bogdanowicz 1 and Jan Sieniawski 2

1 Institute of Materials Engineering, University of Silesia in Katowice, 75 Pułku Piechoty 1a St.,

41-500 Chorzów, Poland; wlodzimierz.bogdanowicz@us.edu.pl
2 Department of Materials Science, Rzeszów University of Technology, Wincentego Pola 2 St.,
35-959 Rzeszów, Poland; jansien@prz.edu.pl
* Correspondence: jacek.krawczyk@us.edu.pl; Tel.: +48-32-3497537

Abstract: In the present study, the dendrites deflection mechanism from the mold walls were
subjected to verification regarding its heat-treated turbine rotor blades. The number of macroscopic
low-angle boundaries created on the cross-section of the blades’ airfoil near the tip was experimentally
determined and compared to the number of low-angle boundaries calculated from a model based
on the dendrites deflection mechanism. Based on the Laue patterns and geometrical parameters of
airfoils, the number of low-angle boundaries occurring at the upper part of the blades airfoil after
heat treatment was calculated. This number for the analyzed group of blades ranged from 5 to 9.

Keywords: superalloys; low-angle boundaries; X-ray topography; turbine blades; crystal growth

1. Introduction
The turbine components of aircraft engines are currently most often produced using





 the CMSX-4 superalloy. The single-crystalline parts made using the CMSX-4 superalloy
possess high strength properties, even at high temperatures, which is especially important
Citation: Krawczyk, J.; Bogdanow-
for turbine rotor blades, as these types of blades are exposed to harsh working condi-
icz, W.; Sieniawski, J. The Number of
tions [1–5]. The single-crystalline rotor turbine blades, which have a very complex shape,
Subgrain Boundaries in the Airfoils
are usually produced by using the Bridgman technique [6–12]. The blades are obtained
of Heat-Treated Single-Crystalline Tur-
bine Blades. Materials 2021, 14, 8.
through directional crystallization using the temperature and withdrawal parameters that
http://dx.doi.org/10.3390/
allow the formation of an array of dendrites nearly parallel to the blade axis, with the
ma14010008 crystal orientation of each dendrite being parallel to the [001] axis. The dendrites and inter-
dendritic areas that are formed during the Bridgman process mainly consist of the Ni-based
Received: 6 November 2020 γ primary solid solution and the Ni3 Al-based γ’ secondary solid solution [13–16]. Due
Accepted: 17 December 2020 to similarity between the structure of both phases and the possibility of obtaining a clear
Published: 22 December 2020 X-ray diffraction pattern, the blades can be recognized as single-crystalline blades [17–19].
The production of the rotor blades includes subjecting them to the heat treatment
Publisher’s Note: MDPI stays neu- process to increase chemical and microstructural homogeneity and to obtain a large amount
tral with regard to jurisdictional claims of the γ’ phase, as well as to decrease the crystal orientation inhomogeneity through
in published maps and institutional elimination of the low-angle boundaries (LABs) created during crystallization [20–23].
affiliations. However, it has been stated that not all macroscopic LABs are eliminated by the heat
treatment but also that new extra LABs may be created as a result of this treatment. All of
the LABs decrease the strength of the rotor blades [24–26].
An airfoil is generally a thin-walled fragment of a blade and has the least durability of
Copyright: © 2020 by the authors. Li-
censee MDPI, Basel, Switzerland. This
all parts of a blade due to its low cross-section and the large complex loads that are acting
article is an open access article distributed
on it during its operation [27]. Therefore, analysis of the number of defects such as LABs in
under the terms and conditions of the the treated blades airfoils is extremely important. The number of the LABs with respect to
Creative Commons Attribution (CC BY) the stretching direction has a strong effect on the creep life of the blades. The LABs also
license (https://creativecommons.org/ affect the adjacent dislocation density, which is also related to the misorientation angle. It
licenses/by/4.0/). is widely accepted that the boundaries with a misorientation of above 1◦ have a significant

Materials 2021, 14, 8. https://dx.doi.org/10.3390/ma14010008 https://www.mdpi.com/journal/materials

Materials 2021, 14, 8 2 of 16

influence on the mechanical properties of the LABs. In a thin-walled airfoil, the interaction
of the dendrites with the mold walls may occur more frequently than in the root; therefore,
the LABs can be formed more often [28].
During directional crystallization, the dendrites grow directly toward the [001]-type
direction, which is only close to the blade axis Z. Therefore, even if the mold walls are
parallel to the Z, this means the dendrites can contact them. Additionally, the inclination of
the airfoil surfaces in relation to the Z axis of the rotor blade makes the growing dendrites
contact the mold walls and interact with them. The character of interactions may depend
on the angle between the axis of the dendrite primary arms and the mold surface [28].
For lower angles, the dendrite primary arms may slightly change their growth direction
near the surface, thereby creating areas of internal stress, and then stop. The higher angles
prevent a further growth of the primary dendrite arms without a change in the growth
direction. In both cases, further growth of a dendrite takes place due to the secondary
arms that are perpendicular to the primary arms [29]. Both mechanisms can lead to the
formation of low-angle boundaries. In the former case, these boundaries may be formed
after heat treatment, for example through the process of dislocation polygonization, while
in the latter case the boundaries may be formed directly during crystallization. These
mechanisms of dendrite interaction with the mold walls were proposed for the first time in
Refs. [28,30] and were referred to as the deflection of dendrites on the mold surfaces.
The aim of the research presented here was to check the assumption that in heat-treated
single-crystalline blades made of a Ni-based superalloy, each type of dendrite deflection
on the mold surface creates LABs. The assessment was performed by using experimental
determination of the LABs number in thin-walled blade airfoils where the probability of
dendrites interaction with the mold walls is high, and a comparison with the number of
LABs could be determined by using a model based on the aforementioned assumption.
The kinetics of the dendrites growth may affect the deflection mechanisms; therefore, it
was decided to examine blades airfoils that were obtained at different withdrawal rates in
the range of 2–5 mm/min, including the most commonly used rate of 3 mm/min.

2. Material and Methods

The Bridgman technique was used for production of two series of single-crystalline
turbine rotor blades. The as-cast blades made of CMSX-4 Ni-based superalloy were heat
treated and then analyzed. Each series consisted of four blades obtained at different
withdrawal rates. The directional crystallization with the use of a spiral selector (S, Figure
1a) and heat treatment process was performed in the Research and Development Laboratory
for Aerospace Materials at the Rzeszów University of Technology, Rzeszów, Poland using
industrial ALD Vacuum Technologies furnaces. In each series, four crystallization processes
were carried out at four different withdrawal rates: 2, 3, 4 and 5 mm/min. The heat
treatment, performed by using several steps, consisted of convection heating to 950 ◦ C (in
Ar or He), radiation heating to 1350 ◦ C (in vacuum), solution annealing and aging. The
temperature-time settings for annealing were: 1277 ◦ C/4 h → 1287 ◦ C/2 h → 1296 ◦ C/3
h → 1304 ◦ C/3 h → 1313 ◦ C/2 h → 1316 ◦ C/5 h → gas furnace quench; for aging, the
settings were: 1140 ◦ C/6 h (step 1) and 871 ◦ C/20 h (step 2).
Materials 2021, 14, 8 3 of 16

Materials 2021, 14, x 3 of 16

Figure 1.
Figure 1. (a)
(a) Illustration
Illustrationof
ofaaturbine
turbineblade
bladewith
witha ascheme
scheme ofof cross-sections
cross-sections I, III, and
II and III and
III and the the location
location of ET,
of the the ST,
ET,EL
ST,and
EL
and SL areas: (b) description of airfoil surface inclinations relative to the axis Z of a blade near the leading edge
SL areas: (b) description of airfoil surface inclinations relative to the axis Z of a blade near the leading edge (LE) and trailing (LE) and
trailing edge (TE); (c) a scheme for obtaining the Laue pattern for the upper sample of an airfoil with an exemplary
edge (TE); (c) a scheme for obtaining the Laue pattern for the upper sample of an airfoil with an exemplary Lauegram.
Lauegram. CL—camber line, BL—base line of cross-section II of an airfoil, δSL, δEL, δST and δET—angles of inclination of LE
CL—camber line, BL—base line of cross-section II of an airfoil, δSL , δEL , δST and δET —angles of inclination of LE and TE
and TE relative to the axis Z, εEL and εET—angles of airfoil camber, describing the rotation of airfoil surfaces to the BL, IB—
relative
incidenttoX-ray
the axis Z, εDB—diffracted
beam, EL and εET —angles
X-rayof beam,
airfoil camber,
IP—image describing
plate inthe rotation
which of airfoil
the Laue surfaces
pattern was to the BL, IB—incident
obtained. Z is perpen-
X-ray beam, DB—diffracted X-ray beam, IP—image plate in which
dicular to the base plane P; Z1, Z12, Z2 and Z12 are parallel to the Z. the Laue pattern was obtained. Z is perpendicular to the
base plane P; Z1 , Z12 , Z2 and Z12 are parallel to the Z.
X-ray diffraction topography and Laue back-reflection diffraction were used to ana-
X-ray
lyze the LABsdiffraction topography
and define the crystalandorientation
Laue back-reflection diffraction
of airfoil samples. Thewere
Laue used to analyze
method is the
the LABs and define the crystal orientation of airfoil samples. The
basic method for defining the crystal orientation which many automatic programs Laue method is the basic
and
method for
indexing defining
systems arethe
also crystal
basedorientation
on [31]. Thewhich many X-ray
Panalytical automatic programs
system (Alamelo, andThe indexing
Neth-
systems are also based on [31]. The Panalytical X-ray system (Alamelo, The Netherlands)
erlands) equipped with a microfocus tube (with a quasi-point source of 40 × 402µm2) emit-
equipped with a microfocus tube (with a quasi-point source of 40 × 40 µm ) emitting
ting characteristic CuKα divergent beam radiation was used for topography studies. The
characteristic CuKα divergent beam radiation was used for topography studies. The anode
anode current of 0.3 mA and an anode-cathode voltage of 30 kV were applied. The topo-
current of 0.3 mA and an anode-cathode voltage of 30 kV were applied. The topograms of
grams of the 113 reflection, which is the reflection with the highest intensity for the ana-
the 113 reflection, which is the reflection with the highest intensity for the analyzed sample
lyzed sample surface (surfaces of the samples are parallel to the (001) crystal plane), were
surface (surfaces of the samples are parallel to the (001) crystal plane), were recorded
recorded on the AGFA Structurix D7 X-ray film with a grain size of 7 µm. The oscillations
on the AGFA Structurix D7 X-ray film with a grain size of 7 µm. The oscillations of the
of the coupled sample and film were applied during exposure of the topograms. The
coupled sample and film were applied during exposure of the topograms. The source-to-
source-to-sample distance was 25 mm and the sample-to-film distance was 10 mm. The
sample distance was 25 mm and the sample-to-film distance was 10 mm. The details of the
details of the experiment are presented in Appendix A. The Laue patterns were obtained
experiment are presented in Appendix A. The Laue patterns were obtained on the image
on the image plates using the X-ray diffractometer of the RIGAKU/EFG XRT-100CCM
plates using the X-ray diffractometer of the RIGAKU/EFG XRT-100CCM system provided
system
by EFG provided by EFG Freiberg
Freiberg Instruments Instruments
(Freiberg, Germany). (Freiberg, Germany).
The accuracy of the The
angle accuracy
measurement of the
angle
in the Laue diffraction method was determined by using the spot size and the precisionsize
measurement in the Laue diffraction method was determined by using the spot of
and the precision
the sample of the
positioning in sample positioningholder.
the diffractometer in the The
diffractometer
reference planeholder. The
of the reference
goniometer
plane
allowed of us
thetogoniometer
set the sampleallowed usholder
in the to set with
the sample
a meaninerror
the holder
of aboutwith
0.3◦a. mean error of
To determine
about 0.3°. To determine the orientation measurement error related to the
the orientation measurement error related to the size and shape of the Laue spots, a circular size and shape
of the Laue
envelope of spots, a circular
each spot envelope
was outlined andofthe
each spotofwas
center theoutlined
envelopeand wasthe center
found. Theof longest
the en-
velope was found. The longest distance from the spot center to the
distance from the spot center to the envelope for the Laue pattern was the mean error envelope for the Laueof
pattern
◦
0.5 . was the mean error of 0.5°.
There are several
There are severalmethods
methodsthat thatcan
canbebeused
usedtotovisualize
visualizelow-angle
low-angle boundaries
boundaries in in sin-
single
gle crystals. They mainly differ in the type of X-ray source, shape and
crystals. They mainly differ in the type of X-ray source, shape and width of the incidentwidth of the incident
beam,
beam, spatial
spatial and angular resolution.
and angular resolution. Table
Table 11 presents
presents some
some parameters
parameters of of these
these X-ray
X-ray
topography
topography methods
methods andand their
their application
application forfor different
different materials.
materials. TheThe methods
methods allowing
allowing
for higher limit resolution with the use of conventional X-ray sources, e.g., the Berg-Bar-
rett or Lang methods, use a highly collimated narrow incident beam. There are two draw-
Materials 2021, 14, 8 4 of 16

for higher limit resolution with the use of conventional X-ray sources, e.g., the Berg-Barrett
or Lang methods, use a highly collimated narrow incident beam. There are two drawbacks
to using such methods when examining large engineering elements: the area covered by
the X-ray beam is relatively small and may not cover the entire sample; additionally, some
areas of the sample with a higher misorientation angle (e.g., several arc degrees) may not
be visible on the topogram due to a failure to meet the Bragg condition. This made it
impossible to visualize all LABs that may be present in the single-crystalline casts made of
the superalloys on the one topogram. Such casts, obtained by using the Bridgman method,
consist of a set of almost parallel dendrites and their groups (called subgrains) with a
fairly large dispersion of the misorientation angle, including from arc minutes to angular
degrees [32]. The X-ray topography with a divergent width beam and oscillation of the
coupled sample and film that was applied in this study seemed to meet all of the relevant
requirements and was suitable for the visualization of all LABs in the relevant casts.

Table 1. The parameters of different X-ray topography methods and their applications.

Analyzed Crystals
Incident Diffraction Limit Single-
The Method X-ray Source Sample Almost
Beam Geometry Resolution Crystalline
Perfect
Superalloys
narrow
Berg-Barrett conventional reflection small arc seconds [33] yes yes
parallel
narrow
Lang conventional transmission small, thin arc seconds [33] yes no
parallel
Applied in wide
conventional reflection large arc minutes [34] yes yes
this study divergent
reflection/
White beam synchrotron parallel wide range arc seconds [35] yes yes
transmission

The rotor blades casts are divided into two main parts—bulk root and fine airfoil
(Figure 1a). Three cross-sections I, II and III of the airfoils were made for each analyzed
blade. The first section (I) was localized near the platform ABC of the root (Figure 1a).
The third cross-section (III) was cut off of the airfoil’s tip part with a height h = 3 mm,
and the second cross-section (II) divided the remaining fragment of the airfoil with the
height L into two parts named the bottom sample and the upper sample. The bottom and
the upper samples had the same height L* = L/2. The tip parts of the airfoils were not
studied because they contained high internal stresses that made it impossible to create clear
diffraction images. The airfoils of rotor blades are bounded by two surfaces, the suction and
pressure surface, which are indicated in Figure 1b by white and black arrows, respectively.
Both surfaces are twisted around blade’ axis Z like a clockwise screw. The twist can be
defined by continuous rotation of the chord line called the base line (BL) (Figure 1c) at each
transverse section along the axis Z. In addition to this rotation, changes in the cambers of
the airfoil may occur, which are related to changes in angles of the airfoil surfaces’ rotation
to the BL, which can be approximately described by the angles ε, marked for example in
Figure 1c as εET and εEL for the upper airfoil samples. The angles ε may be defined as
the angles of rotation of camber line fragments located near the leading edge (LE) and the
trailing edge (TE).
The values of the angles εEL and εET are different for the cross-sections I and II because
the rotation of airfoil surfaces to the BL change continuously along the axis Z (Figure 1a).
The suction and pressure surfaces are inclined towards the axis Z. These inclinations lead
in turn to inclinations of the LE and TE to the Z axis (Figure 1b). The inclination angles δ of
the LE and TE are different to those of the angles ε, and the characteristics of the δ angles’
changes along the Z axis are also different. The angle δ for the LE increases along the axis
Z (δEL > δSL , Figure 1b) and decreases for the TE (δET < δST , Figure 1b). There is a narrow
area in the central part of the airfoil, marked in Figure 1a,c in black, for which both the
Materials 2021, 14, 8 5 of 16

suction and pressure surfaces are parallel to the axis Z. The inclination angle of the area is
δ = 0 along the entire height of the airfoil from its beginning near the root to its tip. The
geometric dimensions, including the length and thickness of the airfoil and the angles of
its edges, were obtained using a 3D scanner. The measurement accuracy was 0.2◦ for the
angles and 0.1 mm for the length dimensions.
In order to experimentally determine the number of LABs, X-ray diffraction topograms
were obtained from the upper sample surfaces marked in Figure 1a by thin black downward
arrows. To obtain the topograms, the samples were oriented using an additional Laue
back-reflection diffraction from the surface Q of section III (Figure 1a,c). The macroscopic
LABs are planar defects and their surfaces in airfoils are approximately parallel to the axis Z
of the blade [28]. Therefore, it can be assumed that the LABs created during crystallization
in the lower part of the airfoil with any distance from the platform ABC would be extended
along the axis Z—the axis which indicates the direction of the crystallization process—and
would pass through the upper parts of the airfoil. Therefore, in cross-section III near the tip
of the airfoil, all of the low-angle boundaries created during crystallization of the airfoil
would appear.

3. Results and Discussion

Figure 2 shows X-ray topograms obtained for airfoils of two series of blades obtained
at the withdrawal rates of 2 mm/min, 3 mm/min, 4 mm/min and 5 mm/min each. The
presented topograms were obtained from the surface Q of the upper sample located near
the tip of the airfoil, where the crystallization of the blades was coming to an end. The
topograms obtained from the cross-section III contain images of all of the LABs created
during the passage of the crystallization front along the axis Z across the entire length
of the blade airfoil, as well as images of LABs that were inherited by the airfoil from the
root [28]. The topograms consist of the groups of contrast stripes or/and spots marked for
example as SG1, SG2, SG3 and SG4 in Figure 2a. The individual contrast spots and stripes
visualize the separate dendrites while the groups indicate the individual subgrains (which
are SG type subgrains—see Figure 2 for further details). The mutual shift of the images of
neighboring dendrites or the images of the neighboring subgrains allows for determination
of the angle of their mutual misorientation, which also describes the disorientation angle
of the LABs. The mutual misorientation angle calculation method is described in Ref. [34].
The misorientation angle between the single dendrites was found to be up to 0.3◦ , and it
was higher between groups of dendrites. This criterion allowed us to identify the subgrain
in nickel-based dendritic superalloys.
There were visible bright bands with a low-contrast (or a lack of contrast) between the
images of subgrains. The bands represent LABs between subgrains. The areas of adjacent
subgrains in the topograms were spaced and/or shifted relative to each other. Sometimes
the low-angle boundaries were visualized in the topograms by using increased contrast,
as presented in Figure 2h—LAB no.3. The reason for the above is that the crystal lattices
(diffraction planes) of certain neighboring subgrains were inclined toward each other in
such a way that their images in the topograms partially overlapped.
The LABs with misorientation angles of above 0.3◦ are marked by the arrows in
Figure 2 and numbered, which allows determination of their number N. The error of the
misorientation angle measurement depended on many factors related to the material of the
sample and the instrument error. The mean orientation error for the presented results was
about 8 arc minutes. The selection of the LAB in the topograms was based on the criteria
described in detail later and related to the mechanism of LABs creation.
Materials 2021, 14, 8 6 of 16

Materials 2021, 14, x 6 of 16

Figure 2. X-ray topograms obtained from micro-section III of an airfoil of I-series (a–d) and II-series (e–h) obtained at a
Figure 2. X‐ray topograms obtained from micro‐section III of an airfoil of I‐series (a–d) and II‐series (e–h) obtained at a
withdrawal rate of 2 mm/min (a,e), 3 mm/min (b,f), 4 mm/min (c,g) and 5 mm/min (d,h). Reflection 113. CuKα radiation.
withdrawal rate of 2 mm/min (a,e), 3 mm/min (b,f), 4 mm/min (c,g) and 5 mm/min (d,h). Reflection 113. CuKα radiation.
The boundaries creation may be related to the mechanism of the growing dendrites
There from
deflection werethevisible bright
surface of thebands with
casting a low‐contrast
mold, which was(or firsta proposed
lack of contrast) between
in Ref. [28]. This
the images of subgrains. The bands represent LABs between subgrains.
mechanism was based on stopping the primary arm growth on the mold wall (at the The areas of adja‐
point
cent subgrains
R, see Figure 3a) in and
the topograms were spaced
the continuation and/or shifted
of crystallization by therelative to each
secondary other.
arms, andSome‐
then
times
(at thethe low‐angle
point boundaries
T, see Figure 3a) by were visualized
the tertiary in the
dendrite topograms
arms. Becauseby theusing increased
secondary con‐
dendrite
trast,
arms as presented
were arranged in in
Figure 2h—LAB
the arrays no.3. The
connecting thereason
suckingfor and
the above
pressureis that the crystal
surfaces of the
lattices (diffraction planes) of certain neighboring subgrains were inclined
airfoil, their image (and also the image of the LABs) was visible along the entire width toward eachof
other in such a way that their images in the topograms partially
the topogram. Such a growth path occurs when the angle δ between the primary arms overlapped.
and The LABs wall
the mold with ismisorientation
higher than the angles of above
critical 0.3° At
one [30]. areamarked
very low byδthe arrows
angle in Fig‐
(Figure 3a)
ure
below2 and
the numbered,
arc minute,which allows determination
the dendrites do not deflectofontheir number
the mold N. Thethis
wall—in error of the
case, the
misorientation
dendrites bendangle measurement
and continue depended
to grow parallel on many
to the TE factors related
axis, while LABsto the material
are not formed of
the sample and the instrument error. The mean orientation error for
either during the dendrite growth from the melt or after the heat treatment. When the the presented results
was
angle about 8 arc minutes.
δ is higher but remainsThelower
selection
thanof the
the LAB level,
critical in thethen
topograms was based
the primary dendriteon arm
the
criteria
may bend described
before in detail later
deflection, and related
which leads to tocreation
the mechanism
of an areaof LABs creation.
of internal stress where
extraThe boundaries
LABs can also be creation
formed may be heat
after related to the mechanism
treatment of the growing
[36]. The surfaces of these dendrites
LABs are
deflection from the surface of the casting mold, which was first proposed in Ref. [28]. This
mechanism was based on stopping the primary arm growth on the mold wall (at the point
 of the topogram. Such a growth path occurs when the angle δ between the primary arms
and the mold wall is higher than the critical one [30]. At a very low δ angle (Figure 3a)
below the arc minute, the dendrites do not deflect on the mold wall—in this case, the
dendrites bend and continue to grow parallel to the TE axis, while LABs are not formed
Materials 2021, 14, 8 either during the dendrite growth from the melt or after the heat treatment. When the
7 of 16
angle δ is higher but remains lower than the critical level, then the primary dendrite arm
may bend before deflection, which leads to creation of an area of internal stress where
extra LABs can also be formed after heat treatment [36]. The surfaces of these LABs are
approximatelyparallel
approximately parallelto
tothe
theblade
bladeaxis
axisZZ[28,30].
[28,30].Therefore,
Therefore, in in
thethe airfoil
airfoil cross-section
cross-section III
III (Figure 1a), all LABs—which formed as a result of deflections that
(Figure 1a), all LABs—which formed as a result of deflections that occurred alongoccurred along the
the en-
entire
tire airfoil
airfoil height
height LL (Figure1a)—appeared.
(Figure 1a)—appeared.ItItfollows
followsthat
thatto
to theoretically
theoretically calculate
calculate the
the
number N of the low-angle boundaries visualized on the cross-section III, it was
number N of the low-angle boundaries visualized on the cross-section III, it was necessary necessary
to calculate
to calculate the
the number
number ofof acts
acts of
of dendrites
dendrites deflection
deflection from
from the
the surface
surface of
of the
the mold
mold walls.
walls.

Figure 3. Schemes
Schemes of ofdendrite
dendritedeflection
deflectionfrom
fromthethe mold
mold walls’
walls’ surfaces
surfaces parallel
parallel toTE
to the theinTEtheinET
the ET fragment
fragment (a) blades
(a) of the of the
blades airfoil. The δ, φ, α* and β* angles are enlarged for figure clarity. Section m in (b,c) is the projection
airfoil. The δ, ϕ, α* and β* angles are enlarged for figure clarity. Section m in (b,c) is the projection of the primary arm of the primary
arm direction
direction parallel
parallel to theto[001]
the [001] onplane
on the the plane defined
defined bypoints
by the the points
M, N,M,N,P
P andand R which
R which is perpendicular
is perpendicular to axis
to the the axis
XT of of
XTthe
the CL (c), and sections m’ and m” in Figure 3c are the projections of secondary and tertiary arms deflected from the
CL (c), and sections m’ and m” in Figure 3c are the projections of secondary and tertiary arms deflected from the fragments
fragments S°I and S°II of mold walls planes of the ET area.
S◦ I and S◦ II of mold walls planes of the ET area.

The
The number
number of of deflections
deflections is particularly important
is particularly important for for fine
fine airfoils.
airfoils. Although
Although the the
angle δ is usually low (less than 12–15°) ◦ because the airfoil dimension
angle δ is usually low (less than 12–15 ) because the airfoil dimension D is also low D is also low (Figure
(Figure
3a),
3a), the
the number
number of of deflections
deflectionsisisfairly
fairlyhighhighasasaaresult.
result.The
Themechanisms
mechanisms forfor LABs
LABs creation
creation in
in the bulk root connected with the selector provide different results. The
the bulk root connected with the selector provide different results. The main reason for this main reason for
this is a fast,
is a fast, unsteady
unsteady lateral
lateral growthgrowth of dendrites
of dendrites nearnear the selector-root
the selector-root connection
connection surface
surface [37].
[37]. Usually,
Usually, two LABs
two LABs are formed
are formed in thein the which
root, root, which are inherited
are inherited by theby the airfoil
airfoil [28].
[28]. These
These macroscopic
macroscopic LABs LABs
created created
in theinrootthe are
roottens
are of
tens of millimeters
millimeters long.long.
The The
LABs LABs
thatthat
are
are inherited by the airfoil pass through its entire cross-section. Taking
inherited by the airfoil pass through its entire cross-section. Taking the aforementioned the aforemen-
tioned mechanisms
mechanisms into account,
into account, the criteria
the criteria used to used to indicate
indicate the LABs
the LABs imageimage
in thein the topo-
topograms
grams
can becan be described
described as follows:
as follows: the decreased
the decreased or increased
or increased contrast
contrast bands
bands representing
representing the
the
LABs LABs
mustmustcrosscross the entire
the entire widthwidth
of theof the topogram;
topogram; these contrast
these contrast bands mustbandsbemust
formedbe
formed
betweenbetween
the otherthe other bands
contrast contrast bands representing
representing the groupsthe groups
of the of theand
dendrites; dendrites; and
the contrast
the
bandscontrast bands representing
representing the dendritethe dendrite
group group (subgrains)
(subgrains) mustintegrally
must be shifted be shifted relative
integrally
to
the adjacent bands representing the other group. Typically, the shift of the contrast bands
representing subgrains is higher than the shift between the contrast spots and/or the
stripes representing the individual dendrite, i.e., a shift greater than 0.3◦ . The error in
determining the misorientation angle is very important when calculating the number of
LABs. The LABs may be created as a result of deflection; therefore, the internal stresses may
appear, causing blurriness or/and a bend of the contrast line in the topograms (e.g., SG3,
Figure 2c). A large misorientation of the single dendrite can also occur, which is visualized
in the topogram by a greater shift between the contrast bands visualizing the neighboring
dendrites (above LAB no.6 in Figure 2h). As a result of these phenomena, incorrect LAB
identification may occur, resulting in inaccurate counting.
Materials 2021, 14, 8 8 of 16

The resolution of the method for determining the number of LABs is related to the
resolution of the X-ray topography, but it is not crucial in this case. The aim of the
experiment was to determine the number of macroscopic LABs formed as a result of
the dendrites deflection mechanism using recorded topograms. Theoretically, for almost
perfect single-crystals, the resolution of the applied X-ray topography method is several
arcmin [34]. However, for the dendritic single-crystalline nickel-based superalloys of the
CMSX-4 type, the resolution ranges from a dozen to several dozen arcmin. The outcome
depends on the existing internal stresses, the X-ray background level and the arrangement
of the diffraction planes in relation to the analyzed surface. For the CMSX-4 containing
several alloying elements, it also depends on the heterogeneity of the spatial distribution
of these elements. Although the resolution of the applied method is lower than that of the
Berg-Barrett or Lang method, it is still useful for visualizing all sample areas with high
misorientation angle ranges from a dozen arcmin to several angular degrees on the one
topogram [32]. Additionally, the divergence of the X-ray beam allowed us to obtain the
topograms from large sample surfaces—even up to approximately 10 cm2 . This is very
important for testing engineering products such as turbine blades.
The linear resolution of the applied method was in the order of 100 µm for almost
perfect single-crystals. The thickness of the dendrites in the analyzed samples of superal-
loys obtained by using the Bridgman technique with the withdrawal rate from the high
temperature zone of 2–5 mm/min ranged from 300 µm to 100 µm [1], so in this case the
images of all dendrites could be seen on the topograms. As the images of the dendrites
were visible in the topograms (Figure 2) in the form of stripes or spots, the linear resolution
limit ranged from 100–300 µm. In the presented research, it was necessary to visualize
all possible existing LABs with a misorientation angle ranging from several arcmins to
several degrees of arc. It was not necessary to increase the resolution to arcsec, which
could have been achieved by using the Berg-Barrett method. The scheme of the primary
dendrite arm arrangement, for example in the fragment ET with the thickness D and height
L* (Figure 3b,c), may be used to calculate the number of dendrite deflections. It can be
correctly assumed that a dendrite grows directly toward the direction [001], as is commonly
believed to occur [38].
SI and SII in Figure 3b are the side walls of the blade airfoil (and the casting mold)
parallel to the TE (Figure 1c). The direction [001] is the direction of the primary dendrite
arm that reaches the point R and then deflects. The unit vector KR indicates the direction
of the dendrite growth. Then the dendrite growth was continued by the secondary arm
up to the point T (Figure 3c). The tertiary arms growth began at the point T and reached
the point U where subsequent deflection occurred. In order to simplify considerations,
it was assumed that the angle between the subsequent rows of dendrite arms is a right
angle (Figure 3c). Since the distance D is small, and the secondary dendrite arm is almost
perpendicular to the mold walls, the distance h (Figure 3b) was small in comparison to b,
therefore it could be assumed that l ≈ b. Using the above assumptions, the Equation (1)
that allowed us to calculate the number of deflections N was obtained (see Appendix B):

L∗
N= × tan α∗ × sin β∗ (1)
D
where α* is the angle between the direction [001] and the TE, and β* is the angle between
the projection of the direction [001] on a certain plane (the plane is perpendicular to TE)
and the axis XT (the axis is parallel to the fragment CL of the airfoil area ET) (Figure 1c).
The angles could be determined using the Laue patterns of the airfoil cross-sections. The
Laue patterns were obtained by arranging the baseline BL* of the image plate parallel to the
baseline BL of the airfoil cross-section (Figure 1c). The primary X-ray beam was directed at
the airfoil region with δ = 0. The Laue patterns were obtained from the points RS and RE
(Figure 1a) of the bottom and the upper samples of each blade airfoil, respectively.
An airfoil can be divided into five areas: one area with the angle δ = 0, the two areas
SL and EL (Figure 1a) (their inclination to the axis Z can be referred to as the inclination of
 and the axis XT (the axis is parallel to the fragment CL of the airfoil area ET) (Figure 1c).
The angles could be determined using the Laue patterns of the airfoil cross-sections. The
Laue patterns were obtained by arranging the baseline BL* of the image plate parallel to
the baseline BL of the airfoil cross-section (Figure 1c). The primary X-ray beam was di-
Materials 2021, 14, 8
rected at the airfoil region with δ = 0. The Laue patterns were obtained from the points RS
9 of 16
and RE (Figure 1a) of the bottom and the upper samples of each blade airfoil, respectively.
An airfoil can be divided into five areas: one area with the angle δ = 0, the two areas
SL and EL (Figure 1a) (their inclination to the axis Z can be referred to as the inclination
the LE relative
of the to Z)
LE relative toas
Z)well as the
as well twotwo
as the areas ST and
areas ET (Figure
ST and 1a) (their
ET (Figure inclination
1a) (their can be
inclination can
referred to astothe
be referred as inclination
the inclinationof theofTE). The area
the TE). with with
The area δ = 0δis=the
0 ismiddle area and
the middle area was
and not
was
considered because
not considered it is relatively
because narrow
it is relatively (Figure
narrow 1a). The
(Figure 1a). areas SL and
The areas SL STandofSTthe
ofbottom
the bot-
sample, as well as the areas EL and ET of the upper sample, are rotated
tom sample, as well as the areas EL and ET of the upper sample, are rotated around around the BL ofthe
the
BLbottom and theand
of the bottom upper samples
the upper by the by
samples angles ε and are
the angles inclined
ε and to the blade
are inclined to the axis
bladeZ axis
by
their
Z byrespective anglesangles
their respective δ. δ.
Figure
Figure44shows
showsaamodelmodelfragmentation
fragmentationand andarrangement
arrangementofofthe thefour
fourairfoil
airfoilareas
areaswith
with
their
their geometrical parameters. The areas were modeled as plates with parallel surfacesofof
geometrical parameters. The areas were modeled as plates with parallel surfaces
the
theaverage
averagethickness
thicknessDDand andheight
heightL*.
L*. The
Thevalues
valuesofofthe
theangles
anglesδδand andε,ε,asaswell
wellasasthe
the
value of L* = L/2 (Figure 1a) for concerned areas are presented
value of L* = L/2 (Figure 1a) for concerned areas are presented in Table 2. in Table 2.

Figure4.4.Model
Figure Modelscheme
schemeofofthe
theareas
areasSL
SLand
andSTSTofofthe
thebottom
bottomsample,
sample,asas well
well asas the
the areas
areas ELEL and
and ET
ET of the upper sample of the blade airfoil with the characteristic parameters of the blades
of the upper sample of the blade airfoil with the characteristic parameters of the blades geometry. geome-
try.
Table 2. Characteristic geometric parameters of the SL, ST, EL and ET airfoil areas.
Table 2. Characteristic geometric parameters of the SL, ST, EL and ET airfoil areas.
Airfoil Area ◦ ε (◦ )
Airfoil Area L* (mm) L* (mm)D (mm)
D (mm)L*/D L*/D δ ( ) δ(°) ε (°)
SL SL 15.0 15.0 3.7 3.7 4.05 4.05 7.5 7.5 45.0
45.0
ST 15.0 1.8 8.33 4.5 48.0
ST 15.0 1.8 8.33 4.5 48.0
EL 15.0 2.0 7.50 11.0 20.0
ET EL 15.0 15.0 1.2 2.0 12.5 7.50 1.5 11.0 20.0
40.0
ET 15.0 1.2 12.5 1.5 40.0
To determine the number of deflections N of each of the areas SL ST, EL and ET using
the Equation (1), it was necessary to experimentally determine the angles α* and β* of
these areas.
Figure 5 shows a scheme of the areas EL and ET of the upper sample, as well as
arrangement of the image plate in which the Laue back-reflection pattern was recorded.
During the experiment, both the sample surface and the image plate were positioned verti-
cally, and the X-ray beam was positioned horizontally. The diffracted beam (Figure 5b) was
directed in the opposite direction to the dendrites growth direction. The crystallographic
 the Equation (1), it was necessary to experimentally determine the angles α* and β* of
these areas.
Figure 5 shows a scheme of the areas EL and ET of the upper sample, as well as ar-
rangement of the image plate in which the Laue back-reflection pattern was recorded.
Materials 2021, 14, 8 During the experiment, both the sample surface and the image plate were positioned 10 ver-
of 16
tically, and the X-ray beam was positioned horizontally. The diffracted beam (Figure 5b)
was directed in the opposite direction to the dendrites growth direction. The crystallo-
graphic orientation—which determines the direction of the growing dendrite—is repre-
orientation—which determines the direction of the growing dendrite—is represented by the
sented by the spot rd on the real lauegram. The spot is obtained by using inversion of the
spot rd on the real lauegram. The spot is obtained by using inversion of the 001 reflection
001 reflection (r spot) relative to the center of the lauegram. The position of the Laue spot
(r spot) relative to the center of the lauegram. The position of the Laue spot r is determined
r is determined by using → the vector n∗⃗, which proceeds in a normal direction towards the
by using the vector ∗
n , which
diffraction plane (001), and itsproceeds
directionin a normal direction
corresponds towards the
to the diffracted diffraction
beam. plane
The direction
→
(001),
of the and
vector n ⃗, whichcorresponds
its direction also proceeds to in
thea diffracted beam. The
normal direction direction
towards of the vector
the diffraction nd ,
plane
which corresponds
(001), also proceedstointhe a normal direction
direction of thetowards
growing thedendrites.
diffractionThe plane (001), corresponds
extension of the dif-
to the direction of the growing dendrites. The extension of
fracted beam up to the intersection with the created virtual lauegram (Figure 5b) the diffracted beam up deter-
to the
intersection with the created virtual lauegram (Figure 5b) determines
mines the location of the spot rd. To determine the location of the rd spot, a virtual the location of the
spot rd . To
lauegram wasdetermine
drawn on thethelocation of the
other side rd spot,
of the samplea virtual
where lauegram was back-reflected
a hypothetical drawn on the
other pattern
Laue side of the couldsample where The
be created. a hypothetical back-reflected
virtual lauegram was created Lauewith
pattern
the could be created.
assumption that
The incident
the virtual lauegram
beam was was createdfrom
directed with thethe assumption that the
top to the point RE. incident beamthe
In this case, was directed
diffracted
from the
beam top through
passes to the point
the R E . In this
virtual case, the
lauegram in diffracted
the spot rdbeam
. Thispasses
spot canthrough the virtual
be transferred to
lauegram in the
the real lauegram, whichspot r d . This spot can be transferred to the real lauegram,
is parallel to the incident beam. As a result of the transfer which is parallel
of the
to therdincident
spot from thebeam. Aslauegram
virtual a result oftothe thetransfer of the spot
real lauegram, an rextra
d from theisvirtual
spot lauegram
created. The posi-to
the real lauegram, an extra spot is created. The position of the spot
tion of the spot rd was determined by inversion of the position of thedspot r relative to the r was determined by
inversion
center of the
of the position of the spot r relative to the center of the lauegram.
lauegram.

Figure 5.
Figure 5. Exemplary
Exemplary illustration
illustration of
ofthe
theareas
areasEL
ELand
andETETofofthe
theupper
uppersample
sampleofof
anan airfoil
airfoil obtained
obtained at at
thethe withdrawal
withdrawal rate
rate of
of 5 mm/min, with geometric description of angles α, β and β* (a) and a diagram explaining how to determine the position
5 mm/min, with geometric description of angles α, β and β* (a) and a diagram explaining how to determine the position of
of the spot rd on the lauegram through inversion of the spot r (b). The plane SXY is parallel to the plane p and cross-sections
the spot rd on the lauegram through inversion of the spot r (b). The plane SXY is parallel to the plane p and cross-sections I,
I, II and III in Figure 1a, while the BL* of the lauegram is parallel to the BL of an airfoil cross-section. IP—image plate, IB
II and III in Figure 1a, while the BL* of the lauegram is parallel to the BL of an airfoil cross-section. IP—image plate, IB
and DB—incident and diffracted X-ray beam, DGD—dendrite growth direction. n→∗⃗ and n ⃗—unit vectors which proceed
∗ →
and DB—incident
in a normal andtowards
direction diffracted
theX-ray beam,plane
diffraction DGD—dendrite
(001) with thegrowth direction.
direction n and ndto
corresponding —unit vectors which
the diffracted beamproceed
and the
dendrite
in growth
a normal direction.
direction towardsZ0, the
Z12 and Z22 are plane
diffraction parallel to the
(001) Z axis
with of the blade.
the direction corresponding to the diffracted beam and the
dendrite growth direction. Z0 , Z12 and Z22 are parallel to the Z axis of the blade.

The angles εEL and εET between the CLL and BL, as well as the CLT and BL, re-
spectively for the areas EL and ET, were determined on the basis of the shape of the
micro-section II (Figure 1a). The εEL was 20◦ and the εET was 40◦ . Afterwards, using the
QLaue software, the Laue patterns recorded from the point RE were rotated around the
axis ZL by using the angles εET and εEL , until the BL* of the lauegram lined up parallel
to the CLT and CLL (lauegram II and III, Figure 5a). The reflex r (Laue pattern I), which
was obtained from the (001)-type diffraction planes, changed location to r’ and r” on the
Materials 2021, 14, 8 11 of 16

rotated Laue patterns II and III, respectively. However, the transformed rd spot was taken
into account in further analysis because it is related to the direction of growing dendrites.
As an example, the area ET of the upper sample was considered. In the cubic system, the
directions of [001]-type are perpendicular to the crystal planes of (001)-type, which allowed
us to define the inclination of the crystallographic direction [001] and the dendrites growth
direction to the pressure and suction surfaces, meaning in relation to the walls of the mold.
The primary arms growth direction may be defined by the position of the spot rd ’ on the
rotated lauegram II. Based on the rotated Laue pattern II and using the QLaue software,
the rotation angles components αM and αN of the primary arms growth direction relative
to the axes M and N, which are respectively perpendicular and parallel to the CLT (XT ),
may be determined (Figure 5). When considering the blades obtained at a withdrawal
rate of 5 mm/min, the angles were found to be αM = 6.0◦ and αN = 8.0◦ for the exemplary
area ET (Figure 5a). It is important to note that for the angle δET , the component δET of
the rotation around the axis N of the primary arms growth may be calculated by using
the equation γET = αN + δET and in a more general case by the equation γET = αN ± δET .
Additionally, the Laue pattern II allowed us to determine the angle β* using the equation
β* = β − εET (β* = −31 − 40 = −71◦ ). The angle γEL may be determined similarly, using
the rotated Laue pattern III.
As an example, for the upper sample, the angles of the surfaces inclination relative to
the axis Z and rotation around the axis Z relative to the BL are as follows: for the area ET −
δET = 1.5◦ , εET = 40.0◦ , for the area EL − δEL = 11.0◦ , εEL = 20.0◦ (see Table 2).
Because the angle β* can take negative values (Laue pattern II, Figure 5), the absolute
value of sin β* must be used in Equation (1). Therefore, the following Equation (2) should
be used for the calculation of N:
L∗
N= tan(α∗ ) × |sin(β∗ )| (2)
D
Taking into consideration
q the components αM and αN of the area ET and the fact that
q
= αM + γET = αM + (αN ± δET )2 , Equation (2) can be denoted into the following
(α∗ ) 2 2 2

Equation (3):
L∗
q 
N= × tan α2M + (αN ± δET )2 × |sin(β ± εET )| (3)
D
The choice of the +/− sign was made on the basis of the localization of the image
plate quadrant in which the spot rd ’ is present.
As an example, calculations of the number of deflections NET for the area ET are
presented below. In this case, there is the sign “−” in front of the δET because the inclination
δET = 1.5◦ of the ET was consistent with the inclination of the dendrite relative to the axis
N. The sign “−” also appears in front of the εET because the rotation of the image plate was
counterclockwise. Given the above, the Equation (3) takes the Equation (4).

L∗
q 
NET = ET × tan α2M + (αN − δET )2 × |sin(β − εET )| (4)
DET

Putting these values into Equation (4), we obtained:

−71◦
 
q  z }| {
NET = 12.5 × tan 62 + (8 − 1.5)2 × sin−31◦ − 40◦  = 1.92 ≈ 2 (5)
 

Similar calculations can be made for the area EL of the upper sample. In this case,
there is the sign “+” in front of the δEL because the inclination δEL = 11◦ (Figure 5a) of the
leading edge and the surfaces’ EL was opposite to the inclination of the component αN of
Materials 2021, 14, 8 12 of 16

the dendrite. The sign “+” also appears in front of the εEL because the rotation of the image
plate was clockwise. Given the above, the equation for the NEL takes the Equation (5).

L∗
q 
NEL = EL × tan α2M + (αN + δEL )2 × |sin(β + εEL )| (6)
DEL

Putting these values into Equation (5), the NEL was obtained as follows:
 
q  −11
z }| {
NEL = 7.5 × tan 9.52 + (3.5 + 11)2 × sin−31◦ + 20◦  = 0.41 ≈ 0 (7)
 

The sinus and the tangent functions can take real numbers, therefore the calculated
values were rounded to integers. The number N of the low-angle boundaries, which can
be determined experimentally from the topograms obtained from the airfoil cross-section
III (Figure 1a), is equal to the sum of the numbers of the low-angle boundaries created by
deflection in the whole airfoil:

N = NST + NET + NSL + NEL (8)

In addition, two LABs from the root are usually inherited to the airfoil [28], which
results in the equation:
N = NST + NET + NSL + NEL + 2 (9)
To verify the aforementioned mechanism of deflection, the data obtained experimen-
tally in topograms were compared to the data calculated using Equation (7). Table 3 shows
the experimental results and the calculations results of the number of LABs in the cross-
section III for two series of blade casts obtained by using the Bridgman technique at the
withdrawal rate of 2, 3, 4 and 5 mm/min and then heat treated.

Table 3. The number of LABs defined by calculations and from X-ray topograms for airfoils of blades obtained in two series
at the withdrawal rates of 2, 3, 4 and 5 mm/min.

W Number of Subgrains Total (+2 from Identified in

Sum
(mm/min) the Root) Topograms
ET ST EL SL
2 2.34 2 1.23 1 2.90 3 0.81 1 7 9 9
3 1.20 1 0.16 0 2.21 2 1.12 1 4 6 5
Series I
4 0.37 0 0.63 1 1.12 1 0.71 1 3 5 6
5 1.92 2 1.22 1 0.41 0 0.03 0 3 5 5
2 1.47 2 1.7 2 0.18 0 0.20 0 3 6 6
Series 3 1.7 2 1.1 1 1.04 1 0.38 0 4 6 7
II 4 2.06 2 1.36 1 1.97 2 0.38 0 5 7 7
5 2.3 2 0.71 1 2.40 2 0.75 1 6 8 8

The analysis of the data presented in Table 3 shows that there is good compatibility of
the model and the experimental data. The differences between them are of the order of one
LAB. However, for the airfoil of the series I of the blades cast at the withdrawal rate of 2
mm/min, the obtained topograms did not allow us to accurately determine the number of
LABs. In the case of the subgrains marked as SG1, SG2, SG3 and SG4, one can state that the
diffraction images of the dendrites (in the form of strips and spots) clearly formed groups
with the same common crystallographic orientation. The other areas of the topograms were
strongly and irregularly fragmented, therefore localization of subgrains and determination
of the number of LABs was difficult. As a result, we could identify two more LABs (Table 3)
in those areas, which are marked by two double red arrows in Figure 2a. The additional
subgrain marked by the arrow with the envelope could be visualized in the topogram
by using three contrast spots. In Figure 2b, all 5 marked LABs are clearly visible due to
Materials 2021, 14, 8 13 of 16

the lack of contrast bands that cross the entire width of the topogram. In Figure 2c, only
the contrast band visualizing LAB no. 3 may be related to the macro-stress rather than to
the misoriented subgrains; therefore, the number of boundaries counted may be one less
than it otherwise would be. Analysis of the topogram presented in Figure 2d allowed us
to indicate one additional LAB (marked by the red arrow). In the case of the topograms
shown in Figure 2e–g, the determination of the LAB number was quite unambiguous. In
the Figure 2h only the contrast band visualizing LAB no.6 could be questionable, therefore
the counted number of boundaries may be one less than it otherwise would be because the
contrast spot above LAB no.6 may belong to the group of dendrites located below LAB
no.6. This is likely because the misorientation angle of LAB no.6 was close to 0.3◦ .
In the present study, the mechanism of dendrites deflection from the mold walls
was verified regarding the heat-treated turbine rotor blades. The number of macroscopic
LABs created on the cross-section of the blades airfoil near the tip was experimentally
determined and compared to the LABs number calculated from the model based on the
dendrites deflection mechanism.
Based on the Laue patterns and geometrical parameters of the airfoils, the number
of the low-angle boundaries occurring at the upper part of the blades airfoil after heat
treatment could be calculated. The number for the analyzed group of blades ranged from 5
to 9 (Table 3).
Due to the complex shape of the analyzed blades airfoil, which is similar in shape to
the applied rotor blades, the aforementioned geometric assumptions based on the division
into four flat areas were significantly simplified, but it is possible to verify this model. All
the low-angle boundaries, which were formed during crystallization and inherited by the
airfoil, appear near the blade tip. In the proposed model, to calculate the number of LABs
in blades airfoils, it is necessary to experimentally determine the α* and β* angles used in
Equation (1) and the values of the angles δ and ε describing the airfoil geometry. The values
α* and β* can be determined in a non-destructive way by obtaining two Laue patterns
directly from the pressure or suction surface, using, for example, the diffractometric method
called Ω-scan and described in Ref. [39]. Determination of the number of LABs for blades
airfoil allows for a non-destructive quality control process during blades production.

4. Conclusions
The dendrites deflection mechanism effectively describes the process of the low-angle
boundaries creation in the airfoil of heat-treated rotor blades and allowed us to calculate
the LABs number. It also confirms the proposed “deflection” mechanisms of the LABs
creation in other thin-walled parts of single-crystalline casts. The dendrites deflection
mechanism was verified for blades airfoils obtained by using directional crystallization in
the direction [001] of the CMSX-4 superalloy at the withdrawal rates of 2 to 5 mm/min.
The simplification of the geometric assumptions in the model could limit its use. However,
the model can be the basis for more precise calculations. To increase the accuracy of the
model, the complex shape of the blades should be taken into account, for example by
using the finite element method. The proposed model is the basis for a non-destructive
technique for determining the number of LABs in the blades airfoils, based only on two
Laue patterns. Application of the method, without the need for cutting the blades and
preparing metallographic sections, allows it to be used for quality control on the production
lines.

Author Contributions: Conceptualization: W.B. and J.K.; methodology: J.K.; software: J.K.; in-
vestigation: J.K.; data curation: W.B. and J.K.; writing—original draft preparation: W.B. and J.K.;
writing—review and editing: J.K.; visualization: J.K.; supervision: J.S.; project administration: J.S. All
authors have read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Data Availability Statement: Data sharing is not applicable to this article.
Conflicts of Interest: The authors declare no conflict of interest.
 Materials2021,
Materials 2021,14,14,
8x 1414ofof1616

Conflicts of Interest: The authors declare no conflict of interest.

AppendixAA
Appendix
TheX-ray
The X-raydiffraction
diffraction topography
topography is based
is based on on
thethe following
following principles.
principles. First,
First, the the
upperup-
per sample
sample is oriented
is oriented using
using the thediffraction
Laue Laue diffraction pattern obtained
pattern obtained from its
from its surface Q surface
(markedQ
(marked
by by downward
thin black thin black arrows
downward arrows
in Figure 1a).inThe
Figure
sample 1a).isThe sample
mounted is mounted
in the holder soin the
that
holder
the zone so
linethat the zone
defined line
by the defined by
reflections from theplanes
reflections from
(001) and planes
(113) (001) and
is arranged (113) is ar-
horizontally
ranged
with the horizontally
simultaneouswith the simultaneous
vertical arrangement vertical arrangement
of the oscillation axisofTthe oscillation
of the sampleaxis andT
X-ray film (Figure A1). The sample is mounted in the center of the horizontal
of the sample and X-ray film (Figure A1). The sample is mounted in the center of the hor- divergent
incident beam (S1) incident
izontal divergent and inclinedbeamat(S1)
the Bragg angle θat
and inclined 113
31◦ toangle
the=Bragg
CuKα 𝜃 (113).
the plane = 31°The α,
to the
which
planeis(113).
the angle
The α,between
which the sample
is the anglesurface
between andthethe plane surface
sample (113), is and
determined
the plane from theis
(113),
Laue pattern. from
determined During
theexposure, the sample
Laue pattern. Duringisexposure,
oscillated the
about the T is
sample axis the θ113
around about
oscillated the T
CuKα
angle within ± ◦
4 .𝜃The X-ray
axis around the anglefilm is arranged
within ±4°. The parallel
X-ray film to the Q sample
is arranged plane to
parallel and thetoQthe T
sam-
axis.
ple plane and to the T axis.

FigureA1.
Figure A1.Diagram
Diagrampresenting
presenting
thethe geometric
geometric arrangement
arrangement of the
of the X-ray
X-ray source,
source, sample
sample and and X-ray
X-ray film
film for the X-ray topography method with the oscillation. S1—Incident divergent beam, S2—
for the X-ray topography method with the oscillation. S1—Incident divergent beam, S2—diffracted
diffracted beam.
beam.

AppendixBB
Appendix
Thenumber
The numberNNofofdendrite
dendritedeflections
deflectionscan
canbe
becalculated
calculatedfor forthe
thearea
areaETETofofthe
theupper
upper
sample in the way presented below. Let’s calculate the number of dendrite
sample in the way presented below. Let’s calculate the number of dendrite arms deflections arms deflec-
tionsthe
from from
moldthesurface,
mold surface, based
based on the on the schemes
schemes from Figure
from Figure 3c. 3c.
FromFigure
From Figure3c3cand
andthe
theassumption
assumptionthat
thathh==00and
andbb≈≈ l,l, itit follows
follows that
that
L∗
N L=∗ (A1)
N= l (A1)
l
where L* is the height of the area ET.
whereFrom
L* is the
the height of ΔNRT
triangle the area(Figure
ET. 3c) it follows that l = , and from the triangle
From the triangle ∆NRT (Figure 3c) it follows that l = cosmϕ , and from the triangle
ΔNRMititfollows
∆NRM thatmm== D ..
followsthat
sin ϕ
Thecomparison
The comparisonofofthe theabove
aboveequations
equationsgives
gives
D
l = l = sin φ × cos φ
D (A2)
(A2)
sin ϕ × cos ϕ
Materials 2021, 14, 8 15 of 16

L∗
By putting Equation (A2) into Equation (A1), N = D sin ϕ × cos ϕ is obtained, and
the next the Equation (A3) is created

L∗ p
N= sin ϕ 1 − sin2 ϕ (A3)
D
Considering the triangle ∆KRM in Figure 3b it can be determined that tan(α∗ ) = nb
and considering the triangle ∆KLM it can be determined that sin(β∗ ) = D
n.
The comparison of the above equations gives that the tan(α ) × sin(β∗ ) = D
∗
b . From
Figure 3b,c it follows that D
b = tan ϕ, so:

tan(α∗ ) × sin(β∗ ) = tan ϕ (A4)

sin ϕ
Taking into account that tan ϕ = cos ϕ and putting it into the Equation (A4) it follows
that
sin ϕ
tan ϕ = p = tan α∗ × sin β∗ (A5)
2
1 − sin ϕ
Treating the right side of the Equation (A5) as comparable to sin2 ϕ, the equations (A6)
are obtained as follow:

tan2 (α∗ ) × sin2 (β∗ ) tan(α∗ ) × sin(β∗ )

sin2 ϕ = , sin ϕ = (A6)
1 + tan2 (α∗ ) × sin2 (β∗ )
q
1 − tan2 (α∗ ) × sin2 (β∗ )

Putting the sin ϕ and sin2 ϕ from Equation (A6) into Equation (A3), after simple
transformation, Equation (A7) is obtained as follow:

L∗ tan α∗ × sin β∗
N= × (A7)
1 + tan2 α∗ sin2 β∗


D

Due to the low value of α* − tan2 (α*) × sin2 (β*) << 1.

Considering the above, the simplified equation, from Equation (A7), is given:

L∗
N= × tan(α∗ ) × sin(β∗ ) (A8)
D

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