Case Study about the Effect of Measurement

Parameters Values on the Microhardness Results

Adrian Catalin Pavalache
Materials and Welding Technology
University Politehnica of Bucharest
Bucharest, Romania
Adrian.pavalache@gmail.com
Ion Mihai Vasile
Materials and Welding Technology
University Politehnica of Bucharest
Bucharest, Romania
vasileionmihai@yahoo.com
Elena-Manuela Stanciu
Materials and Welding Technology
University Politehnica of Bucharest
Bucharest, Romania
Elena.manuela.stanciu@gmail.com
Ionelia Voiculescu
Materials and Welding Technology
University Politehnica of Bucharest
Bucharest, Romania
ioneliav@yahoo.co.uk


AbstractThe paper aims to analyze the effect of the specific
parameters values and the surface preparation on the
microhardness measurement accuracy. The various force and
different time of penetration values has been applied in order to
establish the measurement uncertainly in the case of a Bainitic
steel sample. Also, the effect of the surface roughness and the
scratching test behavior has been analyzed in order to study the
superficial material characteristics.
Keywords-microhardness; bainitic steel; roughness
I. INTRODUCTION
The microhardness test is used to determine the hardness
over very small areas or for ascertaining the hardness of a
delicate machine part. The test is accomplished by forcing a
diamond indenter of specific geometry under a test load of 1
1000 gf (0.00989.8 N) into the surface of the test material
and to measure the diagonal or diagonals of indentation
optically (ASTM E384-84) [1].
The Vickers hardness number for microhardness is
established using the same indenter defined for hardness, with
loads varying from 1 to 1000 gf. Similarly, it can be expressed
as

HV = 1854.4P1/d2 (1)

Where P1 is the load (gf) and d1 is the mean diagonal of the
indentation (m).
The preparation of the specimen surface shall be carried out
in such a way that any alteration of the surface hardness, due to
hear or cold-working, for example, is minimized. Due o the
small depth of Vickers micro hardness indentations, it is
essential that special precautions are taken during preparation.
II. EXPERIMENTAL PROCEDURE
A. Materials
The specimen used for this study has made on Bainitic
material, which is the new pre-hardened steel, suitable for the
manufacture of medium and big size injection mould. The
chemical composition provided by the Lucchini
Sidermeccanica producer is: C = 0.2-0.3 %, Si=0.1-0.4%,
Mn=1.3-1.6%, Cr=1.3-1.5%, Mo=0.4-0.7%, Ni=0.9-1.2%,
P=max. 0.035%, S=max.0.035%.
The steel is supplied in the pre-hardened condition, but the
specimen was heat treated as follows: stress relieving,
hardening, tempering and final stress relieving. After this heat
treatment procedure, the entire structure of the specimen is
Bainitic (fig.1).

Fig.1. Bainitic structure of the sample.
The mechanical properties provided by the producer are
showed in the table 1.


AMUEM 2009 International Workshop on Advanced Methods for Uncertainty Estimation in Measurement
Bucharest, Romania, 6-7 July 2009
978-1-4244-3593-7/09/$25.00 2009 IEEE 54
TABLE I. MECHANICAL PROPERTIES OF THE SPECIMEN
Steel
Mechanical Properties
R, N/mm
2 Rp0.2,
N/mm
2

HB Z, % A, %
KeyLos 1080 980 360 53 17
B. Surface preparation
The preparation involves the cleaning of the specimen
surface in order to remove any extraneous or undesirable
material or deposit at any stage of manufacture, storage or
service. For the first experiments, the specimen has been cut-
out from a bloc of steel, and then has been grinded and
polished using successive type of silicon carbide grinding
paper (Grit. No.: 400, 600, 1000). For the second set of
experiments, the specimen has been polished using both silicon
carbide grinding paper (Grit. No: 1200, 2500). Then the surface
has been polished using other abrasive like diamond paste with
particle size of 0.1m and cerium oxide with particle size of
0.05m. The specimen dimensions are: 70mm length, 35 mm
width and 6.5mm thickness. The roughness of the surface has
been measured in the both state of preparation using a Pocket
Surf III device that prior to the measurements was calibrated
using special calibrating blocks that have a controlled surface
roughness. The specimen had an average (5 points of
measurement) surface roughness of R
a
=0.27 m, for the first
set of experiments, and R
a
=0.06 m for the second set of
experiments.
III. MEASUREMENTS
All the microhardness measurement has been carried out
using a Shimadzu HMV 2T apparatus. The measurement
procedure consisted in two different set of experiments. The
first set has been carried out on the rough polished surface and
the second on the fine polished surface. For each set of
experiments, both the force and the time of penetration have
been varied, the results being acquired by two different
operators with different visual acuity. One of them has visual
correction of +1.5 (Operator 1) and the other has normal visual
acuity (Operator 2). All the order condition of measuring has
been kept constant (environment temperature of 24 0.5
degrees and 48% 2 humidity). In order to establish the
accuracy of the indentation measurement, the specimens have
been analyzed using a SEM Quanta Inspect S electronic
microscope, and the diagonal length has been measured for
different magnification (500x, 1000x) (fig. 2).

Fig.2. The indentation measurement using a SEM microscope.
A. Microhardness results
The microhardness results for the first set of experiments
have been represented as a chart using the mean value as the
representative value and are showed in fig. 3 and fig. 4, while
for the second set of experiments, in fig. 5 and fig.6.
The Evolution of The Mean Value
370
380
390
400
410
420
430
440
5 10 15 20 50
Testing Time [s]
M
i
c
r
o
h
a
r
d
n
e
s
s
HMV0,2
HMV0,3
HMV0,5
HMV1

Fig.3. The average value of microhardness measured by
Operator 1, Set I.
The Evolution of The Mean Value
360
370
380
390
400
410
420
430
5 10 15 20 50
Testing Time [s]
M
i
c
r
o
h
a
r
d
n
e
s
s
HMV0,2
HMV0,3
HMV0,5
HMV1

Fig.4. The average value of microhardness measured by
Operator 2, Set I.

Fig.5. The average value of microhardness measured by
Operator 1, Set II.

Fig.6. The average value of microhardness measured by
Operator 2, Set II.
All the measurements have been carried out using the
distance between the centers of two adjacent indentations of
0,50mm and the distance from the edge of the specimen of 1
mm. The difference between the measured values for the two
55
operators is a consequence of the lack of visual acuity. For the
both set of measurements, the length of indentation depends on
the time of penetration and applied force value. For higher
values penetration time and the higher value of the applied
force, the length of indentation is higher, because the percent of
plastic deformation is higher.
IV. RESULTS
Operators, the time of penetration for each successive
measurement, applied force, surface quality, calibration
procedure and equipments are some factors that contribute to
the variability in the test results.
IV.1. Operators influence. In the paper, we try to
emphasize the influence of the operator visual acuity keeping
the rest of the influence factors constant. For each set of
experiments, we have been calculated the uncertainly values of
the measurements using the SR EN 6507 -1:2005 and SR EN
6507-2:2005 [3, 4]. The values of the uncertainly of the
measurement has been into the range of 2.013 - 2.656.
For the Operator 1 the chart shows that the lowest values of
the standard deviation have been obtained for the HMV0.5 and
HMV1 for all the testing time (fig. 7). The lowest values of the
standard deviation were obtained for larger applied forces and
implicitly for larger indentations, as a result of the lack of
visual acuity of the operator in case of small objects. Also, it is
found that the variation interval for each applied force value is
narrower for higher forces and placed towards smaller values
of the standard deviation (HMV1 and HMV0.5). The spreading
bandwidth of the results for the entire batch of measurements is
relatively high (about 15 units), although for each value of the
force, the deviations values were placed in relatively equals
with those of Operator 2 (about 7 units) (fig.8). For the
Operator 2, the standard deviation reached a narrow data range
especially for the HMV0.5 and time of penetration equal to 15
and 20 seconds (fig. 10). Also it is found that the results
spreading bandwidth is narrower (almost half of the one of
Operator 1), although the individual deviations values are
sometimes higher than those determined by Operator 1, in the
same measurement conditions (fig. 9).
IV.2. Surface quality influence. In comparison to the first
set of experiments, the second set revealed that the evolution of
the standard deviation has a lesser values if the roughness was
lower (Ra 0.06 m comparatively with Ra 0.27 m).
The Evolution of The Standard Deviation
0
5
10
15
20
25
5 10 15 20 50
Testing Time [s]
S
t
a
n
d
a
r
d

D
e
v
i
a
t
i
o
n

[
%
]
HMV0,2 Test
HMV0,3 Test
HMV0,5 Test
HMV1 Test

Fig.7. The evolution of the Standard Deviation for Operator 1,
Set I.
One of explanation can be the fact that if the surface
roughness decreases, the contour of the indentation can be
better visualized.
The Evolution of The Standard Deviation
0
2
4
6
8
10
12
14
16
18
5 10 15 20 50
Testing Time [s]
S
t
a
n
d
a
r
d

D
e
v
i
a
t
i
o
n

[
%
]
HMV0,2 Test
HMV0,3 Test
HMV0,5 Test
HMV1 Test

Fig.8. The evolution of the Standard Deviation for Operator 2,
Set I.

Fig.9. The results spreading bandwidth for Operator 1, Set I.

Fig.10. The results spreading bandwidth for Operator 2, Set I.
The second set of experiments revealed the fact that the in
better roughness conditions, the measurement results have a
lesser coefficient of variation and the mean values obtained by
the two operators are closer to each other (fig. 11 and fig. 12).
That means that the operator visual acuity does not influence
the experiment significantly.
Surprisingly, the highest values of standard deviations were
obtained by Operator 1 for HMV0.5, even above those
determined in terms of a higher roughness of the surface. For
the other values of HMV there is a remarkable nearness of the
results and a shrinking of the results spreading bandwidth
(about 7 units in Operators 1 case for all other measurements,
regardless of measuring time and of the force applied, fig. 13).
56

Fig.11. The evolution of the Standard Deviation for Operator 1,
Set II.

Fig.12. The evolution of the Standard Deviation for Operator 2,
Set II.

Fig.13. The results spreading bandwidth for operator 1 on the
second set of experiments

Fig.14. The results spreading bandwidth for operator 2 on the
second set of experiments
Conversely, in Operators 2 case the standard deviation
achieved for small values of applied force and reduced time of
operation has recorded higher values compared with the first
set and the results spreading bandwidth was extended for
HMV0.2 and HMV0.3 (from 7 units in the first set to 18 units
in the second set, fig. 14).
IV.3. Applied force influence. For both set of experiments and
operators, if the accuracy of the length indentation is higher,
the microhardness value seems to reach the true value. So, if
the magnitude of the microscope objective is higher, the
possibility of length estimation is better (fig. 2). That means
that if the magnification capability of the microhardness tester
would have been higher, the precision of the length the
indentation measurement can increase.
IV.4. Processing time influence. The amount of operating time
seems to be important in terms of shrinking the results
spreading bandwidth, indifferent to the value of applied force
(fig. 12). This observation can be explained by the fact that the
penetration time causes the appearance of residual strains,
leading to the obtaining of a more visible edge of the
indentation, and implicitly of a higher degree of accuracy of the
measurement.
CONCLUSIONS
The paper highlights the effect that certain parameters
regarding the operators and testing conditions may have on the
uncertainty of HMV microhardness testing, expressed through
the evolution of the standard deviation determined
automatically by the measurement device. Thus there were
noticed some original regarding the way in which two
different operators can achieve different performances. For
one of the operators increasing the degree of surface finishing
had a remarkable influence, which led to the halving of the
results spreading bandwidth. For the other operator, this aspect
had led to only a small difference between the results
measured with different force values, without positively
influencing the results spreading bandwidth. Therefore, in the
calculations of the measurement uncertainty expression in the
HMV microhardness determination there should be introduced
corrections regarding the operators characteristics,
penetration force values and penetration time.
ACKNOWLEDGMENT
The research work was financially supported by the
CEEX Romanian Program in the framework of the Project No.
71.039/2007 Innovative technologies for the modular
elements designed for the heat molding process ELMOD.
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[3] Metallic materials - Vickers hardness test - Part 1: Test method (ISO
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[4] Metallic materials - Vickers hardness test - Part 2: Verification and
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