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MSE311-Hardness Fall24 Experiment Sheet

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Department of Materials Science and Engineering

MSE 311-Materials Laboratory I


Hardness
2024-2025

Lecturer:
Assoc. Prof. Fatih TOPTAN

Lab. Assistants:
Res. Asst. Tuğçe ÖZMEN

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MSE311 Materials Laboratory, which is the first department laboratory course of the IZTECH
Materials Science and Engineering Department undergraduate program, aims to provide students with
information about the basic operations in metallurgy and materials engineering. The experiments that
are planned to be shown are laboratory-scale versions of the methods frequently used in the industry.
With this course, the theoretical topics will also be visualized.
We wish success to all students.

Grading System
Quiz 30%
Report 70%

GENERAL RULES OF THE COURSE


1. The starting time of the laboratory is 08:45 on Monday, Faculty of Engineering, A Block, B21.
Students are required to arrive at the laboratory on time.
2. It is of great importance to come to the laboratory prepared by reading the experiment sheet before
the laboratory. Laboratory instructors will conduct a quiz about the experiment.
3. Each student has to experiment with the group specified in the list.
4. Students have to do the make-up experiment during the make-up week, complete all the
experiments and submit all their reports.
5. Reports will be submitted to the Teams homework system. Uploaded after 17.30 the next Monday
will not be accepted.
TURNITIN
Class Number: 46152041
Registration Key: MSE3112024
6. Experiments will be done in groups. However, the preparation of reports should be done
individually. When detecting any duplicate report, it will be automatically graded with zero.
7. It is necessary to get at least 60 points from the quiz to be successful in this lab.

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The objective of the course
 Obtaining theoretical knowledge about different hardness measurement methods.
 Determining the hardness of the materials by using the Vickers hardness measurement method and
obtaining information about their strength based on the resistance they show against the tip dipped
on their surfaces.

Introduction
Hardness testing is defined as the resistance of a material to a harder indenter.
The purpose of this test is to determine the resistance of a material's existing properties such as strength,
hardness and density to permanent deformation such as indentation, abrasion and scratching under
pressure.
Although the hardness test is similar to the tensile test, which measures mechanical resistance to
deformation and separation (plastic flow), it is preferred because it is a relatively non-destructive,
simple, easy and quick to perform test method. It is used to distinguish materials, mostly metals and
alloys, for basic research, analysis, development and improvement of materials and technologies.
Hence, the need to use different hardness tests has arisen because different materials have a wide range
of hardness.
Hardness is an important property that indicates the resistance of a material, but it cannot be defined
as an exact value because it depends on various factors. Hardness testing is done by a specific method
and the results vary according to the method used and the test conditions.
The main factors that influence hardness are the following:
 Test methods
 Test force applied
 Duration of indentation in the material
 Indentation geometry
 Workpiece geometry
When these factors are considered, it becomes clear that hardness tests must be carefully designed and
implemented. In materials engineering, it is important to accurately evaluate hardness values to achieve
desired properties.
1. Theoretical Background
Hardness is usually defined as the resistance of a material to plastic penetration of its surface. There are
three main types of tests used to determine hardness:
• Scratch tests are the simplest form of hardness tests. In this test, various materials are rated on their
ability to scratch one another. Mohs hardness test is of this type. This test is used mainly in mineralogy.
• Static indentation tests are a common method used to determine the hardness of a material. In these
tests, an indentation is created in the material using a penetrator under a given load. The depth or area
of indentation obtained determines the hardness value of the material. Rockwell, Brinell, Knoop and

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Vickers hardness tests are among these static methods, and each is designed to suit different application
areas and material types.
 Dynamic hardness tests determine hardness by measuring the rebound height of objects. In these
tests, a standard mass or object is released, dropped to the surface and observed to bounce back. The
Shore hardness test is one of the most well-known dynamic tests performed by this method. Shore
hardness is highly effective in measuring the stiffness of elastic materials and is used in various
industrial applications.
Both types of tests play an important role in materials engineering and provide the necessary
information to understand the performance of the material. Accurate determination of hardness values
is critical in material selection and application design[1].
For engineering purposes, mostly the static indentation tests are used.

1.1 Scratch Tests


There is an important relationship between hardness and brittleness; generally, hard materials are more
brittle. Hard materials are resistant to external compressive forces and are therefore more at risk of
fracture.
Scratch hardness relates to how easily a sharp edge of one mineral can scratch the surface of another
mineral. This property is measured by the Mohs hardness scale, which was arranged by the Austrian
mineralogist F. Mohs in 1824. The Mohs scale consists of ten basic minerals ranked from 1 to 10, with
each mineral ranked according to its ability to scratch harder minerals.
This scale provides a simple and effective method for comparing the hardness of minerals. Hardness
testing is critical in material selection and engineering applications because the hardness of a material
gives important information about its durability and machinability (Fig. 1).

Figure 1 The Mohs hardness scale and chart for select gems [2].

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1.2 Dynamic Indentation Tests
These methods require special preparation of the sample for hardness measurement.
 Devices that measure hardness by impact,
 Devices that measure hardness according to the amount of splash.
The steel ball-shaped piercing tip leaves a mark on the surface by impact.
The dimensions of the obtained trace are compared with the trace obtained on the gauge and the
hardness value is determined. In the second group, a small weight dropped from a certain height on the
sample bounces back by making more elastic deformation on the sample.
The amount of bounce back after the falling object hits the specimen is proportional to the amount of
elastic energy and this is the principle of the method.
Moving hands are used on the indicator to easily measure the amount of bounce.
The most well-known of the devices working with the bounce principle is the “Shore Scleroscope” [3].
The most important advantage of this type of instrument is that it measures hardness without leaving
any trace and provides the ease of measuring hardness distribution on a very large surface.
1.3 In Static Hardness Tests

As stated in the definition, hardness measurement generally consists of measuring the resistance of the
material against the effect of a conical or spherical standard tip.

Hardness measurement tests performed by immersing a hard object into the material, free fall and
release are given below. There are mathematical relationships between these measurements and it is
possible to switch from one value to another. When making hardness measurements, regardless of the
method, several measurements should be made on the sample and their average should be taken.
a) Brinell hardness measurement method,
b) Vickers hardness measurement method,
c) Rockwell hardness measurement method,
d) Micro-hardness test.

1.3.1 Brinell Hardness Measurement Method


It consists of measuring the trace diameter that occurs as a result of applying a certain load to the surface
for a certain period of time with the help of a ball made of a hard material of a certain diameter.
Brinell hardness value (BHN): It is a value related to the size of the permanent mark created by pressing
the surface of a material for a certain time with a ball of a certain diameter. The Brinell hardness value
is determined by dividing the load applied on the ball by the spherical surface area obtained on the
sample surface (Fig. 2).

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Figure 2 Brinell hardness measurement method [4]

In standard tests, it is generally performed under the conditions of a steel ball with a diameter of 10 mm,
a load of 300 kg and a waiting time of 30 seconds. For other test conditions, information is added next
to the BHN mark in order of ball diameter/load/time. E.g.; An illustration as 60BHN 5/500/30 describes
the test applying a 500 kg load on a 5 mm diameter ball for 30 seconds. However, in practice, smaller
load-ball diameter combinations are used because these loads are too large and cause large crushing on
the surface. The most important disadvantage of this test is that the load-diameter combinations must
be chosen specifically for the material. For example, if the hardness of a steel material is to be measured,
if a 2.5 mm diameter ball is used in the experiment, the required force is 187.5 kg. However, if the
hardness of an Al alloy is to be measured, then a force of 31.25 kg is sufficient[3,6].
Balls used as penetrating tip are made of hardened steel. Considering that the ball may be crushed during
the test, hardness should be measured up to a maximum of 400 BHN with steel balls. It is possible to
experiment using a hard metal (sintered tungsten carbide) ball up to 550 BHN. It is not appropriate to
conduct the Brinell test on metals with higher hardness. In this case, the ball is crushed, increasing its
diameter and causing incorrect measurements in the deformation geometry.

1.3.2 Vickers Hardness Measurement Method


In this method, a pyramid-shaped tip with a square base is immersed under a certain load on the piece
of material whose hardness is to be measured, and the diagonal lengths of the trace that occur after the
load is removed are measured.
The resulting trace base is a square pyramid with diagonal d, and the apex angle is the same as the apex
angle 136° of the penetrating tip. Vickers hardness value is the test load expressed in kg divided by the
trace area expressed in mm2 (Fig. 3) and it is calculated using the following Vickers hardness formula as
shown in Eq 1.

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Figure 3 Schematic principles of operation of Vickers hardness machine [5].

(Eq 1)

Vickers hardness test is defined in ASTM E-92-72, DIN 50133 and TS 207 standards and Vickers hardness
value is symbolized by HV. The Vickers hardness value is shown by adding the numerical values next to
the symbol showing the applied load and the second numerical values showing the application time of
the load. For example, 455 HV/30/20 means 455 Vickers hardness value measured under 30 kg load
applied for 20 seconds[1,6].
Vickers hardness test is used in a wide range of materials from soft materials (5 HV hardness) to hard
materials (1500 HV hardness).
Although Vickers hardness test is one of the methods that give very accurate hardness values, it is not
used as widely as Brinell or Rockwell hardness values. The diamond pyramid tip provides better accuracy
than the value obtained by the Vickers hardness test, Brinell or Rockwell hardness tests, since it has a
wide angle and the diagonals of the trace formed are approximately seven times larger than the depth
of the trace, especially in high hardness metals. This is also based on the fact that the Vickers trail is
smaller than the Brinell trail.
In the measurement of the hardness of very hard materials, distortion of the Brinell ball occurs, while in
the measurement of the hardness of normal materials, some elastic distortion of the ball occurs.
However, in experiments with the Vickers pyramid, the immersing tip is damaged at very low degrees.

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1.3.3 Rockwell Hardness Measurement Method
The Rockwell hardness test (HR) is the most widely used method for measuring the hardness of metals,
as it is very easy to perform and does not require special skill. Rockwell hardness is a unitless number
corresponding to the depth of submersion. The stinging tip is conical or ball-shaped (Fig. 4). Soft
materials are measured with a ball penetrating tip. Very hard materials are measured with a diamond
conical tip.

Figure 4 Rockwell hardness indenter types [7].

In Rockwell hardness measurement, the penetrating tip is inserted into the material with a preload of
10 kg (100 N). Then, the depth obtained by applying the main load to the penetrating tip is measured.
The main load is 100 kg for Rockwell B (HR-B) and 150 kg for Rockwell C (HR-C).
Since the penetration depth will be measured in this method, surface roughness may affect the results.
In order to eliminate this drawback, the tool is adjusted to zero level by immersing the penetrating tip
into the material with a small load (P0=preload). The main load (P1) is then applied to complement the
total load. Finally, the main load (P1) is removed (Fig. 5). The Rockwell hardness value is read from the
current indicator by finding the depth increase in the permanent scar[8].

Figure 5 Schematic representation of the Rockwell hardness measurement [9].

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The Rockwell hardness value is dimensionless. Each 0.002 mm penetration into the long material is taken
as a decrease of 1 number of hardness value. The Rockwell Hardness Value-C (HR-C) can be calculated
with the above formula as the depth of penetration t b between the position of the tip after the preload
is applied and the position of the tip after the main load is removed.
The type of the penetrating tip used in the hardness measurement and the value of the applied load are
shown with a symbol. For this reason, different hardness values measured according to different scales,
that is, under different test conditions, are given with symbols such as HR-A, HR-B, HR-C, HR-D. The
Rockwell hardness of very hard materials is measured under a 150 kg load using a cone-shaped diamond
tip and the results are indicated by the symbol HR-C. In the measurement of the hardness of soft
materials, a steel ball is used as the penetrating tip and the measurement results obtained under a load
of 100 kg are shown with the HR-B symbol. If the hardness value of a material, measured in Rockwell,
exceeds 100, it is not recommended to use a ball as a penetrating tip. Because the use of ball as a
penetrating tip in measuring the hardness of very hard materials causes both the ball to be deformed
and the measurement accuracy to decrease. On the other hand, it is not recommended to use a cone-
shaped diamond tip in measuring the hardness of materials with a Rockwell hardness lower than 20
according to any scale [10].

1.3.4 Micro-hardness test


This test is particularly suitable for measuring the hardness of very small samples and thin sheets. The
hardness of hardened and coated surfaces can also be determined by this method. In addition, the
hardness of various phases and regions in the internal structure of the material are measured by this
method. In this method, the immersion depth usually does not exceed 1 micron.
Micro hardness measuring device is a sensitive device and its control is done automatically. The
difference from macro hardness measuring devices is that the system includes a complete metal
microscope.
The sample whose hardness is to be measured is placed on the microscope table and the table is moved
until a clear image is obtained from the eyepiece. Then, the region to be measured hardness is selected
and the loading is done automatically by pressing the button. Thus, a trace is obtained on the sample.
Leave sizes are usually determined by a manual system.
Two standard inserts are used in microhardness tests. One of them is the pyramid tip (Vickers tip) with
a square base and a 136° apex angle. The other is the 172°30' pyramid tip, known as the Knoop tip. The
Vickers tip leaves a square mark on the sample, while the Knoop tip leaves a rhombic mark.
Load values between 1-10.000 g are generally used in micro-hardness devices.
There are also ultra-hardness testers that use a load of less than 1 g. On the other hand, trace depths in
nm can be obtained by using μN loads with devices known as nano-hardness measuring devices, which
have been developed in recent years.
The surface of the sample to be measured for microhardness must be metallographically prepared. It is
desirable that the surface be clean, polished and generally etched[7,9,11].

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2. Experimental Procedure
The Vickers hardness test can be applied to any type of material, from wide bars to sheets. In general,
the upper and lower surfaces of the sample whose hardness is to be measured should be flat so that the
sample does not move or slide when loaded. In terms of thickness, it is sufficient that the pyramid
penetrating tip is thick enough not to cause any protrusion on the back surface of the sample. In order
for the ends of the diagonals to be fully seen, the surface of the trace must be polished.
The sample whose hardness is to be measured is placed in the sample holder area and raised until it
approaches the tip of the immersing tip. The load is gradually applied to the insertion tip and then the
load is removed. In order to find the Vickers hardness value after the test, it is necessary to measure the
diagonals of the square-shaped trace with the help of the metallurgical microscope attached to the
Vickers test device; The image of the trace created on the sample is transferred to the measuring screen
with the help of a microscope. With the help of two movable rulers on the measurement screen, the
lengths of the diagonals are measured with an accuracy of 0.001 mm and the average is taken.

3. Required
Do not forget to write down the units when filling out the table!
The measurements should be repeated at least 10 times and the mean values should be written with the
calculated standard deviation value.
Sample 1 Sample 2 Sample 3
Vickers Hardness Test

d1 (mm)
d2 (mm)
d=(d1+d2)/2
P (kg)
HV

4. Assignments (Answer of this assignments are expected in your report.)


Q1 - Which factors affect the selecting of the appropriate hardness test?
Q2 - Discuss the advantages and disadvantages of the Brinell, Vickers and Rockwell Hardness Tests.
Q3 - Discuss the relationship between hardness and tensile properties.

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5. References
[1] Chandler, H; Hardness Testing, Second Edition, ASM International, United States of America, 1999.
[2]https://www.gemsociety.org/article/select-gems-ordered-mohs-hardness/(accessed by 20/10/2024)
[3] Purcek, G.; Mechanical Tests Applied to Mechanical Materials (Lecture Notes), 2014
[4] https://www.uludag.edu.tr/dosyalar/otomuh/Laboratuvarlar (accessed by 25/10/2024)
[5] Han, By., Chu, Jj., Du, Wb. et al. Optimization of Ni60A Coating Quality by Supersonic Plasma
Spraying Based on Response Surface Methodology. J Therm Spray Tech 32, 1596–1610 (2023).
https://doi.org/10.1007/s11666-023-01580-8
[6] Oran, K. and Erman, B.; Structural properties of materials, volume II, İ.T.Ü. Faculty of Civil
Engineering, Istanbul, 1993
[7] https://www.tr.noblemetallography.com/aksesuar-ve-sarf-malzemeleri (accessed by 25/10/2024)
[8] Kayali, E.S.; Ensari, C. and Dikec, F.; Mechanical tests of metallic materials, İ.T.Ü. Chemistry Metallurgy
Fa. Offset Workshop, Istanbul, 1990.
[9]https://depo.btu.edu.tr/dosyalar/makine/Dosyalar/BTU_Makine_Laboratuvar%C4%B1_Sertlik_Den
ey_Foyu.pdf (accessed by 25/10/2024)
[10]Gulec, S. and Aran, A.; Material information, Volume 1, TUBITAK Marmara Scientific and Industrial
Research Institute, Gebze, 1988.
[11] Dieter, G.E.; Mechanical Metallurgy, 2nd Edition, Mc Graw Hill Book Comp. Inc., London, 1976.

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