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ME 328-01

Lab Project 3: Microstructure & Hardness of Bolts

Due: 2/9/17

Team 103

Colleen Burrows
Jessica Byun
Charisse Haines
Arisa Kouchi
Introduction:
Four bolts were identified through this experiment: a grade 2 off the shelf, a grade 5 off the shelf,
a grade 5 annealed, and a grade 5 spheroidized. Grade 2 bolts are commonly used for standard
applications, while grade 5 bolts are stronger and found often in automotive applications [1].
The purpose of annealing is to induce softness and to produce a definite microstructure, while the
purpose of spheroidizing is to improve ductility and toughness and makes alpha particle of
cementite [2].

This project is taken from a materials engineering perspective to analyze how different
compositions and heat treatments affect the hardness and microstructure of a bolt to see how they
influence the practical applications of bolts.

Methods:
Each bolt was cut in half using an Abrasimet 250 Cutoff Saw and then mounted using either a
Buehler XPS1 or Allied Mounting Press. The surface of the mounted bolt was then grinded using
either a Buehler or Allied Powerhead Dual Grinding Wheel with a 60m, 25m, and 9m grit
grinding discs. The surface was then polished using either a Stuers or Allied Powerhead Dual
Polishing Wheel using diamond and alumina particle polishing pads, and then etched using the
2% nitric acid nital etchant. Images of the bolt surface were then taken using a Zeiss Microscope
at 10x, 20x, 50x, and 100x magnifications. Lastly, the half of the bolt not used for the etching
was hardness tested using a Wilson Rockwell Series Hardness tester.
Results:
Each bolt was examined under a microscope to see the phases present:

The 2O steel bolt is comprised of spheroidite and coarse pearlite with primary ferrite and
cementite particulates (Figure 1).

Figure 1.a: 2O Steel bolt under 10x magnification (Byun).


Figure 1.b: 2O Steel bolt under 20x magnification (Byun).

Figure 1.c: 2O Steel bolt under 50x magnification (Byun).


Figure 1.d: 2O Steel bolt under 100x magnification (Byun).

The 5O steel is comprised of tempered martensite (Figure 2).

Figure 2.a : 5O Steel under 10x magnification (Burrows)


Figure 2.b : 5O Steel under 20x magnification (Burrows).

Figure 2.c : 5O Steel under 50x magnification (Burrows).


Figure 2.d : 5O Steel under 100x magnification (Burrows).

The 5A steel is comprised of coarse pearlite with and primary ferrite and cementite (Figure 3).

Figure 3.a : 5A Steel under 10x magnification (Haines).


Figure 3.b: 5A Steel under 20x magnification (Haines).

Figure 3.c: 5A Steel under 50x magnification (Haines).


Figure 3.d: 5A Steel under 100x magnification (Haines).

The 5S steel is comprised of spheroidite with primary alpha ferrite and cementite (Figure 4).

Figure 4.a: 5S Steel under 10x magnification (Kouchi).


Figure 4.b: 5S Steel under 20x magnification (Kouchi).

Figure 4.c: 5S Steel under 50x magnification (Kouchi).


Figure 4.d: 5S Steel under 100x magnification (Kouchi).

Each bolt was also hardness tested (Table 1).

Hardness Test

Bolt 1 2 3 4 5 Scale Average Standard Deviation

2O 78.8 80.1 81.3 85.6 81.7 HRB 81.5 2.56

5O 28.6 28.7 34.2 32.9 33.8 HRC 31.6 2.77

5A 75.3 78.6 82.7 79.9 83.7 HRB 80.0 3.36

5S 86.4 87.2 84.0 83.6 85.4 HRB 85.3 1.53

Table 1: Rockwell hardness values for the bolts in HRB and HRC scale. The 5A is the softest bolt and
5O is the hardest bolt.

The hardness values for the given bolts all fall between 80 HRB and 32 HRC with standard
deviations between 1.5 and 3.5. The 2O bolt is softer than the 5O bolt because of its lower
carbon content. The heat treatments lowered the hardness of the steel.
Discussion:
The 2O steel bolt is in the off-the-shelf condition. The images in figure 1 show a spheroidite and
coarse pearlite microstructure with primary alpha ferrite and cementite particulates. The sparse
amounts of particulates in the images suggests a softer and more ductile material. Grade 2 steel
bolts are made of low to medium carbon steel with a 0.29 wt% Carbon content, yielding a lower
hardness value [4]. The published HRB Rockwell Hardness for a 0.29 wt% C between
spheroidite and coarse pearlite ranges between 70 and 80 HRB [3]. The average Rockwell
Hardness of the 2O bolt was 81.50 HRB. Similar to the 2O bolt, the 5O bolt is in the
off-the-shelf condition. The images of the 5O bolt in figure 2 show a crystal structure similar to
tempered martensite. In figure 2.c., particles of cementite and ferrite are present. They are
indicative of tempered martensite. The HRC Rockwell Hardness test resulted in an average
hardness of 31.6. The hardness found from the HRC test is within reason of the expected values
for tempered martensite tempered at 371o C.

The 5A bolt was heat treated at 900o C for two hours and furnace cooled. This got the
microstructure to austenite, and then the gradual cooling formed a coarse pearlite with primary
ferrite (Figure 3). The HRB Rockwell Hardness for a 0.4 wt% C composition at coarse pearlite is
about 85 [3]. The 5A bolt is a bit softer than expected. This could be because it was annealed for
such a short time that the heat was unevenly distributed throughout the bolt causing uncertainty
and variability in the hardness through the volume of the bolt. The 5S bolt was heat treated at
700o C for about 24 hours and cooled in the furnace, which is the heat treatment outlined for
spheroidite. In this process, the bolt started as either pearlite or tempered martensite and heated
to spheroidite, which is consistent with the magnified photos in figure 4. The published HRB
Rockwell Hardness for a 0.4 wt% C composition at spheroidite is about 75 HRB [3]. The results
of this projects hardness testing came out with an average of 85.32 HRB, which is in the same
range [3].

Processing is related to the microstructure of bolts because microstructures change with different
heat treatments. All of the bolts in this project consist of the same phases because they are all at
room temperature which for steel is only ferrite and cementite, but their microstructures all differ
according to their heat treatments. Initially in their off-the-shelf conditions, the grade 2 and
grade 5 bolts had high strengths for fastening steel and automotive parts [1]. The two heat
treated bolts are less adequate than a off the shelf Grade 5 bolt for this same use because
annealing/spheroidizing decreases their strengths. The lower strength of these bolts is detrimental
for this bolt application as it would result in failures at a lower load. However, the heat treated
bolts also increased in ductility making them beneficial for certain applications. They are
comparable to a Grade 2 bolt in strength.
Conclusion:
Annealing metal lowers the strength of the material and changes the microstructure.
With applications requiring higher strengths, annealing and spheroidizing the materials would
not be recommended because these methods lower the strength. However, in applications in
which avoiding brittle failure in bolts overshadows the need for high strength, spheroidizing the
materials would be recommended because it increases the ductility. An important discovery
made from the data is that the grade 2 off-the-shelf bolt has similar properties including
microstructure and hardness with that of the grade 5 spheroidized bolt. A possible reason why a
2O bolt is preferred in manufacturing over the 5S bolt is that the 5S bolt would require an extra
step of heat treating.
Appendix A:
Arisa Kouchi aimed for a hardness of 40-45 HRC, which is supposed to have a martensite
microstructure. To get this hardness level, the bolt was heated to austenite by baking in the oven
for 90 minutes at 825oC, quenching, and then 90 minutes at 900oC and quenching it again. Then,
to bring it to martensite, the bolt was heated it at 450oC for 80 minutes (Figure 5). The resulting
image of the bolt had cross-hatches, indicating a microstructure of martensite, as predicted
(Figure 6). The average hardness of the heat treated bolt was measured to be 37.48 HRC, which
was close to the target hardness and consistent with the hard properties of martensite (Table 2).

Figure 5: The Rockwell Hardness HRC and Tempering Time for 0.4 wt% Carbon 1040 Steel. For a
target hardness level of 40-45 HRC, the metal can be baked for 80 minutes tempered at 450 [5].
Figure 6.a: Heat Treated 1040 steel at 10x magnification

Figure 6.b: Heat Treated 1040 Steel at 20x magnification


Figure 6.c: Heat Treated 1040 Steel at 50x magnification

Figure 6.d: Heat Treated 1040 Steel at 100x magnification


Hardness Test

1 2 3 4 5 Scale Average Standard


Deviation

Heat Treated 37.4 37.2 37.6 36.9 38.3 HRC 37.5 0.526
1040 Bolt

Table 2. Hardness values for heat treated, grade 5, 1040 Steel bolt.
Appendix B:

Figure 7: Graph of Rockwell hardness HRC scale vs. Tempering time for different set temperatures for
1040 steel. Linear trend of lines can be extrapolated for the needed range of 20-25 HRC to find tempering
time and temperature of 650o C for two hours and 25 minutes [5].

Charisse Haines aimed for hardness of 20-25 HRC. For a 1040 steel bolt, this hardness is
between fine pearlite and tempered martensite making it bainite [3] . The heat treatment chosen
was to heat to bolt to 825o C for an hour and a half to get the microstructure to fully austenite
and then quench it to martensite, and then heat the bolt back up to 650o C for two hours and 25
minutes to make it a soft tempered martensite according to a hardness v. tempering time graph
for 1040 steel [5] (Figure 7).

After heating the bolt to 825o C for the hour and a half, a hardness test revealed it was still too
soft to be in full martensite phase. The bolt was placed in a 900o C oven for another hour and a
half to ensure the bolt was fully austenite before quenching. The bolt was then in the martensite
phase. It was reheated to 650o C for two hours and 25 minutes and then quenched to make it a
tempered martensite.

The hardness test revealed it was just under the hardness value it was aimed to be at 97.7 HRB (a
value too low to be valid on the HRC scale). In order to correct this, the bolt should have been
taken out of the oven sooner so that it would be a harder tempered martensite. The
microstructure shows a fine pearlite structure with primary alpha and cementite (Figure 6).
Figure 8.a: Heat treated 1040 Steel under 10x magnification.

Figure 8.b: Heat treated 1040 Steel under 20x magnification.


Figure 8.c: Heat treated 1040 steel under 50x magnification.

Figure 8.d: Heat treated 1040 steel under 100x magnification.


Hardness Test

1 2 3 4 5 Scale Average Standard


Deviation

Heat 98 97.7 96.7 97.2 99.1 HRB 97.7 0.907


Treated
1040 Bolt

Table 3: Rockwell hardness values for heat treated 1040 steel with average hardness from five
consequent tests on the same machine.
Appendix C:

Figure 9: The linear relationship between the hardness values on the HRC scale and the tempering time at
different temperatures for 1040 steel (0.4 wt% C). The hardness values ( 90-95 HRB) were converted into
the HRC scale (11-18 HRC) and used to extrapolate the data for the corresponding points [6]. While these
hardness values are not within the HRC range, they were used for the linear relationship [5].

Jessica Byun designed a heat treatment for a grade 5 (1040 steel) bolt aiming for a hardness
value between 90-95 HRB. The microstructure at this hardness range is between fine pearlite and
tempered martensite [3]. For this heat treatment, the bolt was placed in the oven for two hours at
900oC to get the microstructure to austenite. The bolt was then quenched at room temperature,
yielding a martensite microstructure. The hardness value was approximately 42 HRC after
quenching, which corresponds to a martensite microstructure [3]. The bolt was then placed in the
oven for an additional three hours at 650oC to reach a fine pearlite/tempered martensite
microstructure based on the values from the extrapolation (Figure 9).
The average hardness value for the bolt after the heat treatment was 95.2 HRB with a
standard deviation of 2.90, which is slightly off range. Ultimately, the microstructure of the heat
treated bolt has both indications of tempered martensite and fine pearlite, and most resembles a
bainite microstructure because of the unstructured hash marks (Figure 10). In order to get the
bolt closer within the overall range, the specimen should be heated at 650oC at a longer time.
The grade 5 steel bolt after heat treatment is comprised of bainite microstructure (Figure 10).

Figure 10.a: 1040 steel bolt at 10x magnification after heat treating.

Figure 10.b: 1040 steel bolt at 20x magnification after heat treating.
Figure 10.c: 1040 steel bolt at 50x magnification after heat treating.

Figure 10.d:1040 steel bolt at 100x magnification after heat treating.


Hardness Test (HRB)

1 2 3 4 5 Average Standard Deviation

Heat Treated 96.1 97.7 95.3 96.5 90.2 95.2 2.90


1040 Bolt
Table 4: Rockwell hardness HRB values for the heat treated, grade 5 bolt.
References:

[1] About Fastener Materials, Bolt Depot.


https://www.boltdepot.com/fastener-information/materials-and-grades/materials.aspx
[2] Annealing/Protective Atmosphere Normalizing/Spheroidize, Metlab.
http://www.metlabheattreat.com/annealing-protective-atmosphere-normalizing-spheroidi
ze-annealing.html
[3] W. D. Callister Jr., D. G. Rethwisch, Materials Science and Engineering: An Introduction,
ninth ed., John Wiley & sons, Inc. 2013, pp. 386, 388.
[4] Carbon Steel Bolts in ASTM A301 (Grades A and B), Glaser & Associates, Inc.
https://www.glaserbolt.com/materials-carbon-steel-bolts-in-astm-a307
[5] A. Verma, P. K. Singh, Influence of Heat Treatment on Mechanical Properties of Aisi1040
Steel, IOSR Journal of Mechanical and Civil Engineering, Volume 10, Issue 2 (Nov-Dec
2013), 32-38
http://www.iosrjournals.org/iosr-jmce/papers/vol10-issue2/F01023238.pdf?id=7622
[6] Steel Hardness Conversion Table, Steel Express.
http://www.steelexpress.co.uk/steel-hardness-conversion.html