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All Graduate Theses and Dissertations Graduate Studies

2014

Uncertainty Analysis of Mechanical Properties

from Miniature Tensile Testing of High Strength
Steels
Deepthi Rao Malpally
Utah State University

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 UNCERTAINTY ANALYSIS OF MECHANICAL PROPERTIES FROM
MINIATURE TENSILE TESTING OF HIGH STRENGTH STEELS

by

Deepthi Rao Malpally

A thesis submitted in partial fulfillment

of the requirements for the degree

of

MASTER OF SCIENCE

in

Mechanical Engineering

Approved:

Dr. Leijun Li Dr. Thomas H. Fronk

Major Professor Committee Member

Dr. Steven L. Folkman Dr. Nicholas A. Roberts

Committee Member Committee Member

Dr. Mark R. McLellan

Vice President for Research and
Dean of the School of Graduate Studies

UTAH STATE UNIVERSITY

Logan, Utah

2014
 ii

Copyright
c Deepthi Rao Malpally 2014

All Rights Reserved

 iii

Abstract

Uncertainty Analysis of Mechanical Properties from Miniature Tensile Testing of High

Strength Steels

by

Deepthi Rao Malpally, Master of Science

Utah State University, 2014

Major Professor: Dr. Leijun Li

Department: Mechanical and Aerospace Engineering

Boat samples extracted from scheduled maintenance shutdowns of piping and pressure

vessels provide opportunities for testing for mechanical properties of the service exposed com-

ponents. However, it is not clear whether testing of miniature specimens machined from boat

samples which are about 2 in. long can be a viable replacement for the standard-sized me-

chanical testing. Three steels, stainless steel Type 304, sensitized Type 304, and SA516 Grade

70 carbon steel, are tested by standard-sized specimen and miniature specimen tensile tests.

Mechanical properties as affected by the specimen geometry and tensile testing procedure for

miniature specimen testing are compared to that of conventional specimens tested according

to ASTM A370-10. The miniature tensile testing results are analyzed by using Monte Carlo

Method (MCM) for uncertainty estimation in order to quantify the probability distribution of

mechanical properties. For the steels under study, miniature specimens with a cross-sectional

area of 3 mm2 and 12 mm gauge length are found to produce equivalent mechanical properties

as tested from standard-sized specimens.

(59 pages)
 iv

Public Abstract

Uncertainty Analysis of Mechanical Properties from Miniature Tensile Testing of High

Strength Steels

by

Deepthi Rao Malpally, Master of Science

Utah State University, 2014

Major Professor: Dr. Leijun Li

Department: Mechanical and Aerospace Engineering

This Miniature mechanical testing study is concerned with the use of miniature speci-

mens to identify the mechanical properties of stainless steel Type 304, sensitized Type 304

and SA516 Grade 70 carbon steel as a viable replacement for the standard sized mechanical

testing. The study aims at obtaining suitable specimen geometry and tensile testing proce-

dure for miniature mechanical testing whose mechanical properties are comparable to that of

conventional specimens of ASTM A370-10 of the same steel. All specimens are flat and the

gauge length cross section will be varied to obtain suitable geometry. The miniature tensile

testing results are further validated by using Monte Carlo Method (MCM) for uncertainty

estimation in order to know the probability distribution of mechanical properties. Miniature

specimens with a cross section of 3 mm2 and 12 mm gauge length are found to produce equiva-

lent mechanical properties as tested from standard-sized specimens. If a reasonable agreement

is received, it will provide us with a very useful tool to evaluate mechanical properties of de-

graded materials, which cannot be removed from service for standard testing, for repair and

service life evaluation.

 v

Dedicated to my dearest parents and brother...

 vi

Acknowledgments

I would like to express my highest regards and gratitude to my major professor, Dr. Leijun

Li, for his continued guidance and advice despite several constraints. I will be forever indebted

to him for believing in a novice like me right from the beginning of my career as a research

assistant at USU. I would like to thank my committee members, Dr. Thomas H. Fronk, Dr.

Steven L. Folkman and Dr. Nick Roberts, for their invaluable suggestions and also Dr. Barton

Smith for his advice in uncertainty analysis. I would like to express my sincere gratitude to the

graduate advisor, Christine Spall, for her constant encouragement and for helping in fulfilling

all the requirements to accomplish graduate studies. I would like to thank all past members of

the Materials Processing & Testing Laboratory, Andrew for helping me prepare the specimens,

Jacob, Zhifen, Yin and Bishal for their friendship. Special thanks to Dayakar Naik for being

my mentor academically and emotionally.

Motivation and belief in oneself is of umpteen importance when one is far away from home.

I would like to thank my dear parents, Ravi and Anjana, for believing in me and boosting my

confidence. I hope to make you proud everyday. Thank you my late grandmother, Usha ajji,

for expressing immense happiness in all my endeavours. Whatever little accomplishments I

have today is all because of your blessings and encouragement. Thank you my little brother,

Sanjeev, for filling my absence at home and all my well wishers.

My experience as a graduate student at USU has been wonderful and fun filled only with

the presence of many fellow graduate students who eventually became friends for life. Thank

you Ravi, for helping me beilieve in myself, Neeraj, Bidisha, Saptarishi, Rajee, Ashish, Swati,

Ruchir, Manju, Joe Shope, Kurt, Scott and many others. I would like to thank my friends

back home, Prerita, Rahul and Danny, for helping me in many ways than I could describe. I

am thankful to God for showing me the right direction in life.

Deepthi Rao Malpally

 vii

Contents

Page
Abstract . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iii
Public Abstract . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iv
Acknowledgments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . vi
List of Tables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . viii
List of Figures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ix
Acronyms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . x
1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
2 Literature Review . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .... 3
2.1 Overview of the field of inquiry . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
2.2 Parameters effecting the mechanical properties of miniature specimens . . . . . 6
2.3 Advances to miniature testing techniques . . . . . . . . . . . . . . . . . . . . . 7
3 Experimental Procedure . . . . . . . . . . .... .... .... . .... .... ..... .... . 9
3.1 Component Element Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
3.2 Sensitization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.3 Tensile Specimen Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
4 Experimental Results and Discussion . . . . . . . . . . . . . . .... .... ..... . . . . 17
4.1 Conventional (Macro-sized specimen) Tensile Testing . . . . . . . . . . . . . . . 17
4.2 Miniature Tensile Testing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
4.3 Optimum Specimen Size . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
5 Uncertainty analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
5.1 Tolerance intervals in Sample Populations . . . . . . . . . . . . . . . . . . . . . 29
5.2 Propagation of Mechanical Properties by Monte Carlo Method (MCM) . . . . . 32
5.2.1 General Approach for MCM . . . . . . . . . . . . . . . . . . . . . . . . . 32
5.2.2 Propagation of Mechanical Properties . . . . . . . . . . . . . . . . . . . 34
5.3 Convergence study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
6 Conclusion and Future Work . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
6.1 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
6.2 Future Work . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
 viii

List of Tables

Table Page

3.1 Component element properties . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

4.1 Conventional (Macro-sized) results . . . . . . . . . . . . . . . . . . . . . . . . . 17

4.2 Results obtained from SEMTester 1000 EBSD . . . . . . . . . . . . . . . . . . . 18

4.3 Mechanical properties for Stainless Steel Type 304 miniature specimens . . . . 20

4.4 Mechanical properties for Sensitized Stainless Steel Type 304 miniature specimens 21

4.5 Mechanical properties for SA516 grade 70 carbon steel miniature specimens . . 22

5.1 Specimen area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

5.2 Load values for (YS) and (UTS) in specimens of gauge area (1x3) mm2 . . . . 36

5.3 Variables and their uncertainties - SS grade 304 . . . . . . . . . . . . . . . . . . 36

5.4 Final length of specimens of gauge cross section (1x3) after tensile testing - SS
grade 304 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38

5.5 Variables and their uncertainties - Sensitized SS grade 304 . . . . . . . . . . . . 39

5.6 Final length of specimens of gauge cross section (1x3) after tensile testing -
Sensitized SS grade 304 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

5.7 Variables and their uncertainties - carbon steel SA516 grade 70 . . . . . . . . . 41

5.8 Final length of specimens of gauge cross section (1x3) after tensile testing -
carbon steel SA516 grade 70 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
 ix

List of Figures

Figure Page

2.1 Shear punch test fixture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

2.2 Indigenously developed table top ball-indentation test system . . . . . . . . . . 4

3.1 Microstructure of SA516 steel etched with 4% Nital . . . . . . . . . . . . . . . 10

3.2 Microstructure of 304/304L steel etched with Vilellas reagent . . . . . . . . . . 10

3.3 Microstructure of sensitized 304/304L steel etched with Vilellas reagent . . . . 11

3.4 Microstructure of 304/304L steel . . . . . . . . . . . . . . . . . . . . . . . . . . 12

3.5 Microstructure of sensitized 304/304L steel . . . . . . . . . . . . . . . . . . . . 12

3.6 SEMTester 1000 EBSD instrument for miniature testing . . . . . . . . . . . . . 14

3.7 Specimen cross section at gage length is (1x0.2) mm . . . . . . . . . . . . . . . 15

3.8 Variation in specimen gage thickness from 3 mm to 0.5 mm . . . . . . . . . . . 15

3.9 (a) Tinius Olsen H50KS (b) Specimen test in progress . . . . . . . . . . . . . . 16

4.1 Chauvenets criterion for rejecting a reading obtained from the book Experi-
mentation, Validation and Uncertainty Analysis for Engineers by Coleman and
Steele [1] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

4.2 Tensile strength vs specimen gauge cross section . . . . . . . . . . . . . . . . . 24

4.3 Yield strength vs specimen gauge cross section . . . . . . . . . . . . . . . . . . 25

4.4 Engineering stress vs strain curves for specimen gauge cross section (1x3) . . . 26

5.1 Factors for two-sided tolerance interval [1] . . . . . . . . . . . . . . . . . . . . . 30

5.2 Schematic for MCM for uncertainty propagation when random standard uncer-
tainties for individual variables are used [1] . . . . . . . . . . . . . . . . . . . . 33

5.3 Distribution of MCM results for yield strength of carbon steel SA516 grade 70.
Expanded uncertainties for each variable being calculated at 95% confidence . . 43

5.4 Convergence study for MCM value of UF for 95% combined uncertainty for each
variable . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
 x

Acronyms

ASTM american standards of testing and materials

SEM scanning electron microscope
EBSD electron backscatter diffraction
MEMS microelectromechanical systems
MMST modified miniature specimen test
FE finite element
EDM electric discharge machining
FIB focused ion beam
LVDT linear variable differential transformer
MCM monte carlo method
DRE data reduction equation
SS stainless steel
YS yield strength
UTS ultimate tensile strength
 1

Chapter 1

Introduction

Steels and alloys experience material degradation when encountered with accidents or

exposed to elevated services, especially after long-term exposure. Depending on the types of

materials, the degradation could include embrittlement, creep, sensitization, phase precipi-

tation, other phase transformation/formation, corrosion, oxidation, etcetra. When materials

experience degradation, it is important to evaluate material properties for repair, extended

use, or life prediction. For the material evaluation, it is often to prefer to obtain the actual

material mechanical properties. However, for many important components, such as vessels in

refinery industry, it is not realistic to obtain sufficient material to perform standard mechanical

testing due to the relative large sample size requirement, which typically needs window cut

from vessels. Window cut from service vessels will involve significant challenges of its replace-

ment from cost and code requirements, and thus, it is typically not feasible to obtain materials

for standard mechanical testing. Nevertheless, it is more feasible to obtain boat samples, such

as about 2 in. (50mm) long, from serviced vessels, and it would be highly valuable for material

evaluation if mechanical testing could be performed on boat samples, which requires miniature

mechanical testing method.

Miniature mechanical testing has become an important aspect of industrial and research

labs, especially for analyzing the mechanical properties. The requirement of miniature test-

ing depends on many factors such as availability. A number of tensile testers have been

employed for miniature testing with samples of different sizes and geometries. For example,

MTI SEMTester can test miniature specimens. Universal Tensile Testing machines can also

be employed for miniature testing depending on the minimum cross head travel as miniature

specimens have very short gauge length. However, there is no study to verify the miniature

mechanical testing results against the standard mechanical testing results.

 2

The current study will verfiy the miniature mechanical testing for stainless steel Type 304,

sensitized Type 304 and SA516 Grade 70 carbon steel as a viable replacement for standard

sized mechancial testing. Miniature tensile specimen designs are developed in a combination of

varying gauge cross-sectional area, and then tested on two different tensile testers, Tinius Olsen

H50KS and MTI SEMTester 1000 EBSD. It is shown in this study that miniature specimens of

a particular gauge cross section exhibit similar mechanical properties to that of its equivalent

conventional size.

Since only a minimum number of specimens are tested, there is a possibility of variation

from the expected conventional results from miniature specimens. This uncertainty in the re-

sults could be due to a number of factors, either machine oriented, which classify as systematic

uncertainties, or procedure oriented, which classify as random uncertainties, in a broad sense.

Also, the variation in miniature measurements reflects local variations in the measurements

that are not measured with full sized specimens. This is due to lesser presence of voids and de-

fects in miniature specimens when compared to standard full sized specimens. An estimation

of uncertainty analysis will help generalize the mechanical properties of the materials being

reviewed, and hence can be compared to conventional testing on a general scale which has not

been covered by any study so far.

The objectives for this study are as follows:

To identify an optimum procedure for extraction of miniature tensile specimens of high

strength steels

To obtain a suitable specimen geomtery relevant to that obtained from a boat sample,

and the miniature tensile tester utilized for the purpose

To analyze the data obtained with miniature specimens and compare the results with

the tensile tests of equivalent standard specimen results

To propagate the mechanical properties obtained after tensile testing of miniature spec-

imens by conducting a Monte Carlo uncertainty estimation

 3

Chapter 2

Literature Review

2.1 Overview of the field of inquiry

The origin of miniaturization of specimens is in the nuclear industry because of expensive

and limited irradiation space, specimen sizes had to be miniaturized for experimental purposes

of irradiation programs in reactors. However, in some cases there is a need to keep the test

specimen similar in size to structural components [2]. The miniature specimen test techniques

are broadly classified as follows [3]:

Tests that are based on miniaturization of conventional specimen sizes such as miniature

tensile, fatigue, impact and fracture toughness tests

Tests based on novel techniques using disk sized specimens such as disk bend tests, shear

punch/small punch tests as shown in Figure 2.1. The small specimen test techniques for

disk bend tests and small punch tests do not have conventional counter parts. These

techniques therefore need to be validated before being effectively used

Tests based on ball indentation techniques as shown in Figure 2.2

Fig. 2.1: Shear punch test fixture

 4

Fig. 2.2: Indigenously developed table top ball-indentation test system

A few methodologies that evolved in the past on miniature testing and its requirement in

various fields are briefly described as follows:

1. Service life of a component is greatly dependent on the extent of monitoring the ma-

terial degradation of the component when in service. In order to monitor the service

life, nondestructive testing is required to evaluate material properties while keeping the

component in service. For this purpose miniature mechanical test named small punch

test has been used [4]. Sample punch test is claimed to be the most effective test as the

specimens can be extracted from the highly stressed zones of the components and also,

the samples can be extracted as many times as required allowing continuous monitoring

of the component while in service.

2. Micro-scale testing has also been developed to characterize the performance and reliabil-

ity of Micro-Electro-Mechanical Systems (MEMS). Various testing techniques have been

developed to measure the mechanical response of small specimens. Different method-

ologies aiming at determining the mechanical properties of small scale samples have

evolved in the recent past. A survey describes that a technique involving instrumented
 5

indentation, most specifically, nano-indentation, coupled with careful loading and un-

loading response of the material make it possible to measure both the hardness and

elastic modulus of material [5]. However, strength and strain hardening effects can-

not be measured with indentation techniques. For manufacture of MEMS, a number

of machining processes such as photolithography, vapor deposition and electro plating

are available in exclusive foundries of MEMS. For machining miniature specimens from

bulk specimens, traditional machining processes are applicable such as wire EDM, laser

machining, chemical mechanical polishing, and FIB milling may be used [5].

3. Recent development in nanomaterials and metallic glasses are facing challenges with

preparation, handling and testing of small volumes of materials and also lack clear un-

derstanding of test results. Hence miniaturization has become a general trend [2]. In

the past, Modified Miniature Specimen Test (MMST) was employed to determine yield

strength, tensile strength and uniform elongation of unirradiated and irradiated reactor

pressure vessel steels [6].

4. Quasi static tensile tests were performed for 1.2mm gauge TRIP800 steel sheets with

miniature tensile sample to determine the effects of sample geometry and loading rate

on tensile ductility [7]. The samples with smaller gauge length will yield higher level of

ultimate ductility since the post uniform elongation is achieved mainly in very narrow

neck region. This is because in the miniature sample geometry, there is the localized

nature of the neck during the post-uniform elongation just before fracture [7]. Similar

increase in ductility was observed in miniature samples of AA5182 samples under quasi

static loading in comparison with full size samples. Also, higher loading rate yielded

higher upper yield strength compared to the results for TRIP steels reported by other

authors. This is different from the reported strain rate sensitivity results for mild steel

where a typical reduction of ductility is observed at high strain rates. However these

discussions are valid for quasi static conditions of the sample being tested.
 6

5. In one of the miniature tensile behavioral studies, the samples were made of ultrafine-

grained Cu having the same width of 1mm and varying gauge length while keeping

thickness constant and vice versa were studied. The results showed that thinner samples

are susceptible to shear failure, resulting in smaller reduction in area [8]. However, the

gauge length has no evident influence on the failure mode or area reduction. This article

further summarizes that shorter and thicker specimens tend to be more ductile. The

thickness effect is mainly seen during necking/fracture modes. The gauge length effect

originates from strain.

6. In another study it is shown that tensile testing of very thin sheet metal, usually spec-

imens lesser than 10m (in this case Cu 99.9%), show trend in decreasing mechanical

properties [9]. However, many authors have mentioned the need for efficient modelling

of the constitutive behavior and the use of simulation and FE analysis [10].

2.2 Parameters effecting the mechanical properties of miniature specimens

1. Miniaturization causes scaling effect, which leads to a different material behavior in the

microscale compared to the macroscale. In general, this effect is pronounced largely and

relates to specimen size and geometry and other factors such as microstructural con-

straints (grain size through specimen thickness, microstructural anisotropy, microstruc-

tural inhomogeneity, etc.), surface effect, residual stress [2].

2. Non uniform stress distributions during testing provide an additional length parameter

that affects the size-effect. The tensile specimen size-effect should be considered when

comparing mechanical properties, such as tensile ductility measured on non-standardized

dog-bone specimens [8]. To minimize any undue stress, the sample must be aligned with

the center line of the two test machine grips [11]. Furthermore, with an ever increasing

popularity of miniaturized tensile specimens in research of materials, there is a need for

a standardized protocol to be adopted.

 7

3. Specimen dimensions and strain measurement methods largely influence the tensile

stress-strain curves. Miniature specimens are too small for use with conventional ex-

tensometers so that the strains are usually calculated from the crosshead displacements.

Uniform elongation and post necking elongation increase with decreasing gauge length

and increasing specimen thickness [12]. With a decrease in thickness, the gauge part is

effectively transformed from a bulk to sheet geometry and the stress state within the

gauge changes from a more or less biaxial condition to uniaxial stress state condition

under tension, thereby resulting in a change from diffuse necking to localized necking.

A reduction in gauge length prolongs the stress-strain curves to higher fracture strains

or higher apparent ductility primarily by prolonging the uniform elongation. However,

in [13], the yield stress is known to be thickness independent for thickness larger than

the critical thickness, usually 6 to 10 times the average grain size for ferrous materials.

4. The variation in micro-sample measurements reflects local variations in the material that

are not measured with full sized specimens. This is due to lesser presence of voids and

defects in miniature samples when compared to the standard full size samples [14].

All the above listed effects are not limited to strength dependence on area, many times it

relates to various microstructural constrains [2, 810, 1227].

2.3 Advances to miniature testing techniques

For tensile specimens of most components in service, the dimensions are larger than the

internal microstructural features, and thus the importance of external size-effects on mechan-

ical properties can be a minor issue and hence can be neglected. However, with the advent

of MEMS, and other miniature testing requirement module samples with microstructural di-

mensions, external size effects have become a more prominent feature to look at. Thus many

small scale devices have been designed to get reliable results from these miniature samples [5].

Nevertheless, there is a need for a handbook for collecting accurate and reliable values of

elastic, plastic, fracture, and fatigue properties of materials at different gage lengths.
 8

Optical techniques have emerged replacing the grip system to hold the specimen in position

as the grip displacement do not give correct strain measurements most of the time [5]. Results

from these miniature tests give an insight into size effects such as elastic, plastic brittle and

ductile behavior at miniature level. Also, the influence of voids and boundary cracks and

surface roughness may also have an effect on the mechanical properties that are being tested

for. With the need of requirement of understanding the mechanical behavior at small scale

level, the trend towards miniature testing will increasingly continue.

 9

Chapter 3

Experimental Procedure

3.1 Component Element Properties

The as-received samples of stainless steel Type 304 and SA516 Grade 70 carbon steel

are initially tested for actual composition. The component element properties are as shown

in Table 3.1. One of the sample slabs of stainless steel Type 304 is furnace heat treated to

promote sensitization.

Table 3.1: Component element properties

A: SA516 Steel, 1/2 Plate
C Mn P S Si Cr Ni Mo Cu
0.14-0.20 0.70-1.00 0.040 max 0.050 max
0.17 0.98 0.015 0.007 0.18 0.11 0.11 0.02 0.26
B: 304/304L. Steel, 1/2 Plate
0.03 max 2.00 max 0.045 max 0.03 max 1.00 max 18.0-20.0 8.0-20.0
0.02 1.62 0.029 0.02 0.40 17.8 8.5 0.02 0.26
C: 304/304L. Steel, 1/2 Plate Sensitized
Same as plate B but furnace heat treated (CRESS electric furnace, model C162012/SD)
at 650 C(1200 F) for 7 days (168 hours)

Microstructures of the as-received samples are captured as shown in Figure 3.1, 3.2 and

3.3. For the preparation of material sample, small portion (about an inch) of the samples are

cut with a band saw. These sample pieces are placed in a mold on to which resin and hardener

mixture is poured and is allowed to solidify. The casting on the sample piece aided in grinding

and polishing for the preparation of flat polished sample. After etching on the flat polished

samples, traces of its microstructure are revealed and the image is captured using an optical

microscope.
 10

Fig. 3.1: Microstructure of SA516 steel etched with 4% Nital

Fig. 3.2: Microstructure of 304/304L steel etched with Vilellas reagent

 11

Fig. 3.3: Microstructure of sensitized 304/304L steel etched with Vilellas reagent

3.2 Sensitization

Sensitization occurs when stainless steel is exposed to very high temperatures (425 C to

815 C). Sensitization effect causes precipitation of chromium carbides at grain boundaries as

chromium carbides are insoluble at high temperatures. For carbide to precipitate, it must

get chromium from the surrounding material causing chromium depleted zone around the

grain boundaries. This chromium depleted zone will be less corrosion resistant, specifically

to intergranular corrosion. Sensitization is important at welded joints. This is because the

welded zones experience very high temperatures causing sensitization [28].

The difference in the grain boundaries is evident in the microstructures. The Grain

boundaries in the sensitized microstructure are darker due to the precipitation of carbides.

The microstructures of stainless steel as-received vs sensitized stainless steel taken at 20x

magnification is shown in Figure 3.4 & 3.5.

 12

Fig. 3.4: Microstructure of 304/304L steel

Fig. 3.5: Microstructure of sensitized 304/304L steel

 13

3.3 Tensile Specimen Preparation

The miniature specimens in this study are sheet specimens unlike in most previous research

where only nano-scale or thin films have been studied. An important factor to be considered in

specimen design for tensile tests is the aspect ratio. The ASTM standard specimen size has an

aspect ratio (gauge length/diameter or in this case thickness) of 4:1. In order to get comparable

results to that of the standard specimens, the miniature specimens were designed to have the

same and multiples of the standard aspect ratio to study the effect of varied cross-sectional

area. The gauge length is considered constant in all specimens to have uniform elongation.

The first batch of specimens is tested on the SEMtester 1000 EBSD Figure 3.6 (designed to

be fit inside a scanning electron microscope (SEM)). The minimum sample size (l w) is

(43 10) mm. Maximum displacement travel is 10mm with maximum load capacity of 1000lb

(4500N). Suitable specimen design is created in Solid Edge software after careful examination

of the grip area and the crosshead capacity of the miniature tensile tester. All specimens had

constant gauge length of 18.21 mm. The dimensions were (1 to 2) mm (0.5 to 1) mm. Each

material condition was tested for three specimen dimensions and 2 repeats in each combination.

For machining miniature specimens, traditional machining processes such as wire EDM, laser

machining, and chemical mechanical polishing, and FIB milling maybe used [5, 29, 30]. In this

study, wire EDM and water jet machining were used to cut out miniature specimens. Wire

EDM process is advantageous mainly because it produces a stress and burr-free cutting, has

efficient production capabilities and is cost effective with an excellent finishing.

The cutting mechanism in wire EDM is by bombarding the work piece with intense short

pulses of electricity and each pulse leaves a tiny pit on the work piece [30]. This causes

surface roughness on the specimen. Studies have proven that, the surface roughness that is

induced during specimen preparation causes reduction in fatigue strength and areas of stress

concentration. For example, fatigue strength of the SiC/Al metal matrix composite suffers

due to the presence of surface roughness which is an aftermath of wire EDM machining.

Therefore, the specimens were sanded before testing. Most of the specimens in the first

batch did not fracture upon reaching maximum strain travel resulting in incomplete stress
 14

Fig. 3.6: SEMTester 1000 EBSD instrument for miniature testing

strain curves. Hence repeatability was very poor. Therefore, a second batch of specimens was

designed with reduced gauge length and cross sectional dimensions to see complete failure of

specimens and improve on the repeatability of the results. Keeping the aspect ratio comparable

to that of the standard, the gauge length and width were maintained constant at 8 mm and

1 mm respectively. The thickness varied from 0.1 mm to 0.2 mm Figure 3.7. The sanding of

the specimens causes slight decrease in thickness.

From each material condition and 2 specimen designs, 2 repeats were conducted. Another

batch of specimens was designed to be tested on Tinius Olsen machine Figure 3.9 in order to

have a comparison of mechanical properties from two different tensile testers. The gauge length

and width were maintained constant at 12 mm and 1 mm, respectively. The thickness varied

from 0.5, 1, and 2 to 3 mm Figure 3.8.

 15

Fig. 3.7: Specimen cross section at gage length is (1x0.2) mm

Fig. 3.8: Variation in specimen gage thickness from 3 mm to 0.5 mm

 16

(a) (b)

Fig. 3.9: (a) Tinius Olsen H50KS (b) Specimen test in progress

From each material condition and 4 specimen designs, 4 repeats were conducted to ensure

repeatability. All the tests were conducted at a strain rate of 0.001s1 .

The Tinius Olsen H50KS is a 50KN capacity model having maximum crosshead travel of

1100 mm. Load measurement accuracy is 0.5% of indicated load from 2% to 100% capacity

and position measurement accuracy of 0.01% of reading or 0.001 mm, whichever is greater.
 17

Chapter 4

Experimental Results and Discussion

4.1 Conventional (Macro-sized specimen) Tensile Testing

The same materials under study are tested on a conventional scale and the following results

(from engineering stress-strain curves) are obtained from AZZ WRI facility. The specimens are

designed with respect to ASTM A370-10 standard with a displacement rate of 0.075 in/min

(1.9 mm/min) until 0.4% offset and post yield loading rate at 0.7 in/min (17.78 mm/min)

until failure. Two tests per material is experimented on a Tinius Olsen tester.

Table 4.1: Conventional (Macro-sized) results

Average Average Youngs

Specimen Elongation
Yield Stress (YS) Tensile Stress (UTS) Modulus
Material (%)
(MPa) (MPa) (GPa)
Stainless Steel
(SS) 276.48 610.19 187.88 61
grade 304/304L
Sensitized (SS)
269.59 617.08 165.82 57
grade 304/304L
Carbon Steel 344.39 529.17 204.08 35

4.2 Miniature Tensile Testing

The miniature specimens designed for micro tensile tester are tested, and the Yield

Strength (YS) and Ultimate Tensile Strength (UTS) obtained are as shown in Table 4.2.

All specimens are flat and have a gauge length of 8 mm. The SEMTester 1000 EBSD is usu-

ally used for testing textiles, foods, biomaterials to paper and polymers. Hence, the results

obtained for such high strength metals are not that accurate as that obtained from Tinius

Olsen. Prestress values are taken care of during data analysis. All specimens are tested at a

strain rate of 0.001s1 . The results obtained from Tinius Olsen are as shown in Tables 4.3
 18

Table 4.2: Results obtained from SEMTester 1000 EBSD

Cross-sectional Yield Strength (YS) MPa Ultimate Tensile Strength (UTS) MPa
Gauge Area(mm2 ) (Average value) (Average value)
Stainless Steel (SS) grade 304/304L
1x0.1 129.00 781.84
1x0.2 92.19 1174.57
Sensitized (SS) grade 304/304L
1x0.1 575.00 794.21
1x0.2 172.02 806.55
Carbon Steel
1x0.1 47.57 377.32
1x0.2 48.34 445.50

through 4.5. All specimens are flat and have a constant gauge length of 12 mm. Prestress

values are subtracted (zeroed) during data analysis. All specimens are tested at a strain rate

of 0.001s1 .

Application of Chauvenets Criterion:

The experiment is affected in numerous ways such as human error while mounting the

specimen and taking the readings, vibrations from surrounding instruments etc. All of these

qualify as random errors. Certain errors like load cell defect and LVDT offsets qualify as

systematic errors as the same error value is affecting every test. Also, in sample to sample

experiments, the variability inherent in the samples themselves causes variations in measured

values in addition to the random errors in the measurement system. A combination of these

errors influence the results obtained from the instrument.

Chauvenets criterion is applied to exclude the values which lie outside a certain range as

dictated by the ratio of maximum acceptable deviation to standard deviation

Xmax
(4.1)
Sx

From the table in Figure 4.1, Chauvenets criterion for rejecting a reading [1], for a set of

four specimens in each cross-sectional gauge area, the absolute value of the ratio of Maximum

Acceptable Deviation to Standard Deviation is 1.54. Hence, any ratio greater than 1.54 is

considered as an outlier. The Chauvenets criterion can be applied on any stress value because
 19

if one value is considered an outlier, the entire test on that specimen is discarded on the whole.

Fig. 4.1: Chauvenets criterion for rejecting a reading obtained from the book Experimentation,

Validation and Uncertainty Analysis for Engineers by Coleman and Steele [1]

From the calculations in Tables 4.3 through 4.5, none of the tests had to be discarded.

Thus, the experiment procedure was correct and all the results are valid.

4.3 Optimum Specimen Size

The optimum miniature specimen size is the one whose results correspond to that of

conventional tensile test results. From the comparison, the miniature stainless steel (SS)

and Sensitized SS grade 304 specimens tested on Tinius Olsen give comparable yield and

engineering tensile strength results. However, one can observe that there is a slight increase

in yield strength (YS) values for miniature SS and Sensitized SS specimens when compared to

its equivalent conventional sized specimens.

 20

Table 4.3: Mechanical properties for Stainless Steel Type 304 miniature specimens

Yield Strength Ultimate Tensile

Sl. No. /Sx  /Sx 
   
Elongation (%)



 Xi X  Xi X
(MPa) Strength (MPa)
Specimen Cross-Section (1x3)mm2
1 275.45 1.12 691.00 1.36 58
2 306.70 0.93 640.85 0.15 66
3 303.95 0.75 640.42 0.16 63
4 283.82 0.57 611.00 1.05 66
X1 292.48 645.81 63.25
Sx 2 15.26 33.20 3.77
Interval 292.4815.26 645.8133.20 63.253.77
Specimen Cross-Section (1x2)mm2
1 296.41 0.16 690.07 1.33 50
2 301.92 0.46 620.00 0.37 58
3 306.97 1.02 639.10 0.09 42
4 285.99 1.32 592.10 1.05 46
X 297.82 635.32 49
Sx 8.99 41.29 6.83
Interval 297.828.99 635.3241.29 496.83
Specimen Cross-Section (1x1)mm2
1 191.72 1.35 508.00 1.05 50
2 229.31 1.04 579.06 0.74 46
3 212.73 0.01 524.00 0.65 50
4 217.82 0.31 588.04 0.96 42
X 212.90 549.76 47
Sx 15.73 39.71 3.83
Interval 212.9015.73 549.7639.71 473.83
Specimen Cross-Section (1x0.5)mm2
1 157.69 0.19 543.00 1.01 25
2 147.38 1.15 435.00 1.37 25
3 160.38 0.06 500.00 0.06 46
4 173.45 1.28 511.00 0.30 25
X 159.73 497.25 30.25
Sx 10.73 45.33 10.50
Interval 159.7310.73 497.2545.33 30.2510.50
1 Average Value
2 Standard Deviation
 21

Table 4.4: Mechanical properties for Sensitized Stainless Steel Type 304 miniature specimens

Yield Strength Ultimate Tensile

Sl. No. /Sx  /Sx 
   
Elongation (%)



 Xi X  Xi X
(MPa) Strength (MPa)
Specimen Cross-Section (1x3)mm2
1 301.38 0.76 740.00 1.13 66
2 262.31 0.96 683.42 0.45 58
3 267.01 0.76 548.39 1.17 66
4 305.85 0.96 612.00 0.41 42
X 284.14 645.95 58
Sx 22.65 83.51 11.31
Interval 284.1422.65 645.9583.51 5811.31
Specimen Cross-Section (1x2)mm2
1 263.26 0.66 546.00 0.29 50
2 236.75 0.37 526.00 0.03 42
3 174.29 1.43 443.60 1.33 58
4 266.47 0.73 595.00 1.07 58
X 235.19 527.65 52
Sx 42.73 63.09 7.66
Interval 235.1942.73 527.6563.09 527.66
Specimen Cross-Section (1x1)mm2
1 149.71 0.07 472.00 0.49 58
2 197.64 1.21 485.95 0.90 58
3 105.84 1.24 407.00 1.40 42
4 156.14 0.10 455.00 0.00 46
X 152.33 454.99 51
Sx 37.58 34.40 8.25
Interval 152.3337.58 454.9934.40 518.25
Specimen Cross-Section (1x0.5)mm2
1 79.74 0.85 299.00 1.26 38
2 86.84 0.59 341.00 0.27 50
3 140.15 1.39 398.00 1.06 33
4 103.81 0.04 373.00 0.47 42
X 102.64 352.75 40.75
Sx 26.97 42.76 7.18
Interval 102.6426.97 352.7542.76 30.2510.50
 22

Table 4.5: Mechanical properties for SA516 grade 70 carbon steel miniature specimens

Yield Strength Ultimate Tensile

Sl. No. /Sx  /Sx 
   
Elongation(%)



 Xi X  Xi X
(MPa) Strength (MPa)
Specimen Cross-Section (1x3)mm2
1 301.99 1.33 465.44 1.46 25
2 291.92 0.12 440.00 0.17 33
3 282.37 1.02 432.00 0.68 25
4 287.34 0.43 433.00 0.61 25
X 290.91 442.61 27
Sx 8.36 15.63 4
Interval 290.918.36 442.6115.63 274
Specimen Cross-Section (1x2)mm2
1 318.37 1.12 461.00 0.27 25
2 233.47 0.69 362.00 1.45 33
3 291.50 0.55 465.00 0.34 21
4 219.83 0.98 494.00 0.84 25
X 265.79 445.50 26
Sx 46.84 57.58 5.03
Interval 265.7946.84 445.5057.58 265.03
Specimen Cross-Section (1x1)mm2
1 180.81 0.38 328.00 0.32 42
2 208.90 1.03 350.00 1.25 21
3 106.05 1.34 296.01 1.02 17
4 161.29 0.07 307.00 0.56 25
X 164.26 320.25 26.25
Sx 43.45 23.86 10.99
Interval 164.2643.45 320.2523.86 26.2510.99
Specimen Cross-Section (1x0.5)mm2
1 70.76 1.44 203.00 0.91 17
2 153.42 0.37 240.00 0.33 25
3 145.70 0.20 250.00 0.18 25
4 175.63 0.86 352.00 1.42 13
X 136.38 261.25 20
Sx 45.55 63.79 6
Interval 136.3845.55 261.2563.79 206
 23

This can be explained due to lesser presence of anomalies in the microstructure when

compared to the macro-sized specimens. Also, lesser number of voids is present in a miniature

specimen. Further, sensitized stainless steel is heat treated for several hours (168) leading to

softening of the metal. This is explained due to the diffusion of Cr, C and N towards the

grain boundaries from the grain body, thus indicating a fall in hardness of stainless steel.

This is usually seen after 1 hour of sensitization. When the duration is longer than 1 hour,

the hardness marginally increases due to the precipitation at the grain boundaries and also

formation of martensitic microstructure [31].

The carbon steel specimens show more ductility owing to lesser yield strength (YS) values

at miniature level. Such a ductile nature is seen only in carbon steel specimens unlike the

stainless steel (SS) specimens hence carbon specimens were more sensitive to miniaturization.

Also, the tensile strength values are lower than the conventional results. A plausible reasoning

is due to the brittle nature of carbon steel and at miniature level the volume is much lesser

than the conventional owing to lesser strength and higher ductility. Very thin cross sections

that were tested on microtensile tester gave considerably high results for SS specimens and

slightly comparable results for carbon steel specimens as shown in Figure 4.2 and 4.3.

Considering all the above reasoning, the recommended miniature size for all three ma-

terials is a gauge area of (1 3) with an aspect ratio 4:1 which is the same as that of the

standard ASTM testing for a constant gauge length of 12 mm. The overall specimen size was

approximately 50 mm (2 in.). The engineering stress versus strain curve for four specimens of

gauge dimension (1 3) from each material is as shown in Figure 4.4.

 24

800

700

600

Tensile Strength (MPa)

500

400

300

200

100

0
0 0.5 1 1.5 2 2.5 3 3.5
Cross-Sectional Area (mm2)

(a) Stainless Steel grade 304

800

700

600
Tensile Strength (MPa)

500

400

300

200

100

0
0 0.5 1 1.5 2 2.5 3 3.5
Cross-Sectional Area (mm2)

(b) Sensitized Stainless Steel grade 304

600

500
Tensile Strength (MPa)

400

300

200

100

0
0 0.5 1 1.5 2 2.5 3 3.5
Cross-Sectional Area, (mm2)

(c) Carbon Steel(SA5 16) grade 70

Fig. 4.2: Tensile strength vs specimen gauge cross section

 25

350

300

250

Yield Strength (MPa)

200

150

100

50

0
0 0.5 1 1.5 2 2.5 3 3.5
Cross-Sectional Area (mm2)

(a) Stainless Steel grade 304

350

300

250
Yield Strength (MPa)

200

150

100

50

0
0 0.5 1 1.5 2 2.5 3 3.5
Cross-Sectional Area (mm2)

(b) Sensitized Stainless Steel grade 304

350

300

250
Yield Strength (MPa)

200

150

100

50

0
0 0.5 1 1.5 2 2.5 3 3.5
Cross Sectional Area (mm2)

(c) Carbon Steel(SA5 16) grade 70

Fig. 4.3: Yield strength vs specimen gauge cross section

 26
800

700

600

500

Stress (MPa)
400

300

200
Specimen 1
Specimen 2
100 Specimen 3
Specimen 4
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
Strain (mm/mm)

(a) Stainless Steel grade 304

800

700

600

500
Stress (MPa)

400

300

200
Specimen 1
Specimen 2
100 Specimen 3
Specimen 4
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
Strain (mm/mm)

(b) Sensitized Stainless Steel grade 304

500

450

400

350

300
Stress (MPa)

250

200

150
Specimen 1
100
Specimen 2
Specimen 3
50
Specimen 4
0
0 0.05 0.1 0.15 0.2 0.25 0.3 0.35
Strain (mm/mm)

(c) Carbon Steel(SA5 16) grade 70

Fig. 4.4: Engineering stress vs strain curves for specimen gauge cross section (1x3)
 27

When gauge length is maintained constant, with decrease in thickness, the gauge part is

effectively transformed from a bulk to sheet geometry and the stress state within the gauge

changes from a more or less biaxial to a uniaxial stress state condition, thereby resulting in

a change from diffuse necking to localized necking. In a tension test on a ductile material, a

diffuse necking - so called because its spatial extension is much larger than the sheet thickness

- begins to develop in the sample when the strain hardening is no longer able to compensate

for the weakening due to the reduction of the cross-section. After some elongation under

decreasing load, a localized neck usually appears in the region of the diffuse neck. In the

localized neck, severe thinning occurs leading to ultimate failure. The transition from diffuse

to localized neck happens much faster in a sheet specimen (in this case miniature specimen)

when compared to a bulk specimen (conventional specimen). This causes reduction in yield

strength since elastic zone is shortened and hence, material exhibits more ductility as a sheet

miniature specimen than a conventional specimen.

Miniature specimens have smaller volumes compared to conventional specimens. There-

fore, it might be because of smaller volume, the interatomic forces give way too soon under

tension (as they have small number of grains) causing decreased strain hardening effect.Yield

stress is more sensitive to increase in strain rate than the tensile strength. High rates of strain

cause a yield point to appear in specimens of low carbon steel which otherwise do not appear

when tested under ordinary rates of loading [32]. All specimens were tested with a strain rate

of 0.001s1 . However, miniature carbon steel specimens show yield point as seen in Figure

4.4(c).

The Modulus of elasticity in all three material specimens was found to be as low as about

6895 MPa (1000 ksi) in all the three specimens. There are various reasoning for this behavior of

miniature specimens. The literature shows that with the increase of gauge length, the Youngs

Modulus values also increase with different strain rates [2]. A strong dependence of elastic

modulus on gauge length suggests that some shear might occur causing a deviation from the

linear stress-strain relationship [2].

It is reported in many studies that the smaller the gauge length, the lower the slope of the
 28

linear stress/strain relationship is detected for samples with shorter gauge length (with respect

to the volume of the conventional specimens). However, shorter linear portion of stress strain

graph does not influence the overall elongation of the material until maturation. Also, steel

crystal is highly anisotropic; grain orientation anisotropy can be a valuable explanation for

low Modulus values [33]. Youngs Modulus is the materials resistance to elastic deformation.

The greater the modulus, the stiffer the material or smaller the elastic strain that results from

application of a given stress. On atomic scale, macroscopic elastic strain is manifested as small

changes in the interatomic spacing and the stretching of interatomic bonds.

As a consequence, the magnitude of the modulus is a measure of resistance to separation

of adjacent atoms which is interatomic bonding forces [34].

 29

Chapter 5

Uncertainty analysis

5.1 Tolerance intervals in Sample Populations

In addition to the confidence interval for a sample population, there is a useful statistical

interval called the tolerance interval. The tolerance interval gives information about the parent

population that the specimens came from [1]. The Gaussian interval that contains 95% of the
1.96, i.e the average value of the specimens being tested
parent population is simply the X

1.96 times the random standard deviation. However, when we are dealing with specimens
and Sx , the determination of the range that contains a portion
and the statistical quantities X

of the parent population is not as straightforward. What one can estimate is the range that

has a certain probability of containing a specified percentage of the parent population.

Considering a set of four specimens of (1 3) cross-sectional area, and to find an estimate

of 99% of the parent population with 95% confidence is

 
X CT 95(99) (4) Sx (5.1)

where CT is a factor which is given as a function of the number of readings in Table A.3 as

in Figure 5.1 [1], for four specimens CT 95(99) factor is 8.299. (Here the number of specimens

is four but note that if the number of specimens tends to infinity, the concept of a confidence

level for the tolerance interval does not apply because the tolerance interval approaches the

Gaussian interval.) For YS readings of SS grade 304 specimens with gauge length 12 mm,


using the mean X 292.48 MPa and Sx 15.26 MPa from Table 4.3 in Eq.5.1

292.48 [8.299] [15.26] M P a (5.2)

 30

Fig. 5.1: Factors for two-sided tolerance interval [1]

prob (165.80 419.17) M P a (5.3)

For UTS readings, using the mean X 645.82 MPa and Sx 33.21 MPa in Eq.5.1

645.82 [8.299] [33.21] M P a (5.4)

prob (370.25 921.39) M P a (5.5)

For YS readings of Sensitized SS grade 304 specimens with gauge length 12 mm, using


the mean X 284.14 MPa and Sx 22.65 MPa from Table 4.4 in Eq.5.1
 31

284.14 [8.299] [22.65] M P a (5.6)

prob (96.17 472.10) M P a (5.7)

For UTS readings, using the mean X 645.95 MPa and Sx 83.50 MPa in Eq.5.1

645.95 [8.299] [83.50] M P a (5.8)

prob (47.04 1338.93) M P a (5.9)

For YS readings of carbon steel (SA5 16) grade 70 specimens with gauge length 12 mm,


using the mean X 290.91 MPa and Sx 8.36 MPa from Table 4.5 in Eq.5.1

290.91 [8.299] [8.36] M P a (5.10)

prob (221.56 360.26) M P a (5.11)

For UTS readings, using the mean X 442.61 MPa and Sx 15.63 MPa in Eq.5.1

442.61 [8.299] [15.63] M P a (5.12)

prob (312.89 572.33) M P a (5.13)

Eq.5.3,5.7 and 5.11 gives the tolerance interval for 99% of the parent population with

95% confidence for YS. From Table 4.1, the conventional YS of SS specimens are 276.48 MPa,

Sensitized SS specimens are 269.59 MPa and carbon steel specimens are 344.39 MPa. Eq.5.5,5.9

and 5.13 gives the tolerance interval for UTS. The conventional UTS of SS specimens are 610.19

MPa, Sensitized SS specimens are 617.08 MPa and carbon steel specimens are 529.17 MPa.

Hence our miniature specimen tensile testing experiments give approximate values as that of

the conventional testing as per ASTM A370-10 standard.

 32

5.2 Propagation of Mechanical Properties by Monte Carlo Method (MCM)

Monte Carlo simulation provides a distribution of errors for a result that is a function

of multiple variables. In most cases, the result of our experiment or simulation will depend

on several variables through a data reduction equation (DRE) or a simulation solution. This

method is not limited to simple expressions but can also be used for highly complicated

equations or for numerical solutions of advanced simulation equations.

In this section, a general approach for the MCM for uncertainty propagation is discussed

and this technique is applied to the data reduction equations of the current study. The

mechanical properties of the three materials are propagated to parent population. It is seen

that our experimental results, obtained by a set of four specimens in each gauge cross section,

fall in the same interval as that of the propagated values of the parent population. The

section concludes with a discussion for the convergence of the combined standard uncertainty

(or relative uncertainty with respect to each iteration represnting a specimen) in this MCM

analysis.

5.2.1 General Approach for MCM

Figure 5.2 presents a flowchart that shows the steps involved in performing an uncertainty

analysis by the MCM. The figure shows the sampling techniques of two variables, but the

methodology is general for DREs or simulations that are functions of multiple variables. First,

the assumed true value for each variable (load, area, stress etc.) in the result is the input.

These would be the Xbest values that we have for each variable. Then, the estimates of the

random standard uncertainty, s and the elemental systematic standard uncertainties bk for

each variable are input. An appropriate probability distribution function is assumed for each

error source. The random errors are usually assumed to come from a Gaussian distribution.

The systematic errors are chosen based on the analysts judgment as it is upto the analyst to

use the best information.

 33

Fig. 5.2: Schematic for MCM for uncertainty propagation when random standard uncertainties
for individual variables are used [1]

For the flowchart in Figure 5.2, the random standard uncertainties for X and Y are

assumed to come from Gaussian distributions and that each variable has three elemental

systematic standard uncertainties, one Gaussian, one triangular, and one rectangular.

For each variable, random values for the random errors and each elemental systematic error

are found using an appropriate random number generator (Gaussian, triangular, rectngular,

etc.). The individual error values are then summed and added to the true values of the

variables to obtain measured values. Using these measured values, the result is calculated.

This process corresponds to running the simulation once.

 34

5.2.2 Propagation of Mechanical Properties

The Data Reduction Equations (DRE) for the study are the equations for YS, UTS and

elongation (el) given by,

load
y (M P a) = (5.14)
area

load
(M P a) = (5.15)
area

lf l0
el = (5.16)
l0

where y is YS, is UTS, lf is final gauge length after fracture and l0 is the original gauge

length. The unit of load is in KN and that of area is mm2 . All lengths are in mm. However,

elongation or strain is dimensionless.

Before testing, the thickness and width of the specimens are carefully measured at three

different locations in the gauge length. The average of the readings is considered as the

thickness and the width values which are subsequently used for calculation of area. Random

standard uncertainty for (95%) confidence interval (Eq.5.17) for area is calculated using Table

5.1.

U ncertainty (95%) = 1.96 Sx (5.17)

 35

The uncertainty analysis is conducted only on optimum specimen size as it yields almost

the same mechanical properties as that of a conventional specimen.

Table 5.1: Specimen area

Specimen No. Area (mm2 )
SS grade 304 - (1x3) specimens
1 2.90
2 2.89
3 2.88
4 2.88
Average 2.89
Standard Deviation 0.00957
Sensitized SS grade 304 - (1x3) specimens
1 4.26
2 2.84
3 2.74
4 2.83
Average 3.17
Standard Deviation 0.07297
Carbon Steel (SA5 16) grade 70 - (1x3) specimens
1 2.97
2 2.95
3 2.88
4 2.90
Average 2.93
Standard Deviation 0.04203

For SS 304 = 1.96 0.00957

Uncertainty for area = 0.0188mm2 or 1.8%

For Sensitized SS 304 = 1.96 0.07297.

Uncertainty for area = 0.14303mm2 or 14.30%

For Carbon Steel 70 = 1.96 0.04203

Uncertainty for area = 0.0824mm2 or 8.24%

Below is the table for force applied by the load cell in each test for yielding to take place.

Yielding point is crucial in every material testing as the specimen enters the plastic zone.

Tensile strength does not depend on when the yielding takes place for a given material. The
 36

load cell has a value of +/ 0.5% of the applied load value. This specification is in the Tinius

Olsen manual.

Table 5.2: Load values for (YS) and (UTS) in specimens of gauge area (1x3) mm2

Specimen No. (YS) Load (KN) (UTS) Load (KN)

SS grade 304 - (1x3) specimens
1 0.80 2.01
2 0.89 1.85
3 0.87 1.84
4 0.82 1.86
Average 0.85 1.89
Sensitized SS grade 304 - (1x3) specimens
1 1.28 3.15
2 0.74 1.94
3 0.73 1.50
4 0.86 1.73
Average 0.90 2.08
Carbon Steel (SA5 16) grade 70 - (1x3) specimens
1 0.90 1.38
2 0.86 1.30
3 0.81 1.24
4 0.83 1.25
Average 0.85 1.29

Stainless steel grade 304/304L

Table 5.3: Variables and their uncertainties - SS grade 304

Variables Nominal Value Uncertainty (95%)
Area (A)mm2 2.89 1.8%
YS Load (F )KN 0.85 0.5%
UTS Load (Fu )KN 1.89 0.5%

Calculations for finding the uncertainty of YS using Eq.5.14

Uy 2 Uy 2
   

2 2
Uy = (UF ) + (UA )2
F A
 2 (5.18)
F 2
 
1 2
= (UF ) + (UA )2
A A2
 37

The MCM nominal value (true value) for load and area (variables) are obtained from running

the MCM algorithm for 10000 (M times) iterations in MATLAB. However, since the nominal

value for area is very less, no significant changes were seen after running 10000 iterations,

although the load values changed every single time. 10000 iterations is not just a random

number chosen. It is later seen in this section that this number generates a converged value

for relative uncertainty of the results.

If we assume that all distributions are Gaussian, then the standard uncertainty inputs for

the MCM will be previous percent uncertainties divided by 2. Plugging the nominal values

obtained for the variables from the program, Eq.5.18 becomes

2  2 2  2
0.8452 103 0.005 0.85 103 2.9 1.8 102
 

2 1
Uy = +
2.89 1.96 2.892 1.96

= 0.5565 7.3464

= 7.90

(5.19)

In the above equation, (UF ) is 0.8452 103 (N ) 0.005/1.96 where 0.8452 is the MCM

nominal value for load to cause yielding and multiplied by one standard uncdertainty, i.e the

standard uncertainty inputs for the MCM will be previous percent uncertainties divided by

2 or 1.96 for considering only the random uncertainties at 95% confidence. Similarly, (UA ) is

(2.9 1.8 102 )/1.96 where 2.9 mm2 is the MCM nominal value for area.


Uy = 2.81 MPa

Therefore, the uncertainty in the YS is the average value obtained from our experiment,

292.48 2.81 MPa.

Calculations for finding uncertainty in UTS using Eq.5.15

U 2 U 2
   
(U )2 = (UFu )2 + (UA )2
Fu A
 2 (5.20)
Fu 2
 
1 2
= (UFu ) + (UA )2
A A2
 38

The nominal value of the load changes as the load applied at breaking is different from the

load applied at yielding.

2  2 2  2
1.8942 103 0.005 1.89 103 2.9 1.8 102
 
2 1
(U ) = +
2.89 1.96 2.892 1.96
(5.21)
= 2.7949 36.3211

= 39.12

(U ) = 6.25 MPa

Therefore, the uncertainty in the UTS is the average value obatined from our experiment,

645.82 6.25 MPa.

For finding the uncertainty in elongation, the final length of each specimen needs to be

calculated after testing. The final specimen length was measured from the neck of the gauge

length of the fractured specimen.

Table 5.4: Final length of specimens of gauge cross section (1x3) after tensile testing - SS
grade 304
Specimen No. Final Length lf mm
1 19.00
2 20.00
3 19.50
4 20.00
Average 19.63
Standard
0.4787
Deviation

From Eq.5.17, uncertainty for lf is 0.9383 mm. Therefore, the final length is 19.63

0.9383 mm. Using Eq.5.16, the mean of the final length as 19.63 and the original gauge length

as 12 mm, elongation E is 0.636 or 64%. Calculations for finding uncertainty in E using

Eq.5.16 are

Uel 2 Uel 2
   

2
(Uel )2 = Ulf + (Ul0 )2
lf l0
 2 (5.22)
lf 2
 
1
2
= Ulf + 2 (Ul0 )2
l0 l0
 39

The original length for all specimens is 12 mm nevertheless the least count of the measuring

caliper is taken as the uncertainty. In this case the uncertainty value is 0.001. Upon substitu-

tion of nominal values for final and original length randomly generated by MATLAB for MCM

analysis,

 2  2  2  2
1 20.468 0.9383 19.63 11.99 0.001
(Uel )2 = +
12 1.96 122 1.96 (5.23)
= 0.6667

(Uel ) = 0.8165

Therefore, the total uncertainty in the elongation is within the range of 0.636 0.8165 or

64% 81.6% of the final length. This elongation can be really high if the material is ductile.

A ductile material has low yielding point and hence undergoes yielding for a long period before

failure. Another reason for high elongation is inclusions in the alloy material. Note that when

10000 iterations represents 10000 experimental trials that have random outcomes [35]. When

applied to uncertainty estimation, random numbers are used to ramdomly sample parameters

uncertainty space instead of point calculation carried out by a small test of experiments.

Hence it is a method where propagation of uncertainty is achieved. Therefore, the possibility

of elongation being greater than the value itself is almost insignificant. The range is a number

interval within which elongation may lie without reaching to the extremes.

Sensitized SS grade 304/304L

Table 5.5: Variables and their uncertainties - Sensitized SS grade 304

Variables Nominal Value Uncertainty (95%)
Area (A)mm2 3.17 14.30%
YS Load (F )KN 0.90 0.5%
UTS Load (Fu )KN 2.08 0.5%
 40

Uncertainty calculation in YS is obtained by using Eq.5.14 and 5.18. The nominal value

for load and area are obtained from running the MCM algorithm for 10000 iterations in

MATLAB.

2  2 2  2
0.9105 103 0.005 0.90 103 3.16 14.30 102
 

2 1
Uy = +
3.17 1.96 3.172 1.96
(5.24)

Uy = 21.38 MPa

Therefore, the uncertainty in the YS is the average value obtained in our experiment,

284.14 21.38 MPa.

Calculations for finding uncertainty in UTS using Eq.5.15 and 5.20

2  2 2  2
2.0756 103 0.005 2.08 103 3.16 14.30 102
 
2 1
(U ) = +
3.17 1.96 3.172 1.96
(5.25)

U = 47.77 MPa

Therefore, the uncertainty in the UTS is the average value obtained in our experiment,

645.95 47.77 MPa.

Uncertainty in elongation is calculated based on the following table.

Table 5.6: Final length of specimens of gauge cross section (1x3) after tensile testing - Sensi-
tized SS grade 304
Specimen No. Final Length lf mm
1 20.00
2 19.00
3 20.00
4 17.00
Mean 19.00
Standard
1.414
Deviation

From Eq.5.17, uncertainty for lf is 2.7714 mm. Therefore, the final length is 19.00

2.7714 mm. Using Eq.5.16, the mean of the final length as 19.00 and the original gauge length
 41

as 12 mm, elongation E is 0.583 or 58%. Calculations for finding uncertainty in E using

Eq.5.16 and Eq.5.22

 2  2  2  2
2 1 18.11 2.7714 19 11.99 0.001
(Uel ) = + (5.26)
12 1.96 122 1.96

Uel = 2.1339

Therefore, the uncertainty in the elongation is 0.5383 2.1339.

Carbon steel SA516 grade 70

Table 5.7: Variables and their uncertainties - carbon steel SA516 grade 70
Variables Nominal Value Uncertainty (95%)
Area (A)mm2 2.93 8.24%
YS Load (F )KN 0.85 0.5%
UTS Load (Fu )KN 1.29 0.5%

Uncertainty calculation in YS is obtained by using Eq.5.14 and 5.18. The nominal value

for load and area are obtained from running the MCM algorithm for 10000 iterations in

MATLAB.

2  2 2  2
0.8459 103 0.005 0.85 103 2.90 8.24 102
 

2 1
Uy = +
2.93 1.96 2.932 1.96
(5.27)

Uy = 12.09 MPa

Therefore, the uncertainty in the YS is the average value obtained in our experiment,

290.91 12.09 MPa.

Calculations for finding uncertainty in UTS using Eq.5.15 and 5.20

2  2 2  2
1.2923 103 0.005 1.29 103 2.90 8.24 102
 
2 1
(U ) = +
2.93 1.96 2.932 1.96
(5.28)

U = 18.56 MPa
 42

Therefore, the uncertainty in the UTS is the average value obtained in our experiment,

442.61 18.56 MPa. Uncertainty in elongation is calculated based on the following table.
 43

Table 5.8: Final length of specimens of gauge cross section (1x3) after tensile testing - carbon
steel SA516 grade 70
Specimen No. Final Length lf mm
1 15.00
2 16.00
3 15.00
4 15.00
Mean 15.25
Standard
0.5
Deviation

From Eq.5.17, uncertainty for lf is 0.98 mm. Therefore, the final length is 15.25 0.98

mm. Using Eq.5.16, the mean of the final length as 15.25 and the original gauge length as 12

mm, elongation E is 0.271 or 27%. Calculations for finding uncertainty in E using Eq.5.16

and 5.22

 2  2  2  2
2 1 15.17 0.98 15.25 11.99 0.001
(Uel ) = + (5.29)
12 1.96 122 1.96

Uel = 0.6321

Therefore, the uncertainty in the elongation is 0.271 0.6321.

5.3 Convergence study

The sampling process is repeated M times to obtain a distribution for the possible result

values. The primary goal of the MCM propagation technique is to estimate a converged value

for the standard deviation SM CM , of this distribution. 2s of this distribution is the resultant

uncertainty at 95% confidence (assuming the distribution is Gaussian). An appropriate value

for M is determined by periodically calculating SM CM during the MCM process and stopping

the process when a converged value of SM CM is obtained. The SM CM is the combined standard

uncertainty of the result (uncertainty in each reading/iteration). The number of iterations, in

this case is 10000 (M ).

We do not need to have a perfectly converged value of SM CM to have reasonable estimate

of uncertainty. Once the SM CM values are converged to within 1-5%, then the value of SM CM
 44

is a good approximation of the combined standard uncertainty of the result.

Figure 5.3 gives the distribution for uncertainties calulated in Eq.5.27 for YS in carbon

steel specimens. The resultant uncertainty is calulated using Eq.5.30

 
2UF
(5.30)
F M CM

where, UF is the uncertainty calculated using the true value generated for a variable (load)

in the Eq.5.27 and F is the true value generated by MCM process. This value of expanded

uncertainty is stored with every iteration. In Figure 5.3, load and area uncertainties are

included. The distribution is Gaussian, hence our assumption is valid.

350

300

250
No. of Specimens

200

150

100

50

0
2.5 2.6 2.7 2.8 2.9 3 3.1 3.2 3.3 3.4 3.5
Uncertainty, %

Fig. 5.3: Distribution of MCM results for yield strength of carbon steel SA516 grade 70.
Expanded uncertainties for each variable being calculated at 95% confidence

The averge uncertainty is 3.0344% and the standard deviation is 0.1200% for the entire

range of specimens.

The convergence plot is as shown in Figure 5.4. The plot describes the convergence of

relative uncertainty of the specimens. The value of standard deviation, s of the resultant
 45

uncertainty as in Eq.5.30 was calculated after every iteration, starting from the first iteration.

The plot of these s values which represent combined standard uncertainty, SM CM is plotted

in Figure 5.4. The value of relative uncertainty or the combined standard uncertainty was a

fully converged value from a large number of iterations as seen.

0.08

0.07

0.06
Relative uncertainty, %

0.05

0.04

0.03

0.02

0.01

0
0 1000 2000 3000 4000 5000 6000 7000 8000 9000 10000
Monte Carlo Iterations, M (No. of specimens)

Fig. 5.4: Convergence study for MCM value of UF for 95% combined uncertainty for each
variable

We see that after 1000 iterations, the value has converged to within 3% and by about 2000

iterations to within less than 1% of the fully converged value. About 6.3% is the combined

standard uncertainty for 10000 specimens. Since these are characteristic plots, similar trend

is seen with mechanical properties of stainless steel and sensitized steel as well. Any further

addition to 10000 would still give us a converged value and hence our selection of 10000

iterations is reasonable.
 46

Chapter 6

Conclusion and Future Work

6.1 Conclusions

This study clearly shows that the tensile testing results of miniature specimens are de-

pendent not only on the property of the material itself and testing conditions (strain rate,

tensile machine employed, etc.), but also on specimen size and geometry. Miniature specimens

can be of any cross-section but to choose the best cross-section for a particular application is

challenging. Four different specimen gauge cross-sections having the same or multiple of the

ASTM standard aspect ratio is designed with a constant gauge length of 12mm. With the

current facilities, the specimens were tested upon two different machines, Tinuis Olsen and

SEMTester 1000 EBSD.

From the results obtained, larger consistency in results was obtained from Tinius Olsen

machine. The specimens with gauge cross- section (1 3) shows repeatability in results which

is considerably agreeable to that of the ASME- SA 240 standard and the macro sized testing

performed by AZZ WSI, hence considered an optimum specimen cross-section. The variation

in results is present in all specimen lots but more pronounced in the smaller cross-section

specimens. Variations are attributed to a number of factors such as stress concentration

effects while machining the specimen, especially near the fillet area and voids present within.

To minimize any undue stress, the specimen must be aligned with the center line of the two

test machine grips [11]. Therefore, Chauvenets criterion is applied to remove the results that

are most effected from the above mentioned factors so that more reliable mean and standard

deviation is obtained. However, in the optimum specimen size considered, there was no big

variation that was observed after the application of Chauvenets criterion. Tolerance interval

for the parent population is estimated within 95% confidence and the method assumes to have

a Gaussian parent population. To exclude the assumption made previously, MCM analysis for
 47

uncertainty propagation is employed as the inputs to MCM analysis need not be Gaussian.

The mean of the UTS for SS and Sensitized SS grade 304/304L specimens may lie within

370.25 to 921.39 MPa and 1338.93 MPa, respectively. The mean for the experimented lot in

this study for SS specimens is 645.82 6.25 MPa and for Sensitized SS specimens is 645.95

47.77 MPa, which lies well within the range. The range of UTS within which Carbon Steel

specimens may lie is 312.89 to 572.33 MPa and the mean for the experimented lot from this

study is 442.61 18.56 MPa which is well within the expected range.

A conclusion can be drawn from this study that uncertainty analysis must be conducted in

sample to sample experiments to know whether the range of the results obtained are agreeable

with that of the standard results. In most studies, we see that a certain experiment is simply

rejected for giving inconsistent results failing to understand the random and systematic errors

that are prevalent in experimentation. Propagation of uncertainty is required in every research

field to know whether the experimental results observe the same trend as that of the parent

population.

6.2 Future Work

The mechanical properties obatined with the set of specimens, categorized as optimum

specimen design in this thesis gives a good approximation to that of the conventional spec-

imens. The uncertainty analysis further ensures our study and validates the properties ob-

tained on a large scale. However, the miniature specimens in this study was focussed on high

strength steels. Many types of metals can be studied at miniature level, specimens obtained

from boat samples to understand its behavior. Many a time, structures are subjected to high

temperatures and is difficult to conduct a conventional test of an equivalent material at that

temperature. Miniature mechanical properties should be determined at varied temperature

levels. Further, SEM should be employed along with the SEMTester, miniature testing instru-

ment to find out the physics at miniature level as many properties depend on a large number

of variables.
 48

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