TABLE OF CONTENTS

CHAPTER NO.

TITLE

PAGE NO.

ABSTRACT LIST OF TABLES LIST OF FIGURES 1. 1.1 LITERATURE REVIEW INTRODUCTION 1.1.1 Definition 1.1.2 Composition 1.1.3 Classification 1.1.3.1 Weathering Steels 1.1.3.2 Control Rolled Steels 1.1.3.3 Pearlite Reduced Steel 1.1.3.4 Acicular Ferrite Steel 1.1.3.5 Dual Phase Steel 1.1.3.6 Micro-Alloyed Steel 1.1.4 Properties 1.1.5 Specifications 1.1.6 Applications

8 9 9 10 10 10 10 11

11 12 14

1.2

DEVELOPMENT OF HSLA

15

1.2.1 Mechanism of Alloying 1.2.2 Effect of Alloying Elements on Properties of HSLA 1.2.2.1 Nitrogen 1.2.2.2 Manganese 1.2.2.3 Silicon 1.2.2.4 Copper 1.2.2.5 Phosphorus

15 16

1.2.2.6 Chromium 1.2.2.7 Nickel 1.2.2.8 Molybdenum 1.2.2.9 Aluminum 1.2.2.10 Vanadium 1.2.2.11 Titanium 1.2.2.12 Zirconium 1.2.2.13 Boron 1.2.2.14 Calcium

1.3

STRENTHENING MECHANISM OF HSLA 1.3.1 Grain Refinement 1.3.2 Solid Solution Strengthening 1.3.3 Phase Balance Strengthening 1.3.4 Precipitation Strengthening 1.3.5 Work Hardening

21 21 23 25 28 32

1.4

EFFECT OF GRAIN SIZE ON PROPERTIES OF HSLA 1.4.1 Measurement of ASTM Grain Size Number 1.4.1.1 Comparison Method 1.4.1.2 Grain Counting Method 1.4.1.3 Intercept Method 1.4.2 Importance of Grain Size

33 33

34

2. 2.1

EXPERIMENTATION SAMPLE PREPARATION 2.1.1 Sectioning 2.1.2 Mounting 2.1.3 Coarse Grinding 2.1.4 Medium and Fine Grinding 2.1.5 Mechanical Polishing 2.1.6 Etching

38 38 38 38 39 39 40 41
6

2.2

MICROSCOPIC ANALYSIS

42

2.3

HARDNESS TESTING

42

2.4

HEAT TREATMENT

43

2.5

RETESTING

43

3.

RESULTS AND DISCUSSION

44

CONCLUSION

45

REFRENCES

46

ABSTRACT

Structural steels with a ferrite-pearlite microstructure are widely used in civil, mechanical and chemical engineering. Increased working loads, reliability requirements, extreme temperature and chemically aggressive environments lead to an increased demand for high strength, combined with high toughness, in these steels. The use of welding as a joining method requires good weldability, for which the carbon content in a steel composition should be decreased. A decrease in carbon content results in strength decrease, due to a decrease in the amount of the second phase (pearlite).

To overcome this strength drop, additions of titanium, niobium and vanadium microalloying elements, in amounts no more than 0.15 wt%, have been used to provide precipitation strengthening and grain size refinement. Thus, during the last thirty years high strength low alloy (HSLA) structural steels have found widespread use in automotive, construction and pipe-line transportation industries.

The aim of the present project is to study the influence of steel chemistry on grain size as well as to establish a study of effect of grain size on the mechanical properties of High Strength Low Alloy Steels. To bring about the above study, various literatures were surveyed and related information was gathered. An experiment was also conducted on HSLA steel sample in which the sample was subjected to various heat treatments to bring about change in its grain size and hardness testing was done on the heat treated samples so as to establish a relationship between grain size and hardness.

LIST OF TABLES
S. No. 1 2 3 4 5 6 7 8 9 TABLE NAME Typical composition of HSLA steel SAE HSLA Steel Grade composition SAE HSLA Steel Grade Mechanical properties Experimental value for stress and Ky terms in Hall-Petch equation Strengthening coefficient for a no. of solutes Increment of yield stress from the micro alloying element precipitation Effect of grain size on properties of HSLA Composition of HSLA Sample Under Study Results obtained from experimentation Pg. No. 10 12 13 22 24 31 37 38 44

LIST OF FIGURE
S. No. 1 2 3 4 5 6 7 8 9 10 Fe-Mn Phase Diagram Fe-Si Phase Diagram Fe-Cr Phase Diagram Fe-Ni Phase Diagram Fe-Ti Phase Diagram Strengthening effects of substitutional solute atoms in iron Factors contributing to the strength of C-Mn Steels Effect of pearlite on work hardening rate Influence of carbon content on strength of plain carbon steel Influence of 50% transformation temperature on tensile strength via formation of different steel structures Strengthening contributions of different parameters on yield strength of hot-rolled Addition to strength predicted by Orowan and Ashby-Orowan 12 equations compared with the observed increments of yield strength in micro alloyed steels (vertical lines are experimental data)]
9

FIGURE

Pg. No. 16 17 18 19 20 24 25 26 26 28

11

29

30

CHAPTER 1: LITERATURE REVIEW

1.1: INTRODUCTION
1.1.1 Definition High-strength low-alloy steel (HSLA) is a type of alloy steel that provides better mechanical properties or greater resistance to corrosion than carbon steel. They have carbon content between 0.050.25% to retain formability and weldability. Other alloying elements include up to 2.0% manganese and small quantities of copper, nickel, niobium, nitrogen, vanadium, chromium, molybdenum, titanium, calcium, rare earth elements, or zirconium. These steel alloys provide increased strength-to-weight ratios over conventional low-carbon steels for only a modest price premium. Because HSLA alloys are stronger, they can be used in thinner sections, making them particularly attractive for transportation-equipment components where weight reduction is important.

1.1.2 Composition Typically, HSLA steels are low-carbon steels with up to 1.5% manganese, strengthened by small additions of elements, such as columbium, copper, vanadium or titanium and sometimes by special rolling and cooling techniques. Improved-formability HSLA steels contain additions such as zirconium, calcium, or rare-earth elements for sulfide-inclusion shape control.

Table 1: Typical Composition of HSLA Steels

Element C Mn Nb V Mo

% Composition 0.06 -0.12 1.4 -1.8 0.02 -0.05 0 - 0.06 0.2-0.35

10

1.1.3 Classification 1.1.3.1 Weathering Steel: Steels which have better corrosion resistance. A common example is COR-TEN. 1.1.3.2 Control Rolled Steel: Hot rolled steels which have a highly deformed austenite structure that will transform to a very fine equiaxed ferrite structure upon cooling. 1.1.3.3 Pearlite Reduces Steel: Low carbon content steels which lead to little or no pearlite, but rather a very fine grain ferrite matrix. It is strengthened by precipitation hardening. 1.1.3.4 Acicular Ferrite: These steels are characterized by a very fine high strength acicular ferrite structure, a very low carbon content, and good hardenability. 1.1.3.5 Dual Phase Steel: These steels have a ferritic microstructure that contains small, uniformly distributed sections of martensite. This microstructure gives the steels low yield strength, high rate of work hardening, and good formability. 1.1.3.6 Micro Alloyed Steel: Steels which contain very small additions of niobium, vanadium, and/or titanium to obtain a refined grain size and/or precipitation hardening.

1.1.4 Properties The added elements are intended to alter the microstructure of plain carbon steels, which is usually a ferrite-pearlite aggregate, to produce a very fine dispersion of alloy carbides in an almost pure ferrite. This eliminates the toughness-reducing effect of a pearlitic volume fraction, yet maintains and even increases the material's strength by precipitation strengthening and by refining the grain size, which in the case of ferrite increases yield strength by 50% for every halving of the mean grain diameter. Its yield strength can be anywhere between 250-590 MPa (35000-85000 psi).

HSLA steels are also more resistant to rust then most carbon steels. Although the material quickly becomes covered with surface rust, this is superficial and rust takes a long time to threaten the integrity of a structure made from the material. HSLA steels usually have densities of around 7800 kg/m3.
11

1.1.5 Specification According to the Society of Automobile Engineers, the Standard Steel Grade Compositions for HSLA are as follows:

Table 2: SAE HSLA steel grade compositions % Grade Carbon (max) 0.21 % Manganese (max) 1.35 % Phosphorus (max) 0.04 % Sulfur (max) 0.05 % Silicon (max) 0.90 Niobium or vanadium treated Notes

942X 945A 945C 945X 950A 950B 950C 950D 950X 955X 960X 965X 970X 980X

0.15 0.23 0.22 0.15 0.22 0.25 0.15 0.23 0.25 0.26 0.26 0.26 0.26

1.00 1.40 1.35 1.30 1.30 1.60 1.00 1.35 1.35 1.45 1.45 1.65 1.65

0.04 0.04 0.04 0.04 0.04 0.04 0.15 0.04 0.04 0.04 0.04 0.04 0.04

0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05

0.90 0.90 0.90 0.90 0.90 0.90 0.90 0.90 0.90 0.90 0.90 0.90 0.90 Niobium or vanadium treated Niobium, vanadium, or nitrogen treated Niobium, vanadium, or nitrogen treated Niobium, vanadium, or nitrogen treated Niobium, vanadium, or nitrogen treated Niobium, vanadium, or nitrogen treated Niobium or vanadium treated

12

Table 3: SAE HSLA steel grade mechanical properties Grade 942X Form Plates, shapes & bars up to 4 in. Sheet & strip Plates, shapes & bars: 945A, C 00.5 in. 0.51.5 in. 1.53 in. 945X Sheet, strip, plates, shapes & bars up to 1.5 in. Sheet & strip Plates, shapes & bars: 950A, B, C, D 00.5 in. 0.51.5 in. 1.53 in. 950X Sheet, strip, plates, shapes & bars up to 1.5 in. Sheet, strip, plates, shapes & bars up to 1.5 in. Sheet, strip, plates, shapes & bars up to 1.5 in. Sheet, strip, plates, shapes & bars up to 0.75 in. Sheet, strip, plates, shapes & bars up to 0.75 in. Sheet, strip & plates up to 0.375 in. 50,000 (345) 45,000 (310) 42,000 (290) 50,000 (345) 70,000 (483) 67,000 (462) 63,000 (434) 65,000 (448) 45,000 (310) 42,000 (290) 40,000 (276) 45,000 (310) 50,000 (345) 65,000 (448) 62,000 (427) 62,000 (427) 60,000 (414) 70,000 (483) Yield strength (min) [psi (MPa)] 42,000 (290) 45,000 (310) Ultimate tensile strength (min) [psi (MPa)] 60,000 (414) 60,000 (414)

955X

55,000 (379)

70,000 (483)

960X

60,000 (414)

75,000 (517)

965X

65,000 (448)

80,000 (552)

970X 980X

70,000 (483) 80,000 (552)

85,000 (586) 95,000 (655)

13

1.1.6 Applications Improved-formability HSLA steels were developed primarily for the automotive industry to replace low-carbon steel parts with thinner cross-section parts for reduced weight without sacrificing strength and dent resistance. Typical passenger-car applications include door-intrusion beams, chassis members, reinforcing and mounting brackets, steering and suspension parts, bumpers, and wheels. Trucks, construction equipment, off-highway vehicles, mining equipment, and other heavy-duty vehicles use HSLA sheets or plates for chassis components, buckets, grader blades, and structural members outside the body. For these applications, sheets or light-gage plates are specified. Structural forms (alloys from the family of 45,000 to 50,000-psi minimum yield strength HSLA steels) are specified in applications such as offshore oil and gas rigs, single-pole power-transmission towers, railroad cars, and ship construction. In equipment such as power cranes, cement mixers, farm machinery, trucks, trailers, and power-transmission towers, HSLA bar, with minimum yield strengths ranging from 50,000 to 70,000 psi is used. Forming, drilling, sawing, and other machining operations on HSLA steels usually require 25 to 30% more power than do structural carbon steels.

14

1.2: DEVELOPMENT OF HIGH STRENGTH LOW ALLOY STEELS

1.2.1 Mechanism of alloying Chemical compositions for the HSLA steels are specified by ASTM standards. The principal function of alloying elements in these ferrite-pearlite HSLA steels, other than corrosion resistance, is strengthening of the ferrite by grain refinement, precipitation strengthening, and solid-solution strengthening. Solid-solution strengthening is closely related to alloy contents, while grain refinement and precipitation strengthening depend on the complex effects of alloy design and thermo-mechanical treatment. Alloying elements are also selected to influence transformation temperatures so that the transformation of austenite to ferrite and pearlite occurs at a lower temperature during air cooling. This lowering of the transformation temperature produces a finer-grain transformation product, which is a major source of strengthening. At the low carbon levels typical of HSLA steels, elements such as silicon, copper, nickel, and phosphorus are particularly effective for producing fine pearlite. Element such as, manganese and chromium, which are present in both the cementite and ferrite, also strengthen the ferrite by solid-solution strengthening in proportion to the amount, dissolved in the ferrite. In the presence of alloying elements, the practical maximum carbon content at which HSLA steels can be used in the as-cooled condition is approximately 0.20%. Higher levels of carbon tend to form martensite or bainite in the microstructure of as-rolled steels, although some of the higher-strength low-alloy steels have carbon contents that approach 0.30%. The required strength is developed by the combined effect of: Fine grain size developed during controlled hot roiling and enhanced by micro alloyed elements (especially niobium) Precipitation strengthening caused by the presence of vanadium, niobium, and titanium in the composition.

15

1.2.2 Effect of alloying elements on the properties of HSLA Steels

1.2.2.1 Nitrogen - Additions to high-strength steels containing vanadium are limited to 0.005% and have become commercially important because such additions enhance precipitation hardening. The precipitation of vanadium nitride in vanadium-nitrogen steels also improves grain refinement because it has a lower solubility in austenite than vanadium carbide.

1.2.2.2 Manganese -It is the principal strengthening element in plain carbon high-strength structural steels. It functions mainly as a mild solid-solution strengthener in ferrite, but it also provides a marked decrease in the austenite-to-ferrite transformation temperature. In addition, manganese can enhance the precipitation strengthening of vanadium steels and to a lesser extent, niobium steels.

[Figure-1: Fe-Mn Phase Diagram]

16

1.2.2.3 Silicon - One of the most important applications of silicon is its use as a deoxidizer in molten steel. Silicon has a strengthening effect in low-alloy structural steels. In larger amounts, it increases resistance to scaling at elevated temperatures. Silicon has a significant effect on yield strength enhancement by solid-solution strengthening and is widely used in HSLA steels for riveted or bolted structures.

1`.

[Figure-2: Fe-Si Phase Diagram] 1.2.2.4 Copper Cu in levels in excess of 0.50% also increases the strength of both low- and medium-carbon steels by virtue of ferrite strengthening, which is accompanied by only slight decreases in ductility. Copper can be retained in solid solution even at the slow rate of cooling obtained when large sections are normalized, but it is precipitated out when the steel is reheated to about 510 to 605C (950 to 1125F). At about 1% copper, the yield strength is increased by about 70 to 140 MPa regardless of the effects of other alloying elements. Copper in amounts up to 0.75% is considered to have only minor adverse effects on notch toughness or weldability. Copper precipitation hardening gives the steel the ability to be formed extensively and then precipitation hardened as a complex shape or welded assembly.

17

1.2.2.5 Phosphorous - The atmospheric-corrosion resistance of steel is increased appreciably by the addition of phosphorus, and when small amounts of copper are present in the steel, the effect of the phosphorus is greatly enhanced. When both phosphorus and copper are present, there is a greater beneficial effect on corrosion resistance than the sum of the effects of the individual elements.

1.2.2.6 Chromium -It is often, added with copper to obtain improved atmospheric-corrosion resistance.

[Figure-3 Fe-Cr Phase Diagram]

18

1.2.2.7 Nickel -It is often added to copper-bearing steels to minimize hot shortness.

[Figure-4 Fe-Ni Phase Diagram] 1.2.2.8 Molybdenum Mo in hot-rolled HSLA steels is used primarily to improve hardenability when transformation products other than ferrite-pearlite are desired. Molybdenum (0.15 to 0.30%) in micro alloyed steels also increases the solubility of niobium in austenite, thereby enhancing the precipitation of NbC(N) in the ferrite. This increases the precipitationstrengthening effect of NbC(N). 1.2.2.9 Aluminum It is widely used as a deoxidizer and was the first element used to control austenite grain growth during reheating. During controlled rolling, niobium and titanium are more effective grain refiners than aluminum.

1.2.2.10 Vanadium - It strengthens HSLA steels by both precipitation hardening the ferrite and refining the ferrite grain size. The precipitation of vanadium carbonitride in ferrite can develop a significant increase in strength that depends not only on the rolling process used, but also on the base composition. Carbon contents above 0.13 to 0.15% and manganese content of 1% or more enhances the precipitation hardening, particularly when the nitrogen content is at least 0.01%.
19

1.2.2.11 Titanium It is unique among common alloying elements in that it provides both precipitation strengthening and sulfide shape control. Small amounts of titanium (<0.025%) are also useful in limiting austenite grain growth. However, it is useful only in fully killed (aluminum deoxidized) steels because of its strong deoxidizing effects; the versatility of titanium is limited because variations in oxygen, nitrogen, and sulfur affect the contribution of titanium as carbide strengthened.

[Figure-5: Fe-Ti Phase Diagram] 1.2.2.12 Zirconium It can also be added to killed high-strength low-alloy steels to improve inclusion characteristics, particularly in the case of sulfide inclusions, for which changes in inclusion shape improve ductility in transverse bending. 1.2.2.13 Boron It has no effect on the strength of normal hot-rolled steel but can considerably improve hardenability when transformation products such as acicular ferrite are desired in low-carbon hot-rolled plate.

1.2.2.14 Calcium - Treatment with calcium is preferred for sulfide inclusion shape control.
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1.3: STRENGTHENING MECHANISM OF HSLA

Most HSLA steels are furnished in the as-hot-rolled condition with ferritic - pearlitic microstructure. The controlled-rolled steels with an acicular ferrite microstructure and the dual-phase steels with martensite dispersed in a matrix of polygonal ferrite show high strength. These two types of HSLA steels use the formation of eutectoid structures for strengthening, while the ferritic - pearlitic HSLA steels generally require strengthening of the ferrite. Pearlite is generally an undesirable strengthening agent in structural steels because it reduces impact toughness and requires higher carbon contents. Moreover, yield strength is largely unaffected by a higher pearlite content. Strengthening can be achieved by one or more of the following mechanisms: grain refinement, solid solution strengthening, phase balance strengthening, precipitation strengthening and work hardening. Of these only grain refinement results in higher toughness; the others reduce it. The precise mix of mechanisms used will depend on the specific application of the steel along with other properties such as weldability for construction steels, formability for further metal forming and machinability for engineering steels.

1.3.1 Grain refinement The main relationship between average ferrite grain size, d, and the yield stress in steels, y, is described by the Hall Petch equation:

y = 0 + kyd-1/2
where 0 and ky are constants. The constant 0, friction stress, represents the stress required to move free dislocations along the slip planes in the iron BCC crystal, and can be regarded as the yield stress of a single crystal. This stress is very sensitive to temperature and the chemical composition of the steel.

21

ky is determined from the slope of the line plot between y and d-1/2. It is found to be independent of temperature, chemical composition of the steel grade, and strain rate. Different authors have reported variable values for o and ky due to the different steel grades examined (Table 3). Reported ky values vary by 9%, which is within experimental scatter, but o varies by up to 4.5 times, which indicates a strong dependence of o on steel composition. The effects of elements in solution on the yield stress o can be represented as:

where I is the friction stress of iron, ci is a concentration of ith solute and ki is the strengthening coefficient of ith solute.

Table 4: Experimental values for stress and ky terms in Hall Petch Equation

22

Grain refinement is influenced by the complex effects of alloy design and processing methods. For example, the various methods of grain refinement used in the three different stages of hot rolling (that is, reheating, hot rolling, and cooling) include: The addition of titanium or aluminum to retard austenite grain growth when the steel is reheated for hot deformation or subsequent heat treatment The controlled rolling of microalloyed steels to condition the austenite so that it transforms into fine-grain ferrite The use of alloy additions and/or faster cooling rates to lower the austenite-to-ferrite transformation temperature.

1.3.2 Solid solution strengthening

The main interstitial elements in steel are carbon and nitrogen. Free carbon and nitrogen form interstitial atmospheres around the dislocations, which lead to dislocation immobilization and yield strength increase. However, the solubility of C and N in -iron is limited to 0.02 wt% for C at 723 0C and to 0.1 wt% for N at 590 0C decreasing to < 0.00005 wt% (C) and <0.0001 wt% (N) at 20 0C. Formation of cementite Fe3C and other alloy carbides and nitrides takes free carbon and nitrogen from the solution. Hence, the interstitial solute strengthening effect is limited.

Many metallic elements form substitutional solutions with iron. This also leads to an increase in strength through elastic straining of the iron matrix, which arises from the size mismatch between the alloying element and iron atom (Hume-Rothery effect). With an increase in solute element content strength usually increases (Figure 1). In addition to elastic strain, substitutional solute elements also influence the grain size, amount and interlamellar spacing of pearlite, and the free content of carbon and nitrogen. Thus the negative influence of Cr on strength (Figure 1) can be explained by its removal of free N from solution as chromium nitride.

23

Figure 6: Strengthening effects of substitutional solute atoms in iron.

Strengthening coefficients for various alloying elements can be found in the literature, Table 4, and incorporated into the Hall-Petch equation as:

Table 5: Strengthening coefficients for a number of solutes

Generally, solid solution strengthening is used with other mechanisms as it is limited by solubility limits and other property requirements, such as toughness and formability.

24

1.3.3 Phase Balance Strengthening

The microstructure of steels often consists of several phases. In plain carbon steels the predominant phase is ferrite with pearlite being the commonest second phase. Apart from these phases in alloyed carbon steels, carbides, nitrides, carbo-nitrides and intermetallic compounds of alloying elements may be present. These phases also influence strength. Increased hardenability and/or cooling may replace pearlite by bainite or martensite, which provides increased strength.

For C-Mn steels, increase in carbon content leads to an increase in pearlite content, and, at constant Mn content, an increase in tensile strength (Figure 2), which is due to a faster work hardening rate (Figure 3). The influence of carbon on the yield stress is not so high (Figure 4). At constant carbon content, an increase in Mn (-stabiliser) content lowers the eutectoid composition of carbon increasing the pearlite proportion, whilst Mn itself contributes to strength via solid solution strengthening and grain refinement.

Figure 7: Factors contributing to the strength of C-Mn Steels.

25

Figure 8: Effect of pearlite on work hardening rate

Figure 9. Influence of carbon content on strength of plain carbon steel In the literature there are several empirical equations derived for various mechanical properties to extend the Hall-Petch and solid solution equation. An example for ferrite-pearlite steels containing up to 0.2 wt% C (pearlite content of about 25-30%) is as follows:

26

where

t ITT

- ultimate tensile strength, - impact transition temperature and cMn , cSi , cN ,

cpearlite - weight percent of Mn , Si , free soluble N and pearlite percentage respectively.

The strength of pearlite is influenced by its interlamellar spacing in a similar way to the Hall-Petch equation for ferrite structures:

Here p is the yield stress of pearlite and s is the ferrite path in the pearlite structure. For the twophase steels with more than 25% pearlite the Rule of Mixtures can be used to give mechanical properties as:

where f is the volume fraction of ferrite, p is the pearlite colony size and t is the carbide lamella thickness.
27

Fast cooling from the austenite field restricts carbon diffusion, which results in bainite and/or martensite formation instead of pearlite (Figure 5). Strength increase due to phase balance change depends on carbon content, and the tensile strength may reach 1600 MPa in bainite and to 2000 MPa in martensite. At the same time increase in carbon content reduces weldability and formability due to reduced toughness.

[Figure 10: Influence of 50% transformation temperature on tensile strength via formation of different steel structures]

1.3.4 Precipitation strengthening Precipitation strengthening occurs from the formation of finely dispersed carbonitrides developed during heating and cooling. Because precipitation strengthening is generally associated with a reduction in toughness, grain refinement is often used in conjunction with precipitation strengthening to improve toughness. Precipitation strengthening is influenced by the type of carbonitride, its grain size, and, of course, the number of carbonitrides precipitated.

28

Addition of strong carbonitride formers, e.g. Ti, Nb and V, leads to an increase in strength (Figure 6). Precipitation strengthening, which arises from the dislocation-particle interactions during slip, can be described by the Orowan equation:

where G is shear modulus, b is Burgers vector and L is the spacing between the particle centers. L is related to the particle volume fraction (f) and particle diameter (X) by:

which gives:

[Figure 11: Strengthening contributions of different parameters on yield strength of hot-rolled 0.1% C-0.2% Si-1.4% Mn steel containing either 0.04% Nb or 0.04% Nb-0.07% V [71]: is precipitate strengthening.]
29

Assuming a random distribution of particles the addition to the yield stress from precipitation can be calculated using the Ashby-Orowan equation:

where, X is in m.

The comparison between the last equation and experimental data for Nb- and V-alloyed steels showed that, for the particles larger than 5 nm and with 0.003 0.0015 volume fraction, the AshbyOrowan equation gives a better prediction than the Orowan equation (Figure 7), due to the use of an effective spacing in the Ashby-Orowan equation not the minimum spacing, as in the Orowan model.

[Figure 12. Addition to strength predicted by Orowan and Ashby-Orowan equations compared with the observed increments of yield strength in micro alloyed steels (vertical lines are experimental data)]

More complex modifications of the Orawan equation have been developed by Melander for a random distribution of hard, spherical particles.

30

where = Poissons ratio,

lr = is average distance between obstacle centers in the glide plane, Dg = geometrical mean particle diameter. This equation has been found to give values within 2 11 % of experimental data for small (3-5 nm diameter) VC particles with volume fractions from 0.0033 0.0316, but, as the particle size increases, the Ashby-Orowan equation again becomes more suitable.

In general, all the shown equations indicate, that greater strengthening results from greater volume fractions of finer particles, which depend on composition and processing. The strength increase for various microalloyed steels have been reported between 40 and 150 MPa (Table 5).
Table 6: Increment to the yield stress from the microalloying

elements precipitation

31

1.3.5 Work hardening In the absence of recrystallisation, an increase in dislocation density results in an increase in yield stress, however toughness and ductility may decrease. An increase in the shear stress can be represented by:

where, * describes the dislocation interactions with the short range obstacles and i - with the long range obstacles :

Where V H0 k T l m A

- Activation volume - Activation enthalpy at = 0 - Boltzmanns constant, -Temperature - Length of dislocation line activated - Strain rate - Mobile dislocation density -Area of glide plane covered by dislocation -Frequency of vibration of dislocation line length -Constant -Shear modulus -Dislocation density.

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4: EFFECT OF GRAIN SIZE ON PROPERTIES OF HSLA

1.4.1 Measurement of ASTM Grain Size Number The microstructural quantity known as the ASTM Micro Grain Size Number, n, is defined by the following relationship: N=2n-1 Where N is the number of grains per square inch, measured at a magnification of 100x. The most common method for measuring the values of n are: 1.4.1.1 Comparison Method: This is the simplest yet least quantitative method and is described in section 8 of ASTM E112. The overall appearance of the microstructure is simply compared with a standard set of micrographs or plates for which the ASTM Grain size number has been determined. Because the comparison of grain structure may be influenced by the overall type of microstructure, four standard categories of grain size plates are used for comparison. Plate 1: Untwined grains flat etch at100X. Includes grain size numbers 00, 0,,0.5,1,1.5,2,2.5,3,3.5,4,4.5,5,5.5,6,6.5,7,7.5,8,8.5,9,9.5, and 10

Plate2: Twinned grains flat-etch at 100X. Includes grain size numbers 1,2,3,4,5,6,7, and 8

Plate 3: Twinned grains contrast-etch at 75X. Includes nominal grain boundary diameters of 0.2, 0.15, 0.12, 0.09, 0.07, 0.06, 0.05, 0.045, 0.035, 0.025, 0.020, 0.015, 0.010 and 0.005mm.

Plate 4: Austenitic grains in steel at 100X Includes grain size number 1,2,3,4,5,6,7, and 8.

33

1.4.1.2 Grain Counting Method:

The number of grains per unit is counted directly .The ASTM grain size number is then determined according to the definition. An example of grain counting method is the planimetric procedure also known as Jeffries method.

Inscribe a circle (or other shape) of known area, A, on image of magnification, M. Count the number of grains that are completely within area. Count the number of grains that are partially within the area. Divide the result from (c) by 2 Add the result from (d) to the result from (b). Divide the result from (f) to grains/in @ 100X.

1.4.1.3 Intercept Method:

The number of grain boundary intercepts per unit test line is measured. This is a measure of grain boundary area per unit volume and is, therefore, related to grain size. An example of an intercept method is the linear intercept procedure also known as the Heyn Method. The basic steps to procedure are given here: On a single field of view randomly place one or more straight lines known as combined total length L. Count the total number intercepts, P, between the test lines(s) and the grain boundaries. Triple junction count as 1.5. If P < 50 use additional lines. Divide the number of intercepts, P, obtained from (b) by the total length L. Repeat (a-c) for 2-4 additional fields of view. Obtained P as the average of the result from (c) for all fields of view. The ASTM Grain size Number is given by n= -3.3 + 6.65 log10 (PL) where PL is given in mm-1.

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1.4.2 Importance of Grain Size

For applications at or around the normal temperatures, fine grained steels are preferred over coarse grained steels as fine grained steels have better impact resistance (toughness) for corresponding hardness and strength .The coarse grains raise the ductile to brittle transition temperature.

One of the significant effects is that fine grains improve the strength considerably. Modern steel maker changes the ferrite grain size of mild steel from d-1/2 =2, i.e., d=0.25 mm to d-1/2 =20, i.e., d=0.0025mm, and thus, raises yield strength from 100 MNm-2 to 500 MNm-2. Thus, achieving grain size in the range of 2-10 microns is extremely worthwhile. This has led to wide spread use of HSLA (High strength low alloy) steels having (addition of NB=0.05-0.09%) with yield strengths in range 290-550 MPa and tensile strength in the range of 415-700 MPa.

Grain boundaries act as obstacles to dislocation motion. Fine grains have large grain boundary area. Dislocation moves only a short distance before meeting a grain boundaries and thus increases the strength. In a large grain, the pile up of dislocation contains large number of dislocations, which in turn causes higher stress concentration in the nearing grains to cause slip there.

The shear stress, at the head of dislocation piled of is equal to nt, where n= no. of dislocation involved and t is shear stress on the slip plane. Thus coarser the grain size higher is stress concentration, easier it is to propagate the yielding process.

Hardenability of coarse grain steel is more as martensite forms easily. Coarse grain austenite transform to coarse plate martensite, which is undesirable as it more brittle and a bit less hard. The low carbon martensite (i.e. the lath martensite) has higher yield strength as austenite grain size decreases. Lathe martensite forms a packet, where the packet is effectively a grain. The packet size decreases with the decrease of parent austenitic grain size, thus the strength of lathe martensite may be related with either the packet size or directly with the parent austenitic grain size.

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There is a direct relationship between austenite grain size and the grain size of the nucleation best transformation products. That is finer the austenite grain finer is the grain size of the ferrite-cementite products and vice versa. The annealed or normalize low carbon steel

(predominantly feritic) show increase in strength and toughness with the decrease in grain size of austenite as it results in smaller ferritic grain size too.

Even the fine-grained hardened and tempered steel has impact toughness several times that of coarse grained steel of same grade. Probably, the impurity atoms like Sb, P, Sn, As, co segregate more in coarse grained steel, because of smaller grain boundary area to produce easily intergranular fracture. In slowly cooled hypo eutectoid steels, free ferrite is able to form continuous network along coarse grained steels, which leads to lower impact value, lower elastic ratio and lower elongation. Ms Temperature of Fe-Ni and Fe-Ni-C alloys decreases significantly as austenite grain size decreases, probably due to higher strength of fine grained austenite, which shows greater shear resistance to transformation of austenite to martensite.

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Table 7: Effect of Grain Size on the Properties of HSLA PROPERTY Yield strength Tensile strength Hardness Ductility Toughness Resilience Hardeniability Depth of carburizing Machinability after normalizing Surface finish Orange peel effect Corrosion resistance Creep resistance above equi-cohesive temp. Creep resistance below equi-cohesive temp. Retained austenite Fatigue resistance Work-hardening exponent Strain-rate sensitivity Tendency to quench crack formation Segregation Anisotropy of properties Dispersion of inclusion and micro-porosity Response to heat treatment Possibility of soft-spots in hardening COARSE Less Less Less More Less Less More Deep case More Less More More More Less More Less Less Less More More More Less Less Less GRAIN FINE GRAIN More More More Less More More Less Shallow case Less More Less Less Less More Less More More More Less Less Less More More More

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CHAPTER 2: EXPERIMENTATION
Experiments were carried out to find the relation between grain size of sample and mechanical properties. Hardness testing of the sample was carried out in this regard. The chemical composition of the sample used is as follows:

Table 8: Composition of HSLA Sample Under Study Carbon 0.147 Chromium 0.011 Manganese 1.13 Niobium 0.035 Sulphur 0.028 Vanadium 0.043 Molybdenum 0.002 Titanium 0.003 Phosphorus 0.016 Arsenic 0.002 Silicon 0.2 Tin 0.003 Nickel 0.005 Aluminium 0.025

The steps followed in sample testing are as follows:

2.1 SAMPLE PREPRATION

2.1.1 Sectioning

The sample used was available in the form of a small billet of dimension 1.5cm X 1.5cm X 10cm. For experimental purpose, the sample was cut into pieces of 1.5cm X 1.5cm X 1cm. This was carried out by cutting the sample on a bench vice with the help of hand hacksaw.

2.1.2 Mounting

Small samples are generally mounted for convenience in handling and to protect the edges of the specimen being prepared. Cold mounting of the sample was carried out using following supplies: - ColdMound Kit (Geologists Syndicate Pvt. Ltd., Kolkata). - Plastic mounting ring with open bottom. - Lubricant oil. - Glass Plate.

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The steps involved are as follows: 1. Apply lubricant oil to the inner walls and base of the mounting ring. 2. Place the specimen on the glass plate with the examination surface facedown. 3. Place the mounting ring cylinder on the glass plate so that the sample is at the center of ring base. 4. Mix the appropriate amount of cold Mount (2/1 Powder/Liquid) in a paper cup. 5. Simply pour the epoxy mixture into the mounting ring. 6. After half hour, remove the sample from the mounting ring and proceed with course grinding.

2.1.3 Coarse Grinding

In view of the perfection required in an ideally prepared metallographic sample, it is essential that each preparation stage be carefully performed. The specimen must: 1. Be free from scratches, stains and others imperfections which tend to mark the surface. 2. Retain non-metallic inclusions. 3. Reveal no evidence of chipping due to brittle intermetallic compounds and phases. 4. Be free from all traces of disturbed metal.

The purpose of the coarse grinding stage is to generate the initial flat surface necessary for the subsequent grinding and polishing steps. As a result of sectioning and grinding, the material may get cold worked to a considerable depth with a resultant transition zone of deformed material between the surface and the undistorted metal. Coarse grinding can be accomplished either wet or dry using electrically powered grinding belt, but care must be taken to avoid significant heating of the sample. The final objective is to obtain a flat surface free from all previous tool marks and cold working due to specimen cutting. An important factor throughout the Coarse Grinding and Fine Grinding Stages is that the scratches be uniform in size and parallel to each other in any one grinding stage. Proper grinding involves rotation of the sample by 90o between stages while the grinding angle must be held constant during the grinding at any one stage.

2.1.4 Medium and Fine Grinding

Medium and fine grinding of metallurgical samples are closely allied with the coarse grinding which precedes them. Each stage of metallographic sample preparation must be carefully performed; the
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entire process is designed to produce a scratch free surface by employing a series of successively finer abrasives.

The idea is to carefully move from one stage to the next where the abrasives become finer at each successive stage. Movement from one stage to the next should only proceed when all of the scratches from the preceding stage are completely removed. In general, successive steps are 240, 320, 400 and 600 grit SiC and the grinding rate should steadily decrease from one stage to the next.

For the experimentation process, the medium and fine grinding was carried out in a double disc polishing machine, the specifications of which are as follows: Make Model Max. Speed : : : Presi, Grenoble, France. Minitech 265 700 rpm

2.1.5 Mechanical Polishing

Polishing involves the use of abrasives, suspended in a water solution, on a cloth-covered electrically powered wheel. Diamond abrasives provide the best, and most expensive, compounds utilized in polishing; standard sized aluminum oxide powders are applied for general use purposes. Following the final 600 grit fine-grinding stage, the sample must be washed and carefully dried before proceeding to the first polishing stage. At the polishing stages, even hard dust particles in the air which settles on the polishing cloth can cause unwanted scratching of the specimen. Careful washing of the specimen and the operator's hands must be carried out prior to each stage of polishing. Beginning with suspended aluminum oxide particles (suspended in water) on a Nylon-cloth, the final fine-grinding surface layer resulting from the previous grinding procedure should be completely removed with a rotation rate of 300 rpm.

The specimen is initially held at one position on the wheel, without rotation, until most of the previous grinding marks are removed. It can be rotated slowly, counter to the wheel rotation, until only scratches from the aluminum oxide are visible. During the initial polishing stage, moderate pressure can be applied to the specimen and the entire stage should generally take 1 or 2 minutes.

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After proper polishing, specimen should have a mirror-like surface free of scratches. During final polishing, minimal pressure should be applied and time should be kept to a minimum since the napped material will conform to the specimen shape under pressure.

The wetness of the cloth used for Final Polishing has a great influence on the end result. If the cloth is too wet the sample will show pits; if too dry, buffing and/or smearing will result. To determine the proper wetness, the sample should be removed from the wheel and the time required for the polishing film to dry (five to eight seconds) should be checked. A thin opaque film indicates that sufficient abrasive is present. For precision work, extremely fine grades of diamond abrasives are used for the final polishing sequence.

2.1.6 Etching

Microscopic examination of a properly polished, unetched specimen will reveal only a few structural features such as inclusions and cracks or other physical imperfections. Etching is used to highlight, and sometimes identify, microstructural features or phases present. Even in a carefully prepared sample, a surface layer of disturbed metal, resulting from the final polishing stage, is always present and must be removed. Etchants are usually dilute acid or dilute alkalis in water, alcohol or some other solvent. Etching occurs when the acid or base is placed on the specimen surface because of the difference in rate of attack of the various phases present and their orientation. The etching process is usually accomplished by merely applying the appropriate solution to the specimen surface for several seconds to several minutes. Nital, a Nitric Acid - Alcohol mixture, is the etchant commonly utilized with common irons and steels. Nital is dripped onto the specimen using an eye-dropper or cotton swab. Ten seconds to one minute is usually sufficient for proper etching depending on sample and nital concentration. The sample is immediately washed under running water, rinsed with alcohol and dried in an air blast. Dry off the rinsing alcohol on the specimen with the air blast and then move on to the microscopic examination stage.

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2.2 MICROSCOPIC EXAMINATION

Initial microscopic viewing should be done utilizing a stereomicroscope, which reveals a threedimensional scanning of the specimen surface. The specimen is placed on the stage of the microscope so that its surface is perpendicular to the optical axis.

Detailed viewing is done with a metallurgical microscope. A metallurgical microscope has a system of lenses (objectives and eyepiece) so that different magnifications (25X to 1000X) can be achieved. The important characteristics of the microscope are: (1) magnification, (2) resolution and (3) flatness of field. The resultant magnification is the product of the magnifying power of the objective and that of the ocular.

The grain size of the samples is measured after microscopic analysis by metallurgical microscope. The grain size is measured using the Image Analyzer software by using the Grain Size Measurement Option.

The specifications of the metallurgical microscope used are as follows: Make Software Used Max. Magnification Obtainable : : : Metal Power India Ltd. Image Analyzer 1000X

2.3 HARDNESS TESTING

Hardness of the sample was tested by using the Digital Hardness Testing Machine (Vaishshaikha Electron Devices, Ambala). The indenter used in this regard was a ball indenter with the ball diameter of 1/16 inch. The initial test force was of 98.01 N that was applied to hold the specimen in position. A further load of 980.7 N was applied to obtain a hardness in HRB Scale. The tolerance limit of the said machine is of 2.0%.

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2.4 HEAT TREATMENT

Heat treatment of the samples was done to alter the grain size of the samples. The knowledge about the type of treatment required to obtain a certain grain size was known by going through a number of research papers. Although the exact treatment could not be specified, a tentative treatment schedule was designed for different samples by the project guide. The following heat treatment was carried out:

All the samples were heated in a muffle furnace to a temperature of 900C. On reaching the desired temperature, the furnace was kept on hold at the same temperature for about 30 minutes. Sample 1 was then cooled in the furnace itself. Sample 2 was given a faster cooling rate by cooling in air. Sample 3 was cooled in mobile oil and sample 4 was cooled in ice cold water.

2.5 RETESTING
The grain size and hardness of the samples were tested again after the heat treatment process and the results obtained have been discussed.

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CHAPTER 3: RESULTS AND DISCUSSIONS

The results obtained are as follows: Table 9: Result Obtained After Treatment S. No. 1 2 3 4 5 Type of Treatment Untreated Furnace Cooled Air Cooled Oil Cooled Water Quenched Grain Size* 13.0 10.7 10.3 5.43 3.48 Hardness HRB 92.3 HRB 71.7 HRB 82.1 HRB 75.7 HRB 72.7

*As tested by Image Analyzer Software.

From the literature reviews, it can be concluded that the hardness keeps on increasing as the grain size decreases. The change in hardness, however, is not only a function of grain size but result of various factors like composition of sample, microconstituents, etc. Studies have shown that a moderate cooling rate forms acicular bainite whereas a faster cooling forms a mixed microstructure with dispersed ferrite. This ferrite may be the reason for decrease in hardness of sample even though the grain size obtained is small in the last sample.

Again, the mechanical property changes may be a function of the action of alloying elements at higher temperature. Hence we can say that various factors need to be taken care of to have proper results for the effect of grain size on the properties of HSLA.

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CONCLUSION

As mentioned in previous pages, the need of high strength steels with good corrosion and oxidation resistance has increased in the recent years. This has lead to increase in research work in the field of high strength low alloy steels. The project report gives a brief idea as to how the alloying elements influence the microstructure and grain size of high strength low alloy steels. It can be concluded from the data mentioned in the above pages that the ferrite grain size decreases with an increase in micro alloying element content, due to Zener drag effect. Second phase (pearlite) content decreases with carbon content decrease in steel composition.

The above report also gives an idea of the effect of grain size on the mechanical properties of steel. It is found that the higher alloyed steels show a larger yield stress drop from plate to pipe, due to the higher Bauschinger effect.

Apart from grain size, the mechanical properties of HSLA also depend on a variety of other factors like composition of phases, distribution of phases, etc. Strength of HSLA steels is increased by: increasing the amount of pearlite increasing the fineness of the grains structure increasing the amount of hard precipitate. Further research work in this field can be carried out which will lead to a better idea about the effect of various manufacturing methods like rolling, forging, casting, etc. on the grain size and mechanical properties can be known. Also the effect of individual effect of alloying elements during heat treatment of samples can be known. This will lead to improved properties of HSLA and will result in increased fields of application of HSLA.

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REFERENCES
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10. T.Gladman, B.Holmes and I.D. McIvor, Effect of second-phase particles on strength, toughness and ductility, Effect of second-phase particles on the mechanical properties of steel, Proceedings of a conference, The Iron and Steel Institute, London, 1971. 11. H. Conrad, On the mechanism of yielding and flow in iron, Journal of Iron and Steel Institute, Vol. 198, Aug. 1961. 12. Vijendar Singh, Physical Metallurgy, Reprint 2011. 13. V. Raghvan, Physical Metallurgy, 2008. 14. William D. Callister, Jr., Material Science and Engineering, Reprint 2008. 15. George E. Dieter, Mechanical Metallurgy, SI Metric Edition. 16. Schindler , M. Janoec, E. Msteck, M. R.ika, L. .ek, L.A. Dobrzaski, S. Rusz, P. Suchnek, Effect of cold rolling and annealing on mechanical properties of HSLA steel, Archives of Materials Science and Engineering. 17. J. Zrnk, T. Kva_kaj, P. Hor_ak, V. Vrchovinsk, Acheivements in Mechanical and Materials Engineering, (Conference Proceeding), Polish Academy of Sciences. 46