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Aerospace Engineering. Aerospace Engineering Individual Investigative Project CASTING OF ALUMINUM 201 IN THE SEMI-SOLID STATE BY Latona Nahid Aktare Houssaine May 2012 Supervisors: Dr P. KAPRANOS Dissertation submitted to the University of Sheffield in partial fulfilment of the requirements for the degree of Bachelor of Engineering

Rheocasting of Aluminum 201

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The most prominent technique for the rheocasting of aluminium alloys [Semi-Solid Rheocasting (SSR)] has been dependent on the effectiveness of processing semi-solid slurries. Contraction due to solidification and compensation for shrinkage, pouring technique from the crucible to the mould cavity also dictates its effects on the final microstructures and therefore the mechanical properties. Six batches of rheocasting were performed at varied temperatures and stirred for different times and analysis to evaluate the solid fraction, particle density, particle size, particle shape factor, and particle distribution was performed on the resulting castings. This project examines the difficulties involved in Semi-solid rheocasting (SSR) of aluminum alloy and investigates the alternatives these difficulties could be overcome by refined techniques. The methodology employed in this case is the temperature dropped from the A3 melting point stirred at the required temperature hence poured in metal dies to study the evolution of the microstructure from dendrite to non-dendritic microstructure in its semi-solid state during the SSR process. To explore the success of SSR with an Al-Cu based alloy, the SSR samples were heat treated T6 and undergone tensile testing to achieve appropriate mechanical properties. Comparison in microstructures of naturally cooled and artificially aged samples (T6) were part of the study probing in the progression of the microstructures after homogenization.

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  • Aerospace

    Engineering.

    Aerospace Engineering

    Individual Investigative Project

    CASTING OF ALUMINUM 201 IN THE SEMI-SOLID

    STATE

    BY

    Latona Nahid Aktare Houssaine

    May 2012

    Supervisors: Dr P. KAPRANOS

    Dissertation submitted to the University of Sheffield in partial fulfilment of the

    requirements for the degree of

    Bachelor of Engineering

  • ~i~

    Abstract

    The most prominent technique for the rheocasting of aluminium alloys [Semi-Solid

    Rheocasting (SSR)] has been dependent on the effectiveness of processing semi-solid slurries.

    Contraction due to solidification and compensation for shrinkage, pouring technique from the

    crucible to the mould cavity also dictates its effects on the final microstructures and therefore

    the mechanical properties. Six batches of rheocasting were performed at varied temperatures

    and stirred for different times and analysis to evaluate the solid fraction, particle density,

    particle size, particle shape factor, and particle distribution was performed on the resulting

    castings. This project examines the difficulties involved in Semi-solid rheocasting (SSR) of

    aluminum alloy and investigates the alternatives these difficulties could be overcome by refined

    techniques. The methodology employed in this case is the temperature dropped from the A3

    melting point stirred at the required temperature hence poured in metal dies to study the

    evolution of the microstructure from dendrite to non-dendritic microstructure in its semi-solid

    state during the SSR process. To explore the success of SSR with an Al-Cu based alloy, the

    SSR samples were heat treated T6 and undergone tensile testing to achieve appropriate

    mechanical properties. Comparison in microstructures of naturally cooled and artificially aged

    samples (T6) were part of the study probing in the progression of the microstructures after

    homogenization.

  • ~ii~

    Table of Contents

    1. INTRODUCTION .................................................................................................... 1

    2. LITERATURE REVIEW .......................................................................................... 4

    2.1 History of Semi-Solid Metal Forming............................................................................................... 4

    2.2 Applications of SSM ......................................................................................................................... 5

    2.2.1 Aluminium-Copper Base Alloys (A201).................................................................................... 5

    2.3 Rheocasting Processes ....................................................................................................................... 6

    2.4 Structural Evolution during Rheocasting .......................................................................................... 7

    2.4.1 Grain Density ............................................................................................................................. 7

    2.4.2 Convection ................................................................................................................................. 8

    2.4.3 Dendrite Fragmentation .............................................................................................................. 8

    2.4.4 Particle Stability ......................................................................................................................... 9

    2.4.5 Fluidity of Rheocast Alloy ......................................................................................................... 9

    3. EXPERIMENTAL PROCEDURES........................................................................ 11

    3.1 Experimental Setup ......................................................................................................................... 11

    3.2 Stirring Rod ..................................................................................................................................... 11

    3.3 Microstructures................................................................................................................................ 11

    3.4 Hydrostatic Weighing ..................................................................................................................... 11

    3.5 Heat Treatment ................................................................................................................................ 12

    3.6 Tensile Testing ................................................................................................................................ 12

    3.7 Metallographic Etchants .................................................................................................................. 12

    3. EXPERIMENTAL FIGURES ................................................................................... 13

    3.1.1) Experimental Setup ..................................................................................................................... 13

    3.2.1) Conventional & SSR Experiment 1 ............................................................................................ 14

    3.3.1) SSR Experiment 2 ....................................................................................................................... 15

    3.4.1) SSR Experiment 3 ....................................................................................................................... 16

    3.5.1) Hydrostatic Machine ................................................................................................................... 17

    3.6.1) Tensile Testing Machine ............................................................................................................. 17

    3.5.1) Metallographic Etchants ............................................................................................................. 18

  • ~iii~

    3.5.1.1 Aluminium and Aluminium Alloys ........................................................................................... 18

    3.5.1.2 PREPARATION OF ALUMINUM ALLOYS ......................................................................... 18

    4. RESULTS AND DISCUSSION ............................................................................. 19

    4.1 Microstructures of 1st Experiment ................................................................................................... 19

    4.1.1 Microstructures of Conventional Castings ............................................................................... 19

    4.1.2 Microstructure of SSR Castings ................................................................................................... 20

    4.2 Microstructures of 2nd

    Experiment .................................................................................................. 21

    4.2.1 Microstructures of SSR Castings ............................................................................................. 21

    4.2.2 Evaluation of SSR Casting Particles ........................................................................................ 22

    4.3 Microstructures of 3rd

    Experiment................................................................................................... 23

    4.3.1 Microstructures of SSR Castings ............................................................................................. 23

    4.3.2 SSR Recrystallization Behaviour (T6 Heat-Treatment) ........................................................... 24

    4.4 Relative Densities Evaluation ......................................................................................................... 24

    4.5 Mechanical Properties of SSR Castings .......................................................................................... 25

    4. FIGURES OF A201.0 ALLOY .................................................................................. 26

    4.1.1) AA201.0 Alloy Conventional Sand Casting ............................................................................... 26

    4.1.2) Optical Microstructures at higher resolution .............................................................................. 27

    4.1.3) Conventional Sand Castings and SSR (Rheocasting) ................................................................. 28

    4.2.1) Semi-Solid Rheocasting (SSR) ................................................................................................... 29

    4.2.7) METALLOGRAPHY ANALYSIS ............................................................................................ 32

    4.3.1) Semi-Solid Rheocasting (SSR) ................................................................................................... 33

    4.3.2) Recrystallization Behaviour of SSR ........................................................................................... 35

    4.3.2.1 SSR Microstructures at T6 Conditions .................................................................................. 35

    4.4) POROSITY EVALUATION ......................................................................................................... 38

    4.5) MECHANICAL PROPERTIES .................................................................................................... 39

    4.6) MACROSCOPIC PHOTOGRAPHS ............................................................................................. 42

    5. CONCLUSIONS ................................................................................................... 44

    Summary of Findings: ........................................................................................................................... 44

    Suggested Further Work ........................................................................................................................ 45

    Suggested Manufacturing Configurations: ............................................................................................ 46

    6. REFERENCES ..................................................................................................... 48

  • ~iv~

    Acknowledgement

    I am sincerely and heartily grateful to my supervisor, Dr. Plato Kapranos, for the support and

    guidance he showed me throughout my final year project and dissertation work. His optimum

    level of expertise and assistance enabled me to develop the understanding of the subject. Im

    truly indebted for his time and devotion to the project notwithstanding the fact of his other

    academic and professional commitments.

    I would like to thank all the staff in the Department of Engineering Materials who gave me

    assistance during project, especially Mr Philip Staton for his help with the rheocasting process.

    I do thank all the colleagues in the rheocasting groups including scholars for the helpful

    analytical reviews, National Research University Project of Thailand.

    I also want to thank Mr. Sam Gascoyne for dedicating his time to facilitate my task in terms of

    etching the samples and demonstrating the apt techniques for polishing.

    Last but not least, I owe gratitude particularly to my parents and comrades for their continuous

    support and encouragement throughout my years of study.

  • ~1~

    1. INTRODUCTION

    Semi-solid metal processing in recent years has gained more commercial significance in the

    world of industrial applications. The needs to produce high quality parts at lower costs are the

    centre of attention in the global market. During die filling, from the manufacturing point of

    view, round and smaller crystal grains of less than 10 m [1] through a simple methodology of

    induced convection (by stirring of the molten metal before introducing it into the die) during

    solidification in order to improve the characteristics of metallic materials. Semi-Solid

    Rheocasting (SSR) is the process employed whereby the molten metal is vigorously agitated

    during solidification before being shaped into the final product. This process rips dendrite arms

    due to induced shear forces, creating a highly viscous material that has high fluidity even

    though over ~60% of the metal is solidified [2]. Desirable spheroidal microstructures are

    formed quickly and efficiently from the molten alloy at the liquidus. SSR creates the possibility

    to modify ordinary casting aluminium alloy such as A201 into semi-solid metal slurry with

    properties that are conducive to forming into complex shaped dies. This allows SSR to use

    conventional sand or die-casting to produce high-integrity, near-net-shape parts with strength

    and ductility comparable to squeeze or permanent mould cast components at highly reduced

    costs.

    The main objective of the semi-solid rheocasting (SSR) technique adopted herewith is to

    investigate the evolution of naturally cooled as well as artificially aged (heat treated T6)

    microstructures and obtain good mechanical properties. In order to characterize the early stages

    of the microstructures, the aluminium alloy A201 will be subjected to two different types of

    casting process:

    1) Conventional casting (gravity cast) and

    2) Semi-Solid Rheocasting (SSR), whereby analysis shall illustrate the breakdown of

    dendritic to near non-dendritic microstructures resulting in the desired fine near-

    spheroidal grains.

    After conventionally sand casting a batch of the 201 alloy, a set of five semi-solid rheocasting

    batches at different agitation times were cast to observe the development of the microstructures.

  • ~2~

    Subsequently, samples obtained through the SSR castings were heat treated, then machined and

    subjected to tensile testing, relating the mechanical properties of the material to the

    microstructures and possible defects resulting from the process.

    Experimentation on different convection approaches were explored in order to observe the

    microstructural behaviour of the Al-Cu alloy. As a result of fast growth of spheroidal of

    microstructures at lower temperature when subjected to convection, these factors contribute to a

    potentially significant reduction in operating cost when compared to conventional liquid casting

    process. The challenge of rheocasting has been the limited knowledge about how to efficiently

    process liquid alloy to create non-dendritic metal slurries whilst avoiding possible defects

    introduced by the stirring operation.

    Over the last 40 years, thixocasting process has been on the verge of establishing itself

    as an important route for manufacturing parts quality by the industry [3], making use of

    electromagnetically stirred billet as the starting feedstock, produced by continuous casters [4].

    Feedstock material for semi-solid processing (generally known as thixoforming) has a very

    particular non-dendritic structure that could be easily processed and manufactured into the

    desired shaped upon the reheating of the billet into the solid-liquid temperature range before

    forming into parts. However, poor estimated supply of the 3 inch diameter billets of the 2.7

    million tons of aluminium castings hoard produced by the Magnetohydrodynamic stirring

    (MHD) process, proved to be an Achilles heal for the thixoforming process in the North

    American, European and Japanese markets; these cost challenges almost extinguishing the

    current use of thixoforming in industry [5-6], with only few notable exceptions [7].

    Signs are that in order for current exploitation in semi-solid metal forming to succeed advances

    must be made in the rheocasting approach.

    Rheocasting has immediate advantages over thixocasting:

    1) Globule particles can be formed during solidification via applied convection; and

    2) High recyclability of scrap on site [8].

    Part quality remains the main aspect that is keeping the rheocasting process alive for industries

    that pin their hopes on this process. However, in order for rheocasting to become a viable

    worldwide industrial success, we need not only to understand and improve the initial stages of

    solidification when convection is induced but to have the ability to do this consistently and at a

    reduced cost.

  • ~3~

    The main aim of this study is to develop an understanding of how particle morphology in

    rheocast alloy evolves during the early stages of solidification and compare this to the existing

    literature. The results from various sets of experiments are then compared with published work

    on particle growth and mechanical properties obtained in the A201 alloy.

  • ~4~

    2. LITERATURE REVIEW

    2.1 History of Semi-Solid Metal Forming

    It all started back in the 1970s when SPENCER and FLEMINGS [9] at the MIT found that by

    mechanically agitating a solidifying alloy in the solid-liquid temperature range, the solid phase

    would be in the form of dendrite fragments turning into slurry of near-spherical particles in a

    liquid matrix. Their investigations into the nature of these semi-solid slurries revealed that they

    possessed unique rheological properties; they were thixotropic, i.e. they behaved like solids

    when left undisturbed but they flowed like liquids when put under shear and this effect was also

    time dependant. The thixotropic behaviour of the slurries allowed their formation into metal

    parts of complex shapes, and the higher viscosity associated with them considerably reduced

    the turbulent flow during mould filling, producing near net-shape products with better

    properties due to the reduction of air entrapment and other inclusions. As the non-dendritic

    feedstock microstructure became the key to this new process of metal forming, two semi-solid

    processing routes were quickly established in order to exploit the industrial platform:

    rheocasting and thixocasting. As the potential of this possible fruitful manufacturing route

    for shaping metal alloys was quickly recognised by Prof. M.C. Flemings and his co-workers

    they immediately moved to protect their IP and initiated the early development of semi-solid

    metal forming route (SSM) [10-11-21]. As already stated earlier, the initial industrial

    applications made use of the MHD feedstock production route by electromagnetically stirring

    the melt into a continuously cast slurry that solidified into non-dendritic feedstock. This

    feedstock could then be re-heated to the semi-solid state when needed and injected into a die

    under the appropriate conditions using a forming press. The main drawbacks of the process

    were the higher costs in feedstock production and the inability of the part manufacturers to

    recycle any scrap material. This lead to the parallel re-development of the original Rheocasting

    idea where slurries with dendrite structures disintegrate due to strong stirring agitation resulting

    into non-dendritic structures that can be formed into parts either in sequence or by solidifying

    and re-heating as required; the main difference here being the recyclability of materials. The

    semi-solid metal (SSM) processing has proven to be an interesting route and in some of its

    versions has gained commercial significance in the manufacturing world. However, it has never

  • ~5~

    fulfilled the early indications of its vast potential; it has remained an interesting but niche

    application process. Clearly the most important feature, and probably the factor that made the

    economics of the process more complicated, is the production and control of the non-dendritic

    microstructures throughout the feedstock. In order to attain the homogenization of

    microstructures and the elimination of segregation in a semi-solid alloy feedstock, many

    methods have been developed, such as NRC, SLC

    , SSR

    , rheo-die casting, rapid-

    Solidification and several more [12].

    There is clearly the potential of developing new methodology in terms of manufacturing cost

    effective quality parts such as cylinder engine blocks recently accomplished by Honda in line to

    be marketed in Europe [13-21], but the fact remains that semi-solid rheocasting has not yet

    established a firm foot hold in producing quality parts needed by todays industries on a large

    scale, although it has been successful in the areas of sports equipment & electronic consumer

    products [14].

    2.2 Applications of SSM

    2.2.1 Aluminium-Copper Base Alloys (A201)

    Fuel rising market prices and new environmental laws has resulted in a new drive towards

    lighter and more efficient vehicles providing impetus for possible SSM applications for

    aluminium parts in the automotive industry.

    Alloy 201 (Al-4.6Cu-0.7Ag-0.35Mn-0.35Mg-0.25Ti, wt%) [15] is a very competitive material

    developed for high mechanical properties, excellent machinability and can survive elevated

    temperatures as well as increase damage tolerance through better toughness. Table 1 illustrates

    the mechanical properties covered by the American Aerospace Material Specification AMS

    4229 [15].

    Table 1: Mechanical properties of A201 demonstrated by AMS.

    0.2% Proof Stress/

    MPa

    Tensile Strength/

    MPa

    Elongation/ %

    Separately Cast Specimen 345 414 3

    Designated Casting areas 345 414 3

    Non-designated casting areas 331 386 1.5

    [Courtesy of Casting Technology International][16]

  • ~6~

    This particular material has a high response to age hardening due to its main precipitate

    phase. The addition of silver in the material considerably changes the precipitation process,

    causing orthorhombic form of the tetragonal phase (Al2Cu) to precipitate as very thin,

    coherent plates on the matrix planes rather than plane [15-17]. Aluminium alloy

    has a known binary eutectic system upon solidification as shown in Figure 2.2.1. This eutectic

    reaction occurs during its non-equilibrium solidification phase nonetheless it could be removed

    after the homogenisation of the solute content (heated to a temperature below the eutectic

    temperature and held for a long time sometimes as much as 24hrs).

    Figure 2.2.1(a) & (b) shows alloys with composition (along line bold line) comprising the

    eutectic structure which constitutes layers of and phases. Higher eutectic composition in the

    alloy indicates significant amount of eutectic it contains. While the alloys on the right from

    point O mixture of and the eutectic grains.

    2.3 Rheocasting Processes

    Several processes for creating non-dendritic structures from liquid alloy have been developed.

    Mechanical stirring was the first method employed by SPENCER and FLEMINGS during their

    discovery of the non-dendritic structure [19]. More recently a new method was devised known

    as SLC as mentioned in section 2.1. In the new rheocasting process, liquid aluminium alloy is

    poured into a cooler steel cup at a temperature just above its liquidus. The interaction between

    the melt and cold cup results in the formation of many solid particles. Heat extraction is

    controlled to cool the volume of metal homogeneously. However, pouring at low temperature

    Figure 2.2.1(a): General Phase Diagram [18] Figure 2.2.1(b): Eutectic composition of

    alloys. [18]

  • ~7~

    such as SLC has some disadvantages and a thermally conductive device must be utilized to

    drop the bulk temperature from the entire volume of metal but able to withstand prolonged

    contact with liquid aluminium [19-21].

    SSR process is more effective compared to SLC

    whereby a cool rotating rod is immersed

    into the melt during its solidification stage. Hence, this cools the melt rapidly at localized region

    when providing vigorous agitation due to continuous stir and drops the bulk temperature of the

    melt below the liquidus. Metal slurry could be easily created from liquid metal at varied

    temperatures by the SSR process making it the most effective method to produce aluminium

    alloy slurries [12-20-21]. Figure 2.3 shows the three basic steps in the rheocasting process.

    2.4 Structural Evolution during Rheocasting

    2.4.1 Grain Density

    In rheocast alloy, the grain density is significantly higher as compared to that in conventional

    castings due to a process of dendrite fragmentation and subsequent ripening as required for a

    non-dendritic structure to form. The current theory concerning the evolution of a spheroidal

    microstructure was reviewed by Flemings, who considers the process to be dependent on the

    formation of tiny equiaxed dendrites or dendrite fragments in liquid phase just before

    solidification. In order to reduce porosity in the melt, the higher the grain density in the initial

    Step 1 Step 2 Step 3

    Figure 2.3: Schematic of three basic steps in SSR process.

  • ~8~

    melt, i.e. the more and smaller the initial grains are, the higher the chance of reducing porosity

    for a given increase in solid fraction. With the bulk of grains remaining small, diffusion lengths

    for ripening are also small and hence promote rapid growth of spheroidal particles. Vice-versa

    for larger grains, the diffusion length is equally larger and the dendrites will require more time

    to breakdown into rosettes and later into a spheroids [20-21].

    2.4.2 Convection

    Grain refinement in all rheocasting processes is obtained through convection during the process

    from the star of solidification. This creates a high density of grains throughout the melt. An

    experiment was performed by BOWER and FLEMINGS [22] showing that if convection is

    introduced during solidification, a structure with multiple smaller grains will form. The

    experiment concludes that if the metal is fed into the mould at high temperature, the formation

    of large dendrites would be observed on the surface of the samples and if the metal was fed

    with significantly less superheat, multiple sites of fine dendrites are formed. Coarse grains

    would be the final outcome if convection is not employed during the process. In the case of a

    metal slurry with less superheat, the slurry already starts to nucleate at early stages before the

    tip of the stirrer is introduced and engaged into the melt dispersing fine globular grains

    throughout the casting [21-22].

    2.4.3 Dendrite Fragmentation

    A more advanced study was done within the field of dendrite fragmentation by ESAKA et al

    [23] who recorded images of particles being generated in the mushy zone of the stirred melt.

    The experimentation of ESAKA et al showed that the number of particles generated, and the

    rate of generation is simultaneously augmented when stirring rate intensifies [21-23]. Martinez

    and Flemings showed that if vigorous convection is applied to a melt during its solidification

    state, non-dendritic structures are rapidly formed. Further hypotheses were made by Vogel et

    al. and Doherty et al [24]. that bending of dendrite arms arises due to shear forces and leads to

    from high-angle grain boundaries at the roots of the dendrite arms, thereby increasing energy at

    the root [21-22]. Kattamis et al [25] proposed a coarsening model in which the degeneration of

    dendrite arms has a direct link with its arm spacing, where the dendrite arm spacing is

    responsible for the rate at which the dendrite arms breakdown [21]. This coarsening mechanism

  • ~9~

    proves to be a potential form of multiplication of grains as each detached arm is swept by

    convection into the volumetric melt.

    2.4.4 Particle Stability

    Particle stability plays a vital role when filling the mould cavities in casting. In order to ensure

    proper filling of moulds by the metal slurry, we try to maintain small size of near-spheroid

    structure of the solid particles during the mould filling operation. In cases where the in-gates

    and runners are cooler than the slurry, upon contact, the metal slurry will cool relatively quickly

    creating an unstable condition that might result in microstructural effects such as generation of

    coarser grains, entrapment of air or oxide and other impurities, hence increasing the probability

    of reduced mechanical properties. Therefore, understanding the conditions which maintain

    interface stability in rheocast processing is critical [21].

    2.4.5 Fluidity of Rheocast Alloy

    In the foundry world, fluidity is defined as the length that metal will flow down a channel

    before being stopped by solidification. The correlation between the melt flow and

    microstructure makes the fluidity test a vital aspect of the rheocast process.

    Ragone [26] was the first to perform an arithmetical analysis of the fluidity of pure liquid

    metals. During his experiments he observed that the flow of the molten metal entering the sprue

    was turbulent due to a difference in pressure. The analysis accounted for frictional losses and

    used Bernoullis equation to predict the length the metal would flow before solidifying but

    neglected surface tension and viscosity changes [21-26].

    Another researcher, Niesse [21-27], extended the work of Ragone and found that adding

    small amounts of alloying elements retards the fluidity due to a larger driving force creating less

    mobility. Flemings reflecting on these facts concluded that alloying elements generate a

    retarding force during the early stages of nucleation resulting in the formation of dendrites in

    the liquid state which eventually strive to hinder the rapid flow. Smaller grain size delays

    dendrite entanglement and eases the flow of the alloy further until a higher degree of

    solidification is reached. Kwon and Lee [28] showed that the fluidity of grain refined Al-Cu

    alloy is much greater than non-refined alloy. At temperature above the liquidus, alloy fluidity

  • ~10~

    was found to decrease with decreasing temperature. It involves a direct relationship that dictates

    the increase in solid content in such a way that fluidity of the non-dendritic slurry continued to

    decrease with decreasing temperature occurring below the liquidus temperature [21-22-28].

  • ~11~

    3. EXPERIMENTAL PROCEDURES

    3.1 Experimental Setup

    The main aspect of the experimental setup was to probe in the evolution of the microstructure

    as well as the flow behaviour of the aluminium alloy A201. Figure 3.1.1 illustrates the

    apparatus utilized during the experiment. In a similar way to the typical rheocast process, the

    process has three main components: an open resistance furnace holding the melt, a rotating

    copper rod operating at 110rpm (1st Experiment), a rotating stainless steel rod operating at

    110rpm (2nd

    Experiment), and a preheated mould stacked in sand acting as a source of

    insulation. The stirrer rod is mounted in a hand drill acting as the mechanical stirrer. The probe

    tip of the thermocouple is immersed in the molten metal to record the evolving temperature.

    3.2 Stirring Rod

    The copper stirrer was 8 mm in diameter and 200 mm long, with a rounded end. The rod utilized

    for the 2nd

    experiment was stainless steel with 15 mm diameter and 450mm long. The stirrer

    rods were at room temperature (between 220C and 30

    0C) before being immersed into the melt.

    3.3 Microstructures

    In this experiment, during solidification, the dendritic structure was subjected to shear forces

    due to convection prompted to rip the dendrites into rosettes and later into a larger number of

    spheroidal particles. Figure 3.1.2 below shows the breakoff process from rosette to fine

    spheroids. Final spheroidal particles containing entrapped eutectic arise due to the ripening

    process of rosette arms whereby liquid is entrapped in between those arms.

    3.4 Hydrostatic Weighing

    The hydrostatic weighing also known as hydro-densitometry is based on the Archimedes

    principle. First the dry weight is determined by hanging the sample freely in air as shown in

    Figure 3.5.1. After recording the weight in air, the specimen is then immersed in water without

    touching the sides or bottom of the beaker, expels all the bubbles that might arise due to

    porosity, the underwater weight is recorded.

  • ~12~

    3.5 Heat Treatment

    For the semi-solid rheocast (SSR) A201 alloy specimens, conventional T6 heat treatment 2 h at

    5130C was employed, followed by 17 h at 527

    0C solution treatment, followed by water

    quenching and then a 20 h at 1530C ageing period, shown schematically in Figure 3.5 [16].

    3.6 Tensile Testing

    Specimens, after heat treatment, were machined to specific sizes as shown in Figure 3.6.2, for

    tensile testing. The tests method covers the tensile testing of rheocast alloys carried out on the

    Hounsfield H100KS material testing machine shown in Figure 3.6.1. The specimens are

    gripped by wedge grips at the two extremities and then test parameters were inputted from a

    computer. Cross speed was 3 mm/min, and the gauge length was set to 68 mm. Ultimate tensile

    strength and elongations to fracture values were obtained. Macroscopic photographs of the

    fracture surfaces were taken to observe and relate any factors that may have influenced the poor

    mechanical behaviour of these alloys.

    3.7 Metallographic Etchants

    After preparation of the A201 specimens, obtained from the 1st, 2

    nd and 3

    rd experiments,

    etchants shown in Table 2, were used to reveal the various regions of the resulting

    microstructures.

    2 h

    5130C

    5270C

    17 h

    1530C

    20 h

    Figure 3.5: Schematic of heat treatment stages.

  • ~13~

    3. EXPERIMENTAL FIGURES

    3.1.1) Experimental Setup

    Copper/

    Stainless Steel

    Stirring Rod

    Ceramic

    Crucible

    Aluminium

    Alloy A201

    Thermocouple

    Protective

    Sheath

    With Grounded

    tip

    Electric hand

    drill operating at

    110rpm

    Figure 3.1.1: Schematic of equipment Setup and built for this study.

    Figure 3.1.2: Evolution of structure during solidification with vigorous agitation [20].

    Increasing

    Shear Rate

    Increasing

    time

    Initial Dendrite Structure

    Dendrite Growth

    Rosette

    Ripened Rosette

    Spheroid

  • ~14~

    3.2.1) Conventional & SSR Experiment 1

    Figure 3.2.1: Aluminium alloy sand casting process at different pouring temperatures.

    (a) 9300C Conventional Cast Temperature (b) 8300C SSR Cast Temperature (c) 7300C SSR Cast Temperature

    (a) (b) (c)

    Figure 3.2.2: Final product from the 1st Experiment from conventional to

    rheocast casts respectively.

    (a) Conventional Cast Product (b) 8300C SSR Product (b) 7300C SSR Product

    Copper Stirrer Rod

    (a) (b)

    (c)

  • ~15~

    3.3.1) SSR Experiment 2

    Figure 3.3.1: Semi- solid Rheocasting die cast at two distinct temperatures.

    (Pouring temperature 7000C)

    (a) SSR Cast at 7000C (b) SSR Cast at 6700C

    (a)

    (b)

    (a) (b)

    Figure 3.3.2: SSR final product at different temperatures..

    (Pouring temperature 7000C)

    (b) SSR product at 7000C (b) SSR product at 6700C

  • ~16~

    3.4.1) SSR Experiment 3

    Figure 3.3.2: Samples after heat treatment (T6) and machined to

    specification for tensile testing.

    Number of samples: 24

    Figure 3.3.2: Semi-solid rheocast of 3rd

    experiment employing different

    stir techniques.

    (Pouring temperature at 6700C)

  • ~17~

    3.5.1) Hydrostatic Machine

    3.6.1) Tensile Testing Machine

    Mass

    immersed in

    H2O

    Lid to avoid

    disturbance

    Mass

    hanging

    freely Scale

    Analogue

    Reader

    Figure 3.6.1: Schematic illustrating Mechanical test system [31].

    Figure 3.5.1: Schematic illustrating the hydrostatic weighing apparatus.

  • ~18~

    3.5.1) Metallographic Etchants

    3.5.1.1 Aluminium and Aluminium Alloys

    CAUTION: Beware of when handling potential hazardous chemicals. Be sure to wear

    appropriate clothing and adhere to all warnings on chemical manufacturers. Safety is vital when

    etching.

    Table 2: Etchants applied to reveal the microstructures of A201.0 alloy.

    3.5.1.2 PREPARATION OF ALUMINUM ALLOYS

    PREPARATION OF A201.0 SPECIMENS

    Grind with 240-grit, 800-grit, 1200-grit 2000-grit and 4000-grti SiC water-cooled paper,

    250rpm applying 3lbs per specimen.

    Polish with 6-m Diamond (oil based recommended) on ultra-pol (silk) cloth at 250

    rpm, using a force of 3lbs/specimen for 5 minutes each (counter rotation).

    Polish with 1-m Diamond (oil based recommended) on ultra-pol (silk) cloth at 250

    rpm, using a force of 3lbs/specimen for 3 minutes each (counter rotation).

    Finish with Silico (50% silica and 50% water mix) on micro (cashmere) cloth at 250

    rpm, using a force of 5lbs/specimen, 3 minutes (counter rotation).

    Etchant Concentration

    Mixtures

    Conditions Comments

    Barkers Etch Distilled Water

    Hydrofluoric acid

    200 ml

    5 ml

    Anodize for 40~80s at 20

    V dc.

    Display dendrites well and

    widely used for wrought

    alloys

    Nitric Acid

    Distilled Water

    Hydrochloric acid

    100 ml

    20 ml

    3 ml

    30-45 seconds

    immersion. Add 3ml of

    HCl after each dip.

    Cast Al-Cu alloys. Over

    etching might blemish the

    microstructures.

    8

    7

    92

    12 12 68

    2

    Figure 3.6.2: Dimensions of specimen for tensile testing in millimetres (mm).

  • ~19~

    4. RESULTS AND DISCUSSION

    4.1 Microstructures of 1st Experiment

    4.1.1 Microstructures of Conventional Castings

    The results of this study consist of three set of experiments. The first set comprises of both

    conventional sand and semi-solid rheocasting (SSR) with the remaining three sets of casts being

    Semi-Solidly Rheocast at different agitation times. Figure 4.1.1shows the microstructures for

    the first set of conventional sand casting of A201 at a pouring temperature of 9300C. As

    anticipated, Figure 4.1.1(a) shows the microstructure of a conventional-cast alloy, with large

    dendrites and coarsely spaced arms. The dendrites are surrounded by eutectic composition

    which appears as darker lines in the micrographs. As a result of conventional casting, shrinkage

    macro-porosity is also apparent at the cross section of the sample. The intermetallic Al2Cu

    phase believed to be present in the conventional cast sample can also be seen in Figure 4.1.2,

    appearing as dark under the Polyvar microscope as shown in Figure 4.1.4.

    Grains, after conventional solidification casting, shows that coarse dendrite spaced arms are

    predominant. As shown in Figure 4.1.3(a), the microstructure of the conventional cast at a high

    temperature has a coarse eutectic structure. This takes place when the solidification follows the

    non-equilibrium phase cooling system. Due to the high pouring temperature, the poured

    temperature is directly proportional to the bulk free energy and the relationship of bulk free

    energy is inversely proportional to the activation energy. Due to low activation energy, the

    liquidus starts nucleating faster, speeding up the solidification process due to the high driving

    force (rapid cooling rates).

    The schematic below shows the relationship of nucleation rate as a dependant factor of the

    pouring temperature.

  • ~20~

    4.1.2 Microstructure of SSR Castings

    Based on the analysis of the conventional castings, in order to reduce the chances of porosity

    occurring, low pouring temperatures should be exploited. Figure 4.1.1(b) and (c) shows the

    reduction in microstructural defects, i.e. less porosity and finer structures. The current focus of

    rheocasting is on forming semi-solid slurries containing high fractions solid. The process

    includes mechanical stirring. Initially a copper stirrer was utilized but during extended contact

    with the hot molten metal the copper stirrer partially melted at high temperatures. This

    technique uses different media to apply the agitation to the melt. Upon contact with the slurry,

    due to convection and agitation from the stirrer, dendrite arms caused to be detached by

    breaking off. Nonetheless, the nucleation driving force was too high, during 8300C and 730

    0C,

    in order to create multiple spheroidal structures because of the rapid nucleation rate. Table 3

    demonstrates the poured temperature drop after conventional casting, followed by the SSR casts

    that were stirred for 40s each, before being poured into the mould cavities.

    Type of Cast Pouring

    Temperature/0C

    Stirring

    Time/s

    Type of Stirrer Microstructures

    Analysis

    Conventional

    Casting 930 0 Nil Coarse Dendrites

    SSR 830 40 Copper Much Finer Dendrites

    SSR 730 40 Copper

    Dendrite

    Fragmentation forming

    few globular grains

    As ,

    Table 3: 1st Set of Experimental data.

    Time to form N Nuclei, t=N/I

    C-Curve Kinetics

    High driving force

    Low mobility

    Low driving force

    High mobility

    Tf

    T

    E

    M

    P

    E

    R

    A

    T

    U

    R

    E

  • ~21~

    4.2 Microstructures of 2nd

    Experiment

    4.2.1 Microstructures of SSR Castings

    Figure 4.2.1 illustrates finer microstructures compared to the 1st set of experiments. As a result

    of less superheat and more agitation for approximately 3 to 4 minutes, finer grains with a

    reduction of pores size were obtained. For melt with less superheat and longer vigorous

    agitation to the slurry during nucleation, the convection process forces the dendrite arms found

    at early stages of the alloy to create multiple sites of disintegrated solid particles and fine

    dendrites. Furthermore, high metal temperatures will accentuate shrinkage problems and

    increase the porosity sites.

    The micrographs of AA201 alloy show that the microstructure consists of a mixture of globular,

    rosette, and fine dendrite particles at the final stages of the rheocasting process as shown in

    Figure 4.2.5. These globular and the rosette particles are believed to be the disintegrated

    particles resulting from the dendrite fragmentation due to the stirrer mechanism. This

    mechanism explains that the bulk liquid still consists of several small pools of superheated

    liquid. At early stages, as shown in Figure 4.2.4 (b, c), at 7000C during the first pour, only few

    disintegrated particles survived from the dendritic fragmentation. The instance the slurry

    attained 6700C after a uniform stir of 3~4 minutes, formation of more disintegrated particles

    were observed at lower temperature with longer times of agitation applied as shown in Figure

    4.2.4 (e, f). The growth of the fine spheroid and dendrite particles eventually coarsen to yield to

    a mixed globular and fine dendritic structure, nevertheless, at times the castings still cracked at

    even lower temperatures.

    To obtain an effective dispersion of fine globular grains when adopting rheocasting, both time

    and temperature plays a critical role in this process. The time during agitation should be

    sufficient enough to bring down the temperature and hence augmenting the solid fraction of the

    slurry.

  • ~22~

    4.2.2 Evaluation of SSR Casting Particles

    Figure 4.2.7(a) served to evaluate the important data associated with particles, such as solid

    fraction, particle density, and particles shape factor and particles distribution. The data were

    obtained from Image J processing software.

    4.2.2.1 Total Number of Particles

    In this analysis, the number of particles (N) is defined by:

    Where AT is the total analysed area of the micrographs and AP is the area of an average solid

    particles.

    Total Area of micrographs, AT is:

    Total Area of particles, AP is:

    No. of particles over the analysed surface is 3725.

    4.2.2.2 Particle Size

    Assuming the shape of the particles are circular and analysis carried out under 2D condition, the

    particle size (d) for each primary particle is given by:

    Where, AP is the area of an average solid particle.

    The diameter of the particles were calculated from an average diameter of particles varying

    from 14~23 m in diameter.

    Hence, particle size (d) is .

  • ~23~

    4.2.2.3 Solid Fraction

    The solid fraction (fs) is determined from the image analysis by the following equation:

    [32]

    The solid fraction (fs) of the AA201.0 alloy is 84.9%.

    4.2.2.4 Particle Shape Factor

    The shape factor (F) of a particle is defined by:

    Where P is the perimeter is by: assuming it a perfectly shaped circle. For F=1signifies that

    the particle is a perfect circle and if F

  • ~24~

    conditions, this experiment also entails a heat treatment process at T6 with the purpose to

    provide information about the contrasting microstructure and properties.

    4.3.2 SSR Recrystallization Behaviour (T6 Heat-Treatment)

    Figure 4.3.2.1 shows the considerable reduction of the shrinkage porosity during 6700C with

    the formation of a more desirable spheroidal microstructure which was obtained during

    isothermal heating. At earlier stages, due to lack of convection at 6580C, the size of the pores

    was reduced to some extent, nonetheless not sufficiently to avoid poor mechanical properties.

    During the T6 treatment, extensive recrystallization occurred and more or less a fine equiaxed

    spheroidal microstructure was obtained at 6700C compared to the early stages where the grains

    were more dendritic. Figure 4.3.2.2 shows the evolution in the microstructures converging to

    more disintegrated particles Figure 4.3.2.2(c) but with two long dendrites also seen on the

    surface. During the period of recrystallization, the formation of globules were fine, instead of

    coarsened, with micro holes shown in the micrographs at 6700C. Consequently the

    microstructures at 6700C should result to a better strength of the material rather than the second

    condition 6580C consisting of larger holes.

    4.4 Relative Densities Evaluation

    The evaluation fromTable 3 and Figure 4.4.1 clearly shows that the relative density/ reduction

    in porosity and other defects will tend to yield to an increase in yield strength of the material.

    As anticipated at early stages, the microstructures and any reduction in defects shall dictate the

    mechanical properties. Referring to section 4.1.1, the outcome from conventional casting

    resulted into massive shrinkage porosity and thus holds a much lower density in contrast to

    other cast temperatures. The two ideal cases were from 2nd

    and 3rd

    (with or without Heat

    Treatment) experiments whereby due to the application of convection to the metal slurry during

    solidification, the vigorous agitation not only created fine grain particles but also reduced to

    abundant number of porosity into the material. The data evidently display the ideal temperature

    7000C for processing the slurry in its semi-solid state resulting in a fine dispersion of stabilised

    particles with reduced defects. The relative density of the casts was determined from the

    following formula:

  • ~25~

    4.5 Mechanical Properties of SSR Castings

    Section 4.5 (Figures 4.5.1, 4.5.2 & 4.5.3) shows the average tensile values of the A201.0 alloy

    in normal rheocast and T6 temper conditions. Figure 4.5.6 features the maximum elongation

    from specimens that performed to their optimum level. The data clearly shows that the tensile

    properties decrease with increasing amount of shrinkage porosity, non-metallic inclusions,

    formation of oxides and turbulent flow at feeding gates. It is difficult to produce good

    mechanical properties as so many factors affect the metallurgical integrity of the castings.

    Figure 3.3.2 exhibited a crack, caused by residual stresses induced during contraction.

    This study proved that the more refined spheroidal grain structures clearly govern the

    mechanical properties whilst heat treatment T6 modifies the structures, e.g. 3rd

    experiment,

    consequently resulting in better properties when compared to the 2nd

    Experiment. The

    maximum UTS were achieved at 278MPa at 6700C-T6 with an elongation of 10% which is an

    improvement due to less porosity and other inclusions. Micro-cracking occurred during tensile

    testing of Al-Cu alloy samples at lower temperatures accounting both experiments (7000C,

    6700C, 658

    0C-T6) showed a rather poor elongation to fracture marking a reduction in ductility.

    Conversely, 6700C-T6 specimens demonstrates a varied elongation to fracture amid 1.7%-10%

    which gives hope for improving the mechanical properties of the alloy through refinements in

    the manufacturing methodology adapted in the future. It can be seen that a variety of unwanted

    inclusions, created at the point of manufacture, are damaging the mechanical properties. Figure

    4.6.1 and Figure 4.6.2, illustrates how surface turbulence leads to the creation of oxide

    inclusions and shrinkage porosity defects. With the lack of a proper gating system it will

    eventually have an impact on the metallurgical integrity.

    In this case, the macroscopic images revealed defects such as sand and dross inclusions

    in the alloy due to the vigorous manual agitation in the crucible. With inappropriate gating,

    flaws such as entrapped gases, localised shrinkage, micro-porosity and cracks were generated.

    As a result of those factors, the ultimate tensile strengths and elongations are typically lower

    than expected and ductility was reduced by the presence of such inclusions. Demands for

    improved metallurgical integrity have emerged and recognised improvements shall be sought

    with manufacturing refinements.

  • ~26~

    4. FIGURES OF A201.0 ALLOY

    4.1.1) AA201.0 Alloy Conventional Sand Casting

    (a) (b)

    (c)

    Figure 4.1.1: Optical Microstructure of Conventional Sand Casting of AA201.0

    (a) Conventional Sand Casting at 9300C

    (b) Semi-Solid Rheocasting(SSR) at 8300C

    (c) Semi- Solid Rheocasting(SSR) at 7300C

    200m 200m

    200m

  • ~27~

    4.1.2) Optical Microstructures at higher resolution

    200m 200m

    200m 200m

    200m 500m

    Figure 4.1.2: Microstructure breakdown from coarse dendrite to much finer dendrite

    via conventional sand casting of AA201 alloy. (Pouring temperature 9300)

    a) 9300C centre, riser sample b) 9300C perimeter, riser sample

    c) 8300C centre, riser sample d) 830

    0C perimeter, riser sample

    e) 7300C centre, riser sample f) 730

    0C perimeter, riser sample

    (a) (b)

    (c) (d)

    (e) (f)

  • ~28~

    4.1.3) Conventional Sand Castings and SSR (Rheocasting)

    Three moulds were used at pouring temperatures of 9300C, 830

    0C, and 730

    0C respectively. Due

    to the degree of high pouring temperature and the manual methodology employed for pouring

    the molten metal, turbulent flow resulted as the slurry was poured into the cavity. The result of

    reducing temperatures during casting and stirring while doing so, has been an observed drastic

    reduction in terms of porosity, vacancy and other defects as shown below.

    200m 200m 200m

    (a) 9300C Conventional Sand Casting

    (b) 8300C SSR Casting (c) 730

    0C SSR Casting

    Figure 4.1.3: Reduction of crystal defects as grain coarsening temperature

    decreases exponentially with the cooling rates.

    Figure 4.1.4: Formation of coarse dendritic structure near holes of the

    conventional cast sample (9300C).

    When subjected to solidification, since the

    temperature drops from 9300C and follows a

    non-equilibrium phase it results in eutectic

    formation. Since composition of melt is

    aluminium rich, it crystallizes first as the

    temperature continue to drop. The

    combination of the liquidus and solidus

    forms an intermetallic compound at below

    the A1 temperature, hence is

    formed.

    The solidification near the holes consists of

    coarse dendritic microstructures

    (conventional casting). Dendritic

    microstructures could be broken into a huge

    number of fine disintegrated particles when

    adapting the convection process. AA201.0 Coarse Dentritic mircostructure Conventional Cast

  • ~29~

    4.2.1) Semi-Solid Rheocasting (SSR)

    This section consists of the semi-solid rheocasting results whereby metal-moulds and a stainless

    stirrer were utilized. The metal-moulds were preheated and stacked in a sand pit, acting as an

    insulator preventing heat losses when the molten metal is poured. A stainless steel stirrer was

    utilized in order to avoid any possibility of melting and resulting change in the casting

    composition of the alloy. Pouring was carried out after stirring the melt for 3 minutes, at 7000C

    and 6700C respectively.

    50m 50m

    Figure 4.2.1: Optical Microstructure of SSR casting at 7000 and 670

    0 respectively.

    (Corresponding Pour temperature at 7000 and 670

    0 after agitation of 3~4 minutes each)

    a) 7000C centre, bottom section (Fine Dendritic Grain Boundaries with near

    definite globular grains)

    b) 6700C centre, bottom section ( Much Finer Dendrites attached with multiple

    breakoff particles, spheroidal grains)

    (a) (b)

    Figure 4.2.2: SSR Cast Sample at 7000C,

    stirred for 3 minutes

    Figure 4.2.3: SSR Cast Sample at 6700C,

    stirred for 3 minutes

  • ~30~

    50m 200m

    50m 200m

    200m

    (a) (b) (c)

    (f) (e) (d)

    Figure 4.2.4: AA201.0 Microstructure across and along the plane as well as the top

    and bottom of the samples.

    (Pouring temperature 7000C (a, b, c) and 670

    0C (d, e, f))

    Grains Size reduces from fine dendrite to more single globular

    particles at 7000C

    Grains Size reduces from finer dendrite to multiple globular particles

    at 6700C

    200m

  • ~31~

    100m

    (a)

    (b)

    (c)

    Figure 4.2.5: Different types of particles formed during nucleation of the AA201.0

    alloy (SSR casting process).

    (Pouring temperature 6700C)

    (a) Formation of rosette (b) Formation of fine dendrite (c) Formation of globular particles

    50m

    100m

    (a) (b)

    Figure 4.2.6: Representative of micrographs of SSR at 6700C stirred for 3 minutes

    (Pouring temperature 6700C)

    (a) Illustration of multiple spheroidal sites after nucleation

    (b) Analytical/mathematical calculations of grain diameter

  • ~32~

    (a)

    (b)

    4.2.7) METALLOGRAPHY ANALYSIS

    Figure 4.2.7.1: Representative of metallography evaluation.

    (a) Unmask Contours of grain structure used for grain size evaluation.

    (b) Focus on the formation of near net shaped globular structures.

    Figure 4.2.7.2: Graphical representation of perfectly shaped particles.

  • ~33~

    4.3.1) Semi-Solid Rheocasting (SSR)

    This set of experiments dwells on the SSR (semi-solid rheocasting) process with7000C as the

    commencing temperature for stirring, with a stainless steel stirring the melt for 45s and then

    pouring the resulting slurry into two preheated metal moulds. Preheated moulds were utilized to

    avoid impurities, such as sand inclusions and stacked in a sand pit to avoid heat losses. The

    final temperature recorded prior to pouring was 6580C, lower than the previous experiment.

    From 6700C to 658

    0C Stirred once for 45s.

    50m 50m

    (a) (b)

    Figure 4.3.1: Representative of micrographs of SSR at 7000C stirred for 45 seconds.

    (Pouring temperature 6700C and 658

    0C respectively)

    (a) Fine dendrite with few vacancy sites.

    (b) Dendrite Fragmentation into spheroidal grains with huge porosity sites.

    Figure 4.3.2: SSR Cast Sample at 7000C,

    45s stir. Temp=6700C

    Figure 4.3.3: SSR Cast Sample at 6580C.

  • ~34~

    (e)

    (c)

    Bottom

    Top

    (d)

    (a) (b)

    Top

    Bottom

    (a) (b)

    (c) (c)

    (e)

    Figure 4.3.3: SSR Cast Sample at 6700C and 658

    0C

    Stirred for 45s once.

    (a) 6700C top section (b) 670

    0C bottom section

    (c) 6580C top section (d) 658

    0C cross section

    (e) 6580C cross section

    100m

    200m

    200m 100m

    100m

  • ~35~

    (a) (d)

    (b)

    (c)

    (e)

    (f)

    4.3.2) Recrystallization Behaviour of SSR

    4.3.2.1 SSR Microstructures at T6 Conditions

    Figure 4.3.2.1: T6 SSR Microstructure at 6700C and 658

    0C Stirred for 45s once.

    A201.0-T6/ 670

    0C A201.0-T6/ 658

    0C

    100m 100m

    200m 200m

    100m 200m

  • ~36~

    Cross

    Section

    (a) (b)

    (c) (d)

    200m 200m

    200m 200m

    Figure 4.3.2.2: Recrystallization Effects reflecting on the grain boundaries at 6700C and 658

    0C

    respectively.

    (a) 6700C Bottom Section Sample (b) 6700C Perimeter of Cross Section (c) 670

    0C Long Dendrite at Bottom Area (d) 658

    0C Bottom of Sample

    Figure 4.3.2.3: 6700C SSR AT T6 Sample

    Figure 4.3.2.4: 6580C SSR AT T6 Sample

    Bottom Bottom

  • ~37~

    (b)

    (a)

    At Grain coarsening

    temperature Al

    consume Cu

    Saturated solution of

    copper in alloy.Active

    kinetic particles.

    (a)

    (b)

    (c)

    Figure 4.3.2.5: Micrographs represent the effects of heat treatment at pouring temperature of

    6700C.

    (a) Coarse Dendritic Microstructures at 6700C (b) Finer Dendrite and Spheroidal Particles after heat treatment (T6).

    Simulated Normal Grain

    Coarsening

    TP= 6700C Coarse Dendrite Microstructures

    Porosity

    100m

    Simulated Abnormal Grain

    Coarsening

    TP= 6700C/T6 Finer Dendrite and Spheroidal Particles

    Drastic Reduction InPorosity

    100m

  • ~38~

    4.4) POROSITY EVALUATION

    Section 4.1 (Figures) onwards illustrates the microstructures evolution as well as differentiate

    the series of shrinkage porosity and sizes from distinct experiment at specific temperatures.

    Table 3: Illustration of density relative to the porosity of the cast specimens.

    Experiment Cast

    Temperature/0C

    Wair/g Wwater/g Density/gcm-3

    1

    930 30 18 1.6

    830 27 15 1.8

    730 23 11 2.1

    2 700 7 3.5 2

    670 6 2.5 2.4

    3 670 4 2 2

    658 5 3 1.6

    Figure 4.4.1: Contrast in porosity reduction at distinct pouring

    temperatures.

    Schematic of porosity

    reduction [33].

  • ~39~

    4.5) MECHANICAL PROPERTIES

    Figure 4.5.1 represents a simulated model from Ansys 13.0v, displaying the stress variation

    when the specimens were subjected to tensile deformation load. The maximum stress

    concentration is located round the round of the shank. Previous studies have revealed that

    A201.0 has allowable UTS of 485MPa with 7% elongation [26-27].

    Figure 4.5.1: Specimen Behaviour under Deformation Load.

    Figure 4.5.2: SSR Cast Specimens under 2nd

    Experiment Configuration.

  • ~40~

    Figure 4.5.3: Heat Treated SSR Samples at pouring temperature 6700C

    following the 3rd

    Experiment configuration.

    Figure 4.5.4: Heat Treated SSR Samples at pouring temperature 6580C

    following the 3rd

    Experiment configuration.

  • ~41~

    Figure 4.5.5: Bar Chart Representation of Experiment 2 Maximum Tensile Strength at

    distinct rheocast temperatures.

    Figure 4.5.6: Elongation of samples cast at different

    configurations (2nd

    & 3rd

    Experiments). Pie Chart displays

    max UTS and Elongation.

    Figure 4.5.7: SSR Heat Treated Samples Mechanical Properties Relative with Varied

    Cast Temperatures 7000C and 658

    0C respectively.

  • ~42~

    4.6) MACROSCOPIC PHOTOGRAPHS

    Macroscopic defects found at 6700C are shown below.

    Regions of

    micro pores

    (a)

    Figure 4.6.1: Defects from pouring temperature of 6700C-T6.

    (a) Micro Pores throughout the casts

    (b) Layer of impurities at the edge

    (b)

    Regions of

    oxides or other

    impurities

    Micro holes are

    located

    throughout the

    specimen

    8mm

    MACRO SCALE

  • ~43~

    Macroscopic defects found at 6580C are shown below.

    Shrinkage Porosity

    Non- metallic

    inclusions and oxides

    (a) (b)

    (c) (d)

    Oxides, non-metallic

    inclusions and porosity

    leading to poor

    mechanical properties.

    Regions of

    localized Shrinkage

    Porosity

    Figure 4.6.2: Defects from 6580C-T6 leading to poor mechanical properties.

    (a), (b), (c) and (d) shows different defects influencing the metallurgical integrity.

  • ~44~

    5. CONCLUSIONS

    Summary of Findings:

    5.1 This research reveals the important aspects that influence the formation of globular

    structures during the rheocast process. Unique experiments were setup to observe the

    evolution of those structures in the semi-solid condition. They show how time and

    temperature, at which the alloy is processed, are vital for an initial equiaxed grain to

    ripen sufficiently into a spheroidal one. The unique aspect of this study is how vigorous

    agitation potentially changed the initial microstructures of A201 from dendrite to

    partially non-dendritic structures during its solidification stage.

    5.2 The experimental setup comprised of a furnace, stirring rod (Copper/Stainless Steel),

    and preheated. Convection was then applied to the low superheat melt during rapid

    solidification of A201 alloy creating stable spheroid and fine dendrite arms. This

    signifies the importance of vigorous agitation for the globule formation.

    5.3 Evaluation of micrographs shows spheroid particles roughly varying from 14~20 m in

    diameter. The equiaxed dendrites ripened into spheroids with entrapped eutectic during

    the period of recrystallization. Metallography revealed a small quantity of near-

    spheroidal particles (shape factor near to 1) followed with the fine dendritic arms.

    5.4 Different rheocasting approached were implemented during this study. With the

    application of convection to induce solidification during rapid cooling of the A201

    alloy proving to be essential in increasing the density of the alloy.

    5.5 The results of the rheocasting process clearly indicate that the mechanism for reducing

    porosity in the alloy depends on temperature, convection, as if the initial particle

    density in the metal slurry is large and dendritic, ripening shall occur rapidly into

    spheroids/ fine dendrite arms with micro holes. Nonetheless, if the particle density is

  • ~45~

    low and convention is retained, ripening will result in the growth of dendritic particles

    with large porosity with entrapped eutectic in the final structure.

    5.6 Self-improvised etchants based around Barkers Etch allowed metallographic of

    resulting microstructures.

    5.7 Standard heat treatment T6 procedure showed improvement, both in terms of the

    evolution of the grain structures alongside with the mechanical properties. The tensile

    properties of different rheocast conditions showed wide variation in properties with

    some reasonably good results together with some low and irregular ones.

    5.8 Good elongation to fracture was obtained from SSR specimen at 6700C-T6 with an

    elongation of 10% with a tensile strength of 278 MPa. Several defects contributed to

    the behaviour of the SSR by adversely affecting the metallurgical integrity of the cast

    alloys and ways of reducing their incidence have been proposed.

    Suggested Further Work

    The following is a list of ways to continue this investigation:

    Repeating the rheocasting process at different suggested times at 7000C (if considering

    the usage of two moulds during each experiment): 45s (between each feed), 1 minute

    (between each feed) and 3~5 minutes at 7000C only one feed to the mould. Observation

    of the grain structures should indicate the progress before heat treatment of the samples.

    A good gating system should be considered next time if casting scrap is to be minimised

    and metallurgical integrity improved. A filter should be utilized to physically trap the

    non-metallic inclusions but then should be used up to temperatures not less than 6500C

    to avoid the possibility of blockage during the pour.

    A pouring basin should be considered since the initialflow from the crucible was

    turbulent. A hole from the basin shall impede the turbulent flow at a certain height

    allowing the slurry to stabilise at that point of time. Those aspects should hinder any sort

  • ~46~

    of defects to the microstructure and eventually obtain better properties compared to this

    study.

    It was not possible to record the cooling rates in between the normal solidification and

    induced solidification. Determining the cooling rates would help to understand the

    particle generation during rheocasting and the time the particles spheroidize. Figures

    5.1, 5.2 and 5.3 demonstrates different manufacture configuration that could mitigate the

    adverse of inclusions happening.

    Suggested Manufacturing Configurations:

    Furnace

    Ceramic

    Crucible

    Preheated

    Metal Die

    Turbulent flow

    of melt

    Ceramic Pot

    Stabilizer

    Laminar flow

    of liquid metal

    Feed channel

    at an angle

    Figure 5.1: Schematic of typical gating slanted at an angel with a stabilizing ceramic

    pot limiting turbulent flow.

  • ~47~

    Furnace

    Ceramic Crucible

    Preheated

    Mould

    Turbulent flow

    of molten

    metal

    Ceramic Filter

    v-channelsprue

    Laminar flow

    of melt

    Figure 5.2: Schematic of feeding system including a filter separating non-metallic

    inclusions leaving pure metal in mould.

    Figure 5.3: Schematic of feeding system tilted at an angle. Feeding takes place right

    after vigorous stirring is applied.

    Ceramic

    Crucible

    Laminar flow

    neglecting

    induce gust

    Preheated

    Mould

    Flow behaviour rely

    on the operator

    feeding the mould

    Slanted

    channel

  • ~48~

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