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Mechanical Properties of a Freezing Semi State Alloy and the Criterion Required to Cause Hot Tearing

S. McNicholas 11210390 J. Stokes School of Mechanical & Manufacturing Engineering, Dublin City University, Dublin 9, Ireland

Abstract This review covers the process of solidifcation of semi solid metal alloys and includes the factors that effect the mechanical properties as the liquid fraction decreases during freezing, and how these are relevant and effect the end result of the casting. These factors include grain size and structure as well as grain boundries and also film thickness and viscosity. Also reviewed are the reasons why the defect known as hot tearing occurs. An experiment is setup to see the interactions of mold length, viscosity of the slurry being squeezed into the mold, and a varying cooling profile. From this, it is possible to determine which factors or interaction, play the most important role in causing hot tearing and consequently a reduction in its tensile strength.

Keywords: Semi solid Metal, Solidification, Hot tearing, Viscosity

Introduction Semi State Metals are metals in a molten liquid state with solid particles suspended within the solution. The metal is cooled from a purely molten state, there should also be a small consistent grain size and be devoid of any dendritic formations, since dendrites can lead to poor mechanical properties and usually grow during the freezing process. This can be avoided by stirring or agitating the metal as it cools. It is only at this stage that the slush is squeezed into the mold. Alternatively, this stirring can continue throughout the cooling process until all the liquid is converted into individual solid grains, which results in a powder, where it can be reheated and used at a later date. The advantage of using semi state metals is that they are poured into the mold at lower tempetures and are therefore less susceptable to shrinking than traditional casting techniques, yet because of the relative high viscosity, turbulance is avoided which in turn reduces air entrapment. Overall this technique leads to a more dense and hence stronger than conventional casting. It is also more suitable for more complex shapes than forging can cope with and it can handle heat treatment such as welding if required at a later stage [2]. These materials are currently gaining in popularity and are generally used in the automotive or aerospace industries in the production of structural components where strength to weight ratios are important. Also due to the high surface finish, low defects and high dimension accuracy that these are now increasly being used in the electronic appliances [3, 4].

Literature review of the process of solidifcation Grain Sturcture The are four main stages during solidification, as the solid fraction increases it gradually arrests and immoblises the remaing liquid, these are as follows Mass Feeding, this is where the solid particles are suspended in solutions and both liquid and solid particles are free to move Interdendritic feeding, this is where a skeleton framework is formed that adheres to the side of the mold, the liquid is forced to squeeze through this framework to heal any tears, vicosity and surface tension within the fluid resist movement but any pressure gradients that are built up are equalised through this process Interdendritic sepatartion, At this point the liquid is isolated in pockets and the material is vunerable to tearing during thermal contraction. Solid feeding, this is where the solid fraction has exceeded 90%, the material at this point has developed significant strength and the only way to compensate for thermal contraction is through solid state creep [1].

All of these stages could potentially occur in the same casting at the same time when the slurry was poured into a mold, the bottom of the mold would be the first to solidify and the top layer would be the last

Of all these, time history will be ignored since, the slurry will be continiously stirred and heated until pouring time. In the following experiment, it is assumed that the slurry is mixed long enough achieve consistant grain size and therefore is ignored as a factor Hot Tearing For hot tearing, strain or strain rate plays an important role. This results in a tear that is rough in appearance. Unlike cold cracking which occurs at lower temperatures and is mainly due to a stress riser that builds, nucleates and then propagates, but leaves a smoother crack [5, 6]. Either defect affects the mechanical properties of the casting and needs to be avoided. Figure 1: Different stages of solidification, taken from [7]. Grain Particles and Film Thickness A fine grain structure leads to a higher surface area and hence a bigger interface with the liquid per unit weight. This means the layer of immobilised liquid is increased, which has no relative motion between the fliud layer and the grain boundry. It could said that the effective solid fraction has increased [1]. As the grain size increases the relative surface area decreases with respect to the solid fraction and the opposite effect is seen and hence the viscosity drops. This can be seen when a cooling semi solid slurry is stirred with a constant shear rate, the smaller particles are absorbed into larger ones and shear thinning occurs, this is known as Ostwald ripening [4]. It is along these grain boundries that most of the strain occurs. One of the most important factors in accomadating this is the film thickness which acts as a lubricant between the grains, since the bonding force throught the medium of the liquid for these grains is almost zero. The fluid between the grains is also a source of weakness for tensile forces and a typical path for crack propagation. The fluid is free to move independently of the solid grains and if another semi solid material of the same state was to come into contact with this cast, the fluids would diffuse throughout each other grain boundries result in the two pieces sticking together [4]. As the material cools, shrinkage occurs and stress can increase due to hindered thermal contraction, thermal gradients or metallostatic pressure. These stresses will result in strain, The strain created will follow the most energy efficient route which is along the grain boundaries and if the stress is above the rupture stress of the material the resulting strain will now be in excess of the ductility of the material and hence the fracture strain is reached, and hot tearing will occur, typically starting at pocket of liquid, as surface area is exposed due to the fracture strain, energy due to strain is released, crack propagation will stop once the energy available is no longer strong enough to overcome the critical stress as in the Griffith energy balance approach Eq. (1). (1) and then crack propagation will cease [1].

Viscosity Viscosity is the resistance to flow in a fluid. It is important that the viscosity is low enough to fill the entire mold but yet thick enough to avoid turbulance. It is therefore essential that the viscosity is known. The following are some of the key factors that effect viscosity Viscosity is proportional to solid fraction Viscosity is proportional to time history Viscosity is inversely proportional to shear rate Viscosity is inversely proportinal to grain size Viscosity is inversely proportinal film thickness

Figure 2: A section of I beam was cast, as it cooled shrinkage occurred and the webbing contracted due to the low liquid fraction it was unable to drawn in enough material quick enough from the flanges to compensate, and a hot tear was created, this is an example of hindered thermal contraction. According to Prokhororv the factors that lead a material to exceed its fractrue strain are as follows Grain size is inversely proportional to fracture strain Grain Consistency is proportional to fracture strain Film thickness is proportional to facture strain [1].

The Importance of the cooling profile While liquid is free to move there is no risk of the hot tearing occurring. However, as solid fraction increases, this mechanism is no longer available. The Katgermans criterion Eq. (2) models this scenario (2) Where HCS is the known know as the crack susceptibility coefficient, the higher this term the more likelihood of hot tearing. , known as the vulnerable time, is the time spent when the material has a high solid fraction and is vulnerable to tearing, this is the time taken to move from the moment where the liquid can no longer move to repair any cracks formed to a solid fraction of 99% . , known as the stress relief time, is the time spent when the material has just formed a solid skeleton structure that adheres to the walls of the mold, to the point where the liquid can no longer move to repair any cracks formed. From Eq. (2), it can be seen that to avoid hot tearing, the semi solid metal should spend as much time as possible where liquid movement can occur, and as short as time possible where the liquid movement can no longer occur. So the most desirable temperature profile is to slowly cool the material until it gets to and then accelerate the cooling until it reaches a solid fraction of 99% . Also the thicker the cross section of the material the longer it will take for the cooling effect to reach the centre and this is a typical place for hot tearing or coring to occur [2]. There are other versions of this formula, such as clyne and Davies criterion, but the underlying message is the same, the higher the HCS, the higher the probility of hot tearing, but bear in mind that this has to be applied differently to different geometries, for example a dumbbell shape with a narrow shaft would fail before a thin flat plate with the same HCS value. Another indicator to show hot tearing propability is the lamba curve, where the length of the crack is measure to a ratio of a certain length of the casting in question.

Once the slurry has solidified and cooled to room temperature the yield strength of the sample is measured. The responses obtained will be checked to see if there is any dependences between them

Figure 3: Relationship between Fraction Liquid and Time during cooling. Taken from Eskin et al [1]. In Fig 5, the modified rheometer, is used to both measure the viscosity of the liquid and to apply shear if the viscosity needs to be reduced. In order to measure the viscosity, the angular speed is set to the desired level and the Torque applied is measured, the apparent viscosity is then calculated from Eq. (4). (4) This in turn can be converted to viscosity by using a equation created by M. Hirai in Eq. (5) (5) The temperature is adjusted varying the current to the heating elements, the temperature is measured via a thermocouple. The solid fraction can be estimated from temperature versus solid fraction graphs/tables see Fig. 4

Experimental Procedure The purpose of the following is to determine the hot cracking sensitivity index (HCS) by calculated using the Clyne and Davies equation Eq. (3), which is similar to Katgerman in Eq. (2) and comparing it to length of crack produced in the test sample, or as in this case the area unaffected by the crack generated. (3)

The plunger speed will have to adjusted for viscosity, this is to avoid turbulent flow at the inlet to the mold, yet keep it at a high enough level to ensure that the mold is completely filled. The velocity of the plunger can represented as in Eq. (6). (6) The higher the viscosity the higher the velocity at the molds inlet Where Re is less than 2000 =Velocity of fluid within the feeder =Area of plunger =Viscosity of fluid =Density =Velocity of plunger Inside the mold the temperature is reduced at a constant rate within a fixed time to achieve 90% solid fraction. The second phase of cooling then begins and the mush is then cooled further to achieved a solid fraction of 99%. This again, is done in a fixed time. The two molds has the same overall dimensions with the exception of the length. Once the samples have cooled to room temperature, the resistance across the length of the sample is measured, and from that, the cross sectional area unaffected by the crack created can be calculated. The samples are taken out of the mold where the yield strength is measured. Table 1: Factors that set in the experiment Factor /Parameter Length of Sample Vulnerable Time Stress Relief Time Viscosity Unit mm minutes x 10 minutes x 10 Pas Low Limit 17 2 1 0 High Limit 85 5 3 93

Figure 4: Temperature versus solid fraction for A356 aluminum alloy, taken from X. Jian et al 2004 [7]. Molten metal is poured into the rheometer, the temperature and shear rate is adjusted to achieve 40% sold fraction at one of the fixed viscosities, the slurry is then stirred long enough to ensure that the grain size is consistant. Once achieved, the slurry is squeezed into the mold. See Fig 5.
Doughnut Plunger G Doughnut Plunger

r1
L

Thermocouple

r2

Valve

Heating Element Chilled water channel Feeder

Thermocouple

17

mm

Ohmmeter

Ohmmeter

Figure 5: Modified rheometer used to adjust solid fraction and voscosity by varying temperature and shear rate, connected to a mold where controlling the cooling profile is possible

85

mm

Thermocouple

Results and Discussion Table 2: Responses measured

Once this was confirmed, the slope(1) and the intercept(0.33) was calculated. The relationship could now be predicted for all other ranges by using Eq. (7) (7)

RUN

Area of Cross Section unaffected by crack mm2 39.61 39.21 38.82 38.43 38.05 37.67 37.29 36.92 36.55 36.18 35.82 35.46 35.11 34.76 34.41 34.07

Yield Strength Mpa 36.31 35.91 35.52 35.13 34.75 34.37 33.99 33.62 33.25 32.88 32.52 32.16 31.81 31.46 31.11 30.77

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16

The responses were then entered into Design Expert 8, where the data was tested for errors and any interaction between the factors was measured. The ANOVA factorial model was used. For yield strength, the model was found to be significant and the Pred R-Squared was found to be 0.671 and in reasonable agreement with Adj R-squared which was 0.8265. For the cross sectional area unaffected by the crack generated, the Pred R-Squared was found to be 0.6367 and in reasonable agreement with Adj R-squared which was 0.7871. When a diagnostic was carried out on the data, it was found that RUN 15 exceeded the influence on the fitted value, both the yield strength and the cross sectional area unaffected by cracked generated gave values of 2.41 which is greater than 2. The Factor of viscosity was taken out in the effects tab, since it was below 5%, and this corrected the issue.

Once the responses were measured, the effect of the yield strength by the cause of the cross sectional area of unaffected by the crack was confirmed, to do this, regression was used. First both responses were plotted against each other to see if a straight line relationship existed between both of them.

Tensile Strength MPa

38.00 36.00 34.00 32.00 30.00 32.00 34.00 36.00 38.00 40.00

Figure 7: Cube representation of factors stress relief time, vulnerable time, length of sample giving a response of yield strength Interactions for yield strength From Fig 7. It can be seen that the maximum value obtained is 34.805 which appears in two places, -A+B-C, which means the best yield strength occurs at low sample length, a long stress relief time and a short vulnerable time, this is the expected result. The other point where the same high value was obtained was at A-B+C, which means a high yield strength can also be obtained if there is a low sample length, a short stress relief time and a long vulnerable time. This second result was unexpected and can only be true if the most important factor is the sample length and/or the latter two factors are largely canceling each other out.

Cross Sectional Area that is unaffected by the crack mm2 Figure 6: Scatterplot representing the relationship between yield strength of sample and the cross sectional area unaffected by the crack created.

It appears that the role of viscosity was not as significant as the other factors involved. It would be interesting in the future to examine the relationship between viscosity and yield strength at a safe HCS value. Using different alloys and the same experimental procedure as outlined above, to see what would be the greatest strength to ratio that could be achieved with varying viscosities as the slurry entered the mold.

References 1. D.G. Eskin, Suyitno, and L. Katgerman, "Mechanical Properties in the Semi-Solid State and Hot Tearing of Aluminum Alloys," Prog Mater Sci, Cambridge International Science Publishing, Cambridge, UK, Vol 49 (No. 5), 2004, pp. 629-711. 2. N. Hatami, R. Babaei, M. Dadashzadeh, "Modeling of Hot Tearing Formation during Solidification," J. Mater. Process. Technol, Allied Publishers, New Delhi 23, Vol 205 (nos 1-3), 2008, pp. 506-513. 3. M. Kiuchi, and R. Kopp, "Mushy/Semi-Solid Metal Forming Technology Present and Future," Cirp Ananuf Techn, The International Academy for Production Engineering Vol 51 (No. 2), 2002, pp. 653-670. 4. J. Koke, and M. Modigell, "Flow Behaviour of Semi-Solid Metal Alloys," J Non-Newton Fluid, World Scientific Publishing, River Edge, NJ Vol 112 (nos 2-3), 2003, pp. 141-160. 5. M. Lalpoor, D.G. Eskin, D. Ruvalcaba, "Cold Cracking in DC-Cast High Strength Aluminum Alloy Ingots: An Intrinsic Problem Intensified by Casting Process Parameters," Mater. Sci. Eng., A, Mechanical Engineering Publisher, London, Vol 528 (No. 6) 2011, pp. 2831-2842 6. D.G. Eskin, and L. Katgerman, "A quest for a new hot tearing criterion," Article taken from Solidification Modeling and Microstructure Formation March 13-15, 2006 San Antonio, Texas, United States, TMS Materials Processing and Manufacturing Division, Solidification Committee, 38 A, pp. 1511-1519 7. X. Jian, H. Xu, T.T. Meek, "Effect of Power Ultrasound on Solidification of Aluminum A356 Alloy," Mater. Lett, Nature Publishing Group London Vol 59 (nos 2-3) 2005, pp. 190-193

Figure 8: Cube representation of factors stress relief time, vulnerable time, length of sample giving a response of cross sectional area unaffected by the crack created Interactions for cross sectional area unaffected by the crack generated Here in the Fig. 8. The lowest values are 35.44 which occurs twice, the first is found at A-B+C, which means that the crack length is the biggest at short sample length, high stress relief time and high vulnerable time. If the sample was of a small cross section, this result could be achieved, but doubtful on thicker cross sections. The second low point occurs at AB-C, means that the largest crack length can be found when there is a short sample length, a short period of stress relief and a short period of vulnerable time. These results are unexpected, the largest crack was expected to be at a long sample, high stress relief time and short vulnerable time. The data collected is suspect.

Summary and Conclusions The relationship between yield strength and the cross section area unaffected by the crack generated was established, in future if this experiment was to be repeated only the yield strength would need to be measured, since the cross section area unaffected by the crack generated could be calculated using Eq. (7). The data collected for the cross sectional area unaffected by the crack generated is suspect, since it did not follow established theory. For example, the longer sample should have been where the larger cracks should have appeared, the short mold may have been contaminated, a repeat of the experiment is recommend.

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