CHAPTER 4

EXPERIMENTAL WORK

4.1 INTRODUCTION

In this chapter, details of raw material, two different types of salts and specimen

preparation by in-situ reactive stir casting, experimental setup and metallographic

studies for the composites are presented.

Following are the steps involved in the experimental analysis:

1. After the fundamental study, the casting method and the raw materials viz.,
aluminium A356, K2TiF6, KBF4 were selected.

2. Reaction time, pouring temperature, holding time and % of TiB2 ranges were
selected after trials.

3. Al/TiB2 MMC ingots were cast through stir casting method within the ranges
selected for reaction time, pouring temperature, holding time keeping
constant % of TiB2.

4. Optical, scanning electron microscopic (SEM) and X-ray diffraction analysis

examinations were carried out on Al/TiB2 specimens.

5. Hardness values of the produced composites were determined as well.

4.2 WORK PLAN

The experimental work was planned in the following sequence to attain the objective

and illustrated in the form of a flow chart as shown in Fig. 4.1. The detailed

experimental procedures involved in each stage of the experimental work are briefed

in the following sections.

49
 Fabrication of Purchase of Ti and Purchase of cast
permanent mold B salts aluminium bars

Chipping the
castaluminium bars

Melting and processing of

Al-TiB2 MMC melt

Fabrication of Al-TiB2
MMC ingot by using
permanent mold

6% of TiB2 with 6% of TiB2 with 6% of TiB2 with

pouring temperature pouring temperature pouring temperature
750°C 780°C 810°C

Microstructure by SEM &

Optical microscope

Hardness
Measurement

Thermal analysis by
FEA for 750°C,
780°C and 810°C Analysis
pouring temperatures

Results and
conclusion

Fig. 4.1 Work plan

50
4.3 SPECIFICATION OF COMPONENT MATERIALS SELECTED

The two halide salt powders potassium hexa fluro titanate and potassium tetra fluro

borate (K2TiF6 and KBF4), procured with purity level of 99.5% were used in the

experiments. The particles of the two different salts are irregularly shaped.

Commercial cast aluminium ingot bars machined into small chips were used as base

metal to synthesize Al/TiB2 MMCs. The chemical composition of the cast aluminium

alloy matrix metal is shown in Table 4.1:-

Table 4.1 Chemical Composition of Cast Aluminium Alloy (wt.%)

Si Fe Cu Mn Mg Zn Ti Al

6.5-7.5 0.2 0.2 0.1 0.25- 0.1 0.1 Balance

0.45

This matrix was chosen because it provides an excellent combination of strength and

damage tolerance at elevated and cryogenic temperatures. For analysis aluminium

based MMCs with approximately 6 wt. % TiB2 was synthesized.

4.4 PERMANENT MOLD

The permanent mold was used to make rectangular shape ingots with dimensions, as

shown in Table 4.2. The permanent mold fabricated with mild steel is shown in

Fig. 4.2.

Table 4.2 Dimensions of die

Type of Die Dimensions

Permanent mold With 70 mm * 60 mm useful

cross-section and 230 mm
overall height

51
 Fig. 4.2 Permanent mold

4.5 FABRICATION OF Al/TiB2 MMC BY STIR CASTING ROUTE

The salts such as K2TiF6 (Potassium hexa fluoro titanate), KBF4 (Potassium tetra
fluoro borate) with 99.5% purity level and commercial cast aluminium were used as
the initial materials. This Eqn. 4.1 is used to calculate the amounts of K2TiF6 and
KBF4 by weight for the amount of TiB2 required in the final Al/TiB2 MMC. This is
done with the help of atomic weights of Ti, B, K and F. Hence in the Al/TiB2 MMC
corresponding to 6 % TiB2 reinforcements by weight amounts of K2TiF6 and KBF4
required to be mixed are calculated.

Ti +2B TiB2 (4.1)

The calculated amounts of salts are mixed by hand stirrer in a graphite crucible inside
the aluminium melt. Graphite crucible as shown in Fig. 4.3 is handled carefully
because of continuous and repeated usage. The electric stir casting furnace as shown
in Fig. 4.4 operating under normal atmospheric conditions has been used for melting
and processing.
52
 Fig. 4.3 Graphite crucible

Fig. 4.4 Experimental setup for stir casting

Ti and B bearing salts were preheated at 250°C for one hour in order to remove the

moisture and added into aluminium molten metal with continuous stirring. Initially

pre calculated amount of chips (3 Kg) of the commercial aluminium alloy were

loaded in a graphite crucible and melt in a furnace atmosphere at a set temperature up

to 850 °C. Then the calculated amounts of halide salts of potassium hexa fluro

titanate and potassium tetra fluro borate (K2TiF6 and KBF4) were slowly added to the

53
Al melt and hand stirred using a graphite rod. The temperature was maintained

constant.

The melt in the graphite crucible was kept covered by Argon gas shield with

processing and pouring temperature and holding time as parameters. Nine ingots with

varying pouring temperatures of 750 °C, 780 °C and 810 °C and holding times of 10

minutes, 20 minutes and 30 minutes after mixing the salts were cast. When no fumes

were observed, above the melt, it indicates, the reaction is complete and the Al-TiB2

(Aluminium-titanium diboride) MMC melt is ready for pouring. Then the slag is

removed from the crucible and the Al/TiB2 melt was poured in a metal mold. The

ingots were ejected from metal mold and cooled at room temperature.

4.6 PROPERTIES OF MATRIX MATERIAL SELECTED

Cast aluminium alloy is mainly used where good mechanical properties are required

in the casting with excellent castability in order to achieve the desired standard of

soundness. The casting characteristics (Fluidity – Good, suitable for fairly thin

castings; Hot tearing – The production of castings in this alloy very rarely introduces

problems due to hot tearing; Pouring temperature – The actual temperatures

employed may range considerably about 800°C) are the important reason for

selection of the alloy. The actual mechanical property of cast aluminium alloy

selected is given in Table 4.3.

Table 4.3 Mechanical Properties of Matrix Material

Yield
Tensile Elongation Hardness,
Materials strength,
strength, MPa (%) VHN
MPa
Cast
Aluminium 80-100 130-150 2 55
alloy

54
4.7 PREPARATION OF SPECIMENS FOR EXPERIMENTATION

The specimens were extracted from in-situ formed Al/TiB2 castings and subjected to

reveal the various features and the material was characterized. The details of various

characterizations are presented in the following sections.

4.7.1 Specimens for Mechanical Characterization

Material scientists learn about the mechanical properties by testing them. That is why

we use common procedures or standards, which are published by the ASTM. Often

materials are subject to forces (loads) when they are used. To calculate those forces

and how materials deform or break as a function of applied load, time, temperature

and other conditions, primary mechanical tests such as mentioned below were carried

out.

4.7.2 XRD Specimens

To identify the phases present in the fabricated in-situ Al/TiB2 MMC specimens,

from the different castings the samples were cut as per the dimensions with 10 mm

thick x 10 mm width x 10 mm height XRD analysis was carried out. The test

specimens for XRD are shown in Fig. 4.5. The results obtained were compared with

data from the Joint Committee of Powder Diffraction Standards (JCPDS).

Fig.4.5 XRD test specimens

55
4.7.3 Macro Hardness specimens

The hardness test specimens, as shown in fig. 4.6, were selected from six locations

from top to bottom of the ingot with three replications for each location. The Brinell

hardness tester with the description [load = 100Kgf, ball diameter = 1/16 inch, scale

= B and supplied by M/S Madras Metallurgical Services, Chennai] was used. The

Brinell hardness tester used for the study is shown in fig. 4.7. The ingot sketch

showing the 24 locations at which the cooling rates were studied by ProCAST finite

element software is shown in fig. 4.8. The hardness specimens were taken from

locations 1,4,7,19,21 and 23 as per fig. 4.8 and these locations are selected based on

extreme cooling rates, drastically varying, out of the 24 locations identified for

analysis for the study of cooling rates.

Fig. 4.6 Hardness test specimens

56
Fig. 4.7 Brinell hardness tester

57
Fig. 4.8 Dimensional drawing of ingot cast, shown with 24 different locations
considered

58
4.7.4 Specimens for Microstructural Properties

4.7.5 Specimens for SEM and Optical micrographs

In each of the nine Al/TiB2 MMC ingots cast with different pouring temperature and

holding time specimens of 10x10x10 (mm x mm x mm) were cut at the six locations

selected, as shown in Fig. 4.9.

Fig. 4.9 Al/TiB2 MMC specimens for SEM and optical micrographs

4.7.6 Keller’s Etchant

The machined samples were etched with Keller’s etchant (HF 2 ml + HCl 3 ml +

HNO3 5 ml + H2O 190 ml). The microstructure was then characterized by Scanning

Electron Microscope (JEOL-JSM 6610LV model) shown in Fig.4.10 and optical

microscope. The transient temperature distribution affects the microstructure very

much. Both SEM and optical micrographs show significant variation.

59
 Fig. 4.10 Scanning Electron Microscope (JEOL-JSM 6610LV model)

SUMMARY

The castings were made in the Department of Manufacturing Engineering,

Annamalai University. After casting, the samples were prepared and tested for

microstructural analysis and hardness measurement at the Department of

Manufacturing Engineering, Annamalai University and other institutions.

XRD analysis was carried out at X-Ray Lab, Pondicherry Engineering College,

Puthucherry. SEM analysis was carried out at Scanning Electron Microscope

laboratory, Department of Manufacturing Engineering, Annamalai University. The

results obtained from the experimental work were used for further analysis.

60