1.0 1.

INTRODUCTION Project Background 1.1.1 Powder Metallurgy Archaeological evidence suggests that powder metallurgy originated in Persia around 2500 BC, while sociological evidence indicates that ancient African tribes may have had similar carbothermic technology to produce iron powder which was then compaction bonded (Powder Metallurgy, 11 March 2005). Powder Metallurgy (P/M) process which comprises of powder production, blending, compaction and sintering to impart mechanical properties; is the most diverse manufacturing approach and has numerous advantages for production of high quality complex parts because of its capability to fabricate with optimum material usage and energy savings as well as dimensional accuracy from a wide variety of metal and alloy powders. P/M has become competitive with processes such as casting, forging and machining, particularly for relatively complex parts made of high strength and hard alloys in recent years. In a complete cycle of P/M process, sintering is one of the crucial branches to be observed as it plays major role in influencing the properties of the products.

1.1.2 Sintering Sintering which is one of the oldest human technologies, originating from the prehistoric era with the firing of pottery, is categorized in the synthesis element among the four basic elements of material, science and engineering model including; property, performance and composition (Kang, 2005). Since material synthesis has become vital for material development, sintering started to be studied fundamentally and scientifically by industry practitioners and researchers. Sintering, in general is the process of bonding together of porous aggregate of powders particles at high temperature. The principle variables of the process are time, temperature and furnace atmosphere. The mechanisms of sintering are complex and depend on the composition of the powders particles as well as on the process parameters. The mechanisms are diffusion, vapor phase transport and liquid
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phase sintering, usually involves atomic transport over particle surfaces, along grain boundaries and through the particle interiors. Sintering is used in the agglomeration of ore fines for further metallurgical the fabrication of metal and ceramic components.

1.1.3 Silica Sand Reinforced Steel Composite Powder metallurgical components made of alloy span a variety of industries including medical, aerospace and automotive. Steel alloy is one of the famous materials used in the application. Nevertheless, steel itself has flaws in its properties especially in the sustainability at elevated temperature. With the development of composite, the drawback in the properties of steel are eventually solved. In most of composite-reinforced application, Silica particles (SiO2 ) which is a type of ceramics are used because of its availability and good resistance at elevated temperature. Silica sand reinforced steel composite is a type of metal matrix based composite (MMCs). Metal matrix composites consist of at least two elements with distinct phases suitably distributed to achieve some property improvement. They have outstanding benefits due to the combined metallic and ceramic properties. In the P/M process, the matrix powders and reinforcements are mixed together to form blends of the two components.

1.2

Proble m State ment

Powder metallurgy process and technology appears to build up a wide array of concern among researchers. The diversity of area creates countless opportunity to develop a study. A variety of research papers presented focuses on the sintering characteristic or effects of the process towards diverse materials such as refractory glass, composites, ceramics, metal oxides and alloys. However, the study of sintering mechanism, particularly for Silica sand reinforced steel composite is not well established although it is necessary to understand the mechanism itself for further investigations and improvements in the synthesis of material industry.

1.3

Objective and Scope of Study

Objective of this study is to analyze the mechanism of sintering process of Silica sand reinforced steel composite. The study aims to evidently portray the sintering behavior of the metal matrix composite with ceramic reinforcement. This study employs a complete powder metallurgy process cycle, including the powder production, blending, compacting, and sintering. Vacuum sintering method will be utilized with the application of theoretical sintering time and temperature. The sintered specimen will be observed with optical microscopy with image analysis tool which are the Scanning Electron Microscopic (SEM) and X-Ray Diffraction (XRD). The works will be carried out in the period of two semesters in 2010.

2.0

LITERATURE REVIEW

Kalpakjian and Schmid (2006) define sintering as the process whereby green compacts are heated in a controlled atmosphere furnace to a temperature below the melting point but sufficiently high to allow bonding by fusion of the individual particles. Most of the established study on sintering mechanisms centered on the stages of sintering, effects of doping, and influence of additives and phases. Kang (2005), points out that a number of studies on sintering were carried out with focused to experimentally determine sintering mechanisms by means of measuring the neck growth and shrinkage kinetics. However, he claims that many of the investigations are misinterpreted due to the inherent problems which refer to the possibility of having two to three operative mechanisms in the experimental conditions. According to Shimosaka, Ueda, Shirakawa, and Hidaka (2003) In the sintering process, a series of phenomena occur which include the development of grains and grain boundaries, as well as the shrinking of pores; therefore, it has been a critical challenge to establish control technology that reliably achieves the targeted microstructure. However, the sintering process involves a large number of complicated parameters that mutually influenced one another, such as the characteristics of the initial powder materials, the characteristics of the molding, the temperature field in the oven, and the sintering condition. Therefore, it is not easy to determine the microstructure formation behavior and the many associated parameters through experimentation. This team actually focuses their study on the sintering mechanism of two spheres forming a homogeneous solid solubility neck. Through computer aided model simulation and laboratory experiment, they discovered that the grain boundary diffusion quickly begins and the neck starts to grow as soon as the sintering process starts. Then, as the temperature increases, the surface diffusion becomes active at the grain boundary. This result is applicable for the sintering of two spherical grains having dissimilar compositions. In conclusion, the team summarized that the sintering behavior can vary greatly depending on the characteristics of initial powder materials as well as the process parameters, including the sintering conditions. Apparently, this statement is
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in agreement with theory claimed by Kang (2005), in his book which stated that Depending on the techniques used, not only the sintering conditions but also the sintered properties may vary considerably. Research conducted by Rhamdhani, et al. (2005) successfully illustrated the behavior of sintering, including the grain growth and densification. In their research, samples of a single phase Alumina ceramic comprises of Al2 O3 with MgO doping holding different concentrations are found to experience distinct sintering mechanisms which are either by surface diffusion or grain boundary diffusion. In the results and discussion they points out The experimental results showed that the sample with MgO doping concentrations of 0.1wt% and 0.3% also experience shrinkage. This suggests that other mechanisms that lead to densification such as lattice or grain boundary diffusion were also at play. Although the sintering was dominated by surface diffusion, it does not necessary mean that it was the sole mechanism. This shows that they have deliberately considered the inherent problems discussed by Kang (2005) as mentioned earlier in the text in outlining their conclusion. In their research, the linear shrinkage model is used to determine the sintering mechanism, while the grain growth kinetics is investigated by implementing statistical fluctuation model (SFM) with X-Ray Diffraction data (XRD). Statistical fluctuation model which is develop by Warren (1960), stated that in ideal cases of a material with fine grain sizes, the change of orientation and material position relative to the diffractometer does not change the total area under the peak in the diffraction pattern (Rhamdhani, et.al, 2005). The drawback of their experiment is that the average grain size picked up seems to be a collection of bulk grain size instead of an actual single grain. Thus, the results obtained for the grain analysis might possess certain defects. On the other hand, Zhang, et.al, (2003) performed a study on the final stage sintering behavior of Fe-doped CeO2 samples with focuses to study the microstructural evolution and grain growth of the doping ceramic oxide. For the research, two samples of doped and undoped with 0.5wt% Fe samples are sintered at various temperatures in a period of 1 hour to 8 hours in to investigate the grain growth kinetics. With the idea that the characterization of grain growth engages two

parameters, i.e. grain growth exponent, n, and activation energy, Q, the team makes use the basic grain- growth kinetics equation, i.e.:

Dn - Do n =Kt and = exp ? ?

where D is the average grain size at time, t, Do is the average grain size at time, T=0, n is the growth exponent, K is the rate constant, Ko is the pre-exponential constant, Q is the activation energy grain growth, R and T are the gas constant and absolute temperature. The equations demonstrate that grain growth depends on sintering temperatures and time. Based on the study, they noted the interrelation between activation energy with grain growth which is reduction in activation energy produces a rapid grain growth. Besides, the team discovered that rapid densification rate in a lower temperature range increases the contact area of particles in a compact, which provides the diffusivity of matrix and thus enhances grain growth. This finding can be a reference for further studies on the grain growth kinetics. Hence, the present proposed study focuses on the determination of the dominant sintering mechanism in the ceramic reinforced metal matrix based composite namely SiO2 reinforced steel based composite. Observations will be carried out to analyze the microstructural behavior, shrinkage model and grain growth.

3.0 3.1

METHODOLOGY Materials

SiO2 reinforced steel composite samples are required for the research. Raw materials needed to produce the specimen are powder of steel (20 mesh particle size) as the metallic matrix and fined particle of Silica sand as the ceramic reinforcement.

3.2

Tools and Equipment

The following are major tools and equipments that will be utilized in the laboratory experiment for the research: i) ii) iii) iv) v) vi) Mechanical sieve Powder mixer or blender Cold Pressed / Compactor Furnace Scanning Electron Microscopic (SEM) X-Ray Diffraction (XRD)

3.3

Sample Preparation and Experime nt

SiO2 reinforced steel composite specimens are prepared from pure steel powder and silica sand particles. Mechanical sieve is used to obtain fined SiO2 particles from the raw Silica sand. Scanning electron microscopic (SEM) image of the mixed powder is obtained for interpretation. Next, the powders are combined and lubricated thoroughly by mixing in solid lubricant to reduce die wall friction and to assist the ejection of the compact from die. Then, the lubricated powders are cold-pressed into disk shape. The disk-shaped specimens are then weighted and final dimension, including the density are recorded. After that, the specimens are sintered in a vacuum furnace at four different temperatures range from 930C to 1300C in a suitable period of time, approximately 3 hours to 4 hours to promote maximum densification. The range of sintering temperature is decided by considering the melting point of steel as the domain in the sample of
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composite. The final dimension of the sintered specimen is recorded for the measurement of linear shrinkage. The density of the sintered specimen is measured using both Archimedess method with water or calculated from the mass and dimension of sample. 3.4 Project Planning

The project will be conducted in two semesters, effectively 14 weeks. The Gantt chart prepared for the research is shown in section 3.4.1on next page.

3.4.1 Gantt Chart

15/3 19/3 25/1 - 29/1 15/2 - 19/2 22/2 - 26/2 22/3 - 26/3 12/4 - 16/4 19/4 - 23/4 26/4 - 30/4 10/5 - 14/5 8/2 - 12/2 8/3 - 12/3 29/3 - 2/4

1/2 - 5/2

1/3 - 6/3

5/4 - 9/4

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Detail/Week Selection of Project Topic - Research for project background - Submission of Form01 Research work - Collect literature review - Preliminary interpretation - Submission of Preliminary Report Project Work - Preparation of powder - Mixing and compaction - Analysis Progress Report and Seminar - Interpretation of data - Submission of Progress Report - Seminar Project work continues - Sintering works and analysis Interim Report - Evaluation and discussion of data - Submission of Interim Report Oral Presentation

Key milestone Process 9

Mid Semester Break

3/5 - 7/5

3.4.1 Gantt Chart (continue)

11/10 15/10 18/10 22/10 25/10 29/10 26/7 30/7 16/8 20/8 23/8 27/8 13/9 17/9 20/9 24/9 27/9 1/10 1/11 5/11

Detail/Week

Project work continue - Analysis and evaluation of data gathered - Repeat procedure if necessary (defect) Progress Report 1 - Preparation of report - Submission of Progress Report 1 Project Work continue - Final interpretation Progress Report 2 - Preparation of Progress Report 2 - Submission of Progress Report 2 Project Work continue - Preparation of dissertation - Preparation of poster Poster Exhibition Submission of Dissertation - Soft bound - Hard bound Oral presentation
Mid Semester Break

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11

12

13 14

15

Key milestone Process

2/8 6/8

N o.

4/10 -8/10

9/8 13/8

30/8 3/9

6/9 10/9

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4.0

REFERENCES

Dr. G. Schaffer. 11 March 2005 <http://www.materials.uq.edu.au/powdermetallurgy/htm>. Background to Aluminium Powder Metallurgy, The University of Queensland, Australia. Suk-Joong L.Kang, 2005, Initial Stage Sintering in Sintering Densification, Grain Growth and Microstructure, Great Britain; Elsevier Butterworth-Heinemann. Serope Kalpakjian & Steven Schmid, 2006, Processing of Metal Powders is Manufacturing Engineering and Technology (5th Edition), Singapore; Pearson Education. Shimosaka, A. , Ueda, Y., Shirakawa, Y., and Hidaka, J., 2003, Sintering mechanism of two spheres forming a homogeneous solid solubility neck, Council of Powder Technology Japan , 21, 219-233. Rhamdhani, M.A., Soepriyanto, S., Ramelan, A., and Barliansyah, A., 2005, Determination of sintering mechanism and grain growth kinetics of MgO-doped Al2 O3 , Swinburne Research Bank, Journal of JTM, 12, 148-158. Zhang T.S., Ma J., Kong L.B., Zeng Z.Q., Hing P., and Kilner J.A., 2003, Final-stage sintering behavior of Fe-doped CeO2 , Materials Science and Engineering B: Solid-State Materials for Advanced Technology, 103 (2), pp. 177-183.

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