Microstructure and Physical of Al

2SiO

O Kaolinite Particle

Analysis by Shacking Time and Powder Metallurgy

Agus Nugroho

, Basyirun

, Rizalman Mamat

, Januar Parlaungan Siregar

Dwi Widjanarko

Ramelan

Department of Mechanical Engineering, Universitas Negeri Semarang, Semarang, Indonesia

Department of Mechanical Engineering, Universiti Malaysia Pahang, Pahang, Malaysia

dwi2_oto@mail.unnes.ac.id, ramelan@mail.unnes.ac.id

Keywords: Kaolinite Material Analysis, Nanoparticle, Nanotechnology, Shacking Time.

Abstract: The shacking time effect on the kaolinite material morphology, physical and grain size have been analyzed.

The aim of this study was to synthesize kaolinite material from Indonesian kaolin to gain nanoscale particle

reduction by shacking time and powder metallurgy cycle. Kaolinite particle powder was successfully

synthesized from thick kaolin solution. The increase in the shacking time resulted in the homogenous

dispersion of kaolinite particles, the reduction of grain size particle clustering, and the reduction of distances

between its particles. The significant grain refining during shacking was revealed which showed reduction

of particle size resulting from longer milling time. SEM analysis of the nanoparticle explained that

designated ball shacking presents to the crystalline refining development. It can be discussed that these

morphological and microstructural variations of Al2O

2SiO

O particle powders developed by

designated ball shacking time were found to present to an improvement in the density, grain refinery, grain

size of kaolinite material particle. The modification of particle grain size is possible into an initial nanoscale

by employing shacking and milling powder metallurgy process. A significant reduction of grain size

reduction was acquired in all cases.

1 INTRODUCTION

Kaolin’s group minerals and its derivative metaform

is characterized by a rather simple chemical

composition of Si, Al, O, and H (Dill, 2016). Kaolin

is relatively pure clay and it has been widely used in

ceramic industries for years (Chen, Lan and Tuan,

2000). The main chemical elements of kaolin, is a

hydrous aluminum silicate of the approximate

composition 2H

0-A1

-2SiO

. Structurally,

kaolinite material consists of alumina octahedral

sheets and silica tetrahedral sheets stacked

alternately and has the theoretical composition

46.54% Si, 39.5°/0 A12O

, 13.96% H2O (Prasad,

Reid and Murray, 1991).

The main mineral component of kaolin is

kaolinite, which consists of layers held together

through hydrogen bonds. Each layer consists of a

two-dimensional arrangement of Al-centred

octahedral (O) and a two-dimensional arrangement

of Si-centred tetrahedral (T) (Zsirka et al., 2015).

The layer is formulated of tetrahedral (Si-O) and

octahedral (Al-O) films bonded through common

oxygen. Moreover, kaolinite occupies a unique

asymmetric interlayer arrangement with two

chemically different surfaces: oxygen of the

tetrahedral film and inner surface hydroxyls of the

octahedral film (Matusik and Matykowska, 2014).

This enables for the synthesis of new nanomaterial

products with precisely defined properties (Matusik

and Bajda, 2013).

Kaolinite is a refractory material since it is a

non-metallic material capable of enduring high

temperatures and suitable as construction materials

for industrial furnaces. Their primary purpose is

derived from their resistance to high temperatures

(Aramide and Seidu, 2013). One of its application is

for refractory metal furnace material. However, to

develop reliable metal furnace it requires optimum

material alloy and optimum grain size.

The particular grain size of the material

generates different atomic bonding (Taylor,

Meyersm and Ashworth, 2007). In the term of

material selection that process would affect micro-

Nugroho, A., Basyirun, ., Mamat, R., Siregar, J., Widjanarko, D. and Ramelan, .

Microstructure and Physical of Al2O3 2SiO4 2H2O Kaolinite Particle Analysis by Shacking Time and Powder Metallurgy.

DOI: 10.5220/0009006200480053

In Proceedings of the 7th Engineering International Conference on Education, Concept and Application on Green Technology (EIC 2018), pages 48-53

ISBN: 978-989-758-411-4

structure and which determines the properties of the

material (Callister Jr and Rethwisch, 2009). There-

fore the aim of this work is to prepare AL

2SIO

O particle using mechanical shacking milling

method in order to reduce the existing grain size to

nanoscale particle reduction, dispersion, and mor-

phology of particles. Through milling process, it is

possible to acquire solid materials with wider sur-

face area and different particle sizes (Leonel, 2014).

2 EXPERIMENTAL

2.1 Material

For the preparation of the microstructures, four

samples of Indonesian kaolin were processed. The

untreated kaolin was measure in the ground is

2.24µm. The solvent used: ethanol 70%. The

chemical compositions of the raw kaolin are given in

Table 1, 2, 3 and 4. This chemical composition

acquired by SEM EDX testing from the untreated

sample. The test given in four different spots to get

the average chemical composition of the sample.

2.2 Kaolinite Particle Synthesis

The kaolin powder was purchased from the local

chemical store in Semarang and placed in a plastic

bag prior to the measurement of its weight. 9 grams

of kaolin sample was prepared in a separated

container prior to the treatment. The kaolin powder,

ethanol and ball mill were placed in the stainless

chamber of the shacking mill machine. It was then

shacked and milled in eight axes to optimize its

kaolinite particle fabrication in 30, 60 and 90

minutes individually with ethanol solution

maintaining a liquid ratio of kaolin and ball mill

1:10 by mass. The thick solution was collected for

the synthesis of kaolinite particle. The sample was

handled for drying purpose and moved from the

chamber into a separated container prior

characterization sample preparation. A standardize

coating was done prior to the sample charac-

terization process to investigate its microstructure.

2.3 Structural Characterization

Method

Scanning Electron Microscopy (SEM) - Energy

Dispersive X-Ray (EDX) analyzer from

PhenomProx was employed for structural

characterization of the samples to determine the

chemical elements, microstructure, dispersion,

morphology, and its grain size. Each sample was

placed on a carbon type and coated by Aurum in

18mA for optimal result. Untreated sample as the

first sample was analyzed by Scanning Electron

Microscopy (Choi et al., 2016) and Energy

Dispersive X-Ray (EDX) analyzer (Bhattacharyya

and Behera, 2017).

However, the other three sample which has

been treated were analyzed by Scanning Electron

Microscopy (Takeda et al., 2013) since there is no

additional chemical element process during the

particle synthesis process. The result of each

characterization shown in Figure 2 to 9.

3 RESULT AND DISCUSSION

It is acknowledged that milling processes of

crystalline material enable a significant change in

the morphology of powders as a result of great

plastic deformation of the particles within the

milling process (Hossein-zadeh and Razavi, 2013).

3.1 Particle Chemical Composition

The kaolinite particle chemical composition analysis

was taken from four different spots as shown in

Figure 1.

Figure 1: Scanning Electron Microscopy of untreated

kaolinite material morphology.

Table 1: Kaolin particle chemical composition in spot 1.

Element

Weight Percentage

59.3%

16.1%

13.7%

10.0%

0.9%

Microstructure and Physical of Al2O3 2SiO4 2H2O Kaolinite Particle Analysis by Shacking Time and Powder Metallurgy

Table 2: Kaolin particle chemical composition in spot 2.

Element

Weight Percentage

61.0%

14.8%

15.9%

8.3%

Table 3: Kaolin particle chemical composition in spot 3.

Element

Weight Percentage

57.4%

16.0%

13.9%

9.6%

3.1%

Table 4: Kaolin particle chemical composition in spot 4.

Element

Weight Percentage

58.4%

16.3%

14.0%

10.7%

0.6%

Figure 1 shows Scanning Electron Microscopy

of untreated kaolinite material morphology, the

chemical composition testing was done in four

different spots. It is possible to examine the detail

chemical composition as shown in table 1, 2, 3 and

4. Major chemical compositions of the sample are

Oxygen, Aluminium and Silica are visible in a

significant amount. However, there is a phenomenon

that the sample has Strontium, Barium, and Kalium

at spot number 3. It can be discussed as the

uniqueness of the Indonesian kaolin chemical

composition influenced by the natural development

in the soil.

3.2 Particle Microstructure

The micro kaolinite particles were synthesized and

its morphology and dispersion are shown in Figures

below. Figure 2 describes the microstructure,

morphology and kaolinite particle dispersion of the

untreated sample in 5,000x magnitude and 10µm

length. While Figure 3 describes the microstructure,

morphology and kaolinite particle dispersion of the

untreated sample in 20,000x magnitude and 5µm

length. The grain size was investigated that it is still

possible to perceive the presence of crystalline

materials with a relatively big size throughout the

surface of the sample.

Figure 2: Scanning Electron Microscopy of untreated

kaolinite material.

Figure 3: microstructure, morphology and kaolinite

particle .

The grain size investigation was done in five

different spots as shown in Figure 2 above. The

initial diameter of grain size was investigated, it is

2.24µm. The results examined in Figure 4 and 5

describe the existence of different morphological

transformation phenomena which occur

simultaneously along with the shacking process

(Leonel et al., 2014). It can be explained that the

particular particles initiated to crack due to the

shacking mechanism. As a matter of fact that

kaolinite material is a brittle material, the breakage

of it is particle occurs in a wide dispersion

throughout the particle surface as shown in Figure 4

and 5.

EIC 2018 - The 7th Engineering International Conference (EIC), Engineering International Conference on Education, Concept and

Application on Green Technology

Figure 4: Scanning Electron Microscopy of kaolinite

material morphology after 30 minutes of treatment.

Figure 5: Scanning Electron Microscopy of kaolinite

material grain size after 30 minutes of treatment.

It is explained that the dispersion of its

morphology of the particle is wider, the pores

visibility of the particles are relatively reduced. This

means there is a reduction of the particles into a

smaller grain size. As the result, there is an

escalation of the surface contact area of each

particle. It shows on Figure 6 that the grain size

particles range is between 990nm - 1.07µm. More

detail result can be obtained from Figure 7 which

explains that the grain size range is between 312 –

297nm. Through both Figure 8 and 9 it can be

examined that there is a shrinkage in the width of the

peak demonstrating the formation of a slightly more

homogeneous particle in comparison with the

material before the treatment process (Hubadillah et

al., 2016). There is a significant grain size

decrement subject to each particle of the kaolinite

material. It shows that the morphology of the

material is more homogenous and the pores number

are decreased tremendously. The diameter of grain

size obtained in the range of 211 – 190nm.

Figure 6: Scanning Electron Microscopy of kaolinite

material morphology after 60 minutes of of treatment.

Figure 7: Scanning Electron Microscopy of kaolinite

material grain size after 60 minutes of of treatment.

Furthermore, it can be investigated further from

Figure 9 that the surface area of contact is larger

than the previous ones. Besides, AL2O

2SiO

nanoparticles materialize in large arrays initiate to

disperse within kaolinite particles with a better

homogeneity and smaller area by escalating the

shacking life (Toozandehjani et al., 2017). The

significant disparity in the crystalline size and in the

lattice strain of kaolinite particle is associated to

great plastic deformation and grain size refinement

Microstructure and Physical of Al2O3 2SiO4 2H2O Kaolinite Particle Analysis by Shacking Time and Powder Metallurgy

occurring in particles in the presence of AL2O

2SiO

O initial nanoparticles as the main

subscription to the shacking cycle (Mobasherpour,

To and Ebrahimi, 2013).

Figure 8: Scanning Electron Microscopy of kaolinite

material morphology after 90 minutes of treatmen.

Figure 9: Scanning Electron Microscopy of kaolinite

material grain size after 60 minutes of treatment.

4 CONCLUSIONS

Kaolinite particle powder was successfully

synthesized from thick kaolin solution by shacking

and milling of power metallurgy process. The

shacking-milling mechanism was a crucial step for

generating the quality product of particle. The initial

grain size of the untreated sample range is 2.24µm to

660nm. Furthermore, nanoparticles appear in large

clusters start to disperse within kaolinite particles

with a better homogeneity after 90 minutes of

treatment. As the result, the grain size diameter has

been reduced to 190nm. The by-product initial

nanoparticle hydrous alumina-silica of material

formed in this process is a non-hazardous material.

Thus, we can convey the process followed in this

paper is an accessible, affordable and environment-

friendly method for kaolinite particle synthesis from

Indonesia kaolin. The modification of particle grain

size is possible into a nanoscale by employing

shacking and milling powder metallurgy process. A

significant of grain size reduction was acquired in all

cases.

ACKNOWLEDGMENTS

The researchers would like to thank the Faculty of

Engineering, Semarang State University, Indonesia

for the funding research, to a Physic Laboratory for

SEM characterization and Faculty of Mechanical

Engineering, Universiti Malaysia Pahang, Malaysia

for the great support during the research process.

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Microstructure and Physical of Al2O3 2SiO4 2H2O Kaolinite Particle Analysis by Shacking Time and Powder Metallurgy