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Group 3
Ceramics Assignment 1

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Course Title: Ceramics Lab

Submitted To: Sir Luqman Hashmi
Submitted By: M. Abtahee (200301032)
Laiba Noor (200301023)
M. Zeeshan (200301031)
Laila Maryam (200301029)
Subhan Hassan (200301026)
Class: BE-13A MS&E

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April 22nd 2022

Table Of Contents

1. Abstract………………………………………………………3

2. Introduction………………………………………………….3

3. Experiment Details……….…………………………………5

4. XRD………………………………………..………………….6

5. SEM…………………………..………………………………7

6. EDS……………………………………………………………8

7. Result & Discussion…………………………………….……9

8. Difference between Techniques…………………………….10

9. Conclusion…………………………………………………..11

10. References………………………………………………….12
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Characterization of Alumina

1. Abstract:

Alumina is one of the most widely used ceramic materials such as catalysts, catalyst

foundations and absorbents, and wears a strong adhesive. This study focuses on the

formation and development of alumina powder. Physicochemical structures can be

performed using X-ray diffraction (XRD), high resolution transmission electron

microscopy (HRTEM), field effect scanning electron microscopy (FESEM) and electron

dispersive spectroscopy (EDS). As there are many types of alumina mutations, the XRD

method was used to identify α-alumina and γ-alumina. The average size of the sample-

shaped particles as they were fixed was approximately 28 nm measured by XRD

technology and direct TEM observation. Morphological surface studies from SEM have

shown grain particles with low agglomeration to al2O3 nano-sized size by increasing the

hole temperature. The values found are circular and are not in the same order. EDS

displays aluminum peaks and oxygen in the modified Al2O3.The techniques we have

used to describe them are SEM, XRD and EDS.

2. INTRODUCTION:

Introduction to characterization

Ultrafine particles are of great interest in a variety of applications, from catalyst to

luminescence ceramics, due to their unique and advanced properties determined primarily

by size, texture and structure. Nanometer-sized particles have great potential for use in

electrical, chemical or mechanical industries, as well as appropriate technologies,

including superconductors, catalysts, magnetic materials, building materials and

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engineering. Alumina has important applications in the ceramic industry and can be used

as a brasive .Alumina is an electrical protector but has very high potency. Since it is

chemical-free and white, alumina is a popular plastic supplement. Also, it is a common

ingredient in sunscreen and many cosmetics. Alumina itself is the catalyst for the

conversion of hydrogen sulfide gases into elemental sulfur. Also, alumina is used as a

basis for support for many industrial applications. The most common crystalline form,

alphaalumina, makes it suitable for use as an abrasive and as part of cutting tools. Other

categories, gamma-, delta-, eta- and theta-alumina are also present.

There are many production methods of alumina powder such as sol-gel process,

hydrothermal method, precipitation process, mechanical grinding, vapor phase reaction,

and combustion method. As the process temperature rises dramatically the transition to

multiple phases in gamma-, delta-, theta-, and alpha-alumina is possible. These changes

are accompanied by a sudden decrease somewhere in the immersion process between the

particles, especially from the gamma to the alpha phase. Used as a powerful alpha

alumina structure is required. Also, gamma alumina with a large surface area is well

supported by heat-resistant catalyst. It is not easy to find alpha alumina with nano size

with a calculation process associated with the grain growth of nano particles. One of the

major problems associated with the use of alumina catalysts is the inhibition of coke

formation and pore connections that prevent the spread of substrates and products inside

Fig.1 Properties of alumina powder used

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and outside the catalyst particles. This work describes the synthesis of nanostructured

alumina particles with sol-gel templeting nonsurfactant techniques and the structural and

morphological descriptions of these nanoparticles were performed using XRD, HRTEM,

FESEM and EDS analyzes.

3. EXPERIMENTAL DETAIS

4. X ray diffraction

To determine the chemical composition, visual properties and crystallographic structure of

the sample we will use the X ray diffraction method.

X-ray diffraction (XRD) at 40Kv was used to identify crystal segments and to measure crystal

sizes. Figure 1 shows the X-ray diffraction patterns of powder before and after heat treatment.

Figure 1 (a) shows the XRD pattern of aluminum oxide before pulling. The transformation of

phase γ → α-Al2O3 occurs at temperatures above 1000 ° C. Figure 1 (b) shows the XRD

pattern of aluminum oxide at 1000 ° C. As you can see, a wide selection of γ has emerged

with

Fig.2 XRD pattern

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increasing temperature. . Α- Al2O3 is the only active powder phase calculated above 1000 °

C. The options shown correspond to (012), (104), (110), (113), (024), (116), (018), (300)) and

(119) of the rhombohedral structure of α- Al2O3 were identified using standard data. The

average size of ordered Al2O3 nanoparticles is estimated to be half the full size (FWHM) and

Debye-Sherrer formula.where, 0.89 is the shape factor, λ is x-ray length, B is the line that

extends half the size (FWHM) by radians, and θ is the Bragg angle. The Al2O3 ratio and n-

particulated particles as fixed were 28 nm from this Debye-Sherrer figure.

Fig. 2. XRD pattern of Al2O3

Fig.3 XRD of synthesized alumina

5. SCANNING ELECTRON MICROSCOPY

SEM are Microscopes that produce images using electrons rather than using visible light.

These electrons have much shorter wavelength than visible light. The following information

can be obtained from the SEM images:

• External morphology(texture).

• Chemical composition.

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• Structure.

Fig.4 SEM analysis method

POWDER PREPARATION USING SOL-GEL METHOD:

Solution is obtained from alkoxides or organometallic precursors. This solution is then

polymerized at low temperature to form a wet gel. Proper heat treatment is done after

drying the gel (zero gel). Two precursors have been used “Aluminum chloride (AlCl3)

inorganic and Aluminum Triisopropylate(C3H7O)3Al”. Calcination of the resulting gels will be

done in a furnace for 2 hours at temperature values of 1000 degree centigrade and 1200

degree centigrade.

RESULTING IMAGES AFTER SEM:

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6. Energy Dispersive Spectroscopy

The energy dispersive spectroscopy (EDS) system is widely used to analyze material quality

but is also able to provide intermediate results. Typically, SEM instrumentation is integrated

with the EDS system to allow for the chemical analysis of the features identified in the SEM

monitor. SEM analysis and EDS simultaneously benefit in the event of failure analysis when

spatial analysis becomes more important in reaching a valid conclusion. The signals

generated by the SEM / EDS system consist of a second and rear electron used in image

processing to analyze morphological status and X-rays used to identify and measure the

chemicals present in visual concentration.

EDS can be used

(1) determine the chemical composition of airgel material,

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(2) to detect the presence of any residual scrap metal or unwanted products, and

(3) indicate the distribution of nutrients in the airgel structure.

Fig 5. EDS spectra of Al2O3.

7. RESULTS AN DISCUSSION:

X-ray diffraction (XRD) at 40Kv was used to identify crystalline phases of alumina and to

estimate the crystalline sizes.SEM image of alumina powder obtained by using aluminum

chloride as precursor form different geometries of aggregates(rounded)fig 4, while the SEM

image using aluminum triisopropylate as a precursor have reduced dimensions and are

more homogeneous. (Fig 5)

This is how SEM characterization shows the external morphology, structure etc. of your

desired powder. Energy dispersive spectroscopy (EDS) for Al2O3 prepared by liquid mixing

is confirming the presence of Al and O by weight percentage. EDS was used to analyze the

chemical composition of the substance under SEM. The EDS displays aluminum and oxygen

peaks and shows a few impurities in the modified Al2O3.

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8. Difference Between the techniques:

In SEM X-ray it is caused by an electron bomb. EDS, EDAX or EDX are just a few. So

even if you light a small size, commonly called point analyzes and a 20 nm by 4 micrometer

area or any area of 5 by 5 square micrometers, it is still EDS. XRD uses crystal formation and

composite forms while EDX actually uses the analysis of the composition of the material in

the sample. In fact, EXD or EDS works in conjunction with SEM, while XRD uses another

machine.

9. Conclusion

Conclusion In this lab, "characterization of alumina powder", I concluded that the The Novel

α-Al2O3 nanoparticles ceramic has been successfully synthesized with non-templeting solgel

techniques using an ethanol solution of aluminum nitrate. The XRD spectrum shows the

rhombohedral formation of α-Al2O3 at 1000 ° C. From SEM images, it is clear that with

increasing temperature, the morphology of particles changes into a circle. TEM image shows

that Al2O3 nanoparticles synthesized as al2O3 are solved in a sol-gel channel with an

average diameter of 28 nm. The EDS displays aluminum peaks and oxygen and shows a few

impurities in the modified Al2O3.

10.References:

Zieliński, P.A.; Schulz, R.; Kaliaguine, S; Van Neste, A., (1993). Structural
transformations of alumina by high energy ball milling. J. Mater. Res.,
Hench, L.L.; (1991). Bioceramics: from concept to clinic. J. Am. Ceram., Soc.,
Travitzky, N.; Kumar, P.; Sandhage, K.H.; Janssen, R.; Claussen, N., (2003). Rapid
synthesis of Al2O3 reinforced Fe-Cr-Ni composites. Mater. Sci. Eng. A,

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Ganguly, P.; Poole, W. J., (2003). In situ measurement of reinforcement stress in an

aluminium-alumina metal matrix composite under compressive loading. Mat. Sci.
Eng. A,
Touati, F.; Gharbi, N.; Colomban, P.H., (2000). Structural evolution in polyolysed
organic-inorganic alumina gels. J. Mater. Sci.,
Bujdák, J.; Rode, B.M., (2003). Alumina catalyzed reactions of amino acids. J.
Thermal Anal. Calorim.,
Karim, M.R.; Rahman, M.A.; Miah, M.A.J.; Ahmad, H.; Yanagisawa, M.; Ito, M.,
(2011). Synthesis of γ-Alumina Particles and Surface Characterization, Open Colloid
Sci.,
Rogojan, R.; Andronescu, E.; Ghitulica, C.; Vasile, B.S., (2011). synthesis and
characterization of alumina nanopowder obtained by sol-gel method. U.P.B. Sci. Bull.,
Series B.,
Mirjalilia, F.; Chuahb, L.; Mohamad, M., (2011). Effect of stirring time on synthesis of

ultra fine α-

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