Experiments

EXPERIMENTAL (Link to Video)

Raw Materials

The raw materials that were used during the experimentation process include:

·         99% pure Titanium powder

·         99% pure Aluminum powder

·         99% pure Graphite powder

MATERIALS AND METHOD

We have prepared three samples yet. The powders weighed in mole ratio of Ti : Al : C=3.4:1.5:2.

Firstly the powders were mixed in the glove box. After mixing, the process of ball milling was performed in the planetary type ball mill with rotation speed of 70 rpm. After that the powders were sintered in the furnace at 1400oC. The prepared sample is then crushed by using mortar and pestle to form its powder. After that, the phase of sample was analyzed by XRD and particle size morphology of sample was investigated by using SEM which is equipped with EDS.


Procedure of Sample Preparation

Glove Box

The raw materials or the precursor were mixed in the glove box. The purpose of using glove box is to provide inert environment so that they cannot react with the environment.

Ball Milling

After mixing the powder in the glove box, the process of ball milling was performed in the planetary type ball mill with rotation speed of 70 rpm for 18 hours. The purpose of ball milling is to activate the powders.

Sintering

After ball milling the powder is sintered into pallets and placed in the furnace at temperature 1400oC with holding time 3 hours.

Crushing and XRD

The sample obtained by sintering is then crushed in a mortar pestle to from powder. The powder is then characterized by XRD which shows the peaks of the presence of Ti3AlC2 MAX phase.

Summary of Experimental Work

The methodology takes place for obtaining the efficient precursor MAX phase for catalyst in battery application. The result obtained through XRD and SEM which gives detail about the sample.

Characterization Method

 X-ray Diffraction

XRD of the sample is the first step towards characterization which is done firstly, the powders before mixing or before the preparation of sample secondly, it is done after mixing of powders and thirdly, it is done after the preparation of sample.

The powder of sample was tested under XRD machine present in the advance material characteristic lab which shows peaks through graph formation.

XRD FOR Ti3AlC2
Before applying any procedure, XRD has been carried out to obtain the result of as received powders and then after the preparation of sample XRD has been carried out to analyze the structure of Ti3AlC2.


above figure shows the 2 theta peaks of Ti ,Al, and C after ball mill the sample


Ti3AlC2 MAX phase XRD peaks 

The Reference Xrd peaks are:


https://www.researchgate.net/publication/334522723/figure/fig1/AS:941636175552547@1601514967562/The-XRD-patterns-of-a-Ti3AlC2-b-Ti3C2-and-c-Ti3C2-OH.png

Scanning Electron Microscopy

SEM refers to the high quality as well resolved visual image of particles in detail. In this phenomenon high energy electron beam exposed with sample which provides different useful information include crystallographic structure, grain orientation, composition.


SEM RESULTS FOR PREPARED SAMPLE (TI3ALC2)

Reference SEM Results