COMPLEX ENGINEERING PROBLEM

NAME: HABIBA
ROLL NO: MM-003
BATCH: 2022-2023
DEPARTMENT: MATERIAL ENGINEERING
TOPIC: SYNTHESIS AND CHARACTERIZATION OF GLASS ADDITIVE AND
CERAMIC HOT SINTERED PELLET
ABSTRACT : This work of COMPLEX ENGINEERING PROBLEM is focused on synthesis,
sintering and characterization of sintered pellets which are composed of equal volume
fraction of green tinted soda lime glass and alumina formed by the method POWDER
METALLURGY. Further, green products were hot sintered at two different temperatures to
obtain the effect of temperature on product’s properties. Sintered pellets were examined
under METALLURGICAL MICROSCOPE to analyse the microstructure. Also, hardness test was
performed on both pellets using VICKERS HARDNESS TESTER. Lastly, bulk density was
measured using standard ARCHIEMEDEAN PRINCIPLE.
INTRODUCTION : In this work 50% coarse alumina (Al2O3) ceramic powder and 50% scrap
green tinted glass of compositions approximately 73% silica(SiO2), 15% Na2O, 7% CaO, 4%
MgO with 0.3 to 0.65% Fe2O3 (that impart green colour to glass).
Due to the mineralogical and chemical composition, glass shows fluxing properties and as a
result, can act as a fluxing agent for ceramic.
Flux: A flux is an oxide that lowers the melting or softening temperature of a mix of
materials. SiO2 is a dominant flux.
PROCESS DESCRIPTION:
POWDER METALLURGY : Powder metallurgy is a process of forming precision components
from powders. Powder metallurgy have technical as well as economic benefits. The following
steps were involved in powder metallurgy.
 RAW MATERIAL TO SAMPLE POWDER:
 SEPERATE DRYING: Alumina obtained after beneficiation and leaching
was dried in a furnace at about 500°C to remove moisture.
  BALL MILLING: Alumina was than wet ball milled using ethanol for the
purpose of grinding. It works on the principle of impact and attrition: size
reduction is done by impact as the balls drop from near the top of the
shell. Sizing was bring about through dry or vibrating screens. Coarser
particle size of alumina was taken as sample.

PARTICLE SIZE EFFECTS: (1) ceramics with fine particle size fire quickly and
require lower firing temperatures
(2) dense unfired ceramics fire quickly and remain dense after firing with
lower shrinkage
(3) irregular shaped ceramics fire quickly.
 CRUSHING: Glass was crushed to obtain glass powder, using a heavy
metal rod. Then was sieved and taken for batch calculation.
 CALCINATION: In this step powder is heated to a temperature well below its
melting point to liberate undesirable gases or other material and to bring
about structural transformation to produce the desired composition and
phase product. Calcining typically is carried out in rotary calcines.
 BATCH CALCULATION: According to given composition 50% of coarse alumina
of particle size 46.87 micrometre and glass each was taken.
 GRANULATION: Sample powder is further granulated by hand milling to
improve flow, handling, packing, and compaction. Granulation is
accomplished by direct mixing, which consists of introducing a binder solution
during powder mixing.
 Binders: are polymers or colloids that are used to impart strength to green
or unfired bodies. In our preparation 2 drops of PVA(polyvinyl acetate)
were used as a binder.
 FORMING: In the forming step, dry powder was consolidated and
moulded to produce a cohesive body of the desired shape and size. Dry
forming consists of the simultaneous compacting and shaping of dry
powders in a rigid die or flexible mould. Dry forming was accomplished
by dry pressing under 4MPa pressure that produced pellets of 12.7 mm
diameter.
  SINTERING: Green body of ceramic + glass powder was lastly hot sintered
which is also known as conventional firing.
Conventional firing: is accomplished by heating the green material to
approximately two-thirds of the melting point of the material at ambient
pressure and holding it for a specified time in a periodic or tunnel kiln.
Our material was sintered in a Periodic kilns which are heated and cooled
according to prescribed schedules, shown in a cycle below.
At 600°C binder was burned out. After sintering pellet was cooled at a rate of 10°C /min.

STRUCTURE AND PROPERTIES:

1. THEORITICAL DENSITY:
Density of Alumina(Al2O3): 3.96g/cm^3
Density of glass: Glass has following compositions 73% SiO2, 15% Na2O, 7% CaO,
4.5% MgO and approx 0.5% Fe2O3. Thus the density is given by:
(0.73 × 2.65)+(0.15 × 2.27)+(0.07×3.34)+(0.045×3.58)+(0.005×5.24) = 2.6961 g/cm^3

Average density of our pellet is given by

(0.5×3.96)+(0.5×2.6961) = Davg = 3.328 g/cm^3

2. EXPERIMENTAL DENSITY:
Following weights of pellets were observed
1. FOR PELLETE HEATED AT 1000°C:
Weight of dry pellet = Wd = 0.964 g

Weight of pellet suspended in water = Ws = 0.406 g

 Weight of pellet soaked in water = Ww = 0.972 g

Bulk Density = Wd/(Ww -Ws) = Db = 1.70 g/cm^3

Apparent Porosity = (Ww- Wd)/(Ww -Ws) = 0.014 × 100 = 1.41%

True Porosity = ( Davg – Db)/ Davg = 0.489 × 100 = 48.9%

Closed Porosity = True Porosity – Apparent Porosity = 48.9 – 1.41 = 47.5 %

Volume Fraction of the Total Porosity that consist of Closed Pores = closed porosity/true

porosity = 47.5/48.9 = 0.97

2. FOR PELLET HEATED 1050°C:

Weight of dry pellet = Wd = 0.985 g

Weight of pellet suspended in water = Ws = 0.432 g

Weight of pellet soaked in water = Ww = 1.02 g

Bulk Density = Wd/(Ww -Ws) = Db = 1.68 g/cm^3

Apparent Porosity = (Ww- Wd)/(Ww -Ws) = 0.0595 × 100 = 5.6%

True Porosity = ( Davg – Db)/ Davg = 0.495 × 100 = 49.5%

Closed Porosity = True Porosity – Apparent Porosity = 49.5– 5.6 = 43.9%

Volume Fraction of the Total Porosity that consist of Closed Pores = closed

porosity/true porosity = 43.9/49.5 = 0.89

3. MICROSTRUCTURE:

Microstructure of pellet heated at 1000°C

Microstructure of pellet sintered at 1050°C

 4. DIMENSIONS:

Diameter of both pellets before sintering was 12.7 mm

Dimensions after sintering are shown in a table below

TEMPERATURE DIAMETER (mm) THICKNESS (mm)

1000°C 12.8 3.5

1050°C 12.7 3.5

5. MECHANICAL PROPERTY:

HARDNESS :

Hardness of pellet sintered at 1000°C is found to be 581 HV

Hardness of pellet sintered at 1050°C is found to be 271 HV

HYPOTHESIS AND RESULT:

Since the melting point of glass is 900°C, the diameter and thickness of the pellet was expected to increase because of the melting of the glass and thus

increase in volume of pellet. Also, partial liquid phase of glass in the pellet was expected due to the large difference in melting points of glass and ceramic.

Result shows that the pellet sintered at 1000°C has expand axially due to the transformation from solid to liquid phase of only glass. Whereas, the pellet

sintered at 1050°C, it can be conclude that glass has almost melted and has agglomerated with ceramic or the surface diffusion has occurred.

COMPARISION OF PROPERTIES:

Since the pellet heated at higher temperature has diffused more than the pellet sintered at lower temperature following properties vary:

1. 1000°C sintered pellet shows more hardness than 1050°C pellet due to less glass melted and diffused over surface.

2. Pellet sintered at 1050°C shows more compaction at the core since it has a closed porosity of 43% while the closed porosity of pellet sintered at

1000°C is 47%

3. Both pellets has shown much variation between calculated and theoretical density

4. Dry weight of more compacted pellet(sintered at 1050°C) is higher than that of less compacted pallet(sintered at 1000°C)

5. True porosity of pellet sintered at 1050°C is 49.5% while that of sintered at 1000°C is 48.9%, therefore the weight after the pellets are soaked in

water, weight of pellet with higher porosity is found to be more than that with low porosity.
6. At last, bulk density of pellet sintered at 1050°C is 0.02 % less than that sintered at 1000°C, despite of being more compacted. That is because of

the presence of liquid phase in the pellet sintered at 1050°C.

o Conclusion:

Result shows that pellet sintered at 1000°C has high hardness and less weight while there being very less difference in density as compared

to that sintered at 1050°C.

Therefore if pellets are to be used as wear resistant coatings or to be placed between building blocks to support the structure, for obviously

models, 1000°C sintered pellet is more preferable.

REFERENCES:

o ISFT 2020 by Anupam

o www.valdosta.edu

o www3.epa.gov

o Ceramics and colloids TP3 by Aslam Kunhi Muhammad

o Ceramics by William G. Fahrenholtz