CHAPTER ONE

INTRODUCTION

Research Background

Clay is an earth that forms a sticky mass when mixed with water

(Guggenheim, et al, 1995). When dry, clay becomes firm and when fired in a kiln,

permanent physical and chemical reactions occur. It has physical and chemical

characteristics, which enable it to be shaped by casting, molding, turning, or

pressing in the wet form. On drying and heating to high temperature the shaped

material is stone and can even be beautified by decorations and glazing. However,

the term clay can also be referred to a rock or a deposit containing a large

component of clay-sized materials. Thus, clay can be composed of any inorganic

materials such as clay minerals, allophone zeolites and iron hydrous that possess a

sufficiently fine grain size. Most clay however, is composed primarily of clay

minerals. Although, the composition of clay can vary, clays can share several

properties that result from their fine particles size. These properties include

plasticity when wet, the ability to form colloidal suspensions when dispersed in

water and the tendency to flocculate and settle out in saline water. Clays together

with organic matter, water and air are one of the four main components of soil

(Guggenheim 1995).

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 According to Ryan (1978), clay minerals are typically formed over a long

period of time by the gradual chemically weathering of rocks usually silicate

bearing, by low concentration of carbonic acid and other diluted solvents. In

addition to the weathering process, some clay minerals are formed by hydro-

thermal activity. Clay deposits may be formed in place as residual deposits in soil

but thick deposits usually are formed as a result of a secondary sedimentary

deposition process after there have been eroded and transported from their original

location of formation. Clay is still being produced by natural forced and no doubt

more clay is being formed daily then man is able to use all in ceramics. Clay also

provides the Alumina and Silica required for cement manufacturers.

Clay in its raw state is called green ware. Clay that has been fired but not

glazed is referred to as bisque ware. In Nigeria as a whole and south Easthern

Nigeria in particular, clay occurs in great abundance. It is found in nearly every

local government area. The nation wide occurrence of brick making earth materials

explains the establishment of bricks factories in almost all parts of the federation of

Nigeria (Adejoke et al, 1998). Clay is the most widespread mineral on the earth

surface.

Clay is the product of geological weathering of the surface of the earth

(Rhodes, 1973). This weathering is continuously going on everyday so clay is an

externally common and abundant materials in nature. Clay is a mineral “stew” that
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is the result of the erosion of the earth’s crust over vast spans of time (Art, 186).

Idenyi (2002) opined that clays are complex alumino silicates compound

containing attached water molecules. Clay and soils have their origin in the

mechanical and chemical disintegration of rocks (idenyi 2002). Clay minerals are

hydrous aluminium phylliosilicates sometimes with variable amount of iron,

magnesium, alkalimetals, alkaline, earth metals and therefore other cations. Clay

have structures similar to micas and therefore from flat hexagonal sheets.

Clay is a natural occurring materials composed primarily of fine grained

materials which show plasticity through a variable range of water content and

which can be hardened when dried and or fired. Clay deposits are mostly

composed of clay minerals. Minerals which impact plasticity and harden when

fired and or dried. And variable amount of water trapped in the mineral structure

by polar attraction. Organic minerals / materials which do not impact plasticity

may also be a part of clay deposits which consists of extremely fine particles of

complex aluminosilicates (Okoroafor 2008).

Odewale (2004) reported that geologist recognize two main types of clay, Residual

and Sedimentary

Residual clay: residual clay are those clay which have not been transported to any

other location by natural agencies but have remained in their places or origin. They

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are otherwise called primary clays, kaolin or china clays. The kaolin clays are

white in colour and are the purest types of clay. Residual clays are those clays

which have been formed in the site of their rocks and have not been transported

either by water, wind or glacier road.

Sedimentary clay: The sedimentary, secondary or ball clays are those clays that

have been moved from their original source by agencies of denudation. During

their transpiration, sedimentary clays becomes contaminated with other materials

impurities and the variety of non-clay materials found in them are greater than in

the residual clay.

REFRACTORY: A refractory material or refractory is a material that is resistant

to decomposition by heat, pressure or chemicals attack and contains strength and

form at high temperatures. Refractory are inorganic, non-metallic, porous and

heterogeneous. They are typically composed of oxides or non oxides like cabide,

nitride etc of the following materials. Silicon, aluminium, magnesium, calcium and

zirconium. Some metals like niobium, chromium, zirconium, tungsten,

rheniumilantalum etc are considered as refractors due to their melting points

1850oc.

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ASTMCTI defines refractory as non-metallic material having those chemical and

physical properties that make them applicable for structures, or as components of

systems that are exposed to environments above 1000oc (811k; 538oc).

Refractory materials are used in furnace, kilns, incinerators and reactors,

refractory materials must be chemically and physically stable at high temperatures.

Depending on the operating environment. They must be resistant to thermal shock,

be chemically inert and or have specific ranges of thermal conductivity and of the

coefficient of thermal expansion.

NIB: Refractories must be chosen according to the condition of the face.

CLASSIFICATION OF REFRACTORIES

They are classified in multiple ways, based on:

1. Chemical composition (oxide & non-oxide)

2. Method of manufacture (dry pressing, hand moulding, fused cast, extrusion)

3. Fusion temperature

4. Refractoriness

5. Thermal conductivity

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USES OF REFRACTORY

Refractory material are used for the following functions:

1. Serving as a thermal barier between a hot medium and the wall of a

containing vessel

2. Withstanding physical stresses and preventing erosion of vessel walls due to

hot medium.

3. Protecting against corrosion.

4. Providing thermal insulation.

CHAPTER TWO

LITERATURE REVIEW

Clay is a type of fine-grinded natural soil materials containing clay minerals.

Clays develop plasticity when wet-due to a molecular film of water surrounding

the clay particles but becomes hard, brittle and non-plastic upon drying or firing.

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Most pure clay minerals are white or light coloured, but natural clays show a

variety of colours from impurities such as a reddish or brownish colour from small

amount of iron oxide.

Clay is the oldest known ceramic material. Prehistoric humans discovered the

useful properties of clay and used it for making pottery. Some of the earliest

pottery shards have been dated to around 14,000 BC, and clay tablets were first

known writing medium. Clay is used in many modern industries such as paper

making, cement production and chemical production/filteration. Between one-half

and two-theird of clay materials often baked into bricks as an essential part of its

load bearing structures.

Clay is very common substance, shale formed largely from clay is the most

common sedimentary rock. Although many naturally occurring deposits include

silts and clay, clays are distinguished from other fine grained soil by differences in

size and mineralogy, silts which are fined grained soil that do not include clay

minerals, tend to have larger particles size than clays. Mixture of sand silt and less

than 40% clay are called loam soils high in swelling clays, which are mineral that

readily expand in volume when they absorb water.

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 Clay minerals are “hydrous aluminium Phyllosilicated” sometimes with

variable amount of iron magnesium, Alkal, metals, Alkaline earth metals and other

cations found on or near some planetary surface.

Clay minerals include the following groups;

 Kaolin group includes the minerals kaolinite, dickite, halloysite and

narcritte (polymorphs) of Al2 siosCOH4). Smarsome sources include the

kaolite serpentine group due to structural similarities.

 Smectite group which includes dioctahedral smectites such as

monoomorillonite, nontronite and beidllite and trioctahedral smectites such

as saponite. In 2013, analytical test by the curiosity rover found results

constitute with the presence of smetite clay minerals on the planet Mars.

 Illite group which includes the clay micas. Illite is the only common

minerals.

 Chlotite group consist of a wide variety of similar minerals with

considerable chemical variation.

N/B: other clay types exist such as palygorskite (also known as attapulgite) and

seipolite, clay with long water channels internal to their structure.

FLOOR TILE

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 According to Dennis (1991) tile making was associated with monasteries

and plances, the large building of their time. Potters travelled around the country

using local clays and firing them on site. The tiles were made by flatering the clay

and cutting pieces into shapes after drying, a glaze of lead are applied or sprinkled

on the surface and the tiles were then fired.

According to Hebert Morton (1984) in 184 Richard Prossor patented for

making clay buttons from dust clay. Hebert was to realize these processes could be

converted to make ceramic and he bought a share in the patent the tiles were

different from the encaustic in that they were higher and had a large portion of

calcined flint to produce a white body and usually a supaced glaze decoration.

Ictus (2012) in the early days, the tiles were hand made each tiles were hand

formed and hand painted. This each was a work of air in tiles own right. Ceramic

tile was used almost everywhere on walls, floors, ceilings, fire places in murals and

a san exterior cludding on building. But today ceramic tile throughout this world is

not hand made or hand made for most part. Automated manufacturing techniques

and the human hand does not enter the picture until it is time to install the tile.

Austwisk (1980) highlights the facts that the mixture for the tile body might

contained clay or ball clay, china clay and flint chemicals were added to produces

different colors. Water must be added to form a slip (liquid clay) which was

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sieved. The clay was dried on plater bals, which absorbed the water to bring it to a

plaster state. A pig mill then tempered the clay (formed a compact mass with no air

bubbles) this tile was formed in a metal frame the relief pattern, that clay was

added in a sand wish fasion freshly a thick coarse clay. This method prevented

warping and gave a fire clay surface while the body was robust. A plate was

allowed to dry. He then poured the slip into the surface falling and could be

handled without further drying. As last the tile was forced out of the press by a foot

pedal this method changed little throughout the 19th century except from the

invention of the steam driven press first by mavis in 1873.

PROBLEM STATEMENT

Our country is richly blessed with abundant deposit of clay minerals.

Unfortunately those clays minerals have not been properly harnessed, hence a

problem to the nation economy. Although imported floor tiles used in buildings

have received detailed reaction and their utilization, but clay minerals from Nigeria

clay deposit and their application in floor tile production for example have been

neglected. Hence, Nigeria continues to depend on imported floor tiles for many of

its building.

AIM OF RESEARCH

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The aim of this research work is to produce bathroom floor tiles using nsu and

ekebedi clay, to produce bathroom floor tile by rolling method and testing for

drying, firing shrinkage and porosity at 1200°c temperature level.

OBJECTIVES OF RESEARCH

Contrary to the backdrop of the problem statement above, the objectives of

these research are;

1. To Evaluate the suitability of the different clay minerals for floor tile

production

2. To determine the porosity and compressive strength etc of the tiles produced.

3. To utilize local bathroom floor tiles made with Nsu clay and Ekebedi clay.

4. To determine the chemical and physical properties of the clay minerals from

south Eastern zone (Nsu & Ekebedi; respectively).

5. To Evaluate the suitability of the different clay minerals for floor tile

production.

SIGNIFICANCE OF STUDY

The purpose of this research work is to make possible the utilization of locally

sourced material (clay) for the production of bathroom floor tile, that will be used

in our building or construction instead of depending on imported floor tiles. This

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research work will be able to make people understand that locally sourced clay can

also be used to produce tiles used in our homes.

SCOPE OF RESEARCH

This research is limited to the utilization of Nsu and Ekebedi clays from

bathroom floor tiles and determined by the following tests.

 Porosity test

 Dry shrinkage

 Firing shrinkage

The clay samples used in this research are obtained from clay deposits in Ekebed

Abia state, Nsu clay in Imo Stateall both located in South Eastern Nigeria.

FLOOR TILE

This is a tile manufactured from price of hard waring materials such as

stone, metal, baked clay or even glass generally for several purpose.

Tiles are often used to form walls and floor covering and can range from

simple square tiles to complex or mosaics. The earliest evidence of glazed brick is

the discovering of glazed brick in “Elamite temple” at “Chogha Zanbil” dated to

the 13th century BC glazed and coloured brick were used to make low releifs in

Ancient messopotamis, most famously the Ishtar gate of Babylon (ca. 575 BC),

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now partly reconstructed in Berlin, with sections elsewhere. Mesopotamians craft

men were imported for the palaces of the Persians empire such as Persepolis.

Earliest evidence of floor tile includes:

 Ancient middle east

 Ancient Indian sub-continent

 Ancient Iran

 Islamic

 Medieval Europe

 Far East

 Modern Europe

REFRACTORY

Refractory do not only endure high temperatures but also offers to a

reasonable extent. Resistance to slag and chemical attacks at such high

temperature. Refractory refers to any materials that can withstand or endure high

service temperature without deforming, provided such high services temperature

has not exceeded the melting temperature of the constituents of such refractory

products.

CLASSIFICATION OF REFRACTORIES

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 There are various ways by which refractories can be classified;

Oxide and Non-oxide

Oxide refractories: as the name implies are those that are made of one or more

element mostly metallic or metalloid chemically sombined with oxygen on their

respective stoichiometric ratio e.g S1O2, mgo, cao, Al2O3. 251O2, BeO, Al2O3 etc.

Non-oxide

on the other hand non-oxide refractory do not contain any oxygen but are made of

one or two elements chemically combined e.g Carbon refractories, Sic, S ic, Si3N4

etc.

ACCORDING TO NATURE OF OXIDE

a. Acid refractories: these are based on silica and siliceous compounds

b. Basic refractories: these are oxide of mostly the alkaline earth metal

elements such as Beo, mgo, CaO egtc.

c. Neutral refractories: This class of refractory are so called because they are

relatively inert to noth acidic and basic environment. They include Al 2o3, forsteril

etc.

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d. Special refractories: This group consists of refractories such as Zirconia

(ZnO2), Titania (T1O2), silicon carbon, silicon nitriode etc.

e. Monolithic Refractories: This simply means single mass, hence one single

mass for a part of section of a kiln or furnace.

f.Insulating refractories: These are made from a variety of oxides, most commonly

fire clay or silica and or alumina.

FIRING

Firing process turns raw clay into ceramic through hish temperature heating.

This usually happens in a kiln. Clay often goes through two types of firing, Bisque

firing and glaze firing. Firing process is the key step in the manufacturing of

ceramic products because It controls their property

On further heating of dried clays, more water is given off the effect of heat

on pun kaolinites has attracted a lot attention. After the removal of absorbed

hygroscopic water with which Radio (1988) has reported that it was eliminated at

14oc there remains chemically held water. This is removed by heating at above

450oc.

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 CHAPTER THREE

MATERIALS AND METHOS TO BE USED

Materials to be used are Quartz, feldspar, clay.

 QUARTZ is a hard, crystalline minerals composed of silicon and oxygen

(SiO2).

 FELDSPAR is or are group of rock – forming tectosilicate mineral. It is

added as a fluxing agent. (AT4O8).

 CLAY is fined grained natural soil material. (Using Nsu and Ekebedi for the

research utilization of bathroom floor tiles).

LOCATION OF CLAY SAMPLES TO BE USE

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 The clay samples to be use in this research will be sourced from clay

deposits in Ikwuano L.G.A in Abia state, Nsu clay in Okigwe L.G.A in Imo state

both located in South Eastern Nigeria.

METHOD OF TILE PRODUCTION

This is based on the production of ceramic bathroom floor tile using local

raw material which are Nsu and Ekebedi clay respectively and addition of three

local available source materials such as quartz, feldspar and cac03.

The dry clay “Nsu and Ekebedi” will be weighed out using the weigh

balance and it will be soaked in a bucket or bowl for a long period of weeks for

proper saturation with water.

“Sieving”

The soaked clay will be carefully sieved using 50 mesh, sieve into a clean

plastic bucket. Sieving is the process of removal of unwanted items, “pouring of

the sieved clay”

After sieving, it will be allowed to be settle for 24 hours. Therefore

excess water will be decanted and the clay will be spread on a flat clean surface

concrete floor to dry leather hard.

“Body Preparation”

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 The quartz will be ball milled for several hours after which it will be sieved

using 200 mesh siever.

“Making of the test tile”

Two samples of the bathroom floor tile will be produce and a mark will be

made on the tile to determine shrinkage rate.

FLOWCHART
RAW MATERIAL

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EQUIPMENT TO BE USE

 Ball Mill
 Weigh balance
 Sieve of various sizes
 Kiln
 Plunger
 Ruler
 Working table
 Marker

Firing Temperature: Firing is the process of bringing clay glaze up to a high

temperature. The final aim is to heat the object to the point that the clay and glazes

are mature.

TESTS TO BE CARRIED OUT

“Porosity Test”

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In ceramic testing this term generally refers to the pore space with a fired clay

body. It is measured by weighing a specimen, boiling it in water, weighing it again

and calculating the increase in weight. The % porosity of a body is thus an

indicator of its degree of vitrification.

Equation of porosity is therefore pt = vp/vt x 100

VP = Pore Volume

VT = Total Volume

“Dry Shrinkage Test”

Drying shrinkage is defined as a dimensional change in a fabric or ceramic.

Drying shrinkage results from the loss of capillary water.

Calculating shrinkage, (Dry measurement- fired measurement) divided by dry

shrinkage measurement x 100 = % shrinkage

W1 – W2 x 100
W1

“Firing Shrinkage Test”

Firing shrinkage (shrinkage from dry to fired) is a thus comperative indicator

of the degree of vitrification. As a clay is fired higher it shrinks more and to a point

of maximum shrinkage.

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 W2 – W3 x 100
W2

“Water absorption”

The absorption test will be determined by % loss in weight of samples. The

water content % of A & B will be calculated as wt of clay before drying – wt of

clay after drying divided by original wt x 100.

W1 – W2 x 100
W1

W1 = initial weight

W2 = weight after firing

W3 = Final weight.

Percentage of Raw materials to be use

Batch A

Nsu 45

Ekebedi 20

Feldspar 15

Quartz 20

Total 100

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Batch B

Nsu 45

Ekebedi 20

Feldspar 10

Quartz 25

Total 100

Batch C

Nsu 50

Ekebedi 20

Feldspar 15

Quartz 15

Total 100

CALCULATION AND READING

Determination of Drying Shrinkage

For this determination, the clays were cast into bars with wooden mould.
Immediately the articles were exactly 10cm apart on the clay cast. The clay bars
then dried by the cause of atmospheric pressure for 4 days after the green
strength has been identified from the marked sample. The wet-to-dry shrinkage
was determined after drying by measuring length between the two marks on the

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clay surface. The drying shrinkage were found to be length before drying minus
length after drying.

Determination of Firing Shrinkage

The dried clay bars were fired in the kiln to 1200°C and the fired shrinkage was
calculated. There was again recorded. From the drying and firing shrinkage, the
total shrinkages were calculate and recorded under results.

Determination of Porosity

Boiling method was used for this determination three fired test bars were
weighed accurately. They were then immersed in boiling water in a pot and
boiled for 4 hour. The bars were then removed and their bodies cleaned with a
dry towel and were immediately weighed. The differences in weight between the
boiled and un-boiled pieces were recorded as water porosity. This was expressed
as percentage of the original weight. See results.

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 REFERENCES

Guggenheim, Et al 1995 “clay” and clay mineral USA ceramics section 9,77

Ryan “1978” clay minerals. Pitman publisher New Zealand ltd, wellington pp2

Rhodes 1973 Art 186, Idenyi 2002 clay formation and geology pg3

(http://seo.glendale.edu/ceramics/clays.html2009) clay minerals.

(http://en:wikipedia.org/wiki/clayminerals)

Odewale (2004) ceramics analysis pg 32 straffordshire polytechnic.

Ictus (2012) tiles production pg12 journal of America press.

Dennis (1991) tile making institute of ceramics London pg45.

“Refractory” Mr. O. ABE pg1 2020

Herbet Morton 1984. Unpublished journals pp 108

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