introduction and literature review -...

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CHAPTER-1

INTRODUCTION AND

LITERATURE REVIEW

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1.1. INTRODUCTION AND LITERATURE REVIEWThe term ceramics refers to any pottery made from fired high-quality clay,

silica and feldspar. The word ceramics is derived from the Greek word

keramos which originally meant a drinking vessel but was later applied to

all fired clay products. Ceramics include glass, cement, enamels on a metal

base, and grinding wheels. Here, ceramics are confined to products which

are shaped at room temperature but must be fired in a kiln in order to get

final desired product. The ceramics products are prepared in the four basic

steps that include shaping, drying, firing and glazing 1-3.

Norton4 noted the lack of petrographic work on crystalline glazes in

contrast to the number of papers published showing the wide range of

crystals found in crystalline glazes. Indeed, it has only been within the last

few years that a significant number of papers on crystalline glazes have

emerged in the scientific literature 5-12.

It is apparent from the ceramic art and craft literature13-18 that there is an

active ceramic glaze community within the pottery world which has

clearly adopted the principle of a methodical approach to crystalline glaze

formation advocated by Norton and has used this to good effect when

imparting practical information on crystalline glaze production 19-24.

1.2. GLAZESGlaze is a thin layer of glass or glass and crystals that adheres to the

surface of the clay body. It provides a smooth, non-absorbent surface that

can be coloured and textured in a manner not possible on the clay body

itself. Glazes are composed of various oxides. Silica and boric oxide are

the glass formers but oxides such as Na2O, K2O, CaO, PbO and Al2O3

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must be present in the stoichiometric sense to give the desired properties.

These include, for example, lowering the viscosity of the molten glass so

that the glaze will flow smoothly over the surface of the clay body at the

temperature at which the glaze is fired25. Ceramic glazes26, 27 are applied on

the surface of a variety of clay products to water proof them, facilitate

cleaning and giving them their final aesthetic appearance. They can be

applied by different technologies28and develop their properties of interest

after firing at high temperatures. Since glazes are responsible for the

aesthetic properties of glazed ceramic products, their optical properties

such as gloss, colour, transparency and opacity take on a special relevance

within the set of properties that glazes should present. In several

applications the objective is to achieve transparent glazes 29, 30 on the

surface of ceramic materials31-33.

How to Apply Glaze. If a plain coloured article is being produced,

the glaze is either applied by dipping or spraying on clay body

sample. In case of patterns, the pattern is printed on a special

machine, one colour at a time, with a maximum of three colours.

Some patterns are hand painted. When the glaze is applied, the

articles go through a second glazing kiln, taking up to twelve hours to

cool and reaching a maximum temperature of 1050oC. Some patterns

are put on after glazing by a transfer process, and these articles then

go through another oven at a temperature of 720oC34-35.

Interface between Glaze and Body. The glaze interacts with

the clay body, some of the glaze will sink into the body and some of

the body material will mix with the glaze so that an intermediate layer

is formed between the body and the glaze. This layer bonds the clay

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and glaze together. It is called the glaze-body interface or buffer layer.

The higher is the firing temperature, the stronger the interface layer.

The interface produces a strong bond between glaze and body that

reduces the tendency to craze or peel. Some of the colouring oxides in

the body may enter the glaze and change its colon (composition).

Glazing on the greenware (raw glazing or green glazing or single

firing) promotes interaction between body and glaze. If too much of

the glaze’s flux combines with the refractory materials in the body,

the glaze may become matt or dry36-39. In glaze, the ingredients like

Al2O3 and alkali oxides greatly influence the surface tension and

adhesion of the glaze and the body is completed by the glaze’s power

to stick which is determined by the reaction of both the glaze and the

body40.

Crystalline Glazes: Crystalline glazes are low melting glasses

deposited on a ceramic substrate that partly crystallize under firing

and form crystals of various compounds, size and morphology41.

Crystalline glaze is one of the ceramic craft that has been produced

since 19th century in Europe42, 43. These are widely preferred,

especially to improve the attraction of art wares 44. The art-wares are

catering to international demands for their aesthetic appearance and

design45.

Crystalline glazes were produced commercially on ceramic plates in

the UK and on ceramic pots in Taiwan and Spain. These have been

examined by X-ray diffraction, conventional and polarized light

microscopy, and scanning electron microscopy in order to identify the

crystalline phases present in the glazes. X-ray microanalysis was used

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to ascertain the partitioning behavior of the transition metal ions

which were used to colour the glazes and the crystals developed by

them46. Crystalline glaze is a special type of glazes which develop

large crystals during firing and cooling. These are of two types; one

has small single crystal suspended in the glaze and the second has

large crystal clusters in or on the surface. Both types of crystals tend

to catch and reflect the light47. These glazes can be either raw or

fritted. If the glaze does not contain water-soluble constituents, then

such a raw glaze will be more advantageous than a fritted one, due to

being matured in a shorter time with lower cost 34,48-57.

Crystallization occurs in two steps.

(i) There is a formation of nuclei, that is, properly arranged atoms

form at least one unit cell

(ii) There is a growth of these nuclei by added atoms or atom groups

in a systematic manner.

Two cases may arise; one in which the nuclei forms and grows at same

temperature, and the other for which the temperature range for nuclei

formation and growth do not overlap. The first condition is known as

spontaneous crystallization and the second as controlled crystalllization58.

The nuclei formation occurs between 600oC to 900oC while growth occurs

only between 910oC to 1250oC. Nuclei form rapidly in melting crystalline

glaze and its higher fluidity is needed to limit the number of willemite59. In

order for this to happen, the glaze must remain molten for an extended

period of time. Firing schedules for crystalline glazes usually require a

soaking period at the end of the temperature gain, plus a downfiring

ramp60. To form crystals cooling should be slow. If cooling is rapid the

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glaze will become glossy instead of matt or to avoid crystal formation,

glossy transparent glazes should be cooled quickly after the maturing

temperature without any downfiring ramp61-63.

Glaze should have low viscosity so that the glaze will be free flowing

enough to allow the oxides to move together to form the crystals64-67.

Crystalline glaze are lower in their alumina content than normal. The

oxides in glaze compositions such as MgO, CaO and Al2O3 should be kept

at a certain limit since they increase glaze viscosity and prevent crystal

formations. On the other hand, K2O and Na2O are preferable due to their

ability to decrease viscosity and facilitate crystal formations68-70.

The recent work of Karasu et al.71-74 has shown how standard

microstructural characterization techniques such as X-ray diffraction,

scanning electron microscopy and X-ray microanalysis can be used to

analyse crystalline glazes75.

How Visible Crystals Formation Take Place.

If a glaze contains the proper ingredients it can form zinc crystals. The

process is as follows:

1. As the temperature of the glaze is increased, all the components

begin to melt together.

2. When the glaze reaches to the proper high temperature, seeds begin

to form in it.

3. As the glaze reaches its maximum temperature called peak

temperature, it begins to flow and many of the seeds dissolve.

4. The kiln is then lowered to a sufficient temperature which is known

as crystallization temperature. Crystallization constant increases

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with increase of crystallization temperature. Even at the same

crystallization temperature, crystallization constant also varies in

different soaking time76.

5. When the crystallization temperature reaches to the correct range,

the remaining seeds start to act like magnets and attract the

appropriate minerals in the glaze and the crystals grow on the seeds.

The longer the temperature is held at crystallization range the larger

the crystals grow77-80.The radius of grown zinc silicate crystal is

directly proportional to soaking time81. The types of crystal seeds

have little influence on the growth of zinc silicate crystal in the

glaze; crystallization constant increased with the enhancement of

crystallization temperature82-87.

There are four major factors which affect crystal size and morphology.

(i) Clay body: its composition, texture and bisquing temperature.(ii) Glaze formulation: types, composition and form (fritted or non

fritted) of ingredients

(iii) Thickness of glaze application.

(iv) Firing: Maximum temperature or peak temperature, crystallization

(crystal growing) temperature and soaking time.

When any change is done in these factors they affect crystals either

morphologically or by changing lattice structure77, 88.

The research work is aimed at to investigate (i) the effect of minor

additives (Ca, Co and Nd) i.e. glaze formulation and (ii) the effect of

change in peak temperature and soaking time at this temperature i.e. firing.

The best results of crystal glaze are studied on biscuit porcelain bodies and

are achieved with firing under a natural or oxidizing atmosphere in

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electrically heated furnace89. Continuous production of these glazes at

industrial scales is impossible due to uncontrolled crystallization88.

Once a liquid phase forms, attack on the body begins, leading to the

formation of intermediate compositions which could be either vitreous or

crystalline. The mechanism of this corrosion is similar to acid-base

reactions in aqueous solution90. There is subsequent diffusion of chemical

species from the body into the glaze and from the glaze into the body.

Thus a well developed reaction zone takes place and influences the ability

of the glaze to resist imposed stresses. Once the zone is formed, the

reactions slow down91.

1.3. TYPES OF CRYSTALLINE GLAZESThere are two major types of crystalline glazes:

(i) Microcrystalline Glazes: Microcrystalline glaze have so small crystals

that can not be seen by naked eyes and we need a microscope to see

them. These are called matt glazes.

(ii) Macrocrystalline Glazes: Macrocrystalline glazes have large crystals

to be seen with the naked eye92-94. These crystals have been identified

identical to willemite which is found naturally in certain lime stone

deposits77, 92-93, 95-98.

The main component ensuring crystallization of these glazes is zinc

oxide99-100. The crystals first form a nucleus of a tiny titanium oxide or zinc

oxide crystal. In the favourable circumstances, zinc and silica oxide

molecules will begins to attach themselves to the nucleus crystal. The

molecular bonds are in very specific arrangements, which we can see them

as crystals101. In glazes, ZnO is employed up to approximately 10%. If

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present above 10%, it can cause the glaze to have a matt appearance. By

using lead, feldspar and boric acid with ZnO, defects like bubbling,

boiling, pin holes and discoloration can be eliminated, which appears if

ZnO is used on its own. When a higher level of ZnO is present in glaze

composition, willemite crystals easily occur during slow cooling102. Zinc

is a constituent of glazes that gives a very large selection of naturally

occurring decorative crystals in which colouring agents like transition

metals are absorbed. Combination of zinc with colouring constituents has a

capacity of forming very different crystal formation and distribution.

Therefore, the intensity and depth of colour that are possible in crystalline

glazes along with the variability of crystal size and shape have maintained

many ceramists' interest103.

Titanium is also reported to promote zinc silicate crystal formation by

forming zinc titanate, which is a good nuclei for willemite102, 104. Higher

concentrations of Al2O3 have a negative effect on the crystal formation

process. Therefore the weight content of Al2O3 in glazes should not exceed

10%99. Zinc crystalline glaze can be high fired glazes or low fired glazes.

High fired glazes give the nicest, largest and most interesting crystals.

Since most potters using zinc crystalline glazes use the high fired recipes

for their good results77, 105-107. I have selected the crystalline glaze that is

based on zinc for its large, beautiful crystals.

1.4. WILLEMITE CRYSTALLINE GLAZE. Willemite is found in a wide variety of geological environment. It is a

common accessory mineral formed during the low temperature alteration

of zinc sulphide ore in arid environments108-109. The crystals are formed

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from a combination of zinc and silica known as zinc-orthosilicate similar

to naturally occurring mineral willemite (ZnO.SiO2)110-113.The pure

willemite primary coat glaze is transparent while the crystal is

white114.This glaze was developed at Sevres in France in about 1850 and

become very popular from 1890 to 1915, during the Art Nouveau

period110, 113. Willemite is named in honour of William I (Willlem), king

(1813-1840) of the Netherlands115.Willemite is a rare mineral. Technically,

it is zinc orthosilicate (2ZnO.SiO2 or Zn2SiO4)116-117. It occurs in

crystalline limestone, but rarely forms large crystals and even more rarely,

flat crystals, as found in ceramic glaze116.

The crystals are formed from the combination of zinc oxide and silica

(ZnO.SiO2)118-125. It is found that the homogeneous nucleation rate and the

crystal growth speed are directly proportional to ZnO content114, 126-127.

ZnO is introduced into the glazes being fired upto about 1050°C as an

auxillary fluxing agent118, 128. A high level of ZnO (more than 10 wt.%) in

a crystal glaze composition form willemite (Zn2SiO4) crystals during

cooling and give a naturally brilliant decorative effects on the surface of

the glaze103, 129-130. Zinc oxide combines with free silica to form zinc

silicate crystals also known as willemite. The crystals continue to grow

until the glaze becomes too viscous for the different oxides to isolate

themselves and reform within the matrix of the glaze131. Moreover, ZnO

also helps to improve the glossiness of glaze surface, modifying the action

of chromospheres, and sometimes contributing to opacity118, 128 -Zn2SiO4

(willemite) is extensively used as a host material for cathode ray tubes

phosphors132 and more recently in electroluminescence device133-134. It is

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an important crystalline phase in glass ceramics135, glazes and

pigments136-141.

Willemite, Zn2SiO4 (trigonal, R-3H) with penakite structure is an

orthosilicate with all atoms in general positionand composed by

framework of tetrahedral accommodating zinc and silicon in three different

fourfold crystallographic sites: two slightly different zinc sites Zn1 (Zn-O

1,950 A0) and (Zn-O 1.961 A0), and Si (Si-O 1.635) so resulting in

rhombohedral symmetry142-148.

1. Classification of Willemite149-152: Class : Silicates.

Sub-class : Neosilicates.

Group : Phenakite.

Physical Properties of Willemite:

Lustre : Viterous, Resinous

Streak : White

Hardness (Mohs) : 5 ½

Tenacity : Brittle

Density : 3.89-4.19 g/cm3

Colour : White

Crystallography of willemite: Crystal system : Trigonal

Class (H-M) : 3 – Rhombohedral

Space group : R3

Cell Parameters : a= 13.93 A0, c= 9.31A0

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Ratio : a:c= 1; 0.668

Unit cell volume : V 1,564.53A0 3

Morphology : Bloky, Hexagonal, Barrel-shaped crystals,

often with rounded terminations (Franklin

area); commonly acicular in clusters to

radial-fibrous aggregates; long prismatic,

hexagonal, doubly-terminated crystals;

layered, botryoidal masses (Putta) 153-160.

Isometric minerals are optically isotropic i.e. they have only one ondex of

refraction. Hexagonal, tetragonal and trigonal minerals are unisextual-they

have only one optical axis and two indices of refraction161-164.

The trigonal structure of the willemite and the ability of the crystal to

emerge for the tip of their parent fibers at some angle are relevant to the

cause of the fibrous morphology of the crystals thus, creating a rough

surface165. The crystallization can be achieved with a simple two step heat

treatment (nucleation) and the nuclei growth steps. In the nucleation step,

the mobility of an atom in the glass phase ensures of embryo formation

and nuclei stabilization and the latter promotes growth of crystal to a

desired size166-169.

The crystallization of willemite is dependent on the period of isothermal

holding (soaking time) at crystallization temperature (CT) rather during

cooling from the peak firing temperature. The peaks intensity of willemite

crystals is higher in the glaze with isothermal holding at crystallization

temperature168.

Willemite is of fibrous or needle shape growing along the c-axis170.

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Both chemical composition and heat treatment procedure of glazes

determine when, how and what kind of crystals would form171.

Therefore, ceramists are producing unique modifications by using different

compositions and heat treatment cycles, of course without ignoring

matching properties of glaze and bodies172-173.

The crystal growing temperature for each glaze can be somewhat difficult

to predict. Therefore, DTA analysis is required to the get the exact

values168.

Heat treatment cycles also have a very strong effect on the concentration,

shape and size of crystallites expected to form from original glazes. It is a

very well known fact that when lower crystal growth temperatures are

employed, the final shape of crystallites is spherical, unlike higher growth

temperatures which cause single bars or double axe-head shaped

crystals174-176. With the increase of crystallization temperature the crystal

appearance changes from acicular to the needle shape. As the holding time

of crystallization temperature increased, the crystal appearance from

needle microcrystal gradually transformed into the radial with the change

of fractal dimension. When the glaze layer thickness increased, the crystal

become homogenization and relatively compact and the fractal dimension

increased gradually65, 177.

Norton65 in his investigation carried out the carefully controlled heat

treatment of a single crystalline glaze in which both the crystallizing and

growth velocity were determined. It was found possible to produce crystals

at any desired location by seeding; their size could be controlled by the

growing time and their shape by the growing temperature178-181.

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The temperature can be reduced by adding the correct amount of fluxing

agents into the glazes168.

Furthermore, metal oxides addition as fluxing agents can caused marked

changes in the crystal growth rate, although the activation energy of crystal

growth was changed a little; similarly, the minor additions of various metal

oxides influence the crystal growth rate but do not affect the crystal

structure to any great extent182.

For their formation, precise firing cycles are required. In such application,

in the cycle the glaze should be cooled down slowly from melting

temperature to required temperature levels and finally to room

temperature. Since the glaze is very fluid, one must be careful enough to

ensure that it should not run off the substrate during crystal formation183.

Knowless and Freeman184 stated that crystalline glazes are devitrified

glazes within which spherulites consist of crystalline phase (willemite)

produced during controlled nucleation and growth process. Devitrified

glaze literally means the loss of glassy characteristic as what happen with

crystalline glaze products. Besides that, crystalline glazes have a higher

gloss firing temperatures when compared to ordinary glaze in order to

achieve the molten state of glaze185.

Transparent shiny glazes containing no crystals are referred to as

supercooled liquids. However if a glaze is cooled slowly crystals begin to

form and the resulting glaze often appears matt. This process is known as

devitrification186-187. Devitrification or crystallization of glazes is

undesirable in industrial production. Glaze devitrification has been studied

exhaustively in response to the growing interest in vitroceramic

glazes188-190 in recent years191-193. This phenomenon is directly related to

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the chemical composition of the starting glaze and to the sintering

conditions. Devitrification begins with the appearance of small nuclei,

which lead to the growth of crystalline phases in a vitreous matrix. The

size and quantity of crystals that are formed, which depend on the

nucleation and growth rates, directly affect the properties of the resulting

glazes, e.g., their mechanical, optical and chemical properties.194 Most of

the existing studies in the literature involving the devitrification of ceramic

glazes deal with the increment of mechanical properties195-197, which can

be obtained through vitroceramic systems198-200.

1.5. PHASE DIAGRAM OF WILLEMITEPinckney201 reported that initially -Zn2SiO4 forms in the willemite-

leucite system in the temperature range of 700-850°C. But under

-Zn2SiO4 form

(willemite) was found to be stable202. Williamson and Glasser203 explained

-Zn2SiO4 is thermodynamically metastable and converts to the stable

-willemite on prolonged heating; and that, at 1000°C, the rate of

-phase is very rapid, whilst below 600°C it is very

slow.

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Fig. 1. Phase diagram of Willemite

1.6. COLOURING OF WILLEMITE GLAZE: There is a good practical appreciation of how the incorporation of different

transition metal oxides and carbonates into the raw glaze recipes colours

the glaze168, 204-214. Willemite, Zn2SiO4, has been identified as a suitable

host matrix for many rare earth and transition metal dopant ions for

efficient luminescence215-218. Willemite is also characterized by a low

thermal expansion coefficient and its brilliant crystals are desired for the

fabrication of glazes219. This is because increasing ZnO content leads to a

decrease in the activation energy of crystallization220-228.

In order to colour the precipitating Zinc-Silicate crystals, the colouring

oxide must be able to fit into the lattice structure. To enter the crystal, the

metal colouring atom must be able to occupy one of the six sites, otherwise

held by Zinc in Zinc-Silicate lattice229-232.

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Because of the crystal’s molecular structure, only certain colourants can

migrate into and colour the crystal. These are cobalt, nickel, copper, iron,

chromium, nickel, vanadium, cadmium, selenium, and manganese.

However, due to molecular characteristics these colourants do not all act

the same way233. The suitability of various oxides for inclusion in

crystalline glazes increases according to the following sequence: BaO,

CaF2, SiO2, TiO2, PbO, B2O3, K2O, V2O5 and in this the surface tension

also declines in the same order234-2236.

Ceramic pigments in general were classified on the basis of their crystal

structure237. The elements which are frequently used to colour the zinc-

silicate crystals are copper, cobalt and manganese. They have valence II in

common with zinc and therefore compete for the same sites when new

combination is being formed238-239.

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Specific Objective of the Work

The research work deals with the effect of minor additives (Ca, Co, Nd) on

crystallization of transparent base glaze at moderate temperature. Crystalline

glazes are widely preferred, especially to improve the attraction of art wares. The

art-wares are catering to international demands for their aesthetic appearance and

design. But these glazes are not in use in India due to its high temperature range

formation and unsure firing temperature.

These glazes develop large crystals during firing and cooling process.

There are four major factors which affect crystals size and morphology viz.

Clay body: its composition, texture and bisquing temperature.

Glaze formulation: types of ingredients, composition of ingredients and

form of ingredients (fritted or non fritted)

Thickness of glaze application.

Firing: maximum temperature or peak temperature, crystallization

(crystal growing) temperature and soaking time.

When any change is done in these factors they affect crystals either

morphologically or by changing lattice structure.

This research discussed two of them, first; effect of addition of additives

(Ca, Co and Nd) i.e. glaze formulation and second; change in peak temperature

and soaking time at this temperature i.e. firing.

It is also aimed to develop willemite crystals at low temperature so that it

could be beneficial and applicable to ceramic industries.

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