1
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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