Glass/ceramic/refractory techniques, their development and introduction

into dentistry: A historical literature review

David G. Wildgoose, MPhil,a Anthony Johnson, PhD, MmedSci,b and Raymond B. Winstanley,
MDS, BDSc
School of Clinical Dentistry, University of Sheffield, Sheffield, United Kingdom
This review considered the development of glass, ceramic, refractory materials, and techniques over a
period of 25,000 years, from the time of stone-age man to their introduction into dentistry. Currently
a wide variety of all-ceramic dental restorations are provided using alumina-reinforced, leucite-forming, and novel glass and ceramic materials along with a range of refractory materials and associated
techniques. However, some of the problems of dimensional and thermal change experienced by early
craftsmen still persist during current laboratory fabrication techniques. Early English archaeological
and dental publications were obtained through the Archaeology Education Department of the British
Museum in London and the Archives of the British Dental Association Library. More recent peer-reviewed articles published from 1966 to the present were obtained through MEDLINE. (J Prosthet
Dent 2004;91:136-43.)

t is difficult to consider the development of refractory

mold materials without considering the glass or ceramic
which would be formed within or around their surfaces.
Glass has its history at the beginning of time, with naturally occurring volcanic glasses such as obsidian being
fashioned into implements, tools, and jewelry as early as
stone-age man1 (Fig. 1).
Pliny is said to have suggested that man first produced
glass accidentally when a wood fire was made on a bed of
silica sand.2 It is possible that this method may have
produced temperatures in the range of 560-900C,
which would have been sufficient for an initial fusion of
the 2 predominant elements of sand and soda ash to
form a crude glass.3 However, it is more probable that
the first deliberate attempts to manufacture glass were
the consequence of the potter, whose ancient art was
dependent on fire,1 with some of the earliest burnt clay
objects recorded in areas of Czechoslovakia approximately 23,000 BC4,5 and Russia approximately 16,000
6
BC.
This review of the literature describes the development of glass, ceramic, refractory materials, and techniques over a period of 25,000 years, from the time of
stone-age man to their more recent introduction into
dentistry. A time line (Table I) illustrates some of the
more significant development trends, which were
sourced through the Archaeology Education Department of the British Museum, London, the Archives of
the British Dental Association Library, and through
MEDLINE from 1966 to the present.

Dental Instructor, Department of Adult Dental Care.

Dental Instructor, Department of Adult Dental Care.
c
Reader, Department of Adult Dental Care.
b

136 THE JOURNAL OF PROSTHETIC DENTISTRY

Fig. 1. Obsidian arrowhead, from Teotihuacan, New

Mexico.

EARLY MAN-MADE GLASSFORMING

TECHNIQUES
Early manufactured glasses were formed by the fusion
of quartz, sand, and natron in clay crucibles with the
addition of metallic oxides of copper, iron, or antimony
to provide color and vary the degree of opacity.7 It is
thought that these glasses were poured while molten
into open molds of carved steatite (talc or soapstone) or
molded clay. Alternatively, they may have been poured
onto a smooth surface before the mold was pressed into
the still soft mass.2,8 Among the earliest examples is an
amulet (charm against evil) thought to come from Sumerian Mesopotamia and suggested to date from around
7000 BC.1A number of historians have suggested that
the technique of mold-forming glass may be an adaptation of nonferrous metalwork technology.9 During the
Egyptian XVIII Dynasty (Menkheperra Thutmose III),
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Table I. History of glass and refractory materials and techniques

Time-line of mans early use of glass and refractory materials
Dolni figurines
Tools and jewelry
First refractory molds
First manufactured refractories
Lost wax technique
Glass casting

23,000
8,000
7,000
3,500
1,400
100

BC
BC
BC
BC
BC
BC

Evidence of first burnt clay artifacts

Pre-Neolithic period mans first use of naturally occurring glass (obsidian)
Ancient Egyptians use molds of Steatite to pour or press glass
Egyptians form glass vessels around a refractory core of mud, sand, and animal dung
Evidence of lost wax technique for metal and possibly glass casting
Phidias casts glass into a variety of shapes using clay molds

Introduction of glass and refractory materials and techniques into dentistry

Mayan civilization
Alexis Ducha teau
Murphy
Various researchers

400900
1774 AD
1833 AD
187099

Charles Henry Land

Charles Henry Land
Legro
Brodsky
Moore and Watt
Buonocore
Morrison and Warnick
McLean and Hughes
MacCullock
Francois Duret
Horn
Calamia
Mo rmann and Brandestini
Adair and Grossman
Sadoun
Wohlwend and Scharer
Techceram

1895
1901
1931
1933
1949
1955
1959
1965
1968
1971
1983
1983
1980
1985
1985
1990
1996

AD
AD
AD
AD
AD
AD
AD
AD
AD
AD
AD
AD
AD
AD
AD
AD
AD

AD

AD

First evidence of milled plugs (inlays) of jade or obsidian for esthetic purposes
Developed technique for fired porcelain dentures
Fabricated glass inlays using a platinum foil matrix
Continued to develop glass/porcelain inlays, using gold/platinum foil matrix and/or
refractory die support
Developed platinum foil matrix for fabricating porcelain crowns
Fabricated and fitted the first porcelain laminate veneers
Described use of acid to etch porcelain
Reported first manufactured refractory material for dental use (German-Brillat)
Developed phosphate-bonded refractory material
Reported method of chemically etching enamel
Reported findings of ethyl silicate refractory material for dental use
Developed alumina core material to strengthen dental porcelain
First reported the use of glass casting for dental purposes
First to consider the automatic production for dental restorations (CAD-CAM technique)
Combined etched enamel/porcelain technique to resin bonded restoration
Re-introduced the method of etching porcelain, for resin-bonded restorations
Developed chairside CAD-CAM system for machining dental porcelain (CEREC)
Developed the first commercial castable glass (Dicor)
First developed the alumina-infiltrated glass technique (In-Ceram)
Reported on a technique for pressed glass restorations (Empress)
Commercial introduction of thermal spray technique into dentistry

1527-1475 BC, hollow glass vessels were formed around

refractory cores.1,7,8,10 Although some uncertainty exists,
it has been suggested that these cores may have been
dipped into a glass previously heated in clay crucibles until
molten, or, alternatively, colored rods of softened glass
may have been wound around the core before being rolled
to obtain the desired shape (Fig. 2). Further evidence suggests that the lost wax casting process (cire perdue), used by
the Al Ubaid culture of Ur around 3500 BC11 for casting
metals into enclosed molds,12 was being adopted by these
14th-century Egyptian artisans for the forming of glass
ornaments2,9 (Fig. 3). However, by the 5th century BC,
glass was being cast into a variety of shapes by the Greek
sculptor, Phidias, using clay molds2 (Fig. 4).
It is probable that these soft clay molds improved the
speed of manufacture of hollow vessels, lessening the
possibility of damage during the divesting of the surrounding mold material.9 By the first century BC, glass
blowing techniques appeared in areas around Phoenicia.2,8 However, it was later refractory mold blown glass
that heralded a complete change in glass manufacturing
techniques that would not be matched until the introduction of mechanized methods in approximately
1820 AD.2
FEBRUARY 2004

Fig. 2. Core formed glass vessel of bulti-fish, designed to

hold scented oil, circa 1350 BC. Copyright The British
Museum.

EARLY MANUFACTURED
REFRACTORY MOLD MATERIALS
Although a considerable amount of information is
available about ancient glasses,13 little evidence has been
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WILDGOOSE, JOHNSON, AND WINSTANLEY

Fig. 5. Mayan tooth with jade inlay, circa 800 AD. Image
courtesy of British Dental Association Museum Collection
(LDBDA 7688).
Fig. 3. Intact refractory mold for early gold casting found in
Columbia. Image from Bray12 reprinted with permission from
World Gold Council.

binders of animal dung was used.2,4,14 It may be that

early glass manufacturers modified the compositions of
their refractories in order to achieve the particular refractory property required, as these molds would have to
demonstrate good dimensional stability,4 have a coefficient of expansion slightly greater than that of the glass
in order to prevent cracking,14 and be sufficiently soft to
scrape out.13 Archaeologists Bimson and Werner reported in 1968 at the International Congress on Glass,
London, that additions of calcite, lime wash, or clay
were applied to the surface of a wax pattern prior to
molding the bulk of the refractory, in order for fine
surface detail to be reproduced by both the mold materials and subsequent cast glass.

PORCELAIN/REFRACTORY
TECHNIQUES FOR THE
CONSTRUCTION OF DENTURES

Fig. 4. Sculpture of ram, cast in glass using closed mold

technique, circa 600 BC. Copyright The British Museum.

reported about the diversity of manufactured refractory

mold materials. This may be due in part to the disposable nature of the mold, and that on decomposition it
would be difficult to differentiate the individual materials from the natural surroundings from which they were
developed. Evidence shows that where hollow glass vessels were fabricated, a manufactured refractory core of
mud, sand, and highly ferruginous clay with organic
138

Although naturally formed glasses have previously

been mentioned as being used for general products in
the home or work place, the earliest evidence of glass or
ceramic materials being used for dental restorations was
found in the Central Americas. Asbell (1964, Outlook
& Bulletin, Southern NJ Dental Society) suggests this
dates from the Mayan classical period, AD 300-900, and
later 12th century Aztec civilizations when obsidian and
jade plugs were grounda similar principle to milling
and inlayed into previously prepared teeth for decorative
and esthetic purposes15 (Fig. 5).
The combination of refractory and ceramic materials
was not put into use in dentistry until 1774, when
French apothecary Alexis Ducha teau first requested the
fabrication of porcelain dentures from a Parisian porcelain manufacturer16-19 (Fig. 6). This appears to have met
with limited success; Pearlman, in 1959 (Proceedings of
the Wedgwood Society), stated that difficulty was encountered with uneven contraction of the various mateVOLUME 91 NUMBER 2

WILDGOOSE, JOHNSON, AND WINSTANLEY

Fig. 6. Set of porcelain dentures made in style of Nicholas de

Che mant, late 18th century. Original held by Odontological
Museum, Royal College of Surgeons of England, RSCOM
K1.1. Image courtesy of British Dental Association Museum.

rials. This may have been due in part to volumetric

shrinkage occurring within the porcelain paste materials
during the continued firing processes. A report by Moffit (1887)20 recognized that the warpage and cracking of
the porcelain body may be minimized by dispensing
with investments of plaster and pumice in favor of flint
sand when fabricating continuous gums, thereby encouraging a variety of materials and techniques to be
developed.

DEVELOPMENT OF INDIVIDUAL
FUSED PORCELAIN/GLASS
RESTORATIONS
One of the earliest records of individually fabricated
ceramic restorations was by Murphy in his treatise of
1837.21 The author describes a method of using porcelain, or rods of colored glass fused onto a thin platina
base, to form an inlay. By the 1870s, many inlays were
being ground from manufactured porcelain denture
teeth (a method similar to that of the early Mayan civilization) in order to overcome persistent problems with
FEBRUARY 2004

THE JOURNAL OF PROSTHETIC DENTISTRY

warpage of the foil and firing shrinkage of the powdered

ceramic.22-25 Land (1889)26 describes a method of improving the fit of porcelain fillings by burnishing platinum foil directly into the preparation. Simonis
(1890)27 cites Richter as developing a technique
whereby a colored glass was fused within a matrix of
platinum or gold previously formed by burnishing it into
the preparation. However, Darby (1899)28 described a
method of using pulverized asbestos to support a foil
matrix while fusing occurred. By the late 19th century,
various attempts were being made to use foil matrices,
either independently or in conjunction with what may
loosely be termed an investment mold, during the construction of porcelain and glass restorations.
Simonis, in 1890,27 recommended using pulverized
asbestos or a mixture of plaster and pumice to support
the foil matrix during firing, but failed to provide any
reason why this mixture was preferred. An undisclosed
investment was described by Nyman (1905)29 to support the platinum or gold matrix in order to prevent
warpage due to annealing of the foil matrix and shrinkage of the porcelain during firing. However, Jenkins
(1913)30 observed that whether a matrix was adapted
directly intraorally or indirectly on a cast, a noticeably
disfiguring cement lute, due to defective edges, was
more prevalent with porcelain restorations fabricated on
a platinum matrix than those on gold foil. During the
early part of the twentieth century, numerous authors19,31,32 cited Lands successful development
(1886) and subsequent patent (1889) of the platinum
foil matrix when fabricating ceramic crowns. This technique provided restorations with both a clinically acceptable fit and esthetic quality. The same technique was
again described by Land (1903)33 and much later by
Pincus (1937)34 for the fabrication of artificial ceramic
veneers. However, it was to be much later in the century
before this technique became popular.

DEVELOPMENT OF REFRACTORY DIE

MATERIALS AND TECHNIQUES
A number of investment materials have been reported
to provide direct support to the powdered porcelain or
glass restorative material during firing. Ernsmere35 cites
Herbst as fabricating a mold of plaster and asbestos from
a wax impression; unfortunately, no reason for the selection of material was provided. An investment mold
poured solely of plaster of Paris was preferred by Martin.36 A fine powder of ground porcelain (china cups)
was re-fused within the mold to fabricate the restoration. Simonis27 also recognized that, where deeper and
more angular preparations occur, it was advantageous to
pour a refractory cast of plaster and pumice from an
impression using modeling plastic impression compound.37 Martin36 cites Land as using plumbago (carbon) or sand mixed with plaster to make the investment
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WILDGOOSE, JOHNSON, AND WINSTANLEY

Fig. 7. A, Gypsum bound refractory after firing at 690C. B, Gypsum bound refractory after firing at 950C.

mold in order to fabricate restorations from a variety of

materials. Unfortunately, the author provides no indication as to the effect of plumbago on the color of the
resultant porcelain or glass restoration. A considerable
shrinkage of the fired glass was observed by Ernsmere,35
who suggested that even when a second refractory transfer mold was made, the resultant fit was less than satisfactory. These early twentieth century researchers continued to experiment with a variety of refractory
materials in an endeavor to overcome persistent problems with shrinkage of the refractory, and cracking of the
porcelain or glass during firing.

Gypsum-bonded refractory die materials

One of the first refractory investments commercially manufactured as a refractory mold material
when fabricating dental all-ceramic restorations was
German Brillat No. 2. This was reported in 1933 by
Brodsky38 as being a mixture of 70% mullite, 3Al2O3
2SiO2, a stable compound of alumina-silica which is
not affected by high temperatures,39 and 30% plaster
of Paris. A porcelain powder having a fusing point of
approximately 979C was applied and fired incrementally into the refractory mold. McCabe40 indicated
that because gypsum contracts on heating, it would
have been unsuitable by itself as an investment material. Phillips41 concurred, suggesting that gypsumbonded investments should not be heated above
700C, as decomposition of the gypsum occurs, causing tremendous contraction. In addition, chemical
modifiers, such as boric acid, added to reduce the
contraction of the gypsum binder,41,42 might disintegrate during heating of the mold, thereby resulting in
a rough surface to the metal casting.41 This surface
roughness was also observed by both Brodsky38 and
George43after removal of the refractory investment
material from a ceramic restoration.
140

It is important to recognize that, as dental porcelains

and glasses are fired more than once at temperatures of
approximately 950C, the observed contraction and
roughness may in part be attributed to a continued decomposition of the gypsum binder of the refractory investment (Fig. 7), which may have contributed to the
inaccuracy identified by previous workers.38,43

High heat investments and refractory die

materials
Although, the first high heat refractory was a phosphate-bonded material developed by Moore and
Watts44 in 1949, refractories were initially identified as
casting investments for use with a variety of dental alloys.45,46 However, it was not until 1959 that an ethyl
silicate bonded refractory was reported as the first
high heat refractory die material for the fabrication of
all-ceramic restorations.47 In 1964, Hobo evaluated a
range of refractory and ceramic combinations, reporting
that some material combinations provided a better overall adaptation than others (Master of Science thesis, Indiana University). Other workers continued to identify
problems with dimensional change, suggesting that to
compensate for a contraction of the refractory investment, judicial relieving of the ceramics axial wall, along
with other surface discrepancies, was necessary to allow
the restoration to be adequately adapted.48,49
During the mid-1960s, McLean and Hughes50
developed an alumina-reinforced glass-ceramic to inhibit crack propagation, thereby strengthening the ceramic core upon which the colored dental glass-ceramic
could be applied. This development has lead to a number of modifications, which rely upon the use of either
foil or refractory substrates for a variety of restorative
techniques.
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Fig. 8. Mismatched ceramic and metal thermal expansion

coefficients resulting in ceramic failure.

Fig. 9. Thermal expansion coefficient mismatch of ceramic

and refractory resulting in ceramic failure.

Table II. Mean dimensional change after firing for 7 selected refractory materials
Material
Results %

CeramiteH

CeramiteV

Corum

Flexo-Ceram

Hi-Ceram

Vitadurvest

Whipmix VHT

1st firing
2nd firing
3rd firing
4th firing
5th firing
6th firing

1.18 0.07*
1.24 0.08
1.23 0.08
1.24 0.07
1.25 0.08
1.24 0.07

0.45 0.08
0.51 0.08
0.50 0.08
0.51 0.08
0.53 0.09
0.51 0.08

0.34 0.04
0.32 0.03
0.32 0.04
0.28 0.04
0.29 0.03
0.27 0.04

0.90 0.02
0.91 0.02
0.94 0.02
0.95 0.02
0.96 0.01
0.94 0.01

0.08 0.02
0.08 0.04
0.09 0.02
0.10 0.02
0.11 0.02
0.11 0.02

0.00 0.05
0.03 0.05
0.03 0.06
0.02 0.07
0.05 0.07
0.04 0.07

0.12 0.04
0.08 0.02
0.09 0.03
0.08 0.05
0.07 0.03
0.07 0.03

From Wildgoose and Winstanely73 with permission.

*Mean SD

Refractory die materials for the fabrication of

conventional all-ceramic restorations and
laminate veneers
More recently, a variety of phosphate-bonded refractory materials have been described in the literature when
fabricating a range of all-ceramic restorations.51-56 In
1985, Calamia57 suggested the use of phosphatebonded refractory materials when fabricating all-ceramic
laminate veneers using conventional dental ceramic materials and techniques. However, problems of fit58-61
along with cracking59,60 and adherence of the ceramic to
the refractory material were again recognized.60 For
these reasons, some workers62-64 continued to advocate
using the platinum foil technique to avoid an interaction
of the porcelain with the refractory, while recognizing
the benefit from the support offered by an underlying
refractory cast. However, Hunt65 suggested that all-ceramic veneers made on refractory dies are less susceptible
to warping, and that thermal contraction may be controlled by reducing the size of the refractory die. The
marginal integrity of ceramic veneers fabricated on
matched and unmatched refractory dies was compared
by McIntyre et al in 1993,66 who concluded that a sigFEBRUARY 2004

nificant improvement in marginal accuracy was evident

where the ceramic and refractory were matched.
Many researchers have considered the residual
stress in a number of alloy-porcelain combinations,67-70 concluding that to minimize stress levels in
the veneering porcelain, the thermal expansion/contraction of the porcelain must be matched to the alloy
between its glass transition and room temperature
(Fig 8). Conversely, little has been reported regarding
the consequence of mismatch for current dental refractory and ceramic combinations71 (Fig. 9). Only
recently (2000) has an International Standard (ISO
11245)72 for phosphate-bonded refractory die materials been introduced.
A recent study by Wildgoose and Winstanley73
showed that a wide range of dimensional change occurred during setting, varying between 1.8% 0.05%
and 0.11% 0.02% at 24 hours for 7 phosphate refractory materials identified in a survey.71 When further
investigation was conducted, a final dimensional change
of between 1.24% 0.07% and 0.27% 0.04% was
evident upon completion of 6 identified firing cycles
(Table II). 73
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RECENT DEVELOPMENTS AND NOVEL

TECHNIQUES
There have been many developments in the use of
dental investment/refractory materials since the inception of phosphate bonded refractory materials. However, most of this work has related to metal-ceramic
restorations.
Although novel techniques using castable glass are
recorded as early as 1968,74 it is only since the mid1980s that refractory materials have become popular
when fabricating all-ceramic restorations. Such processes have included both cast (Dicor MCG; Dentsply
International, York, Pa)51 and hot-pressed (IPS Empress; Ivoclar Vivadent, Schaan, Liechtenstein)75,76 ceramics. Both systems utilize the lost-wax process (cire
perdue), requiring the wax pattern to be invested in a
uniquely developed phosphate-bonded refractory material.
For Dicor, the subsequent transparent cast glass is
cerammed in a controlled manner allowing a tetrasilic
mica crystal phase to develop within a glass matrix.51
The development of this crystal phase increases the materials compressive strength and opacity, providing a
substrate with a thermal expansion coefficient (TEC) of
approximately 7106C.
Empress, however, is a leucite-forming glass-ceramic
that is designed to be pressed into the preheated mold.75
These leucite-reinforced glasses are a further development of the early metal-ceramic systems in that the TEC
of the ceramic (approximately13106C) closely resembles that of the metals to which they are to be bonded.77
A particular benefit of both these glass-ceramics when
providing all-ceramic restorations is that they may be
readily etched using hydrofluoric acid solution,78
thereby providing a micromechanical surface which may
be subsequently resin-bonded to previously etched
enamel.79
Other novel techniques are those of In-Ceram (Vita
Zahnfabrik, Bad Sackingen, Germany)80 and Techceram (Techceram Ltd, Shipley, UK).81,82 Both are used
with specially designed stone or refractory die materials
to provide an alumina core base layer by means of either
a slip-cast or thermal spray technique, respectively. Unfortunately, these high-alumina-content ceramics are
difficult to acid-etch, although the manufacturers of
Techceram suggest that a microroughened intaglio surface is created during the thermal spraying process,
thereby optimizing the resin bond.81For some time the
dental industry has been trying to overcome inaccuracies
associated with the traditional, multi-stage production
of indirect restorations.83 There are now a number of
dental computer-aided design/computer-aided manufacturing (CAD/CAM) systems, since their first introduction by Francois Duret in 1971.84 Although these
142

WILDGOOSE, JOHNSON, AND WINSTANLEY

systems continue to improve, their capital costs are considerable, requiring a high production turnover in order
to achieve financial viability.

SUMMARY
There have been many novel refractory and/or ceramic developments. However, many have not been sustainable over time. This may be due to the initial capital
outlay, technique sensitivity, or a need to continually
develop the product in reaction to market forces.
Many conventional ceramic and refractory materials
are currently available, although problems encountered
by the early artisans and technologists relating to ceramic fracture and dimensional change (warpage) still
persist. To date, little has been reported regarding the
selection of refractory materials and laboratory techniques when fabricating all-ceramic restorations on refractory dies.
Information about the dimensional change after multiple firing and thermal expansion coefficients of refractories may enable the laboratory to select a compatible
refractory and ceramic combination.
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