Applied Radiation and Isotopes 83 (2014) 187191

Contents lists available at ScienceDirect

Applied Radiation and Isotopes

journal homepage: www.elsevier.com/locate/apradiso

Preparation methods of thermoluminescent materials for dosimetric

applications: An overview
Juan Azorin n
Autonoma Metropolitana-Iztapalapa Universidad Autnoma Metropolitana-Iztapalapa, Mxico D.F. 09340, Mexico

H I G H L I G H T S

A review of the main methods for preparing thermoluminescent materials is presented.

Emphasis is placed on the methods to produce materials with suitable characteristics for ionizing radiation dosimetry.

As a conclusion it can be said that chemical methods have advantages on physical methods to produce TL materials.

art ic l e i nf o a b s t r a c t

Available online 11 June 2013 Many different natural minerals and synthetic inorganic compounds present the phenomenon of
Keywords: thermoluminescence (TL); however, only a part of them satisfy the requirements to be used as TL
Thermoluminescent materials dosimeters. The mechanism of excitation energy transformation into the output of light is one of the
Phosphors most important points in the TL materials designing. Both the threshold detection dose and accuracy of
Preparation methods measurements depend on the efciency of energy transformation.
The role of diverse mechanisms of energy transfer and energy losses is very different depending on
the nature of the TL material and its composition including intrinsic defects and those induced by
impurities. The structure of these defects can be controlled to a high extent by the preparation method.
That is why the most important fact is to nd the interrelations among the preparation methods, the
structural defects and the TL properties of the material.
The aim of this paper is to give a selected review on the preparation methods of the most popular and
commercially available phosphors as well as those less used or homemade for special studies.
& 2013 Elsevier Ltd. All rights reserved.

1. Introduction by impurities. The structure of these defects can be controlled to a

During the last four decades the application of thermolumines-
cence dosimetry (TLD) in radiation protection has grown steadily
in parallel with the worldwide progress made in the development
of solid thermoluminescent (TL) dosimeters.
Today, TLD is the dominant dosimetric method for the mea-
surement of doses in medical physics personnel dosimetry and
environmental monitoring. Different preparation methods and
properties of several TL materials have been studied so far.
The mechanism of excitation energy transformation into the
output of light is one of the most important points in the TL materials
designing. Both the threshold detection dose and accuracy of mea-
surements depend on the efciency of energy transformation.
The role of diverse mechanisms of energy transfer and energy
losses is very different depending on the nature of the TL material
and its composition including intrinsic defects and those induced
high extent by the preparation method.
That is why the most important fact is to nd the interrelations
among the preparation methods, the structural defects and the TL
properties of the material.
Not all the numerous known TL materials are suitable to be
used as radiation dosimeters. For dosimetric uses a TL material is
expected to have the following characteristics.
Relatively simple glow curve with the main peak at about
200 1C, high sensitivity and stability (low fading), resistance to
environmental factors, independence of the radiation energy, good
linearity in the specic useful range of dose.
Only a few materials have been found so far to match all the
above characteristics. However, research in this area is ongoing
and is expected new appropriate TL materials to be developed in
the near future.
2. Preparation methods

n
Tel.: +52 55 58044600x1151; fax: +52 55 58044611. Preparation method of TL phosphors is critical because it
E-mail address: azorin@xanum.uam.mx generally controls the nal properties of the materials, different

0969-8043/$ - see front matter & 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.apradiso.2013.04.031
188 J. Azorin / Applied Radiation and Isotopes 83 (2014) 187191
preparation techniques are generally based on powder processing
with powder synthesis. However, TL materials processing has also
to consider other techniques of synthesis and crystal growth, such
as thin lms and bulk with desirable microstructures and nanos-
tructures architectures. Structural properties of the materials
change their TL properties, as well as, thermal treatments for
sintering process, by changing the crystallites size particles.
Typically the product of the synthesis of an inorganic material
is a polycrystalline substance which is obtained in powder form.
However, in many cases it is required that the material is obtained
in special forms such as single crystals and thin lms. The required
form is logically determined by the use or application that will
give the material.
Obtaining a single crystal is very important when it comes to
structural characterization. Single crystals are also required for use
in optics and electronics, as many times for certain properties are
anisotropic. Single crystals for thermoluminescent dosimetry are
not suitable because they usually do not have the dopant dis-
tributed homogeneously, so that to obtain a homogeneous mate-
rial, the crystal must be ground.
The thin lm, amorphous or both as mono or polycrystalline
are very important in modern technology. They can be used to
form protective covers on other materials and have played an
essential role in the miniaturization of components of electronic
devices, but also are useful in TLD dosimetry for low energy
radiation. Another important feature is that their properties are
often different from the properties of a bulk material, which is
derived from the large area/volume ratio they possess.
The TL dosimetric materials currently available can be grouped
into two main categories (Azorn, 1990):
(a) Tissue equivalent phosphors, which have an effective atomic
number in the range from 7 to10 and generally show low
sensitivity, such as alkali halides, alkali borates and alkaline
earth metal oxides. For example: LiF, Li2B4O7, BeO, etc.
(b) Phosphors with atomic numbers ranging from 15 to 18, with
high sensitivity but no tissue equivalents such as salts of
alkaline earth metals, and metallic oxides. For example: CaSO4,
CaF2, Al2O3, ZrO2, TiO2, etc.
In general, nominally pure compounds show weak TL signal, and
are not considered efcient dosimetric materials. Much higher
efciency is obtained by doping such materials with proper
impurities which act as activators of TL phenomenon. The impurity
is normally chosen on the basis of the highest TL response, but other
important dosimetric characteristics must be taken into account.
Then, the search of good dosimetric TL materials, points to an
optimized coupling of a suitable host material with a dopant of very
high efciency to be easily introduced into the desired TL phosphor.
The preparation method used depends on the physical form
required for the TL material, either polycrystalline powder, single
crystals or thin lms (Azorn et al., 1993a). Most commonly used
methods for obtaining polycrystalline powder are precipitation
and evaporation; while for single crystals, most commonly used
methods are those of Czochralski, zone melting and precipitation
from solutions or molten phases (ow method). While for thin
lms, the most common methods are chemical vapor deposition,
spray pyrolysis and solgel. Below is a brief description of the
above mentioned methods:
2.1. Precipitation method
In this method, a solution of the precursor reactants is mixed
with dopants in acid solution. Once the precipitate has the desired
compound, the sample is centrifuged and washed repeatedly. The
precipitate is treated at high temperature, then cooled to room
temperature and dried in an inert atmosphere. Thereafter, the
temperature is raised to higher temperature, holding for a time.
Subsequently, the sample is moved slowly toward a zone of lower
temperature to crystallize, then the sample is removed from the
furnace by cooling rapidly to room temperature. Finally, the
product is pulverized and sieved, selecting powder with desired
grain size (Zumdahl, 2009). This method has been used by some
authors for synthesizing diverse materials such as alkaline earths
suldes (Rao, 1986), metallic oxides (Kumar et al., 1994; Azorn-
Vega et al., 2007), strontium aluminate (Chengkang et al.), calcium
phosphate (Madhukumar et al., 2007), lithium uoride (Vu Thi
Thai Ha et al., 2007) or calcium sulfate (Rivera et al., 2010).
2.2. Evaporation method
This method consists in homogeneously mixing the reactants in
acid solution by adding the dopants in the desired concentration.
The mixture is placed in a sealed system for evaporating at a high
temperature for a given time, by carrying the acid with an air or
nitrogen ow. Crystallization is controlled by varying both the
temperature and the gas ow. After the evaporation, crystals whose
dimensions depend on both the initial reagents and the type and
concentration of the dopants are obtained. Crystals obtained are
washed several times to remove the remaining acid and submitted
to a thermal treatment at high temperature. Finally, the product is
pulverized selecting powder with a desired grain size.
Evaporation is the well-known method most widely used to
produce calcium sulfate singly doped or co-doped. Considerable
work has been done on singly or co-doped CaSO4 phosphors in the
last few decades. Rare earths, especially Dy or Tm have been used
as dopants (Yamashita et al., 1971; Prokic, 1978; Azorn et al., 1980;
Azorn et al., 1984; Azorn and Gutirrez, 1989). This method has
been also applied by Furetta et al. (2000); by Ege et al. (2007), for
producing lithium borates. The evaporation method has also been
used to produce metallic oxide TL phosphors (Azorin et al., 2002;
Rivera et al., 2002).
2.3. Czochralski method
In this method a single crystal is grown from a melt of the same
composition. A crystal seed is brought into contact with the
surface of the melt, whose temperature is maintained slightly
above the melting. Withdrawing the seed slowly goes over to the
surface and the melt solidies in the same crystallographic
orientation than the original seed. The growing crystal and the
crucible with the molten usually rotate in opposite directions
during extraction, so as to maintain a constant temperature.
Usually employs an inert gas (argon or xenon) at a high pressure
to prevent volatilization losses (Mller et al., 2004). Jiri Kvapil et al.
(1980) have used this method to produce corundum single crystals
to be used as TL materials. Rare earths phosphates have been also
prepared as TL materials by using the Czochralski method (Bold
et al., 1985). Kelemen et al., 2011 have prepared lithium tetra-
borates single crystals by the Czochralski method.
2.4. Zone melting
In this well-known method crystals are grown by slow cooling
of the small molten zone. Under these conditions the atoms are
arranged such that the crystal is formed with a preferential
orientation (Pfann, 1966). Lithium uoride has been produced by
using this method by Watcher (1982).
2.5. Precipitation from solutions or molten phases. (Flow method)
In this method the crystal growth occurs from a liquid
phase of different compositions to the crystal; for example,
 J. Azorin / Applied Radiation and Isotopes 83 (2014) 187191
crystallization of a hydrated salt from an aqueous solution. It is
also the case that the solvent may be a liquid phase that has no
compositional relationship with the desired crystals (Kimura,
2011). For example, the SiO2 may be precipitated as crystal from
molten halides or borates (these compounds have low melting
temperatures). In these cases, the molten solvent is called
ow because effectively reduces the melting temperature of
the crystals in a large magnitude. Lasky and Moran (1978) used
this method to produce LiF TL phosphors. Other TL materials
produced by this method have been different metallic oxides
(Jayaramaiah et al., 2011), some perovskites (Mendoza-Mendoza,
et al., 2012).
2.6. Chemical vapor deposition (CVD)
The method uses some of the principles related to chemical
transport reactions in the vapor phase, allows obtaining very pure
crystalline lms of semiconductors, including the type IIIV. The
lms are formed by decomposition of gaseous molecules (Dobkin
and Zuraw, 2003). The decomposition is performed by pyrolysis,
photolysis or chemical reaction. The lms deposited by this
method tend to be coupled to the structure of the substrate,
resulting in epitaxial growth mechanisms (preferential growth in
both directions of the substrate surface).
Diamond is one of the most popular TL materials which is
prepared by the CVD method (Borchi et al.,1996; Barboza-Flores
et al., 2003; Karczmarska et al., 2011).
2.7. Spray pyrolysis
In this case, a spray formed by a carrier gas (inert to the system)
and the solution containing the substance to decompose on the
surface of the substrate to yield the desired lm, is impinged on a
substrate heated up to the appropriate temperature. It must be
used substances which decompose at relatively low temperatures
and do not let other solid waste that those must form the lm
(Gurav et al., 1993).
Acetates of different cations are widely used as substrates for
obtaining oxide lms, although also suldes can be obtained.
Many TL materials, both in powder and lm, have been prepared
successfully using the spray pyrolysis method (Azorn et al., 1998;
Garca-Hiplito et al., 2001; Lee et al., 2001; Azorn et al., 2002;
Oztas, 2006; Gmez et al., 2007).
2.8. Solgel
The solgel process is an efcient method which uses the same
type of reactions among the precursors as the other methods,
followed by condensation to yield a polymeric network. Just as the
sol or gel is applied to the substrate and then submitted to a
thermal treatment to remove undesired organic matter (Brinker
and Sherrer, 1990).
This method is very good for obtaining aluminates, oxides,
nitrides, phosphates and suldes (Bao et al., 2007; Aguilar et al.,
2001; Rivera et al., 2007a; Rivera et al., 2010).
3. Thermoluminescent materials
3.1. Tissue equivalent phosphors. Among tissue equivalent
phosphors, some of the most used are LiF, Li2B4O7, BeO, etc.
3.1.1. Lithium uoride (LiF)
Lithium uoride doped with magnesium and titanium (LiF:
Mg,Ti) is widely used for personnel, clinical and environmental
189
dosimetry. Recently the LiF:Mg,Cu,P has been produced and, due
to its high sensitivity, became a standard in modern TL dosimetry.
One of the most used methods to prepare LiF:Mg,Ti is the
precipitation method. This method has been applied as follows
(Azorn et al., 1993b): A few mililitres of a solution of MgCl2 is
added to a solution of LiCl. Meanwhile, metallic titanium is
dissolved in HF, and then the rst mixture is slowly added. Once
LiF is precipitated, the sample is centrifuged and washed repeat-
edly. The precipitate is dried and cooled to room temperature
adding a few mililitres of LiCl solution. This wet material is dried
and then oven heated at a constant temperature during the
desired time, then the sample is moved to a lower temperature
zone to allow crystallization, and then taken out of the oven to be
rapidly cooled to room temperature. Finally, the product is crushed
and sieved to select powder with the desired grain size. In the case
of LiF:Mg,Ti prepared by the above method, the TL response is
linear in the range from 100 mGy up to about 6 Gy, beyond which
superlinearity appears.
LiF:Mg,Cu,P has been developed as a phosphor of low effective
atomic number but high sensitivity. One of the preparation methods
of this phosphor (Azorn, 1990) consist of obtaining rst undoped LiF
from the reaction LiCl+HF-LiF+HCl. Once LiF was precipitated,
dopants in aqueous solution are incorporated until the desired
concentrations are reached. The material obtained is dried and
washed repeatedly. This dried material is oven heated at a constant
temperature during the desired time, and then the temperature is
raised at a higher value and then lowered until medium tempera-
ture and suddenly to room temperature. Finally, the resulting
polycrystalline material is crushed and sieved to select powder with
the desired grain size. The phosphor prepared following this
method, gives linear response between 0.1 mGy and 100 Gy.
3.1.2. Lithium borate (Li2B4O7)
This material has an effective atomic number 7.3 that makes it
tissue equivalent and encourages studies on its TL properties and
preparation methods for dosimetric applications.
One of the most popular methods for preparing Li2B4O7 is the
melting zone method (El-Faramawy et al., 2000) which consists in
mixing Li2CO3 with H3BO3 in the stoichiometric ratio and sufcient
aqueous solution of the desired dopants is added. After stirring and
desiccation, the mixture is melted and rapidly cooled to room
temperature. The resultant material is reheated to assure a com-
plete crystallization, and then ground and sieved to select powder
with the desired grain size. Good performances are reported for
Li2B4O7 doped with Cu, Ag, P or Mn impurities (Singh et al., 2012).
3.1.3. Beryllium oxide (BeO)
This material exhibits a photoelectric absorption equivalent to
that of the biological tissue, the effective atomic number being
equal to 7.4, and excellent TL characteristics when doped with
suitable impurities. This phosphor is obtained by mixing puried
BeO powder and an alkali sulfate, pressing the resulting mixture to
obtain discs or rods, sintering at high temperature, and then
cooling gradually to room temperature (Yamashita et al., 1974).
The glow curve of BeO consist in a single peak at about 180 1C,
showing a TL intensity three to ve times larger than that of LiF. Its
TL response as a function of dose is linear up to 1 Gy.
3.2. No-tissue equivalent phosphors. Among no-tissue equivalent
phosphors, some of the most used are CaSO4, CaF2, Al2O3, ZrO2, TiO2,
etc.
3.2.1. Calcium sulfate (CaSO4)
This phosphor is one of the most sensitive TL materials used in
dosimetry. Evaporation method has been adopted for preparation of
190 J. Azorin / Applied Radiation and Isotopes 83 (2014) 187191
such materials (Azorin et al., 1980; Azorin et al., 1984). CaSO4 is
obtained by dissolving Ca(NO3)2 in concentrated H2SO4. The dopants,
in the required concentration are added and the reagents thoroughly
stirred in a ask connected to a sealed condenser system with
constant air ow as carrier for the acid vapor. Crystallization can be
controlled by varying the temperature and the air ow rate. The
product is washed several times to remove all remaining acid and
thermally treated. This material is ground and sieved to select
powder with the desired grain size. These phosphors have a linear
TL response from few miligray up to 100 Gy.
This material has been prepared also by the precipitation
method (Rivera et al., 2010) consisting in the following: calcium
acetate is dissolved in a minimum quantity of double distilled
water to which a few mililitres of ethanol is added. A solution of
thiourea in water is added to calcium acetate solution and the
dopant in appropriate amount is also added to the solution so as to
give the desired concentration. Ammonium sulfate (NH4)2SO4 is
also dissolved in a minimum amount of distilled water to which a
few mililitres of ethanol are added. (NH4)2SO4 solution is then
added to calcium acetate solution drop wise under vigorous
stirring. White precipitate powder is formed which is then
centrifuged and washed several times to remove the residual salts.
The precipitate is dried in an oven. Finally, the dried sample is
submitted to a thermal treatment.
3.2.2. Calcium uoride (CaF2)
Calcium uoride is no tissue equivalent (Zeff 16.57); it has
been used as a TL dosimeter since 1865 in form of natural uorite.
Both natural and synthetic CaF2 doped with Mn or with rare earths
have been used in TL dosimetry.
A technique for the preparation of CaF2 is the precipitation
from a solution of calcium chloride and ammonium uoride
(CaCl2+2NH4F-CaF2+2NH4Cl)
(Mahesh et al., 1989). The precipitate is dried and heated at a
high temperature in an inert atmosphere, powdered and graded.
TL response of CaF2 is linear up to 2 Gy.
3.2.3. Aluminum oxide (Al2O3)
Aluminum oxide is one of the former materials studied for
possible use as a dosimeter because chromium substitution for
some atoms of aluminum in Al2O3 changes sapphire into ruby
which exhibits TL properties studied since sixties.
One of the most popular methods for preparing Al2O3 is by
evaporation (Barros et al., 2010) from a solution prepared by
mixing appropriate amounts of analytical-grade aluminum nitrate,
urea and the desired dopant, in deionized water. Urea is used as
the reductive fuel for the combustion reaction. The solution is
heated in a hot plate to evaporate the excess of water. After this,
the mixture is transferred to a pre-heated mufe furnace where it
spontaneously ignited within a few seconds. In order to stabilize
the traps, powder obtained is submitted to a specic thermal
treatment at high temperature. The nal product is crushed and
sieved to select powder with grain sizes in the desired range.
The TL response of Al2O3 is linear from 2.4 to 3000 J cm2 of UV
spectral irradiance, and from 50 mGy to 5 Gy of 60Co gamma
radiation (Azorin et al., 2002). This phosphor can be prepared also
as thin lm by the spray pyrolysis method. The spraying solution is
prepared by mixing dimetylformamide with an aluminum acetyla-
cetonate. Doping is achieved by adding to the solution the acet-
ylacetonate of the dopant in the desired concentration. By varying
the deposition temperature and time, lms of different thicknesses
are obtained on substrates of silicon or quartz (Esparza et al., 2000).
3.2.4. Zirconium oxide (ZrO2)
There is a considerable research interest in ZrO2 engendered by
their various technological applications. ZrO2 is known to exist in
three polymorphs: monoclinic, tetragonal and cubic. The physical
and chemical properties of each phase and the role that play dopants
are crucial to decide its application in radiation dosimetry. ZrO2 is
prepared by the evaporation method from a solution consisting of a
mixture of zirconium hexachloride dissolved in ethanol. This mixture
is heated until all the solution be evaporated obtaining an amor-
phous powder. This powder is then submitted to a thermal treatment
in order to stabilize the traps (Rivera et al., 2002). Another method
for preparing ZrO2 is the solgel technique (Rivera et al., 2007b)
which consists in dissolving zirconium propoxyde and propanol in
double-distilled deionized water at room temperature and adding a
water soluble salt of the dopant in the desired concentration. The
components are stirred in order to obtain a uniform and homo-
geneous solution. Then the transparent and homogeneous solution is
placed in a dark place for drying under room conditions. At the end of
this period a transparent xerogel is obtained. Finally, the material is
submitted to a thermal treatment.
3.2.5. Titanium oxide (TiO2)
Interest in titanium oxide-based ceramics has increased con-
siderably in recent years as possible TL dosimeters which could be
used in a wide variety of research activities and applications of
ionizing radiation dosimetry. TiO2 is produced by the co-
precipitation method (Azorn-Vega et al., 2007) starting from
titanium oxysulfatesulfuric acid complex (TiOSO4  H2SO4  H2O)
and a chloride of the dopant. Interest in this method to produce
TiO2 arises from its relatively low cost and the approach that allows
the chemical content and concentration ratio of the elements of the
derived powders to be tailored, with ready fabrication into different
solutions. This material is also prepared by the solgel method
(Mendoza-Anaya et al., 2004), using titanium tetrabutoxide, (TBT)
as a precursor of TiO2. The synthesis is performed at room
temperature, dissolving TBT in ethyl alcohol and shaking for few
minutes; and then, adds the water and nitric acid, continuing the
stirring until gelation. The materials, in powder form, are dried and
thermally treated at different temperatures.
4. Conclusions
The precipitation method not only has the advantages of being
a simple process, suitable for doping and low production cost, but
also can be prepared particles of uniform small size, because the
precipitants are formed slowly and uniformly throughout the
solution during the precipitation process.
Evaporation method is the well-known technique most widely
used to produce sulfates and metallic oxides. We also think that
acid evaporation method is always a better choice to prepare
sulfate phosphors than the precipitation method.
Czochralski and zone melting methods have the advantage of
producing large crystals in a relatively short time and the equip-
ment is relatively simple, but the crystalline quality may be poor
due to the presence of inhomogeneities and high concentrations of
structural defects.
Flow method requires to have detailed information of the
phase diagram of the system involved. Due to that in this method
isothermal conditions and low velocities of growth are used, the
crystals obtained have few defects, but may be contaminated with
the material used to uidize or container.
Chemical vapor deposition (CVD) is a widely used method to
which numerous variations have been established. With this
method metal oxides, semiconductors and insulating materials
can be grown successfully.
Spray pyrolysis method is a fast and economical technique, but
has the disadvantage of requiring precise control of many para-
meters (concentration, ow, spray height, substrate temperature,
 J. Azorin / Applied Radiation and Isotopes 83 (2014) 187191
etc.). Many TL materials, both in powder and lm, can be prepared
successfully using this method.
Solgel method is very good for obtaining a variety of TL materials
such as aluminates, oxides, nitrides, phosphates and suldes.
As a conclusion, it can be said that chemical methods have
advantages on physical methods in which the facilities are often
more simple, but must be carefully selected the reaction system
and the conditions under which the processes are performed.
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