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Physica B

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

A. Ranaivosoloarimanana , T. Quiniou, M. Meyer, J.M. Boyer, F. Rocca

a Cedex, New Caledonia

Pole Pluridisciplinaire de la matie`re et de lEnvironnement (PPME EA 3325), Universite de la Nouvelle-Caledonie, BPR4 - 98851 Noume

a r t i c l e in fo

abstract

Article history:

Received 13 November 2008

Received in revised form

19 May 2009

Accepted 4 June 2009

In this paper, we use an XRD-based 100% approach method to quantify the activity evolution of phase

transformation from annealed powder Mg(OH)2 to MgO. The sample is chemically synthesized. The

isothermal phase transformation is carried out between 300 and 310 1C. The ratio of reacted magnesium

hydroxide is applied and compared with different existing models. The Avrami model An appears to be

the most close-tting. An order of reaction between 1.5 and 2 is observed that it could be considered as

a complex combination of different phenomenon, for which we test different models.

& 2009 Elsevier B.V. All rights reserved.

PACS:

61.05.cp

64.70.K

65.80.+n

Keywords:

Magnesium hydroxide

Powder X-ray diffraction

Kinetic

Thermal decomposition

100% approach

1. Introduction

Magnesium hydroxide and oxide are widely used for industrial

applications. Magnesium oxide is found as pigment in paints, in

neutralizing agents, pharmacological products and sport grips.

Magnesium hydroxide is a component used in re retardant and a

common component of pharmaceutical antiacids and laxatives.

Magnesium hydroxide is a soil constituent.

Magnesium oxide can be obtained in different ways but one of

the most widespread is the thermal decomposition of magnesium

hydroxide [13]. MgO is the product of the isothermal heating of

Mg(OH)2 by the following equation:

MgOH2 ) MgO H2 O:

(1)

the reaction temperature. The study of kinetic decomposition is

reported in numerous studies. The mechanism can be described

using physical and chemical models [4]. The chemical model is

based on two steps, i.e. nuclei formation and the growth of the

dehydrated phase. Several models, which have been developed

from different nucleation and growth laws, were listed by

Sharp et al. [5] and are noted as Dn, Rn, F1, An. In the case of an

Corresponding author. Tel.: +687 26 58 00; fax: +687 25 48 29.

albertranai@yahoo.com (A. Ranaivosoloarimanana).

0921-4526/$ - see front matter & 2009 Elsevier B.V. All rights reserved.

doi:10.1016/j.physb.2009.06.043

reaction is controlled by the growth step, for which the ratelimiting step can be carried out using a diffusion mechanism or

interfacial reaction [6]. Dn and Rn models are the models that

consider the diffusion mechanism and the interfacial reaction,

respectively. n is a parameter that depends on the particle shape.

For the model F1, nucleation and growth remain two successive

steps but the growth is considered instantaneous. Unlike complex

models, which take the competition between the nucleation and

growth process into account, the three aforementioned models

are dened as limits. The An model is one of the complex models

developed from a volume random germination and an isotropic

nucleus growth. It was implemented by Kolmogorov et al. [7] and

is thus known as the KJMA model. n depends on both the particle

morphology and the nucleus shape.

Numerous studies have reported on the thermal decomposition of magnesium hydroxide over the past 70 years [812]. These

studies were carried out in order to obtain the activation energy of

magnesium hydroxide decomposition and led to the establishment of the rst kinetic decomposition models. These studies

include the work of Anderson et al. [9] who examined the

isothermal decomposition of precipitated magnesium hydroxide

by thermogravimetric analysis under vacuum. They modelled

their results by phase boundary controlled mechanism in 2D as a

kinetic model. Turner and Hoffman carried out a similar study at

atmospheric pressure with a differential thermogravimetric

device. Using an isothermal and non-isothermal experimental

ARTICLE IN PRESS

3656

protocol, the model employed to describe the kinetic of precipitate magnesium hydroxide decomposition is a two thirds

order reaction model. More recently Halikia et al. [13] implemented the isothermal thermogravimetric method on pure

magnesium hydroxide. They showed that the kinetic mechanism

depends on temperature. At 350 1C, the data can be tted by a F1

kinetic law, while at 400 1C it is the A2 Avrami model that provides

the best t. At 450 and 500 1C, it was found that the controlling

mechanism remains the nucleus production as described by the

An model. The use of the An model is reported again by Yue et al.

[14] who studied magnesium dehydratation with a non-isothermal thermogravimetric analysis. Thus, the determination of

kinetic behaviour and parameters as activation energy remains

unclear in the case of magnesium hydroxide as for another

crystallized phase [15].

In other studies, the quantitative X-ray powder diffraction is

applied to different experimentations as monitoring phase

analysis [16] or in situ following crystallization, using classical

X-ray apparatus combined with synchrotron radiation [17,18]. The

recent development of an X-ray detector, which reduced the time

needed to perform the data acquisition (curved detector, for

example) enables thermal kinetic monitoring using a laboratorys

X-ray apparatus.

Moreover, previous studies have presented MgO thermal

kinetic investigation based on a Jensen treatment [19]. Recent

studies present suitable quantitative phase determination, which

is based on the 100% approach that takes into account the

intensity of all diffraction peaks [20]. In this study, we propose to

use it for the data treatment of the thermal analysis of magnesium

hydroxide particles carried out in situ X-ray diffraction equipped

with a curved detector.

The second section of this article details the technical

characterization of the particles and the experimental procedure

for the data treatment. The third and fourth sections demonstrate

the data obtained and their application to a literature model in

order to determine the most suitable model.

0.031.

Using both an X-ray diffractometer and a furnace, it becomes

possible to investigate the phase evolution of hydroxide while it

transforms into oxide. Compared to more traditional methods,

such as thermo-gravimetry or calorimetry, X-ray diffraction

allows us to follow up the phase evolution of every diffraction

plane [h k l]. [h k l] are Millerss indices. However, far more time is

required to perform a full-pattern analysis, but this can be

reduced using a curved detector. During our experiments, each

diffraction pattern containing full-pattern diffractogram was

cumulated over 10 min period. The nal output le included all

diffraction patterns, the rst one being the hydroxide and the last

one the oxide.

(c) Data treatment: The diffraction le is analysed using

laboratory-made software developed under Matlab (V7.0 (R14)).

It is designed to automatically enable the processing of multiple

diffraction patterns. The nal purpose of this software is to

investigate the thermal decomposition kinetic of a sample using

an X-ray diffractometer. Particular emphasis is given to the design

and implementation of the user interface.

In the rst stage, diffraction patterns are extracted individually

from the output le. Each diffractogram is then processed and

tted using analytical pseudo-voigt functions [22]. The background, linear in a rst approximation under each peak or group

of peaks, is jointly tted and removed. All of the detected

diffraction peaks are indexed to Mg(OH)2 or MgO crystal planes

from ICDD PDF-2 cards [23]. The software can display different

gures, such as variations of peak intensity, peak position, and

particle size versus time for a given temperature (isothermal

mode) or versus temperature for non-isothermal mode. It can also

display the evolving phase fraction during the Mg(OH)2 sample

transformation. Finally, the experimental curves are compared to

the most important rate equation used in the kinetic analysis of

solid state reactions.

2. Experimental technique

2.1. Particle synthesis [21]

Magnesium hydroxide Mg(OH)2 particles are synthesized by

adding 50 ml of an alkaline solution to 50 ml of a magnesium

nitrate Mg(NO3)2 solution, the molar ratio of base to magnesium

is 50%. This mixture is heated at 80 1C for 60 min under vigorous

stirring. After cooling, the precipitate is isolated by centrifugation and stirred in water. Isolation of precipitate and redispersal in water is performed ve times. Then water is

evaporated at 40 1C.

2.2. Particle characterization

(a) TEM: The morphology of the particles is determined by

transmission electron microscopy (JEOL 100 CX2). Dilute suspensions of Mg(OH)2 particles are dispersed in ethanol using

ultrasonic vibrations and deposited on a carbon-covered grid,

then ethanol is evaporated.

(b) X-ray diffraction: The thermal decomposition of magnesium

hydroxide is carried out in air in an Anton-Paar TTK450 furnace.

During calcination, the powder X-ray diffraction patterns are

acquired using an INEL diffractometer operating at 30 kV and

30 mA. The transmitted X-ray beam is produced from a ltered

cobalt source Ka1 (l 0.178897 nm). The intensity of the

diffracted beam is recorded with a curved position-sensitive

sample quantities and by the moisture. To avoid this interference,

all of our data are obtained from 25 mg of Mg(OH)2 and our

furnace is maintained at 150 1C for a period of 2 h prior to each

experiment to dry the sample [1].

(a) Selection of a suitable isothermal temperature: As a rst step,

linear temperature scanning measurements are carried out to

determine the best temperature interval for the next step, i.e.

isothermal analysis. The temperature for the isotherm experiments are chosen just before a phase transformation (Fig. 1). The

choice is made to avoid a long-time measurement if the

temperature is too low; the beginning of phase transformation

is lost if the temperature is too high.

In order to evaluate the suitable temperature range, diffraction

patterns are measured at regular scanning temperature intervals

between 200 and 400 1C. Fig. 2 shows the diagram evolution

for this rst step. The average temperature variation is

dT/dt 0.5 1C/min.

The second step involves the implementation of the X-ray

diffraction analysis and characterizations for the isothermal phase

shift from Mg(OH)2 to MgO. The selected temperatures for the

isothermal analysis of the magnesium hydroxide sample are 300,

305 and 310 1C. Fig. 3 shows isothermal phases diagram evolution

of Mg(OH)2 to MgO chosen between 300 and 310 1C.

Once the method, the main parameters of analysis and the

isothermal temperature interval have been chosen and determined, an isothermal measurement is carried out. The processing

ARTICLE IN PRESS

A. Ranaivosoloarimanana et al. / Physica B 404 (2009) 36553661

3657

crystalline plane and the concentrations of Mg(OH)2 and MgO.

Thus the Mg(OH)2 fraction reacted ratio on isothermal annealing

can be determined.

(b) Ratio a determination: We denote by a the ratio of MgO

product. The empiric value of the Mg(OH)2 fraction reacted ratio is

determined using the ratio of the modelled surface peaks of

Mg(OH)2 and MgO. The relation of the X-ray powder diffraction

peak, the structural factors and scattering factor, and their

application for mixed phases can be found in the literature [24].

Another method for the calculation of the phase ratio used by

Jensen [19] can be found using the following formula:

at

(non-isothermal measurement).

Ii t Imin

,

Imax Imin

(2)

mixture phases.

Another method, which is slightly different to Eq. (2), is used to

determine the ratio a in this study. The method uses the tted and

modelled integral intensity peaks so-called 100% approach.

The 100% approach method is described by Kahle [20]

introducing mineral intensity factors (MIFs), denoted by Z. To

adopt Kahles denitions, the mineral intensity factor describes

the relationship between the intensity ratio of specic X-ray

diffraction peaks and the weight fraction ratio of two phases in a

mixture. The term 100% approach means that the sum of all of the

phase quantities identied in a sample is 100%.

We also use full-pattern methods to perform quantitative

phase analysis. Full-pattern methods consist in tting complete

experimental diffraction. In our case, we use the entire 1201

aperture for diffraction angle 2y.

According to the Kahle equation [20], the integral intensity I of

the specic diffraction peak of the given phase is

I K W U,

(3)

U is function of the mean mass absorption coefcient and the

structure factor of the mineral.

Then in a mixture of the two phases i and j, a peak intensity

ratio could be described as

Ii

Wi

Ui

.

(4)

Ij

Wj

Uj

Fig. 2. Temperature ramp for annealed Mg(OH)2.

and the weight fraction W i of phase i mixed with any phase n is

determined by

I =Z

.

Wi P i i

n In =Zn

Fig. 3. Diagram evolution for annealed Mg(OH)2 chosen between 300 and 310 1C.

(5)

determined using the following formula:

P

hkl IMgO

P

a P

,

(6)

f S hkl IMgOH2 hkl IMgO

P

where

intensity sum of all [h k l] tted

hkl IMgO is the integral

P

MgO peaks for MgO and hkl IMgOH2 for all [h k l] tted Mg(OH)2

peaks. To make this calculation, as shown, for example in Figs. 6

and 7, the background is already removed during pseudo-voigt

tting.

Our empiric MIF ratio called fS is determined by

P

IMgOpure

f S P hkl

,

(7)

hkl IMgOH2 pure

P

where hkl IMgOpure is the integral intensity measurement from a

P

pure sample of MgO and hkl IMgOH2 pure is the integral intensity

measurement from the same mass of Mg(OH)2 pure sample.

ARTICLE IN PRESS

3658

3. Experimental results

The TEM micrograph of the magnesium hydroxide sample is

shown in Fig. 4. The morphology sample is platelet-like.

Fig. 5 shows the size distribution. The mean size value is

79.5 nm.

The XRD pattern of the magnesium hydroxide is shown in

Fig. 6. All diffraction peaks can be indexed as the hexagonal

structure of magnesium hydroxide (JCPDS le number 86-0441)

[24]. There is no additional diffraction peak in the pattern,

indicating that the sample has no measurable impurity.

The XRD pattern of the magnesium oxide obtained at the end

of the calcination is shown in Fig. 7. All diffraction peaks can be

indexed as the cubic structure of magnesium oxide (JCPDS le

number 78-0430) [24]. There is no additional diffraction peak in

the pattern, thus indicating that the decomposition is complete.

Integral intensity at 310 1C: An example of [h k l] integral

intensity peaks at 310 1C is shown in Fig. 8. The curve has a

sigmoid shape. This data type allows us to determine the

evolution of the ratio a with the formula (6) using all

simultaneous [h k l].

be extracted using acquisition data. For each peak, the rst

appearance of their position is taken as reference. Fig. 9 shows the

difference position during MgO growth.

Thus Fig. 9 shows that a complex phenomenon appears during

calcination, at least during germination and growing crystallization. It appears that cell size changes during the phase

transition.

4. Model tting

As the experimental method used is somewhat original in this

context, a large number of the most commonly used kinetic

models were tested and compared, to solve the kinetic equation of

a solid state reaction

da

k f a:

dt

(8)

time t as t 0 t=t 0:5 is introduced. To analyse our data t 0:5 , whereby

ARTICLE IN PRESS

A. Ranaivosoloarimanana et al. / Physica B 404 (2009) 36553661

3659

Thus, at this time t 0:5 , the ratio a is equal to 0.5 and the reduced

time is equal to 1. This method is well-known for many solid state

reactions [5]. The ratio a and the quadratic differences from the

experimental results are evaluated (Figs. 1015) by introducing

this common reduced time in the F 1 , Dn , Rn , An . Details of those

models are described by Halikia [13].

With different models, the following gures show at different

temperatures, rst, the ratio of reacted magnesium hydroxide a

versus time [5] and, second, the cumulated quadratic difference

between experimental data and different models.

For the reduced time less than 1, the quadratic difference is

then accumulated from 1 to 0. And for the reduced time greater

than 1, the accumulation is from 1 to the end.

Figs. 1012 show the reduced time plot for the sample and the

most important rate equations.

Figs. 1315 show the cumulated quadratic difference between

data and rate equations.

Fig. 7. MgO full-pattern diffractogram.

Fig. 10. The reduced time plot for the sample and the most important rate

equations at 300 1C.

Fig. 9. Evolution of peak position during the transformation phase (310 1C).

Fig. 11. The reduced time plot for the sample and the most important rate

equations at 305 1C.

ARTICLE IN PRESS

3660

At the three temperatures 300, 305 and 310 1C for the reduced

time less than 1, A1.5 model (n 1.5) is the best t for our data. For

the reduced time greater than 1, at temperature 300 and 310 1C,

A1.5 model (n 1.5) is the best t but at 305 1C, A2 model (n 2)

becomes the best t.

AvramiErofeevs tting: We conrm in this analysis that

AvramiErofeevs models [15], dened by

ln12a1=n kt

or

a 12 expktn

(9)

magnesium hydroxide, as already quoted in the literature [13,14].

Thus, our analysis is focused on determining, as described in

the previous AvramiErofeevs equation (9), the best values of n

for each temperature T at 300, 305 and 310 1C. To make it, a is

determined using full-pattern diagram that requires the 100%

approach method. The value n 1.51 for 300 1C, n 1.75 for

305 1C and n 1.52 for 310 1C are obtained, which are shown in

Fig. 16.

Fig. 12. The reduced time plot for the sample and the most important rate

equations at 310 1C.

Fig. 13. The cumulated quadratic difference between data and rate equations at

300 1C.

Fig. 14. The cumulated quadratic difference between data and rate equations at

305 1C.

Fig. 15. The cumulated quadratic difference between data and rate equations at

310 1C.

ARTICLE IN PRESS

A. Ranaivosoloarimanana et al. / Physica B 404 (2009) 36553661

3661

Acknowledgements

particular with those of Yue et al. [14] describing a non-isothermal

experiment, in which the mechanism of decomposition changes

between A1.5 and A2, in this case according to the rising heating

rate.

It is known that AvramiErofeevs models are especially

adapted for random nucleation and nuclei growth process. If the

growth is essentially limited by interfacial reactions, the models

are suitably adapted with integer values of the coefcient n which

appears in the denition (9) of these models. If the growth is

notably limited by diffusion effects, the best models are obtained

with half-integer value of n [25]. It appears that the temperature

interval 300310 1C contains some critical and complex phenomena. It may certainly be expected that, during the experiment

time, which is important (for example 5 h to obtain a 12 for

T 305 1C), both previous mechanisms occur concurrently, and

consequently that the true kinetic equation would be suitably

described using some linear combination of the two models A1.5

(with n 1.5) and A2 (with n 2).

Moreover, other external parameters are to be considered. In

particular, the importance of water vapour is well known [14].

We may conclude that the decomposition mechanism of

magnesium hydroxide would be well described, at least in the

temperature interval [300, 310 1C], taking the AvramiErofeev

model with a coefcient n, which is a function of the temperature

T and some external parameter j, with numerical values in the

interval between 1.5 and 2. So, the equation of the decomposition

takes the form

help with the experimental work and C. Metayer for his

bibliographical support.

a 1 expktnT;j .

(10)

theoretically describes the change of the crystalline microstructure during the reaction. In this way, new experiments in nonisothermal situation can be now expected.

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