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Minerals Engineering 22 (2009) 1154–1159

Contents lists available at ScienceDirect

Minerals Engineering
journal homepage: www.elsevier.com/locate/mineng

A new practical method to determine the microwave energy absorption ability


of materials
S.J. Ma a,*, X.W. Zhou b, X.J. Su a, W. Mo a, J.L. Yang a, P. Liu a
a
School of Resources and Metallurgy, Guangxi University, Nanning 530004, PR China
b
Guangxi Gold Administration Bureau, Nanning 530023, PR China

a r t i c l e i n f o a b s t r a c t

Article history: To quantitatively measure and compare the ability of different materials in absorbing microwave energy,
Received 17 December 2008 a new practical method, only using a home microwave oven with microwave radiation out of the bottom
Accepted 15 May 2009 of the cavity as the major apparatus, was developed. During the measuring process, each target material
Available online 10 June 2009
and water, separately contained with two microwave transparent containers, respectively, were simulta-
neously placed in the oven cavity for microwave irradiation. The water container was above the tested
Keywords: materials container, and the water acted as the medium to absorb the microwave energy surplus to that
Industrial minerals
absorbed by tested materials. By determining the water temperature and then calculating its absorbed
Activated carbon
Comminution
microwave energy, the microwave energy absorbed by the target materials could be obtained. According
Roasting to this method, seven bulk solid materials of reagent grade were tested and the results agree well with
Leaching previous research reports. In addition, the principle and control of the measuring conditions of the novel
method were discussed in this paper.
Ó 2009 Published by Elsevier Ltd.

1. Introduction Theoretically, the microwave energy absorbed by materials can


be inferred through their dielectric and magnetic properties, which
Microwave heating is unique and has a lot of advantages over is proportional to the frequency of the applied electric field, to the
conventional heating such as rapid heating, material selective loss factor and to the square of the local electric field intensity
heating, volumetric heating. Out of these advantages, material (Nanthakumar et al., 2007). However, the permittivities of most
selective heating is one of the most important fundamental prop- materials are related with several variables such as the moisture
erties for microwave energy application in minerals engineering. content of materials, the frequency of the applied electric field,
Material selective heating means there is difference in absorbing the temperature and the density and the structure of materials.
microwave energy for different minerals, so different temperature Therefore, it is actually difficult to obtain the microwave energy
rising rates in microwave field exist, which to a great extent is the absorbed by materials based on theoretical calculation. In fact,
basis of microwave-assisted crushing and grinding. Because of the people often directly measure the material temperature to obtain
material selective heating, microwave can induce stress and even the absorbed microwave energy. Some methods have been re-
the formation of cracks between different ore minerals particles, ported. For example, the temperature of a microwave irradiated
and so improve liberation and increase the comminution efficiency sample can be measured by inserting a measuring device into
(Walkiewicz et al., 1988, 1991; Kingman et al., 2000, 2004; Olu- the hot material immediately after turning off microwave power.
bambi et al., 2007; Scott et al., 2008). Therefore, it is very important Many measuring devices, such as luxtron fluoroptic, accufibre,
to understand the difference of different materials in absorbing optical pyrometer, thermocouple, the ultrasonic temperature
microwaves. As early as 1966, Connell and Moe (1966) studied probe, were used for temperature measurement (Haque, 1999).
heating of minerals by microwave and obtained a US patent for However, many limitations existed in above-mentioned methods
apparatus for ore treatment. Ford and Pei (1967) applied micro- and devices. For instance, measuring devices usually failed in per-
waves to several oxides and sulphides, and concluded that dark formance when contacted with some heated materials which were
colored compounds heated faster than light colored compounds. sensitive to microwave absorption and quickly reached very high
Chen et al. (1984) applied microwave irradiation to 40 minerals, temperature. The temperature measurement was subjected to a
and classified the test materials into two groups based on the gen- limited number of points, so the measured temperatures or their
eration of heat and the change of the materials properties. mean values could not reflect the true temperature characteristic
of the bulk materials, especially for mixed materials. Therefore, it
* Corresponding author. Tel.: +86 771 3232200; fax: +86 771 3233566.
is of significance to seek a new method to look into the character-
E-mail address: shjma@gxu.edu.cn (S.J. Ma). istic of materials in microwave absorption so as to select suitable

0892-6875/$ - see front matter Ó 2009 Published by Elsevier Ltd.


doi:10.1016/j.mineng.2009.05.003
S.J. Ma et al. / Minerals Engineering 22 (2009) 1154–1159 1155

materials in microwave field and to predict the heating behaviours 2.2. Principle
of ore minerals when heated by microwave irradiation.
In this paper, a new method about measuring absorbed micro- It is well known that the interaction between microwave and
wave energy was invented (Publication No. CN101078700 for Chi- matter is the molecular polarization of non-polar molecules and
nese patent censor), in which water, due to its sensitivity to then rotation of dipole, which causes friction among molecules
microwave energy, was used as the medium material to absorb and further heat effect. When microwaves enter the cavity, they
indirectly reflected microwave radiation of the tested materials. are reflected by the metal wall and so distributed in the whole
The method is simple, practical and suitable not only for pure space of the cavity. Therefore, when two or more different matters
materials but for mixed material as well. are placed in the cavity, they would be irradiated by microwaves at
the same time, except metal reflecting microwaves. That is to say,
one matter would not prevent another matter from receiving
2. Principle and methods microwave irradiation. However, the amount of microwaves
absorbed by a matter in a given time could be affected if another
2.1. Apparatus matter exists. This effect can be roughly explained using electro-
magnetic radiation quanta concept. On basis of this concept, the
The system, illustrated as Fig. 1, mainly consisted of a home amount of absorbed microwaves by a matter mainly depends on
microwave oven (1300 kW input electricity power, 800 W micro- the irradiation times and energy density of each irradiation besides
wave output) (G80W23ESL-V9, Galanz Group, China), a rectangular on the properties of the material. For a microwave oven with a
plastic box for containing water, a hardened glass pan for contain- fixed microwave frequency, the irradiation times in a fixed time
ing target materials for test. The inner dimensions of the oven cav- could be thought to be fixed, thus the energy density of each irra-
ity were 214 mm in height, 332 mm in length and 346 mm in diation and the properties of the material become the major factors
width. A flat ceramic plate was installed on the bottom of the metal to affect the amount of absorbed microwaves. But the irradiated
cabinet when manufactured. According to the oven product speci- energy density is inversely related with the properties of the mate-
fication, the outlet of the oven waveguide was under the ceramic rial. Assumed that some matter A sensitive to microwaves be irra-
plate, and so microwaves had to penetrate the ceramic plate before diated twice in an oven cavity by microwaves. The surplus
being directed to the cavity. The plastic box had dimensions of microwave energy, compared to the first supply energy, will re-
100 mm in height, 274 mm in length and 210 mm in width. Its duce after matter A has been irradiated for the first time. When
thickness was about 3 mm with 266 g mass. The major concern the surplus energy is re-reflected by the cavity wall for the second
about the box was to hold the heat of the water and to reduce heat irradiation, the energy density for the second irradiation will de-
loss. The hardened glass pan had a bottom diameter of about cline. The stronger the ability of absorbing microwaves of the mat-
210 mm, top diameter of 254 mm, and height of 50 mm. The glass ter, the less the surplus microwave energy is and so the lower the
thickness of the pan was about 5 mm with 836 g mass, which pro- surplus energy density is for the second irradiation, which is iden-
vided a good heat resisting property. Because the length of the tical to the attenuation of microwaves moving in a very long semi-
plastic box was bigger than the top diameter of the glass pan, conductor. If assumed that there are two matters, called A and B,
the plastic box could directly lay above the glass pan and avoid di- respectively, and that both them have different abilities to absorb
rect contact with the target materials provided the stacking height microwaves, the effect of the existence of matter B on the amount
of the target materials was smaller than the wedge height of the of matter A absorbing microwave energy could be discussed as fol-
pan, which would overcome the water being heated by the target lows. Assumed there are two cases. One case is that only matter A
materials during the microwave irradiation process. is irradiated for two times, and the second one is that both matter
In addition, a digital display temperature controller with elec- A and matter B are simultaneously irradiated for two times too.
tric thermocouple as the probe and a laser temperature instrument Obviously the surplus energy densities for the second irradiation
were used to monitor the temperatures of water and solid materi- will be different for the two cases because of the difference of mat-
als, respectively. They could display the temperature variation of ters A and B in absorbing microwaves. Therefore mutual effect will
0.1 °C. Temperature measurement was carried out when the oven exist when two or more matters are placed together to be irradi-
was switched off. ated in the cavity, which provides a possible theoretical basis
and a way to determine the ability of one matter absorbing micro-
waves from that of another matter.
As demonstrated in Fig. 1, two matters are placed in the cavity
for absorbing microwave. One matter is so-called medium mate-
rial, which is expected to be sensitive to microwave and easy to
mix so that its inner temperature is even to satisfy convenient tem-
perature measurement. Water is typically polar matter and satis-
fies these demands well, so in this new developed method water
was employed as the medium material. In this case, if water phase
change does not occur, the variation of its inner temperature
should be able to reflect the amount of its absorbed microwaves.
Naturally the other matter is the target materials for test.
As regard the discussed microwave oven, when it works, micro-
waves out of the magnetron tube are transported by the waveguide
to its outlet, then penetrate the bottom ceramic plate, and eventu-
ally enter the cavity to be reflected by metal wall and absorbed by
the water and the target materials. During the process, ineffective
loss of microwave energy, which refers to the part of the micro-
wave energy not used for heating the water and the target materi-
als, is unavoidable because microwaves could be absorbed by the
Fig. 1. The diagram of the measuring apparatus. waveguide, the ceramic plate, and the containers. In addition, tak-
1156 S.J. Ma et al. / Minerals Engineering 22 (2009) 1154–1159

ing away heat through radiator electric fan of the oven could also energy can be attributed into two types of causes, one being due
lead to the loss of microwave energy. Therefore, the output micro- to direct microwave absorption by materials such as, the ceramic
wave energy could not be fully transferred into thermal energy to plate, cavity wall and containers , and the other one being caused
increase the temperature of the materials. That means a systematic by heat absorption by these materials from the tested materials
ineffective loss of microwave output exists, and so the available and the medium and by heat escape through the irradiator electric
microwave energy to increase the temperature of the materials fan. Although temperature affects the sensitivity of materials to
would always be less than the microwave output. Nevertheless, microwave, it is acceptable to consider the microwave absorption
this systematic ineffective loss of microwave energy can be re- ability of materials to be constant if the temperature change can
duced by selecting so-called microwave transparent materials for be controlled within a small range. Therefore it is allowed to con-
the containers and by controlling the system temperature, mainly sider a stable direct loss of microwave absorption by the oven itself
referred to the temperature of the cavity space. Theoretically, for a and the containers if the system is controlled with only small tem-
manufactured microwave oven, there is a maximal available perature changes. On the other hand, the microwaves loss caused
microwave energy which is less than the microwave output. by heat absorption and heat escape also mainly depends on the
For the sake of convenient discussion, designate WOM as the to- system temperature. Normally the closer the system temperature
tal output microwave energy, J; WAM as the available microwave is to its surrounding environment temperature, the less this type
energy in the cavity for heating the tested materials and the med- of heat loss becomes. So, under given operation conditions, the to-
ium, J; QL as the ineffective loss of microwave energy, J; and k as tal microwave ineffective loss should be relatively stable and can
the utilization efficiency of the output microwave energy, then be roughly considered to be a constant when the system tempera-
the following equations can be derived: ture is controlled close to its surrounding environment tempera-
ture with small change. Otherwise, ineffective loss would change,
W OM ¼ W AM þ Q L ð1Þ
which was verified by later experiment results. According to this
W AM ¼ kW OM ð2Þ analysis, it is reasonable to consider the same value of k for two
Q L ¼ ð1  kÞW OM ð3Þ experimental cases, one being that water medium and tested
materials are simultaneously irradiated and the other being that
only the water medium with the same mass being irradiated.
When the water medium and some target material are simulta-
The latter case means QTM is zero, so k can be calculated as follows:
neously placed in the cavity and receive microwave irradiation, the
available microwave energy is used to heat the water medium and k ¼ qW =W OM ð9Þ
the tested material. If QW is designated as the microwave energy
where qW is microwave energy absorbed by the water without tar-
absorbed by the water medium, QTM by the tested material, the fol-
get materials in the cavity, J. If let t2 and t1 stand for the tempera-
lowing equation can be written:
tures after and before heated in this case, then qW can be
W AM ¼ Q W þ Q TM ð4Þ obtained as follows:
so qW ¼ mcðt 2  t1 Þ ð10Þ
Q TM ¼ W AM  Q W ð5Þ Thus, the microwave energy absorbed by a tested material can
be obtained on basis of Eq. (6) after WOM has been solved based on
By substituting WAM with k and WOM based on Eqs. (2) and (5)
Eq. (7), QW on Eq. (8), and k on Eqs. (9) and (10). Further, the ability
can be rewritten as follows:
of absorbing microwave for different materials can be compared.
Q TM ¼ kW OM  Q W ð6Þ
2.3. Determining procedure
Eq. (6) indicates that the microwave energy QTM absorbed by
the tested material could be obtained if WOM, QW and k are solved.
The determining procedure included setting the initial operat-
This is the theoretical basis of the new method discussed in this
ing conditions, preparing materials, measuring the medium tem-
article.
peratures and calculating the microwave energy absorbed by the
Generally the output microwave energy can be calculated based
tested materials.
on the selected power and the work time of the microwave oven as
Initial operation conditions mainly included setting the output
follows:
power P and the heating time t. The rated power was conveniently
W OM ¼ Pt ð7Þ set as the output power. Choice of the heating time t had to con-
sider the water vaporization and the thermal resistance of the glass
where WOM is output microwave energy, J; P is the selected output
pan. In the case of the same microwave output, in general the
microwave power of the microwave oven, W; t is the heating time, s.
greater the mass of the water medium, the less the temperature
The energy absorbed by the water medium, in the case of
of the water medium increased and so less the water vaporized
neglecting its undeterminable heat loss for water vaporization,
with higher utilization efficiency of the microwave energy for heat
heat conduction to its container and heat irradiation to its sur-
transfer. Therefore a big mass of water medium allowed a rela-
rounding environment, which is possible and acceptable by select-
tively long heat time. On the other hand, for some materials sensi-
ing optimum operation conditions, can be easily deduced as
tive to microwaves, a long heat time could destroy the glass pan, so
follows:
too long heating was not feasible. In addition, a very short heating
Q W ¼ mcðT 2  T 1 Þ ð8Þ time might hardly increase the water temperature, which is also
not desired, because it would result in large calculation error and
where QW is the energy absorbed by the water medium, J; m is its temperature observation error. Therefore, the heating time had
mass, kg; c is the specific heat of water, J kg1 °C1, T2 and T1 are better be selected based on experimental results.
the temperatures after and before heating, °C. Preparation of materials included water medium and the target
So far, WOM and QW have been solved; the problem left is to seek materials for test. Tap water was chosen as the medium material.
the microwave energy utilization efficiency k. However, the mass of water medium greatly affected the results.
According to prior analysis on microwave transportation and The greater the mass of the water medium, the smaller the temper-
working processes, the ineffective loss of the output microwave ature variation was. In order to control water vaporization and
S.J. Ma et al. / Minerals Engineering 22 (2009) 1154–1159 1157

experimental error, the rational mass was also determined by wave utilization efficiency due to more water vaporization and
experiments as illustrated later. Regarding the tested materials, stronger heat conduction and irradiation in case of high tempera-
they were required to be able to occupy the whole bottom area ture. To look into the relationship of irradiation time with micro-
of the glass pan with a thickness smaller than the height of the wave utilization efficiency, experiments were conducted. During
glass pan wedge. these experiments, 2.0 kg water medium, together with its plastic
Temperature measurement mainly aimed at the water medium. container and the glass pan was placed in the cavity for microwave
Because of its sensitivity and stableness in displaying temperature, irradiation for different time. The irradiation time was set at 40 s,
electric thermo-couple was used as the probe in measuring the 80 s, 120 s, 160 s, 200 s, and 240 s, respectively. The experimental
temperature of the water medium. The electric thermo-couple results are listed in Table 2.
probe was inserted in the water medium only after the oven power Table 2 indicates that, although the heating time changed from
turned off and the water medium was slightly agitated with a glass 40 s to 240 s, the microwave energy utilization efficiency did not
rod to make the inner temperature more even. show obvious relationship with the heating time. So it could be
After the temperature measurement finished, the microwave concluded that change of heating time within this scope would
energy absorbed by the tested materials was calculated in compli- not apparently alter the microwave energy utilization efficiency
ance with the following steps. Firstly, calculated the total micro- for heating 2 kg water. Regarding the fluctuation of the utilization
wave output energy WOM based on Eq. (7). Then, calculated the efficiency, it could be caused by operation error when measuring
microwave energy QW and qW using Eqs. (8) and (10), respectively, the temperature. The stability of the microwave energy utilization
followed by calculating the microwave energy utilization efficiency efficiency should be attributed to the low final temperature, which
k on basis of Eq. (9). Finally, calculated the microwave energy QTM verified again that 2.0 kg water medium was suitable. Therefore, it
absorbed by the tested materials on basis of Eq. (6). is acceptable to consider k stable as described in discussing the
To compare the ability of microwave energy absorbing for dif- principle of the method, provided the experimental operation
ferent materials, the operation conditions were strictly kept con- could be well selected and effectively controlled.
sistent for all materials. To clearly demonstrate the results, the
plotting of absorbing energy versus heating time was given as 3.3. Comparison of materials in absorbing microwave energy
illustrated later.
The ability of different materials in absorbing microwave en-
3. Validation and application ergy was tested. SiO2, CaCO3, CaO, Al2O3, MnO2, Fe3O4, activated
carbon were selected as the target materials for test. All these solid
3.1. Effect of water medium mass on the microwave efficiency materials were reagent grade products. Among these products,
SiO2 was granular with relatively coarse size, and the other mate-
It was mentioned previously that the water medium mass could rials were very fine powders. During the experiments, the micro-
have an important effect on the microwave utilization efficiency. wave output power of the oven was set at 800 W, and 2.0 kg
To testify this point, experiments were carried out, in which only water was employed as the medium. The stacking thicknesses of
water with its plastic container was put in the cavity for micro- materials in the glass pan container ranged from about 12 mm to
wave irradiation. The output microwave power was set at 800 W, 40 mm, depending on their densities and particle sizes. Each tested
and the heating time was 120 s. The results are shown in Table 1. material (0.50 kg) was individually microwaved for 40 s, 80 s,
It can be seen from Table 1 that the medium mass greatly af- 120 s, 160 s, 200 s, and 240 s, respectively. When each heating
fected the energy utilization efficiency. After microwave irradia- was complete, the final temperature of the water medium was
tion for 120 s, the maximal microwave utilization efficiency was determined for calculation of its absorbed microwave energy,
77% at 2.0 kg medium mass. When the medium mass was less than while the temperature of the tested material was determined by
2.0 kg, the microwave utilization efficiency increased with the means of the laser temperature meter, which was used only as a
medium mass. However, the microwave utilization efficiency de- rough reference because of the uneven distribution of the inner
clined with water medium mass when the medium mass was more temperature. The results are shown in Fig. 2.
than 2.0 kg. It means that when medium mass is less than 2.0 kg, Based on the absorbed energy and its variation trend with the
the microwave is surplus. So increase of the medium mass could heating time shown in Fig. 2, the questioned materials could be
promote more energy being absorbed. In a word, 2.0 kg medium classified into four types. The first type, such as activated carbon
mass matched well with 800 W output microwave, which ensured and Fe3O4, was especially sensitive to microwave. The absorbed
the highest microwave utilization efficiency. energy increased rapidly with the heating time, so their tempera-
ture went up quickly. The laser temperature meter displayed the
3.2. Effect of irradiation time on the microwave efficiency surface temperature of Fe3O4 was above 100 °C after microwave
irradiation for 200 s. When the irradiation time was set at 240 s,
For a given water mass, the irradiation time affects the temper- the glass pan cracked due to too high temperature of Fe3O4. How-
ature rising of the medium, and further possibly affects the micro- ever, the medium, heated together with Fe3O4, had a very small

Table 1
Effect of water medium mass on microwave energy utilization efficiency for heat transfer.

Medium mass (kg) Temperature (°C) Absorbed energy (J) Energy utilization efficiency, k (%)
Initial temperature Final temperature Increased temperature
0.5 26.4 53.7 27.3 57,330 59.7
1.0 26.4 42.6 16.2 68,040 70.9
1.5 26.4 37.7 11.3 71,190 74.2
2.0 26.4 35.2 8.8 73,920 77.0
2.5 26.4 33.3 6.9 72,450 75.5
3.0 26.4 31.9 5.5 69,300 72.2
3.5 26.4 30.9 4.5 66,150 68.9
1158 S.J. Ma et al. / Minerals Engineering 22 (2009) 1154–1159

Table 2
Effect of irradiation time on microwave energy utilization efficiency for heat transfer.

Irradiation time (s) Temperature (°C) Absorbed energy (J) Energy utilization efficiency, k (%)
Initial temperature Final temperature Increased temperature
40 24.4 27.2 2.8 23,520 73.5
80 24.4 30.2 5.8 48,720 76.1
120 24.4 32.8 8.4 70,560 73.5
160 24.4 35.2 10.8 90,720 70.9
200 24.4 37.4 13.0 109,200 68.2
240 24.4 40.6 16.2 136,080 70.9

70000 (1967). Therefore, the new developed way, discussed in the paper,
65000 SiO2 to determine the ability of absorbing microwave for different
CaO materials was credible.
60000 CaCO 3
55000 Al2 O 3
In addition, on basis of the description of the absorbed micro-
Absorbed energy /J

50000 MnO2 wave energy and the surface temperature of MnO2, Fe3O4, acti-
45000 Fe3O4 vated carbon, it implied that the rising rate of materials surface
40000 C temperature is not always correlated positively with the amount
35000 of absorbed microwave energy, which also gives the similar infor-
30000 mation expressed by the formula of temperature rising rate that it
25000 depends not only on the absorbed microwave but the specific heat
20000 and the density of the material (Nanthakumar et al., 2007). There-
15000 fore, it can be concluded that it is not appropriate to use the rate of
10000 surface heating to infer the microwave absorption behaviour by a
5000 given material, but that the method presented provides an alterna-
0 tive, according to which the absorption can be quantified directly.
0 40 80 120 160 200 240 280
Heating time /s

Fig. 2. Relationship of absorbed microwave energy with heating time for different
4. Conclusions
materials.
Based on the theory of microwave transportation and interac-
tion mechanism with materials, a new simple and practical meth-
temperature rising, which indicated that the direct heat irradiation od, using water as the medium material to indirectly reflect
out of the tested materials yielded little effect on the medium tem- microwave absorption of the tested materials, was invented to
perature in this designed apparatus. Compared to Fe3O4, although quantitatively measure and to compare the ability of different
the calculated absorbed energy of the activated carbon was bigger materials in absorbing microwave energy. The factors affecting
than that of Fe3O4, the former surface temperature was much low- the reliability of the measurement were discussed. According to
er than that of the latter. The second type, such as MnO2, was com- the developed method, seven materials were tested about the abil-
paratively sensitive to microwave. Its absorbed microwave energy ity of microwave absorbing, and the results showed good consis-
increased with the heat time, but a slow increase occurred from tence with previous reports. In addition, the experimental results
120 s to 200 s. The surface temperatures of MnO2 were also very showed that it is not appropriate to use the rate of surface heating
high and close to 100 °C after microwave irradiation for 240 s, to infer the microwave absorption behaviour by a given material,
which closed to and even exceed those of the activated carbon. but that the method presented provides an alternative, according
The third type, such as Al2O3, was slightly sensitive to microwave to which the absorption can be quantified directly.
and could absorb microwave to slowly enhance its temperature.
Its curve shape was alike with that of MnO2, but the absorbed
microwave energy was less than that of MnO2. The temperature in- Acknowledgement
crease of Al2O3 was less than the first and the second type. The
fourth one, such as SiO2, CaCO3, CaO, was not sensitive to micro- This work was financially supported by the Fund of Excellent
wave and hardly absorbed microwave energy, so the surface tem- Academic Talent Leader in Higher Education Institutes of Guangxi
perature rising of these materials were not obvious. After 240 s of China.
microwave irradiation, the surface temperature did not exceed
35 °C in the case of room temperature close to about 27 °C . References
Above-mentioned description of the classification and the
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