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Ceramics International
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A R T I C LE I N FO A B S T R A C T
Keywords: Porous materials can be effective for sound absorption and noise reduction. A kind of lightweight cellular
Porous material ceramic foam with bulk density of 0.38–0.56 g cm-3 was successfully prepared by conventional molding with
Ceramic foam pore forming agent. The porosity is from 76.4% to 83.7% for the sample with relatively large pores (the average
Sound absorption pore size: 5.3–5.6 mm), and from 74.1% to 81.1% for the sample with relatively small pores (the average pore
size: 1.5–1.7 mm). The effects were investigated for processing parameters on the structure of samples, and for
the pore size, sample thickness and porosity on the sound absorption performance of samples. The results show
that the absorption performance of the ceramic foam product with relatively large pores may be superior to that
with relatively small pores in the case of the approximately same porosity. The first absorption peak moves from
a higher frequency to a lower frequency with the increase of sample thickness. When the porosity increases, the
average sound absorption coefficient increases for all of the samples, and the first absorption peak moves from a
higher frequency to a lower frequency for the sample with relatively large pores but does not change for that
with relatively small pores.
1. Introduction coefficient more than 0.2, can be used for efficiently controlling the
noise [2]. Porous materials may present appropriate properties for a
Great progresses have been made in industry, transportation and number of engineering applications [2–4]. These materials, including
construction, but people have to face up to increasing environmental the inorganic foam, polymer foam and metallic foam, are often used to
pollution arose with the economic development. Noise pollution has absorb the sound energy and decrease the noise in engineering
seriously affected people's everyday life, so more and more researchers [2,3,5–10]. The sound absorption effect of porous materials can be
have begun to study the sound absorption material, which is effective to predicted when the specific acoustic impedance of the material is
relieve the noise [1,2]. known, and the related calculated results indicate the Allard and
The sound experiences three stages from being produced to being Champoux's method could reach the best prediction accuracy for the
received by the human ear: the generation of sound from the sound wool materials [3]. While, the sound absorption characteristic of a
source, the propagation of sound in the medium and the reception of sintered porous ceramic material (the main composition:
sound by the receiver. Accordingly, the receiver can be protected by (Na,K)4CaAl6Si30O72), with the bulk density of 0.5–0.7 g/cm3 and pore
installing some devices near the sound source to interrupt the sound size of 1.0–3.0 mm, is found to be roughly in agreement with Johnson-
wave propagation. Both of sound insulation and sound absorption are Allard model [8]. In another study on the sound absorption property of
mainly adopted in engineering. The sound insulation does not reduce a ceramic hollow sphere structure with micro-sized open cell, the cal-
the sound energy but prevent the sound waves from propagating to the culated results based on Pride-Allard model and experimental data
receiver by means of special materials. Different from this, the sound demonstrated similar trend with the increase of frequency [5]. Inter-
absorption is using porous materials. As sound waves travel to the estingly, research on the acoustic sound attenuation for a natural
porous material, part of them will enter the pores. Due to the viscous porous structure of seafloor sand sediment reveals the attenuation
friction between the air and the material surface in the pore, the sound coefficient can either increase or decrease with temperature depending
energy is partially transformed to thermal energy, which can achieve on the frequency range being examined [6]. Meaningfully, the acoustic
the purpose of “sound absorption” [3]. absorbency of SiC foam under water can be significantly improved by
Usually, the specially structured material or framework is used to filling silicon oil in the pore of the sample at 750–4000 Hz, but the
absorb noise. Sound absorption materials, with the average absorption foams backed by air gap and saturated fully by water display degraded
∗
Corresponding author.
E-mail address: Liu996@263.net (P.S. Liu).
https://doi.org/10.1016/j.ceramint.2020.06.033
Received 30 April 2020; Received in revised form 22 May 2020; Accepted 3 June 2020
Available online 23 June 2020
0272-8842/ © 2020 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
J.H. Chen, et al. Ceramics International 46 (2020) 22699–22708
sound absorption capacity [7]. A novel sort of cellular titanium foam 2. Experimental methods
with 86%–90% porosity and millimeter-scaled pores showed a good
performance of sound absorption, with the absorption coefficient more 2.1. Preparation of the sample
than 0.6 at 3150–6300 Hz and even exceed 0.9 at the resonance fre-
quency, and the main mechanism of sound absorption for this foam Natural zeolite powder was thoroughly mixed with the binder and
should be of the interference silencing or the viscous dissipation in additive agents, and then added the self-made pore forming agent to
different ranges of sound wave frequency [9]. The sound absorption is produce the ceramic foam by means of molding, drying and sintering.
investigated for an aluminium foam (with porosity of 60%–90% and The natural clinoptilolite (Na8[Al8Si40O96]·39H2O) powder with gran-
pore size of 0.5–3.5 mm) produced by press infiltration casting in Ref. ularity of about 10–20 μm was used as the main raw material, mixed
[10], and the results show that the absorption coefficient associates with the self-made nontoxic binder (for example, the jellylike matter
mathematically with the frequency corresponding to the sound wave from modulating the potato starch and solvent) and some additives
and the sound absorption peak, and also with the specific surface area (such as ammonium bicarbonate) including silica powder with the
of the sample. granularity of about 30–50 μm in a certain proportion.
The ceramic foam is a class of porous inorganic materials, of which
the property is related not only to the composition of the material (1) Ingredients matching: The above mixture was fully mechanically
species, but also closely to the porosity, pore structure, pore size and stirred and stood for 60 min, then added some pore forming agent
pore distribution [11–16]. For example, the study on sound absorption and further mixed well. The pore forming agent is spherically and
of a ceramsite porous material (with the porosity of 15%–35% and pore may be divided into two classes: one is 4–5 mm and the other is
size of 0.71–1.44 mm) has shown that the porosity has a significant 1–2 mm in diameter. The ceramic foam with relatively large pores
impact on the high-frequency sound absorption [15]. was prepared by using the larger sized pore forming agent and that
From related works that have been reported, it can be known the with relatively small pores by using the smaller sized pore forming
abundant researches on sound absorption materials have brought an agent. The content of pore forming agent determines the porosity of
unceasing development of improved products with excellent perfor- ceramic foams. When this content is excess, the molding of the
mance. However, there are still some areas that need to be further ceramic foam sample would be difficult; and when it is too little, the
developed, which means, for instance, various developing directions of porosity would be too low to decrease the sound absorption of the
sound absorption materials: porous product. Therefore, it was particularly important to de-
termine the content of pore forming agent.
(1) Environment-friendly sound absorption materials. With the im- (2) Compressive molding: The ceramic foam preform was prepared by
provement of people's life quality, the research should be empha- compressive molding in this experiment. The slurry from the binder
sized on environment-friendly sound absorption materials. People and additive agents was poured into a mold and applied a certain
should adhere to the principle of environmental protection from pressure for 10 min, and then the resultant wet preform sample
raw materials and final products. Especially, non-toxic and tasteless could be taken out from the mold to dry. The investigation was
sound absorption materials should be used to absorb sound and carried out in the sound frequency range of 200–4000 Hz. With the
reduce noise. JTBZ sound absorption coefficient testing system, the sound ab-
(2) Multifunctional sound absorption materials. It is hoped that a spe- sorption coefficient was measured using the circular samples with
cial material of both heat insulation and sound absorption can be different diameters for different frequency ranges [2]. The diameter
used in some special places, such as in steel mills. The material is of samples should be 100 mm at 200–2000 Hz and 50 mm at
also hoped to possess many other excellent properties, such as fire 2500–4000 Hz, respectively. Corresponding to this, the size of the
resistance, flame retardant, waterproof, anti-corrosion and even mold could be designed.
aesthetic requirements. Such multifunctional sound absorption (3) Drying and sintering: The ceramic foam preform was firstly placed
materials can be competitively in practical applications and in at room temperature for 10 h in order to prevent the cracking from
saving the overall cost. rapid drying in a constant temperature box, into which it was then
(3) Composite-type sound absorption materials. The composite sound putted to dry at a relatively low temperature of 60–80 °C for 12 h.
absorption material has a wide range of sound absorption fre- The SX-G36163 high-temperature electric furnace was used to
quencies, which can effectively absorb sound at low and inter- sinter the ceramic foam. The heat treatment process was increasing
mediate frequencies. the temperature at a rate of 20 °C/min up to 1150–1200 °C, at
which the sample was sintered for 60 min and cooled down to the
room temperature in the furnace. Fig. 1 shows the sintered samples
of the lightweight ceramic foam after grinding to achieve the
Fig. 1. Ceramic foam samples with different pore sizes: (a) with relatively large pores; (b) with relatively small pores.
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Table 1 there will be a short cessation period of pore growth when it achieves a
Elementary parameters of samples with relatively small pores by different balance between the internal and external air pressures. In the last
sintering processes. stage, this short balance period ends, the air pressure inside pores
Sample No. Sintering Sintering Bulk Porosity/% Average continues to decrease and the surface tension continues to increase,
temperature/ period/ density/ pore size/ leading these pores to shrink and the relatively large pore to become
°C min g·cm-3 mm smaller or split into two smaller pores. All these three stages need spend
a certain time, and the higher temperature makes a shorter period for
1 1150 60 0.56 74.1 1.57
2 1170 60 0.55 74.7 1.61 the early and the second stages. When the sintering temperature is
3 1190 60 0.43 79.9 1.64 higher, the crystal water contained in natural zeolite will vaporize
4 1190 20 0.50 76.8 1.60 faster, so the vitrification degree of zeolite becomes higher. In this
5 1190 40 0.46 78.9 1.63
sintering process, the viscosity of ceramic sample increases, the va-
6 1200 60 0.43 80.0 1.64
porized crystal water produces more secondary pores, and the pore size
becomes larger. This makes the expansion coefficient of ceramic sample
Table 2 increase at a higher sintering temperature. As the sintering temperature
Elementary parameters of samples with relatively large pores by different sin- continually increases, the viscosity also continually increases, so the
tering processes. surface tension further increases and the pore continues to shrink.
Therefore, it isn't that the higher temperature can make a greater
Sample No. Sintering Sintering Bulk Porosity/% Average
temperature/ period/ density/ pore size/
transverse linear change rate. When the temperature goes up to higher
°C min g·cm-3 mm than a certain point, the transverse linear change rate will remain
constant.
7 1150 60 0.51 76.4 5.31 At the same sintering temperature, the transverse linear change rate
8 1170 60 0.46 78.8 5.39
9 1190 60 0.38 82.4 5.52
of the sample will increase when the sintering period extends, and it
10 1190 20 0.43 80.1 5.43 may arrive at 15.9% for all samples sintered at 1190 °C for 60 min. The
11 1190 40 0.40 81.6 5.47 most efficient heat process should occur in the third stage, when the
12 1200 60 0.38 82.3 5.50 liquid phase with appropriate viscosity can be generated to keep a
balance between the surface tension and the air pressure in the pore. In
this case, the pore size may be constantly modified to form a complete
Table 3 pore structure.
Transverse linear change rate of samples with relatively small pores before and
after sintering.
3.2.2. Microstructure
Sample No. Sintering Sintering Diameter Diameter Transverse Fig. 3 shows the SEM image of ceramic foam samples sintered at
temperature/ period/ before after linear
different temperatures for 60 min, by using the pore forming agent with
°C min sintering/ sintering/ change
mm mm rate/%
the smaller size of 1–2 mm. It can be seen that the pores in the sample
could be divided into two classes at different levels: one is the primary
1 1150 60 63 67 6.3 pore (macropore) that is caused by the pore forming agent, referring to
2 1170 60 63 68 7.9 point a shown in Fig. 3(a), (b) and (c); and the other is the secondary
3 1190 60 63 73 15.9
4 1190 20 63 69 9.5
pore (micropore) that is produced by the action of additive agent and
5 1190 40 63 71 12.7 the volatilization of crystal water contained in zeolite, referring to point
6 1200 60 63 73 15.9 b shown in Fig. 3(a), (b) and (c). When the sintering temperature rises
from 1150 °C to 1190 °C, the wall of primary pores becomes smooth
gradually. As the temperature rises, the liquid phase produced in zeolite
Table 4 increases and the evaporated crystal water cannot run out from the
Transverse linear change rate of samples with relatively large pores before and zeolite in time, which causes the secondary pore in the primary pore
after sintering. wall to be larger and the shape to change from irregular at 1150 °C
Sample No. Sintering Sintering Diameter Diameter Transverse (Fig. 3a) to roughly spherical at 1190 °C (Fig. 3c).
temperature/ period/ before after linear
°C min sintering/ sintering/ change
3.2.3. XRD analysis
mm mm rate/%
Fig. 4 shows the XRD patterns of ceramic foam samples sintered at
7 1150 60 63 67 6.3 different temperatures (1150 °C, 1170 °C and 1190 °C) for 60 min.
8 1170 60 63 69 9.5 These patterns are for the powder from grinding the foam sample, so
9 1190 60 63 73 15.9 they include all the phases contained in the sample. From this figure, it
10 1190 20 63 70 11.1
11 1190 40 63 72 14.3
can be seen that the zeolite phase disappeares and the albite phase
12 1200 60 63 73 15.9 appeares in the foam sample after sintering. The phase compositions of
these three samples are basically the same, but their intensity of char-
acteristic peaks decreases obviously with the raise of sintering tem-
display an evident change in the size of the samples before and after perature, indicating the amorphous phase formed more easily at the
sintering at different temperatures for different periods. With the same higher sintering temperature. Fig. 5 shows the XRD patterns of ceramic
sintering period, the transverse linear change rate of samples will in- foam samples sintered at 1190 °C for different periods (20 min, 40 min,
crease when the sintering temperature goes up, but the increasing rate and 60 min). It also reveals the basically same characteristic peaks for
gradually slows down and finally tends stable. In the early stage of these three samples. The intensity of characteristic peaks gradually
sintering, there is relatively high air pressure in the pore and the gen- decreases as the sintering period increases from 20 min to 60 min, in-
erated liquid phase is a little to result in a relatively small surface dicating more amorphous phase formed at the same sintering tem-
tension, so those pores expand rapidly and become connected with each perature of 1190 °C for a longer period. More importantly, carbon from
other. In the second stage, the air pressure decreases in the pore due to the decomposition of pore-forming agent is found to become less and
the continually connected pores and some fractured pores. The surface less with the increase of the sintering period by SEM observation.
tension continually increases with the increase of liquid phase, and then Several experiments all showed that the pore-forming agent could be
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Fig. 3. SEM images of ceramic foam samples prepared at different sintering temperatures from the pore forming agent with the smaller size of 1–2 mm: (a) 1150 °C/
60min; (b) 1170 °C/60min; (c) 1190 °C/60min.
the range of 1150 °C–1190 °C for the same sintering period, the sample
will achieve a higher porosity, with the lower porosity for the sintering
temperature at 1200 °C than that at 1190 °C. This indicates an optimal
sintering temperature at 1190 °C for achieving the maximum porosity.
The change trend of the porosity shown in Fig. 6 agrees to that of
the transverse linear change rate, which reveals that there is a re-
lationship between these two parameters of the ceramic foam. Also,
such change can be explained by the expansion mechanism of zeolite,
as mentioned above.
Fig. 7 shows the change curve of the porosity of ceramic foam
samples sintered at 1190 °C for different periods. In this figure, it can be
seen that the porosity of samples always increases with the increase of
sintering period and reaches the maximum value of 82.4% under the
optimized process (with the sintering temperature of 1190 °C and the
sintering period of 60 min). The experimental results suggest again that
the optimal sintering period should be 60 min in this work.
Fig. 5. XRD pattern of ceramic foam samples sintered at 1190 °C for different
periods. 3.2.5. Pore size distribution
Pore size is another important parameter of porous materials, and it
completely decomposed and volatilized to leave no carbon in the can be characterized by the maximum pore size, pore size distribution
sample when the sample was sintered at 1150 °C–1190 °C for 60 min, so and average pore size. In this work, the pore size of ceramic foams has a
this period of 60 min may be regarded as the optimal sintering period. relatively narrow distribution, so the average pore size could be rea-
sonable to use as an effective research parameter, which can be cal-
culated by using the optical microscope to directly observe and measure
3.2.4. Porosity the pores in the cross-section [2]. The average chord length (L) of pores
Fig. 6 shows the change curve of porosity for ceramic foam samples in the cross-section is read or marked through a microscope or micro-
sintered at different temperatures. Sintering at higher temperature in photograph and then is converted to the average pore size (D). Finally,
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Table 6
Sound absorption coefficients of the sample with relatively small pores.
Frequency (Hz) 1 2 3 4 5 Average value
Fig. 7. Influence of the sintering period on the porosity of ceramic foam sam-
ples.
the average pore size is calculated to be about 5.52 mm for the sample
with relatively large pores and about 1.64 mm for the sample with
relatively small pores, respectively.
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Table 7 Table 9
Porosity (%)/Average pore size (mm) corresponding to the ceramic foam. Sound absorption coefficients of the sample with relatively small pores.
Sample Volume fraction of pore-forming agent Frequency (Hz) 76.6% 79.9% 81.1%
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Table 11
Sound absorption coefficients of the sample with relatively large pores.
Sound wave Sample thickness: Sample thickness: Sample thickness:
frequency (Hz) 10 mm (one layer) 20 mm (two 30 mm (three
layers) layers)
Table 10
Sound absorption coefficients and pore parameters of the ceramic foam samples.
Sample type With relatively small pores With relatively large pores
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Table 12
Sound absorption coefficients of the sample with relatively small pores.
Sound wave Sample thickness: Sample thickness: Sample thickness:
frequency (Hz) 10 mm (one layer) 20 mm (two 30 mm (three
layers) layers)
requirements.
Fig. 14 shows the sound absorption curve of the sample with rela-
tively small pores. For both the sample thicknesses of 10 mm and
20 mm, the curve is almost consistent that the first absorption peaks
appears at 2500 Hz, and the corresponding absorption coefficient is
about 0.56–0.58, which is slightly higher for the thickness of 20 mm
than for that of 10 mm. The sound absorption coefficient at 4000 Hz
reaches to the maximum value of 0.78 for the thicknesses of 10 mm and
0.80 for that of 20 mm, respectively. For the sample with thickness of
30 mm, the first absorption peak appears at 1000 Hz and the corre-
sponding absorption coefficient is 0.46. With the increase of the fre-
quency, the absorption coefficient gradually decreases in the range of
1000–3150 Hz and rises in that of 3150–4000 Hz to reach up to the
maximum value of 0.89.
Fig. 15 displays the relationship between the sample thickness and
average sound absorption coefficient of the sample with relatively small
pores. From this figure, the average absorption coefficient changes just
Fig. 12. Sound absorption coefficients of the sample with relatively large pores
a little with the thickness of the sample, which indicates that it is un-
for different sample thickness.
advisable to improve the sound absorption performance by increasing
the thickness of samples with relatively small pores. For economic
consideration, the 10 mm thick foam is advocated to use instead of the
30 mm thick foam. In practical applications, the ceramic foam product
can be designed with different thicknesses to meet the actual frequency
requirements. For instance, the porous product with thickness of 10 mm
can be used to absorb the sound at 200–2000 Hz, and that with
Fig. 13. Relationship between the average sound absorption coefficient and
thickness of the sample with relatively large pores.
significantly with the increase of thickness for the sample with rela-
tively large pores. This average coefficient is 0.32 for the thickness of
10 mm and 0.44 for that of 30 mm, which suggests a good sound ab-
sorption performance. In practical applications, the ceramic foams with Fig. 15. Relationship between the average sound absorption coefficient and
different thicknesses can be designed according to the actual frequency thickness of the sample with relatively small pores.
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thickness of 20 mm will achieve a better effect of sound absorption at 0.32 for the 10 mm thick sample to 0.44 for the 30 mm thick
2000 Hz. sample, but that with relatively small pores keeps at 0.28–0.29.
(1) Two classes of ceramic foams with different pore sizes were suc- Acknowledgements
cessfully prepared by conventional molding with pore forming
agent: one is the product with the pore size of 4–5 mm, and the This work was supported in part by the Testing Foundation of BNU
other is that with the pore size of 1–2 mm. Using higher volume grant no. C19. The authors thank Dr Y.L.Li for his experimental assis-
fraction of the pore-forming agent will make higher porosity of the tance in SEM observation.
porous product, and the maximum porosity could reach 83.7% for
the ceramic foam with relatively large pores and 81.1% for that References
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