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Materials Today: Proceedings 17 (2019) 1001–1007 www.materialstoday.com/proceedings

RAMM 2018

Foamability of Natural Rubber via Microwave Assisted Foaming

with Azodicarbonamide (ADC) as Blowing Agent
N.S Ahmad Zauzia,b*, Z.M. Ariffa, and S.R. Khimia
a
School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia, Nibong Tebal 14300, Malaysia
b
Faculty of Engineering, Universiti Malaysia Sarawak, Kota Samaraha 94300, Malaysia

Abstract

Utilization of microwave in material processing has attracted significant interest due to its advantages such as rapid and
volumetric heating capability. However, the use of microwave in rubbers is usually focused on vulcanization and devulcanization
of rubber, but very limited on rubber foaming. Therefore in this study, attempt was made to understand the foaming behavior of
natural rubber foam (NRF) via microwave assisted processing using azodicarbonamide (ADC) as the blowing agent. The
microwave settings were varied and evaluated in relation to expansion behavior and foam structure of the produced NRF. Three
settings were used, i.e. microwave heating only, conventional heating only and third heating was sequential heating with
microwave and followed by convection heating. The results indicated that the NR can be foamed via microwave heating in less
than six minutes. However good foam structure can be produced by the sequential heating setting between microwave and
convection heating. The obtained results demonstrated that microwave can be potentially used as alternative heating to
conventional oven heating in production of rubber foams.

© 2019 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of the scientific committee of the 6th International Conference on Recent Advances in Materials,
Minerals & Environment (RAMM) 2018.

Keywords: Natural Rubber Foam; Microwave; Azodicarbonamide (ADC)

* Corresponding author. Tel.: +6-04-599-1010; fax: +6-04-599-6907.

E-mail address: syuhadazauzi@gmail.com

2214-7853 © 2019 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of the scientific committee of the 6th International Conference on Recent Advances in Materials,
Minerals & Environment (RAMM) 2018.
1002 N.S. Ahmad Zauzi et al. / Materials Today: Proceedings 17 (2019) 1001–1007

Nomenclature

P Power
T Temperature
t time
W Watt
Pphr part per hundred rubber
Ho Initial Height before foaming
Hf Height after Foaming

1. Introduction

Microwave irradiation is state of the art technique in heating a material. This technique has gradually replaced a
conventional heating in many industries such as in sintering process of ceramic, cement and concrete industries and
many other industries which involving thermal processes [1,2]. In rubber industries, microwave technique has been
extensively studied in rubber vulcanization and devulcanization [3–5]. Microwave irradiation offers many benefits
compared to conventional heating method including rapid heating rates which can save energy and time due to its
volumetric heating mechanism [2,6].
In the production of rubber foams, a chemical or physical blowing agent is the main ingredient in governing the
end properties of foam rubber. Azodicarbonamide (ADC) based chemicals is a commercial chemical blowing agent
used in the rubber foam production [7]. During rubber foam processing, there are two processes occurring
simultaneously in the rubber matrix which are expansion process by the blowing agent and curing process by the
curing agent. When heat is applied, the ADC undergoes thermal decomposition and produce gases, and this
subsequently leads to an expansion of the rubber matrix volume. Both reactions are time and temperature dependent
processes, which will determine the quality of foam produced [7,8]. Currently, there are two methods used in rubber
foaming process, namely conventional heating which can be divided into single stage and heat transfer process.
However, both methods require a minimum about 20 minutes to achieve pre-vulcanization, curing and foaming
process [8–10].
However, to date research on the utilization of microwave in rubber foaming is limited. Therefore, knowledge of
rubber expansion using the microwave is considered lacking. In this study, the effects of microwave foaming
condition on the NRF with ADC as a chemical blowing agent are investigated. The study will focus on the properties
of foam cell such as relative density, expansion ratio and cell structure with respect to various foaming conditions.

2. Experimental Methods

2.1. Materials and Sample Preparation

Natural rubber (NR) type of SMR-L was obtained from a local supplier and having technically specified
standard set by the Malaysia Rubber Board. Azodicarbonamide (ADC) and other ingredients such as stearic acid,
zinc oxide (ZnO), benzothiazyl-2-cyclohexyl-sulfenamide (CBS), tetramethyl thiuram disulfide (TMTD) and sulfur
used in this study were of industrial grade chemicals. The role of ADC and other ingredients were as blowing agent
and to act as vulcaniation agent, respectively for the rubber compound. The rubber was compounded using two roll
mills, Model XK-160, and the sequence of ingredient added is based on the list stated in Table 1. All compounds
were kept in the freezer for at least 24 hours before the foaming process.
 N.S. Ahmad Zauzi et al./Materials Today: Proceedings 17 (2019) 1001–1007 1003

Table 1. Natural Rubber Foam Ingredients

Ingredients Pphr
SMR L 100.0
Stearic acid 2.0
ZnO 4.0
CBS 1.0
TMTD 2.5
ADC 4.0
Sulfur 1.5

2.2. Foaming Process

The foaming process was conducted using a Panasonic Microwave Oven model NN CD565B, with an
operating frequency of 2.45 GHz and 27 liter size capacity. The formulated rubber compound was cut into disc
shape with approximately 5 mm thickness and 45 mm diameter and then placed in a glass mould. The sample was
irradiated in the microwave oven at different power (P), and heating period (t). The processing approach was set in
three different conditions which were microwave heating (M) only, conventional heating (C) only and sequential
heating of microwave and conventional heating (SMC). Preliminary study was conducted to find the processing
window that able give the lower and upper processing limit for successful foaming, i.e. without the occurrence of
foam collapse and rubber degradation.

2.3. Physical Appearances and Morphological Studies

The physical appearance of NRF was captured using digital camera after the compound has been successfully
foam using the microwave processing technique. While, morphology studies of foam prepared were carried out
using Tabletop Scanning Electron Microscope, model TM3000.

2.4. Physical Properties

The relative foam density of NRF was calculated according to ASTM D3575-93, using Equation 1. The solid
density is the density of unfoamed rubber compound. The foam density was measured with top and bottom skin
surface. The foam expansion ratio was determined according to Equation 2. The values obtained were an average
from triplicate measurement.

Foam Density
Relative Density 
Solid Density (1)

H f  Ho
Expansion Ratio  (2)
Ho

3. Results and Discussion

3.1. Physical Appearances

Fig. 1 shows the physical appearances of NRFs produced via different microwave processing conditions. From
the observation during the foaming process, decomposition of ADC occurs approximately at 6 mins and 8 mins of
microwaving process at 1000W and 600W, respectively. High microwave power (electric field) can generate high
local volumetric heating inside the sample and at the same time it gives an effect of sudden temperature increases as
1004 N.S. Ahmad Zauzi et al. / Materials Today: Proceedings 17 (2019) 1001–1007

compared to low microwave power [5]. High microwave power has high energy and therefore able to decompose
the foaming agent within the rubber compound in a shorter time.
In comparison between microwave and conventional heating, the NRFs produced via conventional heating has
smooth and even skin surface. It is noticeably that the NRFs produced via microwave heating have blisters. This is
attributed by the surrounding medium in microwave chamber is at ambient temperature since it is not heated directly
by the microwave radiation [11,12]. This indicates that the crosslinking process is delayed on the top of sample
surface. This can be enlightened by understanding the heating mechanism of microwave and conventional heating.
Microwave energy can penetrate the sample through molecular interaction with electromagnetic field and cause
internal heat generation. Therefore, foaming and crosslinking process is initiated from the inner section of the
sample. In contrast, conventional heating is also known as heat transfer process in which the thermal energy is
delivered to the outer section of the sample and will be transferred to bulk of the sample via conduction. The top or
exposed sample surface receives the highest energy and this allow crosslinking to take place before foaming process
occur [1,13]. As a comparison, both heating methods have different heating mechanism, where microwave is based
on volumetric heating while heating mechanism of oven is based on heat transfer. Therefore, oven heating will
cause crosslinking on the top of the sample and followed by foaming and crosslinking in the next layer of the
sample. Whereas, in microwave energy, some of the energy is absorbed by the material and converted to heat, in
turns the interior parts of the sample (inner) are hotter than its surface and initiate foaming and crosslinking
simultaneously [14].
NRF 4 shows two big cells in the inner section of the foam. This can be elucidated by the thermal decomposition
of ADC occurs at the higher rate compared to crosslinking process within this section. The vulcanization degree of
the matric phase is lower at the time when the foaming agent’s decomposed. This resulted in abrupt rupture or cell
collapse of the uncured cell walls producing big cells. According to Ariff. et. al., (2008) [15], crosslinking must be
formed before the decomposition of foaming agent accomplishes because the melted rubber would flow and could
not maintain the cell wall from collapsing.
NRF 5 and 6 were produced via sequential heating where microwaves heating was conducted first and then
followed by conventional heating. Through observation of foaming process for NRF 1 to 4 (single heating mode
approach), the thermal decomposition of ADC occurred at 8 mins at 1000 Watts. In order to avoid the larger cell
forming due to cell collapse in the inner section and blisters appearing on the foam skin, conventional heating was
introduced after the microwave heating to crosslink the outer skin of the sample and at the same time to stop
foaming process in the inner section of the sample. Therefore, the sequential heating of NRF 5 produced better foam
skin without blister formation and more uniform foam cell size was obtained. Whereas, NRF 6 demonstrates
apparent foam collapse and shrinkage phenomenon. It was observed that immediately after the foaming process, the
compound was nicely blown but due to low power and time, the foam experienced collapse which resulted from
insufficient crosslink. It projected that the foaming process needs longer than 8 mins for low power in first heating
sequence to ensure the inner rubber matrix has cured before second heating sequence is initiated.

3.2. Morphological Studies

Fig. 2 shows the morphology of various NRFs produced using different processing condition. As can be seen, the
cell shapes of all NRFs are combination of spherical and ellipsoidal shapes. The cell size is not uniform as some of
the cell was formed from two or more cells due to cell wall rupture and cell collapse. It can be observed from the
images that the NRFs produced are combination of open and close cell structure. The open cell is clearly shown by
the cross sectional images as there are more than one cell interconnection at the cell wall of neighbouring cells.
According to Mosanenzadeh. et. al., (2013) [16], open cells are interconnected throughout the material, and closed
cells are discrete and isolated from outside. Some of open cells are shown by arrow in the images. Other than that,
the closed cell can be observed from the thin layer appears at the cell walls (some of the thin walls are shown by
circle).
1006 N.S. Ahmad Zauzi et al. / Materials Today: Proceedings 17 (2019) 1001–1007

a (i) NRF 1 a (ii) NRF 2 a (iii) NRF 3

a (iv) NRF 5 b (i) NRF 1 b (ii) NRF 2

b (iii) NRF 3 b (iv) NRF 5

Fig. 2. SEM images of (a) perpendicular and (b) cross sectional of NRF produced at different setting conditions.

3.3. Relative Density and Expansion Ratio

Table 2 shows relative densities and expansion ratios of NRFs produced at different processing conditions. Here,
the solid density of unvulcanised NR is 0.93 g/cm3. It is observed that the relative density value is proportional to
foam density. The result show significant decreased in NRFs density due to more gas volume is available within the
rubber matrix resulted from thermal decomposition of ADC [17]. The result unveils that the microwave power has
profound effect on foam density. The lowest and highest relative densities are displayed by NRF 5 and NRF 6,
respectively. This can be explained by the physical appearance of NRFs as shown in Fig. 1. NRF 5 has the preferred
foam cell morphology as compared to other NRFs. All the other NRFs exhibit larger and uneven cells size in the
inner section of the foam. Whereas, NRF 6 has the highest relative density due to absence of foams cell formation in
the inner section of the foam.
The expansion ratio has similar trends with relative density except for NRF 4. For foam that was produced via
conventional heating, NRF 4 demonstrates the highest expansion ratio but based on the physical appearance, the cell
 N.S. Ahmad Zauzi et al./Materials Today: Proceedings 17 (2019) 1001–1007 1007

structure reveals that the foam cells are not created well enough and can be considered as unsuccessful foam
formation.
Table 2. Relative Density and Expansion Ratio for Natural Rubber Foams produced at different setting condition

Heating Conditions Sample Relative Density Expansion Ratio

Microwave Heating Only NRF 1 0.286 ± 0.008 1.851 ± 0.046
NRF 2 0.306 ± 0.014 1.723 ± 0.291
NRF 3 0.297 ± 0.006 1.738 ± 0.125
Conventional Heating Only NRF 4 0.285 ± 0.012 3.262 ± 0.896
Sequential Heating: NRF 5 0.258 ± 0.007 1.980 ± 0.317
Microwave and Conventional Heating NRF 6 0.704 ± 0.043 0.564 ± 0.072

4. Conclusion
It can be concluded that microwave heating was able to produce Natural Rubber Foam (NRF) in a shorter time as
compared to conventional heating. It was found that sequential heating at high microwave power was able to
produce good foam morphology which was connected to the better cell size distribution. Consecutive heating of
microwave and conventional heating which have different in heating mechanisms gave out uniform heat distribution
and allowed curing and foaming processes to occur at the suitable period, thus eliminating blister formation on the
foam skin and larger cell size in the middle section of the foam.

Acknowledgements
The authors would like to thank Universiti Sains Malaysia for the fund provided through the Research University
(RUI) grant (ref. no.: 1001/PBAHAN/80114041). Appreciation is also expressed to Universiti Malaysia Sarawak
and Ministry of Education for the financial support.

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