Pigment & Resin Technology

Preparation and characterisation of aluminium pigments encapsulated by composite layer containing

organic silane acrylate resin and SiO2
A.H. Gao P.H. Pi X.F. Wen D.F. Zheng Z.Q. Cai J. Cheng Z.R. Yang
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A.H. Gao P.H. Pi X.F. Wen D.F. Zheng Z.Q. Cai J. Cheng Z.R. Yang, (2012),"Preparation and characterisation of aluminium
pigments encapsulated by composite layer containing organic silane acrylate resin and SiO2", Pigment & Resin Technology,
Vol. 41 Iss 3 pp. 149 - 155
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 Preparation and characterisation of
aluminium pigments encapsulated by
composite layer containing organic silane
acrylate resin and SiO2
A.H. Gao
School of Chemistry and Chemical Engineering, South China University of Technology,
Guangzhou, China and
School of Chemistry and Chemical Engineering, Zhao Qing University, Zhaoqing, China, and
P.H. Pi, X.F. Wen, D.F. Zheng, Z.Q. Cai, J. Cheng and Z.R. Yang
School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou, China
Downloaded by New Mexico State University At 14:04 17 September 2016 (PT)

Abstract
Purpose – The purpose of this paper is to enhance the anticorrosion property of aluminium pigments and to improve their compatibility with polymers
in coating.
Design/methodology/approach – Aluminium pigments encapsulated by organic-inorganic layer were prepared by hydrolysis and condensation of
organic silane acrylate resin and tetraethoxy silane (TEOS) on the surface of pigments via sol-gel method. TEOS and poly (methyl methacryalte-n-butyl
acrylate-vinyl triethoxysilane) (PMBV) formed in advance by co-polymerisation of methyl methacrylate (MMA), n-butyl acrylate (BA) and vinyl
triethoxysilane (VTES) were used as precursors. The adhesion property of the aluminium pigments was measured by peel test, and the loss of silvery
appearance after encapsulation and acid soaking were both evaluated by colour lightness difference (DL) measurement. The encapsulated aluminium
pigments were further characterised by means of FTIR, SEM, TG and XPS.
Findings – It was found that PMBV-SiO2 thin films could be formed on the surface of aluminium pigments smoothly and uniformly, and the adhesion
and anticorrosion performances of encapsulated aluminium pigments were improved significantly.
Research limitations/implications – The organic silane acrylate resin used as a precursor in the sol-gel process could be synthesised from other
aclyate monomers. In addition, the hydrolysis and condensation mechanism of organic silane acrylate resin on the surface of aluminium pigments need
further studies.
Practical implications – The method developed provided a good solution to the two problems of aluminium pigments and increased their application
values.
Originality/value – The method of improving adhesion and anticorrosion properties of aluminium pigments was novel and could find numerous
applications in surface coatings and adhesives.

Keywords Metals, Pigments, Corrosion resistance, Anticorrosion, Resins, Aluminium, Organic-inorganic, Sol-gel, One-step encapsulation,
Colour lightness difference

Paper type Research paper

Introduction Liu et al., 2008). There are two approaches as useful

Aluminium pigments have been widely applied in the fields of
paints, inks and plastics industries for many years due to their
special metallic appearances and floating properties. Since
aluminium pigments cannot endure in acid or basic corrosion
media, a lot of researches on surface modification of aluminium
pigments to enhance their anti-corrosion have been endeavored
in the last decade (Karlsson et al., 2006; Supplit and Schubert,
2007; Kiehl and Greiwe, 1999; Iriyama et al., 1996;
The current issue and full text archive of this journal is available at
www.emeraldinsight.com/0369-9420.htm
Pigment & Resin Technology
41/3 (2012) 149– 155
q Emerald Group Publishing Limited [ISSN 0369-9420]
[DOI 10.1108/03699421211226435]
techniques to protect pigments from corrosion. One is surface
treatment with corrosion inhibitors and the other is
encapsulation of the pigments in an organic or inorganic
material (Liu et al., 2007; Glebov et al., 2001; Müller and
Fischer, 2006). SiO2 encapsulation of aluminium pigments has
been found to be one of the best methods due to its high
chemical resistance and friendliness to the environment
(Karlsson et al., 2006; Supplit and Schubert, 2007).
However, there is another limitation that raw aluminium
pigments and SiO2 encapsulated aluminium pigments have
poor compatibility with most polymers because of their
The work has been financially supported by projects of the Natural
Science Foundation of China (20976059), the Fundamental Research
Funds for the Central Universities (2009ZM0141) and the Guangdong
Provincial Natural Science Foundation of China (07006528). The authors
are grateful to K. Chen, J.X. Yang (for SEM) and F. Jiang (for FTIR) for
their experimental and measurement contributions.

149
 Preparation and characterisation of aluminium pigments
A.H. Gao et al.
distinct difference of surface properties. It causes aluminium
pigments may not be dispersed well in paints or inks and
easily be peeled off. Therefore, improving the compatibility of
aluminium pigments with resins is an important and
necessary issue for industrial application of aluminium
pigments. To encapsulate them with polymers is one
effective method. It cannot only hold good properties of
inorganic particles, but also offer them well compatibility with
resins since the polymer coatings on the interphase can
combine resins and inorganic particles very well.
It could be a good solution to the two problems of aluminium
pigments aforementioned by encapsulating them with SiO2 and
polymers. Li et al. (2008) prepared double-layer coated
aluminium pigments by encapsulating bare aluminium
pigments with vinyl group modified SiO2, followed by coating
acrylate polymer film on the surface of aluminium pigments
through polymerisation. The anti-corrosion of two-layer
encapsulated aluminium pigments were remarkably
enhanced. However, there was no discussion about effect
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of encapsulation on metallic appearance and adhesive property
of aluminium pigments. In our previous work, double-layer
coated aluminium pigments were also prepared through sol-gel
method and solution polymerisation (Gao et al., 2009).
Corrosion resistance and adhesion of encapsulated pigments
were both improved while with much loss of metallic
appearance. Nevertheless, the process of double-layer
encapsulation is too complicated to apply in industry.
In this work, the composite layer coated aluminium
pigments were prepared by reacting silane acrylate resin
with tetraethoxyl silane (TEOS) on the surface of pigments
through sol-gel method. First, organic silane acrylate resin
poly (methyl methacryalte-n-butyl acrylate-vinyl trieth
oxysilane) (PMBV) was synthesised by radical
copolymerisation of methyl methacrylate (MMA), n-butyl
acrylate (BA) and vinyltriethoxysilane (VTES). Subsequently,
PMBV and TEOS formed a thin organic-inorganic layer on
the surface of aluminium pigments during the hydrolysis and
co-condensation process. The structure and morphology of
encapsulated aluminium pigments were characterised by
means of Fourier transition infrared spectrometer (FTIR),
scanning electron microscopy (SEM), thermal gravity (TG)
and X-ray photoelectron spectroscopy (XPS). Peel test and
colour difference analysis were carried out to investigate the
adhesion and chemical resistance properties of aluminium
pigments.
Experimental
Materials
Aluminium pigments are flaky particles with median size of
30 mm (Tianlong Trade Co., Ltd, China). MMA and BA are
both purchased domestically in chemical grade and used
directly without further purification. TEOS and VTES are
purified by distillation before use. Dimethylbenzene, butyl
acetate, absolute alcohol, ammonia water and benzoyl
peroxide (BPO) are all analytical grade and used without
further purification.
Preparation of silane acrylate resin PMBV
5 mL dimethylbenzene and 5 mL butyl acetate were added
into a flask and heated to about 1308C. Then a mixture of
10.0 g MMA, 12.8 g BA, 9.6 g VTES and 0.966 g BPO, which
was pre-dissolved with 15 mL dimethylbenzene and 15 mL
150
Pigment & Resin Technology
Volume 41 · Number 3 · 2012 · 149 –155
butyl acetate, was dropped into the flask slowly and reacted
for 3 h under stirring and nitrogen flowing. After reaction, the
mixture solution was vacuum distillated under the
temperature of 808C for 24 h to obtain organic silane
acrylate resin PMBV.
Encapsulation of PMBV-SiO2 on surface of aluminium
pigments
First 1.5 g aluminium pigments and 50 mL ethanol were put
into a four neck-round bottom flask connected to a
condenser, a thermometer, and a nitrogen gas inlet/outlet.
The solution was stirred at room temperature for 1 h and then
pre-heated to 558C. A mixture of 3 g PMBV (dissolved in
10 mL dimethylbenzene), 2 mL TEOS and 30 mL ethanol
and another mixture of 3 mL ammonia, 5 mL distilled water
and 30 mL ethanol were added drop-by-drop over 1 h to the
aluminium pigments dispersion simultaneously. The mixing
solution was further stirred for 6 h before vacuum filtered.
The filter cake was washed with ethanol and acetone for
several times, and then dried under vacuum at 508C for 24 h.
Characterisation
Infrared absorption spectra of aluminium pigments were
recorded by using a FTIR Vector 33 (FTIR, Bruker Co.).
Microstructure and morphology of aluminium pigments were
observed via a SEM (XL-30, Philips Co.). Surface element
analysis of aluminium pigments was performed by an XPS
(Axis Ultra DLD, Kratos Co.). TG analysis of aluminium
pigments was carried out by using a synthetically thermal-
analytical instrument (Model STA 449C, Netzsch Co.) with
the heating rate of 108C/min using nitrogen gas as sweeping
and shielding gas.
In order to evaluate the adhesion of aluminium pigments
with resins, peel test was carried out as follows: aluminium
pigments were mixed with thinner and acrylic resin according
to mass ratio of 3:63:34, then the mixture was sprayed onto a
black plastic board and subsequently put in a vacuum oven at
temperature of 608C to be dried until fixed weight balance.
A special adhesive tape (3 M, 1.5 £ 6.0 cm) was attached
tightly on the coating board containing aluminium pigments
and then was pulled off at full tilt. The weight of aluminium
pigments pulled off was measured by calculating the weight
difference of the pre- and post-peeled tape.
In order to evaluate the effect of surface modification on
colour gloss of aluminium pigments, L-value of coating
containing aluminium pigments was measured via colour-eye
(Model 3100, Macbeth Co.). The colour lightness difference
of encapsulated aluminium pigments was calculated by using
raw aluminium pigments as reference (Mardalen et al., 2008).
The chemical stability of aluminium pigments was tested by
dipping the board partially in pH ¼ 1 HCl solution at 258C
for 24 h. L-values of the surface before and after dipping test
were measured to calculate the colour lightness difference of
acid-dissolved aluminium pigments.
Results and discussion
Process of encapsulation
Figure 1 shows the preparation process of PMBV-SiO2/Al
pigments. According to the common viewpoint in previous
literature (Jones et al., 2000), siloxane containing double
carbon bonds can copolymerise with conjugative monomer
through free radical polymerisation rather than self
 Preparation and characterisation of aluminium pigments Pigment & Resin Technology
A.H. Gao et al. Volume 41 · Number 3 · 2012 · 149 –155

Figure 1 Scheme of preparation of PMBV and PMBV-SiO2/Al

CH3 COOC4H9 CH3

BPO, heating
p CH2=CH + qCH2=CH + r CH2=C CH2 CH p CH2 CH q CH2 C r
C2H5O Si OC2H5 COOC4H9 COOCH3 C2H5O Si OC2H5 COOCH3
OC2H5 OC2H5

Abbreviated as C2H5O Si OC2H5

OC2H5

OC2H5 C OH C
ethanol/H2O
C 2 H 5O Si OC2H5 + C2H5O Si OC2H5 HO Si OH + HO Si OH
NH4OH
OC2H5 OC2H5 OH OH

Si
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O O
Si
OH O
OH O C
C
–H2O Si Si
Al OH + HO Si OH + HO Si OH O O Al O
HO O
Si Si
OH OH
C O
O
OH Si
O O
Si

polymerisation. So organic silane acrylate resin PMBV can be Figure 2 TG curves of aluminium pigments
formed by copolymerisation of MMA, BA and VTES at high
temperature in the presence of initiators. Silica based organic- 102
inorganic hybrid film can be coated on the surface of
aluminium pigments through a base catalysed sol-gel process.
100
By this method PMBV and TEOS can hydrolyse and
condense together in the ethanol/water median and using
ammonia as catalyst. At the same time, hydroxyl groups on
98
the surface of aluminium particles can also participate in the
TG/%

sol-gel condensation reaction with PMBV and TEOS to form

a chemical linkage, SiZOZAl, between the aluminium and 96 a raw Al
resin, which may produce strong interaction of the sol-gel
layer on the aluminium interface. The encapsulation process
can be further verified by FTIR analysis as below. 94

Characterisation of PMBV-SiO2/Al b PMBV-SiO2/Al

TG analysis
92
TG measurements of the aluminium pigments were carried 0 100 200 300 400 500 600 700 800
out using nitrogen gas as sweeping and shielding gas. As can Temperature (°C)
be seen in Figure 2, the weight of each sample decreases with
temperature increasing until about 6008C. It may be mainly Notes: (a) raw aluminium pigments; (b) PMBV-SiO2/Al
attributed to the thermal decomposition of organic silane
acrylate resin grafted on the surface of aluminium pigments.
In addition, the oxide film on the surface of aluminium which than that of raw aluminium pigments (about 3.7 per cent).
can react with Al to produce Al2O cause the weight-loss of It may indicate aluminium pigments were encapsulated
aluminium pigments samples. This is because that Al2O may successfully by organic resin with the organic weight ratio of
vaporise at high temperature of 500-6008C. The reaction 2.8 per cent. When the temperature increases above 6008C,
equation can be expressed as follows (Cai et al., 1998): the oxide film is destroyed and then N2 molecules can
penetrate inside the aluminium paste, introducing the
Al2 O3 þ 4Al ! 3Al2 O reaction to form AlN as follow (Cai et al., 1998):
It can be found that the total weight-loss rate of PMBV-SiO2/
Al sample (about 6.5 per cent) below 6008C is much greater 2AlðsÞ þ N2 ðgÞ ! 2AINðsÞ

151
 Preparation and characterisation of aluminium pigments
A.H. Gao et al.
It finally causes the weight-increase of pigments samples as
demonstrated in Figure 2.
XPS analysis
Figure 3 shows the XPS full-survey spectra of raw aluminium
pigments and PMBV-SiO2/Al pigments. The two spectra
reveal the presence of carbon, oxygen and aluminium
elements in both samples. Compared to the XPS spectrum
of bare aluminium flakes (curve a), there are two new peaks
appeared with binding energies of 101.2 eV (Si 2s) and
153.6 eV (Si 2p) in the XPS spectrum of PMBV-SiO2/Al
pigments (curve b), indicating the presence of silica on the
surface of PMBV-SiO2 coated aluminium pigments.
The surface elemental composition is listed in Table I. By
comparison with raw and encapsulated aluminium pigments,
the relative atomic concentration of C and Al for PMBV-
SiO2 /Al pigments decreased 9.9 and 19.9 per cent,
respectively. In contrast, the oxygen content increased
19.8 per cent. As we know, the relative atomic
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concentration is directly related to the materials on the
surface of aluminium pigments. The carbon element on the
surface of raw aluminium flakes comes from the lubricant,
such as fatty acids, used in the grinding process of the
aluminium foil (Karlsson et al., 2006), while the carbon on
the surface of coated aluminium pigments is partly from the
PMBV-SiO2 film. By analysing the contents of elemental
resources in lubricants, monomers and precursors listed in
Table II, it can predict theoretically that the contents of
oxygen and silica will increase on the surface of pigments and
the content of aluminium atom will definitely decrease after
encapsulation with a film of PMBV-SiO2, which is consistent
Figure 3 XPS survey spectra of (a) raw aluminium pigments and (b)
PMBV-SiO2/Al
O 1s
CPS
b PMBV-SiO2/Al
C 1s
Si 2s
Si 2p
Al 2p
O 1s
C 1s
a raw Al
Al 2s
Al 2p
0 200 400 600 800
Binding Energy (ev)
Table I Elemental contents on the surface of different aluminium
pigments
Elemental contents (%)
Sample C O
Raw aluminium pigments 51.8 22.1
PMBV-SiO2/Al 41.9 35.6
Pigment & Resin Technology
Volume 41 · Number 3 · 2012 · 149 –155
Table II Contents of C, O and Si in different materials
C (%) O (%) Si (%)
Stearic acid 76.0 11.0 0
Oleic acid 76.7 11.3 0
BA 65.6 25.0 0
MMA 60.0 32.0 0
VTES 22.6 45.3 26.4 Hydrolyse completely
TEOS 0 66.0 29.1 Hydrolyse completely
with the experimental results performed in this paper. The
reduced content of element carbon on the coated aluminium
surface may indicate somehow the thinness of the
encapsulated film.
SEM morphology
The SEM micrographs of raw aluminium pigments and
PMBV-SiO2/Al pigments are present in Figure 4(a) and (c).
Figure 4(b) is the SEM photo of SiO2-coated aluminium
pigments (SiO2/Al) prepared as described in Li et al. (2007).
The surface of SiO2/Al sample is rough, while the surface
of PMBV-SiO2/Al pigments is much smoother. The rough
surface of SiO2/Al pigments is attributed to the random
deposit of inorganic silica granules and makes great loss of
metallic appearance. However, the encapsulated film on
PMBV-SiO2 /Al pigments is organic-inorganic hybrid
membrane, products of hydrolysis and co-condensation of
TEOS and PMBV (Joshua et al., 2001), having little influence
on the lightness of aluminium pigments.
FTIR spectroscopy
According to the process of encapsulation expressed in Figure 1,
there will be new functional groups formed on the surface of
aluminium pigments after encapsulation with PMBV and
TEOS. Figure 5 gives the FTIR spectra of VTES (curve a),
PMBV (curve b) and PMBV-SiO2/Al (curve c). The absorption
peaks appeared near 758-786 and 1,080 cm2 1 in curve a are
assigned to SiZC and SiZO group, respectively, which are the
characteristic peaks of VTES. They can also be found in curve b
near 781 and 1,110 cm2 1, suggesting VTES was involved in the
polymerisation. The peak near 1,730 cm2 1 in curve b is due to
the stretching vibration of CvO group and the characteristic
peak of CvC 1,600 cm2 1 disappeared in curve b. It also
indicates that VTES has reacted with MMA and BA to form
PMBV (the conversion rate is determined up to 98 per cent).
Comparison of curve c and curve b shows that there are new
peaks of SiZOH formed in curve c near 847 and 955 cm2 1
(Crist, 1999). It can be deduced that it is the result of sol-gel
process of PMBV and TEOS.
1,000 1,200 Adhesion of aluminium pigments in acrylate resin
The weight of aluminium pigments fallen off from coating
during peel test (Wp), was used to describe the adhesion
property of aluminium pigments in coatings. It means that
high WP value of aluminium pigments denotes poor adhesion
performance. For comparison, Wp of samples with different
encapsulation layers were shown in Figure 6. The PMBV/Al
sample was prepared by sol-gel progress as described in
Al Si experimental section but without TEOS. The vinyl-activated
26.1 0.0 aluminium pigments (V-SiO2/Al) and the polyacrylate and
6.2 16.3 SiO2 coated aluminium pigments (PA/SiO2/Al) were prepared
according to Gao et al. (2009). The results of peel test indicate
152
 Preparation and characterisation of aluminium pigments Pigment & Resin Technology
A.H. Gao et al. Volume 41 · Number 3 · 2012 · 149 –155

Figure 4 SEM micrographs of (a) raw aluminium pigments; (b) SiO2/Al and (c) PMBV-SiO2/Al (X5.0 K)

(a) (b)
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(c)

Figure 5 FTIR spectra of VTES, PMBV and PMBV-SiO2/Al Figure 6 Peel test results of different samples

a VTES 12

10
Wp/(g·m–2)

b PMBV
6

c PMBV-SiO2/Al 4

0
raw Al SiO2/Al TV/Al PA/SiO2/Al PMBV/Al PMBV-SiO2/Al

characteristic to the resin used and improves the

compatibility of aluminium pigments with coatings. The
500 1,000 1,500 2,000 2,500 3,000 3,500 4,000
adhesion of raw aluminium pigments is stronger than that of
Wavenumber (cm–1) SiO2/Al and V-SiO2/Al, because that raw aluminium pigments
are wrapped by agents which make them be consistent to resin
that the adhesion of samples encapsulated by polymers, and solvents and easy to disperse in coatings. Compared to
especially PA/SiO2/Al, is much stronger than that of bare raw aluminium pigments, the surface of SiO2/Al and V-SiO2/
aluminium flakes and other samples. The strong adhesion of Al are much more hydrophilic, resulting in seemly poor
PMBV/Al, PMBV-SiO2/Al, and PA/SiO2/Al in coatings is adhesion to coatings. Figure 6 shows that the novel single
attributable to the polyacrylate grafted on the surface of composite layer encapsulation has similar adhesive strength
aluminium pigments, which shows especially similar with the double-layer encapsulation.

153
 Preparation and characterisation of aluminium pigments
A.H. Gao et al.
Colour lightness difference analysis
The special metallic appearance of aluminium pigments is an
important factor for its widespread use in many fields.
However, surface modification may somewhat weaken the
lightness of aluminium pigments, or even cause them lose
their application value. DL is used to evaluate the lightness
difference of two colours according to CIE uniform colour
space (Mardalen et al., 2008). The L-value, indicating the
lightness of a colour, increases as a colour becomes lighter and
decreases as it becomes darker. Results of colour difference
testing were listed in Table III. DLe and DLa refer to colour
difference of aluminium pigments by encapsulation and by
acid dipping, respectively.
As the encapsulated layer is not completely transparent,
lightness of aluminium pigments will decrease after coated.
Results of DLe in Table III show that the biggest lightness
difference is that of SiO2/Al, and followed by that of PA/SiO2/
Al, which is somewhat larger than that of V-SiO2/Al. L-value
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of SiO2/Al is 9.51 lower than that of sample V-SiO2/Al. The
difference between them arises from the different coated silica
layers. The silica film of SiO2/Al sample is formed by
randomly accumulation of granular silica, but the vinyl-
activated SiO2 film of V-SiO2/Al sample is a smooth and
dense layer. Both DLe values of PMBV/Al and PMBV-SiO2/Al
are very small, 21.10 and 2 0.24, respectively, which may be
attributed to the thin and smooth organic or composite film
on the surface of aluminium pigments.
Since, in general, the colour of a metal is light and it becomes
darker when it is corroded, the L-value can be an indicator of the
degree of corrosion of metal surfaces. Raw aluminium pigments
tend to be corroded for that lubricating agents wrapped on the
surface dissolve in dimethylbenzene and butyl acetate and lose
their protection. Comparison of DLa values in Table III
indicates that anti-corrosion performance of aluminium
pigments can be improved by coated with silica or polymer,
but the effect relies on the component and denseness of
encapsulation film. The L-value of coating containing raw
aluminium pigments dropped significantly, demonstrating that
the surface had been corroded seriously. However, DLa values of
SiO2/Al, V-SiO2/Al, PA/SiO2/Al and PMBV-SiO2/Al were very
small, which indicate excellent anti-corrosion property of these
samples. It may be attributable to shielding effect of the dense
SiO2 film and its acid resistance. By contrast, the anti-corrosion
of PMBV/Al sample performed much weakly. In a word, the
PMBV-SiO2 encapsulated layer on aluminium pigments not
only held metallic appearance of aluminium pigments well, but
also enhanced the anti-corrosion of aluminium pigments, and
improved the compatibility of aluminium pigments to resins.
Table III Colour lightness difference of samples
Sample DLe DLa
Raw aluminium pigments 0.00 249.95
SiO2/Al 2 14.66 2 0.33
V-SiO2/Al 25.15 2 0.37
PA/SiO2/Al 26.67 2 0.30
PMBV/Al 21.10 241.66
PMBV-SiO2/Al 20.24 2 0.56
154
Pigment & Resin Technology
Volume 41 · Number 3 · 2012 · 149 –155
Conclusions
PMBV-SiO2/Al were successfully prepared by a base catalysed
sol-gel method using organic acrylate silane resin PMBV and
TEOS as precursors to promote anti-corrosion of aluminium
pigments and enhance their compatibility with polymers in
coating. Compared to raw aluminium pigments, the Wp value of
PMBV-SiO2 /Al pigments dropped remarkably, which
indicating the compatibility of aluminium pigments with resin
was improved obviously. The analysis of metallic colour
lightness and chemical stability demonstrated that the novel
single-layer composite PMBV-SiO2 film has the same corrosion
resistance performance as the double-layer organic-inorganic
encapsulation, while it can keep better metallic appearance of
raw aluminium pigments than that of the double-layer coating.
According to the comparison of PMBV-SiO2/Al to some other
samples, it was found that the coated organic-inorganic
composite PMBV-SiO2 layer provided the improvement of
compatibility and anti-corrosion property.
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Corresponding author
P.H. Pi can be contacted at: phpi@scut.edu.cn

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