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Barrier properties created by dispersion coating

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 PEER-REVIEWED COATING

Barrier properties created

by dispersion coating
ROGER BOLLSTRÖM, ROGER NYQVIST, JANET PRESTON, PEKKA SALMINEN,
AND MARTTI TOIVAKKA

ABSTRACT: The objective of this work was to gain insight into 1) how a coating layer with barrier properties is
built up, 2) how different polymer dispersions and pigments function as a barrier against gases and fluids, and 3)
how the thickness and evenness of the coating layer affect barrier properties. In addition to tests for permeability of
water vapor, barrier properties required for functional applications (i.e., against solvents and acids) were studied.
Permeability of an organic solvent (ortho-dichlorobenzene) and hydrochloric acid was studied as a function of barrier
layer structure. Providing a barrier to these materials is important in the processing of printing functionality on
paper. Pigment particle orientation and tortuosity were examined by infrared spectroscopy and by high-resolution,
focused ion beam milling and imaging. The barrier properties were influenced by the thickness and evenness of the
coating layer and the mass ratio between the pigment and latex. A barrier against water vapor did not always ensure
a barrier against the organic solvent or the acid. In addition to barrier properties, the choice of coating materials
affects coatability and may provide possibilities for cost savings.
Application: Optimization of the coated barrier structure can improve barrier properties and process runnabili-
ty and lead to cost savings for end-products.

T he packaging industry uses various types of barrier

layers, such as laminated plastic and metal foils. In
conventional paper coating, mineral pigments such as clay
and calcium carbonate are used to improve the print qual-
ity, gloss, brightness, and opacity of the paper product.
The use of mineral pigments in dispersion coating to pro-
vide improved barrier properties also has been proposed
[1–14]. Dispersion coating has been suggested to be a more
environmentally friendly alternative with regard to biode-
gradability and repulping than conventional lamination
or extrusion coating [15,16]. However, extrusion-coated
biodegradable soy protein isolate-based coatings and poly-
lactic acid coatings also have been proposed to be used
for food packaging [17-18]. In these types of products, the
barrier properties are normally needed on the inside of
package to prevent grease and moisture penetration.
Recently, new value-added products with novel function-
alities (e.g., paper- or board-based printed devices for sensors,
displays, and electronic applications) have received much at-
tention [19,20]. For these products to come into everyday use,
devices with reasonable electrical performance and negligible
production cost are required. A multilayer-coated, paper-
based substrate that is suitable for printed electronics has
been developed [21-23]. In this multilayer structure, a thin
layer of mineral pigments is coated on the top of a dispersion-
coated barrier layer. The penetration of ink solvents and func-
tional materials stops at the barrier layer, which improves the
performance of the functional material and eliminates poten-
tial fiber swelling and debonding that occur when the solvents
are allowed to penetrate into the base paper.
The most common way for measuring barrier properties
is ASTM E 96/E96M-10 (“Standard Test Methods for Water
Vapor Transmission of Materials”), which monitors the water
vapor penetration as a function of time at a chosen tempera-
ture and humidity [24]. In functional printing or coating, con-
ductive, semiconductive, or insulating materials usually are
dissolved in organic solvents such as dichlorobenzene or tolu-
ene. Although these liquids are brought into direct contact
with the substrate, the solvents evaporate quite rapidly, sug-
gesting that short-term barrier properties might suffice. On
the other hand, in throw-away sensor applications, such as
medical use, acidic or basic analytes may be used and the sen-
soring process might last for several minutes, so that longer
term barrier properties are needed [25-31].
The objective of this study was to gain insight into how a
dispersion coated barrier layer is optimally built up and how
different polymer dispersions and pigments function as a
barrier against water vapor and against an organic solvent
and an acid. Different size, shape, and shape factor pigments
were blended with different amounts of styrene-acrylate,
styrene-butadiene, or ethylene-acrylate latex. The main focus
in this study was set on kaolin, shape factors, and their
influence on particle alignment and barrier properties. For
barrier dispersions, a specific ratio between the pigment and
the latex exists, acting as a threshold at which barrier
properties change significantly. Knowledge of this critical
pigment volume concentration is of great importance for
barrier coating. We also studied the influence of latex type
and amount and the requirements of coating layer thickness
for barrier properties.
APRIL 2013 | VOL. 12 NO. 4 | TAPPI JOURNAL 45
COATING

Dispersing
Shape Particle size
Trademark Definition Mineral Solids CPVC
Factor (%<2µm)
Content (%)

Barrisurf HX Platy kaolin Kaolin 100 - 58 55.7

ND1695 Fine kaolin Kaolin 30 - 55 62.8
Capim DG Std. kaolin Kaolin 15 92 68 60.3
Carbital 60 GCC GCC 1 60 78 68.0
WG333 Mica Mica >200 * 55 54.5
*55% > 45µm, d50 = 40 µm.

I. Mineral pigment properties. Main focus was set on the kaolins marked with italics.

MATERIALS AND METHOD Coating methods

Pigments and latexes
A pre-coated base paper (107 g/m²) was first blade coated with
a 10 g/m² kaolin (Barrisurf FX [Imerys Minerals Ltd.;
Cornwall,UK, plus 7 pph styrene-butadiene latex [Styron Eu-
rope GmbH; Samstagern, Switzerland] and DL 920 [Dow;
Hamina, Finland]) layer to increase the surface smoothness.
On this smoothing layer, various barrier layers were deposit-
ed. The pigments studied for use in the barrier layer were Bar-
risurf HX, ND1695, Capim DG kaolin, Carbital 60 ground cal-
cium carbonate (GCC), and WG333 mica, all delivered by
Imerys Minerals Ltd, UK. Table I summarizes the barrier
layer pigments and properties. Three latexes, one styrene-
butadiene latex (Styron Europe GmbH, HPU 120, particle size
140 nm and Tg 5°C), one styrene-acrylate copolymer latex
(Styron Europe GmbH, HPU 121, particle size 110 nm and Tg
0°C), and one ethylene-acrylic acid copolymer latex (Tecseal,
E-799/35, from Trüb Emulsions Chemie Ag; Ramsen, Switzer-
land) were used. All pigments were delivered in powder form
and dispersed in laboratory scale. Make down was carried out
in 4 kg batches with a mixer at about 1400 rpm for 30 min. A
small amount (0.2-0.5 pph) of dispersing agent (sodium poly-
acrylate) was added according to instructions from the sup-
plier. Table I lists the dispersing solids contents. The pH was
adjusted to 8.5 for all coating colors by required addition of
sodium hydroxide.
The barrier coatings were applied using laboratory-scale blade
coating (Rotary Koater, RK Print Coat Instruments Ltd; Lit-
lington, UK) or reverse gravure coating technique (MiniLabo,
Yasui Seiki Co.; Kanagawa, Japan) or pilot-scale slide curtain
coating (Styron R&D Center, Samstagern, Switzerland; and
Ilford Imaging, Marly, Switzerland). Figure 1 shows the coat-
ing methods schematically.
Determination of CPVC
The critical pigment volume concentration (CPVC) was deter-
mined by measuring light scattering as a function of drying
time with a spectrophotometer [32-34]. Latex and pigment
particles have a higher refractive index compared to water or
air. In the wet coating color, the latex and pigment particles
are surrounded by a water layer, resulting in interfaces caus-
ing high light scattering. As the coating color dries, the water
layers disappear, resulting in a decrease in light scattering. Air
voids (porosity) in the coating, coupled with the disappear-
ance of water, cause the light scattering to increase again as a
function of air and pigment interfaces. A plateau value in light
scattering means all voids are filled with latex and the critical
pigment volume concentration is not yet reached (Fig. 2).
Characterization methods
Water vapor transmission rate (WVTR) was measured accord-

1. Principle of coating methods; A: reverse gravure coating, B: blade coating, C: slide curtain coating.

46 TAPPI JOURNAL | VOL. 12 NO. 4 | APRIL 2013


2. Principle for determining pigment volume concentration
by measuring light scattering as function of drying time. The
schematic image shows the air voids (pores) at pigment volume
concentrations above the critical pigment volume concentration.
ing to ASTM E 96/E96M-10 [24]. In the current work, a tem-
perature of 23°C and a relative humidity (RH) of 85% were
used. Barrier properties against an organic solvent, ortho-di-
chlorobenzene (DCB), and against 1 M hydrochloric acid
were measured with the prism method described in Bollström
et al. [35]. The method monitors penetration of a liquid
through a substrate as a function of time with a glass prism.
The contact angles were measured in ambient conditions (RH
= 22 ±3%, temperature = 22 ±2°C) using a contact angle go-
niometer. Surface roughness was measured with a Parker
Print-Surf roughness meter. A field emission scanning electron
microscope was used for surface cross-section and layer thick-
ness measurement. A gallium focused ion beam instrument
was used for sectioning and high-resolution imaging of paper
cross sections. A double beam dispersive infrared spectrom-
eter was used for the attenuated total reflectance (ATR) infra-
red (IR) analysis. Penetration depths were about 0.5-0.6 μm
for all the coatings, using a KRS5 crystal with θ = 45° [36]. The
shape factor was determined through the conductivity based
measurement method described in Webb et al. [37].
RESULTS
Critical pigment volume concentration
CPVCs for all pigments were determined by the light scatter-
ing method (Fig. 2). Having pigments with a smaller particle
size and lower shape factor results in tighter packing, and
thereby higher CPVC, as well as allowing for a higher dispers-
ing solids content. The particle size distribution also affects
the CPVC, because a broader distribution allows for tighter
pigment packing. Figure 3 plots the measured CPVC values
vs. shape factor. The shape factor of the mica is in reality larg-
er than 200, but because of limitations of the measurement
method, shape factors larger than 200 could not be reliably
measured.
Surface properties
The contact angle for water was measured to determine the
COATING
3. Critical pigment volume concentration (CPVC) as a function of
shape factor. The shape factor of mica is in reality larger than
200. Lower shape factor pigments resulting in a higher CPVC
also allows for higher dispersing solids content.
hydrophobicity of the coated barrier surfaces. None of the
surfaces had apparent contact angles greater than 90°, which
means there will be wetting on all of the surfaces and the hy-
drophobicity will not significantly affect the barrier proper-
ties. Surface roughness (PPS 1000) was measured to provide
information about the effect of filler amount on surface char-
acteristics. The pure latex coatings provided the smoothest
layers, when defects caused by blocking (undesired adhering
of barrier-coated side to the uncoated side of paper in a roll)
problems were excluded. Adding platy kaolin clearly increas-
es roughness. The surfaces could, however, be smoothed by
calendering.
Particle alignment
Particle alignment (K) differences were determined with ATR
IR analysis by comparing the relative heights of two kaolin
–OH absorption peaks above 3500 cm-1[36,38]. The peak ob-
tained at 3695 cm-1 (surface of the kaolin particle) is divided
by the peak obtained at 3620 cm-1 (edge of the kaolin particle)
as K = I3695/I3620. A low K value indicates a high clay particle
alignment. However, raw materials influence the measured K
values, which introduce uncertainty when comparing differ-
ent types of clays. High shape factor kaolin coatings generally
had higher alignments at higher pigment volume concentra-
tion (Fig. 4). The blade coated fine kaolin coatings showed
no significant difference in particle alignment. The –CH2 peak
area below 3000 cm-1 and the sharp peak at 1730 cm-1 were
used in an attempt to assess differences in the amount of or-
ganic material present at the surface in relation to the kaolin
–OH absorption peak areas above 3500 cm-1. As expected,
significantly less organic material was found at the surface of
the coatings at the higher pigment volume concentrations.
Styrene acrylic latex was used as binder in all ATR IR particle
alignment measurements.
The alignment of mineral particles was further investigat-
ed by focused ion beam imaging. Figure 5 shows the differ-
ence between highly aligned, high shape factor kaolin and
APRIL 2013 | VOL. 12 NO. 4 | TAPPI JOURNAL 47
COATING
4. Particle alignment determined by infrared spectroscopy
for high shape factor and standard shape factor kaolin at two
different styrene-acrylate latex amounts coated with both blade
and reverse gravure methods. Average and standard deviation
values are based on three parallel measurements.
5. Focused ion beam images showing the alignment of the
kaolin particle filled latex barrier layer; A: blade coated platy
kaolin (shape factor 100) /styrene-acrylate latex (PVC 57),
coating grammage 19 g/m², B: blade coated fine kaolin (shape
factor 30) / styrene-acrylate latex (PVC 57), coating grammage
14 g/m². The inserted images show, schematically, the longer
pathway for liquid to penetrate the highly aligned platy kaolin
coating structure, compared to the pathway through the lower
shape factor kaolin structure.
48 TAPPI JOURNAL | VOL. 12 NO. 4 | APRIL 2013
less aligned, lower shape factor kaolin. The alignment of the
curtain-coated, high shape factor kaolin was only studied by
focused ion beam. Coating method did not show any signifi-
cant difference in particle alignment. The alignment of par-
ticles influences the tortuosity (i.e., the pathway for a liquid
to find its way through the structure). This is illustrated in the
inserted images for both structures (Fig. 5).
Barrier properties
Barrier properties against water vapor were measured at 23°C
and 85% RH as a function of coated layer thickness. Different
humidity and temperature conditions were used, but the ones
performed at higher humidity or higher temperature provide
clearer differences between high and low barrier properties
[39]. A barrier layer can be built up by use of pure latexes,
which, however, easily results in blocking problems. An addi-
tion of mineral pigments into the latex reduces the blocking
problem and, depending on the size and shape factor, also
might improve the barrier properties. Taking into account the
price, significant cost savings can be achieved by filling the
latex film partially with mineral pigments. However, the
amount of pigment added should not exceed the critical pig-
ment volume concentration to avoid loss of barrier properties.
In the current work, the addition of blocky carbonate or low
shape factor kaolin significantly reduced the blocking prob-
lems, but no improvement in the barrier properties could be
observed. The unstable viscosity of extremely high shape fac-
tor (>200) mica resulted in coatability problems and uneven
coating layers. However, the barrier properties with this pig-
ment measured on small defect-free areas indicated signifi-
cantly improved barrier properties (58 g/m²/day at a coat
weight of 18 g/m² and PVC of 44% blended with styrene-acry-
late latex). The addition of high shape factor (100) platy kaolin
reduced the blocking and improved barrier properties.
Figure 6 shows the influence on barrier properties
(WVTR, normalized to 15 μm) by addition of high (100) and
low (30) shape factor kaolin at different amounts. For low
shape factor kaolin, the improvement is minimal compared
with pure styrene-acrylate latex. At low pigment volume con-
centration (40) a significant improvement can be observed.
One explanation is the blocking problem with the sticky sur-
face of the pure latex, which caused defects in rewinding. The
addition of high shape factor (100) kaolin significantly reduc-
es the penetration at both pigment volume concentration lev-
els when combined with styrene-acrylate latex. The standard
deviations of the barrier properties measured from the coat-
ings containing low shape factor kaolin were significantly
larger compared with the negligible standard deviation of the
barrier results obtained from the coatings filled with high
shape factor kaolin. This might be a result of nonhomogenous
or poor alignment of the particles (Fig. 5b).
Figure 7 shows the WVTR for three latexes filled with
high shape factor kaolin. The most obvious difference can be
seen for the styrene acrylate latex where addition of kaolin
clearly improves the barrier properties at the same layer thick-

6. Normalized (15 μm thickness) water vapor transmission rate
at 23°C and 85% RH for kaolin with a shape factor of 30 (fine
kaolin) and 100 (platy kaolin) combined with different amounts
of styrene-acrylate and styrene-butadiene latexes. Coating
method was reverse gravure.
7. Barrier properties against water vapor transmission rate at
23°C and 85% RH as function of barrier layer thickness. The
values are average values of three parallel measurements,
with a negligible standard deviation (B = tendency for blocking,
P = risk for pinholes). The values are an average of three
parallel measurements, measured over two days (six values).
The standard deviation is negligible (±0.2–5 g/m²/day), which
is a sign of defect free coated areas.
ness, whereas for the styrene butadiene latex the difference
is smaller. While the highest barrier properties could be ob-
tained by using pure ethylene acrylic latex, an addition of 44
vol-% kaolin did not significantly weaken the barrier proper-
ties against water vapor. All the coatings (Figs. 7-9) were
applied by reverse gravure technique except for the platy
kaolin combined with ethylene acrylic latex at a pigment vol-
ume concentration of 44%, which was applied by curtain
coating. The WVTR barrier properties for the base paper (in-
cluding precoating and smoothing layer) were 795 g/m²/day.
In addition to barrier properties against water vapor, bar-
rier properties against liquids directly applied onto the sur-
face of the substrate were measured. These measurements
COATING
8. Barrier properties against ortho-dichlorobenzene. The figure
shows the time in seconds for the liquid to penetrate the
substrate (B = tendency for blocking, P = risk for pinholes).
9. Barrier properties against 1 M hydrochloric acid. The figure
shows the time in seconds for the liquid to penetrate the
substrate (B = tendency for blocking, P = risk for pinholes).
were made to mimic a coating or printing operation, or an
analysis procedure in a printed functional application. In
such applications, organic solvents are common as ink vehi-
cles and acids as analytes in sensor applications. These re-
quire barrier properties for varying times. An example of a
practical example is ion-selective electrodes manufactured
by printing on multilayer coated paper [31]. During the print-
ing process, the paper must withstand the organic solvents
in the inks; during the analysis procedure, which may take
up to 1 h, the paper needs to withstand an acidic analyte.
Figure 8 plots the time it takes for DCB to penetrate the sub-
strates. As can be seen for all the latexes, the addition of high
shape factor kaolin clearly improves the barrier properties.
This might be related to the increased tortuosity through the
particle filled structure (Fig. 5a). The organic solvent par-
tially dissolves the latex, but the inert high shape factor min-
eral particles create a long pathway for the solvent to migrate
through. Differences in dissolving or degrading of the latexes
also can be seen; the styrene-butadiene and styrene-acrylic
dissolve most rapidly, while the ethylene-acrylic withstands
the organic solvent for a longer time.
Contrary to the barrier properties against DCB, the pure
APRIL 2013 | VOL. 12 NO. 4 | TAPPI JOURNAL 49
COATING
latexes and the layers with low pigment volume concentra-
tion show the best barrier properties against 1M hydrochloric
acid. This can be related to voids existing in the layers filled
to 57% by pigments, because the critical pigment volume
concentration for the platy kaolin is at 55.7% (Figs. 2 and 3),
and the lower amount organic material on the surface of
these layers resuls in a more hydrophilic surface and more
complete wetting (Table II) [40]. In the case of the thin (5
μm) kaolin and ethylene acrylic latex layer, the penetration
was caused by pinholes. The latexes were all inert against the
hydrochloric acid, showing none of the degradation or dis-
solving tendency that was seen with the organic solvent. The
DCB and the hydrochloric acid both penetrate the basepaper
(including precoating and smoothing layer) in less than 5 s.
price differences between oil-based latexes and mineral-based
pigments, filling the latex based barrier layer with an opti-
mized amount of pigments might offer significant cost sav-
ings, along with improved barrier properties and reduced
blocking tendency. Although we faced coatability problems
with the mica pigment with the laboratory-scale coating
equipment, high shape factor mica might be an excellent ma-
terial for creating tortuous barrier structures. TJ
ACKNOWLEDGEMENTS
Marco Ahtinen and the laboratory personnel at Styron Europe
Samstagern and Gilbert Gugler and the laboratory personnel
at Ilford Imaging Marly carried out the curtain coatings, and
the Academy of Finland provided financial support.

CONCLUSIONS LITERATURE CITED

Dispersion coating has received increasing attention as a pro-
duction method to apply barrier coatings, being hailed as
more environmentally friendly compared with extrusion coat-
ing or lamination. High barrier properties against gases and
liquids are required, and the growing interest for paper to be
used as a substrate in functional applications sets new require-
ments regarding barrier properties against solvents and acids.
The latex, whether it is styrene or ethylene based, can be con-
sidered the most important material for creating a sealed layer.
Adding mineral pigments can improve the coating barrier
properties and reduce runnability problems. Latexes, espe-
cially with low Tg, tend to cause blocking problems, but add-
ing any mineral pigment can significantly reduce the blocking
problem. The addition of high shape factor kaolin improved
barrier properties by increasing tortuosity. The tortuosity cre-
ated by the inert mineral pigments was extremely important
against DCB, which can dissolve or degrade the latexes. The
addition level of mineral pigments should not exceed the crit-
ical pigment volume concentration, because any porosity will
deteriorate the barrier properties. Taking into account the
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Contact Angle (°) PPS 1000 (μm)

Barrier Layer Formulation Layer Thickness (μm)
Avg Std. dev. Avg Std. dev.

100% SA* 12 82.2 2.3 0.68 0.11

Platy kaolin / SA, PVC = 57 24 75.9 0.6 1.98 0.03
Platy kaolin / SA, PVC = 40 15 73.8 1.2 1.28 0.02
100% SB* 18 72.1 1.7 1.04 0.03
Platy kaolin / SB, PVC = 57 14 46.1 2.0 2.02 0.02
Platy kaolin / SB, PVC = 40 14 68.8 2.6 1.56 0.04
100 % EA 17 85.0 1.0 1.02 0.03
Platy kaolin / EA, PVC = 44 13 86.0 0.8 2.05 0.04
* Blocking tendency, results obtained from defect free areas.

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ABOUT THE AUTHORS
We chose this topic to research because of the grow-
ing interest of using paper as a substrate for various
printed functional applications. A detailed under-
standing of the requirement of barrier properties and
how to optimally meet those demands is needed.
In this work, we focused on barrier properties re-
quired for functional applications (i.e., solvent and
acid barrier properties), which generally are not re-
quired for ordinary products. During this research, we
found that the pigments with extreme shape factor
were difficult to disperse and coat, but important as
reference material. Of particular interest was the high
alignment of the platy kaolin pigments.
Bollström Nyqvist Toivakka
View publication stats
COATING
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For mills, optimization of the coated barrier struc-
ture can improve barrier properties and process run-
nability, and lead to cost savings.
The next step is to use multilayer dispersion coat-
ed paper as substrate for various printed function ap-
plications, and development of novel applications.
Bollström is researcher, Nyqvist was a student, and
Toivakka is professor at the Center for Functional
Materials, Laboratory of Paper Coating and Converting,
Department of Chemical Engineering, Åbo Akademi
University, Turku, Finland. Preston is senior scientist
with Imerys Minerals Ltd., Cornwall, England. Salminen
is R&D Fellow at Styron Europe GmbH, Samstagern,
Switzerland. Email Bollström at roger.bollstrom@abo.fi.
Preston Salminen
APRIL 2013 | VOL. 12 NO. 4 | TAPPI JOURNAL 51