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Evaluation of wood gap fillers composed of microcrystalline cellulose, paper

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 Evaluation of wood gap fillers composed
of microcrystalline cellulose, paper pulp,
and glass microballoons
Ebtehal Mahmoud Montaser
Conservation Center, Grand Egyptian Museum, Giza, Egypt
Nesrin M.N. El Hadidi
Cairo University, Cairo, Egypt, and
Enas Abo Elenen Amin
Minia University, Minya, Egypt

Abstract
Purpose – This paper aims to provide a deeper understanding of using filling materials that are used to fill gaps in wooden objects, and their
response to changes in the surrounding environment to evaluate wood gap fillers and choose the best material. As a wide variety of materials, but
most of them were unsuitable for filler mixtures. Specific materials were used, which can adapt to changes in wood size in response to changes in
humidity. This research discusses the results of experiments that were conducted to determine how gap fillers composed of glass microballoons,
microcrystalline cellulose and paper pulp fills are mixed with Klucel G, Paraloid B-72 and methyl cellulose as binders, and respond in various
conditions.
Design/methodology/approach – It requires using several scientific and analytical techniques to provide a deeper understanding of filling
materials characterization, dimensional stability, their shrinkage and study mechanical properties.
Findings – The analytical study of filling gaps in wooden objects with different filling materials allowed defining that the main drawbacks of the
examined gap fillers were low water resistance, poor dimensional stability upon drying, or exposure to water vapor or liquid water, and fragility.
Two types of gap fillers with high mechanical properties and pH values similar to those of wood were found to be appropriate for application on
wooden archaeological artifacts.
Originality/value – The importance of the experimental study was to determine suitable filling materials and provide the basic characteristics of
filling materials reversibility, workability, dimensional stability, lack of shrinkage, drying, ability to take color and be shaped, stability with aging,
compatibility with wood in terms of behavior with changing humidity and non-toxicity. Also, strength properties or their likelihood to deform easily
allowing changes in the shape of the wooden object during the movement of wood, either of which may be desirable in specific circumstances.
Keywords Mechanical properties, Gap, Microcrystalline cellulose, pH value, Filling materials, Microballoons, Paper pulp
Paper type Research paper

Introduction wood is the process by which missing parts are completed, and
degraded parts can be replaced to protect them from continued
Wooden artifacts are unceasingly subjected to various abiotic damage (Unger et al., 2001; Cleary, 2014). Filling the gaps
and biotic factors that cause their degradation due to the nature in such objects requires the use of specific materials that in
of wood by their response to changes in their environment particular can adapt to changes in wood dimensions in response
(Kryg and Broda, 2019). to humidity variations (Kryg and Broda, 2019). Gap-filling
Moisture causes wood deformation or even cracking due to wooden objects, which are in an advanced state of decay, raise
cyclic swelling and shrinkage. It also causes paint and gilding to serious issues to any conservator, but that differs from one case
peel off and then promotes microbial decay (Pamic and to another. The weight of the filler material and thermal
Pohleven, 2015). Changes in temperature, UV radiation and expansion may be suitable, but because of its hygroscopic
insect activity cause additional damage. As a result, severely properties when the moisture content increases, a
decayed wood artifacts are often full of losses, cracks and microbiological infection may occur (Rowell, 2005).
crevices of various shapes and sizes (Tolvaj et al., 2016; Acceptable filling material has been defined as being either
Fulcher, 2017). The filling of cultural heritage objects made of lower or having a lower compression module than that of the
surrounding wood material. Filler materials should deform
The current issue and full text archive of this journal is available on Emerald before wood, if the wooden object was subjected to stresses
Insight at: https://www.emerald.com/insight/0369-9420.htm (Fulcher, 2015). Therefore, the applied filling material must be

Pigment & Resin Technology Received 17 August 2021

© Emerald Publishing Limited [ISSN 0369-9420] Revised 30 December 2021
[DOI 10.1108/PRT-08-2021-0096] Accepted 8 January 2022
 Evaluation of wood gap fillers Pigment & Resin Technology
Ebtehal Mahmoud Montaser et al.

Table 1 Different materials chosen for gap fillers

Materials Manufacturer Notes
Filler Microballoon CTS The hollow glass microspheres consist essentially of an aluminosilicate glass of a glass
composition (Matsubara et al., 2002)
Microcrystalline Egypt Nano Technology Microcrystalline cellulose (MCC) is produced by depolymerization of cellulose materials with
cellulose (MCC) Center Cairo University solutions of mineral acids at increased temperatures up to the level-off degree of polymerization
(LODP) from 120 to 250
Paper pulp CTS Pulp is a lignocellulosic fibrous material prepared by chemically or mechanically separating
cellulose fibers
Binder Klucel G CTS Hydroxypropyl cellulose is a cellulose ether KG with a weight of 5 g that was added to 100 ml of
distilled alcohol with stirring for 2 h until complete miscibility
Paraloid B-72 CTS High-molecular thermoplastic resin composed of two monomers (methyl acrylate and ethyl
methacrylate). Paraloid B72 in 100 ml of acetone with a weight of 0.15 g was dissolved in a flask
and stirred for 4 h until complete miscibility
Methyl cellulose CTS MC with a weight of 1 g was added to 100 ml of distilled water with stirring for 1 h until complete
miscibility

compatible with the essence, the age, the way the support is Materials and methods
manufactured and used in work, state of conservation and
Sample preparation
patrimonial value. The filling of the wood support is the
Different mixtures were formed by choosing various
operation through which the missing parts are completed and
components (Table 1) and different concentrations as shown in
the degraded ones are replaced.
Table 2. The materials were mixed together with a hand mixer
The substances used for wood protection must be efficient
until a homogeneous product was obtained. The prepared
against insects and fungi, but must not have toxic effects on
material was immediately placed in a cube-shaped silicone
persons. Also, it must not change the wood’s color or have
mold with inner dimensions (3 cm
3 cm
3 cm) for
negative effects on its properties (Hutanu, 2013) Typically, a
compressive strength tests and a rectangle-shaped mold
fill material consists of two components, one of which is a filler,
(10 cm
2 cm
2 cm deep) (Figure 1) for tensile strength
such as wood powder and cellulose or glass microballoons, and
testing. The intent of the presented research was to characterize
the other is a binder, which could be chosen from a variety of
the properties of gap fillers themselves and choose the most
natural glues, waxes and resins (Abdallah et al., 2016).
appropriate materials. After two weeks of air-drying at room
Although the filling materials are very varied, none of them
temperature (22 6 3°C), the gap fillers were removed from the
meets all the requirements. The most important and common
silicone molds and left to dry for two further weeks, after which
problem is their susceptibility to changes in temperature and
the properties of the dried material were studied.
humidity and the related dimensional stability, i.e. excessive
swelling or shrinkage that threatens the integrity of wooden Sample characterization
objects (Deurenberg-Wilkinson, 2015). Other disadvantages of The surface of the filler material should be similar to the
bad adhesion are formation of open spaces between the fill and preserved wooden objects. It can be processed into various
wood substrate, or non-removability, which damages surfaces shapes using simple tools. Previously dried fill samples of each
(i.e. changes in wood color, leaks, destruction of paints and fill material were swabbed with water and acetone, using a
gildings), low mechanical resistance, short working times, or in cotton swab. A scalpel blade was used to try to adjust the shape
the case of natural materials, high susceptibility to of the samples by carving or shaving the sides, and they were
biodegradation (Craft and Solz, 1998). As a result, there is a abraded using medium-grade garnet paper (120).
continued need to identify more appropriate gap fillers to One of the most common ways of achieving color to filler
adequately protect historic high-value wood objects (Young samples is by mixing dry dyes with the fill while it is being
et al., 2002; Szczepi
nska, 2014). prepared, or painting the fill after curing. In this research, the
The different steps of this study and the purpose of the work surface of the samples was painted after curing. The ease with
presented aim to provide a systematic comparison of various which the cured fills could be painted was observed by creating
filling materials by conducting a sample characterization and flat areas of each fill, approximately 5 cm square, that were
identifying the toughness and compressibility/flexibility of fill, painted with acrylic emulsion paint, watercolor paint (mixed
in addition to the feasibility of coloring or shaping the fill after from solid block using tap water), gouache (premixed in a tube)
curing. The study includes measuring the dimensional and oxide colors.
shrinkage of the fills upon curing and pH of fill before and after Measuring pH The pH of the samples was determined by an
aging. extraction method. An impervious pH–temperature pocket
Mechanical tests were performed to determine the highest tester with replaceable probe was used (Adwa). The samples
compressive strength of the 12 selected filling materials. were ground to form a powder, and 2 g of powder was added to
Significant shortcomings will determine the direction of further 50 ml of boiling deionized water and agitated for 5 min in a
research toward developing new enhanced conservation measuring device. The mixture remained in the enclosed tester
materials. for 30 min and was cooled at room temperature. The sample
 Evaluation of wood gap fillers Pigment & Resin Technology
Ebtehal Mahmoud Montaser et al.

Table 2 Materials used in preparation of gap-filling samples

Volume
Sample name Filler material Binder concentration of binder General description
KM Microballoon KG in ethyl alcohol 5% 4 ml Hard and compact, easily scratched
Klucel 1 Microballoon
MC.M Methyl cellulose in water 2% 2 ml Very soft and fragile, easily
Methyl cellulose 1 Microballoon scratched
B72.M ParaloidV
R B-72 in acetone 3 ml Compact, hard, difficult to scratch
Paraloid B-72 1 Microballoon 15%
K.M.Pp Microballoon KG in ethyl alcohol 5% 4 ml Very brittle, easily scratched
Klucel 1 Microballoon 1 paper pulp and paper pulp 1:1
MC.M.Pp Methyl cellulose in water 1% 2 ml Very brittle, easily scratched
Methyl cellulose 1 Microballoon 1
paper pulp
B72.M.Pp ParaloidV
R B-72 in acetone 5 ml Compact, hard, difficult to scratch
Paraloid B-72 1 Microballoon 1 15%
paper pulp
K.M.MCC Microballoon and KG in ethyl alcohol 5% 4 ml Easily scratched, quite hard
Klucel G 1 Microballoon 1 microcrystalline
microcrystalline cellulose cellulose 1:3
MC.M.MCC Methyl cellulose in water 1% 4 ml Very soft, incoherent
Methyl cellulose 1 Microballoon 1 2%
microcrystalline cellulose
B72.M.MCC ParaloidV
R B-72 in acetone 3 ml Hard, difficult to scratch
Paraloid B-72 1 Microballoon 1 15%
microcrystalline cellulose
K.Pp Paper pulp KG in ethyl alcohol 5% 4 ml Easily scratched, not too hard
Klucel G 1 paper pulp
MC.Pp MC in Water 2% 3 ml Very soft, easily scratched
Methyl cellulose 1 paper pulp
B72.Pp B72 in acetone 15% 5 ml Compact, difficult to scratch
Paraloid B-72 1 paper pulp
R B-72; KG – KlucelV
Notes: The abbreviation scheme is as follows: Binders: B72 – ParaloidV R G; and MC – methyl cellulose. Fillers: M – glass microballoons;

MCC – microcrystalline cellulose; and Pp – paper pulp

was filtered, and the pH of the solution was measured using a to 25 years of life of the objects, was performed on samples at
pH meter (Humar et al., 2001). 80°C and 65% relative humidity for 120 h in a Binder dryer
Aging of samples Accelerated thermal aging conditions were with digital indicator, model no. 9240300 (Kaminska et al.,
applied to give a fair representation of the actual long-term 2004; Arias, 2013; Pentzien et al., 2011).
behavior of materials inside the museum (Zidan et al., 2006) to Dimensional stability and shrinkage To evaluate the
determine if the pH value and mechanical properties are dimensional stability of spatial fillers during drying, the
affected by artificial aging. Thermal aging, which is equivalent traditional method of measurement between the two sides of
the material was conducted after filling the prepared material
Figure 1 Samples in a silicone mold during preparation and drying into a wooden mold of Pinus halepensis, which contained round-
process shaped apertures with a 20-mm diameter and 20-mm depth.
After thermal aging conditions of the samples, the
measurements in two directions were recorded. All the
measurements were taken by digital calipers with an accuracy
of 0.01 mm as all changes in the dimensions of each sample
were presented as linear shrinkage (Sl) in two directions and
calculated according to the following equation:
l0  l1
S ¼  100ðwhere l0 – initial dimension of a sample
10
and l1 – final dimension of a sample after agingÞ

The equation was also used to calculate dimensional changes

in the samples.
 Evaluation of wood gap fillers Pigment & Resin Technology
Ebtehal Mahmoud Montaser et al.

The shrinkage experiment assessed the amount of shrinkage Figure 3 Samples that failed to give good results: paper pulp with
that occurred after drying. This was conducted by filling the methyl cellulose
prepared fill materials in the previously prepared wooden mold.
Fill materials were left to dry for a week, after which the
thickness and diameter of each sample were measured with a
digital caliper. This was followed by exposing the samples to
thermal aging at 80°C for 120 h (five days), which is equivalent
to 25 years of an object’s lifetime, after which the dimensions of
the samples were measured again.
Compressive strength Samples were compressed in the
transmitter, and it is believed to far exceed the maximum force
that could be applied to a fill in wood objects. The effect of
sample loading and the load at which samples fracture, if any,
were observed (H5KT/130-5000N [ASD 3 787 ASTM Ball
TEST TSX-2O]).
Tensile strength Tensile tests aim to evaluate the mechanical
behavior of the fill under tension, in addition to evaluating the
adhesion of the filling system (N 200 WOLPERT-AMSLER
750 TUZ 20. M).

Results and discussion

After drying, some samples started cracking, crumbled and chemical stability, transparency, reversibility and mechanical
began to separate in some parts, except for four samples with resistance.
the following fillers: microballoon: paper pulp 1:1 and The overall appearance and finishing properties of the
microballoon: microcrystalline cellulose 1:3. The samples examined gap fillers (which are used for convenience going
mixed with different binders such as KlucelV R G (KG) and forward) are described in Table 3. To simplify the evaluation of
Paraloid B72 formed relatively good cubes, but methyl finishing properties.
cellulose (MC) samples were much weaker (Figures 2 and 3).
Their surface was smoother and more uniform, thus easier to Facility of coloring or shaping
finish and tailored to the appearance of the surrounding The paints were easier to apply to the filler that had a smoother
wooden material of the conserved artifact. However, they were surface, such as microballoon: microcrystalline cellulose 1:3,
also quite brittle, especially in combination with ParaloidV R which were the easiest fillings to paint, followed by
B-72. microballoon: paper pulp 1:1 and also microballoon filling
KlucelVR fillers were easy to mix and formed in the most samples. Painting with acrylic was generally easier than with
coherent and pliable pastes, were with a high concentration of water color or oxide colors, because the acrylic emulsion
adhesive, small particle size and compatibility of solvents. The covered all surfaces well, and was easier to apply on fillings with
samples that mixed well, those made with microballoons, a flat surface (Figure 4).
formed the smoothest paste but were brittle. Those made with
short fiber paper pulp also had a smooth surface but were more Shaping
flexible. Also, the ParaloidV R B72 fillers were very hard and For the tested filler, the ones with smaller particle size, such as
strong, and also had compatibility with various materials, microballoon: microcrystalline cellulose 1:3 or microballoon,

Figure 2 Samples that gave good results, from left: microcrystalline Figure 4 Paints applied to fills for coloring test
cellulose: microballoon with Klucel G and paper pulp: microballoon with
Klucel G
Table 3 Notes on materials used for shaping the gap fillers

Filling materials Binders Acetone IMS Water Scalpel Sanding

Evaluation of wood gap fillers
Ebtehal Mahmoud Montaser et al.

Microballoon R
Klucel G
V Softens and dulls edge The material is removed quicker than with Some parts were Can be shaved with a Sands neatly and smoothly
water; the shape may be altered removed sharp blade
Methyl Quickly removes large Fast removal of a lot of material Removes the material; Easy to carve Very easily tampered with by
cellulose quantities of material the shape may change sanding
ParaloidVR Controls the removal of No effect No effect Can cut but not treat, and Very hard; sandblast able but
B-72 material requires a lot of force slow (garnet)
Microballoon R G
KlucelV Quick removal of Removes material; shape can be altered Removes material; Easy to carve Very easily tampered with by
and materials shape can be modified sanding
microcrystalline Methyl Quick removal of Removes material; shape can be altered Quick removal of Maybe razed with a sharp Leaves the surface softer
cellulose 1:3 cellulose materials materials blade
ParaloidVR Controls the removal of No effect No effect Can cut but not treated Very hard; possible to sand but
B-72 material and requires much force slow
Paper pulp R G
KlucelV Removes material; shape Removes material; shape can be changed Material softened and Easy to carve Very easily tampered with by
can be modified removed somewhat sanding
Methyl Removes the material; Removes material; shape can be altered Material softened and Can be shaved with a Leaves the surface softer
cellulose the shape may change removed somewhat sharp blade
ParaloidVR Controls the removal of No effect No effect May cut but not clean and Very hard; possible to sand but
B-72 material requires much strength slow
Microballoon R G
KlucelV Quick removal of Removes material; shape can be altered Removes material; Easy to carve Very easily tampered with by
and Paper Pulp materials shape can be modified sanding
1:1 Methyl Quick removal of Removes material; shape can be altered Quick removal of Maybe razed with a sharp Leaves the surface softer
cellulose materials materials blade
ParaloidVR Controls the removal of No effect No effect Easy to shave, but requires Sand has a smoother finish with
Pigment & Resin Technology

B-72 material a lot of strength vigorous scrubbing (garnet)

 Evaluation of wood gap fillers Pigment & Resin Technology
Ebtehal Mahmoud Montaser et al.

were easier to shape and had the smoothest surfaces. Samples material just like wood powder, thus its moisture behavior is
of paper pulp: microballoon 1:1 (with KG and ParaloidV R B-72) quite similar). She showed that all the samples containing paper
resulted in a more coherent and stronger fill that gave good pulp shrunk significantly more than samples based on glass
results when applying pressure of a scalpel blade or sandpaper. microballoons, regardless of the adhesive or solvent type.
The ethyl alcohol applied by swabbing showed to have little However, in our study, no marked tendency to contraction can
effect on the shaping using a scalpel in the samples containing be observed while comparing the applied fillers.
KG, although this is an excellent solvent for the adhesive; while Thereby, the results obtained for the examined material
acetone applied by swabbing showed a good effect on the allows concluding that the properties of a binders play a greater
shaping with a scalpel in the samples containing ParaloidV R B- role in their dimensional stability upon drying than the nature
72. of the filler applied. No sample cracking and no particular
Results from the experiment of shaping after curing, using influence of the adhesive concentration in the gap fillers on
solvent, scalpel and sanding with garnet paper and their shrinkage upon drying was observed.
microballoon, showed that there was no difference in terms of
ability to shape between the microcrystalline cellulose or fibers Compressive strength
of paper pulp: microballoon, which were added to a KG Fills made with paper pulp mixed with KG or MC readily
solution (Table 3). deformed under pressure at about 15 kg, and did not suddenly
Dimensional stability fail. In comparison, fills made with microballoon and KG or
The perfect gap filler should not change in dimensions during MC did not compress, but rather resisted compression until a
drying to ensure complete filling of the gap and good adhesion point of failure. Fills made with ParaloidV R B72 did not

on the surface of the wood. From that point of view, none of the compress or fail at the maximum loading point at about 25 kg.
examined materials performed perfectly and all of the applied All samples made with paper pulp: microballoon 1:1 with
gap-filling mixtures shrank upon drying (Figure 5). In most KG were compressed to a maximum of 25 kg without failure.
cases, shrinkage was directly related to the binder/filler ratio; When the load was removed, KG fills remained intact. The
the higher the proportion of binder, the more prominent samples made with paper pulp: microballoon 1:1 with MC
shrinkage was observed, which means that the binder plays an began to crumble or fold when the load was removed, and the
important part in the dimensional stability. The higher the MC fills broke apart.
proportion of binder, the more prominent shrinkage was Fills with microballoon: microcrystalline cellulose 1:3
observed. It was also linked to the type of solvent contained in compressed under a load without disruption and showed no
the binder. signs of damage after removal of loading. Although, the fills
Basically, the samples based on KG or MC (with were permanently compressed to a thickness of 4 mm (from 6
microballoon or with paper pulp) shrunk most significantly, mm).
while those based on KG or ParaloidV R B-72 such as the The MC fills were made with mixture 1 (microcrystalline
mixtures of microballoon: microcrystalline cellulose 1:3 and cellulose: microballoon) crumbled, with a substantial loss of
microballoon: paper pulp 1:1 were the most dimensionally material from the sample KG, was compressed to the
stable. This is in line with the data obtained by Grattan and maximum weight without failure.
Barclay (1988) or Fulcher (2017), who also observed that as ParaloidVR B72 in different samples, with mixture 2
the great majority of the filling mixtures was the solvent, so the (paper pulp: microballoon 1:1), mixture 3 (microballoon:
solvent was a major agent of impact on their behavior upon microcrystalline cellulose 1:3) and mixture 4 (paper pulp)
drying. Owing to the fact that wood powder is more samples, withstood compression force with no apparent effect
hygroscopic than glass microballoons and is more prone to (Figure 6).
change its dimensions at different humidity levels (Skaar, 1984;
Hatchfield, 1986), its greater instability upon drying can be Tensile strength
expected. This kind of observation was reported by Fulcher Averages from tensile strength test showed an increase in the
(2017) for gap fillers based on paper pulp (which is a cellulosic force required to fracture the fill as the strength of the adhesive

Figure 5 Shrinkage of gap fillers after aging of the samples

25

20

15

10

Diameter aer curing (mm) Thickness aer curing (mm)

 Evaluation of wood gap fillers Pigment & Resin Technology
Ebtehal Mahmoud Montaser et al.

Figure 6 Compressive strength (N) of fill materials samples

5000
4500
4000
3500
3000
2500
2000
1500
1000
500
0

Compressive strength

Figure 7 Tensile strength (N) of fill materials samples

400
350
300
Tensile strength

250
200
150
100
50
0

gap fillers

increased. However, the behavior of the filler is affected by both different materials together, the pH values of the gap filler were
the strength of the adhesive and the type of bending agent used. slightly acidic before and after aging, yet it was still within the
As all tested of fillers showed a fragile behavior. Furthermore, range of the pH of the wood sample.
all breaks were within the filler, except for samples KG with In Table 4, the pH values of two different gap-filling
paper pulp: microballoon 1:1 and KG with microballoon: materials before and after aging are presented.
microcrystalline cellulose 1:3, indicating that they are strongly
adhesive (Figure 7). Conclusion
Concerning the MC filler, no measurement could be
obtained, because all the samples were badly fragmented inside The research studied the desirable characteristics of the filler
the silicone mold before the test, which indicates that this filler materials used in the treatment of wood objects as defined in
is more brittle than the other ones, which were mixed with KG the literature may be summarized in a few main points, such as
in paper pulp, and breaks at much less shearing load than the reversibility, workability, lack of shrinkage, ability to take color
other tested fills, but only two measurements were successful and be shaped, stability with aging, compatibility with wood in
with this fill. In the other cases, the failure of the fill occurred terms of behavior with changing humidity and non-toxicity.
before the test, indicating a weakness and stiffness. Also, it is useful to consider their strength properties, or their
KG/microballoon fill shows dispersed results with a high likelihood to deform easily allowing changes in the shape of the
standard deviation. The two fills made of ParaloidV R B72 were

consistently strong with an average failure point at 650 N and

754 N, respectively, for ParaloidV R B72 samples in paper pulp:
Table 4 Measurements of pH in wood and two different gap-filling
microballoon 1:1 and B72 samples with microballoon: samples
microcrystalline cellulose 1:3.
pH value pH value
Determination of the pH value Materials before aging after aging
The pH of gap-filling samples that failed to give good results Wood 4.5 4.8
was not measured in this paper, but the materials that gave Microballoon: paper pulp 1:1
the most suitable results had to be tested to make sure that Mixed with KG 4.6 4.7
they would not cause any future deterioration to the treated Microballoon: microcrystalline
wood. cellulose 1:3
The pH of microballoon is 7.5, pH of microcrystalline Mixed with KG 5 4.8
cellulose is 6.1 and pH of paper pulp is 5.2. After mixing the
 Evaluation of wood gap fillers Pigment & Resin Technology
Ebtehal Mahmoud Montaser et al.

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Further reading
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