TUBALL™ MATRIX
Dilution Guidelines
TUBALL™ MATRIX 201, 202, 203, 301
1
CONTENTS
1.
Dilution Equipment ........................................................................................................ 3
2.
Dilution Principles .......................................................................................................... 4
3.
Dilution Procedure ......................................................................................................... 5
3.1. TUBALL™ MATRIX 201/203/301 (epoxy and polyester resins) .................................... 5
3.2. TUBALL™ MATRIX 201/202/203/301 (polyurethane resins)......................................... 6
3.3. TUBALL™ MATRIX 202 (polyvinyl chloride resins) ....................................................... 7
4.
Viscosity Management................................................................................................... 8
5.
Quality Control ............................................................................................................... 9
6.
Application Examples .................................................................................................. 11
6.1. TUBALL™ MATRIX 201 for epoxy resin...................................................................... 11
6.2. TUBALL™ MATRIX 202 for polyvinyl chloride resin .................................................... 12
6.3. TUBALL™ MATRIX 203 for epoxy resin (solvent-borne)............................................. 13
6.4. TUBALL™ MATRIX 301 for polyurethane resin .......................................................... 14
7.
Troubleshooting ........................................................................................................... 15
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1. Dilution Equipment
For laboratory tests: a mechanical overhead stirrer with a mixing speed up to 2000 rpm (such
as the Heidolph RZR series or the IKA EUROSTAR series).
For industrial production: dissolvers similar to the DISPERMAT CA series.
Dilution should be conducted in a cylindrical mixing container with a flat bottom. An example
of a dissolver for industrial production is shown in Figure 1. The recommended impeller blade
shape for maximum effectiveness is shown in Figure 2.
Figure 1. Example of a dissolver
Figure 2. Recommended impeller blade
shape
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2. Dilution Principles
 The target dosage of TUBALL™ MATRIX refers to the loading in the whole final
formulation. For example, if the system consists of 50% resin and 50% fibre, and the
required level of volume resistivity is 106 Ω·cm, the target TUBALL™ MATRIX dosage
should be 0.5 wt.% for the whole system and 1.0 wt.% for the resin.

The temperature, time and mixing speed may need to be adapted to obtain a final mixture
that is homogeneous.
 During the dilution process, check the impeller blade, walls and bottom of the container for
stuck masses of TUBALL™ MATRIX (for more information, refer to Section 5).
 For best results, add the curing agents and polymerise the compound with TUBALL™
MATRIX as soon as possible after diluting the TUBALL™ MATRIX. When dispersed in a
thermoset compound, single wall carbon nanotubes tend to agglomerate.
 The shelf life of the final compound in the liquid state must be determined experimentally
for each particular compound.
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3. Dilution Procedure
Uniform distribution of TUBALL™ MATRIX in the resin plays a key role in enhancing the
electrical conductivity of the final compound. In order to obtain a high-quality TUBALL™
MATRIX dispersion, OCSiAl recommends that close attention be paid to the dilution
procedure.
3.1. TUBALL™ MATRIX 201/203/301 (epoxy and polyester resins)
Achieving the highest quality of TUBALL™ MATRIX dispersion in the final compound requires
a two-stage dilution procedure, with the first dilution stage being under high shear of the
concentrate in a liquid ingredient of the final formulation to achieve a homogeneous mixture.
The second stage is mixing of the resulting mixture with the other components of the final
formulation.
First stage:
- take 2–5 wt.% of TUBALL™ MATRIX + 95–98% of the base resin (epoxy or polyester
component),
- mix at 1500–2000 rpm (depending on type of resin) for 20-40 minutes until the dispersion
quality reaches that shown in Figure 6 (Section 5).
Note: for more viscous resins, the dilution dosage for the first stage should be closer to
2 wt.% of TUBALL™ MATRIX and, for less viscous resins, it should be closer to 5 wt.%.
Second stage:
- add the base resin to the mixture from the first stage to further dilute the TUBALL™
MATRIX to the target dosage in the final formulation, which should be determined against
the percolation curve (which can be found in the relevant Technical Data Sheet),
- mix at 1500–2000 rpm (depending on type of resin) for 20-40 minutes until the dispersion
quality reaches that shown in Figure 6 (Section 5),
- mix at 100 rpm for at least 5 minutes (defoaming step),
- add the other relevant components of the formulation (if necessary) according to the
following sequence:
1. white pigment (TiO2 or others),
2. colour pigment,
3. deaerating agent and antifoaming agent,
4. viscosity-regulating additives,
5. curing agent.
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Note: After adding each component, it is necessary to mix the system until it is homogeneous.
OCSiAl also recommends that the mixture be left to stand for a period of time before adding a
curing agent. This will help the rest of the air bubbles to leave the mixture.
3.2. TUBALL™ MATRIX 201/202/203/301 (polyurethane resins)
Achieving the highest quality of TUBALL™ MATRIX dispersion in the final compound requires
a two-stage dilution procedure, with the first dilution stage being under high shear of the
concentrate in a liquid ingredient of the final formulation to achieve a homogeneous mixture.
The second stage is mixing of the resulting mixture with the other components of the final
formulation.
First stage:
- take polyol,
- add the other relevant components of the formulation (if necessary) according to the
following sequence:
1. deaerating agent,
2. dehydrating minerals,
3. mineral fillers,
4. white pigment (TiO2 or others),
Note: After adding each component, it is necessary to mix the system until it is homogeneous.
- add TUBALL™ MATRIX, stir at 1000 rpm for 20 minutes;
- add the other relevant components of the formulation (if necessary) according to the
following sequence: deaerating agent,
1. dispersing agents,
2. pigment paste,
Note: After adding each component, it is necessary to mix the system until it is homogeneous.
- mix at 10 rpm for 15 minutes (defoaming step),
- leave a mixture to stand for 30 minutes,
- add isocyanate, mix the system until it is homogeneous.
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3.3. TUBALL™ MATRIX 202 (polyvinyl chloride resins)
The highest quality of TUBALL™ MATRIX dispersion in polyvinyl chloride resin can be
achieved with a one-stage procedure.
Procedure:
- take the total volume of plasticizer in the final formulation + the TUBALL™ MATRIX volume
required to get the target dosage in the final formulation, which should be determined
against the percolation curve (which can be found in the relevant Technical Data Sheet),
- mix at 1500–2000 rpm (depending on type of resin) for 20-40 minutes until the dispersion
quality reaches that shown in Figure 6 (Section 5),
- add the other components of the formulation (if necessary) according to the following
sequence:
1. white pigment (TiO2 or others),
2. colour pigment,
Note: After adding each component, it is necessary to mix the system until it is homogeneous.
- add polyvinyl chloride resin, mix the system until it is homogeneous.
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4. Viscosity Management
TUBALL™ single wall carbon nanotubes, even in small quantities, lead to increased viscosity
of the formulation. Figure 3 shows the typical increase in viscosity resulting from the
application of TUBALL™ MATRIX concentrate.
Figure 3. Typical viscosity rate with TUBALL™ MATRIX
35000
30000
Viscosity, cP
25000
20000
15000
10000
5000
0
0,0
0,5
1,0
1,5
2,0
2,5
3,0
3,5
4,0
TUBALL™ MATRIX, wt.%
* Brookfield viscosity measured at 25°С, spindle SC4-6, 20 rpm.
Tested in D.E.R. 351 epoxy resin. Measurements conducted according to AS D2983 standard.
Methods for reducing viscosity:
 reduce thixotropic and thickening agents,
 add viscosity-regulating additives (solvent, plasticizer or reactive diluent),
 heat the mixture if allowed (up to 40°C).
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5. Quality Control
Quality control should be conducted after each dilution stage.
The quickest and easiest method of examining the dilution quality is to take tip samples with a
glass or plastic stick and then to flatten the sample into a thin layer on a white sheet of paper
(Figure 4). If non-uniformities are present (Figure 5), continue stirring until another sample
shows that complete dissolution has been achieved (Figure 6).
Figure 4. Quality control procedure.
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Figure 5. “Bad” quality dispersion (many large particles of TUBALL™ MATRIX).
Figure 6. “Good” quality dispersion (homogeneous mixture).
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6. Application Examples
This section presents three examples of exact recipes of TUBALL™ MATRIX applications. In
general, the composition of the final compound and the dilution procedure can be changed
according to the specific application.
6.1. TUBALL™ MATRIX 201 for epoxy resin
 Desired level of conductivity is 106 Ω·cm,
 Composition of final compound (1 kg):
 73.9% of D.E.R. 351 epoxy resin (739 g),
 25.1% of Epikure 960 curing agent (251 g),
 0.5% of Tego Airex 922 deaerating agent (5 g),
 0.5% of TUBALL™ MATRIX 201 (5 g) – the dosage was determined against the
percolation curve from the Technical Data Sheet.
First stage:
 mix 5 g of TUBALL™ MATRIX 201 (5%) + 95 g of epoxy resin (95%) at 1500 rpm for 20
minutes at room temperature until the dispersion quality reaches that shown in Figure 6
(Section 5).
Second stage:
 add the remaining 644 g of epoxy resin to the mixture to further dilute the TUBALL™
MATRIX 201,
 mix at 1500 rpm for 20 minutes at room temperature until the dispersion quality reaches
that shown in Figure 6 (Section 5),
 add 5 g of deaerating agent, mix the system until it is homogeneous,
 mix at 100 rpm for 5 minutes at room temperature (defoaming step),
 add 251 g of the curing agent,
 mix the system until it is homogeneous.
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6.2. TUBALL™ MATRIX 202 for polyvinyl chloride resin
 Desired level of conductivity is 104 Ω·cm,
 Composition of final compound (1 kg):
 57.8% of PVC resin (578 g),
 31.2% of Hexamoll Dinch plasticizer (312 g),
 10% of colour pigment (100 g),
 1% of TUBALL™ MATRIX 202 (10 g) – the dosage was determined against the
percolation curve from the Technical Data Sheet.
Procedure:
 mix 10 g of TUBALL™ MATRIX 202 + 312 g of plasticizer at 1500 rpm for 20-40 minutes at
room temperature until the dispersion quality reaches that shown in Figure 6 (Section 5),
 add 10 g of colour pigment,
 mix the system until it is homogeneous,
 add 578 g of curing PVC resin,
 mix the system until it is homogeneous.
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6.3. TUBALL™ MATRIX 203 for epoxy resin (solvent-borne)
 Desired level of conductivity is 106-108 Ω
 Composition of final compound (1 kg):
 41.6% of D.E.R. 351 epoxy resin (416 g),
 40.0% of Toluene solvent (400 g),
 17.8% of Epikure F 205 curing agent (178 g),
 0.5% of BYK-555 deaerating agent (5 g),
 0.1% of TUBALL™ MATRIX 203 (1 g) – the dosage was determined against the
percolation curve from the Technical Data Sheet.
First stage:
 mix 1 g of TUBALL™ MATRIX 203 (5%) + 49 g of epoxy resin (95%) at 1500 rpm for 20
minutes at room temperature until the dispersion quality reaches that shown in Figure 6
(Section 5).
Second stage:
 add the remaining 367 g of epoxy resin to the mixture to further dilute the TUBALL™
MATRIX 203,
 mix at 1500 rpm for 20 minutes at room temperature until the dispersion quality reaches
that shown in Figure 6 (Section 5),
 add 400 g of solvent + 5 g of deaerating agent,
 mix at 1000 rpm for 10 minutes at room temperature until it is homogeneous,
 leave the mixture to stand for 10-15 minutes,
 add 178 g of curing agent,
 mix the system until it is homogeneous.
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6.4. TUBALL™ MATRIX 301 for polyurethane resin
 Desired level of conductivity is 106-108 Ω·cm,
 Composition of final compound (1 kg):
 42.4% of polyol CAPA 4101/Castor oil FSG (424 g),
 23.5% of isocyanate MDI (235 g),
 11.8% of mineral filler Hydrophobic CaCO3 5-20 µm (118 g),
 9.4% of dehydrating mineral 40% zeolite paste in castor oil (94 g),
 9.4% of white pigment Crystal TiO2 (94 g),
 1.0% of dispersing agent BYK-9076 (10 g),
 1.0% of pigment paste Polipigment Helio green (10 g)
 0.5% of TUBALL™ MATRIX 301 (5 g) – the dosage was determined against the
percolation curve from the Technical Data Sheet.
Dilution procedure:
 Mix 424 g of polyol and 10 g of deaerating agent at 200 rpm for 5 minutes;
 Add 94 g of dehydrating mineral and stir at 400 rpm for 5 min;
 Add 118 g of mineral filler and 94 g of white pigment and stir at 400 rpm for 15 minutes;
 Add 5 g of TUBALL™ MATRIX 301 and stir at 1000 rpm for 20 minutes;
 Add 10 g of dispersing agent and stir at 400 rpm for 15 minutes;
 Add 10 g of pigment paste and stir at 400 rpm for 10 minutes;
 Apply coating on a substrate by brush or roller;
 Apply deaerating step by mixing at 10 rpm for 15 min and leave a mixture to stand for 30
minutes;
 Add 235 g of isocyanate, mix the system until it is homogeneous.
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7. Troubleshooting
Problem
Possible solution
add reactive diluent
add solvent
High level of viscosity
heat the mixture if allowed (up to 40°C)
reduce amount of thixotropic and thickening agents
use impeller blade for high-viscosity mixing
Unsatisfactory dilution
(large particles of
TUBALL™ MATRIX
remaining)
increase mixing time
increase temperature of mixing
increase rotation speed
add deaerating agent
increase time of defoaming step
Many bubbles
apply vacuum degassing procedure
use deaerating impeller such as Visco Jet
add antifoaming agent
Foaming
increase time of defoaming step
apply vacuum degassing procedure
add reactive diluent or solvent
Poor self-levelling in
flooring applications
add levelling agents
remove thixotropic and thickening agents from
Colour too dark
add white pigment (such as TiO2, etc.)
Appearance of white
pigment on the surface
add dispersing agent for white pigment
(e.x. DispeBYK-110 for TiO2)
Sticking material on
impeller blade
clean out the mixing box
mix for up to an additional 15 minutes
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