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1 Introduction 4
4 Test Methods 8
4.1 Flowability 8
4.1.1 Angle of Repose 8
4.1.2 Bed Expansion 8
4.2 Transfer Efficiency 8
4.3 Faraday Cage Effect 8
4.4 Gloss 9
4.5 Gel Time 9
8 Conclusion 15
The global market for powder coatings is expected to AEROSIL® fumed silica is an amorphous silicon dioxide with an
grow at rates higher than liquid coatings due to the ongoing extremely small primary particle size. Hydrolysis of chlorosi-
shift from conventional solvent-borne to more environmental- lanes in an oxygen-hydrogen flame produces this fluffy white
ly-friendly coating systems. The overall growth rate is estimat- powder of high purity. Primary particles in the range of 7 to
ed to be in the range of 5 – 6 % in the years ahead. While North 40 nm result, in a wide range of specific surface areas, from
America and Western Europe should see a more moderate 380 down to 50 m2/g. By using the AEROSIL® process, other
growth, an above average increase in powder coatings produc- special oxides (brand name AEROXIDE®) such as fumed alu-
tion and consumption is expected for South-East-Asia, China, minium oxide, titanium dioxide or zirconium oxide have been
India and Eastern Europe. developed.
In order to remain competitive, it will be essential for powder AEROSIL® and AEROXIDE®
coating manufacturers to develop innovative solutions and • Improve free flow characteristics
systems offering superior performance. Differentiation from • Enhance storage stability
the competition can be achieved by demonstrating proper- • Reduce moisture pick-up
ties such as free flow, transfer efficiency and edge covering. • Improve edge covering
AEROSIL® fumed silica and AEROXIDE® fumed oxides are well • AEROXIDE® Alu C increases the electropositive
known for enhancing and optimizing manufacturing, quality, chargeability of tribo powders
appearance and overall performance of powder coatings.
To considerably improve free flow properties, 0.1 to 0.3 %
A recent study performed between the Evonik Industries AG by weight (on total) of AEROSIL® fumed oxides should be
and the University of Western Ontario, Canada, shows the added to the powder coating. When incorporating AEROSIL®
performance of newly developed fumed oxides in comparison fumed oxides by suitable feeders before the final milling step,
to the established product range of AEROSIL® fumed silica and high homogeneous distribution results throughout the powder
AEROXIDE® fumed oxides. All tests were conducted in a coating can be achieved. Another common incorporation
polyester based coarse powder coating in comparison to a method is the addition of AEROSIL® fumed oxides at the end of
fine powder coating system and we will present the findings the milling process by dry blending (after classification). Using
beginning in Chapter 3. this approach, there is a possibility that larger agglomerates
may remain. Finally, the manufacturer has the option to adjust
the incorporation to suit their specific processes and perfor-
mance requirements.
AEROSIL® 200 and AEROSIL® 380 are hydrophilic fumed AEROSIL® R 972 imparts a slight hydrophobic character to the
silicas which can be added into the hopper at 0.1 - 0.3 % by powder preventing moisture pick-up during storage which
weight (based on total) to improve blending of powders giving can cause caking. AEROSIL® R 972 can be dry blended after
a more homogeneous dry mix ready to be fed into the extrud- pulverization if it is not possible to add prior due to being
er. Processing rheology is improved which allows for faster separated out in the classifiers. The loading levels of
throughput and less hang-up in the extruder. AEROSIL® R 972 are within the same range whether added
before or after pulverization, however, before pulverization
AEROSIL® R 972 is a hydrophobic fumed silica which can be gives the optimum results.
added into the hopper at 0.1 – 0.3 % by weight (based on total)
to improve blending and give a more homogeneous dry mix.
Excessive static charge build-up of powdered raw materials
in the hopper causes fine particle size components to cling to
the walls preventing a homogeneous blend and the feeding of
material into the extruder. AEROSIL® R 972 can also be added
at 0.1 – 0.3 % by weight (based on total) before pulverization
and ground with the powder to reduce static charge, improve
flow of the final product and flow during deposition.
This Technical Information brochure provides information The main objective of the study was to evaluate the effective-
regarding a recent study of performance properties including ness of different fumed silicas and aluminium oxides on the
flow behavior, which can be influenced by fumed silica or performance of powder coatings. All tests have been made in
aluminium oxides in a customary powder coating. Increasing a black polyester based formulation. To get a comprehensive
environmental concerns, combined with the need to contain overview about the performance in powder coatings of
costs and achieve improved appearance properties have different fineness, two particle sizes were chosen
accelerated the trend toward development of thinner powder (fine powder: d50 = 21.5 µm / coarse powder: d50 = 31.0 µm).
coating films. This is being achieved through the use of smaller The additive concentration was set 0.5 % by weight (based on
particle size powder coatings and as a consequence opens the total) for the fine and 0.3 % by weight (based on total) for the
door to using different additives to optimize performance. coarse powder coating. For both fine and coarse particles the
additives were incorporated into the powder coating with AMC
To meet the existing and future requirements of powder coat- milling equipment using proprietary technology of the Uni-
ings, two different particle sizes were included in the study and versity of Western Ontario, Canada. As a general rule, slightly
a variety of performance properties were tested. Specific at- higher loading levels of additive are needed to adequately
tention was paid to ultra fine powders, as good flow and spray cover smaller particle size powders. This is the background of
characteristics are known to be a challenge to achieve. the difference in loading levels, based on powder particle size.
While use of hydrophilic and hydrophobic fumed silica The following tests have been performed with the
(AEROSIL®), and hydrophilic aluminium oxide (AEROXIDE®) polyester powder coatings:
are well known in the powder coatings industry, Evonik has
developed new fumed oxides, which enhance the properties • Angle of Repose (Flowability)
of powders. In cooperation with the University of Western • Bed Expansion (Flowability)
Ontario, Canada, these new particles were tested in compari- • Powder Transfer Efficiency
son to the established product portfolio offered by Evonik • Faraday Cage Effect
for many years. This Technical Information gives an overview • Gloss
about the performance of fumed oxides in a polyester based • Gel Time
powder coating including both, coarse and fine powders.
All products included in this study are listed in Table 2 with
their respective physical properties.
m1 m2 m3
E1+ E 2 + E 3 + +
4.1.2 Bed Expansion 3.0 3.0 3.0
Transfer Efficiency E = =
Bed expansion ratio (BER) is another commonly used param- 3 3
eter in determining the flowability of a powder. BER is defined
as the ratio of fluidized bed height H over the initial fixed bed
height H 0 , which changes with the air velocity passing through where m1, m 2 and m 3 were the powder mass transferred to the
the bed. A higher expansion ratio suggests improved powder target panel.
performance, fluidization ability and flowability.
4.3 Faraday Cage Effect
Faraday Cage Effect tests were conducted with a specially
designed aluminium panel of 7“ x 6“ with a 1“ deep x 1“ wide
trough located in the centre, as shown in the the picture below.
Aluminium sheets
Aluminium panels
and fixed strips after
spraying
Then the whole panel was hung in the spray booth with ground- All samples for the tests of fumed silica and fumed aluminium
ing connection. Each of the 3 strips was weighed before and after oxides were prepared as described in chapter 3. The proce-
each spray to get the mass of powder deposited. By comparing the dure for fluidization tests, transfer efficiency, Faraday Cage
powder mass on the back wall inside the trough (minternal) with Effect, gloss and gel time were done according to chapter 4.
the average powder mass on the 2 strips outside of the trough
(mouter) with
5.1 Flowability
mouter (top) + mouter (bottom)
mouter = , 5.1.1 Angle of Repose Test
2 In coarse as well as in fine polyester powder coatings,
AEROXIDE® Alu C 805 showed the highest positive impact
the Faraday Cage Effect can be determined by the ratio of on the flow characteristics among the tested fumed
these two mass numbers: aluminium oxides. The second best performing product was
AEROXIDE® Alu 130 for both particle sizes (Figure 1 and 2).
minternal
R=
mouter
Figure 1 Angle of Repose of aluminium oxides in a
coarse powder coating
with R = 1 denoting no Faraday Cage Effect and R = 0
representing a maximum Faraday Cage Effect and no 50
45
40
35
4.4 Gloss
30
The evaluation of the gloss values for the different samples
25
of coarse and fine polyester powder was performed with the
Novo-Gloss Gloss meter manufactured by Rohpoint Instru- 20
Control AEROXIDE® AEROXIDE® AEROXIDE®
mentation Ltd. According to the manufacturer, the assigned Alu C Alu C 805 Alu 130
test are 20 ˚ and 60 ˚, these values are widely used in industry
as a standard for gloss measurements. Each individual panel
was measured six times at different points to calculate the Figure 2 Angle of Repose of aluminium oxides in a
fine powder coating
average gloss value.
50
Angle of Repose*
45
4.5 Gel Time
The ASTM standard test method (D 4217-02) for gel time of a
40
45
Figure 5 Bed Expansion test with silica and aluminium oxides in the
Figure 4 Angle of Repose of silicas in a fine powder coating fine powder coating
50 0.5
Worse
Angle of Repose*
45
Air Velocity U [cm/s]
0.4
40
0.3
35
0.2
30
0.1
25
Better
20 0
Control AEROSIL® AEROSIL® AEROSIL® AEROXIDE® AEROXIDE® AEROXIDE® AEROSIL® AEROSIL® AEROSIL®
R 812 200 R 972 Alu C 805 Alu C Alu 130 R 812 200 R 972
0.4
0.2
0.1
Better
0
AEROSIL® AEROXIDE® AEROXIDE® AEROSIL® AEROSIL® AEROXIDE®
R 812 Alu C 805 Alu 130 200 R 972 Alu C
10
Transfer
5.2 Transfer Efficiency
Efficiency [%] 80 78 75 65
To evaluate the transfer efficiency with the corona process, a
GEMA spray gun with a target panel of 30 cm diameter and
20 cm distance between panel and gun was used. 3 g of pow-
der coating were sprayed to cover the disks. The higher the
coverage of the disks after spraying, the more powder coating
was transferred. The drying time was ten minutes at 200 °C. 5.3 Faraday Cage Effect
For the tests of the Faraday Cage Effect the powder coatings
It was evident that the results for the transfer efficiency were sprayed with the GEMA spray gun onto the panels. The
are very much dependent on the particle size of the powder final evaluation of the covering effect was evaluated as out-
coating. Additives which enhanced the transfer efficiency for lined in chapter 4.3. A maximum Faraday Cage Effect provides
fine powders tended to reduce the transfer efficiency of the bad coverage and that corresponds to a low “R” value. R = 1
coarse powder coating. In fine powders AEROSIL® 200 and represents no Faraday Cage Effect and a uniform coverage
AEROSIL® R 812 performed best (Table 3) while in coarse over the entire substrate.
powders AEROXIDE® Alu 130 and AEROXIDE® Alu C gave
favourable results (Table 4). In fine powder materials, silica additives help to overcome the
Faraday Cage Effect and achieve a more uniform coverage of
the substrate results show AEROSIL® R 812 clearly improves
this performance attribute.
0.75
Better
0.72
0.69
R
0.66
0.63
Worse
0.60
AEROSIL® AEROSIL® AEROSIL® Control
R 812 200 R 972
11
In coarse powder materials, only AEROXIDE® Alu C 805 In addition to the improvement of the flow properties, fumed
improved the coverage slightly. All other tested silica and aluminium oxide is often used to improve the chargeability of
aluminium oxides did not provide noticeable benefits for the powders for the tribo application. For this reason, the influence
Faraday Cage Effect. of different aluminium oxide additives on the transfer efficiency
and the Faraday Cage Effect was evaluated separately.
5.4 Gloss
Gloss reductions were observed from the addition of each of 6.1 Transfer Efficiency
the silica additives, for both incident angles (20° and 60°) The transfer efficiency was again performed as outlined in
and for both coarse and fine powders. AEROSIL® R 972 pro- chapter 4.2. For the tests of different aluminium oxides a tribo
vided less influence on the gloss compared to all other tested application with a Nordson Tribomatic 631302C manual spray
fumed silicas. gun was used.
The test results indicate that generally silica additives have All tested aluminium oxides improved the transfer efficiency of
a greater impact to gloss than the aluminium oxide additi-ves. the polyester material. While for the corona application the re-
Excellent performance was demonstrated by sults are very much dependent on the particle size of the pow-
AEROXIDE® Alu C 805, which did not influence the der coating (see chapter 5.2), AEROXIDE® Alu C 805 showed
gloss of the powder coatings panels. a superior improvement of the transfer efficiency in the tribo
application, independent of the powder coating particle size.
60
55
50
Control AEROXIDE® AEROXIDE® AEROXIDE®
Alu C 805 Alu C Alu 130
80
Transfer Efficiency E [%]
75
70
65
60
55
50
Control AEROXIDE® AEROXIDE® AEROXIDE®
Alu C 805 Alu C Alu 130
12
1.0
Better
0.8
0.6
R
0.4
0.2
Worse
0.0
Control AEROXIDE® AEROXIDE® AEROXIDE®
Alu C 805 Alu C Alu 130
13
AEROSIL® AEROXIDE®
Testmethod Unit 200 380 R 972 R 812 R 8200 Alu 130 Alu C Alu C 805
Specific surface area (BET) m2/g 200 ± 25 380 ± 30 110 ± 20 260 ± 30 160 ± 25 130 ± 20 110 ± 15 90 ± 15
Tapped density
(approx. value ex plant)
acc. to DIN EN ISO 787/XI, Aug. 1983 g/l 50 50 50 60 140 50 50 50
Moisture
(ex plant) 2 hours at 105 °C wt. % ≤ 1.5 ≤ 2.0 ≤ 0.5 ≤ 0.5 ≤ 0.5 ≤ 5.0 ≤ 5.0 ≤ 2.0
pH-value
in 4 % dispersion 3.7 – 4.7 3.7 – 4.7 3.6 – 4.4* 5.5 – 7.5 ≥ 5.0 4.4 – 5.4 4.5 – 5.5 3.0 – 4.5
Carbon content wt. % – – 0.6 – 1.2 2.0 – 3.0 2.0 – 4.0 – – 3.5 – 4.5
SiO2 -content
based on ignited material wt. % ≥ 99.8 ≥ 99.8 ≥ 99.8 ≥ 99.8 ≥ 99.8 ≤ 0.10 ≤ 0.10 ≤ 0.10
Al2O3 -content
based on ignited material wt. % ≤ 0.05 ≤ 0.05 ≤ 0.05 ≤ 0.05 ≤ 0.05 ≥ 99.8 ≥ 99.8 ≥ 95.0
14
15
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