FIELD OF THE INVENTION
[0001] This invention relates to a method for coating carrier particles. It relates especially
to a method for coating carrier particles to be used as carrier particles in multi-component
developers for electrostatic imaging with magnetic brush development as well as cascade
development.
BACKGROUND OF THE INVENTION
[0002] There are several methods for coating solid with one or more chemical substances.
For instance, a fluidised bed of carrier particles can be created whereto the coating
solution of a chemical substance in a solvent is then added. Subsequently, the solvent
is evaporated. This is for instance disclosed in "Method of and apparatus for fluidized
bed coating of electrophotographic toner carrier particles", Anonymous, Product Licensing
Index no. 100, August 1 1972, pages 69-71, XP-002147126; and in the German published
patent application DE 3825954 A1; and in United States patent US5,340,677 where a
fluidised bed coater (referred to as the Spiracoater) is used. This method may give
good coating results, but the amount of air required to form the fluidised bed is
such that the evaporated solvent (which in most cases is an organic solvent) contaminates
a large volume of air, which can not without further treatment be vented in the open
atmosphere. Therefore the installations for fluidised bed coating are quite large
and expensive. Moreover, in a fluidised bed the carrier particles are strongly agitated
and many collisions occur which damage the coating around the carrier particles.
[0003] In another method, the carrier particles are mixed (dispersed) in a solution of the
chemical compound or compounds that are to be applied on the surface of the carrier
particles and the particles are then spray-dried. Again this method gives good coating
results, but the installation required for spray drying is expensive. Moreover, in
these prior-art coating methods, based on a fluidised bed or spray drying, frequently
some of the carrier particles to be coated adhere during the coating process to the
wall of container of the fluidised bed or spray drying apparatus, and these particles
are only coated from one side.
[0004] In several documents it is disclosed to bring a solution of coating compounds in
a low temperature boiling solvent in contact with the carrier particles to be coated
in a vessel. Usually the carrier particles in the vessel or subjected to mechanical
agitation, optionally combined with or followed by a step of evaporating the solvent
by heating at a constant elevated temperature. An example thereof is United States
patent 3,507,686, which discloses a method of coating carrier particles, wherein the
carrier particles in the vessel are first subjected simultaneously to pre-heating
at an elevated temperature and oscillatory vibration. The vibration is terminated
and the coating solution is added to the heated carrier particles and thereafter the
oscillatory vibration is reinitiated. Other examples are for instance United States
patent US5,102,769 and European patent application EP0800118 where the coating solution
and the carrier particles are mixed while heating at an elevated constant temperature.
A further example is disclosed in the British patent application GB2014876 where the
coating solution and the carrier particles are agitated by oscillatory vibration while
heating at an unspecified temperature. In some of these disclosures, fairly large
amounts of solvents are used for bringing the coating chemicals on the carrier particles.
This is undesirable as these large amounts of solvents have to be evaporated and,
with respect to environmentally friendly manufacture, recuperated.
[0005] A method using a small amount of solvent for bringing coating chemicals to the carrier
particles has been disclosed in the European patent application EP898206 (or its US
counterpart US5888692). In this disclosure carrier particles are coated by forming
first a loose bed of these carrier particles by mechanical means instead of by an
air flow as in a fluidised bed or spray coater and then continuously adding the coating
solution to that loose bed at such a rate that, at any time, said solvent is present
in an amount lower than 1.25 10
-4 ml per cm
2 of surface of said carrier particles to be coated. During this whole process the
carrier particles are heated to an elevated constant temperature.
[0006] When coating carrier particles for use in electrostatic imaging the coating has to
be very homogenous over the surface of the particles to be coated. In electrostatographic
imaging the carrier particles are mixed with toner particles (and with other ingredients)
to form a developer. When the developer is to be used in magnetic brush development,
the carrier particles are magnetic, when the developer is used in cascade development,
the carrier particles can be coated glass beads. In any case the rubbing of the carrier
particles and the toner particles induces a tribo-electric charge in the toner particles
and the nature of the coating on the carrier particles determines, together with the
toner ingredients, the polarity of the charge on the toner particles as well as the
amount of the charge. When the coating of the surface of the carrier particles is
not even and has interruptions, then problems in charging the toner particles can
occur. Thus in coating carrier particles it is of utmost importance to have an even,
closed coating on the surface of the particles.
[0007] The prior-art methods described may provide coated carrier particles with good properties,
but the homogeneity of the coating, i.e. having the same quality coating on each carrier
particle, leaves still room for improvement.
[0008] Thus, it is still desirable to have a simple, inexpensive, environmentally friendly
method for coating particles with a homogenous surface layer.
OBJECTS AND SUMMARY OF THE INVENTION
[0009] It is an object of the present invention to provide a method for coating carrier
particles with chemical substances that is simple, fast and reliable and that makes
it possible to apply a thin homogenous layer, without interruptions, on the surface
of the particles.
[0010] It is another object of the invention to provide a method enabling the application
of a thin homogeneous coating layer on carrier particles in a vessel by preventing
the carrier particles from sticking to each other as well as sticking to the wall
of the vessel while using limited mechanical agitation in order to prevent damaging
of the coating.
[0011] It is a further object of the invention to provide a method for coating carrier particles
in an environmental friendly way by using low amounts of organic solvent.
[0012] It is still a further object of the invention to provide a method for coating carrier
particles wherein only a low volume of air is contaminated by organic solvents and
wherein said contaminated air can be easily purified.
[0013] The objects of the invention are realised by providing a method for coating carrier
particles having a volume average diameter between 20 and 200 µm, for use in electrostatic
developers, comprising the steps of:
a) forming a coating mixture in a vessel at a temperature from 15 to 40 degrees C
by adding a coating solution comprising B ml of at least one solvent to carrier particles
having a volume of A ml in said vessel, said volume A and said volume B being selected
such that 0.5 ≤ A/B ≤ 5; and
b) evaporating said solvent by mechanically agitating and gradually heating said coating
mixture to a temperature of at most 10 degrees C above the boiling point of the solvent
with the lowest boiling point.
[0014] In a preferred embodiment of the invention, the carrier particles to be coated are
brought in a stationary vessel wherein the mechanical agitation is executed with a
mechanical stirrer.
DETAILED DESCRIPTION OF THE INVENTION
[0015] The method described in EP898206 or in the US-counterpart US5,888,692, necessitates
quite rigorous control of the rate of addition of the coating solution. Although this
control poses no insurmountable problem a method wherein less control of the rate
of addition of the coating solution is necessary remains desirable. The inventors
have now surprisingly found that such a method exists and that a bulk coating process
with low amounts of solvent in the coating solution could be designed. Surprisingly
it was found that such a method could not only dispense with the control of the rate
of addition of the coating solution, but also a very homogenous layer of coating chemicals
could be applied to the carrier particles so that on the particles a layer with very
few or no pinholes at all could be produced.
[0016] According to the method of the present invention, a coating mixture is formed in
a vessel by adding a coating solution comprising B ml of at least one solvent to carrier
particles having a volume of A ml in said vessel, said volume A and said volume B
being selected such that 0.5 ≤ A/B ≤ 5, or 1.5 ≤ A/B ≤ 5, or 2.5 ≤ A/B ≤ 5. While
the volume B is defined as the total amount of solvent(s) of the coating in ml, the
volume A [ml] is defined as the total weight [g] of carrier particles in the vessel
divided by its density [g/cm
3] at 293K. The temperature of the coating mixture in the vessel is about room temperature
to prevent agglomeration of the carrier particles. The temperature may be in the range
from 15 to 40 degrees C or from 20 to 30 degrees C. Preferably no external heat is
applied at this stage. The coating mixture may be mechanically agitated for a predetermined
period, that can be chosen; from about 1 minute to several hours depending on the
properties of the carrier particles and the coating solution where the coating mixture
is composed of. Several embodiments of mechanical agitation are useful in the method
of this invention. In a first preferred embodiment, the coating mixture is agitated
in a stationary vessel by means of a mechanical stirrer. In a second embodiment, no
stirrer is present in the vessel, but the coating mixture is agitated by oscillatory
vibration, e.g. the vessel is mounted on a vibrating table. In a further embodiment
of the invention, the vessel used for implementing the method of this invention, is
a tube, capped on both ends and after filling the tube with carrier particles to be
coated and coating solution, the tube is agitated, e.g., by rolling the tube parallel
to its cylindrical axis.
[0017] Further according to the method of the present invention, the coating mixture in
the vessel, which is optionally already subjected to mechanical agitation, is subjected
to an evaporation process in order to remove the solvent(s), which thereafter can
be recuperated, and to apply a homogeneous layer of the coating substance on the carrier
particles. The solvent(s) are evaporated by mechanically agitating and simultaneously
gradually heating said coating mixture to a temperature of at most 10 degrees C above
the boiling point of the solvent with the lowest boiling point. Preferably the mechanical
agitation is by means of a mechanical stirrer.
[0018] In a preferred embodiment of the invention, the mechanical agitation of the carrier
particles is such that it can be described by a Froude number from 0.02 to 20, or
from 0.05 to 10, or from 0.1 to 5.
[0019] It is found that, contrary to the disclosure in EP898206, the coating can proceed
and yield a good quality coating even when the Froude number is relatively low. The
Froude number is a description of a specific ratio of inertia versus gravity forces,
both forces being of importance in the description of agitation, and is a dimensionless
number defined as:
wherein v represents the velocity of mixing, e.g. circumferential speed of the
outer portion of the mixing blade in m/s, g is the gravitational constant (9.81 m/s
2), and ℓ is a typical dimension of the mixing set-up expressed in m, e.g. radius of
mixing blade. Provided agglomeration of the carrier particles can be prevented, it
is advantageous to have a low Froude number, as a higher Froude number corresponds
with a heavier agitation which may result in damaging of the carrier particles and/or
the coating layer already formed on the carrier particles. It is observed that, despite
the relatively low Froude number and the low amounts of solvent(s), the risk of having
the carrier particles tending to agglomerate is quite low using the method of this
invention. It is believed that this is amongst others because the coating solution
is added to the carrier particles at low temperature, i.e. from 15 to 40 degrees C,
while the solvent(s) in the coating mixture formed is (are) gradually removed by mechanically
agitating and simultaneously gradually heating the coating mixture to a temperature
of at most 10 degrees C above the boiling point of the solvent with the lowest boiling
point. Alternatively the coating mixture may be heated to a temperature of at most
5 degrees above the boiling point of the solvent with the lowest boiling point, or
to a temperature of at most about the boiling point of the solvent with the lowest
boiling point, or to a temperature of at most 10 degrees below the boiling point of
the solvent with the lowest boiling point. The boiling point to be considered is the
boiling point at the pressure at which the coating proceeds. The pressure in the vessel
at which the coating proceeds is selected from 50 % of the atmospheric pressure to
200 % of the atmospheric pressure. Preferably the pressure is about atmospheric pressure.
The gradual heating is preferably such that the temperature is gradually increased
at an average rate in the range from 0.5 to 3 degrees C per minute. Preferably the
heating proceeds at a rate of at most 2 degrees C per minute. The rate of heating
and the time of heating are adapted to the properties, such as for instance boiling
point(s) and vapour tension(s), of the solvent(s) used in the coating solution. The
solvent(s) is (are) thus evaporated and recuperated. The gradual heating of the coating
mixture can beneficially take a time from about 10 minutes to several hours, preferably
the gradual heating proceeds over a time interval from about 30 minutes to two hours.
[0020] Still further according to the method of the present invention, after removal of
the solvent(s) the coated particles can optionally be post-treated in the coating
vessel or in a separate vessel, preferably equipped with heating means and mechanical
agitation means. Such a post-treatment may be desirable to evacuate traces of solvent,
of moisture, etc. The post-treatment may also be desirable to harden the coating.
The post-treatment proceeds at a temperature above 75 degrees C, preferably the post-treatment
temperature is from 75 to 180 degrees C, more preferably from 100 to 150 degrees C.
During post-treatment, the coated particles can be agitated as well as not. Preferably
the agitation is executed intermittently both to avoid agglomeration of the coated
carrier as well as to avoid damaging of the coating layer.
[0021] In a preferred embodiment of this invention, the vessel for implementing the method
of the present invention is equipped with a stirrer of which the blades are essentially
perpendicular (i.e. a deviation of 10 degrees is acceptable) to the bottom of the
vessel. Preferably, the vessel, wherein carrier particles are coated by the method
of this invention, is basically cylindrical and the walls of the cylinder are placed
in a basically horizontal plane and that the shaft of the stirrer is mounted essentially
parallel to the walls of the cylinder and the blades perpendicular to these walls.
A very useful type of mixing apparatus according to the present invention is a ploughshare
mixer. Such a mixer is, e.g., commercially available from Gebrüder Lödige Maschinenbau
GmbH, D33050 Paderborn, Germany. In such a mixer the blades on the shaft of the stirrer
have the shape of a ploughshare. Another interesting embodiment is the use of a vessel,
mounted on a vibrating stage, as sold by Fritsch GmbH, Industriestrasse 8, Idar-Oberstein,
W-Germany.
[0022] Carrier particles coated in a method of the present invention can be used to prepare
multi-component developers for use in electrostatographic methods were an electrostatic
latent image has to be developed, e.g., ionography, electrophotography as well as
in electrostatographic methods were toner particles are directly image-wise applied
to a final image receiving substrate as in Direct Electrostatic Printing, described
in e.g. European patent application EP675417. When the developer is used in cascade
development, the carrier particles can be glass particles that have been coated in
the method according to this invention, when the developer is used in magnetic brush
development, the carrier particles contain magnetic material or are magnetic particles.
The method of this invention can be used to coat composite carriers, which are carriers
wherein a magnetic pigment is incorporated in a matrix, this matrix being e.g. a resin,
glass, etc., as well as carriers composed of pure magnetic material. As magnetic material
as well metal, metaloxides, as any magnetisable material can be used. For instance
metals and metal derivatives of metals can typically be selected from the group of
Ca, Cr, Mn, Fe, Co, Ni, Cu, and Zn or mixtures thereof.
[0023] The method according to the present invention can be used for any type of coating,
it can be used to coat polymers on the particles, when e.g., addition polymers comprising
styrene moieties, acrylic moieties, etc., addition polymers, e.g., polyesters, polyamides,
polyimides etc., polymers comprising fluor containing moieties, silicon containing
polymers, etc., are solved in (a) suitable solvent(s). The method can as well be used
to coat particles with mixtures of polymers. The method of this invention can also
be used to coat reactive mixtures on the particles, e.g. silicone polymers together
with functional organosilanes as disclosed in United States patent US4,977,054.
[0024] The method of this invention is very well suited for coating particles with a solution
comprising chemical compounds that are selected from the group consisting of a monomeric
polyfunctional organosilane, an oligomeric polyfunctional organosilane, a product
of the hydrolysis of a polyfunctional organosilane, a reaction product of a polyfunctional
organosilane and a organosilane containing a hetero-atom, and a reaction product of
polyfunctional organosilane and an alkoxide. These compounds have been disclosed as
carrier coatings in International patent application WO98/53372, International patent
application WO98/52992, and European patent application EP1004942, all of them are
hereby incorporated by reference. When using the method of this invention to coat
carrier particles with e.g. the chemicals as described in WO98/53372, it is possible
to have a pre-reaction take place when using a monomeric polyfunctional organosilane
and an alkoxide in the coating solution, or the solution of the reactants can be added
without any pre-reaction to the carrier particles to be coated. When using the method
to coat carrier particles with the chemicals disclosed in WO98/53372 it is preferred
to use the following chemicals:
polyfunctional organosilanes
[0025] Polyfunctional organosilanes for use in the present invention comprise at least 2,
preferably 3 Si-atoms coupled to 1 to 3 hydrolysable groups and/or a group that can
be cross-linked by polycondensation. The latter groups are preferably alkoxy-, acyloxy
or hydroxygroups. The Si-atoms are preferably coupled by a Si-C bond to an organic
group, e.g., to a linear or branched C1 to C10 alkylgroup, to a C5 to C10 cycloalkylgroup,
to an aromatic group or combinations thereof.
Polyfunctional organosilanes useful to prepare a coating according to this invention
correspond to formula (III), (IV) and (V)
(R
5)
4-iSi[(CH
2)
pSi(OR
6)
a(R
7)
3-a]
i (III)
wherein
i is an integer with value between 2 and 4, preferably i = 2
p is an integer with value between 1 and 4, preferably
2 ≤ p ≤ 4
a is an integer with value between 1 and 3
R5 is an alkyl or aryl group
R6 hydrogen, alkyl or aryl when a = 1
R6 alkyl or aryl when a = 2 or a = 3
R7 alkyl or aryl, preferably methyl.
wherein
m is an integer with value between 3 and 6, preferably m = 3
q is an integer with value between 2 and 10, preferably q =2
b is an integer with value between 1 and 3
R8 is a C1-C6 alkyl or C6-C14 aryl group, preferably CH3, C2H5
R9 hydrogen, alkyl or aryl, preferably H, CH3, C2H5, C3H7 when b = 1
R9 alkyl or aryl, CH3, C2H5, C3H7 when b = 2 or b = 3
R10 alkyl or aryl, preferably methyl.
(R
14)
4-kSi[OSi(R
11)
2(CH
2)
rSi(OR
12)
c(R
13)
3-c]
k (V)
wherein
k is an integer with value between 2 and 4, preferably k = 4
r is an integer with value between 1 and 10, preferably
2 ≤ r ≤ 4
c is an integer with value between 1 and 3
R14 is an alkyl or aryl group
R13 alkyl or aryl, preferably methyl
R12 hydrogen, alkyl or aryl, preferably H, CH3, C2H5, C3H7
when c = 1
R12 alkyl or aryl, CH3, C2H5, C3H7 when c = 2 or c = 3
R11 alkyl or aryl, preferably methyl.
[0026] Typical examples of polyfunctional organo silane useful in this invention are :
Si[(CH
2)
2Si(OH)(CH
3)
2]
4
H
3C Si[(CH
2)
2Si(OH)(CH
3)
2]
3
H
6C
5 Si[(CH
2)
2Si(OH)(CH
3)
2]
3
Si[(CH
2)
3Si(OH)(CH
3)
2]
4
cyclo-{OSiCH
3[(CH
2)
2Si(OH)(CH
3)
2]}
4
cyclo-{OSiCH
3[(CH
2)
2Si(O CH
3)(CH
3)
2]}
4
cyclo-{OSiCH
3[(CH
2)
2Si(O CH
3)
2CH
3]}
4
cyclo-{OSiCH
3[(CH
2)
2Si(O C
2H
5)
2CH
3]}
4
cyclo-{OSiCH
3[(CH
2)
2Si(O C
2H
5)
3]}
4
Organosilanes containing a hetero-atom
[0027] The organosilanes containing an hetero-atom for use in a carrier coating according
to this invention consist of at least one silicon atom carrying an hydrolysable group
and/or a group that can be cross-linked by polycondensation and at least one organic
rest group, bound to the silicon atom by a carbon atom, wherein the rest group contains
an hetero atom and can be an alkyl, cycloalkyl or aryl group. The silicon atom carrying
an hydrolysable group and/or a group that can be cross-linked by polycondensation
can be -SiOR, wherein R can be H, an alkyl, cycloalkyl or aryl group. Preferably H
or an alkyl group or -SiOH. The hetero atoms can be N, P, S, F, Cl, Br, O, B and Al,
but are more preferably N or F.
Very preferred nitrogen containing organosilanes for use in a coating according to
this invention have the formula (I):
(R
2)
2-N[(CH
2)
mNR
2]
n(CH
2)
mSi(OR
3)
3-o(R
4)
o (I)
wherein 1 ≤ m ≤ 10, preferably m = 2 or 3, 0 ≤ n ≤ 2 preferably n = 2, 0 ≤ o ≤ 2,
preferably o = 0, R
2 is hydrogen, alkyl or aryl, preferably hydrogen, R
3, R
4 that are equal or different are alkyl or aryl groups, preferably CH
3 or C
2H
5.
Typical useful nitrogen containing alkoxysilanes are :
H
2N-(CH
2)
3Si(OCH
3)
3
H
2N-(CH
2)
3Si(OC
2H
5)
3
H
2N-(CH
2)
2-HN-(CH
2)
3Si(OCH
3)
3
H
2N-(CH
2)
2-HN-(CH
2)
3Si(OCH
3)
2CH
3
C6H5-HN-(CH
2)
3Si(OCH
3)
3
C6H5-HN-(CH
2)
3Si(OC
2H
5)
3
H
2N-(CH
2)
2-HN-(CH
2)
2-HN-(CH
2)
3Si(OCH
3)
3
H
2N-(CH
2)
2- HN-(CH
2)
2-HN-(CH
2)
3Si(O C
2H
5)
3
[0028] Typical useful fluor containing alkoxysilanes are :
F
3C-(CH
2)
2SiR'
3-x(OR)
x
F
3C-(CF
2)
7-(CH
2)
2SiR'
3-x(OR)
x
(F
3C)
2CF-O-(CH
2)
3SiR'
3-x(OR)
x
(3-F
3C-C
6H
4)-SiR'
3-x(OR)
x
(3-F
3C-C
6H
4)
2-Si(OR)
2
wherein 1 ≤ x ≤ 3, R, R' equal or different are alkyl, cycloalkyl or aryl, preferably
R and R' are either methyl or ethyl.
The alkoxide
[0029] The alkoxide for use in a coating according to this invention corresponds preferably
to formula (II):
M
1(OR
1)
y (II)
Wherein
M1 = Si, Sn, Ti, Zr, B , P or Al
R1 = alkyl or aryl, preferably a C1 to C4 alkyl, more preferably CH3 or C2H5.
y = 4 when M1 = Si, Sn, Ti, Zr, y = 3 when M1 = B , P or Al.
[0030] Preferred alkoxides are : Si(OC
2H
5)
4, B(OC
2H
5)
3, Al(O-i-C
3H
7)
3 and Zr(O-i-C
3H
7)
4. It is highly preferred to use Si(OC
2H
5)
4 as alkoxide in a polycondensation network on the carrier particles of this invention.
[0031] As solvent in the coating solution any low boiling solvent capable of dissolving
the coating chemicals can be used. Since it is preferred in the method of this invention
to use coating chemicals as disclosed in WO98/53372, WO98/52992, and EP1004942, it
is preferred to use lower aliphatic alcohols as solvent.
EXAMPLES
[0032] In every example the coating chemicals are:
- D4-Diëthoxid = (cyclo-{OSiCH3[(CH2)2Si(OC2H5)2(CH3)]}4)
- TEOS (Si(OC2H5)4) and the coating is formed by hydrolysis and condensation of these
reactants on the carrier surface.
COMPARATIVE EXAMPLE 1:
[0033] The components of the coating solution (for coating 1,000 g of Cu-Zn-Ferrite carrier
particles with a density of 5.1 g/cm
3) and the relative amounts both in weight and in volume are given in the table 1 immediately
below.
Table 1
Component |
mass (g) |
volume (ml) |
D4-Diëthoxid |
5.29 |
|
Isopropanol |
2.00 |
2.55 |
TEOS |
5.02 |
|
Water |
1.1 |
1.1 |
Formic acid |
1.0 |
0.82 |
[0034] The solution was pre-reacted at room temperature for one hour under gentle stirring.
Then the solution was further diluted by adding 27.3g of isopropanol, and 0.155g of
a Nitrogen containing charge controller (H
2N-(CH
2)
2- HN-(CH
2)
2-HN-(CH
2)
3Si(OCH
3)
3). From this solution above an amount of 313 g was prepared as final coating solution
for 7,500 g of carrier particles. 7,500g of Cu-Zn-Ferrite carrier particles were stirred
in a vessel and kept at a constant temperature of 80 degrees C. The solution above
was added to the carrier at a rate of 14 g/min over 22 minutes. Then the temperature
of the carrier particles was raised to 140 degrees C for post-treating, particularly
hardening, the coating on the carrier.
INVENTION EXAMPLE 1
[0035] The same composition as given in table 1 was prepared, except for the amount of isopropanol
which now was 113 g per 1000g of carrier particles instead of 29.3 g and no nitrogen
containing charge controller was present. 7,500 g Cu-Zn-Ferrite carrier particles,
i.e. a volume A of 1,470 ml, as used in comparative example 1, were stirred in a vessel
at room temperature (about 25 °C). The coating solution of 941g, comprising a volume
B of 1,080 ml of solvent, was added at once, without any pre-reaction. Under continuous
stirring the carrier particles and coating solution were gradually heated to a temperature
of 80 degrees C over 1 hour thereby slowly evaporating the solvent. After the removal
of the solvent, the coated carrier particles were subjected to a post-treatment wherein
the temperature of the coated carrier particles was raised to 140 °C while stirring
intermittently in order to harden the coating.
INVENTION EXAMPLE 2 (IE2)
[0036] Invention example 2 is executed using the same procedure as in Invention example
1 except for the presence of 0.155g nitrogen containing charge controller added to
the solution after the addition of the isopropanol.
MEASUREMENT OF THE QUALITY OF THE COATING
[0037] Uncoated as well as coated carrier particles, i.e. coated as described in the different
afore-mentioned examples, were measured with XPS (X-ray photoelectron spectroscopy)
to evaluate the amount of metal atoms that reside at the surface. The carrier particles
used were Zn-Cu ferrite particles. The results from XPS, as in Table 2, are a measure
for the quality of the coating, as the lower the amount of metals at the surface,
the better the coating.
Table 2
|
Cu [%] |
Zn [%] |
Fe [%] |
Non-coated carrier core |
1.1 |
1.7 |
16.1 |
Comparative example |
0.1 |
0.3 |
2.6 |
Invention example 1 |
- |
- |
0.2 |
Invention example 2 |
- |
- |
0.2 |
It is clear that the quality of the coating using the method of the invention is
superior to the coating obtained by the prior art coating method. In the comparative
example 16% of the Fe signal of the non-coated carrier core is found at the surface
of the coated carrier while in the invention examples this is only 1.2%.