Title: Modification of surfaces in order to increase the surface tension
Abstract: A process is provided for the production of a surface coating as well as the use of surface coatings to increase the surface tension of objects. The surface coating is obtained by depositing a layer of at least one element that can be oxidized with water or an alloy that can be oxidized with water. Subsequently, the deposited layer is subjected to boiling water or water vapor. The element is generally derived from the following group of elements: Al, Si, Ti, V, Cr, Mn, Fe, Co, Ni, Zn, Ga, Ge, Zr, Nb, Cd, In, Sn, Sb.
Patent Number: 7,025,836 Issued on 04/11/2006 to Zimmer, et al.
| Inventors:
|
Zimmer; Volker (Dossenheim, DE);
Braun; Hans-Peter (Weinheim, DE)
|
| Assignee:
|
Roche Diagnostics GmbH (Mannheim, DE)
|
| Appl. No.:
|
555618 |
| Filed:
|
January 23, 2001 |
| PCT Filed:
|
January 23, 2001
|
| PCT NO:
|
PCT/EP98/07851
|
| 371 Date:
|
January 5, 2001
|
| 102(e) Date:
|
January 5, 2001
|
| PCT PUB.NO.:
|
WO99/29435 |
| PCT PUB. Date:
|
June 17, 1999 |
Foreign Application Priority Data
| Dec 04, 1997[DE] | 197 53 848 |
| Current U.S. Class: |
148/277; 73/64.48; 73/64.52 |
| Current Intern'l Class: |
C23C 8/16 (20060101) |
| Field of Search: |
148/277
73/644.8,645.2
|
References Cited [Referenced By]
U.S. Patent Documents
| 3255035 | Jun., 1966 | Clough et al.
| |
| 3730783 | May., 1973 | Streel.
| |
| 3926564 | Dec., 1975 | Giaever.
| |
| 4722906 | Feb., 1988 | Guire.
| |
| 4759805 | Jul., 1988 | Saruwatari et al.
| |
| 4973493 | Nov., 1990 | Guire.
| |
| 4979959 | Dec., 1990 | Guire.
| |
| 5002582 | Mar., 1991 | Guire et al.
| |
| 5414075 | May., 1995 | Swan et al.
| |
| Foreign Patent Documents |
| A 0 045 416 | Feb., 1982 | EP.
| |
| 1373816 | Jun., 1966 | FR.
| |
| 2100817 | May., 1973 | FR.
| |
| A 895879 | May., 1962 | GB.
| |
| A 1084696 | Sep., 1967 | GB.
| |
| A 2075556 | Nov., 1981 | GB.
| |
Other References
The Making, Shaping and Treating of Steel, Edited by Harold E. McGannon, United
States Steel, eighth edition, 1964, pp. 317-318, 1964.
AN 15: 237352 , Protective oxide coating on alumium and magnesium alloys, Res.
Discl. (1991), 330, 798, 1991.
Ikawa et al., Comparison of a New Microcrystalline Aluminum Oxide Hydroxide and
Amorphous Aluminum Hydroxide for Binding to Phosphate, Proteins, Neucleotides,
Lipids and Carbohydrates, Chem. Pharm. Bull. 41(6) 1055-1059 (1993).
|
Primary Examiner: Ip; Sikyin
Attorney, Agent or Firm: Woodburn; Jill L., Sage; Justin, Knauer; Richard
Claims
The invention claimed is:
1. Method of increasing the surface tension of at least one solid object, the
method comprising the steps of: providing at least a portion of an analytical test
element that is formed to transport a sample liquid from a sample application site
to a determination site, the test element including a polyester foil having a surface
of an element that can be oxidized with water or an alloy that can be oxidized
with water that defines the at least one solid object having a surface,
depositing a layer of at least one element that can be oxidized with water or
an alloy that can be oxidized with water on the surface of the polyester foil that
defines the solid object to form a deposited layer, and
subsequently applying boiling water or water vapour on the deposited layer, whereby
the resulting deposited layer is solid and more hydrophilic than the surface of
the polyester foil that defines the solid object.
2. Method of claim 1, wherein the element is derived from at least one element
selected from the group consisting of Al, Si, Ti, V, Cr Mn, Fe, Co, Ni, Zn, Ga,
Ge, Zr, Nb, Cd, In, Sn, Sb.
3. Method of claim 2, wherein the element is derived from at least one element
selected from the group consisting of Al, Si, Ti, Zr.
4. Method of claim 3, wherein the element is Al.
5. Method of claim 1, wherein the alloy contains at least two components selected
from the group of elements consisting of Al, Si, Ti, V, Cr, Mn, Fr, Co, Ni, Zn,
Ga, Ge, Zr, Nb, Cd, In, Sn, Sb.
6. Method of claim 1, wherein the alloy contains at least one component selected
from a first group of elements consisting of Al, Si, Ti, V, Cr, Mn, Fe, Co, Ni,
Zn, Ga, Ge, Zr, Nb, Cd, In, Sn, Sb, which are alloyed with at least one element
selected from a second group of elements consisting of Mg, Ca, Sr, Ba.
7. Method of claim 6, wherein the alloy contains at least one component selected
from a first group consisting of Al, Si, Ti, Zr, which is alloyed with at least
one element selected from a second group consisting of Mg, Ca, Sr, Ba.
8. Method of claim 7, wherein the alloy is composed of Al which is alloyed with
at least one element selected from the group consisting of Mg, Ca, Sr, Ba.
9. Method of claim 1, wherein the deposited layer has a thickness between 1 nm
and 500 nm.
10. Method of claim 1, wherein the oxide layer has a thickness between 0.1 nm
and 500 nm.
11. Method of claim 10, wherein the oxide layer has a thickness between 10 nm
and 100 nm.
12. Method of claim 2, wherein the deposited layer has a thickness between 1
nm and 500 nm.
13. Method of claim 2, wherein the oxide layer has a thickness between 0.1 nm
and 500 nm.
14. Method of claim 5, wherein the deposited layer has a thickness between 1
nm and 500 nm.
15. Method of claim 5, wherein the oxide layer has a thickness between 0.1 nm
and 500 nm.
16. Method of claim 6, wherein the deposited layer has a thickness between 1
nm and 500 nm.
17. Method of claim 6, wherein the oxide layer has a thickness between 0.1 nm
and 500 nm.
18. Method of increasing the surface tension of at least one solid object, the
method comprising the steps of:
providing at least a portion of an analytical test element that is formed to
transport a sample liquid from a sample application site to a determination site,
the test element including a polyester foil having a surface of an element that
can be oxidized with water or an alloy that can be oxidized with water that defines
the at least one solid object having a surface,
depositing on the surface of the polyester foil a layer of at least one element
that can be oxidized with water or an alloy that can be oxidized with water and
subsequently applying superheated water vapour to the deposited layer, whereby
the resulting deposited layer is solid and more hydrophilic than the surface of
the polyester foil the defines the solid object.
19. Method of claim 18, wherein the element is derived from the elements selected
from the group consisting of Al, Si, Ti, V, Cr, Mn, Fe, Co, Ni, Zn, Ga, Ge, Zr,
Nb, Cd, In, Sn, Sb.
20. Method of claim 18, wherein the alloy contains at least two components selected
from elements in the group consisting of Al, Si, Ti, V, Cr, Mn, Fe, Co, Ni, Zn,
Ga, Ge, Zr, Nb, Cd, In, Sn, Sb.
21. Method of claim 18, wherein the alloy contains at least one component selected
from a first group consisting of Al, Si, Ti, V, Cr, Mn, Fe, Co, Ni, Zn, Ga, Ge,
Zr, Nb, Cd, In, Sn, Sb.
22. Method of claim 18, wherein the deposited layer has a thickness between 1
nm and 500 nm.
23. Method of claim 18, wherein the oxide layer has a thickness between 0.1 nm
and 500 nm.
Description
BACKGROUND AND SUMMARY OF THE INVENTION
The invention concerns a process for the production of surface coatings as well
as the use of a surface coating to increase the surface tension of objects.
The coating of surfaces of solid objects is a widely used means of specifically
changing the surface properties of objects. Here reference is only made to the
countless methods of corrosion protection for everyday objects made of base metals
or the painting of objects with the aim of changing their optical appearance.
Coating is usually understood as a manufacturing process for applying a firmly
adhering layer of a shapeless material to a work piece or a supporting sheet. One
can in principle distinguish between four groups of coating processes which each
differ by the state of the coating material before coating:
- 1. Coating from a gaseous or vaporous state such as evaporation coating
or metallizing;
- 2. Coating from a liquid, pulpy or paste-like state such as painting,
dispersion or hot-melt coating;
- 3. Coating from an ionized state by electrolytic or chemical depositing
such as among others the eloxal process or electrophoretic painting.
- 4. Coating from a solid i.e. granular or powder state such as powder
coating or coating by sintering.
Plastics have turned out to be the production material of choice for fields
of application in which cheap single-use articles are used especially in medical
diagnostics or environmental analysis. Since plastics and in particular cheap,
easy-to-process commodity plastics that can be almost shaped at will, are usually
composed of non-polar organic polymers, most of them cannot be wetted or only poorly
wetted by polar media such as water and aqueous liquids, in particular biological
samples. This property is utilized for certain applications especially where adherence
of the liquid to the plastic object is not desired such as for disposable pipette
tips. On the other hand there are numerous fields of applications for plastic objects
in which a wettability with polar liquids is desired such as for example in the
field of rapid diagnostics in which plastics can serve as materials for taking
up biological sample liquids.
There is therefore no lack of different processes which have the aim of hydrophilically
modifying plastic surfaces. Hydrophilic surfaces are characterized by a high surface
tension which have a value near to the value of the surface tension of water (72
mN/m). Examples of a hydrophilic modification of plastic surfaces are corona plasma
treatment, plasma chemical vapour deposition (PACVD, e.g. Antec Co. Kelkheim),
the covalent binding of hydrophilic polymers with a photoreactive capability onto
a plastic surface described for example in U.S. Pat. No. 4,973,493 (Photo Link
Surface, BSI Corporation Co., Eden Prairie, Minn., USA), the application of layers
containing wetting agents onto a plastic surface (for example Adhesive Research
Co., Glen Rock, Pa., USA) or coating of inorganic-organic nanocomposites by means
of sol-gel technology on the surfaces to be modified (for example INM, Co. Saarbrücken).
The processes mentioned above which each have advantages and disadvantages have
been able to establish themselves for the hydrophilic modification of plastic surfaces
whether of foils or formed pieces.
The corona plasma treatment leads to an increase in the surface tension which
continuously decreases after the treatment over a short period of several days
up to a few weeks. Moreover the surface tensions that can be achieved are relatively low.
Slightly higher surface tensions than those of the corona plasma treatment
can be achieved with the PACVD technology. Although this method leads to surface
coatings that are more stable over time, a decrease of the surface tension with
time is still observed in this case.
Surfaces which are furnished with so-called photo link surfaces or which
have been coated with layers containing wetting agents have a surface tension which
is stable over time. However, both variants do not lead to optimally high surface
tensions. An additional fundamental disadvantage of coating with layers containing
wetting agents is that the wetting agents accumulate in a liquid aqueous sample
that is contacted with the layer and can thus change it or make it unusable.
Coating of inorganic-organic nanocomposites by means of sol-gel technology
on the surfaces to be modified leads to increased surface tensions. However, a
disadvantage is that the process itself is very complicated and time-consuming
which is why it does not appear to be suitable for modifying mass-produced plastic articles.
The object of the present invention was to eliminate the disadvantages of the
prior art. In particular it was intended to provide surface coatings with a high
surface tension that are stable over time to be used for example for the hydrophilic
modification of objects. Moreover it should be possible to carry out the coating
in a simple and reliable manner in order to be suitable for the modification of
mass-produced articles.
The object is achieved by the subject matter of the invention as characterized
in the patent claims.
The invention concerns a process for the production of a surface coating to increase
the surface tension of objects characterized in that a layer of at least one element
that can be oxidized with water or an alloy that can be oxidized with water is
deposited on an object and this is at least superficially oxidized by the subsequent
action of boiling water or water vapour on the deposited layer.
The invention additionally concerns the use of a surface coating to increase
the surface tension of objects characterized in that the surface coating is obtained
by deposition of a layer of at least one element that can be oxidized with water
or an alloy that can be oxidized with water and subsequent action of boiling water
or water vapour on the deposited layer.
Boiling water or water vapour and particularly preferably deionized water
is preferably used to treat the deposited surface coating.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a top view of a portion of an analytical test element
FIG. 2 is a view taken along lines 2—2 of FIG. 1.
DETAILED DESCRIPTIN OF THE INVENTION
The increase in the surface tension results from an increase in the polarity
and corresponds to an increased hydrophilicity of the observed surfaces. The hydrophilicity
is the water affinity of a surface. In this connection hydrophilic surfaces are
water-attracting surfaces. Aqueous samples also including biological samples like
blood, urine, saliva, sweat and samples derived therefrom such as plasma and serum
spread well on such surfaces. Such surfaces are characterized among others in that
a boundary surface of a water drop forms an acute rim or contact angle on them
(cf. for example the statements under the entry "Benetzung" in the "CD Römpp
Chemie Lexikon" version 1.0, 1995). In contrast an obtuse rim angle is formed at
the interface between a water drop and a surface on hydrophobic i.e. water repellent surfaces.
The rim angle which is a result of the surface tensions of the test liquid and
of the surface to be examined is a measure of the hydrophilicity of a surface.
Water for example has a surface tension of 72 mN/m. If the value of the surface
tension of the observed surface is much below this value i.e. more than 20 mN/m,
then the wetting is poor and the resulting rim angle is obtuse. Such a surface
is referred to as hydrophobic. If the surface tension approximates the value which
is found for water then the wetting is good and the rim angle is acute. If, in
contrast, the surface tension is the same as or higher than that of the value found
for water, then the drop runs and there is a total spreading of the liquid. It
is then no longer possible to measure a rim angle. Surfaces which form an acute
rim angle with water drops or on which a total spreading of a water drop is observed
are referred to as hydrophilic.
According to the invention the surface coating should be carried out by
depositing a layer of at least one element that can be oxidized with water or an
alloy that can be oxidized with water on an object. All objects come into consideration
as objects to be coated whose surface in the uncoated state has a lower hydrophilicity
than in the coated state after treatment. Examples are plastic, metal, glass, ceramics,
paper, fleece, cardboard etc. where the objects can have any shape e.g. flat, three-dimensional
or porous.
All 4 coating processes mentioned above can in principle be used to deposit the
layer i.e. coating from a gaseous or vaporous state, from a liquid, pulp or paste-like
state, from an ionized state or from a solid state. The coating is preferably carried
out from a gaseous state. A layer of an element or an alloy that can be oxidized
with water is particularly preferably applied to the surface to be modified in
a vacuum coater. This process is for example used cost-effectively for large surfaces
for the packaging industry and electrical industry for example with aluminium as
the element that can be oxidized with water.
The layers can be applied to the object to be coated as a continuous layer covering
the whole area but also in the form of any two-dimensional patterns.
It is essential for the subject matter of the invention that the deposited layer
of the element that can be oxidized with water or alloy that can be oxidized with
water is subsequently treated by the action of boiling water or water vapour after
the actual coating process. In this case it is sufficient to allow boiling water
or water vapour to act at normal pressure. However, it is preferably to use superheated
water vapour since this considerably reduces the exposure times. For example a
30 nm thick aluminium layer can be completely oxidized through with superheated
water vapour within ca. 45 s.
In this treatment the deposited layer of the element that can be oxidized with
water or the alloy that can be oxidized with water is at least superficially oxidized.
In this process at least the surface of the deposited layer of the element that
can be oxidized with water or the alloy that can be oxidized with water loses its
elemental properties. In the case of metals or alloys thereof this means among
others the loss of lustre and conductivity. In this process the oxidation of the
surface goes beyond the layer that may be present as a natural protective layer.
Thin metallic layers are oxidized during treatment with boiling water or water
vapour to such an extent that they completely lose their metallic appearance and
may become completely transparent.
The treatment with boiling water or water vapour is preferably carried out with
pure water and preferably with deionized water (for example aqua purificata according
to DAB). The surfaces obtained in this process are not contaminated with chemicals
which are found in other oxidation processes in particular wet chemical oxidation
processes such as oxidation with oxidizing acids. Purification and rinsing steps
can therefore be omitted and make the process more simple and cost-effective.
According to the invention it is possible to use base elements for the
coating which can be oxidized by boiling water or water vapour. The elements Al,
Si, Ti, V, Cr, Mn, Fe, Co, Ni, Zn, Ga, Ge, Zr, Nb, Cd, In, Sn, Sb are preferred.
Al, Si, Ti, Zr are particularly preferred. Al is quite especially preferred.
Base alloys that can be oxidized by boiling water or water vapour can also be
used according to the invention. These are preferably alloys which contain at least
two components from the following group of elements comprising Al, Si, Ti, V, Cr,
Mn, Fe, Co, Ni, Zn, Ga, Ge, Zr, Nb, Cd, In, Sn and Sb. An alloy of 99% by weight
Al and 1% by weight Si is for example suitable.
Alloys are also suitable which contain at least one component from the following
first group of elements comprising Al, Si, Ti, V, Cr, Mn, Fe, Co, Ni, Zn, Ga, Ge,
Zr, Nb, Cd, In, Sn and Sb which are alloyed with at least one element from the
following second group of elements comprising Mg, Ca, Sr and Ba such as for example
an alloy of 95% by weight Al and 5% by weight Mg. Alloys are particularly preferred
which contain at least one component from the following first group of elements
comprising Al, Si, Ti and Zr which are alloyed with at least one element of the
following second group of elements comprising Mg, Ca, Sr and Ba. Alloys that are
composed of aluminium which is alloyed with at least one element from the following
group of elements comprising Mg, Ca, Sr and Ba are quite especially preferred.
The deposited coat according to the invention preferably has a thickness of 1
nm to 500 nm. The action of boiling water or water vapour on the deposited layer
leads to the formation of oxide layers which are preferably between 0.1 nm and
500 nm, particularly preferably between 10 nm and 100 nm thick.
The surface coatings produced according to the invention are homogeneous inorganic
oxide layers which have a high surface tension and high polarity, which are stable
over a long period and have a good adherence with concomitant elasticity on the
coated object.
The characterization of surfaces with high surface tensions (high-energy surfaces)
causes certain technical measurement problems. In various measuring methods such
as contact angle measurement the interfacial effects of the surface to be examined
relative to test liquids are used. Since it is hardly possible to produce test
liquids with surface tensions that are considerably above the value for water (72
mN/m), there are certain limits to being able to extrapolate above this value.
Kinetic effects also add to the problems. A liquid which wets a surface, spreads
over a short period typically less than 1.5 s. However, spontaneous wetting is
important for the determination of the surface tension with regard to capillary
activity. In dynamic contact angle methods one refers to the progressive angle
of wetting of a drop that is becoming continuously larger. However, the dosing
of the drop and measurement of the drop with commercially available automated contact
angle measuring instruments is too slow for the hydrophilic surface coatings presented
here to be able to unequivocally describe the surface coatings according to the
invention. It therefore turned out to be practical to measure the surface coating
according to the invention by comparative determination of the filling time of
a test capillary.
The cylindrical test capillary is composed of two parallel opposing foils which
are kept at a defined distance from one another by an exactly defined spacer in
the form of a double-sided adhesive tape which determines the length, width and
height dimensions of the capillary. The opposing surfaces of the two foils are
provided with the coating to be tested. The dimensions of the capillary are 0.1
mm height, 2 mm width and 15 mm length where the length of the capillary corresponds
to the available transport path of the liquid and the height of the capillary is
that dimension which causes the capillarity. The capillary has an opening that
serves to take up the test liquid with a cross-sectional area of 0.1 mm×2
mm which corresponds to the base area of the cylindrical capillary. A vent opening
is provided at the opposite end of the capillary which allows the displaced air
in the capillary to escape when the test liquid is sucked in. The test liquid is
preferably distilled water or aqua purificata according to DAB but it is also possible
to use other test liquids depending on the field of application of the surface
coating such as blood or other body fluids. The filling times for the test liquids
are measured at half (7.5 mm transport path) and complete filling (15 mm transport
path). Comparative results are described in example 1.
The surface coatings
18 are particularly preferably used according to
the invention in analytical test elements
10 to increase the hydrophilicity.
The invention therefore also concerns an analytical test element or a test strip
in which the sample liquid is transported from a sample application site
12
to a determination site
14 in which a detection site lies upstream of the
sample application site in the transport direction. In this connection it is important
that the analytical test element
10 has at least one surface
16 which
is composed of at least one element that can be oxidized with water or an alloy
that can be oxidized with water which has been treated by the action of boiling
water or water vapour. The materials described above come into consideration as
elements and alloys.
Surfaces that have been made hydrophilic are especially essential for capillary
gap test elements. Capillary gap test elements are test elements in which the sample
liquid is moved in a transport channel (capillary channel, capillary gap) from
a sample application site to a distant sample detection site with the aid of capillary
forces in order to undergo a detection reaction at this site.
The ability of a capillary to suck up a liquid depends on the wettability of
the channel surface with the liquid. This means for aqueous samples that a capillary
should be manufactured from a material whose surface tension almost reaches 72
mN/m or exceeds this value.
Sufficiently hydrophilic materials for the construction of a capillary
which rapidly sucks up aqueous samples are for example glass, metal or ceramics.
However, these materials are unsuitable for use in test carriers since they have
some disadvantages such as risk of breaking in the case of glass or ceramics. Therefore
plastic foils or moulded parts are usually used to manufacture test elements. As
a rule the plastics used hardly exceed a surface tension of 45 mN/m. Even with
the, in a relative sense, most hydrophilic plastics such as polymethylmethacrylate
(PMMA) or polyamide (PA) it is only possible—if at all—to construct
slowly sucking capillaries. Capillaries made of hydrophobic plastics such as for
example polystyrene (PS), polypropylene (PP) or polyethylene (PE) essentially do
not suck aqueous samples. Consequently it is necessary to endow the plastics used
as a construction material for test elements with capillary active channels with
hydrophilic properties i.e. to hydrophilize them.
Therefore in analytical test elements with capillary gaps at least one,
but preferably two and especially preferably two opposing surfaces which form the
inner surface of the channel capable of capillary liquid transport are preferably
hydrophilized. If more than one surface is hydrophilized then the surfaces can
either be made hydrophilic using the same or different methods. Hydrophilization
is particularly necessary when the materials that form the capillary active channel
are themselves hydrophobic or only very slightly hydrophilic because they are for
example composed of nonpolar plastics. Nonpolar plastics such as for example polystyrene
(PS), polyethylene (PE), polyethylene terephthalate (PET) or polyvinyl chloride
(PVC) are advantageous as carrier materials because they do not absorb the liquids
to be examined and thus the sample volume can be effectively utilized by the detection
reaction. The hydrophilization of the surface of the capillary channel enables
a polar, preferably aqueous, sample liquid to readily enter the capillary channel
and be rapidly transported there to the site of the test element where the detection
takes place.
The hydrophilization is quite especially preferably achieved by using thin layers
of oxidized aluminium. These layers are either applied directly to the desired
components of the test element for example by vacuum coating the work pieces with
metallic aluminium and subsequently oxidizing the metal, or by using metal foils
or metal-coated plastics for the construction of the test carriers which also have
to be oxidized to achieve the desired hydrophilicity. In this case metal layer
thicknesses of 1 to 500 nm are adequate. The metal layer is subsequently oxidized
to form the oxidized form whereby according to the invention oxidation in the presence
of water vapour or by boiling in water have proven to be especially suitable methods.
The oxide layers formed in this manner are between 0.1 and 500 nm, preferably between
10 and 100 nm thick depending on the method. Larger layer thicknesses of the metal
layer as well as of the oxide layer can in principle be realised in practice but
do not exhibit any additional advantageous effects.
Further applications according to the invention of surface coatings are
- making polymer foils, fabrics, fleeces or three-dimensional formed pieces
hydrophilic and detergent-free to improve their adhesive properties for paint,
adhesive or plastic coats,
- adsorptive binding of polar molecules or materials in particular for
the adsorption of biologically active molecules such as proteins, enzymes, antibodies,
nucleic acids (cf for example Chem. Pharm. Bull. 41, (1993) 1055) since the increased
surface tension is associated with an increase in the polarity of the surface,
- production of surface patterns such as cross-pieces for the transport
of polar liquids, for a defined boundary between polar and nonpolar areas in which
case these patterns can be produced by the structure of the deposited material
itself or subsequently by selectively covering certain areas of the deposited material
layer with for example wax when it is treated with boiling water or water vapour.
The invention is elucidated by the following example.
EXAMPLE 1
Comparison of the Filling Times of a Test Capillary
A cylindrical test capillary was constructed from two parallel opposing foils
which
are kept at a defined distance from one another by an exactly defined spacer in
the form of a double-sided adhesive tape which determines the length, width and
height dimensions of the capillary. The opposing surfaces of the two foils were
provided with the coating to be tested. The foils that were used were polyester
foils (Melinex®, ICI) which were variously modified as follows.
1.) Foil which was coated with photoreactively equipped hydrophilic polymers (BSI)
2.) Foil which was subjected to a corona plasma treatment (Antec)
3.) Foil on which a layer containing a wetting agent was applied (A.R.)
4.) Foil on which inorganic-organic nanocomposites were coated by means
of sol-gel technology (INM)
5.) Foil on which aluminium oxide was vapour deposited but which was not
subsequently treated with boiling water or water vapour (Alu—Ox).
6.) Foil on which firstly a layer of aluminium of 30 nm thickness was vapour
deposited which was subsequently completely oxidized for 45 s with water vapour (Alu—Ox/H2O).
The dimensions of the capillary are 0.1 mm height, 2 mm width and 15 mm length
where the length corresponds to the transport path of the liquid and the height
is that dimension which causes the capillarity. The capillary has an opening that
serves to take up the test liquid with a cross-sectional area of 0.1 mm×2
mm which corresponds to the base area of the cylindrical capillary. A vent opening
is provided at the opposite end of the capillary which allows the displaced air
in the capillary to escape when the test liquid is sucked in. The test liquid was
in one case distilled water, aqua purificata according to DAB and in the other
case human blood (containing EDTA as an anticoagulant, haematocrit 44%). The filling
times for the test liquids were measured at half (7.5 mm transport path) and complete
filling (15 mm transport path). The capillary was kept vertical during filling
so that the test liquid had to cover the filling path of 15 mm against the force
of gravity. The comparative results are shown in Table 1.
| |
TABLE 1 |
| |
|
| |
|
|
Filling time |
| |
|
Filling time for blood [s] |
for water [s] |
| |
Coating |
after 7.5 mm after 15 mm |
after 15 mm |
| |
|
| |
| |
BSI |
0.5-0.6 |
2.1-2.7 |
0.6-0.9 |
| |
Antec |
1.4-2.3 |
4.7-8.4 |
4.0-7.0 |
| |
A.R. |
0.4-0.5 |
1.8-2.1 |
0.4-0.5 |
| |
INM |
|
1.0-3.0 |
| |
Alu-Ox |
— |
1.2 |
— |
| |
Alu-Ox/H2O |
0.2-0.3 |
0.7 |
<0.2 |
| |
|
The coating according to the invention (Alu—Ox/H
2O) is the one
which wets most actively among all tested layers. The coating according to the
invention (Alu—Ox/H
2O) produced by the action of water vapour
after coating the metal has a considerably improved hydrophilicity compared to
a surface (Alu—Ox) that was coated directly with aluminium oxide but was
not oxidized by the action of water vapour. The production process according to
the invention is relatively simple, can be controlled well and leads to stable
coatings with high surface tensions that remain constant over time.
*
