Coating processes – Measuring – testing – or indicating – Thickness or uniformity of thickness determined
Reexamination Certificate
1995-05-01
2001-10-02
Meeks, Timothy (Department: 1762)
Coating processes
Measuring, testing, or indicating
Thickness or uniformity of thickness determined
C427S575000, C427S567000, C427S585000, C427S596000, C427S255310, C427S255320
Reexamination Certificate
active
06296895
ABSTRACT:
BACKGROUND OF THE INVENTION
The invention pertains to a process for the application of a transparent metal oxide layer on a film, in which a metal is vaporized in a receiver and brought into contact in the vapor phase with oxygen.
Systems which operate according to a process of this type are known in coating technology. As an example, see U.S. Pat. No. 5,302,208, although it does not have reactive vapor deposition as its object. In the system described in this publication, an electron beam is used to vaporize a metal oxide. The vapor cloud is converted to a plasma by microwave energy, which is supplied by way of a horn antenna, as a result of which layers with especially good properties are obtained.
For an example of the reactive vaporization of a metal for the coating of a substrate, see U.S. Pat. No. 4,777,062. Like the preceding patent, this document does not deal with the problem of controlling the vaporization rate and thus not with the problem of producing a layer of precisely defined thickness.
For the coating of films with aluminum, it is known that several optical sensors can be provided in the receiver, behind the coating window, distributed across the width of the film. These sensors measure the transmission or optical density of the film coated with aluminum, and the power and/or motion of the electron beam over the metal crucible are controlled in accordance with output of these sensors. When a film is coated with a transparent material such as Al
2
O
3
, it is not possible to monitor the thickness of the layer in this way if the coated material is highly transparent. Such transparency is required, for example, in the case of films used to package food products, because it must be possible to see the food products easily, because the color of the food products may not be negatively affected by the packaging, and finally because it must be possible to heat quickly the contents of package in its packaging by means of microwaves. So far, the thickness of transparent layers has been measured by means of x-rays, but this is a relatively complicated method.
SUMMARY OF THE INVENTION
The invention is based on the problem of determining the thickness of a transparent oxide layer on a film in a very simple manner during the application process.
This problem is solved by introducing a slightly substoichiometric amount of oxygen, i.e., an amount not sufficient to produce a completely transparent metal oxide layer, into the receiver. To determine the thickness of the applied layer and to control the vaporization rate, optical sensors are provided in an area where the layer, thanks to presence of unoxidized metal, has an absorption sufficient for optical measurement; and in that, after the transparency has been determined by the sensors, the layer is subjected to a secondary oxidation process.
By means of a process such as this, it is possible, even in the production of highly transparent metal oxide layers, to determine the layer thickness on-line with simple optical sensors and to control the coating system accordingly. The basic idea of the invention is first to produce a layer which is not completely transparent so that it is still possible to measure the layer thickness by means of the transmission or optical density of the layer, and then to make the layer completely transparent afterwards by means of a secondary oxidation step. Conducting the coating process with a substoichiometric amount of oxygen in the receiver offers the additional advantage that the undesirable formation of a porous layer which can result from an excessive amount of oxygen can be reliably prevented. The process according to the invention will be used primarily for the coating of transparent films. By means of the optical sensors, therefore, the light which will be measured will be that which shines through the coated film. But it is also possible for sensors to determine the reflective power of a coating. Then the process according to the invention can also be applied to opaque films.
The secondary oxidation step can be accomplished in various ways. It is especially simple when the secondary oxidation is conducted outside the receiver by means of the oxygen content of the air. A secondary oxidation of this type can be carried out, for example, while the film is being unwound from a supply roll and packaging materials are being made from it.
It is also possible, however, as an alternative, to carry out the secondary oxidation in an oxidation stage installed downline from the optical sensors.
In principle, the process according to the invention is independent of how the metal is vaporized. When an electron beam passing over a crucible filled with metal is provided as the means of vaporizing the metal, then, as a way of controlling the thickness of the layer, it is advantageous to adjust the power of the electron beam as a function of the measurement values of the optical sensor.
Transparent oxide layers can be produced from the oxides of various metals, especially Al, Cr, Si, Sn, and Al alloys. In practice, the process of the invention has been tested and found especially advantageous for the production of a layer of aluminum oxide.
The properties of the layer, especially the barrier effect with respect to oxygen and odors vital to good food packaging materials, are especially advantageous when a plasma is produced in the receiver. As a result of this measure, the metal oxide molecules are in the form of ions when they strike the layer at elevated velocity, and a denser layer is produced as a result.
It is advantageous for the plasma to be produced by feeding microwave energy into the cloud of metal vapor.
A layer of uniform thickness can be produced even over the entire width of wide films when the absorption of the film is measured at several points across the width, and when the power and/or the movement of the electron beam over the crucible with the metal to be vaporized is controlled on the basis of these values.
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Hoffmann Gerd
Ludwig Rainer
Steiniger Gerhard
Balzers Und Leybold Deutschland Holding AG
Fulbright & Jaworski LLP
Meeks Timothy
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