Method for producing thin film coated magnetic disks and thin film magnetic disks thus obtained

Abstract: The known process in which a base coating and on this the magnetic coating and finally a top coating are applied, have the disadvantage that the corrosion resistance is not adequate: there are defects. It is not inconceivable that it is possible for water to diffuse into the substrate. In accordance with the invention, a barrier layer is interposed between the substrate and the base coat by medium frequency pulsed sputtering at a frequency of 10 to 200 kHz and a pulse length to pulse pause ratio from 5:1 to 1:10. The invention finds application preferably for hard magnetic disks of high storage density.

Description: The invention concerns a method for coating thin film coated magnetic disks of high storage density for use in hard magnetic disks, by means of magnetron sputtering, and a thin film magnetic disk produced using this method. The methods of producing thin film magnetic disks in vertical continuous coaters for a large number of substrates to be coated together, or in single disk coaters, are already known. The substrates for the production of thin film magnetic disks consist of glass or of highly polished aluminium disks galvanised with a nickel-phosphorous coating. In future, various alternative materials such as aluminium borocarbide will be used. Irrespective of the substrate material, a number of thin coats are applied by physical and/or chemical atomisation of the coats. These are base coats, mostly consisting of chromium, magnetic storage layers, mostly consisting of composite alloys of cobalt, chromium and other metals, and a top coat, mostly consisting of carbon. DC magnetron sputtering is the most commonly used coating method in the production of thin film magnetic disks. For high-quality thin film magnetic disks, a storage density in excess of 3 Gbit/in 2 is required. The resulting flying heads of the magnetic heads are below 40 nm. A reduction in noise and in holidays on the storage surface and effective adaptation to the heads are pre-requisites for the realisation of this storage density. The method of achieving the low flying heads by improving the topography of the surface of the finished thin film magnetic disk and reducing the thickness of the coatings, especially the magnetic coat and the top coat, is already known. By using new alloys for the magnetic storage layer and specially adapted underlying structures, thin film magnetic disks with coercive field strengths of > 1,99 x 10 5 A/m (2500 Oe) and remanent magnetisation layer thickness (Mrt) of ≥ 0.5 can be produced with good reproducibility. New problems, not previously encountered, have arisen chiefly due to demands for increasing storage density and reducing the thickness of the coatings. A decisive shortcoming is the fact that increased corrosion occurs with the use of aluminium substrates. This corrosion gives rise to blooming and warping on the surface of the magnetic disk, which results in areas which can no longer be written on or read. There is a danger that these may come into contact with the heads, as the flying head is around the same height as the blooming. Two factors have an effect on corrosion. On the one hand, errors in polishing the substrates and residues from wet processes are triggers for corrosion. On the other hand, the atomised coats are only tight and non-porous to a limited extent. Amongst other things, the reduction in coat thickness from 30 nm to 10 nm has the effect of worsening corrosion behaviour. The top coat can only perform the function of the mechanical protection of the magnetic coat against contact with the heads and, in conjunction with the lubricant, safeguards the sliding capability of the heads. (The problem of corrosion is described in detail by Chia, Wang, Tang and Lee in "Overview of accelerated corrosion tests on thin film magnetic media" in The Minerals, Metals & Materials Society, 1998, p. 311-319.) Although the substrates are polished to a mirror finish, the topography of the finished magnetic disks is less than ideal. Microscopic cracks and pinholes can be detected.These defects on the surface of the substrates stand in the way of optimum cleaning during the washing process. This decreases the evenness of the atomisation of the coats and results in less effective covering of the edges. It is known that corrosion can be reduced by increasing the thickness of the base coat and applying a negative direct current to the substrate during the atomisation of the base coat. Neither measure solves the problem. They only reduce the number of corrosion points revealed in acid tests with HCl or HNO 3 . The usefulness of the measures is not unlimited. The increase in thickness of the base coat is in contrast to the requirements as regards magnetism. The application of a negative direct current to the substrate can only be used in the case of conductive substrates. The basis of the invention lies in the task of creating a method of coating thin film magnetic disks by improving the production thereof to such an extent that, in the case of metallic substrates, the corrosion resistance of magnetic disks is significantly increased and, in the case of non-metallic substrates, the diffusion of water to the substrate and of freely moveable ions from the substrate is drastically reduced. The method is intended for use with all substrate materials - both conductive and insulating. It is intended that the method can be implemented for industrial use in the usual coating plants. A further task of the invention is to create a thin film magnetic disk with increased corrosion resistance. In accordance with the invention, the task is solved according to the features of claims 1 and 9. Further advantageous basic features of the method are described in claims 2 to 8. The finding was the placing of a barrier layer between the substrate and the series of magnetic coatings in such a way that the magnetic values such as coercive field strength and remanent magnetisation layer thickness are not influenced. This reduces the corrosion resistance to such an extent that practically no holidays caused by corrosion can be detected on the magnetic disks using known testing methods. This represents an improvement by one to two orders. Surprisingly, the effect is achieved at a thickness as low as just a few nm. In accordance with the method, aluminium or chromium are the preferred materials for application as barrier layers. Very good properties are achieved where the process gas contains a proportion of oxygen and/or nitrogen. The increase in coercive field strength which can be noted in the pulsed atomisation of the base coat is not activated when the barrier layer in accordance with the invention is used. Spraying on a chromium coating for the barrier layer is very advantageous, as the crystal formation in the subsequent steps is not disturbed. It is of particular advantage that the effect of the barrier layer can be adapted to the relevant substrate material by means of the choice of material to be atomised, the variation in coating thickness and the selection of the frequency and pulse ratio for the sputtering process. A frequency of 50 kHz has been shown to be particularly suitable. This frequency evidently brings about a favourable atomisation rate to plasma excitation ratio, to atomise very tight, defect-free coats with a high yield of sputtered excited particles. The freedom from defects here relates to coats without pinholes or a columnar structure. The method in accordance with the invention can be implemented for all magnetic disk coaters. This suitability for integration into production plants is a great advantage of the method. The invention will be illustrated in more detail using an example of embodiment. A single disk coater, which is in itself known, is used to atomise a series of magnetic coats and a barrier layer on an aluminium substrate which has a protective coating of nickel phosphorous, applied galvanically, to produce thin film magnetic disks. As proof of the effectiveness of the method in accordance with the invention, a standard process is drawn on. For the coated thin film magnetic disks, the magnetic properties and the properties of the barrier layer are determined. These values must be within the specified tolerances. A sample of the coated magnetic disks is subjected to an acid test using HNO 3 in order to evaluate the corrosion resistance. After the reference samples have been prepared, the thin film magnetic disks are produced in accordance with the invention. To do this, in addition to the process steps used hitherto: heating, atomisation of the base coat, atomisation of the magnetic coats and atomisation of the protective coating, a further process step of applying the barrier layer is introduced after the heating stage. Here, the substrates are heated to 220°C, and a barrier layer is atomised before atomisation of the base coat. The process time for the atomisation of the barrier layer is 4 seconds at a pressure of 0.8 Pa. Oxygen with a partial pressure of 0.1 Pa is mixed in with the inert carrier gas. An aluminium target with a standard magnetron arrangement is used. The energy is pulsed into the plasma. The pulse frequency is 50 kHz, and the pulse length to pulse gap ratio is adjusted to 1:1. The resulting plasma switching on time is 10 µs and the gap is also 10 µs. The primary power, i.e. the power fed into the pulsing device, is 150 W averaged over time. The method in accordance with the invention has also shown that, with a pulse length of 14 µsec and cycle duration of 20 µsec the positive effect starts to decrease once more, i.e. the corrosion holidays start to increase sharply again. The table shows measurement values for magnetic properties and measured corrosion values. The introduction of a very tight, pinhole-free barrier layer atomised by means of medium frequency pulsed magnetron sputtering improves corrosion behaviour by one to two orders. The application of a negative direct current to the substrate during atomisation of the barrier layer further improves corrosion resistance. The magnetic values of coercive field strength and remanent magnetisation layer thickness do not change when the method is carried out using the stated parameters (see table below) Barrier Pulse ratio for barrier Substrate bias Corrosion points per disk Hc [Oe] average values Md average values Standard no no 85 - 105 2,07x 10 5 2595 0.59 Variant 1 yes 1:1 no 1 - 4 2,05x 10 5 2575 0.61 Variant 2 yes 1:1 yes 0 - 2 2,08x 10 5 2610 0.6 The greatest effect is achieved by the introduction of the barrier layer in accordance with the invention in itself. Variant 1 shows that the number of corrosion points which are discovered in the course of a HNO 3 test is very small compared with the standard process. Variant 2 shows that the atomisation of the barrier layer with a negative direct current applied to the substrate produces a further improvement.

Claims: Method for coating thin film magnetic disks by magnetron sputtering, comprising a substrate, on which a series of layers consisting of base coats, magnetic coats, intermediate coats and a top coating is applied, characterized in that between the substrate and the first base coating of the series of coatings a barrier layer is applied by medium-frequency sputtering at a frequency between 10 and 200 kHz, preferably 50 kHz and with a pulse length to pulse gap ratio in the region of 5:1 to 1:10. Method in accordance with Claim 1, characterised in that the barrier layer is deposited by atomising a chromium target. Method in accordance with Claim 1 and 2, characterised in that the pressure on atomising the barrier layer is adjusted to 0.1 to 1.5 Pa, preferably to 0.5 Pa. Method in accordance with Claim 1 to 3, characterised in that during the atomisation of the barrier layer other gases, preferably reactive gases such as oxygen and/or nitrogen, are mixed with the carrier gas. Method in accordance with Claim 1 to 4, characterised in that a thin layer is applied to the substrate to be coated before atomising the barrier layer. Method in accordance with Claim 1 to 5, characterised in that a direct current of -50 V to -500 V, preferably - 200 V is applied to the substrate during the atomisation of the barrier layer. Method in accordance with Claim 1 to 5, characterised in that a pulsed voltage, preferably with a frequency of 50 kHz is applied to the substrate during the atomisation of the barrier layer. Method in accordance with Claim 1 to 5, characterised in that a high frequency alternating current with a frequency of preferably 13.56 MHz is applied to the substrate during the atomisation of the barrier layer. Thin film magnetic disk comprising a substrate, on which a series of layers consisting of base coats, magnetic coats, intermediate coats and a top coating is applied, characterized in that a barrier coating is applied between the substrate and the first base coating by medium frequency pulsed magnetron sputtering.

Inventors: BAUR HEINZ, BLUETHNER RALF, BUCHBERGER HANS, GOEDICKE KLAUS, JUNGHAEHNEL MICHAEL, LEHNERT KARL-HEINZ, MUELLER MANFRED, SCHNEIDER HANS-HERMANN, WINKLER TORSTEN, BAUR, HEINZ, BLUETHNER, RALF, BUCHBERGER, HANS, GOEDICKE, KLAUS, JUNGHAEHNEL, MICHAEL, LEHNERT, KARL-HEINZ, MUELLER, MANFRED, SCHNEIDER, HANS-HERMANN, WINKLER, TORSTEN, Blüthner, Ralf , Junghähnel, Michael , Müller, Manfred 
Applicants: FRAUNHOFER GES FORSCHUNG, IBM, FRAUNHOFER-GESELLSCHAFT ZUR FOERDERUNG DERANGEWANDTEN FORSCHUNG E.V., INTERNATIONAL BUSINESS MACHINES CORPORATION
Application year: 1999
Main classification: C23C14
IPC codes: C23C14, G11B5, B05D7