JPH0925576A - Film forming method and film forming device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To make it possible to control the thickness of magnetic metallic thin films with high accuracy by measuring the light transmittance and transmitted X-ray intensity of the formed films and adjusting the output of an electron gun and the supply rate of the gaseous oxygen in accordance with the measured information. SOLUTION: The signals from light transmittance measuring means 10, 11 and the signal from a transmitted X-ray intensity measuring means 12 are inputted to a control means 13 in the process of forming the magnetic metallic thin films. When the fluctuation in the transmitted X-ray intensity is not admitted and the fluctuation in the light transmittance is admitted, the supply rate of the gaseous oxygen from a nozzle 7 is adjusted according thereto. When the fluctuation in the light transmittance is not admitted and the fluctuation in the transmitted X-ray intensity is admitted, the output of the electron gun 8 is adjusted according thereto. When the fluctuation is admitted in both of the light transmittance and the transmitted X-ray intensity, the output of the electron gun 8 and the supply rate of the gaseous oxygen from the nozzle 7 are adjusted according thereto. As a result, a magnetic recording medium having high quality is produced at a good yield.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a film forming technique such as a method for manufacturing a magnetic recording medium or a manufacturing apparatus.

[0002]

In a magnetic recording medium such as a magnetic tape, a magnetic layer provided on a non-magnetic support is not a coating type using a binder resin because of a demand for high density recording. It is well known that a metal thin film type that does not use a binder resin has been proposed.

That is, there has been proposed a magnetic recording medium having a magnetic layer formed by a wet plating means such as electroless plating, or a dry plating means such as vacuum deposition, sputtering or ion plating. This kind of magnetic recording medium is suitable for high-density recording because of its high packing density of magnetic material. In particular, the means for forming a magnetic film by vapor deposition means is said to be preferable because the film formation rate is higher than that by sputtering.

An apparatus for manufacturing a magnetic recording medium by this vapor deposition means is generally constructed as shown in FIG. still,
In FIG. 2, 31 is a cooling can roll, 32a is a polyethylene terephthalate (PET) film 33 supply side roll, 32b is a PET film 33 take-up side roll, 34
Is a shielding plate, 35 is a crucible, 36 is a magnetic alloy, and 37 is a vacuum chamber. That is, after evacuation of the vacuum chamber 37 to a predetermined degree of vacuum, the electron gun 38 is operated to evaporate the magnetic alloy 36 in the crucible 35, and magnetic alloy particles are deposited (evaporated) on the PET film 33, thereby magnetically A recording medium is manufactured.

By the way, one of the important things when forming a magnetic film by vapor deposition is to make the thickness of the formed magnetic film uniform. That is, when the thickness of the magnetic film is not uniform, there arises a problem such as output fluctuation. For this reason, a technique is proposed in which a transmission-type film thickness meter is provided in the film formation process, the thickness of the formed film is obtained by measuring the transmittance, and this information is reflected in the film formation conditions. (JP-A-6-150309).

The above proposed technique should have been able to make the thickness of the film to be formed uniform. However, according to the research by the present inventor, it has been found that it is not enough to use the transmission type film thickness meter. That is, when the composition of the formed magnetic film is constant, the light transmittance is the same if the thickness is the same, but if the composition of the magnetic film changes, for example, the degree of oxidation changes. In some cases, there is a variation in light transmittance for the same thickness. Therefore, it is not possible to control the thickness of the film to be formed with high accuracy only by measuring the light transmittance.

[0007]

Means for Solving the Problems While earnestly advancing the study from such a viewpoint, if the transmitted X-ray intensity and the light transmittance of the formed film are measured, I noticed that the thickness can be controlled with high accuracy. That is, since it is possible to obtain information about the amount of the constituent components of the formed film from the information of the transmitted X-ray intensity, it is possible to control the physical quantity such as the evaporation amount, and to form the information from the light transmittance. Since the information on the degree of oxidation of the formed film can be obtained, the thickness of the formed film can be made uniform by controlling these in combination.

The present invention has been achieved based on such knowledge, and an object thereof is to provide a technique for forming a uniform film. An object of the present invention is a method for forming a film by causing particles having an M element component to fly and depositing them on a support, which has a step of depositing particles having an M element component and an oxidizing property. The step of supplying the components and the X for obtaining the transmitted X-ray intensity of the formed film.
And an O step of obtaining a light transmittance of the formed film, and when there is no change in the information obtained in the X step and the O step, the deposition amount of particles having an M element component and When the supply amount of the oxidizable component is maintained as it is, and the information obtained in the step X does not change and the information obtained in the step O does change, the oxidizable substance has a corresponding oxidizing property. If the information obtained in the step O is not changed and the information obtained in the step X is fluctuated by varying the supply amount of the component, the deposition amount of the particles having the M element component is correspondingly changed. And the information obtained in the steps X and O is changed, M
This is achieved by a film forming method characterized by varying the deposition amount of particles having an elemental component and the supply amount of an oxidizing component.

Further, particles having an M element component are flown in,
An apparatus for forming a film by depositing on a support, comprising means for depositing particles having an M element component, means for supplying an oxidizing component, and transmitted X-ray intensity for the formed film. When no variation is found in the transmitted X-ray intensity measuring means to be obtained, the light transmittance measuring means to obtain the light transmittance of the formed film, and the information obtained by the transmitted X-ray intensity measuring means and the light transmittance measuring means. Shows that the amount of particles having the M element component and the amount of the component having the oxidizing property supplied are maintained as they are, and that the information obtained by the transmitted X-ray intensity measuring means has no fluctuation, and In the case where the obtained information is fluctuated, the supply amount of the oxidizing component is changed accordingly, and the information obtained by the light transmittance measuring means is not fluctuated, and the transmitted X-ray intensity measurement is performed. There is a fluctuation in the information obtained by means In the case is because, according to this M
By varying the deposition amount of particles having an elemental component, the transmission X
When the information obtained by the line intensity measuring means and the light transmittance measuring means is fluctuated, the control means for fluctuating the deposition amount of the particles having the M element component and the supply amount of the oxidizing component accordingly. And a film forming apparatus comprising:

The support used in the present invention may be either magnetic or non-magnetic, but is generally non-magnetic. Such a support is a polyester such as PET,
An organic material such as an olefin resin such as polyamide, polyimide, polysulfone, polycarbonate, or polypropylene, a cellulose resin, or a vinyl chloride resin is used. An undercoat layer for improving the adhesion of the magnetic layer (metal magnetic thin film) is appropriately provided on the surface of the support.

A magnetic thin film is provided on one surface of the support by, for example, oblique vapor deposition means. As the material of the magnetic particles forming the metal magnetic thin film, for example, in addition to metals such as Fe, Co, and Ni, a Co—Ni alloy, a Co—Pt alloy, and a Co—
Ni-Pt alloy, Fe-Co alloy, Fe-Ni alloy, F
e-Co-Ni alloy, Fe-Co-B alloy, Co-Ni
-Fe-B alloy, Co-Cr alloy, or A
A material containing a metal such as l is used. Also, Fe
-N alloy, Fe-NO alloy, Fe-C alloy, Fe-C
An -O alloy or the like is also used. Oxidizing gas such as oxygen is supplied when the metal magnetic thin film is formed, and a protective layer made of an oxide film is formed on the surface layer of the metal magnetic thin film.

The vapor deposition apparatus shown in FIG. 1 can be employed as an apparatus for depositing a metal magnetic thin film by oblique vapor deposition means. In FIG. 1, 1 is a cooling can roll, 2a is a supply side roll of the non-magnetic support 3, 2b is a winding side roll of the support 3, and 4 is a MgO filled with a magnetic material 5 such as metal Co. Crucible, 6 is a shielding plate, 7 is an oxidizing gas (oxygen) supply nozzle, 8 is an electron gun with an output of 16 kW, and 9 is a vacuum chamber. Incidentally, such an oblique vapor deposition device is well known.

Reference numerals 10 and 11 denote light transmittance measuring means composed of a light emitting element and a light receiving element (including an amplifier circuit if necessary). The light transmittance measuring means 10 includes a cooling can roll 1 and a supply side roll 2a. Is provided in a traveling path (before the metal magnetic thin film is formed) between the cooling can roll 1 and the winding side roll 2b (the metal magnetic thin film is formed). It is provided in the later stage). These light transmittance measuring means 10 and light transmittance measuring means 1
By considering the output of 1 and 1, the light transmittance of the metal magnetic thin film formed on the support 3 can be detected.

Numeral 12 is a transmitted X-ray intensity measuring means provided on a traveling path between the cooling can roll 1 and the winding side roll 2b. This makes it possible to obtain information on the amount of constituent components of the metal magnetic thin film. Reference numeral 13 is a control means, which receives signals from the light transmittance measuring means 10 and 11 and the transmitted X-ray intensity measuring means 12 to output the electron gun 8, the shield amount by the shield plate 6 and / or the support 3. It is configured to control the traveling speed and the oxygen gas supply amount from the nozzle 7. That is, when there is no change in the light transmittance or the transmitted X-ray intensity, the output of the electron gun 8, the amount of shielding by the shielding plate 6, the traveling speed of the support 3 (all of which are determined by the accumulated amount of metal particles). The factor to be adjusted) and the amount of oxygen gas supplied from the nozzle 7 are maintained as they are. If there is no change in the transmitted X-ray intensity and there is a change in the light transmittance, the nozzle is adjusted accordingly. When the oxygen gas supply amount from 7 is adjusted and the light transmittance is not changed and the transmitted X-ray intensity is changed, the output of the electron gun 8 and the shield amount by the shield plate 6 are correspondingly changed. When the traveling speed of the support 3 is adjusted and / or the light transmittance and the transmitted X-ray intensity are changed, the oxygen gas supply amount from the nozzle 7 and the output of the electron gun 8 are correspondingly changed. , The amount of shielding by the shielding plate 6 and / or
Alternatively, the traveling speed of the support 3 is adjusted.

According to the present invention configured as described above,
Since it is possible to control the degree of oxidation and the amount of magnetic metal deposited,
The thickness of the film that has undergone surface oxidation can be controlled uniformly. Therefore, since the formed metal magnetic film becomes uniform, it is difficult for output fluctuation to occur, and there is little variation,
High quality products can be obtained with good yield. In the above description, a magnetic recording medium is manufactured, but the present invention is applicable to any case where metal particles are deposited while supplying an oxidizing component.

[0016]

DETAILED DESCRIPTION OF THE INVENTION The apparatus shown in FIG. 1 was used. That is, after the vacuum chamber 9 is evacuated to a vacuum degree of about 10 ⁻⁴ to 10 ⁻⁶ Torr, for example, 2.1 × 10 ⁻⁵ Torr, the magnetic material in the crucible 4 ( Metal Co) 5 is melted and evaporated, and cooling can roll 1
Particles of metal Co5 were obliquely vapor-deposited on the 3 surface of the support (PET film) attached to the. When vapor deposition,
The standard of the amount of oxygen gas supplied from the nozzle 7 is 120 sccm.
I made it. The traveling speed of the support 3 was set to 1 m / min (constant).

In the process of forming such a metal magnetic thin film, the signals from the light transmittance measuring means 10 and 11 and the signal from the transmitted X-ray intensity measuring means 12 are input to the control means 13. Then, the control means 13 receives the light transmittance information and the transmitted X-ray intensity information to control the oxygen gas supply amount to the nozzle 7 (increase / decrease of the oxygen gas supply amount) and the output of the electron gun 8 (from the crucible 4). Increase or decrease the evaporation amount of the metal Co).

That is, when no change is observed in the light transmittance or the transmitted X-ray intensity, the output of the electron gun 8 and the oxygen gas supply amount from the nozzle 7 are maintained as they are.
When the transmitted X-ray intensity is not changed and the light transmittance is changed, the oxygen gas supply amount from the nozzle 7 is adjusted accordingly. For example, the oxygen gas supply amount is decreased or increased according to the increase or decrease of the light transmittance.

If there is no change in the light transmittance but there is a change in the transmitted X-ray intensity, the electron gun 8 is accordingly responded.
Adjust the output of. For example, the output of the electron gun 8 is decreased or increased according to the increase or decrease of the transmitted X-ray intensity. When the light transmittance and the transmitted X-ray intensity both fluctuate, the output of the electron gun 8 and the oxygen gas supply amount from the nozzle 7 are adjusted accordingly. For example, the output of the electron gun 8 is reduced and the oxygen gas supply amount from the nozzle 7 is reduced in accordance with the increase of the light transmittance and the intensity of the transmitted X-ray to increase the light transmittance and the intensity of the transmitted X-ray. In accordance with the decrease, the output of the electron gun 8 is increased, the oxygen gas supply amount from the nozzle 7 is decreased, the light transmittance is decreased, the output of the electron gun 8 is decreased in accordance with the increase of the transmitted X-ray intensity, and The amount of oxygen gas supplied from the nozzle 7 is increased, the output of the electron gun 8 is increased in accordance with the decrease of the light transmittance and the decrease of the transmitted X-ray intensity, and the nozzle 7
Increase the oxygen gas supply from.

By the way, when the variation in the case of depositing 2000 Co of metal Co on the support having a length of 1000 m was examined by the reproduction output, the output variation was within 5%. On the other hand, when the film thickness control was attempted only by the signal from the light transmittance measuring means without inputting the information from the transmitted X-ray intensity measuring means to the control means, the output variation reached 10%. .

From the above, it can be seen that according to the present invention, the film thickness of the metal magnetic thin film can be controlled with extremely high accuracy, and a high quality magnetic recording medium can be manufactured with a high yield.

[0022]

According to the present invention, a film having a uniform thickness can be formed with high yield.

[Brief description of drawings]

FIG. 1 is a schematic view of an entire magnetic recording medium manufacturing apparatus according to the present invention.

FIG. 2 is a schematic view of an entire conventional magnetic recording medium manufacturing apparatus.

[Explanation of symbols]

 1 Cooling Can Roll 2a Supply Side Roll 2b Winding Side Roll 3 Support 4 Crucible 5 Magnetic Material 6 Shielding Plate 7 Oxidizing Gas Supply Nozzle 8 Electron Gun 9 Vacuum Tank 10, 11 Light Transmittance Measuring Means 12 Transmission X-ray Strength Measurement Means 13 Control means

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Akira Shiga 2606 Akabane, Kai-cho, Haga-gun, Tochigi Prefecture Kao Corporation Company Information Science Laboratory

Claims (2)

[Claims] 1. A method of forming a film by causing particles having an M element component to fly and depositing the particles on a support, comprising the steps of depositing particles having an M element component and oxidizing a component having an oxidizing property. It comprises a supplying step, an X step of obtaining a transmitted X-ray intensity of the formed film, and an O step of obtaining a light transmittance of the formed film, and the information obtained in the X step and the O step has a fluctuation. If not observed, the deposition amount of the particles having the M element component and the supply amount of the oxidizing component are maintained as they are, and there is no change in the information obtained in the X step, and the information obtained in the O step. If there is a change in the value, the supply amount of the component having an oxidizing property is changed according to the change, and the information obtained in the step O is not changed, but the information obtained in the step X is changed. In the case of M yuan accordingly When the deposition amount of the particles having the component is varied and the information obtained in the X step and the O step is varied, the deposition amount of the particles having the M element component and the component having the oxidizing property are correspondingly changed. A film forming method characterized by varying the supply amount. 2. A device for forming a film by causing particles having an M element component to fly and depositing them on a support, comprising means for depositing particles having an M element component, and an oxidizing component. Supplying means, transmitted X-ray intensity measuring means for obtaining transmitted X-ray intensity for the formed film, light transmittance measuring means for obtaining light transmittance for the formed film, the transmitted X-ray intensity measuring means and light When no change is found in the information obtained by the transmittance measuring means, the deposition amount of the particles having the M element component and the supply amount of the oxidizing component are maintained as they are, and the information obtained by the transmission X-ray intensity measuring means is obtained. When the information obtained by the light transmittance measuring means is not changed, the supply amount of the oxidizing component is changed accordingly, and the light transmittance measuring means is used. Fluctuations in information obtained Not observed,
When the information obtained by the transmitted X-ray intensity measuring means is fluctuated, the deposition amount of the particles having the M element component is changed accordingly, and the transmitted X-ray intensity measuring means and the light transmittance measuring means are used. When the obtained information is fluctuated, it is provided with a control means for changing the deposition amount of the particles having the M element component and the supply amount of the oxidizing component according to the fluctuation. apparatus.