EP0417951B1 - Fe-Si-Al alloy magnetic thin film and method of manufacturing the same - Google Patents

Fe-Si-Al alloy magnetic thin film and method of manufacturing the same Download PDF

Info

Publication number
EP0417951B1
EP0417951B1 EP19900309606 EP90309606A EP0417951B1 EP 0417951 B1 EP0417951 B1 EP 0417951B1 EP 19900309606 EP19900309606 EP 19900309606 EP 90309606 A EP90309606 A EP 90309606A EP 0417951 B1 EP0417951 B1 EP 0417951B1
Authority
EP
European Patent Office
Prior art keywords
oxygen
target
thin film
magnetic thin
oxygen concentration
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP19900309606
Other languages
German (de)
French (fr)
Other versions
EP0417951A3 (en
EP0417951A2 (en
Inventor
Kazuhiro C/O Nippon Mining Co. Ltd. Saito
Yukihiko C/O Nippon Mining Co. Ltd. Yashima
Hisakazu C/O Nippon Mining Co. Ltd. Yachi
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Eneos Corp
Original Assignee
Japan Energy Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Japan Energy Corp filed Critical Japan Energy Corp
Publication of EP0417951A2 publication Critical patent/EP0417951A2/en
Publication of EP0417951A3 publication Critical patent/EP0417951A3/en
Application granted granted Critical
Publication of EP0417951B1 publication Critical patent/EP0417951B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F10/00Thin magnetic films, e.g. of one-domain structure
    • H01F10/08Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
    • H01F10/10Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
    • H01F10/12Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys
    • H01F10/14Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing iron or nickel
    • H01F10/142Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing iron or nickel containing Si
    • H01F10/145Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing iron or nickel containing Si containing Al, e.g. SENDUST
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/14Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
    • H01F41/18Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/14Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
    • H01F41/18Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering
    • H01F41/183Sputtering targets therefor

Definitions

  • the present invention relates to an Fe-Si-Al alloy magnetic thin film and to a method of manufacturing this thin film.
  • the film contains, as its main components, Fe Si and Al, and additionally contains oxygen.
  • the method manufactures such an Fe-Si-Al alloy magnetic thin film by effecting sputtering in an inert gas-based atmosphere containing a regulated amount of oxygen gas.
  • One type of alloy magnetic thin film has been drawing attention as a magnetic thin film of a magnetic head capable of meeting such demands.
  • This is a magnetic thin film of a Sendust alloy, an Fe-Si-Al alloy containing Fe, Si and Al as its main components.
  • a Sendust alloy magnetic thin film i.e., an Fe-Si-Al alloy magnetic thin film
  • an Fe-Si-Al alloy magnetic thin film generally has superior magnetic characteristics.
  • the durability of such a magnetic thin film is inferior. Therefore, various proposals have been made to provide Fe-Si-Al alloy magnetic thin films excellent in both magnetic characteristics and durability.
  • Japanese Patent Application Public Disclosure No. 220914/1985 discloses the art of adding 0.005 to 6% by weight (hereinafter abbreviated to "wt%") of oxygen to an Fe-Si-Al alloy magnetic thin film, so as to obtain a magnetic thin film which has both excellent magnetic characteristics and high hardness.
  • the present inventors have conducted many studies and experiments in order to obtain an Fe-Si-Al alloy magnetic thin film which has as excellent magnetic characteristics as that shown in the above-mentioned patent application, but which also has high hardness. As a result, the present inventors have found that, if the amount of oxygen contained in the magnetic thin film is within that wide range from 0.005 to 6 wt% specified in the patent application, the Fe-Si-Al alloy magnetic thin film will not always exhibit excellence in both magnetic characteristics and durability.
  • the present inventors have found that, in order to obtain an Fe-Si-Al alloy magnetic thin film having excellent and superior magnetic characteristics and high hardness, it is of great importance that the amount of oxygen contained in the magnetic thin film be kept within a very limited range from 0.17 to 0.46 wt%.
  • a Sendust alloy magnetic thin film or an Fe-Si-Al alloy magnetic thin film, is formed by sputtering an Fe-Si-Al alloy onto a substrate of crystallized glass or ceramics in an inert gas atmosphere.
  • the oxygen-containing Fe-Si-Al alloy magnetic thin film manufactured by this method is capable of maintaining high magnetic permeability and high hardness while avoiding the risk of a drop in the saturation flux density, of maintaining a coercive force (Hc) of not more than 0.35 Oe, and of maintaining a value ⁇ defined hereafter of less than 0.20 that is indicative of a change in the specific initial magnetic permeability at 1 MHz caused by the application of a certain strain.
  • Hc coercive force
  • the value ⁇ indicates a certain quality of a magnetic film which is very important in determining whether the film is practically usable or not.
  • the magnetic head will not exhibit the performance levels required of a high-vision magnetic head (that is, the maximum value of the normalized output voltage for MP (Metal Powder) tape should exceed 90 [nV 0-p /»m ⁇ turn ⁇ (m/sec)], and the CN (Carrier to Noise) ratio at 19 MHz must be equal to or greater than 58 dB measured with 30 KHz resolution bandwidth).
  • Japanese Patent Application Public Disclosure No. 218821/1985 discloses a method of manufacturing an Fe-Si-Al alloy magnetic thin film by effecting sputtering in an inert gas-based atmosphere containing oxygen.
  • the atmosphere contains 0.01 to 40% by volume of oxygen.
  • the amount of oxygen contained in the inert gas-based atmosphere is less than 400 ppm by volume, there can be cases where the amount of oxygen contained in the resultant magnetic thin film is less than 0.17 wt%. In such cases, the coercive force will exceed 0.35 Oe.
  • the amount of oxygen contained in the inert gas-based atmosphere exceeds 1500 volumetric ppm, there can be cases where the amount of oxygen contained in the resultant magnetic thin film greatly exceeds 0.46 wt%. In such cases, the value ⁇ will be 0.20 or greater.
  • the present inventors have also found that, if 3000 volumetric ppm of oxygen is contained in the inert gas-based atmosphere, the film will peel from the substrate, becoming unusable in practice.
  • the art disclosed in the above-mentioned publication specifies too wide a range of the amount of oxygen in the inert gas-based atmosphere to exclude a practically unusable range and to assure industrial utilization.
  • the conventional art fails to teach or suggest that the oxygen content in the inert gas-based atmosphere must be within a very narrow range in order to effectively manufacture an Fe-Si-Al alloy magnetic film.
  • the present inventors have found that it is possible to effectively manufacture an Fe-Si-Al alloy magnetic thin film containing 0.17 to 0.46 wt% of oxygen only if the amount of oxygen contained in the inert gas-based atmosphere is within a very narrow and specific range.
  • the oxygen concentration in the inert gas-based atmosphere must be 400 to 1500 volumetric ppm.
  • the oxygen concentration in the inert gas-based atmosphere must be adjusted in accordance with the oxygen concentration in the target and set at a suitably low level because the oxygen already contained in the target can influence the inert gas-based atmosphere. For instance, if the target used consists of a normally used sintered target which contains 0.14 wt% of oxygen, the initial oxygen concentration of the inert gas-based atmosphere is set at about 500 volumetric ppm.
  • the present invention has been made on the basis of the above-described novel finding.
  • the magnetic thin film is capable of exhibiting a coercive force (Hc) of not more than 0.35 Oe, and the value ⁇ of less than 0.20.
  • the nub of the present invention resides in an Fe-Si-Al alloy magnetic thin film containing, as its main components, Fe, Si and Al, and additionally containing 0.17 to 0.46 wt% of oxygen.
  • the Fe-Si-Al alloy magnetic thin film containing oxygen within the above-specified range can be very advantageously manufactured by first preparing a sputtering target and an inert gas-based atmosphere having a strictly regulated concentration of oxygen.
  • the oxygen concentration in the inert gas-based atmosphere is set at 400 to 1500 volumetric ppm if the target is a cast product, whereas, if the target is a sintered product, the oxygen concentration is adjusted in accordance with the oxygen concentration in the target and is set at a level lower than the above-mentioned range. For instance, if the sintered target contains 0.14 wt% of oxygen, the oxygen concentration in the inert gas-based atmosphere should preferably be set at about 500 volumetric ppm. Then, sputtering is effected employing the target and the inert gas-based atmosphere.
  • the proportion of the main components Fe, Si and Al in the chemical composition is not particularly specified.
  • the magnetic thin film should preferably contain 4 to 7 wt% of Al, 8 to 12 wt% of Si, and the balance of Fe.
  • a part of Fe more specifically, a part of Fe which is not more than 60 wt% thereof, may be substituted with such elements as Co and Ni.
  • various elements may be added as additives within a range of less than 10 wt% of the magnetic thin film.
  • Examples which may be used as the additives include: Y and other elements in the IIIb group; Ti, Zr, Hf and other elements in the IVb group; V, Nb, Ta and other elements in the Vb group; Cr, Mo, W and other elements in the VIb group; Mn, To, Re and other elements in the VIIb group; La, Ce, Nd, Gd and other elements in the lanthanum series; Cu, Ag, Au and other elements in the Ib group; Ga; In; Ge; Sn; Sb; and Bi.
  • Other types of additives are possible, and such additives are selected in accordance with necessity and are added suitably.
  • the magnetic thin film by the method of the present invention, it is possible to adopt any of the normally conducted various types of sputtering.
  • diode DC glow discharge sputtering, triode DC glow discharge sputtering, RF glow discharge sputtering, magnetron sputtering, or ion beam sputtering may be suitably employed.
  • Fig. 1 schematically shows a DC magnetron sputtering (RF bias application) apparatus suitable for use in carrying out the method according to the present invention.
  • DC sputtering apparatus 30 includes a cathode 32 connected to a high-voltage DC power source 31, and a substrate holder 34 connected to an RF bias power source 33 and electrically insulated.
  • a target 35 is disposed on the cathode 32, while a substrate 11 is supported by the holder 34.
  • the apparatus 30 has a first port 36 through which the interior of the apparatus is vacuum pumped by a vacuum pump (not shown), and a second port 37 through which an inert gas is introduced.
  • Such gas as He, Ne or Ar can be used as the inert gas. Normally, Ar is used.
  • the pressure of the inert gas-based atmosphere is maintained within the range from 1 x 10 ⁇ 4 to 2.0 x 10 ⁇ 1 Torr. (1.33 x 10 ⁇ 4 to 2.67 x 10 ⁇ 1 hPa).
  • oxygen gas is introduced into an inert gas atmosphere, and the oxygen concentration is strictly regulated in such a manner that the oxygen concentration in the inert gas-based atmosphere will be 400 to 1500 volumetric ppm during sputtering. If a casted target which contains only a very small amount of oxygen of the order of 3 to 5 ppm by weight is used as the target 35, the oxygen concentration in the inert gas-based atmosphere will, during sputtering, fall within the same range, i.e., from 400 to 1500 volumetric ppm.
  • the oxygen in the target can, during sputtering, flow into the inert gas-based atmosphere and influence the same. Therefore, in this case, the concentration of oxygen contained in the atmosphere must be adjusted before sputtering in accordance with the oxygen concentration in the target and set at a level lower than the above-described range. For instance, if a sintered target containing 0.14 wt% of oxygen is used, the concentration of the inert gas-based atmosphere is preferably set at about 500 volumetric ppm.
  • oxygen gas is introduced from the second port 37 of the sputtering apparatus 30 together with Ar gas.
  • the present inventors have found as a result of their studies and experiments that, during the introduction, the oxygen-containing Ar gas should preferably be supplied as directed toward the substrate 11. If the oxygen-containing Ar gas is directed toward the target 35, this results in the following disadvantages. Oxide film may adhere to a shield (not shown), thereby making frequent cleaning of the shield necessary. Sputtering may become so unstable that a higher oxygen concentration is necessary to achieve the same effect as in the case where the gas supply is directed toward the substrate 11.
  • the present inventors have conducted various experiments to examine the relationship between the oxygen concentration in the sputtering atmosphere and the oxygen content in the deposited magnetic thin films.
  • a sputtering apparatus such as that shown in Fig. 1, was used, and a plurality of samples of Fe-Si-Al alloy magnetic thin film were each formed with a thickness of 20 »m (i.e., the thickness corresponding to the total thickness of a magnetic film portion of an actual alloy magnetic film) on a high-purity (purity level: 99.9995%) Ni substrate having a thickness of 0.2 mm and a diameter of 50 mm.
  • the film deposition conditions adopted in the experiments are as follows:
  • Inert gas Ar gas Oxygen concentration: 1500 ppm Volume Rate of Flow of Inert Gas: 100 sccm Sputtering Gas Pressure: 5.6 x 10 ⁇ 3 Torr(7.47 x 10 ⁇ 3 hPa) Input power: 500 W Substrate temperature: 60°C Film Deposition Rate: 0.4 »m/min
  • the average of the amounts of oxygen contained in the Fe-Si-Al alloy magnetic thin film samples was 0.40 wt%, and the relative error of analysis was within ⁇ 15%, accounting for 0.06 wt% at most.
  • the oxygen concentration in the inert gas-based atmosphere should be maintained within the range from 400 to 1500 volumetric ppm. This is because, as will be seen from Fig. 3, if the amount of oxygen contained in the inert gas-based atmosphere is less than 400 volumetric ppm, the amount of oxygen contained in the resultant magnetic thin film can be less than 0.17 wt%. In such cases, the coercive force will exceed 0.35 Oe.
  • the amount of oxygen contained in the inert gas-based atmosphere exceeds 1500 volumetric ppm, the amount of oxygen contained in the resultant magnetic thin film can greatly exceed 0.46 wt%. It is clear that, in such cases, the value ⁇ will be 0.20 or greater.
  • Used as the target 35 was a cast target essentially consisting of Si: 11.2 wt%; Al: 0.5 wt%, and Fe: the balance, and containing 5 ppm by weight of oxygen, which cast target had a diameter of 4 inches and a thickness of 4 mm.
  • the substrate 11 consisted of a ceramic substrate containing, as its main components, manganese oxide and nickel oxide. The substrate had dimensions of 0.5 mm x 20 mm x 20 mm, and had mirror-finished surfaces. The substrate 11 and the target 35 were placed in the apparatus with a distance of 50 mm therebetween.
  • An oxygen-containing Ar gas was introduced from an oxygen-containing Ar gas container into the sputtering apparatus while the flow of gas was directed to a position which was 5 mm separated from the substrate 11.
  • the concentration of oxygen in the gas within the apparatus was maintained at a predetermined value.
  • the gas pressure was 5.6 x 10 ⁇ 3 Torr(7.47 x 10 ⁇ 3 hPa), and the volume rate of flow of the gas was 100 sccm.
  • the input power was 500 W, and the substrate was at 60°C.
  • An Fe-Si-Al alloy film was deposited on the substrate 11 at a film deposition rate of 0.4 »m/min through a thickness of 5 »m.
  • the thus obtained alloy film had the composition of Si: 9.0 wt%, Al: 5.0 wt%, and Fe: the balance.
  • the microstructure of the alloy film was examined, it was different from a columnar microstructure of an alloy film deposited in an atmosphere composed of pure Ar.
  • the sputtering atmosphere contained 1500 ppm of oxygen, the resultant alloy film had a dense, fine-grained microstructure.
  • an inter-layer film (insulating film) was deposited on the Fe-Si-Al alloy film.
  • the interlayer film deposition was conducted by using the magnetron sputtering apparatus used in the Fe-Si-Al alloy film deposition, in which an SiO2 target having a diameter of 4 inches (10 cm) and a thickness of 5 mm was disposed.
  • Ar gas alone was introduced into the sputtering apparatus.
  • the Ar gas pressure was 4 x 10 ⁇ 3 Torr (5.33 x 10 ⁇ 3 hPa), and the input RF power was 300 W. Under these conditions, an SiO2 film with a thickness of 0.3 »m was deposited on the alloy film on the substrate.
  • a glass film was deposited by a normal method.
  • the resultant film product was subjected to a forming process, and it was then used in the fabrication of a thin film stacked magnetic head.
  • Fig. 2 shows, in solid lines, changes in the coercive force (Hc) of the Fe-Si-Al alloy magnetic thin film and in the value ⁇ which occurred when the oxygen concentration in the inert gas-based sputtering atmosphere was changed to various values.
  • the coercive force was measured by means of a 50 Hz B-H tracer.
  • the graph shown in Fig. 4 is the summary of the relationship of the coercive force and the value ⁇ with the oxygen concentration in the film. In the summarization, the recurrence formula obtained from Fig. 3 was used.
  • Fe-Si-Al alloy magnetic thin film manufactured in an inert gas-based atmosphere having an oxygen concentration of 400 to 1500 volumetric ppm had good magnetic characteristics.
  • the saturation flux density was 11 kilo-Gauss, and the specific initial permeability at 1 MHz was 3000.
  • the thin film also had a Vickers hardness of 600 kg/mm2, a sufficiently satisfactory level.
  • the oxygen concentration in the film ranged from 0.17 to 0.46 wt%.
  • Soft magnetic film samples and thin film stacked magnetic head samples were produced in the same manner as in Example 1 except that a sintered target was used as the target 35, the sintered target essentially consisting of Si: 11.2 wt%; Al: 5.0 wt%; and Fe: the balance, and containing 0.14 wt% of oxygen.
  • the coercive force and the value ⁇ of the resultant Fe-Si-Al alloy magnetic thin film in relation to the oxygen concentration in the sputtering atmosphere is indicated by broken lines in Fig. 2.
  • Fe-Si-Al alloy magnetic thin film manufactured in an inert gas-based atmosphere having an oxygen concentration of 300 to 800 volumetric ppm had good magnetic characteristics.
  • the saturation flux density was 11.2 kilo-Gauss, and the specific initial permeability at 1 MHz was 3000.
  • the thin film also had a Vickers hardness of 600 kg/mm2, a sufficiently satisfactory level.
  • the target used is a sintered target containing a not-negligible amount of oxygen
  • the oxygen in the target can, during sputtering, flow into the inert gas-based atmosphere and influence the same
  • the initial oxygen concentration in the inert gas-based atmosphere must be adjusted in accordance with the oxygen concentration in the target and set to a level lower than the range adopted in Example 1 where a casted target was used.
  • the Fe-Si-Al alloy magnetic thin film obtained in Example 2 and manufactured in a sputtering atmosphere having an oxygen concentration of 300 to 800 volumetric ppm had its oxygen concentration measured by means of the above-mentioned oxygen-nitrogen analyzing apparatus (a product of LECO; trade name: LECO TC-36). As a result, the oxygen concentration in the film ranged from 0.17 to 0.46 wt%.
  • Example 2 Other experiments were conducted under the same condition as those in Example 2 except that a sintered target containing 0.10 wt% of oxygen was used. As a result, magnetic thin film which was manufactured in an inert gas-based atmosphere having an oxygen concentration of 550 to 1050 volumetric ppm had good magnetic characteristics. If a sintered target is used, the initial oxygen concentration Ca (in volumetric ppm) in the inert gas atmosphere is selected from the range expressed by the following formula: 1175 - (5/8) ⁇ Ct ⁇ Ca ⁇ 1675 - (5/8) ⁇ Ct where Ct represents oxygen concentration (ppm by weight) in the target.
  • an Fe-Si-Al alloy magnetic thin film and a method of manufacturing the same are characterized by the following:
  • the oxygen concentration in the inert gas-based atmosphere during sputtering is strictly regulated so that the amount of oxygen in the resultant Fe-Si-Al alloy magnetic thin film will be specified as being within a very limited range.
  • This regulation enables the provision of an Fe-Si-Al alloy magnetic thin film having a coercive force (Hc) of not more than 0.35 Oe and a value ⁇ of less than 0.20 that indicates a change in the specific initial permeability at 1 MHz caused by application of a certain strain.
  • the thin film is also capable of maintaining high magnetic permeability and high hardness while avoiding the risk of a drop in saturation flux density.

Landscapes

  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Physical Vapour Deposition (AREA)
  • Thin Magnetic Films (AREA)

Description

  • The present invention relates to an Fe-Si-Aℓ alloy magnetic thin film and to a method of manufacturing this thin film. The film contains, as its main components, Fe Si and Aℓ, and additionally contains oxygen. The method manufactures such an Fe-Si-Aℓ alloy magnetic thin film by effecting sputtering in an inert gas-based atmosphere containing a regulated amount of oxygen gas.
  • Recently, in the field of magnetic recording technology, recording density has been improved remarkably. Improved recording density has led to increases in demand for track width reduction in a magnetic head such as a video head or computer head, for increased magnetization saturation of a core material, and for improved magnetic permeability in high-frequency areas.
  • One type of alloy magnetic thin film has been drawing attention as a magnetic thin film of a magnetic head capable of meeting such demands. This is a magnetic thin film of a Sendust alloy, an Fe-Si-Aℓ alloy containing Fe, Si and Aℓ as its main components.
  • A Sendust alloy magnetic thin film, i.e., an Fe-Si-Aℓ alloy magnetic thin film, generally has superior magnetic characteristics. However, the durability of such a magnetic thin film is inferior. Therefore, various proposals have been made to provide Fe-Si-Aℓ alloy magnetic thin films excellent in both magnetic characteristics and durability.
  • For instance, Japanese Patent Application Public Disclosure No. 220914/1985 discloses the art of adding 0.005 to 6% by weight (hereinafter abbreviated to "wt%") of oxygen to an Fe-Si-Aℓ alloy magnetic thin film, so as to obtain a magnetic thin film which has both excellent magnetic characteristics and high hardness.
  • The present inventors have conducted many studies and experiments in order to obtain an Fe-Si-Aℓ alloy magnetic thin film which has as excellent magnetic characteristics as that shown in the above-mentioned patent application, but which also has high hardness. As a result, the present inventors have found that, if the amount of oxygen contained in the magnetic thin film is within that wide range from 0.005 to 6 wt% specified in the patent application, the Fe-Si-Aℓ alloy magnetic thin film will not always exhibit excellence in both magnetic characteristics and durability.
  • Specifically, the present inventors have found that, in order to obtain an Fe-Si-Aℓ alloy magnetic thin film having excellent and superior magnetic characteristics and high hardness, it is of great importance that the amount of oxygen contained in the magnetic thin film be kept within a very limited range from 0.17 to 0.46 wt%.
  • In general, a Sendust alloy magnetic thin film, or an Fe-Si-Aℓ alloy magnetic thin film, is formed by sputtering an Fe-Si-Aℓ alloy onto a substrate of crystallized glass or ceramics in an inert gas atmosphere.
  • In the course of the present inventors' studies into manufacturing, by sputtering, an Fe-Si-Aℓ alloy magnetic thin film containing oxygen, they have found that, if an oxygen gas is introduced into the inert gas atmosphere and in an amount within a very limited range, it is possible suitably to manufacture an Fe-Si-Aℓ alloy magnetic thin film containing the above-specified amount of oxygen.
  • It has been found that the oxygen-containing Fe-Si-Aℓ alloy magnetic thin film manufactured by this method is capable of maintaining high magnetic permeability and high hardness while avoiding the risk of a drop in the saturation flux density, of maintaining a coercive force (Hc) of not more than 0.35 Oe, and of maintaining a value η defined hereafter of less than 0.20 that is indicative of a change in the specific initial magnetic permeability at 1 MHz caused by the application of a certain strain.
  • The value indicating a change in the specific initial permeability at 1 MHz caused by the application of a certain strain (the value will hereinafter be symbolized as "η") is calculated, with the following formula (1) : η = 20 log (»/»₀)
    Figure imgb0001

    from (a) the specific initial permeability »₀ at 1 MHZ when an Fe-Si-Aℓ alloy magnetic thin film sputtered onto a substrate is subjected to no strain and (b) the specific initial permeability » at 1 MHz of smaller value when the magnetic thin film is subjected to either a tensile or a compressive strain of 1 x 10⁻⁴ corresponding to the strain that can be caused by the difference in thermal expansion coefficient between the substrate and the thin film as well as by deformation of the substrate. Thus, the value η indicates a certain quality of a magnetic film which is very important in determining whether the film is practically usable or not.
  • Whether or not the coercive force (Hc) is not more than 0.35 Oe, and whether or not the value η is less than 0.20 matters because if these conditions are not met, the magnetic head will not exhibit the performance levels required of a high-vision magnetic head (that is, the maximum value of the normalized output voltage for MP (Metal Powder) tape should exceed 90 [nV0-p/»m·turn·(m/sec)], and the CN (Carrier to Noise) ratio at 19 MHz must be equal to or greater than 58 dB measured with 30 KHz resolution bandwidth).
  • Japanese Patent Application Public Disclosure No. 218821/1985 discloses a method of manufacturing an Fe-Si-Aℓ alloy magnetic thin film by effecting sputtering in an inert gas-based atmosphere containing oxygen. However, in the sputtering effected in that disclosed method, the atmosphere contains 0.01 to 40% by volume of oxygen.
  • According to the result of certain studies and experiments conducted by the present inventors, if the amount of oxygen contained in the inert gas-based atmosphere is less than 400 ppm by volume, there can be cases where the amount of oxygen contained in the resultant magnetic thin film is less than 0.17 wt%. In such cases, the coercive force will exceed 0.35 Oe. On the other hand, if the amount of oxygen contained in the inert gas-based atmosphere exceeds 1500 volumetric ppm, there can be cases where the amount of oxygen contained in the resultant magnetic thin film greatly exceeds 0.46 wt%. In such cases, the value η will be 0.20 or greater. The present inventors have also found that, if 3000 volumetric ppm of oxygen is contained in the inert gas-based atmosphere, the film will peel from the substrate, becoming unusable in practice.
  • In this way, the art disclosed in the above-mentioned publication specifies too wide a range of the amount of oxygen in the inert gas-based atmosphere to exclude a practically unusable range and to assure industrial utilization. In other words, the conventional art fails to teach or suggest that the oxygen content in the inert gas-based atmosphere must be within a very narrow range in order to effectively manufacture an Fe-Si-Aℓ alloy magnetic film.
  • As discussed above, the present inventors have found that it is possible to effectively manufacture an Fe-Si-Aℓ alloy magnetic thin film containing 0.17 to 0.46 wt% of oxygen only if the amount of oxygen contained in the inert gas-based atmosphere is within a very narrow and specific range.
  • This finding leads to the following. If the sputtering is to be effected by using, as the sputtering target, a cast target which contains substantially no oxygen (i.e., contains only 3 to 5 ppm by weight), the oxygen concentration in the inert gas-based atmosphere must be 400 to 1500 volumetric ppm. If a sintered target which contains a relatively large amount of oxygen is to be used, the oxygen concentration in the inert gas-based atmosphere must be adjusted in accordance with the oxygen concentration in the target and set at a suitably low level because the oxygen already contained in the target can influence the inert gas-based atmosphere. For instance, if the target used consists of a normally used sintered target which contains 0.14 wt% of oxygen, the initial oxygen concentration of the inert gas-based atmosphere is set at about 500 volumetric ppm.
  • The present invention has been made on the basis of the above-described novel finding.
  • It is an object of the present invention to provide an oxygen-containing Fe-Si-Aℓ alloy magnetic thin film having high hardness and excellent durability, the amount of oxygen contained in the magnetic thin film being specified within a specific range. The magnetic thin film is capable of exhibiting a coercive force (Hc) of not more than 0.35 Oe, and the value η of less than 0.20.
  • It is another object of the present invention to provide a method of manufacturing such an oxygen-containing Fe-Si-Aℓ alloy magnetic thin film, the method being adapted strictly to regulate the oxygen concentration in the inert gas-based atmosphere to achieve a suitable oxygen concentration in the atmosphere during sputtering.
  • The above-stated objects are achieved by an Fe-Si-Aℓ alloy magnetic thin film and a method of manufacturing the thin film, both according to the present invention. In brief, the nub of the present invention resides in an Fe-Si-Aℓ alloy magnetic thin film containing, as its main components, Fe, Si and Aℓ, and additionally containing 0.17 to 0.46 wt% of oxygen.
  • The Fe-Si-Aℓ alloy magnetic thin film containing oxygen within the above-specified range can be very advantageously manufactured by first preparing a sputtering target and an inert gas-based atmosphere having a strictly regulated concentration of oxygen. The oxygen concentration in the inert gas-based atmosphere is set at 400 to 1500 volumetric ppm if the target is a cast product, whereas, if the target is a sintered product, the oxygen concentration is adjusted in accordance with the oxygen concentration in the target and is set at a level lower than the above-mentioned range. For instance, if the sintered target contains 0.14 wt% of oxygen, the oxygen concentration in the inert gas-based atmosphere should preferably be set at about 500 volumetric ppm. Then, sputtering is effected employing the target and the inert gas-based atmosphere.
  • The invention will now be explained in more detail in the following description, which is given by way of example only, and with reference to the accompanying drawings in which:
    • Fig. 1 is a schematic illustration of a sputtering apparatus suitable for use in carrying out a manufacturing method according to the present invention;
    • Fig. 2 is a graph showing the coercive force and the value η indicative of a change in the specific initial permeability at 1 MHz caused by a strain, both in relation to the oxygen concentration in the inert gas-based atmosphere;
    • Fig. 3 is a graph showing the amount of oxygen contained in magnetic thin film in relation to the oxygen concentration in the inert gas-based atmosphere and;
    • Fig. 4 is a graph showing the coercive force and the value η in relation to the oxygen concentration in the film.
  • Detailed explanations will first be given of an Fe-Si-Aℓ alloy magnetic thin film according to the present invention. If the amount of oxygen contained in the magnetic thin film is less than 0.17 wt%, the coercive force will exceed 0.35 Oe. On the other hand, if the amount of oxygen contained in the magnetic thin film exceeds 0.46 wt%, the value η will be 0.20 or greater.
  • The proportion of the main components Fe, Si and Aℓ in the chemical composition is not particularly specified. However, the magnetic thin film should preferably contain 4 to 7 wt% of Aℓ, 8 to 12 wt% of Si, and the balance of Fe.
  • If desired, a part of Fe, more specifically, a part of Fe which is not more than 60 wt% thereof, may be substituted with such elements as Co and Ni. Further, in order to improve the corrosion resistance and the wear resistance of the magnetic thin film, various elements may be added as additives within a range of less than 10 wt% of the magnetic thin film. Examples which may be used as the additives include: Y and other elements in the IIIb group; Ti, Zr, Hf and other elements in the IVb group; V, Nb, Ta and other elements in the Vb group; Cr, Mo, W and other elements in the VIb group; Mn, To, Re and other elements in the VIIb group; La, Ce, Nd, Gd and other elements in the lanthanum series; Cu, Ag, Au and other elements in the Ib group; Ga; In; Ge; Sn; Sb; and Bi. Other types of additives are possible, and such additives are selected in accordance with necessity and are added suitably.
  • Next, detailed explanations will be given of a method of manufacturing an Fe-Si-Aℓ alloy magnetic thin film containing a specified amount of oxygen according to the present invention.
  • In order to suitably manufacture the magnetic thin film by the method of the present invention, it is possible to adopt any of the normally conducted various types of sputtering. For instance, diode DC glow discharge sputtering, triode DC glow discharge sputtering, RF glow discharge sputtering, magnetron sputtering, or ion beam sputtering may be suitably employed.
  • Fig. 1 schematically shows a DC magnetron sputtering (RF bias application) apparatus suitable for use in carrying out the method according to the present invention.
  • DC sputtering apparatus 30 includes a cathode 32 connected to a high-voltage DC power source 31, and a substrate holder 34 connected to an RF bias power source 33 and electrically insulated. A target 35 is disposed on the cathode 32, while a substrate 11 is supported by the holder 34. The apparatus 30 has a first port 36 through which the interior of the apparatus is vacuum pumped by a vacuum pump (not shown), and a second port 37 through which an inert gas is introduced.
  • Such gas as He, Ne or Ar can be used as the inert gas. Normally, Ar is used. During sputtering, the pressure of the inert gas-based atmosphere is maintained within the range from 1 x 10⁻⁴ to 2.0 x 10⁻¹ Torr. (1.33 x 10⁻⁴ to 2.67 x 10⁻¹ hPa).
  • According to the present invention, oxygen gas is introduced into an inert gas atmosphere, and the oxygen concentration is strictly regulated in such a manner that the oxygen concentration in the inert gas-based atmosphere will be 400 to 1500 volumetric ppm during sputtering. If a casted target which contains only a very small amount of oxygen of the order of 3 to 5 ppm by weight is used as the target 35, the oxygen concentration in the inert gas-based atmosphere will, during sputtering, fall within the same range, i.e., from 400 to 1500 volumetric ppm. On the other hand, if a sintered target containing a not-negligible amount of oxygen is used, the oxygen in the target can, during sputtering, flow into the inert gas-based atmosphere and influence the same. Therefore, in this case, the concentration of oxygen contained in the atmosphere must be adjusted before sputtering in accordance with the oxygen concentration in the target and set at a level lower than the above-described range. For instance, if a sintered target containing 0.14 wt% of oxygen is used, the concentration of the inert gas-based atmosphere is preferably set at about 500 volumetric ppm.
  • In practice, oxygen gas is introduced from the second port 37 of the sputtering apparatus 30 together with Ar gas. The present inventors have found as a result of their studies and experiments that, during the introduction, the oxygen-containing Ar gas should preferably be supplied as directed toward the substrate 11. If the oxygen-containing Ar gas is directed toward the target 35, this results in the following disadvantages. Oxide film may adhere to a shield (not shown), thereby making frequent cleaning of the shield necessary. Sputtering may become so unstable that a higher oxygen concentration is necessary to achieve the same effect as in the case where the gas supply is directed toward the substrate 11.
  • The present inventors have conducted various experiments to examine the relationship between the oxygen concentration in the sputtering atmosphere and the oxygen content in the deposited magnetic thin films. In those experiments, a sputtering apparatus, such as that shown in Fig. 1, was used, and a plurality of samples of Fe-Si-Aℓ alloy magnetic thin film were each formed with a thickness of 20 »m (i.e., the thickness corresponding to the total thickness of a magnetic film portion of an actual alloy magnetic film) on a high-purity (purity level: 99.9995%) Ni substrate having a thickness of 0.2 mm and a diameter of 50 mm. The film deposition conditions adopted in the experiments are as follows:
  • Film Deposition Conditions:
  • Inert gas: Ar gas
    Oxygen concentration: 1500 ppm
    Volume Rate of Flow of Inert Gas: 100 sccm
    Sputtering Gas Pressure: 5.6 x 10⁻³ Torr(7.47 x 10⁻³ hPa)
    Input power: 500 W
    Substrate temperature: 60°C
    Film Deposition Rate: 0.4 »m/min
  • Target:
    Cast target (Si: 11.2 wt%, Aℓ: 5.0 wt%, and
    Fe: the balance, oxygen content: 5 ppm by weight)
  • When the plurality of alloy magnetic thin film samples were deposited, the amount of oxygen contained in each Fe-Si-Aℓ alloy magnetic thin film sample deposited on the Ni substrate was examined by means of an oxygen-nitrogen analyzing apparatus (a product of LECO; trade name: LECO TC-36) by an inert gas fusion method.
  • As a result, the average of the amounts of oxygen contained in the Fe-Si-Aℓ alloy magnetic thin film samples was 0.40 wt%, and the relative error of analysis was within ±15%, accounting for 0.06 wt% at most.
  • Next, two other film samples were deposited by adopting the same film deposition conditions as above except that the oxygen concentration was changed to 400 ppm and 750 ppm. The formed film samples were analyzed in the same manner. As a result, the Fe-Si-Aℓ alloy magnetic thin film samples respectively contained 0.20 wt% of oxygen and 0.31 wt% of oxygen. The analysis relative error was estimated to be within ±15%.
  • The results of the above-described experiments were analyzed. As a result, it has been found that, as far as those experiments are concerned, the following formula best approximates the relationship between the oxygen content (expressed as y (wt%) in the formula) in the Fe-Si-Aℓ alloy magnetic thin film and the oxygen concentration (x (wt%)) in the sputtering atmosphere. This relationship is also shown in Fig. 3. y = -0.70 + 0.35 logx
    Figure imgb0002

       (coefficient of correlation = 0.99
       the value of y has a variation range of ±15%)
  • From the above-described results of the experiments, it will be understood that, when the amount of oxygen contained in the inert gas-based sputtering atmosphere is 400 volumetric ppm, the amount of oxygen in the resultant magnetic thin film is 0.17 to 0.23 wt%, whereas when the amount of oxygen contained in the inert gas-based sputtering atmosphere is 1500 volumetric ppm, the amount of oxygen in the resultant magnetic thin film is 0.34 to 0.46 wt%. It has also been found that these results of the experiments can be sufficiently supported by a lot of other studies and experiments on alloy magnetic film conducted by the present inventors in view of practical use.
  • From the above-described studies and experiments of the present inventors, therefore, it has been found that when a cast target is used, it is of importance that the oxygen concentration in the inert gas-based atmosphere should be maintained within the range from 400 to 1500 volumetric ppm. This is because, as will be seen from Fig. 3, if the amount of oxygen contained in the inert gas-based atmosphere is less than 400 volumetric ppm, the amount of oxygen contained in the resultant magnetic thin film can be less than 0.17 wt%. In such cases, the coercive force will exceed 0.35 Oe. On the other hand, if the amount of oxygen contained in the inert gas-based atmosphere exceeds 1500 volumetric ppm, the amount of oxygen contained in the resultant magnetic thin film can greatly exceed 0.46 wt%. It is clear that, in such cases, the value η will be 0.20 or greater.
  • The present invention will now be described by way of the following non-limiting examples.
  • Example 1:
  • Various Fe-Si-Aℓ alloy magnetic thin film samples were each manufactured in the following manner by using the sputtering apparatus shown in Fig. 1.
  • Used as the target 35 was a cast target essentially consisting of Si: 11.2 wt%; Aℓ: 0.5 wt%, and Fe: the balance, and containing 5 ppm by weight of oxygen, which cast target had a diameter of 4 inches and a thickness of 4 mm. The substrate 11 consisted of a ceramic substrate containing, as its main components, manganese oxide and nickel oxide. The substrate had dimensions of 0.5 mm x 20 mm x 20 mm, and had mirror-finished surfaces. The substrate 11 and the target 35 were placed in the apparatus with a distance of 50 mm therebetween.
  • An oxygen-containing Ar gas was introduced from an oxygen-containing Ar gas container into the sputtering apparatus while the flow of gas was directed to a position which was 5 mm separated from the substrate 11. The concentration of oxygen in the gas within the apparatus was maintained at a predetermined value. At this time, the gas pressure was 5.6 x 10⁻³ Torr(7.47 x 10⁻³ hPa), and the volume rate of flow of the gas was 100 sccm.
  • Then, sputtering was done. The input power was 500 W, and the substrate was at 60°C. An Fe-Si-Aℓ alloy film was deposited on the substrate 11 at a film deposition rate of 0.4 »m/min through a thickness of 5 »m. The thus obtained alloy film had the composition of Si: 9.0 wt%, Aℓ: 5.0 wt%, and Fe: the balance. When the microstructure of the alloy film was examined, it was different from a columnar microstructure of an alloy film deposited in an atmosphere composed of pure Ar. When, in Example 1, the sputtering atmosphere contained 1500 ppm of oxygen, the resultant alloy film had a dense, fine-grained microstructure.
  • Thereafter, an inter-layer film (insulating film) was deposited on the Fe-Si-Aℓ alloy film. The interlayer film deposition was conducted by using the magnetron sputtering apparatus used in the Fe-Si-Aℓ alloy film deposition, in which an SiO₂ target having a diameter of 4 inches (10 cm) and a thickness of 5 mm was disposed. Ar gas alone was introduced into the sputtering apparatus. At this time, the Ar gas pressure was 4 x 10⁻³ Torr (5.33 x 10⁻³ hPa), and the input RF power was 300 W. Under these conditions, an SiO₂ film with a thickness of 0.3 »m was deposited on the alloy film on the substrate.
  • The above-described operations were repeatedly conducted four times so as to subsequently deposit alloy films overlying on and alternating with inter-layer insulating films. As a result, a soft magnetic film having a total thickness of 20 »m was obtained, which film was then heat treated.
  • Further, on the thus obtained soft magnetic film, a glass film was deposited by a normal method. The resultant film product was subjected to a forming process, and it was then used in the fabrication of a thin film stacked magnetic head.
  • Fig. 2 shows, in solid lines, changes in the coercive force (Hc) of the Fe-Si-Aℓ alloy magnetic thin film and in the value η which occurred when the oxygen concentration in the inert gas-based sputtering atmosphere was changed to various values. The coercive force was measured by means of a 50 Hz B-H tracer.
  • It will be understood from Fig. 2 that if the amount of oxygen contained in the inert-gas based atmosphere is less than 400 volumetric ppm, the coercive force exceeds 0.35 Oe, whereas if that amount of oxygen exceeds 1500 volumetric ppm, the value η becomes 0.20 or greater. When that amount of oxygen was 3000 volumetric ppm, the film peeled from the substrate.
  • The graph shown in Fig. 4 is the summary of the relationship of the coercive force and the value η with the oxygen concentration in the film. In the summarization, the recurrence formula obtained from Fig. 3 was used.
  • It will be understood from Fig. 4 that, if a range of ±15% is allowed for relative error in the analysis of the oxygen concentration in the film, the oxygen concentrations in the film that make the coercive force not more than 0.35 Oe and the value η less than 0.20 range from 0.17 to 0.46 wt%.
  • Fe-Si-Aℓ alloy magnetic thin film manufactured in an inert gas-based atmosphere having an oxygen concentration of 400 to 1500 volumetric ppm had good magnetic characteristics. In particular, the saturation flux density was 11 kilo-Gauss, and the specific initial permeability at 1 MHz was 3000. The thin film also had a Vickers hardness of 600 kg/mm², a sufficiently satisfactory level.
  • When the amount of oxygen contained in the Fe-Si-Aℓ alloy magnetic thin film manufactured in the sputtering atmosphere having an oxygen concentration of 400 to 1500 volumetric ppm was measured by means of the above-mentioned oxygen-nitrogen analyzing apparatus (a product of LECO; trade name: LECO TC-36), the oxygen concentration in the film ranged from 0.17 to 0.46 wt%.
  • Example 2:
  • Soft magnetic film samples and thin film stacked magnetic head samples were produced in the same manner as in Example 1 except that a sintered target was used as the target 35, the sintered target essentially consisting of Si: 11.2 wt%; Aℓ: 5.0 wt%; and Fe: the balance, and containing 0.14 wt% of oxygen. The coercive force and the value η of the resultant Fe-Si-Aℓ alloy magnetic thin film in relation to the oxygen concentration in the sputtering atmosphere is indicated by broken lines in Fig. 2.
  • It will be understood from Fig. 2 that if the amount of oxygen contained in the inert-gas based atmosphere is less than 300 volumetric ppm, the coercive force exceeds 0.35 Oe, whereas if that amount of oxygen exceeds 800 volumetric ppm, the value η becomes 0.20 or greater. When that amount of oxygen was 2000 volumetric ppm, the film peeled from the substrate.
  • Fe-Si-Aℓ alloy magnetic thin film manufactured in an inert gas-based atmosphere having an oxygen concentration of 300 to 800 volumetric ppm had good magnetic characteristics. In particular, the saturation flux density was 11.2 kilo-Gauss, and the specific initial permeability at 1 MHz was 3000. The thin film also had a Vickers hardness of 600 kg/mm², a sufficiently satisfactory level.
  • When, as in the case of Example 2, the target used is a sintered target containing a not-negligible amount of oxygen, because the oxygen in the target can, during sputtering, flow into the inert gas-based atmosphere and influence the same, the initial oxygen concentration in the inert gas-based atmosphere must be adjusted in accordance with the oxygen concentration in the target and set to a level lower than the range adopted in Example 1 where a casted target was used.
  • The Fe-Si-Aℓ alloy magnetic thin film obtained in Example 2 and manufactured in a sputtering atmosphere having an oxygen concentration of 300 to 800 volumetric ppm had its oxygen concentration measured by means of the above-mentioned oxygen-nitrogen analyzing apparatus (a product of LECO; trade name: LECO TC-36). As a result, the oxygen concentration in the film ranged from 0.17 to 0.46 wt%.
  • Other experiments were conducted under the same condition as those in Example 2 except that a sintered target containing 0.10 wt% of oxygen was used. As a result, magnetic thin film which was manufactured in an inert gas-based atmosphere having an oxygen concentration of 550 to 1050 volumetric ppm had good magnetic characteristics. If a sintered target is used, the initial oxygen concentration Ca (in volumetric ppm) in the inert gas atmosphere is selected from the range expressed by the following formula: 1175 - (5/8) · Ct ≦ Ca ≦ 1675 - (5/8) · Ct
    Figure imgb0003

       where Ct represents oxygen concentration (ppm by weight) in the target.
  • As has been described above, an Fe-Si-Aℓ alloy magnetic thin film and a method of manufacturing the same, both according to the present invention, are characterized by the following: The oxygen concentration in the inert gas-based atmosphere during sputtering is strictly regulated so that the amount of oxygen in the resultant Fe-Si-Aℓ alloy magnetic thin film will be specified as being within a very limited range. This regulation enables the provision of an Fe-Si-Aℓ alloy magnetic thin film having a coercive force (Hc) of not more than 0.35 Oe and a value η of less than 0.20 that indicates a change in the specific initial permeability at 1 MHz caused by application of a certain strain. The thin film is also capable of maintaining high magnetic permeability and high hardness while avoiding the risk of a drop in saturation flux density.

Claims (7)

  1. An Fe-Si-Aℓ alloy magnetic thin film containing, as the main components thereof, Fe, Aℓ and Si, and additionally containing 0.17 to 0.46% by weight of oxygen, the alloy having a coercive force (Hc) of not more than 0.35 Oe and a strain sensitivity (η) of less than 0.20 dB.
  2. A film according to claim 1, which contains 4 to 7 wt % Aℓ and 8 to 12% Si.
  3. A film according to claim 1 or claim 2, which contains Co and/or Ni, for instance in an amount up to about 52 wt % of the film.
  4. A film according to claim 1, 2 or 3, wnich contains in an amount of less than 10 wt % of the film, one or more elements selected from: Y; Ti, Zr, Hf; V, Nb, Ta; Cr, Mo, W; Mn, Tc, Re; La, Ce, Nd, Gd, Cu, Ag, Au; Ga; In; Ge; Sn; Sb; Bi.
  5. A method of manufacturing an Fe-Si-Aℓ alloy magnetic thin film according to any one of claims 1 to 4 comprising the steps of:
       preparing a sputtering target and an inert gas-based atmosphere having a strictly regulated concentration of oxygen, the oxygen concentration of said inert gas-based atmosphere being set at 400 to 1500 volumetric ppm if said target is a cast target, whereas, if said target is a sintered target, said oxygen concentration is adjusted in accordance with the oxygen concentration in said target and set at a level lower than the above-mentioned range; and
       effecting sputtering employing said target and said inert gas-based atmosphere.
  6. A method according to claim 5, wherein the target is a sintered target and the initial oxygen concentration in the inert atmosphere (Ca) in volumetric ppm is set such that: 1175 - (5/8) x Ct ≦ Ca ≦ 1675 - (5/8) x Ct
    Figure imgb0004
    where Ct is the oxygen concentration in the target in ppm by weight.
  7. A method according to claim 5, wherein the target is a sintered target having an initial oxygen concentration of 0.14 wt % and the oxygen concentration in the inert atmosphere is set to 300 to 800 volumetric ppm.
EP19900309606 1989-09-12 1990-09-03 Fe-Si-Al alloy magnetic thin film and method of manufacturing the same Expired - Lifetime EP0417951B1 (en)

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
JP236624/89 1989-09-12
JP23662489 1989-09-12
JP49527/90 1990-03-02
JP4952790 1990-03-02
JP2140261A JPH088169B2 (en) 1989-09-12 1990-05-30 Method for producing Fe-Si-Al alloy magnetic thin film
JP140261/90 1990-05-30

Publications (3)

Publication Number Publication Date
EP0417951A2 EP0417951A2 (en) 1991-03-20
EP0417951A3 EP0417951A3 (en) 1992-01-22
EP0417951B1 true EP0417951B1 (en) 1994-06-15

Family

ID=27293668

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19900309606 Expired - Lifetime EP0417951B1 (en) 1989-09-12 1990-09-03 Fe-Si-Al alloy magnetic thin film and method of manufacturing the same

Country Status (3)

Country Link
EP (1) EP0417951B1 (en)
JP (1) JPH088169B2 (en)
DE (1) DE69009917T2 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100430464B1 (en) * 1999-12-28 2004-05-10 쇼꾸바이 카세이 고교 가부시키가이샤 Method of forming a silica-containing coating film with a low dielectric constant and semiconductor substrate coated with such a film
JP5554420B2 (en) * 2011-09-30 2014-07-23 Jx日鉱日石金属株式会社 Fe-Al alloy sputtering target

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60218821A (en) * 1984-04-14 1985-11-01 Sony Corp Manufacture of fe-al-si system alloy thin film
JPS60220914A (en) * 1984-04-18 1985-11-05 Sony Corp Magnetic thin film
JPS6324060A (en) * 1986-04-25 1988-02-01 Nippon Kokan Kk <Nkk> Target of sputtering device
JPS63188921A (en) * 1987-02-02 1988-08-04 Nkk Corp Manufacture of soft magnetic sputtering target
JPS6424403A (en) * 1987-07-21 1989-01-26 Sony Corp Soft magnetic thin film

Also Published As

Publication number Publication date
DE69009917T2 (en) 1994-10-20
EP0417951A3 (en) 1992-01-22
DE69009917D1 (en) 1994-07-21
JPH03278408A (en) 1991-12-10
EP0417951A2 (en) 1991-03-20
JPH088169B2 (en) 1996-01-29

Similar Documents

Publication Publication Date Title
EP0288316B1 (en) Compositionally modulated, nitrided alloy films and method for making the same
EP0114076A2 (en) Magnetic head
US5976326A (en) Method of sputtering selected oxides and nitrides for forming magnetic media
EP0008328B1 (en) Amorphous magnetic films and a method of making such films
EP0350940B1 (en) Method and apparatus for producing a magnetic recording medium
EP0105137A1 (en) Corrosion-resistant and wear-resistant amorphous alloy and a method for preparing the same
EP0159028B1 (en) Magnetic thin film
US5262248A (en) Soft magnetic alloy films
US4969962A (en) Magnetic alloys for magnetic head
EP0417951B1 (en) Fe-Si-Al alloy magnetic thin film and method of manufacturing the same
US5478416A (en) Magnetic alloy
US5182690A (en) Fe-n-based soft magnetic thin films and magnetic heads using such films
EP0298840B1 (en) Magnetic recording medium and manufacturing method thereof
US6746776B1 (en) Laminated structure, and manufacturing method thereof
EP0273195A2 (en) A method of making a thin magnetic pole piece
EP0183120B1 (en) Magnetic recording member
EP0430504A2 (en) Soft magnetic alloy films
JP2996553B2 (en) Soft magnetic alloy thin film
EP0413354A1 (en) Sputtering target for DC magnetron reactive sputtering, process for forming thin layer by use of the target, and optical disk having a layer formed by the process
US5198309A (en) Magnetic recording member
KR930002479B1 (en) Magnetic head and method of producing the same
JP2586050B2 (en) Method for manufacturing composite magnetic head
JPH0744107B2 (en) Soft magnetic thin film
JP3020245B2 (en) Magnetron sputtering method and method for manufacturing magnetic recording medium
JPH02138463A (en) Target material for sputtering

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19901228

AK Designated contracting states

Kind code of ref document: A2

Designated state(s): DE FR GB

PUAL Search report despatched

Free format text: ORIGINAL CODE: 0009013

AK Designated contracting states

Kind code of ref document: A3

Designated state(s): DE FR GB

17Q First examination report despatched

Effective date: 19930721

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: JAPAN ENERGY CORPORATION

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): DE FR GB

REF Corresponds to:

Ref document number: 69009917

Country of ref document: DE

Date of ref document: 19940721

ET Fr: translation filed
PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 19960823

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 19960829

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 19961120

Year of fee payment: 7

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19970903

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: THE PATENT HAS BEEN ANNULLED BY A DECISION OF A NATIONAL AUTHORITY

Effective date: 19970930

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 19970903

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19980603

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST