JPH06228716A - Soft-magnetic alloy film - Google Patents

Abstract

PURPOSE:To provide a soft-magnetic alloy film excellent in soft-magnetic properties, thermal stability, and corrosion resistance. CONSTITUTION:The alloy of this invention is a soft-magnetic alloy film having a composition represented by FeaLfMcBdCe, (Fe1-bXb)aLfMcBdCe, FeaYgMcBdCe, (Fe1-bXb)aYgMcBdCe, and (Fe1-bXb)aYgLfMcBdCe. In the above composition, L is at least one or >=2 elements among Ti, V, Mo, and W, M is at least one or >=2 elements among Zr, Nb, Hf, and Ta, X is Co and/or Ni, and Y is at least one or >=2 elements among Cr, Cu, Ru, Rh, Pd, Ag, Ir, Pt, and Au.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION The present invention relates to a magnetic disk device, V
The present invention relates to a core material of a magnetic head used for TR and the like, and particularly to a soft magnetic alloy film having high magnetic permeability, low coercive force, low magnetostriction, high saturation magnetic flux density, corrosion resistance and the like.

[0002]

2. Description of the Related Art With increasing recording density in the field of magnetic recording, soft magnetic thin film materials for magnetic heads, particularly metal-in-gap heads, thin film magnetic heads, etc., are required to have high saturation magnetic flux density. Further, there are some cases in which gap formation or the like needs to be performed by glass welding, and thermal stability capable of withstanding high temperatures in the glass welding process has also been demanded.

The characteristics generally required in a soft magnetic thin film for a magnetic head are as follows. 1. High saturation magnetic flux density (hereinafter referred to as Bs). 2. High magnetic permeability (hereinafter referred to as μ). 3. Low coercive force (hereinafter referred to as Hc). 4. The magnetostriction constant (hereinafter referred to as λs) is small. 5. The soft magnetic characteristics are thermally stable.

Various thin films have been developed so far in order to obtain a soft magnetic thin film satisfying these characteristics. As the conventional soft magnetic thin film, an Fe-Si-Al-based alloy (Sendust), an Fe-Ni-based alloy (Permalloy), or a Co-based alloy as found in JP-A-1-125911, JP-A-1-181503, or the like. There are amorphous alloys and the like.

[0005]

However, although the sendust has excellent soft magnetic characteristics, it has a Bs of 11K.
G has a low defect. Permalloy also has a low Bs of 10 KG, which deteriorates the soft magnetic characteristics at a high temperature in the glass welding process, and also lowers the magnetic permeability in the high frequency band due to the low electric resistance. Also, in Co-based amorphous alloys, Bs
9KG, it is possible to weld with a low melting point glass, but it is difficult to weld at 600 ° C. or higher, and a medium to high melting point glass excellent in environmental resistance cannot be used.

Further, in order to improve the above-mentioned drawbacks of the soft magnetic thin film, the applicant of the present invention has proposed Fe in Japanese Patent Application No. 3-131977.
A -M-B-C type soft magnetic alloy thin film was proposed, but its corrosion resistance was insufficient and there was a problem in the environment resistance.

The present invention has been made in view of the above problems, and an object thereof is to provide a soft magnetic alloy film having both good soft magnetic characteristics and thermal stability.

[0008]

In order to solve the above-mentioned problems, the invention according to claim 1 has a metal structure formed by subjecting an alloy film to a heat treatment, which basically has an average crystal grain size of 0.0.
It is a soft magnetic alloy film composed of crystal grains of 8 μm or less, and its composition formula is Fe _a L _f M _c B _d C _e .

However, L is at least one or more of Ti, V, Mo and W, and M is Zr, Nb, Hf and T.
a is at least one element or two or more elements, and the composition range thereof in atomic% is 70 ≦ a ≦ 90, 5 ≦ c ≦ 15,
0.5 ≦ d ≦ 15, 0.5 ≦ e ≦ 15, 0.1 ≦ f ≦ 1
5, 1 ≦ d + e ≦ 20.

In order to solve the above-mentioned problems, the invention described in claim 2 is a soft structure in which a metal structure formed by subjecting an alloy film to heat treatment is basically composed of crystal grains having an average crystal grain size of 0.08 μm or less. It is a magnetic alloy film and its composition formula is (F
e _1-b X _b ) _a L _f M _c B _d C _e .

However, X is one or two of Co and Ni.
, L is at least one or more of Ti, V, Mo and W, M is at least one or more of Zr, Nb, Hf and Ta, and the composition range is b
≤0.05, in atomic% 70≤a≤90, 5≤c≤15,
0.5 ≦ d ≦ 15, 0.5 ≦ e ≦ 15, 0.1 ≦ f ≦ 1
5, 1 ≦ d + e ≦ 20.

In order to solve the above-mentioned problems, the invention described in claim 3 is a soft structure in which a metal structure formed by subjecting an alloy film to heat treatment is basically composed of crystal grains having an average crystal grain size of 0.08 μm or less. It is a magnetic alloy film and its composition formula is Fe.
It is obtained by a _{a Y g M c B d C} e.

However, Y is Cr, Cu, Ru, Rh, P
At least one or more elements selected from d, Ag, Ir, Pt, and Au, M is at least one element or two or more elements selected from Zr, Nb, Hf, and Ta, and the composition range is 70% by atomic%. ≦ a ≦ 90, 5 ≦ c ≦ 15, 0.5 ≦ d ≦ 1
5, 0.5 ≦ e ≦ 15, 0.1 ≦ g ≦ 10, 1 ≦ d + e
≦ 20.

In order to solve the above-mentioned problems, the invention according to claim 4 is a soft structure in which a metal structure formed by subjecting an alloy film to heat treatment is basically composed of crystal grains having an average crystal grain size of 0.08 μm or less. It is a magnetic alloy film and its composition formula is (F
It is obtained by the _{e 1-b X b) a} Y g M c B d C e.

However, X is one or two of Co and Ni.
Seed, Y is Cr, Cu, Ru, Rh, Pd, Ag, Ir,
At least one or more of Pt and Au, and M is at least one or more of Zr, Nb, Hf, and Ta, the composition range of which is b ≦ 0.05 and 70% by atom%. ≦ a ≦ 90, 5 ≦ c ≦ 15, 0.5 ≦ d ≦ 1
5, 0.5 ≦ e ≦ 15, 0.1 ≦ g ≦ 10, 1 ≦ d + e
≦ 20.

The invention according to claim 5 is a soft magnetic alloy film, the metal structure of which is produced by heat-treating the alloy film, and is basically composed of crystal grains having an average crystal grain size of 0.08 μm or less. The formula is (Fe _1-b X _b ) _a Y _g L _f M _c B
_d C _e .

However, X is one or two of Co and Ni.
Seed, Y is Cr, Cu, Ru, Rh, Pd, Ag, Ir,
At least one or two or more of Pt and Au, L is at least one or two or more of Ti, V, Mo and W, and M is at least one or two or more of Zr, Nb, Hf and Ta. Element and its composition range is b ≦ 0.0
5, in atomic% 70 ≦ a ≦ 90, 5 ≦ c ≦ 15, 0.5 ≦
d ≦ 15, 0.5 ≦ e ≦ 15, 0.1 ≦ f ≦ 15, 0.
1 ≦ g ≦ 10 and 1 ≦ d + e ≦ 20.

The invention according to claim 6 is the above-mentioned claim 1,
The soft magnetic alloy film described in 2, 3, 4 or 5 is a soft magnetic alloy film containing an amorphous phase.

The present invention will be described in more detail below. The reasons for limiting the compositions of the soft magnetic alloy film of the present invention and the reasons for adding them are as follows.

Fe is a main component and an element that plays a role in magnetism. In order to obtain soft magnetic characteristics, the content needs to be 90 atomic% or less, and in order to obtain Bs of 10 KG or more, 70 atomic% or more is required.

X (= Co, Ni) is an element added by substituting Fe for adjusting the magnetostriction. As will be described later, when X is not added or when the total amount of B and C is relatively small, the magnetostriction. Is a negative value. In this case, by adding X, it is possible to obtain a value of 10 ⁻⁷ . Since X is also an element that plays a role in magnetism, the phenomenon of Bs can be suppressed low. However, if too much is added, the magnetostriction becomes too large and it becomes difficult to obtain soft magnetic characteristics, so it is necessary to be 5 atomic% or less. When the heat treatment temperature is relatively low and the total amount of B and C is relatively large, it is not necessary to add X.

M (= Ti, V, Mo, W) is for facilitating obtaining the amorphous phase in a state prepared by vapor phase quenching (state before heat treatment) in order to improve soft magnetic characteristics. ,is necessary. 5 atom% or more to maintain soft magnetic properties 1
It must be 5 atomic% or less. If 15 atomic% or more is added, an amorphous phase is obtained, but good soft magnetic characteristics cannot be obtained even if heat treatment is performed.

B has the effect of improving the soft magnetic characteristics, the effect of easily obtaining an amorphous phase, the effect of suppressing the formation of a compound phase which adversely affects the soft magnetic characteristics when heat treatment is applied, and Fe as a main component. And b. c. It is considered to have the effect of suppressing c-grain growth. To obtain good soft magnetic properties,
It is necessary to be 0.5 at% or more and 15 at% or less.

C has the effect of making it easier to obtain an amorphous phase in order to improve the soft magnetic characteristics, and b. c. It has the effect of making the precipitation of c uniform. In order to obtain good soft magnetic characteristics, it is necessary to set the content to 0.5 at% or more and 15 at% or less.

By adding B and C in combination, b.
c. The precipitation of the c phase is made uniform, the growth of the precipitated crystal grains is suppressed, and the structure becomes a fine crystal grain structure, and good soft magnetic characteristics can be obtained in a relatively wide composition range. It should be noted that if the shipping costs of B and C are 20 atomic% or more, amorphous can be obtained by as depo, but good soft magnetic properties cannot be obtained even by heat treatment, so the total amount of B and C is 20 atomic%. There is a need to.

L (= Ti, V, Mo, W) is necessary in order to improve the soft magnetic characteristics, and to facilitate obtaining an amorphous phase in the state of being prepared by vapor phase quenching.

Y (= Cr, Cu, Ru, Rh, Pd, A
g, Ir, Pt, Au) has a function of improving the corrosion resistance of the film. In order not to significantly deteriorate the saturation magnetic flux density and the soft magnetic characteristics, the content needs to be 10 atomic% or less.

[0028]

EXAMPLES The thin films of the following examples were prepared by using an RF bipolar sputtering device on a Fe target to form Co, Ni, Nb, Hf,
Ta, B, C (graphite) Ti, V, Mo, W, C
A composite target in which r, Ru, and Rh pellets were appropriately selected and arranged was sputtered using Ar gas to form a film having a thickness of 5 to 6 μm. Substrate is 4mm x 2
A 4 mm crystallized glass substrate was used.

Various heat treatments were applied to each of the obtained alloy films to examine the influence of the composition of the alloy film on μ, Hc, λs and Bs. All the heat treatments were performed in the absence of a magnetic field, the temperature was raised to the set temperature for 40 minutes, kept at the set temperature for 20 minutes, and lowered from the set temperature to room temperature at 1.5 ° C./min. Also,
The film structure at that time was examined by using an X-ray diffractometer using Co-Kα rays.

The magnetic permeability was measured by using a figure 8 coil, the coercive force was measured by a DC BH loop and a racer, the saturation magnetic flux density was measured by VSM, and the magnetostriction constant was measured by an optical lever method.

[0031]

[Table 1] Table 1 shows that Fe- (Co, Ni) -Ta-BC has Ti,
FIG. 3 shows the relationship between μ, Hc, λs, and Bs at 1 MHz and the film composition when V, Mo, and W were added and heat-treated at 600 ° C. As is clear from Table 1, μ of 2000 or more and Hc of 1 Oe or less were obtained for each composition. In addition, especially No. Magnetostriction on the order of 10 ⁻⁷ was obtained in the compositions of Nos. 1 to 3, 5, and ⁷ . 1-4,
Bs of 15 KG or more were obtained for the compositions of 6, 7, and 9, indicating that the soft magnetic alloy film of the present invention has excellent soft magnetic properties. On the other hand, Comparative Example 1, which is out of the scope of the present invention, does not have the properties required for the soft magnetic alloy film, and cannot be applied to a magnetic head or the like. Similar characteristics can be obtained when elements such as Zr, Nb, and Hf other than Ta are added alone or in combination.

[0032]

[Table 2] Table 2 shows that Fe- (Co, Ni) -Ta-BC has Cr, R
FIG. 3 shows the relationship between μ and Hc at 1 MHz and the film composition when heat treatment is performed at 600 ° C. with u and Rh added. Each composition has μ of 1000 or more. Each of the compositions 1, 2, 4, and 7 has a coercive force of 1 Oe or less, and has excellent soft magnetic characteristics.

In addition, Table 2 shows a relative comparison of the degree of corrosion progress when the samples after magnetic measurement were immersed in physiological saline for 24 hours at room temperature. ⊚ indicates that no corrosion was observed at all, and ∘ indicates that the amount of corrosion was 20% or less. Further, Δ indicates that the amount of corrosion was 20% or more. As a result, by adding Cr, Ru, and Rh in combination, the corrosion resistance is remarkably improved although μ is slightly decreased, and the soft magnetic alloy film of the present invention has excellent soft magnetic characteristics and corrosion resistance. I understand. In addition to the above Cr, Ru, Rh, Cu, Pd, Ag, Ir, P
Similar effects can be obtained by adding t, Au or the like alone or in combination.

[0034]

[Table 3] Table 3 shows that Fe- (Co, Ni) -Ta-BC has Ti, C
1M when heat-treated at 600 ° C with r added
It shows the relationship between μ and Hc of Hz and film composition.
Good soft magnetic properties are obtained also in these compositions.

FIG. 1 shows No. 1 in Table 1. 2 is an X-ray diffraction pattern of the film of No. 1. The pattern in the as depo state shows a halo pattern peculiar to amorphous,
The pattern after the heat treatment at 600 degrees is b. c. c-Fe
The reflections of the {110} plane and the {200} plane of are shown. S
The crystal grain size obtained from the Herrer's equation is about 10 nm, which indicates that a fine crystal phase is precipitated. Further, there is no big difference in the diffraction pattern from the compositions shown in the above table, and the crystal structures are basically the same. By thus making the crystal structure of the alloy film finer, excellent soft magnetic characteristics can be obtained.

Since the soft magnetic alloy film according to the present invention basically has a crystal structure of a fine crystal structure having an average crystal grain size of 0.08 μm or less, the fine crystal structure is 50 vol% of the whole. As long as it is in the above range, it is possible to obtain the magnetic characteristics and the like targeted by the present invention even when the amorphous phase is mixed.

FIG. 2 shows sample No. 1 in Table 1. 1 (white circle) and sample No. It is the graph which showed the magnetostriction (lambda) of 9 (black circle), and the relationship of heat processing temperature. Sample No.
By subjecting both 1 and 9 to heat treatment at an appropriate temperature, λs
It can be seen that shows a small value of 10 ^-7 .

Although all the heat treatments in this embodiment are heat treatments in a non-magnetic field, they are macroscopically anisotropic by heat treatment in a static magnetic field and using the hard axis of magnetization as a magnetic path, or heat treatment in a rotating magnetic field. It is possible to further improve the soft magnetic characteristics by suppressing the property dispersion.

Next, an example of using the soft magnetic alloy film of the present invention in a magnetic head will be described with reference to FIG. Figure 3
FIG. 6 is a perspective view of a magnetic head using the soft magnetic alloy film according to the present embodiment. This type of magnetic head is called an MIG (metal-in-gap) head.
-Jikikoa (1a) made from Zn ferrite,
A soft magnetic alloy film (2) is formed on (1b) by a sputtering method or the like, and magnetic cores (1a) and (1b) are joined and integrated by a fused glass (3). At this time, heat treatment of the soft magnetic alloy film (2) is simultaneously performed. Further, a gap (4) is formed on the abutting surfaces of the magnetic cores (1a) and (1b).
Is formed, the winding hole (6), the winding locking groove (7a), (7
The wire (5) is wound for a predetermined turn through b) to form the coil (8).

It is apparent that the magnetic head thus formed exhibits excellent recording / reproducing characteristics because it uses the soft magnetic alloy film. The magnetic head is MIG.
Although it is used for a head, it can also be used for a laminated type magnetic head, a thin film magnetic head, or the like.

[0041]

According to the inventions set forth in claims 1 and 2, it is possible to provide an excellent soft magnetic alloy film having a high magnetic permeability, a high saturation magnetic flux density and a low coercive force.

According to the inventions set forth in claims 3, 4, and 5,
It is possible to provide a soft magnetic alloy film having excellent corrosion resistance while maintaining high permeability, high saturation magnetic flux density and low coercive force. Furthermore, according to the present invention, the magnetostriction constant is ± 10 ⁻⁶ to 10
^-7 is good, and since it is heat-treated at a high temperature of 600 ° C. or higher, it is possible to use a medium to high melting point glass having excellent environmental resistance when applied to a magnetic head or the like.

Further, in the present invention, by adding B and C in combination, b. c. Precipitation of the c-phase results in a uniform fine grain structure, and adverse effects on soft magnetism due to crystal magnetic anisotropy are reduced, so that good soft magnetic characteristics can be obtained.

Further, by adding a small amount of the element T (= Co, Ni) and adjusting the magnetostriction constant, the above effect can be further enhanced.

[Brief description of drawings]

FIG. 1 is a graph showing an X-ray diffraction pattern of an example of a soft magnetic alloy film of the present invention.

FIG. 2 is a graph showing a relationship between a magnetostriction constant λs and a heat treatment temperature of an example of a soft magnetic alloy film of the present invention.

FIG. 3 is a perspective view when the soft magnetic alloy film of the present invention is used in a magnetic head.

[Explanation of symbols]

 1a, 1b Magnetic core 2 Soft magnetic alloy film 3 Welding glass 4 Gap 5 Wire rod 6 Winding hole 7a, 7b Winding locking groove

Claims (6)

[Claims] 1. A soft magnetic alloy film in which a metallographic structure formed by heat-treating an alloy film having a composition represented by the following formula is basically composed of crystal grains having an average crystal grain size of 0.08 μm or less. Fe _a L _f M _c B _d C _e However, L is at least one or more of Ti, V, Mo and W, and M is at least one or more of Zr, Nb, Hf and Ta. It is an element, and its composition range in atomic% is 70 ≦ a ≦ 90, 5 ≦ c ≦ 15, 0.5 ≦ d ≦
15, 0.5 ≦ e ≦ 15, 0.1 ≦ f ≦ 15, 1 ≦ d +
e ≦ 20. 2. A soft magnetic alloy film in which a metallographic structure formed by subjecting an alloy film having a composition represented by the following formula to a heat treatment is basically composed of crystal grains having an average crystal grain size of 0.08 μm or less. (Fe _1-b X _b ) _a L _f M _c B _d C _e However, X is one or two of Co and Ni, and L is T.
i, V, Mo, W, at least one element or two or more elements, M is Zr, Nb, Hf, Ta, or at least one element or two or more elements, and the composition range is b ≦ 0.0.
5, in atomic% 70 ≦ a ≦ 90, 5 ≦ c ≦ 15, 0.5 ≦
d ≦ 15, 0.5 ≦ e ≦ 15, 0.1 ≦ f ≦ 15, 1 ≦
d + e ≦ 20. 3. A soft magnetic alloy film having a metal structure basically formed by crystallizing grains having an average grain size of 0.08 μm or less by subjecting an alloy film having a composition represented by the following formula to heat treatment. Fe _a Y _g M _c B _d C _e However, Y is Cr, Cu, Ru, Rh, Pd, Ag, I.
at least one or two or more of r, Pt, and Au,
M is at least one element or two or more elements of Zr, Nb, Hf, and Ta, and the composition range thereof is 70% in atomic%.
a ≦ 90, 5 ≦ c ≦ 15, 0.5 ≦ d ≦ 15, 0.5 ≦
e ≦ 15, 0.1 ≦ g ≦ 10, 1 ≦ d + e ≦ 20. 4. A soft magnetic alloy film in which a metal structure formed by subjecting an alloy film having a composition represented by the following formula to a heat treatment is basically composed of crystal grains having an average crystal grain size of 0.08 μm or less. (Fe _1-b X _b ) _a Y _g M _c B _d C _e However, X is one or two of Co and Ni, and Y is C.
r, Cu, Ru, Rh, Pd, Ag, Ir, Pt, Au
At least one or more of them, M is Zr, N
At least one element or two or more elements of b, Hf, and Ta, the composition range of which is b ≦ 0.05, 70% by atomic%
≦ a ≦ 90, 5 ≦ c ≦ 15, 0.5 ≦ d ≦ 15, 0.5
≦ e ≦ 15, 0.1 ≦ g ≦ 10, 1 ≦ d + e ≦ 20. 5. A soft magnetic alloy film in which a metal structure formed by heat-treating an alloy film having a composition represented by the following formula basically comprises crystal grains having an average crystal grain size of 0.08 μm or less. (Fe _1-b X _b ) _a Y _g L _f M _c B _d C _e However, X is one or two of Co and Ni, and Y is C.
r, Cu, Ru, Rh, Pd, Ag, Ir, Pt, Au
Of these, at least one or more, L is Ti, V,
At least one or more of Mo and W, and M is Z
At least one element or two or more elements out of r, Nb, Hf, and Ta, the composition range of which is b ≦ 0.05, atomic%
70 ≦ a ≦ 90, 5 ≦ c ≦ 15, 0.5 ≦ d ≦ 15,
0.5 ≦ e ≦ 15, 0.1 ≦ f ≦ 15, 0.1 ≦ g ≦ 1
0 and 1 ≦ d + e ≦ 20. 6. The soft magnetic alloy film according to claim 1, wherein the metal structure produced by heat treatment contains an amorphous phase.