JPH0653903B2 - Ni-Fe system high permeability magnetic alloy - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION "Object of the Invention" (Industrial field of application) The present invention relates to a Ni-Fe-based high-permeability magnetic alloy, which has improved magnetic characteristics, and particularly in a direct current and a low frequency range. The present invention relates to the magnetic alloy having excellent magnetic properties such as magnetic permeability and shielding performance.

(Prior Art) Ni-Fe magnetic alloys equivalent to JIS PC are magnetic materials that have a very wide range of applications, such as magnetic head cases, various cores, metamorphic magnetic cores, and various magnetic shield materials. That is, such PC permalloy is characterized by high magnetic permeability and low coercive force.
80% Ni-5% Mo-Fe (supermalloy) and 77% Ni
-5% Cu-4% Mo-Fe (Mo, Cu permalloy), etc., and the level of magnetic permeability usually obtained with these alloys is that the initial magnetic permeability (hereinafter referred to as μi) is 150,000 and the maximum magnetic permeability (hereinafter referred to as μm). ) Is about 300,000.

However, due to recent advances in electronics, miniaturization and high performance of various devices have progressed, and further improvement in the characteristics of magnetic alloys as described above is desired. That is, in order to meet such demands, Japanese Patent Laid-Open Nos. 62-227053 and 62-227054 have been developed in which the magnetic properties of the above-described magnetic alloys are improved by reducing impurity elements and adding Cr.

Further, Japanese Patent Application Laid-Open No. 63-149361 discloses that in a material in which B is added to the alloy of the above-mentioned component system in order to improve hot workability during manufacturing, B is removed during magnetic annealing to improve magnetic properties. .

On the other hand, in the above component system, Ni is contained at about 80 wt% and is expensive, so the component system was fundamentally reviewed, Ni was reduced, and instead, Cu and Mn, which are cheaper than Ni, were added to increase the initial permeability. In addition to the technique of JP-B-62-13420, which has achieved the above-mentioned characteristics, JP-A-63-247336 and JP-A-63-247336 in which an appropriate amount of Al is added in addition to the technique of JP-B-62-13420 to reduce oxide inclusions and enhance magnetic properties. Sho 63-24
7339 technology is also being developed. In particular, these JP-A-63-247
The μi of alloys proposed by 336 and JP-A-63-247339 is as high as 426,000.

In addition to the above-mentioned demands for improving the magnetic properties, it has recently been required to manufacture the required properties at a lower cost. From this viewpoint, the technique disclosed in JP-A-1-100,232 has been proposed. That is, this technique is characterized by adding 1 to 4 wt% of Si to ordinary Mo supermalloy and obtaining a sufficiently satisfactory magnetic permeability even at a relatively low magnetic annealing temperature of about 1030 ° C or less. .

(Problems to be Solved by the Invention) DC magnetic characteristics after the final heat treatment (1100 ° C. × 3 hours) in a hydrogen atmosphere even with the reduction of impurities and the addition of Cr, which are the features of JP-A-62-227053 and 227054. Is, for example, at most 100,000 in μi, and is inevitably unsuitable for applications in which magnetic characteristics higher than that are required.

Further, in the proposal of JP-A-62-227054, since Cr is newly added to the usual Ni-Fe-Mo-based or Ni-Fe-Mo-Cu-based component, the cost becomes high. On the other hand, according to the proposal of Japanese Patent Laid-Open No. 62-227053, in addition to the high cost due to the addition of Cr, the Mn is made higher than the normal level (1.2 to 10 wt%), so that the hot workability is extremely deteriorated. I also have.

In both of the above two proposals, B is added, but the addition of B in this case is to improve hot workability and punchability. Only the addition of B intended in these proposals is performed. However, no clear improvement in magnetic properties was observed, and in some cases deterioration was observed.

Further, in Japanese Patent Laid-Open No. 63-149361, the magnetic characteristics are improved by the B-removing treatment, but the magnetic characteristics obtained after this treatment are at most 75,000 μi, which is a normal Ni- level.
This is the level obtained with Fe-Mo-Cu alloys. Therefore, this technique is inevitably unsuitable for applications requiring higher magnetic properties.

On the other hand, JP-B-62-13420, JP-A-63-247336 and 247339.
Can provide high μi permalloy,
Since Mn and Cu are increased, there is a manufacturing problem that hot workability during manufacturing is essentially lowered. The saturation magnetic flux density of the alloy obtained by this proposal is, for example, at most 5000 gauss when viewed in terms of B ₁₀ (magnetic flux density at 10 oersteds), and B ₁₀ of B ₁₀ in supermalloy, Mo, and Cu permalloy.
Low compared to 7,000-8,000 gauss. This means that this alloy saturates the magnetic flux in the material with an external magnetic field lower than Supermalloy, Mo, and Cu Permalloy,
When used as a shield material, it must be used in a place where the external magnetic field is relatively high.

Further, the technique disclosed in Japanese Patent Laid-Open No. 1-100232 has a problem that since a large amount of Si is added, workability deteriorates and manufacturability deteriorates. Also, with this technology, the shielding performance of 50 Hz is
Although it had the required level, it had a drawback that the shield performance at DC was slightly inferior.

“Structure of the Invention” (Means for Solving the Problems) The present invention was devised through repeated studies to solve the above-mentioned problems in the conventional ones, and has been proposed in DC and low frequency regions. In order to essentially improve the magnetic properties such as magnetic permeability and the shielding performance, and to obtain the required properties at the same level as before, magnetic annealing was performed at 100 ° C
For the purpose of enabling to lower the temperature to some extent, the effect of the main components such as Ni, Mo, Cu and Fe on the magnetic properties was further investigated, and the relation between the obtained properties and the components was
The present invention has been completed as a result of conducting experiments and studies by expanding to an addition system. That is, the present invention is as follows.

(1) Ni: 77.5 to 79.5 wt%, Mo: 3.8 to 4.6 wt%, Cu: 1.8 to 2.5 wt%, Mn: 0.1 to 1.10 wt%, P: 0.010 wt% or less, S: 0.0020 wt% or less, O: 0.0030 wt% or less, N: 0.0010 wt% or less, C: 0.020 wt% or less, and B: Contained within the range of, and the balance basically consists of Fe, and
Ni, Mo, Cu, Mn, Fe Ni which is contained in a range satisfying
-Fe-based high-permeability magnetic alloy.

(2) It has the composition as described in the preceding paragraph, and the amount of B in the austenite grain boundary and its vicinity is 10 to 5 after magnetic annealing.
Ni-Fe based high permeability magnetic alloy characterized by being 0 atm%.

(Operation) According to the present invention, under proper control of impurity elements,
It is not found in conventional Mo, Cu permalloy or supermalloy by the same system by optimizing the addition amount of Ni, Mo, Cu, Mn, Fe and B and controlling the component balance of each amount within a specific range. In addition, it is possible to lower the magnetic annealing temperature by about 100 ° C. as compared with the conventional one in order to achieve high magnetic permeability and shield property and obtain the required characteristics at the same level as the conventional one.

That is, first, the improvement of the magnetic properties intended in the present invention is achieved under the control of the impurity level in the alloy, and P, S, O, N,
The reason for the limit of C is wt% (hereinafter simply referred to as%) and is as follows.

P is an element that is detrimental to the hot workability of the high Ni-Fe alloy targeted by the present invention, and weakens the tendency to form a cubic texture during the final hydrogen annealing, and this P is 0.010.
%, The magnetic permeability deteriorates and the hot workability also deteriorates, so the upper limit was made 0.010%. The lower limit is preferably 0.0010% from the economical aspect of melting.

S is detrimental to hot workability, and it inhibits grain growth during final hydrogen annealing through the formation of sulfides, and the grain size after annealing is small, so magnetic permeability does not improve. On the other hand, it is an extremely harmful element. If the S content exceeds 0.0020%, Ni, Mo,
Even if the Cu, Fe, and B contents are optimized, the magnetic properties intended in the present invention cannot be improved, and the hot workability is significantly deteriorated, so 0.0020% is required as the upper limit. . In order to improve the permeability of DC and AC differently, 0.00
Less than 05% is more desirable.

O exists as an oxide inclusion in the alloy targeted by the present invention, and if the amount thereof is large, it inhibits grain growth during the final hydrogen annealing, and since the grain size after annealing is small, the magnetic permeability is high. Since it does not improve, it is an extremely harmful element for magnetic properties. That is, if this O amount exceeds 0.0030%, N
Even if the amounts of i, Mo, Cu, Fe, and B are optimized, the magnetic properties intended in the present invention cannot be improved, so 0.0030% is set as the upper limit. In order to further improve the magnetic permeability at direct current, 0.00
10% or less is more preferable.

In an alloy based on the addition of B, N easily combines with B to form BN, so that the amount of effective B decreases. In addition, if a large amount is contained in the alloy for the reason that the formed BN causes the magnetic properties to be remarkably deteriorated, it has an adverse effect. That is, if this N exceeds 0.0010%, the magnetic properties deteriorate remarkably for the above reason, so 0.0010% was made the upper limit. In addition, in order to further improve the magnetic permeability with alternating current, 0.
0005% or less is more preferable.

C exists as an interstitial element in the target alloy of the present invention, and if it is present in a large amount, the magnetic permeability decreases, so it is an element harmful to the magnetic properties. If it exceeds 0.020%, C is for this reason. Since the deterioration of magnetic properties becomes remarkable, the upper limit was set at .020%.

Now, in the present invention, under the control of the impurity elements as described above, the addition amounts of Ni, Mo, Cu, Fe and B are optimized,
The object is achieved by setting the component balance of each amount within a specific range, and these are as follows.

In the range of 77.5 to 79.5%, Ni can obtain high magnetic characteristics and high shielding characteristics intended by the present invention. If this Ni content is less than 77.5% or more than 79.5%, the magnetic permeability decreases in any case.
% Was the lower limit and 79.5% was the upper limit.

Mo can achieve the high magnetic properties and high shielding properties aimed at by the present invention in the range of 3.8 to 4.6%. That is, if Mo is less than 3.8% or exceeds 4.6%, the improvement of magnetic permeability cannot be achieved, so it is necessary to set it to 3.8 to 4.6%.

Cu is an alloy which falls within the scope of the present invention, and is B described later.
In the presence of, the DC magnetic characteristics are dramatically improved, the effective magnetic permeability of AC is also improved, and AC (50Hz)
It also has the effect of improving the squareness (Br / Bm). The effect of Cu is 77.5 to 79.5% for Ni and Mo: 3.8.
Appears when the content is up to 4.6%, and the optimum Cu content is from 1.8 to 2.
5%. In addition, if Cu is less than 1.8%, such Cu
However, if Cu exceeds 2.5%, the characteristic deteriorates. Therefore, the range of Cu is 1.8-2.5%.
I decided.

Mn is an element that affects the magnetism of the alloy of the present invention like Mo and Cu described above, and even if this Mn is 1.10% or less, the high magnetic permeability targeted by the present invention can be achieved, but 1.10 If it exceeds%, such improvement in magnetic permeability cannot be achieved, so 1.1
The upper limit is 0%. On the other hand, if Mn is less than 0.10%, hot workability deteriorates, which is not preferable, so 0.10% was made the lower limit.

B is an essential element for achieving the high magnetic permeability intended in the present invention.

([B] and [N] are the addition amounts of B and N in the alloy,
%), The object of the present invention can be effectively achieved in the range of 0.0005 to 0.0070%, but if it is less than 0.0005%, the magnetic permeability does not improve, while if it exceeds 0.0070%, the magnetic permeability decreases. The lower and upper limits of 0.0005% and 0.0070% were set, respectively.

Next, under the optimized addition amount of each component mentioned above, Ni, M
It is necessary to optimize the component balance of o, Cu, Fe and B in order to improve the characteristics intended in the present invention, and FIGS. 1 to 4 show the parameters that define these component balances (this Parameter is X, Where) is the horizontal axis and the amount of B added is the vertical axis, the initial magnetic permeability, the degree of shielding, and the effective magnetic permeability at 1 kHz obtained for each test material,
It shows the squareness at 50Hz, but it is
All test materials in the figure are Ni, Mo, Cu, Mn, B, P, S,
A JIS ring having an outer diameter of 45 mm and an inner diameter of 33 mm was prepared from a thin plate sample having a thickness of 0.5 mm, which was prepared by repeating hot rolling, cold rolling and annealing after the contents of O, N and C were within the scope of the present invention. After punching, the sample was heat-treated at 1100 ° C for 3 hours in an atmosphere of high-purity hydrogen gas that had been permeated with a palladium membrane and purified, and the temperature between 1100 ° C and 650 ° C
It was cooled at 100 ° C./hr and then furnace cooled.
The degree of shielding is the same as above, and a Helmholtz coil is applied to a cylinder with a plate thickness of 0.5 mm, a diameter of 50 mm, and a length of 200 mm, and an external magnetic field (H ₀ ) is applied to the cylinder in a direction perpendicular to the axial direction of the cylinder. It was obtained by measuring the internal magnetic field H ₁ at the center of the inner side of the cylinder. The numbers (blocking degree) in the figure are the values of H ₀ / H ₁ . The measurement was performed in a box that was magnetically shielded to a level where the effect of geomagnetism could be ignored. The effective magnetic permeability at 1 KHz is obtained by measuring the inductance magnetic permeability of 5 mOersted using a ring sample with a plate thickness of 0.35 mm that has been subjected to the same magnetic annealing as above, and the squareness at 50 Hz measures the effective magnetic permeability. Using the same ring sample I did,
It was calculated from the ratio of Br and Bm in a magnetic field of 0.1 Oersted. Bm is the magnetic flux density in the material when an external magnetic field of 0.1 oersted is applied, and Br is the magnetic flux density when the external magnetic field is removed from the state in which the external magnetic field of 0.1 oersted is applied. This is simply Br and Bm below.
Is written.

Parameter X is in the range of 3.3 to 3.8, and Is 0.0005 to 0.0070% and the initial permeability μi is 350,000.
While the values are high as above, when X is less than 3.3 or more than 3.8, μi is at a low level of less than 200,000. Moreover, even if X is in the range of 3.3 to 3.8, Is less than 0.0005, μi is less than 200,000, showing no improvement. On the contrary, when the ratio exceeds 0.0070%, μi decreases.
Further, from FIG. 2, the shielding degree also shows a high value of 300 or more in the range of the present invention, which is higher than the shielding degree in the materials other than the range of the present invention.

FIG. 3 shows the effective magnetic permeability, which is as high as 6500 or more in the range of the present invention, which is higher than that of the materials other than the present invention. Further, FIG. 4 shows that the squareness at 50 Hz is as high as 0.90 or more in the range of the present invention, which is higher than that of the materials other than the present invention. From these facts, in the present invention, as a component balance that obtains high μi, high shielding degree, high effective magnetic permeability, and high squareness, N
The range of i, Mo, Cu, Mn, B of the present invention is as described above, and the parameter X is defined as within the range of 3.3 to 3.8.

By the way, the inventors of the present invention conducted a study to further enhance the magnetic properties by using the alloy of the present invention as described above, and as a result, after the heat treatment for enhancing the final magnetism, the austenite grain boundary of the alloy and its vicinity It was confirmed that the initial magnetic permeability μi and the degree of shielding were further improved when the amount of B was in the specific range. That is, FIGS. 5 (a) to 5 (d) respectively show the μi shielding degree, the effective magnetic permeability, the squareness and the austenite grain boundary of the alloy within the composition range of the present invention (inventive alloy 3 of Example 1 described later) and the vicinity thereof. B
It shows the relationship of the amount, μi after hot working with the above alloy,
A JIS ring with an outer diameter of 45 mm and an inner diameter of 33 mm was punched out from a thin plate sample with a thickness of 0.5 mm prepared by repeating cold rolling and annealing, and using this as a sample, a palladium membrane was made to permeate through it, and was refined through a palladium membrane to produce 1100 in an atmosphere of a high-purity hydrogen stream. Heat treatment for 3 hours at ℃, 50 ~ 400 ℃ / from 1100 ℃ to 650 ℃
The results obtained by measuring μi with a sample cooled at a constant cooling rate within the range of hr and then cooled in a furnace are summarized in relation to the B content in the austenite grain boundaries and in the vicinity thereof. That is, the amount of B in the austenite grain boundaries and in the vicinity thereof was cut out from a sample having a thermal processing history similar to that of a thin plate sample for which μi was measured, a notched test piece that could be attached to an auger observation stage was cut, and electrolytic hydrogen was added by the cathode electrolysis method. , The grain boundary embrittlement treatment was performed to perform the grain boundary fracture in vacuum, and the component analysis of the exposed grain boundary fracture surface was performed for 10 different points by Auger spectroscopy, and the average was obtained. atm%. The degree of shielding is the same as the above manufacturing history. A cylinder with a plate thickness of 0.5 mm, a diameter of 50 mm and a length of 200 mm is applied to a Helmholtz coil with an external magnetic field (H ₀ ), 50
It was determined by measuring the internal magnetic field H ₁ at the center of the inside of the cylinder when 0 milligauss was applied in the direction perpendicular to the axis of the cylinder. The degree of shielding (= H ₀ / H ₁ ) was measured in a box that was magnetically shielded to a level where the effect of geomagnetism could be sufficiently ignored. The effective magnetic permeability at 1 KHz is obtained by measuring the inductance magnetic permeability at 5 mOersted using a ring sample with a plate thickness of 0.35 mm that has been subjected to the same magnetic annealing as above, and the squareness at 50 Hz is the effective magnetic permeability. Using the same ring sample as that measured, it was determined from the ratio of Br and Bm in a magnetic field of 0.1 Oersted.

It is clear that μi in FIG. 5 (a) is improved in the amount of B in the austenite grain boundary and its vicinity in the range of 10 to 50 atm%, particularly in the range of 15 to 40 atm%.
It is more than 480,000. The cause of such an improvement in μi is not clear, but the presence of an appropriate amount of B at and near the grain boundaries changes the properties of the grain boundaries, and this change causes
In particular, it is presumed that the ease of movement of the domain wall, such as the initial magnetic permeability, or the ease of rotational magnetization has a good influence on the required characteristic value. From these results, alloys in the composition range of the present invention have a higher μi, a higher degree of shielding, a relatively high effective magnetic permeability, and a relatively high squareness as a condition to combine austenite grain boundaries after magnetic annealing and the vicinity thereof. B content of 10 to 50 atm% was determined.

The Ni-Fe alloy targeted by the present invention is inferior in hot workability. As a method of improving the workability, a combination of a small amount of B and a small amount of Ca is often combined, but even if such a small amount of Ca is added, the constituent requirements of the present invention as described above can be satisfied. For example, the improvement of the initial magnetic permeability which is the object of the present invention is achieved. Further, in the present invention, in addition to the above-described component composition, Si and Al inevitably included in the case of forming an iron alloy will not be described in detail.
Content within the range of 0.3% or less and Al: 0.03% or less is allowed.

(Example) A specific example of the present invention will be described below.

Example 1 Inventive alloys and comparative alloys of high Ni-Fe alloys having the chemical composition as shown in the following Table 1 were melted by vacuum melting, which was hot worked, descaled, and cooled. Prepared rolled material. The Si content is 0.05 to 0.15 in any of the test materials.
Within the% range. Further, these materials were then cold rolled and annealed to form thin plate samples of 0.5 mm, and JIS rings having an outer diameter of 45 mm and an inner diameter of 33 mm were punched out from these samples. The magnetic properties of these samples were heat-treated at 1100 ° C. for 3 hours in an atmosphere of high-purity hydrogen gas that had been purified by passing through a palladium film, and then subjected to heat treatment at 1100 ° C. to 65 ° C.
It was cooled at 400 ° C / hr during 0 ° C, then cooled in a furnace and measured, and the result obtained by measuring μi as the magnetic permeability at 0.005 Oersted and the degree of shielding, effective magnetic permeability, squareness at 50 Hz, The results of coercive force and magnetic flux density are also shown in Table 1.

The degree of shielding was the same as the above manufacturing history. A cylinder with a plate thickness of 0.5 mm, a diameter of 50 mm, and a length of 200 mm was applied to a cylinder with a Helmholtz coil with an external magnetic field (H ₀ ), and 500 milligauss was applied in the direction perpendicular to the axial direction of the cylinder. In this case, it was obtained by measuring the internal magnetic field H ₁ at the central portion inside the cylinder. Shielding degree (= H ₀
/ H ₁ ) was measured in a box that was magnetically shielded to a level where the influence of geomagnetism could be sufficiently ignored.

The effective permeability at 1 kHz is obtained by measuring the inductance permeability at 5 mOersted using a ring sample with a thickness of 0.35 mm that has been subjected to the same magnetic annealing as above, and the squareness at 50 Hz is the effective permeability. Br at 0.1 Oersted magnetic field using the same sample ring as measured
And Bm.

The magnetic flux density and the coercive force were measured using the same sample ring as that used for obtaining the initial magnetic permeability. The magnetic flux density is B ₁₀₀₀ is 10
It is the magnetic flux density when an external magnetic field of 00 A / m is applied, and the coercive force is the strength of the magnetic field at which the magnetic flux density is 0 after the external magnetic field of 1000 A / m is applied and then the magnetic field is reversed.

That is, alloy No. 1 and No. 2 materials are C, P, S, O, N,
The amounts of B, Ni, Mo, Cu and Mn are all within the range of the composition of the present invention, and μi shows a high magnetic permeability of 350,000 or more, and the shielding degree shows a high value of about 300 or more. or,
The effective magnetic permeability, squareness at 50 Hz, and coercive force are also at superior levels compared to the comparative example.

Alloy Nos. 3 and 4 are C, P, S, O, N, B, N
i, Mo, Cu and Mn amount is an alloy within the present invention component range, and is an alloy with a trace amount of Ca added with the intention of improving hot workability, but in this case, each characteristic value Is about the same level as alloys No. 1 and No. 2 described above. That is, it was confirmed that the effect of the present invention is sufficiently exerted even in the alloy in which the trace amount of Ca is added as described above.

Further, in alloy No. 5 material, C, S, O and N are reduced to more preferable levels, and respective characteristic values are higher than those of No. 1 to No. 4. In addition, these No. 1-N
In the case of the invention alloy of o.5, deterioration of the initial magnetic permeability when the surface pressure of 4 kgf / mm ^{2 is} applied is also the comparative alloys Nos. 6 to 22, No. 22 and No. 14 to No. 22 described later.
It is smaller than that of (1), and it can be seen that the deterioration of the characteristics due to strain is also small.

On the other hand, the alloys No. 6 and No. 7 have Ni content exceeding the upper limit or less than the lower limit, respectively, and the alloys No. 8 and No. 9 have the Mo amount exceeding the upper limit. Beyond
Or less than the lower limit, alloy No. 10 and N
No. 11 shows that the Cu content exceeds the upper limit or less than the lower limit, respectively. Further, alloy No. 12 has Mn content exceeding the upper limit, No. 13 has less than each lower limit, and alloys No. 14 and No. 15 have B content exceeding the upper limit, or Less than the lower limit, and further alloy N
o.16 to No.20 are C, P, S, O, N respectively
Which exceeds the composition range of the present invention, or alloy No. 2
No. 1 and No. 22 are those in which the parameter X exceeds the upper limit and less than the lower limit specified in the present invention, respectively, but these test materials No. 6 to No. 21 are all other than No. 13 It is at a lower level than the invention. It should be noted that alloy No. 13 has the Mn content below the lower limit specified in the present invention as described above, and each characteristic value level shows a high value at the same level as in the present invention. The workability was extremely poor.

That is, according to the present invention, the amount of Ni, Mo, Cu, Mn, B, and Fe is individually controlled and the balance thereof is strictly defined under the reduction of impurity elements such as C, P, S, O, and N. Excellent initial permeability, shielding degree, effective permeability, 50Hz
For the first time, it is possible to reduce the deterioration of the characteristics with respect to squareness, coercive force, and strain. In order to obtain the required characteristics in the present invention, the gas used for the heat treatment can be a high-purity H ₂ gas as shown in this example, but similar characteristics are defined in JIS. It can also be obtained by performing heat treatment in a normal H ₂ atmosphere, that is, in a H ₂ gas stream having a dew point of −40 ° C. or lower.

Example 2 With respect to the alloys No. 1 to No. 4 of the present invention of Example 1 described above, the outer diameter is 45 m from the 0.5 mm thin plate sample that has been cold rolled and annealed.
A JIS ring having a diameter of 33 mm and an inner diameter of 33 mm was punched to prepare a sample. In addition, a notched test piece that can be attached to the stage for auger observation was cut out from the same sample.

The samples obtained as described above were heat-treated at 1100 ° C. for 3 hours under various atmospheres as shown in Table 2 below, and the cooling rates varied between 1100 ° C. and 650 ° C. The magnetic properties and the degree of shielding were measured using a sample that was cooled in a furnace and then cooled in a furnace. Further, the amount of B in the austenite grain boundaries and the vicinity thereof is determined by adding cathodic electrolysis hydrogen by the cathodic electrolysis method to perform grain boundary embrittlement treatment after the heat treatment, and performing grain boundary fracture in vacuum to reveal the grain boundaries. The component analysis of the fractured surface was carried out for 10 different points by Auger spectroscopy, and the results were averaged. These results are as shown in Table 2 together.

That is, the test material No. 1 using the alloy No. 1 of the present invention
In No. 4, the B content in the austenite grain boundary and its vicinity is within the definition of the present invention, and the μi and the shielding degree are the B content in the austenite grain boundary and its vicinity not being the specification of the present invention. It is higher than .6. Inventive alloy No.
In the case of using No. 2, the amount of B in the austenite grain boundaries and in the vicinity thereof in each of the test materials No. 8 to No. 11 is within the scope of the present invention, and the μi and the degree of shielding are the austenite grain boundaries and the The B content in the vicinity is higher than that of each of the test materials No. 7 and No. 12, which are out of the regulation of the present invention.

In the case of using the alloy No. 3 of the present invention, the test materials No. 14 to N
The amount of B in the austenite grain boundary and its vicinity in each of the o.16 materials is within the definition of the present invention, and the μi and the degree of shielding have a B content in the austenite grain boundary and the vicinity thereof that are outside the specifications of the present invention. It is higher than those of No. 13 and No. 18.

Furthermore, in the case of using the alloy No. 4 of the present invention, the test material N
The amount of B at and near the austenite grain boundaries in each of Nos. 19, 20, 22, and 23 is within the specifications of the present invention, and its μi and shielding degree are outside the specifications.
It is higher than that of o.24. The amount of B at and near the austenite grain boundary is within the range of the test material N
o.1 to No.4, No.8 to No.11, No.14 to No.16, No.
Nos. 19, No. 20, No. 22, and No. 23 have excellent initial permeability and shielding, and relatively high effective permeability and 50 Hz.
It also has the squareness of.

The test materials No. 2, No. 14, No. 15, No. 18, No.
19 has a higher initial permeability and these materials have a lower coercivity. It is also understood that in these test pieces, the deterioration of initial magnetic permeability when a surface pressure of 4 kgf / mm ^{2 is} applied is smaller than that of the comparative alloy of Example 1, and the characteristic deterioration due to strain is small.

Each of the test materials Nos. 5, 17, and 21 in Table ₂ is the case where the dew point of H ₂ is higher than −40 ° C. while maintaining the atmosphere at 1100 ° C. × 3 hr, and is heat treated under such conditions. The sample had a distinctly low μi of about 200,000, and the shielding degree was around 100, which is lower than that of other invention examples. That is, the effects of the present invention are appropriately exhibited by performing heat treatment at H ₂ having a dew point of −40 ° C. or lower defined by JIS.
Further, the effect of the present invention can be exhibited even by heat treatment under a high vacuum of 1 × 10 ⁻⁵ Torr.

(Example 3) Samples were prepared under the same manufacturing conditions as in Example 2 with respect to the alloy No. 4 of the present invention of Example 1 described above and the comparative alloy No. 23 having the components shown in Table 3 respectively. Heat treatment was performed under the magnetic annealing conditions as shown in FIG. 4, and the magnetic characteristics and the degree of shielding were the same as in Example 2. The results are shown in Table 4.

In addition, in this comparative alloy No. 23, Ni and Cu are outside the scope of the present invention, and the other components are within the scope of the present invention.

Inventive alloy No. 4 shows a value almost the same as or slightly higher than the magnetic properties obtained after magnetic annealing at 1000 ° C. for 1 hour. That is, according to the present invention, it can be seen that the magnetic annealing temperature can be lowered by about 100 ° C. to obtain the same characteristics as the comparative alloy.

The present invention is not limited to the manufacturing method of the embodiment, and may be melted / melted, cast into a thin cast plate, as-cast or after hot working and / or descaled, cold rolled, and annealed.

Instead of hot working, or warm working may be performed to improve the efficiency of cold rolling.

However, when surface texture, plate thickness and dimensional accuracy are required, it is better to perform cold rolling before final melting.

Further, instead of one cold rolling, cold rolling, recrystallization annealing (for example, 800 ° C. or higher), and cold rolling may be repeated.

Even with the manufacturing method as described above, almost the same method can be obtained within the scope of the present invention.

"Effects of the Invention" According to the present invention as described above, the magnetic characteristics of the Ni-Fe-based high-permeability magnetic alloy are appropriately improved, and particularly the magnetic characteristics such as the magnetic permeability in the DC and low frequency regions, And, by providing a high magnetic permeability magnetic alloy that has dramatically superior shield performance to the conventional PC Permalloy, various porcelain shield materials, magnetic head cases, cores, and more It can be widely applied to materials used for non-linear applications such as magnetic amplifiers and pulse transformers, and it is also possible to reduce the magnetic annealing temperature by about 100 ° C compared to the conventional method to obtain the required characteristics at the same level as the conventional method. In addition, the characteristic deterioration due to distortion is small, and the required magnetic characteristics can be exhibited even when it is used as a structural part such as a shielded room. Which is a great invention industrially its effect because it is capable of properly readiness against demand.

[Brief description of drawings]

The drawings show the technical contents of the present invention. FIG. 1 shows the initial permeability μi and the parameter X, Fig. 2 shows the relationship between Fig. 3 shows the relationship between the effective magnetic permeability of AC and the parameter X, Fig. 4 shows the relationship between the squareness and parameter X at 50Hz. And FIG. 5 is a chart showing the relationship between the initial magnetic permeability μi and the B content in the austenite grain boundaries and in the vicinity thereof.

Claims (2)

[Claims] 1. Ni: 77.5 to 79.5 wt%, Mo: 3.8 to 4.6
wt%, Cu: 1.8 to 2.5 wt%, Mn: 0.1 to 1.10 wt%, P: 0.010 wt% or less, S: 0.0020 wt% or less, O: 0.0030 wt% or less, N: 0.0010 wt% Hereinafter, C: 0.020 wt% or less is contained, and B is Contained within the range of, and the balance basically consists of Fe, and
Ni, Mo, Cu, Mn, Fe Ni which is contained in a range satisfying
-Fe-based high-permeability magnetic alloy. 2. A Ni-Fe-based high permeability having the composition of claim 1 and having a B content of 10 to 50 atm% at and near the austenite grain boundaries after magnetic annealing. Magnetic susceptibility magnetic alloy.