JPH06287730A - Production of soft magnetic alloy material - Google Patents

Abstract

PURPOSE:To provide a method for producing soft magnetic allay stock (sheet material) in which the adhesion between parts can be prevented without using alumina powder or the like in magnetic annealing in a vacuum. CONSTITUTION:At the time of producing the sheet material with >=0.5mum Rz surface roughness or >=0.06mum Ra surface roughness of a soft magnetic alloy contg. 35 to 85% Ni and 0.1 to 1.2% Al, and the balance Fe with inevitable impurities or a soft magnetic allay contg. 35 to 60% Ni, 0.1 to 1.2% Al and <=0.5 to 14% Cr, and the balance Fe with inevitable impurities or a soft magnetic alloy contg. 60 to 85% Ni, 0.1 to 1.2% Al, <=6% Mo and <=4% Cu, and the balance Fe with inevitable impurities, it is subjected to final annealing at 1000 to 1200 deg.C in gaseous hydrogen or in a mixed gas of gaseous hydrogen and an inert gas, and the finish cold rolling ratio after the final annealing is regulated to <=50%.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention is used in magnetic shield parts and various iron core parts.
The present invention relates to improvement of a Cr-based or Fe-Ni-Mo (Cu) -based soft magnetic alloy sheet material, and relates to prevention of mutual adhesion of components that occur during magnetic annealing after component processing.

[0002]

2. Description of the Prior Art Iron core parts represented by various magnetic shield members, watches, and cores of small transformers are provided in JIS-P.
B, JIS-PC and improved Fe-Ni-
Cr-based and Fe-Ni-Mo (Cu) -based alloys are widely used.

Generally, these magnetic alloys are magnetically annealed in order to exert their magnetic properties after being molded. Magnetic annealing is 900 to 120 in a hydrogen atmosphere or in a vacuum.
Since the operation is performed at a high temperature of 0 ° C. × 0.5 to 2 hours for a long time, when the parts are brought into contact with each other during magnetic annealing, a phenomenon that the parts are attached to each other at a contact point (referred to as adhesion) is likely to occur.
This is a particular problem when the number of processed parts is large. Therefore, conventionally, when a large number of processed parts are annealed at one time, the processed parts are magnetically annealed by sprinkling the processed parts in a large amount of alumina powder to prevent close contact between the processed parts.

[0004]

In the annealing method using alumina powder, there is a problem that the cost of magnetic annealing is increased because it takes time and effort to screen and clean the processed parts after annealing. Therefore, in order to eliminate the complexity of using the alumina powder, the present inventors formed an alumina film on the surface of the component during magnetic annealing in a hydrogen atmosphere by adding an appropriate amount of Al and adjusting the surface roughness, so that the We have developed a material that can prevent parts from sticking to each other.
I proposed in.

However, in the material proposed in Japanese Patent Application No. 4-88366, when the magnetic annealing is performed in a vacuum, the alumina film is not formed on the surface of the material, so that the mutual adhesion of the parts cannot be prevented. Therefore, from the electronics and magnetic industries, where production costs are being reduced and product miniaturization and high performance are being promoted urgently, we provide materials that do not cause mutual adhesion of parts without using alumina powder in vacuum magnetic annealing. There is a strong desire to do so.

Therefore, the present invention has been devised in order to solve such a problem, and Fe-Ni type and Fe-Ni-type are proposed.
An object of the present invention is to make it possible to prevent mutual adhesion between components of a Cr-based or Fe-Ni-Mo (Cu) -based soft magnetic alloy even if magnetic annealing after component processing is performed in a vacuum.

[0007]

The inventors of the present invention have set Al to 0.
Fe-Ni system, Fe-Ni-Cr containing 1 to 1.2%
-Based or Fe-Ni-Mo (Cu) -based soft magnetic alloys having a surface roughness of Rz ≧ 0.5 μm or Ra ≧ 0.06
When manufacturing a plate having a thickness of μm, the final annealing is performed in hydrogen gas or a mixed gas of hydrogen gas and an inert gas at 100
It should be noted that by carrying out at 0 to 1200 ° C. and setting the finish cold rolling rate after final annealing to 50% or less, it is possible to prevent the mutual adhesion of the processed parts without using alumina powder in magnetic annealing in vacuum. I found a fact.

[0008]

With respect to the reason for limiting the main components of Ni, Cr, Mo and Cu, it is necessary to obtain JIS-PB, PC, PD and PE grade magnetic characteristics.
In the PE class low Ni region, Ni was limited to 35 to 65%. In the high Ni region of JIS-PC class, N
i was limited to 60 to 85%, Mo was ≤6%, and Cu was ≤4%. Further, in order to obtain the JIS-PC grade magnetic permeability in the low Ni region, Cr: 0.5 to 14% is necessary.

Al is an important additional element in the present invention, and is necessary for forming an alumina film on the surface of the plate material during the final annealing in the process of manufacturing the plate material which is a raw material before the parts are processed. If the Al content is less than 0.1%, the amount of alumina film formed during the final annealing is small, and therefore adhesion cannot be prevented during magnetic annealing in vacuum. On the other hand, when the Al content exceeds 1.2%, the magnetic permeability is lowered and the magnetic properties are adversely affected. Therefore, the Al content is limited to 0.1 to 1.2%.

Ti and Zr are added to improve hot workability. When the content of Ti is less than 0.05%, the effect of improving hot workability is not recognized, and when it exceeds 0.5%, the surface quality of the material is deteriorated. If Zr is less than 0.001%, the effect of improving hot workability is not recognized, and if it exceeds 0.02%, the magnetic properties are deteriorated. Therefore, Ti is 0.05 to 0.5%, and Zr is 0.001 to 0.
It was set to 02%.

Next, the reasons for limiting the final annealing conditions will be described. FIG. 1 shows that the Fe-46% Ni alloy is subjected to final annealing for 1 minute at various temperatures in an atmosphere of 75% hydrogen + 25% nitrogen, and a glow discharge spectroscopic analysis (G
DS) shows the results. In the figure, the vertical axis is the detected intensity of Al, and the black-filled plot is 110 in vacuum for the sample.
Adhesion occurred when magnetic annealing was performed at 0 ° C. × 1 hr, and a white plot indicates that adhesion did not occur. From this figure, in the sample containing 0.1% or more of Al, Al was significantly concentrated in the surface coating when the final annealing temperature was 1000 ° C. or higher.
It can be seen that, in the sample in which is markedly concentrated, adhesion does not occur due to magnetic annealing in vacuum. On the other hand, Al is 0.1%
For samples of less than 1%, Al concentration was not found in the surface coating at any final annealing temperature, and it can be understood that adhesion cannot be prevented by magnetic annealing in vacuum.

In FIG. 2, Fe-containing 0.12% Al
The photoelectron spectroscopy analysis (ESCA) result of the surface film produced when the final annealing was performed for 1000% x 1 minute in 75% hydrogen + 25% nitrogen atmosphere about 46% Ni is shown. A peak of alumina is observed, and it can be seen that it is effective to form an alumina film on the surface in order to prevent adhesion by magnetic annealing in vacuum. This alumina film is formed during annealing in hydrogen gas or a mixed gas of hydrogen gas and an inert gas. Dew point of atmospheric gas is 0 to -60 ℃
It is desirable to keep The higher the final annealing temperature, the larger the amount of alumina produced, which is advantageous for preventing adhesion, but it is difficult to anneal at a temperature higher than 1200 ° C in actual operation. From the above findings, the final annealing temperature of the material (plate material) is 1000 to 12
Limited to 00 ° C.

Next, the finish cold rolling rate after the final annealing will be described. The material (plate material) before component processing is required to have appropriate material strength according to the application. When the material strength after the final annealing is lower than the required material strength, finish cold rolling can be performed after the final annealing to obtain an appropriate strength.
In Figure 3, 75% hydrogen + 2 for Fe-46% Ni alloy
Results of Glow Discharge Spectroscopy (GDS) analysis of surface coatings when final cold rolling was performed at various cold rolling ratios after final annealing on a sample that was subjected to final annealing at 1000 ° C for 1 minute in a 5% nitrogen atmosphere. Indicates. In the figure, the vertical axis represents the detected intensity of Al, and the black plot indicates the sample in vacuum 1
Adhesion occurred when magnetic annealing was performed at 100 ° C. × 1 hr, and a white plot indicates that adhesion did not occur. From this figure, in the sample containing Al by 0.1% or more, the detected strength of Al decreases as the finish cold rolling rate increases, and the magnetic strength in vacuum is reduced when the cold rolling rate is 50% or less. It can be seen that the adhesion can be prevented by annealing. It is considered that this is because when the cold rolling rate increases, the alumina coating on the surface becomes thinner as the plate thickness decreases, and when the cold rolling rate exceeds 50%, the alumina coating breaks more.
Therefore, the rolling ratio of finish cold rolling performed after the final annealing is 5
Regulate below 0%.

Surface roughness is an important factor for preventing adhesion during magnetic annealing. When the surface roughness is Rz ≧ 0.5 μm or Ra ≧ 0.06 μm, adhesion during magnetic annealing can be prevented. As a method of adjusting the surface roughness, a method of polishing an appropriate amount before the final annealing can be considered. The material (plate material) obtained by the method of the present invention has a better adhesion preventing effect than the material (plate material) by the conventional method even when subjected to magnetic annealing in an atmosphere other than vacuum (for example, in hydrogen). To be

[0015]

EXAMPLE An alloy having the composition shown in Table 1 was melted in a vacuum of 400 kg and subjected to normal hot rolling to cold rolling to obtain a plate thickness of 1.5 to 0.4.
mm alloy strip was produced. After polishing these alloy strips to various roughnesses using emery paper, the material (plate material) in a continuous annealing furnace in an atmosphere of 75% hydrogen + 25% nitrogen
Final annealing, followed by finish cold rolling with various rolling rates to obtain an alloy strip having a plate thickness of 0.4 mm, the surface roughness of which was adjusted. Next, 5000 parts for a magnetic head cover were formed from these alloy strips, and then magnetic annealing was performed at 1100 ° C. × 1 h in a vacuum using a badge type vacuum annealing furnace.

[0016]

[Table 1]

Table 2 shows the hot rolling yield, the final annealing temperature of the material,
The finish cold rolling rate, surface roughness before magnetic annealing, and adhesion failure rate after magnetic annealing are shown in comparison with the conventional method using alumina powder. The hot workability of the material and the effect of preventing adhesion during magnetic annealing were evaluated by the hot rolling yield and the adhesion failure rate, respectively, shown below. Hot rolling yield (%) = (weight of hot rolled coil after defective part removal /
Original weight of hot-rolled coil) × 100 Adhesion failure rate (%) = (number of adhered samples / total number of annealed samples) × 100

[0018]

[Table 2]

From Table 2, it can be seen that the adhesion failure rate in each of the examples of the present invention is as good as about 0.2 to 0.5%, which is equivalent to the conventional method using the alumina powder during magnetic annealing. It is also found that the inclusion of Ti or Zr improves the hot rolling yield.

[0020]

As described above, according to the present invention, even in magnetic annealing in vacuum, it is possible to prevent the work parts from adhering to each other without using alumina powder. It is possible to provide a magnetic alloy that can significantly reduce the cost involved.

[Brief description of drawings]

FIG. 1 is a graph showing the relationship between the final annealing temperature of a material and the Al strength in the surface coating after the final annealing by glow discharge spectroscopy (GDS).

FIG. 2 is a graph showing the alumina strength in the surface coating after the final annealing of the material by photoelectron spectroscopy (ESCA).

FIG. 3 is a graph showing the relationship between the cold rolling rate after final annealing of the material and the Al strength in the surface coating by glow discharge spectroscopy (GDS).

─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁵ Identification number Reference number within the agency FI Technical display location C22C 38/00 303 S 38/14 H01F 1/147 (72) Inventor Toshihiko Takemoto Shinnanyo Yamaguchi Prefecture 4976 Ichinomura-Minamimachi Nisshin Steel Co., Ltd.

Claims (8)

[Claims] 1. Ni: 35-85%, Al: 0.1-
1.2% and the balance Fe and unavoidable impurities, and the surface roughness is Rz ≧ 0.5 μm or Ra ≧ 0.06.
When manufacturing a soft magnetic alloy sheet having a thickness of μm, the final annealing is performed at 1000 to 1200 ° C. in hydrogen gas or a mixed gas of hydrogen gas and an inert gas, a method for manufacturing a soft magnetic alloy material. . 2. Ni: 35-60%, Al: 0.1-
1.2%, Cr ≦ 0.5 to 14%, balance Fe and unavoidable impurities, and surface roughness Rz ≧ 0.5 μ
m or Ra ≧ 0.06 μm, when producing a plate material of a soft magnetic alloy, the final annealing is performed in hydrogen gas or a mixed gas of hydrogen gas and an inert gas at 1000 to 1200 ° C.
A method of manufacturing a soft magnetic alloy material, characterized in that 3. Ni: 60-85%, Al: 0.1-
1.2%, Mo ≦ 6%, Cu ≦ 4%, balance Fe and unavoidable impurities, and surface roughness Rz ≧ 0.5
When manufacturing a plate material of a soft magnetic alloy with μm or Ra ≧ 0.06 μm, final annealing is performed in hydrogen gas or in a mixed gas of hydrogen gas and an inert gas in the range of 1000 to 1200.
A method for producing a soft magnetic alloy material, which is performed at ℃. 4. Further, at least one of Ti: 0.05 to 0.5% or Zr: 0.001 to 0.02% is contained and the surface roughness is Rz ≧ 0.5 μm or Ra ≧ 0. 06
When manufacturing the plate material of the soft magnetic alloy according to any one of claims 1 to 3, the final annealing is 100 in hydrogen gas or a mixed gas of hydrogen gas and an inert gas.
A method for producing a soft magnetic alloy material, which is performed at 0 to 1200 ° C. 5. When manufacturing the plate material of the soft magnetic alloy according to claim 1, final annealing is performed in hydrogen gas or a mixed gas of hydrogen gas and an inert gas at 1000 to 1200 ° C., and then rolling. A method for producing a soft magnetic alloy material, which comprises performing finish cold rolling at a rate of 50% or less. 6. When manufacturing the plate material of the soft magnetic alloy according to claim 2, final annealing is performed in hydrogen gas or a mixed gas of hydrogen gas and an inert gas at 1000 to 1200 ° C., followed by rolling. A method for producing a soft magnetic alloy material, which comprises performing finish cold rolling at a rate of 50% or less. 7. When manufacturing the plate material of the soft magnetic alloy according to claim 3, final annealing is performed in hydrogen gas or a mixed gas of hydrogen gas and an inert gas at 1000 to 1200 ° C., and then rolling. A method for producing a soft magnetic alloy material, which comprises performing finish cold rolling at a rate of 50% or less. 8. When manufacturing the sheet material of the soft magnetic alloy according to claim 4, final annealing is performed in hydrogen gas or a mixed gas of hydrogen gas and an inert gas at 1000 to 1200 ° C., followed by rolling. A method for producing a soft magnetic alloy material, which comprises performing finish cold rolling at a rate of 50% or less.