JPS6191331A - Manufacture of grain oriented high silicon electrical iron sheet - Google Patents

Abstract

PURPOSE:To manufacture the titled iron sheet superior in magnetic characteristic stably and freely capable of setting magnetized direction easily, by providing grooves on surface of high Si iron alloy sheet having a specified Si content in a suitable direction, then annealing the sheet at a suitable temp.. CONSTITUTION:High Si iron alloy sheet contg. 2-8wt% Si has grooves having saw teeth shaped-section along a desired easily magnetized direction or that vertical thereto, or both thereof, on at least one part of upper and lower surface thereof, and is manufactured by cooling rapidly and solidifying continuously molten high Si iron alloy of said compsn. by using cooling body such as cooling roll providing grooves of a desired size. As the groove, about 60-120 deg. top angle theta or theta' and about 1-5mum depth are suitable. The grooved plate material is annealed at 800-1,300 deg.C, to obtain the titled sheet freely capable of setting easily magnetized direction.

Description

[Detailed Description of the Invention] <Field of Application in Industry E> This invention relates to a method for stably manufacturing a oriented high-silicon electromagnetic iron plate with excellent magnetic properties, easily and freely setting the magnetization direction. It is something.

<Prior Art> In general, high-silicon iron alloy plates with a Si content of around 3 to 4% c or less (component ratios are based on weight) are used as magnetic cores for generators, transformers, electric motors, etc.

It is considered to be a very important soft magnetic material in the electrical industry.

Conventionally, high-silicon iron alloy plates as mentioned above have been used for hot piezoelectric and 1.
It is common practice to obtain a thin sheet material from a piece of a predetermined composition by cold rolling multiple times with intermediate annealing, and then subjecting it to magnetic properties and annealing under strict conditions.

However, the method described above requires a large number of steps to obtain a product, and has the disadvantage that the manufacturing cost becomes extremely high. : 2~84i?A proprietary "ultra-quenching method" is applied to the production of thin sheets of silicate iron alloys containing 2 to 84i?, and thin sheets are manufactured directly from molten silicate iron alloys without any plastic processing such as rolling. However, this 1: annealing to improve magnetic properties! A method of producing desired electromagnetic iron plates has come to be adopted.

In addition to the single-roll method and twin-roll method as shown in the schematic diagram of the second factor and FIG. However, in short, the method of injecting molten metal onto the surface of a cooling body that is continuously moved and renewed, and directly converting it into a carbon ribbon, is collectively referred to as the 1 super-quenching method. In Figures 2 and 3, reference numeral 1
2 is a molten metal container, 2 is a molten metal spouting nozzle, 3 is a cooling roll, and 4 is a strip-shaped thin plate product.

By the way, the above-mentioned high-silicon iron alloy plate has a plate surface C (100
It is known that preferential growth of crystal grains having ) planes or (110) planes occurs.

Using this, (100)<ok/>, (11s<br
tz> or (110)<001> has also been proposed (for example, JP-A-57-94527, JP-A-58-4534).
No. 9, JP-A-58-113319, etc.).

<Problems to be Solved by the Invention> However, the above conventional method does not require the use of hot rolling, cold rolling, etc., which have strict condition regulations in order to preferentially grow crystal grains that are non-oriented in the plane or have a specific orientation. Or, even if a oriented electromagnetic iron plate with desired magnetic properties can be obtained, it is almost impossible to adjust the direction of easy magnetization. Therefore, there is currently a strong desire for a means for manufacturing oriented high-silicon electromagnetic iron plates that is industrially stable and allows the direction of easy magnetization to be set freely.

<Means for Solving the Problems> From the above-mentioned viewpoints, the present inventors have not only been able to obtain a product with excellent magnetic properties, but also improved the composition of the material and the rolling conditions C: We have conducted research to find a means of manufacturing oriented high-silicon electromagnetic iron plates that are industrially stable and easy to set the magnetization direction σ.

(JLl) When performing recrystallization annealing in which surface energy acts on a high silicon iron alloy plate containing 2 to 8% by weight of Si″4 to cause grain growth, both sides of the high silicon iron alloy plate or If a groove with a sawtooth cross section is formed on one side or at least a part thereof (for example, FIG. For example, crystal grains with (110) planes grow preferentially on the plate surface due to the energy on the plate surface. Known to do!, temperature = 110
During vacuum annealing at a temperature of 0 to 1200°C and a degree of vacuum of 10-'Torr, crystal grains with (110) planes first grow on the slopes of the sawtooth grooves, as shown in Figure 4. Therefore, the surface groove direction is set to the <(401> direction) (Zo
o) A bidirectional isotropic silicon-iron alloy plate having a <001> texture was obtained.

■ Type of annealing conditions (for example, the plate surface has (100) planes due to the energy of the plate surface. It is known that crystal grains preferentially grow. Temperature = 1000 to 1150°C, degree of vacuum: 10") Torr vacuum annealing), as shown in Figure 5, the surface groove direction is
A oriented high-silicon iron alloy plate having a (110)<001> texture in the 001> direction is obtained.

(b) Therefore, when grooving a high-silicon iron alloy plate before recrystallization annealing, the direction of easy magnetization of the oriented high-silicon iron alloy plate can be freely adjusted by appropriately setting the direction of the grooves. (C) By implementing the means shown in item (a) 62 above, oriented high silicon iron with excellent magnetic properties can be produced without being affected by the composition of the high silicon iron alloy plate or the piezoelectric conditions. Alloy plates can be stably manufactured.・After f (a)～(
The findings shown in C) were obtained.

The present invention has been made based on the above findings, and provides a high-silicon iron alloy plate containing 2 to 8% by weight of silicon, and at least a portion of the upper and lower surfaces thereof. Prepare a plate material having a sawtooth cross-section groove along the magnetization direction, or in a direction perpendicular to it, or in both directions,
In addition, by annealing at a temperature of 800 to 1300°C, a oriented high-silicon electromagnetic iron plate with excellent magnetic properties can be easily and freely set in the magnetization direction, and stably manufactured.
It has the following characteristics.

Next, in the method of this invention, Si in the high silicon iron alloy is
The method for producing a grain-oriented high-silicon electromagnetic iron plate of the present invention will be explained in more detail, along with the reasons for numerically limiting the content and annealing temperature as described above.

A) Si content of high-silicon iron alloy plate The Si component is an essential element for improving the soft magnetic properties of electromagnetic iron plates, but if its content is less than 2% by weight, r-phase will appear during high-temperature annealing. It is difficult to ensure the desired magnetic properties because the texture is broken, and on the other hand, if the Si content exceeds 8%, the iron plate becomes brittle and the saturation magnetic flux density decreases significantly. was determined to be 2 to 8% by weight.

In addition, c, NIO, S I'P 5AJt, v
Even if impurities such as d-electronic mcreNi, Cu, 5nlCQ, MO, etc. are present, the effects of the present invention are not hindered. In particular, Ni, A1. MO can be actively included in the ψ1 range of 1% by weight or less for processing properties, and V.

Mn * Cr, co 1 to improve magnetic properties
It is also possible to contain it in a range of less than % by weight.

B) Shape of surface of high-silicon iron alloy plate In the method for producing an electromagnetic iron plate of the present invention, recrystallization (: for example, the first A major feature is the use of a high-silicon iron alloy plate l with a sawtooth cross-section as shown in the figure, but the direction of the grooves is determined by the directionality plate in order to have magnetic directionality in the desired direction. Either the direction you want it to have (the direction in the plane of the plate that improves the soft magnetic properties), the direction perpendicular to that direction, or both directions.

Further, the depth of the groove is not particularly limited, and even a very fine groove with a depth of about 1 to 5 μm can exhibit a sufficient effect. If the depth of the grooves is about 1 to 5 μm, after recrystallization annealing (: without removing the grooves, it can be used as a normal electrical steel sheet). □Even in the case of iron alloy plates, after recrystallization annealing, cold rolling with a rolling ratio of about 109!1, and further strain relief annealing at about 800°C, can reduce the thickness to 1μ.
It is also easy to make a directional high silicon electromagnetic iron plate with a surface roughness of m or less.

The apex angle θ or θ'C of the sawtooth cross-sectional groove (see Fig. 1) is.

Preferably it is 90 [degrees], but 60 to 12
A sufficient effect can be obtained with an angle of about 0 degrees. And the corners don't have to be completely sharp, they can be rounded.

Furthermore, the grooves do not need to be provided on the entire surface of the high-silicon iron alloy plate; they may be provided on only one side, or may be provided on only a portion of one or both surfaces.

To form the high-silicon iron alloy plate surface C;@, the surface of the alloy plate obtained by rolling may be ground or rolled. It is advantageous to produce a plate with a defined surface shape directly from.

To obtain a directly grooved plate by the molten metal super-quenching method 52.

As shown in Figure 6, the molten metal is continuously rapidly solidified using a cooling body (such as a cooling roll) with grooves of the desired size on one surface, and the groove pattern on the surface of the cooling body is transferred to the plate surface. However, even high-silicon iron alloy plates having very fine grooves with a depth of about 1 to 20 μm can be manufactured easily and with good accuracy using this method.

C) Annealing temperature If the annealing temperature is less than 800°C, recrystallization due to surface energy will not occur sufficiently.On the other hand, annealing at a temperature exceeding 1300°C is extremely difficult for industrial purposes. was set at 800 to 1300°C.

As mentioned earlier, the annealing conditions including the annealing temperature i are such that crystal grains having (110) planes parallel to the plate surface grow preferentially, for example, temperature = 1100 to 1200.
℃ degree, dry hydrogen atmosphere or degree of vacuum: 10-6 Torr
conditions), or annealing conditions (for example, temperature:
About 1000-1150℃, degree of vacuum: l Q-"l'
Conditions for orr) may be selected as appropriate.

Without further ado, this invention will be explained in more detail with reference to Examples and in comparison with Comparative Examples. A 3% silicon steel plate (alloy A in Table 1) was prepared, hot-rolled to make one edge thick, and then cold-rolled to 0.3mm thickness (alloy A in Table 1). .5 A slightly thickened 696 silicon steel plate (Alloy B in Table 1) was surface ground to have apex angles θ and θ' of 85 to 95 [degrees] and a groove width of 20 to 20.
A sawtooth groove with a cross section of 25 μm was provided to obtain a microgrooved plate as shown in FIG.

For comparison, the surface roughness of the same material was set to 0.
A flat material with a thickness of 3 μm was also prepared.

Next, as shown in Table 2, in soft hydrogen or 10''2T
Heating temperature: 1150℃ in a vacuum of orr
, annealing was performed for a holding time of 4 hours.

For the annealed material thus obtained, the magnetic flux density at a magnetization speed of 100 A/m in the groove direction and in the direction perpendicular to the grooves was measured, and texture analysis was performed using the X-ray pole factor.

These results are also shown together with the second increase.

From the results shown in Table 2, it is clear that (
110) Since grains with two parallel planes grow preferentially,
For both alloys A and B, the surface flat material has an (ito) in-plane non-directional texture, while the 5 surface grooved material has a (100) <001> texture, with no direction in the groove direction. ξ
The magnetic flux density in two orthogonal directions is 0.33~ compared to a flat surface material.
It can be seen that the height is 0.48 T higher.

On the other hand, in a vacuum of 10-” TOrr, (10
0) Because crystal grains with parallel planes grow preferentially, a material with a flat surface has a (100) in-plane non-oriented texture, but a material with a surface groove has a (1107<001> texture). Therefore, the magnetic flux density in the groove direction is 0.12 T compared to the flat surface material.
You can see that it's getting higher.

As described above, according to the method of the present invention, grain-oriented silicon steel sheets can be stably produced without requiring strict hot rolling conditions, cold rolling conditions, or adjusting the amount of trace elements as in the past. It is clear what you get.

Example 2 First, a molten metal of high-silicon iron alloy C having the composition shown in Table 3 was prepared, and a twin-roll molten metal quenching method (on the surface,
Vertical angle = 85 to 95 [degrees], groove width: 5 μm, diameter = 100 rolls with unevenness as shown in Fig. 6), thickness: approximately 100 μm, width: approximately 1 The surface grooved ribbon was directly manufactured.

Note that the obtained grooved ribbon had almost the same irregularities as the cooling roll transferred onto its surface.

Next, this thin ribbon was placed in hydrogen with a dew point of 45°C or 10-2
When annealed at 1150°C for 4 hours in a Torr vacuum, the X-rays (200) shown in Figures 7 and 8, respectively.
As shown in the pole figures, it was confirmed that the texture was s(100)<001> or (]10)<001>.

As described above, it is clear that in the method of the present invention, the molten metal super-quenching method can be effectively utilized, and a grain-oriented high-silicon iron alloy plate can be stably obtained on an industrial scale.

Reference Example First, a molten metal of high-silicon iron alloy B having the composition shown in Table 1 was prepared, and a roll (diameter: 100 m ) with a twin roll type molten metal super-quenching device, thickness: approx. iooμ
A surface-grooved ribbon with a width of approximately ICl11 was produced directly.

When the surface and cross section of the obtained ribbon were observed under an optical microscope, it was found that the same irregularities as the surface of the cooling roll were transferred to the surface of the ribbon.

In this way, several types of thin strips were created in which the apex angle θ of the sawtooth cross-sectional grooves was varied.

Next, these thin strips were soaked in hydrogen with a dew point of 45°C for 1 hour.
After annealing at 200° C. for 4 hours, the magnetization characteristics in the longitudinal direction of the ribbon (direction of the C groove) were investigated.

The results obtained are shown in factor 9.

FIG. 9 is a graph showing the relationship between the apex angle θ and magnetic flux density (vertex angle dependence of magnetic flux density) when a magnetic field of 100 A/m is applied in the longitudinal direction of the sample. From the figure, if possible, the apex angle θ of the cross-sectional sawtooth groove is 60 to 12'0[
It can be seen that it is best to set the temperature at 80 to 100 degrees.

As mentioned above, the uneven grooves on the surface of the silicon-iron alloy plate before annealing play an important role in the method of the present invention, but in addition to those described above.

The grooves have a function of reducing seizure between each layer when the plate is annealed in a coiled or laminated form, and also have a function of preventing the annealing atmosphere from penetrating between the eyebrows and providing good results in annealing using surface energy. It also has.

<Overall Effects> As explained above, according to the present invention, it is possible to stably manufacture high-silicon electromagnetic iron sheets with excellent magnetic properties without being affected by the material composition, rolling conditions, etc. This brings about extremely useful industrial effects, such as being able to freely set the direction of easy magnetization of the produced high-silicon magnetic iron plate.

[Brief explanation of the drawing]

Figure 1 is a schematic perspective view of a plate material with grooves with a sawtooth cross-section formed on the upper and lower surfaces. Figure 2 is a schematic diagram of manufacturing a thin plate material from molten metal using the single-roll ultra-quenching method. Schematic diagram, FIG. 3 is a schematic diagram illustrating how a thin plate material is manufactured by the twin-roll ultra-quenching method. Figure 4 shows the state of crystal grains with (110) planes parallel to the plate surface, which are preferentially grown on a high-silicon iron alloy plate with saw-tooth grooves on the top and bottom surfaces! Schematic diagram. Figure 51 is a schematic diagram illustrating the state of crystal grains with (100) planes parallel to the plate surface, which are preferentially grown in a high-silicon iron alloy plate with saw-tooth grooves on the upper and lower surfaces, Figure j146. IJ! is a schematic perspective view of a cooling roll for ultra-quenching molten metal with a sawtooth-like unevenness on its surface. Figure 7 shows the (200) pole figure of the high silicon iron alloy plate after annealing in soft hydrogen in Example 2. Figure 8 shows the (200) pole figure after annealing in a 10-"l'orr vacuum in Example 2. (200) pole figure of the high silicon iron alloy plate. Figure 9 shows the magnetic properties of the high silicon iron alloy plate surface ζ= after annealing.
3 is a graph showing the dependence of a shadow-formed cross-sectional sawtooth groove on the apex angle Cθ). In rotation, 1... molten metal container, 2... molten metal spouting nozzle. 3... Cooling roll, 4... Strip-shaped thin plate product. Applicant Sumitomo Metal Industries Co., Ltd. Agent Tomi 1) Kazuo and 2 others'. Figure 4 Figure 5, ゛ Flower 6 Figure

Claims (1)

[Claims] A high-silicon iron alloy plate containing 2 to 8% by weight of silicon, and in which at least a portion of the upper and lower surfaces thereof has a cross section along a desired easy magnetization direction, a direction perpendicular thereto, or both directions. Prepare a plate material with sawtooth grooves,
A method for producing a grain-oriented high-silicon electromagnetic iron plate, which comprises annealing it at a temperature of 800 to 1300°C.