KR100701413B1 - Amorphous powder flakes and their preparation method thereof - Google Patents

Abstract

In the present invention, the amorphous alloy prepared by quench solidification using a high energy mill to prepare a flake-shaped amorphous powder. The amorphous powder flakes prepared using the high energy mill of the present invention can be usefully applied to the production of electromagnetic wave absorption thin films.

Amorphous powder, high energy wheat, flake

Description

Amorphous powder flakes and its manufacturing method {AMORPHOUS POWDER FLAKES AND THEIR PREPARATION METHOD THEREOF}

1 is a scanning electron micrograph of 89.4Fe-8.3Si-2.3B amorphous powder prepared by a gas spray method.

FIG. 2 is a scanning electron micrograph of 89.4Fe-8.3Si-2.3B amorphous powder of Flake shape.

3 is an XRD pattern of 89.4Fe-8.3Si-2.3B amorphous powder in the shape of a Flake.

4 is a scanning electron micrograph of an Flake-shaped 90.4Fe-6.1Si-3.5B amorphous powder.

5 is a scanning electron micrograph of an Flake-shaped 90.4Fe-7.6Si-2.0B amorphous powder.

Fig. 6 is a scanning electron micrograph of 83.5Fe-7.7Nb-5.6Si-3.2B amorphous powder in Flake shape.

FIG. 7 is a scanning electron micrograph of 82.7Fe-5.7Nb-8.0Si-2.2B-1.3Cu amorphous powder in Flake shape. FIG.

Fig. 8 is a scanning electron micrograph of 86.1Fe-8.0Si-3.4B-2.0Cr-0.5C amorphous powder of Flake shape.

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to flake shaped amorphous powders prepared using high energy mills, and more particularly, to amorphous powder flakes suitable for electromagnetic wave absorbing thin films and a method of manufacturing the same.

The electromagnetic wave absorbing thin film having a function of absorbing electromagnetic waves in various electric and electronic devices is manufactured in a film form by dispersing and mixing a thin flake soft crystalline soft magnetic powder in a polymer resin as a filler. With the development of electrical and electronic devices, the frequency bands of these devices become high and the frequency of next-generation information and communication devices increases, resulting in noise in the high frequency bands, resulting in malfunction and deterioration of electrical and electronic devices. Has emerged seriously, and a new electromagnetic wave absorption thin film that can cope with this is needed. Amorphous soft magnetic alloys have excellent corrosion resistance, abrasion resistance, strength, and the like compared to crystalline materials, and have high permeability and high frequency characteristics, and thus can be used as magnetic elements of various devices of electrical and electronic devices.

 In order to use the soft magnetic amorphous alloy in the electromagnetic wave absorption thin film, it has to be manufactured in the shape of a thin flake like the crystalline soft magnetic alloy. However, unlike crystalline materials, amorphous alloys have a large elastic limit and hardly undergo plastic deformation, making it difficult to prepare flaky amorphous powders.

Therefore, an object of the present invention is to solve the problems of the prior art as described above, and to manufacture a flake-shaped amorphous powder flaky with respect to an amorphous alloy at low cost.

The object of the present invention as described above is achieved by providing an amorphous powder flake having a high aspect ratio and a method for producing the same by changing the shape of the amorphous powder using an amorphous powder as a high energy mill.

Amorphous powder flakes having a high appearance ratio according to the present invention have a flake shape having a thickness of about 0.1 to 5 μm by milling a high-energy mill with an amorphous powder having a particle size of 200 μm or less prepared by rapid solidification. It is to prepare an amorphous powder.

In the milling process, the flakes of the amorphous powder are preferably set to 7 hours or less at 1000 rpm or less. Larger rotational speeds of the high energy mills or longer milling times are not preferred because the amorphous powder is not flaked and pulverized into small powders.

In one embodiment of the present invention, the amorphous powder contains iron (Fe) as a main component, and includes silicon (Si) and boron (B), that is, Fe-Si-B-based amorphous powder was used.

In the case of Fe-Si-B-based amorphous powder, the composition is preferably 88.5-90.5% by weight, 6.0-9.0% by weight and 2.0-3.5% by weight of Fe, Si and B.

However, in the present invention, the amorphous powder is not limited to having the composition as described above, and includes a metal selected from the group consisting of Zr, Cu, Fe, Al, Ti, Mg, Ln, Pd, Co, and Ni as a main component. Zr-Cu-Ni-Al-Ti-based, Zr-Ti-Cu-Ni-Be-based, Zr-Al-Ni-Cu-based, Zr-Ti-Nb-Ni-Cu-Be-based, Cu-Ti-Zr- Ni- (Sn) -Si-based, Fe-Cr-Mo-CB-based, Fe-B-Si-based, Fe-Si-BC-based, Fe-Si-BCP-based, Fe-Cr-B-Si-C-based, Fe-Si-B-Nb-based, Fe-Zr-B- (Ni) -based, Fe-Cu-Nb-Si-B-based, Fe-Co-Ni-Zr-B-based, Fe-Al-B- (Nb , Cu) -based, Fe-Nb-B-based, Fe-Zr-B-Cu-based, Fe-Cr-Mo-CB-based, Al-La (Ce, Y) -Ni-based, Ti-Cu-Ni-Sn- Be-Zr-based, Ti-Zr-Cu-Ni-based, Mg-Cu (Ni) -Ag-Y (Ce) -based, Mg-Ca-Al-based, La-Al-Ni-based, Pd-Ni-Cu-P Type, Pd-Ni-P type, Co-Fe-Si-B type, Co-Fe-Ni- (Mo) -B-Si type, Ni-Cr-Fe-Si-B type, Ni-Nb-Cr- All possible types of amorphous powders can be included, including Mo-PB-based and Ni-B-Si-based amorphous powders.

Flakes amorphous powder and a method for producing the same according to the present invention

(1) to prepare an amorphous powder by rapid solidification,

(2) obtaining the amorphous powder flakes by changing the shape of the amorphous powder obtained in the step (1) using a high energy mill.

Step (1) includes preparing an alloy of the required composition according to high frequency vacuum induction melting, and rapidly solidifying it to convert it into an amorphous powder.

Rapid solidification of step (1) may be performed by water atomization, gas atomization, centrifugal atomization, or melt spinning and then grinding. In the case of gas spraying among these methods, irgon gas, helium gas or nitrogen gas may be used, and the pressure is preferably 30 to 100 bar. The amorphous powder prepared in this way has a particle size of 200 μm or less.

In the step (2) it is possible to obtain an amorphous powder flake by changing the shape of the amorphous powder using a high energy mill.

Among them, it is preferable to dry or wet the amorphous powder using the high energy mill in the step (2) using a ball mill or an attrition mill or the like. In the embodiment of the present invention was used Symoloyer, a high energy mill from Zoz, Germany. In this case, it is preferable that the flake forming conditions of the amorphous powder be within 7 hours at 1000 rpm or less.

Hereinafter, the present invention will be described in more detail with reference to Examples, but the Examples are only illustrative of the present invention, and the scope of the present invention is not limited thereto.

Example 1

The powder of amorphous powder having a composition of 89.4Fe-8.3Si-2.3B having a weight ratio of 89.4: 8.3: 2.3 of Fe: Si: B prepared by gas atomization was prepared using high energy mill. Flaking was performed. FIG. 1 is a scanning electron microscope photograph of 89.4Fe-8.3Si-2.3B amorphous powder prepared by gas atomization, and is close to a spherical shape.

89.4Fe-8.3Si-2.3B amorphous powder was milled by dry method under argon (Ar) atmosphere for 7 hours at a rotational speed of 1000 rpm or less, preferably 6 hours at 600 rpm using Symoloyer, a high energy mill. . Figure 2 shows a scanning electron micrograph of 89.4Fe-8.3Si-2.3B amorphous powder flakes obtained by this method. It can be seen that the shape of the powder was changed from the spherical shape to the shape of flakes having a thickness of about 1 μm by the flattening process. FIG. 3 shows that the amorphous phase is maintained as it is after the flaking process as an XRD pattern of amorphous powder flakes.

Example 2

The same procedure as in Example 1 was repeated except that 90.4Fe-6.1Si-3.5B amorphous powder was used instead of 89.4Fe-8.3Si-2.3B amorphous powder. Figure 4 shows a scanning electron micrograph of 90.4Fe-6.1Si-3.5B amorphous powder flakes obtained by this method.

Example 3

The same procedure as in Example 1 was repeated except that 90.4Fe-7.6Si-2.0B amorphous powder was used instead of 89.4Fe-8.3Si-2.3B amorphous powder. Figure 5 shows a scanning electron micrograph of the 90.4Fe-7.6Si-2.0B amorphous powder flakes obtained by this method.

Example 4

The same procedure as in Example 1 was carried out except that 83.5Fe-7.7Nb-5.6Si-3.2B amorphous powder was used instead of the 89.4Fe-8.3Si-2.3B amorphous powder. Figure 6 shows a scanning electron micrograph of the 83.5Fe-7.7Nb-5.6Si-3.2B amorphous powder flakes obtained by this method.

Example 5

The same procedure as in Example 1 was carried out except that 82.7Fe-5.7Nb-8.0Si-2.2B-1.3Cu amorphous powder was used instead of the 89.4Fe-8.3Si-2.3B amorphous powder. Figure 7 shows a scanning electron micrograph of the 82.7Fe-5.7Nb-8.0Si-2.2B-1.3Cu amorphous powder flakes obtained by this method.

Example 6

The same procedure as in Example 1 was repeated except that 86.1Fe-8.0Si-3.4B-2.0Cr-0.5C amorphous powder was used instead of the 89.4Fe-8.3Si-2.3B amorphous powder. The milling was carried out in the same manner as in Example 1 except that at a rotational speed of 600 rpm for 7 hours at 700 rpm instead of 6 hours. Figure 8 shows a scanning electron micrograph of the 86.1Fe-8.0Si-3.4B-2.0Cr-0.5C amorphous powder flakes obtained by this method.

In the above embodiment, only the amorphous powder flake and its manufacturing method using high-energy mill from the amorphous powder containing Fe as a main component are described to those skilled in the art. It will be apparent that it can be applied to the preparation of amorphous powder flakes from a series of amorphous powders.

Amorphous flakes, which have a high elastic limit and hardly undergo plastic deformation, are difficult to produce into flaky flake shapes in an economical manner. The amorphous powder flakes according to the present invention may be particularly useful as soft magnetic amorphous powder flakes that can be used for producing electromagnetic wave absorbing thin films.

Claims (16)

A first step of rapidly solidifying the amorphous alloy to obtain spherical amorphous powder, A method for preparing amorphous powder flakes comprising milling the spherical amorphous powder using a high energy mill to obtain amorphous powder flakes flaky 0.1 to 5 μm thick. The method of claim 1, wherein the amorphous powder in the first step comprises at least one selected from Fe, Si, B, Cr, C, Nb, and Cu. The method for preparing amorphous powder flakes according to claim 1, wherein in the first step, the amorphous powder has Fe, Si, and B content of 88.5 to 90.5 wt%, 6.0 to 9.0 wt%, and 2.0 to 3.5 wt%, respectively. The method for preparing amorphous powder flakes according to claim 1, wherein the content of Fe, Si, B and Nb in the amorphous powder in the first step is 83.5 wt%, 5.6 wt%, 3.2 wt% and 7.7 wt%, respectively. The amorphous powder flakes according to claim 1, wherein the content of Fe, Si, B, Nb, and Cu in the amorphous powder in the first step is 82.8 wt%, 8.0 wt%, 2.2 wt%, 5.7 wt%, and 1.3 wt%, respectively. Manufacturing method. The amorphous powder flakes according to claim 1, wherein the contents of Fe, Si, B, Cr and C in the amorphous powder in the first step are 86.1 wt%, 8.0 wt% and 3.4 wt%, 2.0 wt% and 0.5 wt%, respectively. Manufacturing method. The method for preparing amorphous powder flakes according to claim 1, wherein the amorphous powder of the first step is obtained by pulverizing a melt of an alloy composed of constituents of the amorphous powder after gas spraying, centrifugal spraying, water spraying, or melt spinning. The method of claim 1, wherein the particle size of the amorphous powder in the first step is 200 μm or less. delete The method of claim 1, wherein the high energy mill is performed using a Symoloyer (high energy mill manufactured by Zoz, Germany), a ball mill or an attrition mill. The method for preparing amorphous powder flakes according to claim 10, wherein the milling is performed within 7 hours at 1000 rpm or less when using Symoloyer (high energy mill manufactured by Zoz, Germany). The method for preparing amorphous powder flakes according to claim 10, wherein the milling is performed by a dry or wet method. According to claim 1, wherein the amorphous powder is Zr-Cu-Ni-Al-Ti containing as a main component a metal selected from the group consisting of Zr, Cu, Fe, Al, Ti, Mg, Ln, Pd, Co and Ni-based Zr-Ti-Cu-Ni-Be, Zr-Al-Ni-Cu, Zr-Ti-Nb-Ni-Cu-Be, Cu-Ti-Zr-Ni- (Sn) -Si, Fe-Cr-Mo-CB-based, Fe-B-Si-based, Fe-Si-BC-based, Fe-Si-BCP-based, Fe-Cr-B-Si-C-based, Fe-Si-B-Nb-based, Fe-Zr-B- (Ni) -based, Fe-Cu-Nb-Si-B-based, Fe-Co-Ni-Zr-B-based, Fe-Al-B- (Cu, Nb) -based, Fe-Nb- B-based, Fe-Zr-B-Cu-based, Fe-Cr-Mo-CB-based, Al-La (Ce, Y) -Ni-based, Ti-Cu-Ni-Sn-Be-Zr-based, Ti-Zr- Cu-Ni, Mg-Cu (Ni) -Ag-Y (Ce), Mg-Ca-Al, La-Al-Ni, Pd-Ni-Cu-P, Pd-Ni-P, Co-Fe-Si-B-based, Co-Fe-Ni- (Mo) -B-Si-based, Ni-Cr-Fe-Si-B-based, Ni-Nb-Cr-Mo-PB-based and Ni-B- A method for producing amorphous powder flakes, which is any one selected from Si-based. delete delete delete

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