KR20160077465A - Fe-Ni ALLOY HAVING EXCELLENT CURL PREVENTING PROPERTY AND METHOD FOR MANUFACTURING THE SAME - Google Patents

Abstract

The present invention relates to an Fe-Ni alloy used for an electronic device such as an organic light emitting diode (OLED), a secondary battery, a solar battery, or the like; and a method to manufacture the same. According to the present invention, a method to manufacture the Fe-Ni alloy having excellent curl preventing property comprises: a step of manufacturing the Fe-Ni alloy; and a step of heat treating the Fe-Ni alloy.

Description

FIELD OF THE INVENTION [0001] The present invention relates to a Fe-Ni alloy having excellent anti-

The present invention relates to an Fe-Ni alloy used for an electronic device such as an organic light emitting diode (OLED), a secondary battery, and a solar cell, and a method of manufacturing the same.

The Fe-Ni alloy has a low coefficient of thermal expansion (CTE) and is used as an encapsulating material for an organic light-emitting diode and a fine metal mask (FMM), and is attracting attention as a collector of a secondary battery or a substrate of an electronic device It is a situation.

Meanwhile, as a method for producing the Fe-Ni alloy, there is a method of casting iron and nickel into ingot, and rolling and annealing repeatedly to form a thin film. The Fe-Ni alloy thus produced has a high elongation percentage and has an advantage that the surface is smooth and cracks are not generated. However, according to the above-mentioned method, it is difficult to manufacture Fe-Ni alloy having a width of 1 m or more due to mechanical limitations at the time of manufacturing, and it is difficult to manufacture the Fe-Ni alloy at a certain thickness or less.

Recently, Fe-Ni alloy thin films should be economically provided to meet the trend of thinning of displays and electronic devices. Therefore, EF (Electro-Forming) has been emphasized as an Fe-Ni alloy manufacturing method which can relatively easily adjust the thickness with low manufacturing cost.

The Fe-Ni alloy manufacturing method using the electroforming method is characterized in that a negative electrode of a drum or belt type provided in an electrolytic bath containing an electrolytic solution and a pair of arc-shaped positive electrodes opposed to the negative electrode are provided, and the electrolytic solution is continuously supplied And electroplating the Fe-Ni alloy on the surface of the negative electrode drum by applying current.

On the other hand, in the case of the Fe-Ni alloy thin film, a curl called curl is generated. When the curling property is increased, damage to the precision equipment in the process such as photoresist coating of the etching process And the patterning may not be constant.

One aspect of the present invention is to provide an iron-nickel alloy having excellent anti-curl property, and a method of manufacturing the Fe-Ni alloy using the electroforming (EF) method.

One aspect of the present invention relates to a method of manufacturing an iron-nickel (Fe-Ni) alloy, the method comprising: preparing an iron-nickel (Fe-Ni) alloy using electroplating (EF); And

And a step of heat-treating the iron-nickel alloy at a temperature of 300 to 400 ° C for 1 to 60 minutes, wherein the iron-nickel alloy is excellent in anti-curling properties.

Another aspect of the present invention provides an iron-nickel alloy produced by the electroforming (EF) method and excellent in anti-curl property with a grain size of 15 to 100 nm.

The Fe-Ni alloy thin film of the present invention is dense in structure through heat treatment, minimizes internal stress, and can suppress curling. Therefore, it is possible to realize an electronic device such as a display, a battery and the like having a curl-preventing property of the same level as that of the Fe-Ni alloy thin film manufactured through a rolling process at a low cost.

The Fe-Ni alloy produced by Electroforming (EF) is a nanocrystalline material having a crystal grain size of about 10 nm. These nanocrystalline Fe-Ni alloys have higher mechanical properties than rolled materials of the same composition produced by the conventional rolling process. However, Fe-Ni alloys having such nano-sized crystal grains have a problem of showing rapid thermal behavior due to a change in crystal structure at a certain temperature. In general, the Fe-Ni alloy produced by electroforming (EF) may have atomic densities lower than that of rolled materials due to the addition of atoms combined by chemical methods and added during the process. In addition, since there is no diffusion process, internal stress is increased, and curling, also called curl, is likely to occur.

Accordingly, the inventors of the present invention have made studies to solve the above problems, and as a result, the present invention has been made.

Hereinafter, the present invention will be described in detail. First, the method for producing the Fe-Ni alloy of the present invention will be described in detail.

In the method for producing the Fe-Ni alloy of the present invention, an iron-nickel alloy is first prepared by the electroforming (EF) method. The electrolytic solution is produced by disposing a cathode and an anode in an electrolytic cell containing an electrolytic solution, and applying an electric potential through a current device so that the Fe-Ni alloy is electrodeposited on the surface of the cathode.

The method for producing the Fe-Ni alloy by the electrophoresis method is not particularly limited in the present invention, and a preferable example thereof is a method for producing Fe-Ni alloy according to the above electroforming method, wherein the iron concentration is 1 to 40 g / L, the nickel concentration is 5 to 80 g / , A stress relieving agent of 1.0 to 20 g / L, a conductive auxiliary agent of 5 to 40 g / L, and a Fe reducing agent of 0.2 to 3.5 g / L, and the electrolytic solution has a pH of 1.0 to 5.0, an electrolyte temperature of 40 to 90 ° C., 1 to 80 A / dm 2, and a flow rate of 0.2 to 5 m / sec.

The Fe-Ni alloy produced by the electroplating method depends on the concentration of Fe and Ni in the electrolyte, as well as the type and content of the current density, flow rate, additives, and the like. For example, when the concentration of iron in the electrolyte is increased, the Fe component of the alloy becomes higher, and when the current density becomes lower, the Fe component becomes higher.

The Fe-Ni alloy preferably contains Ni in an amount of 34 to 64% by weight and the balance of Fe and unavoidable impurities. By adjusting the components of the electrolytic solution and the process conditions, an Fe-Ni alloy of 34 to 64 wt% Ni can be produced.

The prepared Fe-Ni alloy is subjected to a heat treatment at a temperature of 300 to 400 DEG C for 1 to 60 minutes. The Fe-Ni alloy structure is stabilized through the heat treatment. That is, the size of the Fe-Ni alloy before the heat treatment is 5-15 nm, but the size of the crystal grains becomes 15-100 nm through the heat treatment.

The Fe-Ni alloy produced by the electroplating method has nanocrystalline grains of about 5 to 15 nm, so that the dislocations within the structure are produced in a state where it is difficult to move. When the heat treatment is performed, some crystal grain growth occurs, and the internal stress is relieved because the state of the potential is rearranged. That is, when heat treatment is performed at a temperature of less than 300 DEG C or less than 1 minute, sufficient crystal grains and dislocation do not arise and sufficient internal stress can not be solved. However, in the heat treatment at an excessively high temperature or for a long time, abnormal crystal grains are grown, There arises a problem that the temperature is lowered.

Hereinafter, the Fe-Ni alloy of the present invention will be described in detail. The Fe-Ni alloy of the present invention preferably contains Ni in an amount of 34 to 64 wt%, and the balance of Fe and unavoidable impurities.

The Fe-Ni alloy of the present invention preferably has a grain size of 15 to 100 nm. As described above, the Fe-Ni alloy produced by the electroplating method has a grain size of 10 nm in size, so that dislocation is hard to occur and curling due to internal stress occurs. However, in the Fe-Ni alloy of the present invention, the size of the crystal grains grows to 15-100 nm level through the heat treatment, and the decrease of the strength is minimized, so that the Fe-Ni alloy suppressing curling can be manufactured . If the crystal grains are excessively large in size, the strength is lowered.

The Fe-Ni alloy of the present invention has a characteristic that curling is reduced. In the present invention, when the Fe-Ni alloy is formed into a size of 100 X 100 mm, it is preferable that the height of the horizontally rising portion is 5 mm or less.

The thickness of the Fe-Ni alloy of the present invention is preferably 0.001 to 0.1 mm.

Hereinafter, embodiments of the present invention will be described in detail. The following examples are for the purpose of understanding the present invention and are not intended to limit the present invention.

(Example)

First, a Fe-Ni alloy thin film was prepared by using the electroplating method (EF). An electrolytic solution containing an Fe concentration of 17 g / L, an Ni concentration of 35 g / L, a stress relieving agent of 5 g / L as an additive, 20 g / L of a conductive auxiliary agent and 1.0 g / L of an antioxidant was prepared, A Fe-Ni alloy thin film was prepared on a cylindrical negative electrode made of titanium at a temperature of 65 占 폚 and a flow rate of 1.0 m / s and then peeled off to form a 20 占 퐉 thick Fe-42wt% Ni Alloy thin films were prepared.

The prepared Fe-Ni alloy thin films were subjected to heat treatment under the conditions shown in Table 1 below, and the curling phenomenon and the tensile strength of each of the specimens were measured. The results are shown in Table 1. The curling phenomenon of the present invention was measured when the specimen was made to have a size of 100 X 100 mm and the height raised horizontally.

division Heat treatment condition Average grain size (nm) Curling height (mm) Tensile Strength (GPa) Temperature (℃) Time (minutes) Comparative Example 1 - - 7.1 6 1.3 Inventory 1 300 10 18.1 One 1.2 Inventory 2 350 10 30.1 <1 1.1 Inventory 3 350 30 35.4 <1 1.1 Honorable 4 400 10 86.3 <1 1.0 Comparative Example 2 500 15 460.1 <1 0.5

As shown in the results of Table 1, in the inventive example satisfying the conditions of the present invention, it was confirmed through the stabilization of the structure that the curled height of the Fe-Ni alloy was 5 mm or less. However, in Comparative Example 1 in which heat treatment was not performed, it was confirmed that a curling height of 6 mm was generated. In Comparative Example 2 in which the heat treatment was performed in excess of the temperature suggested in the present invention, curling did not occur, I could find that there was a problem.

Claims (7)

Preparing an iron-nickel (Fe-Ni) alloy by using electroplating (EF); And
Heat-treating the iron-nickel alloy at a temperature of 300 to 400 ° C for 1 to 60 minutes
Wherein the iron-nickel alloy has an anti-curling property.
The method according to claim 1,
Wherein the iron-nickel alloy having a grain size of 5 to 15 nm before the heat treatment is excellent in the anti-curling property of the iron-nickel alloy.
The method according to claim 1,
Wherein the iron-nickel alloy contains 34 to 46% by weight of nickel (Ni), and the balance includes Fe and unavoidable impurities.
An iron-nickel alloy manufactured by electroforming (EF), excellent in anti-curl property having a grain size of 15 to 100 nm.
The method according to claim 4,
The iron-nickel alloy has excellent anti-curl property including 34 to 46% by weight of nickel (Ni) and the balance of Fe and unavoidable impurities.
The method of claim 4,
An iron-nickel alloy excellent in anti-curl property with a horizontal height of 5 mm or less when the specimen is made in the size of 100 x 100 mm of the iron-nickel alloy.
The method of claim 4,
The iron-nickel alloy has a thickness of 0.001 to 0.1 mm and is excellent in anti-curl property.