KR20160071619A - Method for manufacturing fe-based superalloy - Google Patents
Method for manufacturing fe-based superalloy Download PDFInfo
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- KR20160071619A KR20160071619A KR1020140178970A KR20140178970A KR20160071619A KR 20160071619 A KR20160071619 A KR 20160071619A KR 1020140178970 A KR1020140178970 A KR 1020140178970A KR 20140178970 A KR20140178970 A KR 20140178970A KR 20160071619 A KR20160071619 A KR 20160071619A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/28—Ferrous alloys, e.g. steel alloys containing chromium with titanium or zirconium
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Abstract
Description
More particularly, the present invention relates to an iron-based super-heat-resistant alloy, and more particularly, to a method of pulverizing a molten metal containing an oxide-forming element by a gas atomization method, whereby an oxide- And a method of manufacturing an iron-based super-heat-resistant alloy having increased strength.
The superalloy is a highly heat-resistant alloy that does not change its shape for a long time even at a high temperature of 650 ° C or higher. As a metal, iron, cobalt, nickel and the like are mainly used.
In connection with the production of a super-heat-resistant alloy, Korean Patent Laid-Open Publication No. 2011-01027430 discloses that the manufacturing process is simplified by using a vacuum spraying casting apparatus for the production of a nickel-base superalloy alloy.
Korean Patent Publication No. 2006-0106635 discloses a method of manufacturing a superalloy composition containing nickel, cobalt and tantalum by a powder metallurgy process.
Korean Patent Publication No. 1998-022301 discloses a casting method of a nickel base superalloy for turbine blades.
The nickel or nickel / cobalt superalloy alloy described above is a method of producing a superalloy by using nickel or cobalt as a main component and pulverizing a casting or an alloy.
On the contrary, the dispersion strengthening super-high temperature alloy increases the high temperature strength by finely dispersing the oxide which is not dissolved in the matrix even at a high temperature.
The dispersion-strengthening super-heat-resistant alloy as described above is produced by preparing an alloy powder of various alloys by a spraying method and then mixing and ball milling yttrium oxide or the like to produce a composite alloy powder by sintering Has been used.
However, since the alloy powder is divided into a plurality of alloy elements and powdered, and then the oxide particles are mixed together to produce a composite powder, various steps are required to produce the alloy sintered body. Therefore, And the size distribution of the particles is not uniform. Thus, there is a limit in increasing the high temperature strength.
An object of the present invention is to solve the various problems including the above problems, and it is an object of the present invention to form an iron-based alloy powder by a gas spraying method from a melt obtained by melting an alloy element forming a metal matrix and an element forming an oxide, The present invention provides a method for producing an iron-based super-heat-resistant alloy having a strengthened strength at a high temperature by a strong oxide-forming element exhibiting solid solution strengthening and dispersion strengthening effect.
A method of manufacturing an iron-based super heat resistant alloy according to an embodiment of the present invention includes the steps of preparing a molten metal alloy containing chromium (Cr), aluminum (Al), titanium (Ti), yttrium (Y) , Producing an alloy powder by gas atomization of the molten metal of the alloy, sintering the alloy powder, and rolling the sintered alloy formed by sintering.
The inside of the alloy powder produced by the gas atomization method exists not only in the state where the yttrium (Y) is dissolved, but also the yttrium oxide (Y 2 O 3 ) can be dispersed.
The iron-based powder by the gas atomization method can form a nano-scaled oxide film on the surface.
The method of manufacturing the iron-based super refractory alloy may further include ball milling the alloy powder before sintering.
The method of manufacturing the iron-based super heat resistant alloy may further include oxidizing the alloy powder before ball milling the alloy powder.
The molten metal of the alloy includes 20% by weight of Cr, 6% by weight of aluminum, 0.5% by weight of titanium and 0.5-1.3% by weight of yttrium, .
The gas spraying method may be performed at a gas pressure of 70 bar or more and a vacuum degree of 2.2 x 10 -4 torr or more.
The sintering conditions at the time of sintering the alloy powder are sintering temperature: 900 ° C. or more, degree of vacuum: 10 -2 torr or more, heating rate: 25 ° C./min, sintering time: 35 minutes or more, and spark plasma sintering Lt; / RTI >
The rolling may include hot rolling and cold rolling, and the hot rolling may have a thickness reduction ratio of 90% or more at 1,050 ± 50 ° C, and the cold rolling may have a thickness reduction ratio of 10% or more at a temperature below the recrystallization temperature.
In the ball milling, the ratio of the alloy powder to the ball mill by the gas spraying method is 1: 5, and the ball milling time is 100 minutes or more.
The oxidation of the alloy powder may be carried out at a temperature of 980 캜 or higher for 1 to 5 hours in an atmosphere gas composed of argon and 20% by volume of oxygen.
According to the method for producing an iron-based super-heat-resistant alloy according to the present invention, a powder obtained by gas-atomizing a molten metal in which an element forming an oxide is dissolved together with a matrix metal is used to produce a solid solution of an oxide- By simultaneously realizing strengthening and dispersion strengthening, a heat-resistant alloy having high strength at high temperature can be economically produced.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a view showing a manufacturing process of an iron-based heat resistant alloy according to the present invention. FIG.
FIG. 2 is a view showing a powder produced by a gas spraying method of a molten alloy when forming a powder for the production of an iron-based super heat resistant alloy according to the present invention.
FIG. 3 is a graph showing an increase in specific mass according to oxidation time when an alloy powder of an iron-based super heat resistant alloy according to the present invention is oxidized.
FIG. 4 is a view showing a structure after ball milling by high energy ball milling of a post oxidation iron-based alloy powder after gas spraying. FIG.
5 is a scanning electron microscope (SEM) photograph of a sintered body obtained by spark plasma sintering a powder obtained by gas spraying and a powder obtained by oxidizing the powder after gas spraying.
6 is a view showing the microstructure of a sintered body obtained by sintering and rolling an alloy powder prepared by a gas atomization method of a molten iron-based alloy having different contents of yttrium (Y).
7 is a graph showing the density according to the yttrium content of the powder by the gas atomization method and the powder after the gas atomization.
8 is a graph showing the change in hardness (H R C) according to the yttrium content of a powder obtained by gas spraying and a powder oxidized after gas spraying.
9 is a graph showing the results of a tensile test according to the yttrium content of powders obtained by gas spraying and powders oxidized after gas spraying.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Some embodiments of the present invention are provided to more fully describe the present invention to those skilled in the art, and the following embodiments may be modified in various other forms, The present invention is not limited to the following examples. Rather, these embodiments are provided so that this disclosure will be more thorough and complete, and will fully convey the concept of the invention to those skilled in the art. In the drawings, the thickness and size of each layer are exaggerated for convenience and clarity of explanation.
It is to be understood that throughout the specification, when an element such as a film, region or substrate is referred to as being "on", "connected to", "laminated" or "coupled to" another element, It is to be understood that elements may be directly "on", "connected", "laminated" or "coupled" to another element, or there may be other elements intervening therebetween. On the other hand, when one element is referred to as being "directly on", "directly connected", or "directly coupled" to another element, it is interpreted that there are no other components intervening therebetween do. Like numbers refer to like elements. As used herein, the term "and / or" includes any and all combinations of one or more of the listed items.
Although the terms first, second, etc. are used herein to describe various elements, parts, regions, layers and / or sections, these elements, parts, regions, layers and / It is self-evident. These terms are only used to distinguish one member, component, region, layer or section from another region, layer or section. Thus, a first member, component, region, layer or section described below may refer to a second member, component, region, layer or section without departing from the teachings of the present invention.
Also, relative terms such as "top" or "above" and "under" or "below" can be used herein to describe the relationship of certain elements to other elements as illustrated in the Figures. Relative terms are intended to include different orientations of the device in addition to those depicted in the Figures. For example, in the figures the elements are turned over so that the elements depicted as being on the top surface of the other elements are oriented on the bottom surface of the other elements. Thus, the example "top" may include both "under" and "top" directions depending on the particular orientation of the figure. If the elements are oriented in different directions (rotated 90 degrees with respect to the other direction), the relative descriptions used herein can be interpreted accordingly.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the singular forms "a," "an," and "the" include singular forms unless the context clearly dictates otherwise. Also, " comprise "and / or" comprising "when used herein should be interpreted as specifying the presence of stated shapes, numbers, steps, operations, elements, elements, and / And does not preclude the presence or addition of one or more other features, integers, operations, elements, elements, and / or groups.
Hereinafter, some embodiments of the present invention will be described with reference to the drawings schematically illustrating ideal embodiments of the present invention. In the figures, for example, variations in the shape shown may be expected, depending on manufacturing techniques and / or tolerances. Accordingly, the embodiments of the present invention should not be construed as limited to the particular shapes of the regions illustrated herein, but should include, for example, changes in shape resulting from manufacturing.
1 is a view showing a manufacturing process of an iron-based super heat resistant alloy according to the present invention.
As shown in FIG. 1, the method for producing an iron-based super-heat resistant alloy according to the present invention is a method for producing a superalloy alloy of chrome (Cr), aluminum (Al), titanium (Ti), yttrium (Y) A step (S20) of preparing an alloy powder by gas atomization of the molten alloy, a step (S30) of sintering the alloy powder, and a step of rolling the alloy sintered body formed by sintering (Step S40).
The basic components of the iron-based super heat resistant alloy according to the present invention include Cr, Al, Ti, Y and Fe.
The inside of the alloy powder produced by the gas atomization method is characterized in that not only yttrium (Y) is present in a solid state but also yttrium oxide (Y 2 O 3 ) is dispersed.
In the present invention, unlike the conventional case, the oxide (Y 2 O 3 ) of yttrium (Y), which is a strong oxide-forming element, is not mixed with the powder of the alloy elements constituting the metal matrix but the yttrium is mixed with the alloy element And spraying the molten molten metal together with the molten metal.
During the formation of the iron-based powder by the gas atomization method, yttrium is dispersed in the iron-based alloy powder while forming a fine oxide, and yttrium which is not oxidized is solid-dissolved in the matrix of the metal matrix in the iron- .
In addition, a very fine thickness nano-scaled oxide film is formed on the surface of the powder during the production of the iron-based powder by the gas atomization method.
The method of manufacturing the iron-based super-heat resistant alloy further includes ball milling the alloy powder before sintering. In this case, the size and distribution of the powder can be more uniformly maintained by ball milling, The illuminance can be improved.
Further, the method of manufacturing the iron-based super-heat-resistant alloy further includes oxidizing the alloy powder before ball milling the alloy powder, thereby adjusting the thickness of the nano-scale oxide film formed on the surface of the iron- It is possible to change the physical properties of the substrate.
In this case, the thickness of the oxide film of the iron-based alloy powder by post oxidation can be adjusted from 50 nm (initial) to 500 nm in the case of gas spraying.
The molten metal of the alloy includes 20% by weight of Cr, 6% by weight of aluminum, 0.5% by weight of titanium and 0.5-1.3% by weight of yttrium, By controlling the content of yttrium to 0.5 to 1.3 wt%, it is possible to control the effect of solid solution strengthening and dispersion by yttrium.
When the content of yttrium is less than 0.5% by weight, the amount of the oxide dispersion required for the strength increase is small and the desired high temperature strength can not be increased. When the content of yttrium is more than 1.3% by weight, This is because the increase in the high-temperature strength due to the increase in the bulk density is saturated and is not economical.
The gas atomization is performed at a gas pressure of 70 bar or more and a vacuum degree of 2.2 × 10 -4 torr or more and a gas pressure of 70 bar or more and a degree of vacuum of 2.2 × 10 -4 torr or more, A nanoscale oxide layer of an appropriate size can be formed on the surface.
The sintering conditions for the sintering are as follows: sintering temperature: 900 ° C. or more, degree of vacuum: 10 -2 torr or more, heating rate: 25 ° C./min, sintering time: 35 minutes or more and spark plasma sintering .
The rolling includes hot rolling and cold rolling, wherein the hot rolling is performed at a temperature reduction ratio of 90% or more in a temperature range of 1,050 占 폚 to 50 占 폚, and the cold rolling has a thickness reduction ratio of 10% or more at a temperature below the recrystallization temperature.
The strength of the super refractory alloy can be further increased by increasing the bonding force between the sintered particles by rolling the sintered body of the sintered alloy powder.
In the ball milling, the ratio of the alloy powder to the ball mill by the gas spraying method is 1: 5, the ball milling time is 100 minutes or more, and the ball mill is a ball mill made of stainless steel.
The oxidation of the alloy powder is performed at a temperature of 980 DEG C or higher for 1 to 5 hours in an atmosphere of argon and 20 vol% oxygen, and the growth rate of the oxide film is controlled to be constant You can adjust it at one speed.
Hereinafter, a method for producing an iron-based super heat resistant alloy according to the present invention will be described in detail with reference to the following examples.
<Examples>
(Y) are 0.5%, 0.8% and 1.3%, respectively, and the balance is composed of iron (Fe) in an amount of 20% by weight of chromium (Cr), 6% And melted at 1,700 DEG C to prepare a 10-kg molten metal.
The melt was gas sprayed at a gas pressure of 70 bar and a vacuum of 2.2 x 10 <" 4 & gt ;.
Fig. 2 shows the shape of the iron-based alloy powder formed by the gas atomization method, and Table 1 summarizes the main alloy components (% by weight) of the iron-based alloy powder.
The iron-based powder produced by the gas atomization method was heated to 980 ° C and oxidized. At this time, the heating rate was 5 ° C / min, and the atmosphere was controlled with argon gas and 20% by volume of oxygen.
3 and FIG. 2 show the increase in specific mass with respect to the oxidation time when the powder produced by the gas atomization method is oxidized (at 980 ° C).
After the oxidation to powder was completed, high energy ball milling was performed. The conditions of the ball milling were such that the volume ratio of the iron-based alloy powder to the ball milling ball was 1: 5, the ball mill used was stainless ball, and the mass of the iron-based powder and the stainless steel ball was 60 g: 500 g.
Ball milling was done in wet corrosion of alcohol.
4 shows the particle size after high-energy ball milling of the iron-based alloy powder produced by the gas atomization method.
FIG. 4 shows particles after ball milling of the iron-based powder subjected to oxidation treatment for 5 hours. It can be seen that particles oxidized by high-energy ball milling are finely pulverized. From the bulk form having a particle size of 40 μm or more, Is contained in a form of 5-20 mu m fragment.
After the oxidation treatment, the iron - based alloy powder having high - energy ball milling was sintered in a disk shape by spark plasma sintering. The sintering conditions were a temperature range of 900-950 ℃, a heating rate of 31 ℃ / min and a pressure of 52 MPa.
Then, the iron-based powder was rolled. Rolling was performed by sintering the powder produced by the gas atomization method and by sintering the ball milled powder after oxidizing the produced powder.
Fig. 6 is a diagram showing a structure obtained by sintering and rolling the iron-based alloy powder produced by the gas atomization method. The average oxide size is in the range of 0.503 nm-0.978 nm and the mean grain boundary width is 2.99 탆 - 4.59 탆 .
Then, the mechanical properties such as density, hardness, tensile strength and elongation were evaluated for each powder.
7 and the following Table 3 show the densities after sintering and the densities after rolling of the powders produced by the gas atomization method and the powders oxidized after the gas atomization.
8 and Table 4 are obtained by evaluating the hardness after rolling the sintered body of the powder produced by the gas spraying method and the powder oxidized after the gas spraying.
As shown in FIG. 8 and Table 4, it can be seen that the hardness of the sintered body after sintering after oxidation after gas spraying is higher than that of rolling the sintered body after sintering after gas spraying. It is considered that the hardness of the sintered body is increased due to the formation of the oxide film or the formation of the oxide-forming element by the oxidation of the powder produced by gas spraying, and the dispersion of the oxide having a high hardness in the sintered body.
9 and Table 5 show the tensile test results of the product obtained by rolling the sintered body of the powder produced by the gas atomization method and the powder after oxidized after the gas atomization.
As a result of evaluation of physical properties of the sintered body at room temperature (300K), the yield strength and tensile strength of the powder sprayed with gas were higher than that of the comparative example (MA956), and the elongation was relatively low.
In addition, the yield strength of the powder rolled after oxidation for 5 hours is very low and the elongation is also low.
As a result of evaluation of physical properties of the sintered body at a high temperature (773K) by tensile test, it was found that the tensile strength of the powder sprayed with gas was much higher than that of the comparative example (M956).
As a result of evaluation of physical properties of the sintered body after sintering the powder oxidized for 5 hours, the tensile strength was found to be very low as compared with the comparative example.
While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the invention. Accordingly, the true scope of the present invention should be determined by the technical idea of the appended claims.
Claims (11)
Preparing an alloy powder by the gas atomization of the molten alloy;
Sintering the alloy powder; And
And rolling the alloy sintered body formed by sintering
A method for producing an iron-based super heat resistant alloy.
Wherein the inside of the alloy powder produced by the gas atomization method is not only present in a state in which yttrium (Y) is solved, but also in which yttrium oxide (Y 2 O 3 ) is dispersed.
Wherein the iron-based powder by the gas atomization method has a nano-scaled oxide film on the surface thereof.
Further comprising ball milling the alloy powder before sintering the alloy powder.
Further comprising the step of oxidizing the alloy powder before ball milling the alloy powder.
The molten metal of the alloy includes 20% by weight of Cr, 6% by weight of aluminum, 0.5% by weight of titanium and 0.5-1.3% by weight of yttrium, Based alloy. ≪ RTI ID = 0.0 > 11. < / RTI >
Wherein the gas spraying method is performed at a gas pressure of 70 bar or more and a vacuum degree of 2.2 × 10 -4 torr or more.
The sintering conditions for the sintering are as follows: sintering temperature: 900 ° C. or more, degree of vacuum: 10 -2 torr or more, heating rate: 25 ° C./min, sintering time: 35 minutes or more and spark plasma sintering Based alloy.
Wherein the rolling includes hot rolling and cold rolling, wherein the hot rolling is performed at a temperature reduction ratio of 90% or more in a temperature range of 1,050 占 폚 to 50 占 폚, and the thickness reduction ratio is 10% or more at a temperature lower than the recrystallization temperature. Gt;
Wherein the ball milling is performed at a ratio of the alloy powder to a ball mill by a gas spraying method of 1: 5 and a ball milling time is 100 minutes or more.
Wherein the oxidation of the alloy powder is carried out at a temperature of 980 캜 or higher for 1 to 5 hours in an atmosphere of argon and 20% by volume of oxygen.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102370831B1 (en) * | 2020-10-26 | 2022-03-07 | 한국생산기술연구원 | Nanoparticle dispersion strengthened titanium powder with improved uniformity and manufacturing method thereof |
| KR102370830B1 (en) * | 2020-10-26 | 2022-03-07 | 한국생산기술연구원 | Nanoparticle dispersion strengthened titanium powder and manufacturing method thereof |
| KR102370832B1 (en) * | 2020-10-26 | 2022-03-07 | 한국생산기술연구원 | Nanoparticle dispersion strengthened composite powder and manufacturing method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102370831B1 (en) * | 2020-10-26 | 2022-03-07 | 한국생산기술연구원 | Nanoparticle dispersion strengthened titanium powder with improved uniformity and manufacturing method thereof |
| KR102370830B1 (en) * | 2020-10-26 | 2022-03-07 | 한국생산기술연구원 | Nanoparticle dispersion strengthened titanium powder and manufacturing method thereof |
| KR102370832B1 (en) * | 2020-10-26 | 2022-03-07 | 한국생산기술연구원 | Nanoparticle dispersion strengthened composite powder and manufacturing method thereof |
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