US20150354048A1 - Metal composite comprising aligned precipitate and preparation method therefor - Google Patents

Metal composite comprising aligned precipitate and preparation method therefor Download PDF

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US20150354048A1
US20150354048A1 US14/762,772 US201314762772A US2015354048A1 US 20150354048 A1 US20150354048 A1 US 20150354048A1 US 201314762772 A US201314762772 A US 201314762772A US 2015354048 A1 US2015354048 A1 US 2015354048A1
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precipitate
solid solution
alloy
creating
metal composite
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Seung Zeon HAN
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Korea Institute of Machinery and Materials KIMM
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon

Definitions

  • the present invention relates to a metal composite with an oriented precipitate and a method of manufacturing the same, and more particularly, to a metal composite with an oriented precipitate that has improved strength and electric conductivity by forcibly creating a precipitate through aging after creating a solid solution, which is created by selectively adding precipitation-promoting metal to an alloy and performing solution treatment or homogenization, and by orienting the forcibly created precipitate through plastic working, and a method of manufacturing the metal composite.
  • copper alloys are used for connectors, accumulators, or connectors for connecting a controller to various electric parts, actuators, and sensors in vehicles equipped with increased electric devices and it is strongly required to downsize these connectors.
  • connectors disposed close to an engine are exposed to the heat and vibration of the engine, and when a large amount of current is applied to the connectors, the connectors generate heat and increase the temperature to a high level. Accordingly, those connectors require high reliability under such environments.
  • a Cu—Fe—P alloy (Korean Patent No. 10-0997560) or a Cu—Mg—P alloy (Korean Patent No. 10-0417756) have been disclosed.
  • the strength of the former alloy is improved by precipitating a Fe—P compound based on the addition of both of Fe and P.
  • the latter alloy is improved in tensile strength, electric conductivity, and mitigation of stress resistance by improving strength and creeping characteristic by adding Mg and P.
  • copper alloys can improve its electric conductivity, thermal stability, and strength by adding various components.
  • An object of the present invention is to provide a metal composite with an oriented precipitate that has improved strength and electric conductivity by forcibly creating a precipitate through aging after creating a solid solution, which is created by selectively adding precipitation-promoting metal to an alloy and performing solution treatment or homogenization, and by orienting the forcibly created precipitate through plastic working, and a method of manufacturing the metal composite.
  • the present invention provides a metal composite with an oriented precipitate, in which a solid solution is created by performing solution treatment or homogenization on an alloy, a discontinuous cellular precipitate or lamellar precipitate of 40% or more per unit area of 500 ⁇ m ⁇ 500 ⁇ m is forcibly created by aging, and the forcibly created precipitate is oriented by plastic working.
  • the present invention provides a metal composite with an oriented precipitate, in which a solid solution is created by performing solution treatment or homogenization on an alloy, a discontinuous cellular precipitate or lamellar precipitate of 40% or more per unit area of 630 ⁇ m ⁇ 480 ⁇ m is forcibly created by aging, and the forcibly created precipitate is oriented by plastic working.
  • the present invention provides a metal composite with an oriented precipitate, in which a solid solution is created by performing solution treatment or homogenization on an alloy, a discontinuous cellular precipitate or lamellar precipitate is forcibly created by aging, and the forcibly created precipitate is oriented by plastic working to have a length of 2.0 ⁇ m or more per unit area of 3.5 ⁇ m ⁇ 1.5 ⁇ m in a copper base.
  • the oriented precipitate has a length to diameter aspect ratio of 100 or more.
  • the alloy that became the solid solution is rapidly cooled by water quenching or cooled by air.
  • the aging is performed for three hours or more.
  • Precipitation-promoting metal is added in the solution treatment or homogenization process.
  • the precipitation-promoting metal includes any one of titanium (Ti) and vanadium (V).
  • the present invention provides a method of manufacturing a metal composite with an oriented precipitate which includes: a material preparing step of preparing a molded alloy; a solid solution creating step of creating a solid solution by performing heat treatment on the alloy in a single phase area; a precipitate forcible-creating step of creating a cellular precipitate or a lamellar precipitate of 40% or more per unit area of 500 ⁇ m ⁇ 500 ⁇ m by aging the alloy containing the solid solution; and a precipitate orienting step of orienting the precipitate by performing plastic working on the alloy containing the precipitate.
  • the present invention provides a method of manufacturing a metal composite with an oriented precipitate which includes: a material preparing step of preparing a molded alloy; a solid solution creating step of creating a solid solution by performing heat treatment on the alloy in a single phase area; a precipitate forcible-creating step of creating a cellular precipitate or a lamellar precipitate of 40% or more per unit area of 630 ⁇ m ⁇ 480 ⁇ m by aging the alloy containing the solid solution; and a precipitate orienting step of orienting the precipitate by performing plastic working on the alloy containing the precipitate.
  • the present invention provides a method of manufacturing a metal composite with an oriented precipitate which includes: a material preparing step of preparing a molded alloy; a solid solution creating step of creating a solid solution by performing heat treatment on the alloy in a single phase area; a precipitate forcible-creating step of creating a cellular precipitate or a lamellar precipitate of 40% or more per unit area of 630 ⁇ m ⁇ 480 ⁇ m by aging the alloy containing the solid solution; and a precipitate orienting step of orienting the precipitate to have a length of 2.0 ⁇ m or more per unit area of 3.5 ⁇ m ⁇ 1 . 5 ⁇ m in a copper base by performing plastic working on the alloy containing the precipitate.
  • precipitation-promoting metal including any one of titanium (Ti) and vanadium (V) is added.
  • the solid solution creating step is a process of performing heating within a temperature range of above the lowermost temperature where a single phase is maintained in the state diagram and below the melting temperature ⁇ 7.5 ⁇ X (X is wt % of an added component other than copper base) of a copper base phase for two hours or more.
  • the precipitate forcible-creating step is performed at a temperature below 47 ⁇ X (X is wt % of an added component other than copper base)+melting temperature of a copper base phase ⁇ 0.4(K, absolute temperature).
  • the alloy is a copper alloy and (Ni+Si), which is X, is 4.8 to 7.5wt %.
  • the present invention relates to a metal composite with an oriented precipitate that can function as a reinforcing material of a composite by artificially orienting an artificially created precipitate through plastic working.
  • FIG. 1 is a picture of microstructures, obtained by an optical microscope, of a continuous precipitate and a discontinuous precipitate before plastic working in a metal composite with an oriented precipitate according to the present invention.
  • FIG. 2 is a picture of a microstructure obtained by a transmission electron microscope, enlarging the portion A of FIG. 1 .
  • FIG. 3 is a picture of a microstructure, obtained by a transmission electron microscope, of a metal composite with an oriented precipitate according to the present invention.
  • FIG. 4 is a diagram comparing changes in hardness and electric conductivity before/after aging in a metal composite with an oriented precipitate according to the present invention.
  • FIG. 5 is a flowchart illustrating a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 6 is a schematic diagram illustrating a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 7 is a Cu—Ni 2 Si two-phase diagram for examining temperatures to be applied in a step of creating a solid solution and a step of forcibly creating a precipitate in a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 8 is a picture of a microstructure in a comparative example aged without a step of creating a solid solution in a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 9 is a picture of a microstructure after a step of creating a solid solution and a step of forcibly creating a precipitate in a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 10 is a picture of a microstructure in plastic working on a comparative example where slow cooling has been applied in a step of creating a solid solution in a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 11 is a picture of a microstructure in plastic working on an embodiment where rapid cooling has been applied in a step of creating a solid solution in a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 12 is a picture of a microstructure in a comparative example without a step of creating a solid solution in a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 13 is a picture of a microstructure in an embodiment with a step of creating a solid solution in a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 14 is a picture of a microstructure in a comparative example where slow cooling has been performed without precipitation-promoting metal in a step of creating a solid solution in a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 15 is a picture of a microstructure in an embodiment where rapid cooling has been performed with precipitation-promoting metal in a step of forcibly creating a precipitate in a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 16 is a picture of a microstructure in heat treatment at 500° C. after hot rolling on the comparative example of FIG. 14 .
  • FIG. 17 is a picture showing a change in the microstructure according to heat treatment temperature and time change in the embodiment of FIG. 15 .
  • FIGS. 18 and 19 are graphs showing changes in area ratios of discontinuous precipitation after a step of forcibly creating a precipitate in a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 20 is a picture of a microstructure, obtained by an electron microscope, in a preferred embodiment that has undergone a step of forcibly creating a precipitate in a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 21 is a picture of a microstructure when a step of forcibly creating a precipitate (up) and a step of orienting a precipitate (down) in a comparative example without a step of creating a solid solution.
  • FIG. 22 is a picture comparing microstructure before/after a step of orienting precipitate in a method of manufacturing a metal composite with an oriented precipitate according to the present invention.
  • FIG. 23 is a graph comparing mechanical properties before/after a step of orienting precipitates employing a drawing process in a comparative example and a preferred embodiment.
  • FIG. 24 is a graph comparing mechanical properties before/after a step of orienting precipitates employing a rolling process in a comparative example and a preferred embodiment.
  • FIG. 25 is a graph comparing the test results of FIG. 23 step by step.
  • a metal composite 20 with a discontinuous cellular precipitate or a lamellar precipitate according to the present invention is described hereafter with reference to FIGS. 1 to 3 .
  • FIGS. 1 and 2 are pictures of microstructures, obtained by an optical microscope, of a continuous precipitate and a discontinuous precipitate before plastic working, with FIG. 2 being the enlarged picture of portion A in FIG. 1 , in a metal composite with an oriented precipitate according to the present invention and FIG. 3 is a picture of a microstructure, obtained by a transmission electron microscope, of a metal composite 20 with an oriented precipitate according to the present invention.
  • the present invention provides a metal composite 20 that has improved strength and electric conductivity by providing a composite type strengthening effect by creating and artificially orienting a precipitate of a cellular or lamellar structure that reduces mechanical strength in metal.
  • the metal composite 20 of the present invention was achieved by artificially creating a precipitate in an alloy 10 , as in FIGS. 1 and 2 , and artificially orienting the precipitate, as in FIG. 3 .
  • the precipitate may be a discontinuous cellular precipitate or a continuous lamellar precipitate and, for the plastic working, various processes such as drawing, rolling, and extruding may be selected.
  • FIG. 4 is a chart comparing changes in hardness and electric conductivity before/after aging in the metal composite 20 with an oriented precipitate according to the present invention.
  • precipitation-promoting metal 10 for increasing the amount of a precipitation may be added to the alloy in the process of manufacturing the metal composite 20 .
  • the precipitation-promoting metal is titanium (Ti) or vanadium (V) and a copper alloy was selected in a preferred embodiment of the present invention.
  • the length to diameter aspect ratio of a precipitate, artificially created by aging for more than three hours before plastic working, is 100 or more and a discontinuous precipitate area of 40% or more of the entire area of the alloy 10 is formed, so as to improve strength and electric conductivity.
  • the present invention it is possible to forcibly create a discontinuous cellular precipitate or lamellar precipitate of 40% or more per unit area of 500 ⁇ m ⁇ 500 ⁇ m through aging after creating a solid solution by performing solution treatment or homogenization on the alloy 10 and it is also possible to create a discontinuous cellular precipitate or a continuous lamellar precipitate of 40% or more per unit area of 630 ⁇ m ⁇ 480 ⁇ m.
  • the forcibly created precipitate it is possible to orient the forcibly created precipitate to have a length of 2.0 ⁇ m or more per unit area of 3.5 ⁇ m ⁇ 1.5 ⁇ m in a copper base through plastic working.
  • a method of manufacturing the metal composite 20 is described hereafter with reference to FIG. 5 .
  • FIG. 5 is a flowchart illustrating a method of manufacturing the metal composite 20 with an oriented precipitate according to the present invention.
  • the method of manufacturing the metal composite 20 of the present invention includes a material preparing step (S 100 ) of preparing a molded alloy 10 , a solid solution creating step (S 200 ) of creating a solid solution by thermally treating the alloy 10 in a one phase area, a precipitate forcible-creating step (S 300 ) of creating a cellular precipitate or a lamellar precipitate by aging the alloy 10 containing the solid solution, and a precipitate orienting step (S 400 ) of orienting the precipitate by performing plastic working on the alloy 10 containing the precipitate.
  • the material preparing step (S 100 ) is a process of preparing an alloy (see FIGS. 5 and 6 ), in which the precipitation-promoting metal described above may be selectively prepared.
  • the alloy 10 which is a copper alloy containing Ni—Si in an embodiment of the present invention, is a mold formed by any one of rolling, drawing, and extruding and contains a residual precipitate.
  • the precipitation-promoting metal includes any one of titanium (Ti) and vanadium (V).
  • the weight percent (wt %) of (Ni+Si), which is the sum of nickel (Ni) and silicon (Si), is limited to 81% or more of the highest solid solubility to the entire weight of the alloy 10 , that is, 4.8 to 7.5wt % and the balance is copper (Cu) and other unavoidable impurities.
  • the precipitation-promoting metal is selectively included, and titanium (Ti) of 0.025 to 0.24wt % or vanadium (V) of 0.028 to 0.086wt % may be included.
  • the solid solution creating step (S 200 ) is a process for removing a residual precipitation, and when precipitation-promoting metal is included in the material preparing step (S 100 ), the solution solubility may be low.
  • the solid solution creating step (S 200 ) is a process of heating the alloy 10 and the precipitation-promoting metal at a predetermined temperature or more and the preferred temperature in the solid solution creating step (S 200 ) is preferably 950° C. or more for the copper-based alloy and under 1084 (melting point of pure copper) ⁇ 7.5 ⁇ X.
  • X is the weight percent (wt %) of (Ni+Si) described above, 1084 ⁇ 7.5 ⁇ X where a liquid state is not produced and 950° C. or more that is the highest solid solution limit temperature where a solid solution can be produced are preferable for the Cu—Ni—Si, Cu—Ni—Si—Ti, Cu—Ni—Si—V alloy 10 that is an embodiment of the present invention.
  • the discontinuous precipitate forcible-creating step (S 300 ) is performed.
  • the precipitate forcible-creating step (S 300 ) is a process of creating a discontinuous cellular precipitate or a discontinuous lamellar precipitate in the alloy 10 , and in an embodiment of the present invention, when water quenching or air cooling is performed and precipitation-promoting metal was added after the solid solution creating step (S 200 ), aging was performed for two or more hours, and when precipitation-promoting metal was not added, aging was performed for five or more hours, thereby forcibly creating a discontinuous precipitate.
  • FIGS. 8 and 9 are pictures of microstructures in a comparative example and an embodiment employing different ways of cooling in the solid solution creating step (S 200 ). It was slowly cooled in a furnace in the comparative example, whereas it was rapidly cooled in the embodiment.
  • FIG. 10 is a picture of a microstructure in plastic working on a comparative example in which slow cooling was performed in the solid solution creating step (S 200 ) in the method of manufacturing the metal composite with an oriented precipitate according to the present invention
  • FIG. 11 is a picture of a microstructure in plastic working on an embodiment in which rapid cooling was performed in the solid solution creating step (S 200 ) in the method of manufacturing the metal composite with an oriented precipitate according to the present invention.
  • the precipitate forcible-creating step (S 300 ) is a step for increasing the amount of a precipitate formed in the alloy 10 in the solid solution creating step (S 200 ), and aging was performed in an embodiment of the present invention.
  • Microstructures before/after the precipitate forcible-creating step (S 300 ) are comparatively described with reference to FIGS. 12 to 19 .
  • FIG. 14 is a picture of a microstructure in a comparative example in which precipitation-promoting metal was not added and slow cooling was performed in the solid solution creating step (S 200 ) in the method of manufacturing a metal composite 20 with an oriented precipitate according to the present invention and FIG.
  • FIG. 15 is a picture of a microstructure in an embodiment in which precipitation-promoting metal was added and rapid cooling was performed in the solid solution creating step (S 200 ) in the method of manufacturing a metal composite 20 with an oriented precipitate according to the present invention, in which microstructures after the solid solution creating step (S 200 ) and the precipitate forcible-creating step (S 300 ) was finished, when vanadium (V) was added in the material preparing step (S 100 ) are shown, and it could be seen that formation of a discontinuous precipitate was promoted in the same way as titanium (Ti).
  • FIG. 16 is a picture of a microstructure in a heat treatment of 500° C. after hot rolling in the comparative example of FIG. 14
  • FIG. 17 is a picture showing changes in a microstructure according to changes in heat treatment temperature and length of time in the embodiment of FIG. 15 .
  • the microstructure did not show a large change in the comparative example before the precipitate forcible-creating step (S 300 ), as in FIGS. 14 and 16 , but in the embodiment, it could be seen that the discontinuous precipitate increased with the lapse of time, as in FIGS. 15 and 17 .
  • FIGS. 18 and 19 are graphs showing changes in area ratios in discontinuous precipitation after the precipitate forcible-creating step (S 300 ) in the method of manufacturing a metal composite 20 with an oriented precipitate according to the present invention.
  • X which is the weight percent (wt %) of (Ni+Si), is in the range of 4.8 to 7.5wt % in the state diagram shown in FIG. 7 . Furthermore, it is possible to estimate from the state diagram that all of precipitated alloys show the same phenomenon, so the same phenomenon occurs in an alloy containing 81% of the highest solution solubility.
  • the temperature (° C.) for the discontinuous forcible creating step (S 300 ) is 47 ⁇ X+260° C(533K) or less and has this relationship.
  • the temperature (° C.) for the solid solution creating step (S 200 ) is 1084 ⁇ 7.5 ⁇ X and 950° C. or more, which is the highest soluble limit where a solid solution can be created and has this relationship.
  • the discontinuous precipitate is created from 0.4 ⁇ the melting point (K, absolute temperature) of copper-based metal or more where dispersion starts, so a discontinuous precipitate is forcibly created in the area in the state diagram shown in FIG. 7 from the relationship with additional components other than the base metal proposed in the present invention.
  • the precipitate orienting step (S 400 ) is performed after the discontinuous precipitate forcible-creating step (S 300 ).
  • the precipitate orienting step (S 400 ) is a process for artificially orienting a discontinuous precipitate or a discontinuous lamellar precipitate formed inside in accordance with the embodiment described above.
  • FIG. 11 is a picture of a microstructure of the metal composite 20 manufactured by rolling (upper) and drawing (lower) in FIG. 11 , and it can be seen that discontinuous precipitates are arranged in parallel in the metal composite 20 manufactured in accordance with a preferred embodiment of the present invention.
  • Microstructures of a comparative example and an embodiment are compared hereafter with reference to FIGS. 21 and 22 .
  • FIG. 21 is a picture of a microstructure when a precipitate orienting step was performed in a comparative example without the solid solution creating step (S 200 ) and FIG. 22 is a picture comparing microstructures before/after the precipitate orienting step (S 400 ) in the method of manufacturing the metal composite 20 with an oriented precipitate according to the present invention.
  • the precipitate orienting step (S 400 ) was performed on an alloy where a precipitate was not created in the precipitate forcible-creating step (S 300 ) since the solid solution creating step (S 200 ) was not performed.
  • the orientation of the microstructure is very different from the embodiment (the lower picture in FIG. 22 ) where the precipitate orienting step (S 400 ) was performed after a solid solution was created (the upper picture in FIG. 22 ).
  • FIG. 23 is a graph comparing mechanical properties before/after the precipitate orienting step (S 400 ) where drawing was employed in a comparative example and a preferred embodiment
  • FIG. 24 is a graph comparing mechanical properties before/after the precipitate orienting step (S 400 ) where rolling was employed in a comparative example and a preferred embodiment.
  • the strength was 600 MPa before drawing, but it slightly increased to 800 MPa after drawing in the comparative example, but in the embodiment, the strength was about 500 MPa before drawing, but it increased close to 1100 MPa after drawing. Accordingly, it can be seen that the strength of the alloy 10 is higher in the embodiment than the comparative example after the precipitate orienting step (S 400 ).
  • a precipitate can function as a reinforcing material by forcibly creating a precipitate through the precipitate forcible-creating step (S 300 ) and then forcibly orienting the precipitate.
  • FIG. 24 shows an example when rolling was used in the precipitate forcible-creating step (S 400 ), in which the strength was 600 MPa before rolling in the comparative example, which is higher than 550 MPa, which is the strength in the embodiment, but after the precipitate forcible-creating step (S 400 ) was performed, the strength was less than 800 MPa in the comparative example, but the strength in the preferred embodiment of the present invention was 900 MPa, so an effect of increasing strength according to orientation of a precipitate could be seen.
  • FIG. 25 is a graph comparing the test result of FIG. 23 in each stage, in which effects of increasing strength in each process are shown sequentially in the upward direction starting from the bottom.
  • the comparative example and the embodiment show the same strength of 200 MPa in the state of the alloy 10 , but the strength of the comparative example increased to 430 MPa, which is higher than the strength of the embodiment, after the solid solution creating step (S 200 ) and the precipitate forcible-creating step (S 300 ).
  • the strength in the embodiment increased by 480 MPa, which shows an effect of increasing strength of 290 MPa in comparison to the comparative example.
  • titanium was used as precipitation-promoting metal in an embodiment of the present invention, but vanadium may also be used.
  • the present invention relates to a metal composite with an oriented precipitate functioning as a reinforcing material for a composite by artificially orienting a precipitate, which is artificially created, through plastic working, and a method of manufacturing the metal composite, so electric conductivity and strength are improved. Furthermore, if necessary, it is possible to artificially adjust the amount of precipitate by selectively adding precipitation-promoting metal, so it can be used in various fields by adjusting electrical and mechanical properties.

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KR101708285B1 (ko) * 2015-07-29 2017-02-20 창원대학교 산학협력단 배향형 석출물을 포함하는 금속복합재료 및 이의 제조 방법
KR101760076B1 (ko) * 2016-06-09 2017-07-24 한국기계연구원 석출물을 포함하는 강도와 연신율이 향상된 알루미늄-아연 합금 및 이의 제조방법
KR102012952B1 (ko) 2019-01-15 2019-08-21 (주)일광주공 알루미늄 합금 및 그 제조방법

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