WO2014115920A1 - 배향된 석출물을 가지는 금속복합재료 및 이의 제조방법 - Google Patents

배향된 석출물을 가지는 금속복합재료 및 이의 제조방법 Download PDF

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WO2014115920A1
WO2014115920A1 PCT/KR2013/001163 KR2013001163W WO2014115920A1 WO 2014115920 A1 WO2014115920 A1 WO 2014115920A1 KR 2013001163 W KR2013001163 W KR 2013001163W WO 2014115920 A1 WO2014115920 A1 WO 2014115920A1
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precipitate
alloy
solid solution
precipitates
metal composite
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PCT/KR2013/001163
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English (en)
French (fr)
Korean (ko)
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한승전
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한국기계연구원
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Priority to US14/762,772 priority Critical patent/US20150354048A1/en
Priority to JP2015555085A priority patent/JP6209621B2/ja
Publication of WO2014115920A1 publication Critical patent/WO2014115920A1/ko

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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 material having an oriented precipitate and a method for manufacturing the same, and more particularly, to the addition of a precipitate promoting metal to an alloy, and to a solution treatment or homogenization treatment to produce a solid solution, and then to an aging treatment.
  • the present invention relates to a metal composite material having an oriented precipitate forcibly generating precipitates through which the forcibly produced precipitates are oriented through plastic working and thereby improving strength and electrical conductivity.
  • Copper is widely applied to electrical / electronic circuits because of its high electrical conductivity. However, copper is exposed to high currents and voltages when applied to electrical / electronic circuits due to high integration and light weight of telecommunication components.
  • copper alloys are widely used as connectors for connecting connectors, accumulators, or controllers to various electrical components, actuators, sensors, and the like in automobiles equipped with more electric devices, and miniaturization of such connectors is urgently required.
  • the connector installed close to the engine is exposed to the engine's heat and vibration environment, and when a large amount of current is sent to the connector, the connector generates heat and rises to a high temperature. Therefore, such a connector is required to have high reliability under the above-mentioned environment.
  • Cu-Fe-P alloy (Korean Patent No. 10-0997560) or Cu-Mg-P alloy (Korean Patent No. 10-0417756) is known as a material of a copper alloy connector for a conventional automobile or the like.
  • the former alloy is an alloy whose strength is improved by precipitation of Fe-P compounds based on the simultaneous addition of Fe and P.
  • alloys having improved mobility resistance by addition of Zn Japanese Patent Laid-Open No. 168830
  • alloys having improved stress relaxation resistance by addition of Mg Japanese Patent Laid-Open No. 358033
  • the latter alloy is an alloy that improves tensile strength, electrical conductivity and stress relaxation resistance by adding Mg and P to improve strength and thermal creeping characteristics.
  • the copper alloy can improve electrical conductivity, thermal stability, strength, and the like by adding various elements.
  • An object of the present invention is to solve the problems of the prior art as described above, more specifically, by selectively adding a precipitation promoting metal to the alloy and performing a solution treatment or homogenization treatment to produce a solid solution through the aging treatment
  • the present invention provides a metal composite material having a oriented precipitate forcibly generating precipitates and having the strength and electrical conductivity improved by aligning the forcibly produced precipitates through plastic working.
  • the alloy according to the present invention is subjected to a solution treatment or homogenization treatment to produce a solid solution, and then aged and treated to discontinuous cell precipitates or lamellar precipitates of 40% or more per 500 ⁇ m ⁇ 500 ⁇ m. It is forcibly produced, characterized in that the forcibly produced precipitates are oriented through plastic working.
  • the alloy is subjected to solution treatment or homogenization to produce a solid solution, and then aged and treated at 40% or more discontinuous cellular precipitates or lamellar precipitates per unit area of 630 ⁇ m ⁇ 480 ⁇ m.
  • Forcibly produced characterized in that the forcibly produced precipitates are oriented through plastic working.
  • the metal composite material having the oriented precipitates according to the present invention is produced by dissolving or homogenizing the alloy to form a solid solution, and then forcibly producing discontinuous cellular precipitates or lamellar precipitates through aging treatment.
  • the precipitate is characterized in that the substrate is oriented to have a length of 2.0 ⁇ m or more per unit area of 3.5 ⁇ m ⁇ 1.5 ⁇ m through plastic working.
  • the oriented precipitates are characterized by having an aspect ratio of 100 or greater in length and diameter.
  • the alloy in which the solid solution is produced is characterized in that it is quenched or air cooled by a water quenching method.
  • the aging treatment is characterized in that it is carried out for more than 3 hours.
  • the precipitation promoting metal is added during the solution treatment or homogenization treatment.
  • the precipitation promoting metal is characterized in that it comprises any one of titanium (Ti), vanadium (V).
  • the method for producing a metal composite material having an oriented precipitate according to the present invention includes a material preparation step of preparing a cast alloy, a solid solution generation step of generating a solid solution by heat-treating the alloy in a single phase region, and an alloy in which a solid solution is produced. Aging treatment to form a precipitate forcing to form more than 40% of the cell precipitate or lamellar precipitate per 500 ⁇ m ⁇ 500 ⁇ m unit area, and the precipitate orientation step of orienting the precipitate by plastic processing the alloy containing the precipitate; do.
  • the method for producing a metal composite material having an oriented precipitate according to the present invention includes a material preparation step of preparing a cast alloy, a solid solution generation step of generating a solid solution by heat-treating the alloy in a single phase region, and an alloy in which a solid solution is produced. Aging treatment to form a precipitate forcing to form a cell precipitate or lamellar precipitate of at least 40% per unit area of 630 ⁇ m ⁇ 480 ⁇ m, and a precipitate orientation step of orienting the precipitate by plastic processing the alloy containing the precipitate; do.
  • the method for producing a metal composite material having an oriented precipitate according to the present invention includes a material preparation step of preparing a cast alloy, a solid solution generation step of generating a solid solution by heat-treating the alloy in a single phase region, and an alloy in which a solid solution is produced.
  • the precipitation promoting metal containing any one of titanium (Ti), vanadium (V) is included.
  • the solid solution generation step is a process of heating for 2 hours or more in a temperature range of at least the minimum temperature for maintaining a single phase in the state diagram, the melting temperature of the known phase-7.5 ⁇ X (X is wt% of the composition added to the matrix). It is done.
  • the precipitate forcing production step is characterized in that it is carried out at a temperature of 47 ⁇ X (X is the wt% of the composition added outside the matrix) + the melting temperature of the matrix phase ⁇ 0.4 (K) or less.
  • the alloy is a copper alloy, X (Ni + Si) is characterized in that it contains 4.8 to 7.5% by weight.
  • the present invention relates to a metal composite material having an oriented precipitate that can artificially orient the artificially generated precipitate through plastic working to serve as a reinforcing material of the composite material.
  • the amount of precipitates can be adjusted by selectively adding the precipitation promoting metal.
  • 1 is an optical microscope microstructure photograph of continuous and discontinuous precipitates before plastic processing in a metal composite material having an oriented precipitate according to the present invention.
  • Figure 2 is a transmission electron microscope microstructure photograph of the enlarged portion A of FIG.
  • FIG. 3 is a transmission electron microscope microstructure photograph of a metal composite material having an oriented precipitate according to the present invention.
  • Figure 4 is a figure comparing the hardness and electrical conductivity change before and after aging treatment in a metal composite material having an oriented precipitate according to the present invention.
  • FIG. 5 is a process flow chart showing a method for producing a metal composite material having an oriented precipitate according to the present invention.
  • FIG. 6 is a schematic view showing a method for producing a metal composite material having an oriented precipitate according to the present invention.
  • FIG. 8 is a microstructure photograph of a comparative example subjected to aging without performing a solid solution generation step in the method for producing a metal composite material having an oriented precipitate according to the present invention.
  • FIG. 9 is a microstructure photograph after performing a solid solution generation step and precipitate forcing step in the method for producing a metal composite material having an oriented precipitate according to the present invention.
  • Figure 11 is a microstructure photograph during plastic working for the embodiment subjected to quenching in the solid solution generation step in the method for producing a metal composite material having an oriented precipitate according to the present invention.
  • FIG. 12 is a microstructure photograph of a comparative example without performing a solid solution generation step in the method for producing a metal composite material having an oriented precipitate according to the present invention.
  • Figure 13 is a microstructure photograph of the embodiment subjected to the solid solution generation step in the method for producing a metal composite material having an oriented precipitate according to the present invention.
  • FIG. 14 is a microstructure photograph of a comparative example in which a slow cooling is performed during the solid solution generation step in the method for producing a metal composite material having an oriented precipitate according to the present invention and no precipitation promoting metal is added.
  • 15 is a microstructure photograph of an embodiment in which a quenching is performed in a solid solution generation step and a precipitation promoting metal is added in the method of manufacturing a metal composite material having an oriented precipitate according to the present invention.
  • FIG. 16 is a microstructure photograph of 500 ° C. heat treatment after hot rolling for the comparative example of FIG. 14.
  • FIG. 17 is a photograph showing microstructure changes according to changes in heat treatment temperature and run time for the example of FIG. 15.
  • 21 is a microstructure photograph when the precipitate compulsory generation step (top) and the precipitate orientation step (bottom) for the comparative example was not performed solid solution generation step.
  • Figure 22 is a photograph comparing the microstructure before and after the precipitate alignment step in the method for producing a metal composite material having an oriented precipitate according to the present invention.
  • FIG. 25 is a graph comparing the experimental results of FIG. 23 step by step; FIG.
  • FIG. 1 and 2 are optical microscopic microstructure photographs of continuous and discontinuous precipitates before firing in the metal composite material having the oriented precipitates according to the present invention, and the enlarged portion A of FIG. 1, and FIG. A transmission electron microscope microstructure photograph of a metal composite material 20 having an oriented precipitate.
  • the present invention is a metal composite material (20) to improve the strength and electrical conductivity by producing a cellular or lamellar precipitate of the mechanical strength in the metal and then artificially oriented to have a composite type strengthening effect.
  • the precipitates are artificially generated inside the alloy 10, and then the precipitates are artificially oriented as shown in Fig. 3 to complete the metal composite material 20 of the present invention.
  • the precipitate may include a discontinuous cellular precipitate or a continuous lamellar precipitate, and the plastic working may be selected from various processes such as drawing, rolling, and extrusion.
  • the precipitation promoting metal for increasing the amount of precipitate may be included in the alloy 10.
  • titanium (Ti) or vanadium (V) is applied, and a preferred embodiment of the present invention employs a copper alloy.
  • the precipitates artificially generated by aging for 3 hours or more before the plastic working process have an aspect ratio of 100 or more in length and diameter, and a discrete precipitate region is formed in an area of 40% or more with respect to the total area of the alloy 10. By doing so, strength and electrical conductivity can be improved.
  • the present invention may be subjected to the solution treatment or homogenization treatment to the alloy 10 to produce a solid solution, and through the aging treatment can be forcibly produced more than 40% discontinuous cellular precipitate or lamellar precipitate per 500 ⁇ m ⁇ 500 ⁇ m unit area More than 40% of discontinuous cellular precipitates or continuous lamellar precipitates per unit area of 630 ⁇ m ⁇ 480 ⁇ m.
  • the precipitates forcibly produced can be oriented so as to have a length of 2.0 ⁇ m or more per unit area of 3.5 ⁇ m ⁇ 1.5 ⁇ m in the substrate through plastic working.
  • FIG. 5 is a process flow chart showing a method for producing a metal composite material 20 having oriented precipitates according to the present invention.
  • the method of manufacturing the metal composite material 20 of the present invention as shown in the drawing the material preparation step (S100) for preparing the cast alloy 10, and the solid solution to generate a solid solution by heat-treating the alloy 10 in a single phase region Producing step (S200), precipitates for forming a cellular precipitate or lamellar precipitates by aging the alloy (10) in which the solid solution is produced, and forging the precipitate (S300), and the alloy (10) containing the precipitates by plastic processing It consists of a precipitate alignment step (S400) to orientate.
  • the material preparation step (S100) is a process of preparing an alloy (see FIGS. 5 and 6), and the aforementioned precipitation promoting metal may be selectively prepared.
  • the alloy 10 is a copper alloy containing nickel (Ni) -silicon (Si) in an embodiment of the present invention, and a cast formed by any one of rolling, drawing, and extruding is adopted to have residual precipitates. Done.
  • the precipitation promoting metal is composed of any one of titanium (Ti), vanadium (V).
  • the sum of the weights of nickel (Ni) and silicon (Si) ((Ni + Si) wt% is limited to include 81% or more of the highest solid solubility, that is, 4.8 to 7.5 wt% based on the total weight of the alloy (10).
  • the balance is copper (Cu) and other unavoidable impurities.
  • the precipitation promoting metal may be optionally included, 0.025 to 0.24% by weight of titanium (Ti), or 0.028 to 0.086% by weight of vanadium (V) may be included.
  • the solid solution generation step (S200) is a process for removing residual precipitates, when the precipitation-promoting metal is included in the material preparation step (S100) may have a low solubility.
  • the solid solution generation step (S200) is a process of heating the alloy 10 and the precipitation promoting metal at a temperature higher than a predetermined temperature, the preferred temperature of the solid solution generation step (S200) is 950 °C or more in the case of the copper base alloy (10), The temperature of 1084 (pure copper melting point)-7.5xX or less is preferable.
  • X is the above-described weight% value of (Ni + Si) is applied, Cu-Ni-Si, Cu-Ni-Si-Ti or Cu-Ni-Si-V alloy (10) which is an embodiment of the present invention
  • the silver liquid is preferably 1084-7.5 ⁇ X in which no liquid phase is formed, and 950 ° C. or more, which is the maximum employment limit temperature at which a solid solution can be formed.
  • the discontinuous precipitate forced generation step (S300) is carried out.
  • the precipitate forcing generation step (S300) is a process of generating a discontinuous cellular precipitate or discontinuous lamellar precipitate inside the alloy 10, in the embodiment of the present invention after the solid solution generation step (S200) to perform water quenching or air cooling and precipitation Discontinuous precipitates were forcibly produced by aging for 2 hours or more when the promoting metal was added and by aging for 5 hours or more when the precipitation promoting metal was not added.
  • FIG. 10 is a microstructure photograph during plastic working of the comparative example subjected to the slow cooling in the solid solution generation step (S200) in the manufacturing method of the metal composite material 20 having the oriented precipitates according to the present invention
  • FIG. 10 In the manufacturing method of the metal composite material 20 having the oriented precipitates by the quenching in the solid solution generation step (S200) of the embodiment is a microstructure photograph during plastic working.
  • the precipitates were not oriented, but in the case of the quenched embodiment in the solid solution generation step (S200), the precipitates were subjected to the processing direction and the processing direction. It can be seen that they are oriented side by side.
  • the solid solution generation step (S200) it is preferable to quench using water quenching or air cooling.
  • the precipitate forcing generation step (S300) is a step for increasing the amount of precipitate formed in the alloy 10 in the solid solution generation step (S200), in the embodiment of the present invention was applied to the aging treatment (aging).
  • FIG. 14 is a microstructure photograph of a comparative example in which a slow cooling process is performed during the solid solution generation step (S200) and no precipitation promoting metal is added in the method of manufacturing a metal composite material 20 having an oriented precipitate according to the present invention
  • FIG. 14 is a microstructure photograph of a comparative example in which a slow cooling process is performed during the solid solution generation step (S200) and no precipitation promoting metal is added in the method of manufacturing a metal composite material 20 having an oriented precipitate according to the present invention
  • FIG. 16 is a microstructure photograph of a heat treatment at 500 ° C. after hot rolling with respect to the comparative example of FIG. 14, and
  • FIG. 17 is a photograph showing a change in microstructure according to temperature and execution time during heat treatment with respect to the embodiment of FIG. 15.
  • the precipitate forcing generation step (S300) was performed and a small amount of discontinuous precipitate was formed even though it was continued for a long time, and thus showed a result contrary to the preferred embodiment.
  • the weight% X of (Ni + Si) on the state diagram shown in Figure 7 is preferably carried out in the range of 4.8 to 7.5% by weight. And since the state diagram realizes the same phenomenon in all precipitated alloys, it can be predicted that the same phenomenon occurs in the alloy added with 81% of the highest solid solution.
  • the implementation temperature (° C.) of the discontinuous precipitate forcing generation step (S300) a temperature of 47 ⁇ X + 260 ° C. (533K) or less is adopted and has such a relationship.
  • the implementation temperature (° C.) of the solid solution generation step (S200), 1084-7.5 ⁇ X and the maximum employment limit that can form a solid solution of 950 °C or more is adopted and has such a relationship.
  • discontinuous precipitate is forced in the region shown in the state diagram shown in FIG. 7 from the relationship with the addition composition other than the base metal found in the present invention. Is formed.
  • the precipitate alignment step (S400) is a process for artificially aligning the discrete precipitates or discrete lamellae precipitates formed therein according to the embodiment as described above.
  • Figure 11 is a fine of the metal composite material 20 produced by adopting the rolling (upper) and drawing (lower) As a structure photograph, it can be seen that the metal composite material 20 prepared according to the preferred embodiment of the present invention has discontinuous precipitates arranged in parallel with each other.
  • FIG. 21 is a microstructure photograph when the precipitate alignment step is performed for the comparative example in which the solid solution generation step (S200) is not performed
  • FIG. 22 is a precipitate in the manufacturing method of the metal composite material 20 having the precipitates oriented according to the present invention. It is a photograph comparing the microstructure before / after the alignment step (S400).
  • the comparative example was performed by performing a precipitate alignment step (S400) on an alloy in which precipitates were not produced in the precipitate forcing generation step (S300) because the solid solution generation step (S200) was not performed (FIG. 22).
  • a precipitate alignment step (S400) on an alloy in which precipitates were not produced in the precipitate forcing generation step (S300) because the solid solution generation step (S200) was not performed (FIG. 22).
  • S400 precipitate alignment step
  • the difference in the orientation of the microstructure shows a large difference in mechanical properties as shown in FIGS. 23 and 24.
  • Figure 23 is a graph comparing the mechanical properties before and after the implementation of the precipitate alignment step (S400) is adopted with respect to the comparative example and the preferred embodiment
  • Figure 24 is a rolling process is adopted for the comparative example and the preferred embodiment
  • This is a graph comparing the mechanical properties before / after the precipitate alignment step (S400).
  • an example of completing the aging treatment showed a strength of 500 MPa or less, which was lower than 600 MPa, which is the strength of the comparative example.
  • the strength of 600 MPa before the drawing process was increased to 800 MPa after the drawing process, but in the case of the example, the strength was about 500 MPa before the drawing process, and the strength was close to 1100 MPa after the drawing process. Rather, after the precipitate orientation step (S400) it can be seen that the strength of the alloy 10 of the embodiment is superior to the comparative example.
  • the rolling process was adopted in the precipitation forcing production step (S400).
  • the strength was higher than 550 MPa, which is 600 MPa before the rolling process.
  • the comparative example showed a strength of less than 800 MPa, while the preferred embodiment of the present invention exhibited a strength of 900 MPa to confirm the effect of increasing the strength according to the orientation of the precipitate.
  • FIG. 25 is a graph comparing the experimental results of FIG. 23 step by step, in which the strength increase effect for each process is sequentially stacked from the bottom to the top.
  • Comparative Example and Example showed the same strength of 200 MPa in the alloy 10 state, and after the solid solution generation step (S200) and the precipitate forcing generation step (S300), rather, the strength of the comparative example was increased by 430 MPa. Higher than the intensity of the example.
  • the comparative example after the precipitate alignment step (S400) was increased by 190 MPa while the example was confirmed that the strength improvement effect of 290 MPa compared to the comparative example was increased by 480 MPa.
  • the metal composite material 20 manufactured according to the preferred embodiment of the present invention has superior mechanical properties compared to the metal composite material 20 produced by the manufacturing method in which discontinuous precipitates are arranged in parallel to each other and the mechanical properties are overnight. It was confirmed that the increase.
  • titanium is used as the precipitation promoting metal
  • vanadium may also be applied.
  • the present invention relates to a metal composite material having an oriented precipitate so that the artificially generated precipitates can be artificially oriented through plastic working to serve as a reinforcing material of the composite material, and the electrical conductivity and strength thereof are improved. If necessary, it is possible to artificially adjust the amount of precipitates by selectively adding the precipitation promoting metal, so that it is applicable to various fields by controlling the electrical and mechanical properties.

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PCT/KR2013/001163 2013-01-22 2013-02-14 배향된 석출물을 가지는 금속복합재료 및 이의 제조방법 WO2014115920A1 (ko)

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US14/762,772 US20150354048A1 (en) 2013-01-22 2013-02-14 Metal composite comprising aligned precipitate and preparation method therefor
JP2015555085A JP6209621B2 (ja) 2013-01-22 2013-02-14 配向された析出物を有する金属複合材料及びその製造方法

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KR101708285B1 (ko) * 2015-07-29 2017-02-20 창원대학교 산학협력단 배향형 석출물을 포함하는 금속복합재료 및 이의 제조 방법
JP6695570B2 (ja) * 2015-10-02 2020-05-20 大同特殊鋼株式会社 時効硬化型ベイナイト非調質鋼を用いた部品の製造方法
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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