CN111850696A - Copper-aluminum-nickel-based single crystal alloy and preparation method thereof - Google Patents
Copper-aluminum-nickel-based single crystal alloy and preparation method thereof Download PDFInfo
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- CN111850696A CN111850696A CN202010771220.XA CN202010771220A CN111850696A CN 111850696 A CN111850696 A CN 111850696A CN 202010771220 A CN202010771220 A CN 202010771220A CN 111850696 A CN111850696 A CN 111850696A
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/01—Alloys based on copper with aluminium as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
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Abstract
The invention relates to the technical field of single crystal alloys, in particular to a copper-aluminum-nickel-based single crystal alloy and a preparation method thereof. The as-cast alloy of the intermediate product of the copper-aluminum-nickel-iron single crystal alloy contains a large amount of nano-phases, and the size of the nano-phases is between tens of nanometers and hundreds of nanometers. When the as-cast alloy is directly subjected to heat treatment in a high-temperature single bcc phase region, the nano phases can be dissolved back into the bcc phase of the matrix in a solid solution manner, so that the abnormal growth of crystal grains of the alloy is promoted, and the copper-aluminum-nickel-iron single crystal can be directly prepared. The preparation method of the copper-aluminum-nickel-based single crystal alloy is simple and convenient, does not have a complex process, and saves cost and time.
Description
Technical Field
The invention relates to the technical field of single crystal alloys, in particular to a copper-aluminum-nickel-based single crystal alloy and a preparation method thereof.
Background
Generally, metal materials are often prepared by solution treatment and annealing, and after the treatment, the alloy will have a polycrystalline structure due to nucleation and growth of grains with different orientations. Polycrystalline materials tend to be brittle at break because of the high energy accumulated at the grain boundaries, and the materials are easily broken along the grain boundaries when stressed. Single crystal alloys generally have superior mechanical and functional properties to polycrystalline alloys, and methods for obtaining single crystals mainly include directional solidification or annealing or dynamic recrystallization after macroscopic deformation; however, directional solidification requires an extremely complex set of processes and equipment, which is time-consuming and expensive in the whole process of obtaining single crystals; the phenomenon of abnormal growth of crystal grains can be caused by the method of annealing or dynamic recrystallization after macroscopic deformation, most of single crystals obtained by the method are wire rods, the application of large devices cannot be met, the whole preparation process is complicated, the cost is high, and batch production cannot be realized.
In view of the above problems, Omori et al, 2013, found that an alloy with a composition of 71.6% copper, 17% aluminum and 11.4% manganese, after being subjected to 900 ℃ single-phase zone homogenization treatment, is cooled to 500 ℃ at a cooling rate of 3.3 ℃/min for 10 minutes, then is heated to 900 ℃ at a heating rate of 10 ℃/min for 600 minutes, and is quenched in water after 10 cycles of the above heat treatment, a single crystal exceeding the order of centimeters can be obtained (T.Omori, T.Kusama, S.Kawata, I.Ohnuma, Y.Sutou, Y.Araki, K.Ishida, R.Kinuma, Absomal grain growth induced by cycle heat attack, Science 341(2013) 1500-. Omori et Al further obtained single crystals in a FermaneAlNiNi quaternary alloy material by a cyclic heat treatment method in 2016 (T.Omori, H.Iwaizakoo, R.Kainuma, abnormal grain growth induced by cyclic heat treatment in Fe-Mn-Al-Ni subelastic alloy, mater.Des.101(2016) 263-269). The cyclic heat treatment process is time-consuming and extremely complex, and particularly has strict requirements on the temperature rise and reduction rate, so that the cyclic heat treatment process is not beneficial to practical production and application.
Therefore, the main reason that the single crystal material cannot be widely applied is that the preparation cost is high, and the single crystal prepared by the preparation method can be used only in some special fields, so that the application of the single crystal is limited. Therefore, the search for a simple and low-cost single crystal alloy is a problem to be solved.
Disclosure of Invention
The invention aims to provide a copper-aluminum-nickel-based single crystal alloy and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a copper-aluminum-nickel-based single crystal alloy which comprises the following alloy elements in percentage by mass: 69-81% of copper, 10-15% of aluminum, 4-8% of nickel and 5-8% of iron;
the preparation method of the copper-aluminum-nickel base single crystal alloy comprises the following steps:
according to the mass ratio, mixing copper, aluminum, nickel and iron, and then smelting to obtain an as-cast alloy;
annealing the as-cast alloy to obtain the copper-aluminum-nickel base single crystal alloy;
the temperature of the annealing treatment is 1000-1020 ℃, and the annealing time is not less than 24 hours.
Preferably, the following alloying elements are included: 71.5 to 77 percent of copper, 12.5 to 14.5 percent of aluminum, 4.5 to 7.5 percent of nickel and 5.5 to 7.5 percent of iron.
Preferably, the following alloying elements are included: 72 to 75 percent of copper, 13 to 14 percent of aluminum, 5 to 7 percent of nickel and 6 to 7 percent of iron.
The invention also provides a preparation method of the copper-aluminum-nickel-based single crystal alloy, which comprises the following steps:
according to the mass ratio, mixing copper, aluminum, nickel and iron, and then smelting to obtain an as-cast alloy;
annealing the as-cast alloy to obtain the copper-aluminum-nickel base single crystal alloy;
the temperature of the annealing treatment is 1000-1020 ℃, and the annealing time is not less than 24 hours.
The invention provides a copper-aluminum-nickel-based single crystal alloy which comprises the following alloy elements in percentage by mass: 69% -81% of copper, 10% -15% of aluminum, 4% -8% of nickel and 5% -8% of iron, and the preparation method of the copper-aluminum-nickel-based single crystal alloy comprises the following steps: according to the mass ratio, mixing copper, aluminum, nickel and iron, and then smelting to obtain an as-cast alloy; annealing the as-cast alloy to obtain the copper-aluminum-nickel base single crystal alloy; the temperature of the annealing treatment is 1000-1020 ℃, and the annealing time is not less than 24 hours. The as-cast alloy of the intermediate product of the copper-aluminum-nickel-iron single crystal alloy contains a large amount of nano-phases, and the size of the nano-phases is between tens of nanometers and hundreds of nanometers. When the as-cast alloy is directly subjected to heat treatment in a high-temperature single bcc phase region, the nano phases can be dissolved back into the bcc phase of the matrix in a solid solution manner, so that the abnormal growth of crystal grains of the alloy is promoted, and the copper-aluminum-nickel-iron single crystal can be directly prepared. The preparation method of the copper-aluminum-nickel-based single crystal alloy is simple and convenient, does not have a complex process, and saves cost and time.
Drawings
FIG. 1 is a microstructure view of an as-cast alloy and a copper-aluminum-nickel-based single crystal alloy prepared in example 1;
FIG. 2 is a photograph of the as-cast alloy and the copper aluminum nickel base single crystal alloy prepared in example 1;
FIG. 3 is a microstructure diagram of an as-cast alloy and a copper aluminum nickel base single crystal alloy prepared in example 2;
FIG. 4 is a photograph of the as-cast alloy and the copper aluminum nickel base single crystal alloy prepared in example 2;
FIG. 5 is a microstructure diagram of an as-cast alloy and a copper aluminum nickel base single crystal alloy prepared in example 3;
FIG. 6 is a photograph of the as-cast alloy and the copper aluminum nickel base single crystal alloy prepared in example 3;
FIG. 7 is a microstructure view of an as-cast alloy and a copper aluminum nickel base single crystal alloy prepared in example 4;
FIG. 8 is a photograph of the as-cast alloy and the copper aluminum nickel base single crystal alloy prepared in example 4.
Detailed Description
The invention provides a copper-aluminum-nickel-based single crystal alloy which comprises the following alloy elements in percentage by mass: 69-81% of copper, 10-15% of aluminum, 4-8% of nickel and 5-8% of iron;
the preparation method of the copper-aluminum-nickel base single crystal alloy comprises the following steps:
according to the mass ratio, mixing copper, aluminum, nickel and iron, and then smelting to obtain an as-cast alloy;
annealing the as-cast alloy to obtain the copper-aluminum-nickel base single crystal alloy;
the temperature of the annealing treatment is 1000-1020 ℃, and the annealing time is not less than 24 hours.
In the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
The copper-aluminum-nickel-based single crystal alloy comprises 69-81% of copper by mass, preferably 71.5-77% of copper by mass, and more preferably 72-75% of copper by mass. In the invention, the copper has the function of forming a body-centered cubic bcc matrix phase with aluminum and nickel, and the component alloy is a single bcc matrix phase in a heat treatment temperature range of 1000-1020 ℃.
The copper-aluminum-nickel-based single crystal alloy comprises 10-15% of aluminum, preferably 12.5-14.5%, and more preferably 13-14% by mass. In the invention, the aluminum and the copper nickel form a body-centered cubic bcc matrix phase, and the component alloy is a single bcc matrix phase in a heat treatment temperature range of 1000-1020 ℃.
The copper-aluminum-nickel-based single crystal alloy comprises 4-8% of nickel, preferably 4.5-7.5%, and more preferably 5-7% by mass. In the invention, the nickel and copper are used for forming a body-centered cubic bcc matrix phase, and the component alloy is a single bcc matrix phase in a heat treatment temperature range of 1000-1020 ℃.
The copper-aluminum-nickel-based single crystal alloy comprises 5-8% of iron, preferably 5.5-7.5%, and more preferably 6-7% by mass. In the invention, the iron and aluminum form a beta (FeAl) nano phase, and the beta (FeAl) nano phase can be dissolved back into a matrix phase in a heat treatment temperature range of 1000-1020 ℃ to promote abnormal growth of alloy grains, so that the iron and aluminum nano phase is a key factor for preparing single crystals.
In the invention, the preparation method of the copper-aluminum-nickel base single crystal alloy comprises the following steps:
according to the mass ratio, mixing copper, aluminum, nickel and iron, and then smelting to obtain an as-cast alloy;
annealing the as-cast alloy to obtain the copper-aluminum-nickel base single crystal alloy;
the temperature of the annealing treatment is 1000-1020 ℃, and the annealing time is not less than 24 hours.
According to the invention, copper, aluminum, nickel and iron are mixed according to the mass ratio and then smelted to obtain the as-cast alloy. The invention does not have any special requirements on the state and purity of the copper, the aluminum, the nickel and the iron, and the state and purity which are well known to the technical personnel in the field can be adopted. The present invention does not limit the mixing in any particular way, and the mixing may be carried out by a process known to those skilled in the art.
In the invention, the smelting temperature is preferably not less than 1600 ℃, and more preferably 1800-2000 ℃; the smelting time is preferably less than or equal to 60min, and more preferably 20-40 min. In the present invention, the number of times of melting is preferably 3 to 6 times, and more preferably 5 times. In the present invention, the melting is preferably performed in an electric arc furnace.
After the smelting is finished, the invention preferably further comprises cooling, and the cooling is carried out by adopting a process known by a person skilled in the art without any special limitation in the invention.
After the as-cast alloy is obtained, the invention carries out annealing treatment on the as-cast alloy to obtain the copper-aluminum-nickel base single crystal alloy. In the invention, the temperature of the annealing treatment is 1000-1020 ℃, and preferably 1000-1010 ℃; the time of the annealing treatment is more than or equal to 24 hours.
In the invention, the annealing treatment leads the nano-phase in the as-cast alloy to be dissolved in the matrix phase in a solid solution way, on one hand, the pinning effect of the nano-phase in preventing the crystal grain from growing is removed, on the other hand, the solid solution process of the nano-phase provides enough driving force for the abnormal growth of certain crystal grains, and the abnormal growth of the crystal grains of the alloy is promoted, so that the single crystal is formed.
After the annealing treatment is completed, the present invention preferably further comprises rapid cooling, which is preferably quenching.
After the quenching is finished, the invention also preferably comprises a process of cutting the bulk single crystal material from the super large crystal grains by a cutting method.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Note: the mass percentages described in examples 1 to 10 are not required for the mass unit of each raw material, and may be mixed in the mass units known to those skilled in the art.
Example 1
Mixing 76.5% of copper, 14% of aluminum, 4% of nickel and 5.5% of iron, repeatedly smelting for 5 times in an electric arc furnace, wherein the smelting temperature is 2000 ℃, the time is 20min, cooling to obtain an as-cast alloy, and cutting an alloy block with the thickness of 5mm from the as-cast alloy;
annealing the as-cast alloy block at 1000 ℃ for 24 hours, and then quenching to obtain the copper-aluminum-nickel-based single crystal alloy;
wherein, fig. 1 is a microstructure diagram of an as-cast alloy and a copper-aluminum-nickel-based single crystal alloy (the left diagram is the as-cast alloy, and the right diagram is the copper-aluminum-nickel-based single crystal alloy), fig. 2 is a photograph of the as-cast alloy and the copper-aluminum-nickel-based single crystal alloy (the left diagram is the as-cast alloy, and the diagram is the copper-aluminum-nickel-based single crystal alloy), and as can be seen from fig. 1, the alloy microstructure is obviously changed before and after heat treatment, an ingot is a martensite polycrystalline structure, and a parent phase + martensite single crystal structure is formed after heat; as can be seen from FIG. 2, a Cu-Al-Ni-Fe single crystal of about 20mm can be prepared by a direct annealing process.
Example 2
Mixing 74% of copper, 13% of aluminum, 7% of nickel and 6% of iron, repeatedly smelting for 5 times in an electric arc furnace, wherein the smelting temperature is 2000 ℃, the smelting time is 20min, cooling to obtain an as-cast alloy, and cutting an alloy block with the thickness of 5mm from the as-cast alloy;
annealing the as-cast alloy block at 1000 ℃ for 48 hours, and then quenching to obtain the copper-aluminum-nickel-based single crystal alloy;
wherein, fig. 3 is a microstructure diagram of an as-cast alloy and a copper-aluminum-nickel-based single crystal alloy (the left diagram is the as-cast alloy, and the right diagram is the copper-aluminum-nickel-based single crystal alloy), fig. 4 is a photograph of a solid as-cast alloy and a copper-aluminum-nickel-based single crystal alloy (the left diagram is the as-cast alloy, and the right diagram is the copper-aluminum-nickel-based single crystal alloy), and as can be seen from fig. 3, the alloy microstructure is obviously changed before and after heat treatment, an ingot is a mother phase polycrystalline structure, and the ingot is a mother phase single crystal structure; the microstructure of the alloy is obviously changed before and after heat treatment, and the alloy grows into single crystals from polycrystal; as can be seen from FIG. 4, a Cu-Al-Ni-Fe single crystal of about 20mm can be prepared by a direct annealing process.
Example 3
Mixing 77% of copper, 13% of aluminum, 4.5% of nickel and 5.5% of iron, repeatedly smelting for 5 times in an electric arc furnace, wherein the smelting temperature is 2000 ℃, the time is 20min, cooling to obtain an as-cast alloy, and cutting an alloy block with the thickness of 5mm from the as-cast alloy;
annealing the as-cast alloy block at 1020 ℃ for 24 hours, and then quenching to obtain the copper-aluminum-nickel-based single crystal alloy;
wherein, fig. 5 is a microstructure diagram of an as-cast alloy and a copper-aluminum-nickel-based single crystal alloy (the left diagram is the as-cast alloy, and the right diagram is the copper-aluminum-nickel-based single crystal alloy), fig. 6 is a photograph of a solid-cast alloy and a copper-aluminum-nickel-based single crystal alloy (the left diagram is the as-cast alloy, and the right diagram is the copper-aluminum-nickel-based single crystal alloy), and as can be seen from fig. 5, the alloy microstructure is obviously changed before and after heat treatment, an ingot is a mother phase polycrystalline structure, and a martensite single crystal structure is obtained after heat; as can be seen from FIG. 6, a Cu-Al-Ni-Fe single crystal of about 25mm can be prepared by a direct annealing process.
Example 4
Mixing 73% of copper, 14% of aluminum, 8% of nickel and 5% of iron, repeatedly smelting for 5 times in an electric arc furnace, wherein the smelting temperature is 2000 ℃, the smelting time is 20min, cooling to obtain an as-cast alloy, and cutting an alloy block with the thickness of 5mm from the as-cast alloy;
annealing the as-cast alloy block at 1000 ℃ for 48 hours, and then quenching to obtain the copper-aluminum-nickel-based single crystal alloy;
wherein, fig. 7 is a microstructure diagram of an as-cast alloy and a copper-aluminum-nickel-based single crystal alloy (the left diagram is the as-cast alloy, and the right diagram is the copper-aluminum-nickel-based single crystal alloy), and fig. 8 is a photograph of a real as-cast alloy and a copper-aluminum-nickel-based single crystal alloy (the left diagram is the as-cast alloy, and the right diagram is the copper-aluminum-nickel-based single crystal alloy), and as can be seen from fig. 7, the alloy microstructure is obviously changed before and after heat treatment, an ingot is a mother phase polycrystalline structure, and a martensite single crystal structure is obtained; as can be seen from FIG. 8, a Cu-Al-Ni-Fe single crystal of about 10mm can be prepared by the direct annealing process.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. The copper-aluminum-nickel-based single crystal alloy comprises the following alloy elements in percentage by mass: 69-81% of copper, 10-15% of aluminum, 4-8% of nickel and 5-8% of iron;
the preparation method of the copper-aluminum-nickel base single crystal alloy comprises the following steps:
according to the mass ratio, mixing copper, aluminum, nickel and iron, and then smelting to obtain an as-cast alloy;
annealing the as-cast alloy to obtain the copper-aluminum-nickel base single crystal alloy;
the temperature of the annealing treatment is 1000-1020 ℃, and the time of the annealing treatment is more than or equal to 24 hours.
2. The copper aluminum nickel base single crystal alloy of claim 1, comprising the following alloying elements in mass percent: 71.5 to 77 percent of copper, 12.5 to 14.5 percent of aluminum, 4.5 to 7.5 percent of nickel and 5.5 to 7.5 percent of iron.
3. The copper aluminum nickel base single crystal alloy according to claim 1 or 2, comprising the following alloying elements in mass percent: 72 to 75 percent of copper, 13 to 14 percent of aluminum, 5 to 7 percent of nickel and 6 to 7 percent of iron.
4. The method for preparing the copper-aluminum-nickel-based single crystal alloy according to any one of claims 1 to 3, comprising the steps of:
according to the mass ratio, mixing copper, aluminum, nickel and iron, and then smelting to obtain an as-cast alloy;
annealing the as-cast alloy to obtain the copper-aluminum-nickel base single crystal alloy;
the temperature of the annealing treatment is 1000-1020 ℃, and the annealing time is not less than 24 hours.
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Citations (3)
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| CN1173926A (en) * | 1995-02-02 | 1998-02-18 | 弗盖弗拉克斯公司 | Metal frame for spectacles |
| CN108179471A (en) * | 2018-01-10 | 2018-06-19 | 厦门大学 | A kind of ferrimanganic aluminium base single crystal alloy |
| CN109593986A (en) * | 2018-12-24 | 2019-04-09 | 厦门大学 | A kind of copper zinc-aluminium iron monocrystal alloy material |
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- 2020-08-04 CN CN202010771220.XA patent/CN111850696B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1173926A (en) * | 1995-02-02 | 1998-02-18 | 弗盖弗拉克斯公司 | Metal frame for spectacles |
| CN108179471A (en) * | 2018-01-10 | 2018-06-19 | 厦门大学 | A kind of ferrimanganic aluminium base single crystal alloy |
| CN109593986A (en) * | 2018-12-24 | 2019-04-09 | 厦门大学 | A kind of copper zinc-aluminium iron monocrystal alloy material |
Non-Patent Citations (1)
| Title |
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| YU. G. NOSOVA等: "Deformation of the Shape Memory and Surface Microrelief of Ni-Fe-Ga-Co and Cu-Al-Ni Alloy Single Crystals", 《TECHNICAL PHYSICS LETTERS: LETTERS TO THE RUSSIAN JOURNAL OF APPLIED PHYSICS》 * |
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