CN114752807A - Cu-Cr-Nb-Zr alloy and preparation method thereof - Google Patents
Cu-Cr-Nb-Zr alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Cu-Cr-Nb-Zr alloy and a preparation method thereof. The method comprises the following specific steps: and (3) putting the cathode Cu, CuCr, CuNb and CuZr intermediate alloy into a crucible in a vacuum induction furnace for smelting, pouring into a water-cooled copper casting die for rapid cooling, and obtaining the Cu-Cr-Nb-Zr cast ingot. And (4) carrying out mechanical processing, solid solution treatment and aging treatment on the cast ingot to obtain a finished Cu-Cr-Nb-Zr alloy product. The invention realizes the proportion and distribution control of precipitated phases by controlling the mass fraction ratio of Cr to Nb, and generates coarse high-temperature resistant phase Cr at crystal boundary2The Nb phase stabilizes the crystal boundary, generates fine Cr precipitation phase in the crystal to strengthen the matrix, realizes the improvement of the high-temperature creep resistance of the Cu-Cr-Nb alloy, and adopts the alloy preparation of non-powder metallurgyThe process realizes low cost of material preparation.
Description
Technical Field
The invention relates to the technical field of copper alloy preparation, in particular to a high creep resistance Cu-Cr-Nb-Zr alloy and a preparation method thereof.
Background
The CuCrZr alloy exhibits higher room temperature strength due to the Cr precipitate phase in the structure having a dimension less than 10nm, but the existing CuCrZr alloy has poor creep resistance at temperatures above 400 ℃, due to the rapid coarsening of the Cr precipitate phase at high temperatures above 400 ℃ and the alloy lacks other pinning grain boundary secondary phases. In contrast, CuCrNb alloy (a typical alloy is Cu-8Cr-4Nb, at.%) is due to the large amount of Cr distributed in the crystal and at the grain boundaries2Nb phase has higher high temperature creep resistance. However, because the atomic fraction of Nb is high in the CuCrNb alloy, all Cr atoms in the alloy and Nb generate Cr together2And (4) a Nb phase. The CuCrNb alloy contains high content of Cr and Nb elements, and needs to be prepared by high-cost powder metallurgy industry to avoid forming too coarse Cr in the conventional casting process2A Nb phase. The high manufacturing cost ensures that the CuCrNb alloy can only be applied to the inner wall of a high-end rocket engine combustion chamber, and the application of the alloy is limited. The high-temperature creep mechanism of the copper alloy material mainly comprises a grain boundary sliding mechanism, a dislocation movement mechanism and the like, and in order to improve the high-temperature creep resistance of the copper alloy, a second phase for stabilizing the grain boundary and inhibiting the dislocation slip in the alloy needs to be added. Therefore, there is a need to develop a copper alloy based on the existing copper alloy, which not only has lower manufacturing cost, but also improves the high-temperature creep resistance of the material by adding a second phase element.
The patent "a preparation method of a high-strength high-conductivity copper alloy bar" (CN 107586977B) and the patent "a preparation method of Cu-Cr-Nb alloy" (CN 107653386B) respectively disclose methods for preparing a high-strength high-conductivity CuCrNb alloy by casting in an argon-protected vacuum induction melting furnace in combination with a fine-diameter graphite mold and melting by only adopting an argon-protected vacuum induction melting furnace. The alloy comprises 0.5-1.5% of Cr and 0.1-0.5% of Nb by mass percent, and because the proportion of Cr/Nb elements is not specifically limited and elements for purifying grain boundaries are added, the distribution of precipitated phases in a microstructure cannot be accurately controlled. The patents CN111440963B, CN112553500A, and CN110218897A all adopt an aerosol method to prepare CuCrNb alloy powder, and then use hot pressing, SPS and other processes to realize alloy preparation, and expensive rare elements such as Co, Ti, and rare earth elements are added to the alloy, which increases the cost of raw materials, and meanwhile, in the preparation process, the cost of gas atomization energy consumption is also high, the alloy preparation process is cumbersome, and is not beneficial to the low cost of alloy preparation. According to the current literature search, the current Cu-Cr-Nb alloy and the preparation method thereof have certain technical defects in alloy component design and process routes, and the improvement of the high-temperature creep resistance and the low-cost production are difficult to realize.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high creep resistance Cu-Cr-Nb-Zr alloy and a low-cost preparation method thereof.
The invention is realized by the following technical scheme.
A Cu-Cr-Nb-Zr alloy, characterized in that the composition of said alloy comprises, in weight percent: 1.0-2.0% of Cr, 0.85-1.7% of Nb and 0.05-0.2% of Zr; the balance of Cu and inevitable impurities.
Further, the mass percentage of Cr and Nb in the components of the Cu-Cr-Nb-Zr alloy satisfies the following condition: Cr/Nb is more than 1.15 and less than 1.5.
The invention provides a preparation method of a Cu-Cr-Nb-Zr alloy, which is characterized by comprising the following steps:
(1) preparing materials according to the weight percentage of each element, and introducing argon into a vacuum induction furnace for smelting, wherein the alloy is heated to 1150-1200 ℃ firstly, and the temperature is kept for 15-30 min; then heating to 1350-1500 ℃, preserving heat for 20-30min, and then pouring into a water-cooled copper mold to rapidly cool to obtain a Cu-Cr-Nb-Zr alloy ingot;
(2) and (2) mechanically processing the Cu-Cr-Nb-Zr alloy ingot obtained in the step (1) to obtain a Cu-Cr-Nb-Zr alloy plate, and then carrying out solid solution and aging treatment.
Further, the raw materials of each element in the step (1) are as follows: the Cu adopts electrolytic copper with the purity of more than or equal to 99.99 percent, the Cr adopts CuCr intermediate alloy to be added, the Nb adopts CuNb intermediate alloy to be added, and the Zr adopts CuZr intermediate alloy to be added.
Further, the solution treatment temperature in the step (2) is 950-1000 ℃, the heat preservation time is 0.5-2h, and then water quenching is carried out; the aging treatment temperature is 400-500 ℃, and the heat preservation time is 3-5 h.
Furthermore, the obtained alloy microstructure contains coarse Cr distributed in grain boundary of 2-10 μm2Nb phase, 2-10nm fine Cr phase and 20-40nm Cu phase distributed in the crystal5Zr phase, the grain size of the alloy is controlled within the range of 25 to 120 μm.
The invention has the beneficial technical effects that the Cr element and the Nb element in the structure are realized by controlling the proportion of the Cr element and the Nb element in the Cu-Cr-Nb alloy2The proportion and distribution of Nb and Cr precipitated phases are controlled. Fine and dispersed nano-scale Cr phases are precipitated in the crystal after solid solution and aging treatment, a copper matrix is strengthened, and a dislocation motion mechanism in the alloy creep process is inhibited; coarse high-temperature resistant Cr is generated at grain boundary2The Nb phase stabilizes the crystal boundary and inhibits a dislocation slip mechanism; by adding trace element Zr, impurity elements of grain boundaries are captured, and the alloy strength is improved while the grain boundaries are purified. Cr in alloy2The Nb phase is enriched in the crystal boundary, the grain growth at high temperature is inhibited, and the copper alloy matrix with the multi-mode grain size of fine grains and coarse grains is obtained. Passing through grain boundary Cr2The high-temperature creep resistance of the copper alloy is effectively improved by the Nb phase, the fine dispersed Cr precipitated phase and the multi-mode grain size, and the creep rate at 500 ℃ and 90MPa can reach 6.7 multiplied by 10-5S; the cost reduction of material preparation is realized by adopting a non-powder metallurgy alloy preparation process.
Drawings
FIG. 1 is a process flow diagram of the preparation method of the present invention.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
a Cu-Cr-Nb-Zr alloy comprises the following components in percentage by weight: 1.5 percent of Cr, 1.25 percent of Nb1.05 percent of Zr; the balance of Cu and inevitable impurities.
The method for preparing the Cu-Cr-Nb-Zr alloy according to the present embodiment includes the following steps:
(1) placing the prepared raw materials in a crucible of a vacuum furnace, and vacuumizing to 1 × 10-3And introducing argon as a protective gas to smelt in a vacuum induction smelting furnace, firstly heating the alloy to 1150 ℃, preserving heat for 15min, then heating to 1350 ℃, preserving heat for 30min, then pouring the alloy liquid into a water-cooled copper mould below, and introducing circulating cooling water into the water-cooled copper mould to ensure that the ingot is rapidly cooled to obtain the Cu-Cr-Nb-Zr alloy ingot.
(2) And (2) carrying out 70% cold rolling on the Cu-Cr-Nb-Zr alloy ingot obtained in the step (1) to obtain a Cu-Cr-Nb-Zr alloy plate.
(3) And (3) placing the alloy plate obtained in the step (2) into a heat treatment furnace, carrying out solution treatment of maintaining the temperature at 970 ℃ for 1h, and then carrying out water quenching.
(4) And (4) placing the plate sample obtained by the treatment in the step (3) into a heat treatment furnace for aging treatment, wherein the temperature is 460 ℃, and the heat preservation time is 3 hours.
This example gives an alloy with an average grain size of 103 μm and a microstructure comprising coarse Cr of 4-6 μm distributed at the grain boundaries2Nb phase, fine Cr phase of 2-8nm distributed in the crystal, and Cu of about 30nm5A Zr phase.
Example 2
A Cu-Cr-Nb-Zr alloy comprises the following components in percentage by weight: 1.6 percent of Cr, 1.12 percent of Nb1.12 percent of Zr and 0.2 percent of Zr; the balance of Cu and inevitable impurities.
The method for preparing the Cu-Cr-Nb-Zr alloy according to the present embodiment includes the following steps:
(1) placing the prepared raw materials in a crucible of a vacuum furnace, and vacuumizing to 1 × 10-3And introducing argon as a protective gas to smelt in a vacuum induction smelting furnace, firstly heating the alloy to 1170 ℃, preserving heat for 30min, then heating to 1450 ℃, preserving heat for 20min, then pouring the alloy liquid into a water-cooled copper mould below, and introducing circulating cooling water into the water-cooled copper mould to ensure that the ingot is rapidly cooled to obtain the Cu-Cr-Nb-Zr alloy ingot.
(2) And (2) carrying out 80% cold rolling on the Cu-Cr-Nb-Zr alloy ingot obtained in the step (1) to obtain a Cu-Cr-Nb-Zr alloy plate.
(3) And (3) placing the alloy plate obtained in the step (2) in a heat treatment furnace, performing solution treatment at 990 ℃ for 2 hours, and then performing water quenching.
(4) And (4) placing the plate sample obtained by the treatment in the step (3) into a heat treatment furnace for aging treatment, wherein the temperature is 490 ℃, and the heat preservation time is 5 hours.
The alloy obtained in this example had an average grain size of 85 μm and a microstructure comprising coarse Cr of 2-6 μm distributed in the grain boundaries2Nb phase, 4-8nm fine Cr phase and 15-30nm Cu phase distributed in the crystal5A Zr phase.
Example 3
A Cu-Cr-Nb-Zr alloy comprises the following components in percentage by weight: 1.8% of Cr, 1.38% of Nb1.38% of Zr and 0.13% of Zr; the balance of Cu and inevitable impurities.
The method for preparing the Cu-Cr-Nb-Zr alloy according to the present embodiment includes the following steps:
(1) placing the prepared raw materials in a crucible of a vacuum furnace, and vacuumizing to 1 × 10-3And introducing argon as a protective gas to smelt in a vacuum induction smelting furnace, heating the alloy to 1190 ℃, preserving heat for 25min, heating to 1400 ℃, preserving heat for 25min, pouring the alloy liquid into a water-cooled copper mould below, and introducing circulating cooling water into the water-cooled copper mould to ensure that the ingot is rapidly cooled to obtain the Cu-Cr-Nb-Zr alloy ingot.
(2) And (2) carrying out 85% cold rolling on the Cu-Cr-Nb-Zr alloy ingot obtained in the step (1) to obtain a Cu-Cr-Nb-Zr alloy plate.
(3) And (3) placing the alloy plate obtained in the step (2) into a heat treatment furnace, carrying out solution treatment of keeping the temperature at 960 ℃ for 0.8h, and then carrying out water quenching.
(4) And (4) placing the plate sample obtained by the treatment in the step (3) into a heat treatment furnace for aging treatment, wherein the temperature is 430 ℃, and the heat preservation time is 4 hours.
The alloy obtained in this example had an average grain size of 57 μm and a microstructure comprising coarse Cr distributed in the grain boundaries in the range of 3 to 7 μm2Nb phase, 2-5nm fine Cr phase and 25-40nm Cu phase distributed in the crystal5A Zr phase.
Example 4:
a Cu-Cr-Nb-Zr series alloy comprises the following components in percentage by weight: 2.0% of Cr, 1.5% of Nb1.5% of Zr and 0.15% of Zr; the balance of Cu and inevitable impurities.
The method for preparing the Cu-Cr-Nb-Zr alloy according to the present embodiment includes the following steps:
(1) placing the prepared raw materials in a crucible of a vacuum furnace, and vacuumizing to 1 × 10-3And introducing argon as a protective gas to smelt in a vacuum induction smelting furnace, firstly heating the alloy to 1200 ℃, preserving heat for 20min, then heating to 1500 ℃, preserving heat for 30min, then pouring the alloy liquid into a water-cooled copper mould below, and introducing circulating cooling water into the water-cooled copper mould to ensure that the ingot is rapidly cooled to obtain the Cu-Cr-Nb-Zr alloy ingot.
(2) And (2) carrying out 65% cold rolling deformation on the Cu-Cr-Nb-Zr alloy ingot obtained in the step (1) to obtain a Cu-Cr-Nb-Zr alloy plate.
(3) And (3) placing the alloy plate obtained in the step (2) into a heat treatment furnace, carrying out solution treatment of keeping the temperature at 980 ℃ for 1.5h, and then carrying out water quenching.
(4) And (4) placing the plate sample treated in the step (3) into a heat treatment furnace for aging treatment, wherein the temperature is 475 ℃, and the heat preservation time is 3.5 hours.
The alloy obtained in this example had an average grain size of 30 μm and a microstructure including grain boundaries distributed thereinCoarse Cr of 5-10 μm2Nb phase, 2-8nm fine Cr phase and 20-30nm Cu phase distributed in the crystal5A Zr phase.
Comparative example:
a Cu-Cr-Zr-based alloy was prepared as a comparative example, comprising the following contents of components in weight percent: 1.2 percent of Cr and 0.85 percent of ZrC; the balance of Cu and inevitable impurities.
The method for producing the Cu-Cr-Zr alloy of the present comparative example includes the steps of:
(1) placing the prepared raw materials in a crucible of a vacuum furnace, and vacuumizing to 1 × 10-3And introducing argon as a protective gas to smelt in a vacuum induction smelting furnace, firstly heating the alloy to 1150 ℃, preserving heat for 25min, then heating to 1350 ℃, preserving heat for 25min, then pouring the alloy liquid into a water-cooled copper mould below, and introducing circulating cooling water into the water-cooled copper mould to ensure that the cast ingot is rapidly cooled to obtain the Cu-Cr-Zr alloy ingot.
(2) And (2) carrying out cold rolling on 80% of the Cu-Cr-Zr alloy ingot obtained in the step (1) to obtain a Cu-Cr-Zr alloy plate.
(3) And (3) placing the alloy plate obtained in the step (2) into a heat treatment furnace, carrying out solution treatment of keeping the temperature at 960 ℃ for 1h, and then carrying out water quenching.
(4) And (4) placing the plate sample obtained by the treatment in the step (3) into a heat treatment furnace for aging treatment, wherein the temperature is 450 ℃, and the heat preservation time is 4 hours.
The comparative example obtained an alloy having an average grain size of 50 μm and a microstructure comprising a fine Cr phase with a size of 2-8nm and a Cu5Zr phase with a size of 10-30 nm.
The high temperature creep property test results of the Cu-Cr-Zr alloy sheets prepared in the comparative examples are shown in Table 1.
TABLE 1 creep properties of CuCrZr alloy compositions of inventive examples 1-4 and comparative examples and samples prepared by different processes
As can be seen from Table 1, in the examples, compared with the comparative examples, since the alloy structure of the comparative examples only contains the Cr phase, coarsening occurs at high temperature, so that the creep resistance of the alloy is poor, and the creep rate is obviously higher than that of the 4 examples. The proportion of Cr2Nb phase is minimal in example 1, and the ability to stabilize grain boundaries is relatively weak, so the creep resistance of the alloy is less than that of examples 2, 3 and 4. Therefore, the preparation method of the high creep resistance Cu-Cr-Nb-Zr copper alloy has the advantages that the steps are mutually cooperated and matched, the alloy element proportion is controlled, and the Cr in the obtained alloy microstructure is subjected to solution treatment and aging treatment2The Nb phase is distributed in the crystal boundary and combined with the crystal boundary element Zr to effectively inhibit the crystal boundary sliding in the creep process, and the Cr phase strengthens the matrix in the crystal, so that the finally obtained product has more excellent creep resistance index, and the market competitiveness of the product is improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.
Claims (6)
1. A Cu-Cr-Nb-Zr alloy, characterized in that the composition of said alloy comprises, in weight%: 1.0-2.0% of Cr, 0.85-1.7% of Nb and 0.05-0.2% of Zr; the balance of Cu and inevitable impurities.
2. The Cu-Cr-Nb-Zr-based alloy according to claim 1, wherein said alloy has a composition in which the mass percentages of Cr and Nb are as follows: Cr/Nb is more than 1.15 and less than 1.5.
3. A method for producing a Cu-Cr-Nb-Zr-based alloy according to claim 1 or 2, characterized by comprising the steps of:
(1) preparing materials according to the weight percentage of each element, and smelting in a vacuum induction smelting furnace with argon protection, wherein firstly, the alloy is heated to 1150-1200 ℃, and the temperature is kept for 15-30 min; then heating to 1350-1500 ℃, preserving heat for 20-30min, and then pouring into a water-cooling copper mould to be cooled to obtain a Cu-Cr-Nb-Zr alloy ingot;
(2) and (2) mechanically processing the Cu-Cr-Nb-Zr alloy ingot obtained in the step (1) to obtain a Cu-Cr-Nb-Zr alloy plate, and then carrying out solid solution and aging treatment.
4. The preparation method according to claim 3, wherein the raw materials of each element in the step (1) are as follows: the Cu adopts electrolytic copper with the purity of more than or equal to 99.99 percent, the Cr adopts CuCr intermediate alloy to be added, the Nb adopts CuNb intermediate alloy to be added, and the Zr adopts CuZr intermediate alloy to be added.
5. The preparation method according to claim 3, characterized in that the solution treatment temperature in the step (2) is 950-1000 ℃, the holding time is 0.5-2h, and then water quenching is carried out; the aging treatment temperature is 400-500 ℃, and the heat preservation time is 3-5 h.
6. The method according to claim 3, wherein the microstructure of the obtained alloy contains coarse Cr of 2-10 μm distributed in grain boundaries2Nb phase, 2-10nm fine Cr phase and 20-40nm Cu phase distributed in the crystal5A Zr phase.
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