CN111139373A - High-strength metastable elastic copper alloy and preparation method thereof - Google Patents
High-strength metastable elastic copper alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of non-ferrous metal material preparation, and discloses a high-strength metastable elastic copper alloy and a preparation method thereof, wherein the high-strength metastable elastic copper alloy comprises the following components in percentage by mass: 9.5 to 10.5 percent of Al, 11.5 to 12.5 percent of Mn, 0.5 to 1.5 percent of Fe and the balance of Cu, and the preparation method is simpler than the common elastic copper alloy and increases the metastable state treatment compared with the common aluminum bronze preparation method. Compared with the common high-strength elastic copper alloy, the elastic copper alloy has the advantages of low cost, higher corrosion resistance and no elements harmful to the environment. The tensile strength of the alloy is more than or equal to 1000MPa, the elongation is more than or equal to 6 percent, the softening resistance temperature of the alloy exceeds 300 ℃, and based on the characteristics, the copper alloy can be applied to occasions with high requirements on strength, heat resistance and corrosion resistance, such as high-strength spring gaskets and contact springs for chemical equipment, and elastic elements in instruments and meters under a corrosive environment.
Description
Technical Field
The invention belongs to the field of preparation of non-ferrous metal materials, and particularly relates to a low-cost high-strength metastable elastic copper alloy and a preparation method thereof.
Background
The elastic copper alloy has the characteristics of corrosion resistance, high strength, no magnetism and the like, and is an important elastic material in the manufacture of industrial equipment and instruments, wherein the high-strength elastic copper alloy is mainly applied to buffering and energy storage occasions such as pressure elastic contact pieces, spring gaskets, elastic energy storage devices and the like. With the increasing use requirements of industrial production instruments and equipment and the increasingly harsh use environment, the requirements on the strength and the heat and corrosion resistance of the elastic copper alloy are increased.
The elastic copper alloy commonly used at present comprises Cu-Be alloy and Cu-Ni alloy. The Cu-Be alloy is a representative of high-strength elastic copper alloy, the typical properties of the hard state of the alloy are 750-1100MPa of tensile strength and 2-12% of elongation, and the Cu-Be alloy is widely used as a spring material. However, because the alloy contains Be, the cost of the alloy is high, toxic emissions are generated in the production and use processes, and beryllium bronze is gradually replaced by other environment-friendly high-strength copper alloys in many occasions. In addition, the heat resistance of the alloy is not so high that there is a possibility of accelerated failure when exceeding 200 ℃.
The elastic copper alloy in the Cu-Ni series alloy comprises Cu-Ni-Sn and Cu-Ni-Mn alloy, the tensile strength of the alloy is about 800MPa to 950MPa, and the elongation is about 4 percent to 12 percent. Since such alloys contain metals such as Ni and Sn, they are expensive and tend to absorb gas during melting and casting, which adversely affects the properties of the final product.
In addition, the production process of the Cu-Be and Cu-Ni series elastic copper alloy comprises solid solution and aging procedures, which not only increases the production cost, but also increases the difficulty for process control.
In view of the above situation, the development of an environment-friendly elastic copper alloy with low cost, simple production process, strength of more than or equal to 1000MPa and elongation of more than or equal to 5% for replacing part of the existing high-strength elastic copper alloy becomes an urgent need in the manufacture of modern instruments and equipment.
The existing elastic copper alloy mainly improves the mechanical property of the copper alloy in a precipitation strengthening mode, and the strengthening mechanism has the defect that a matrix needs to generate supersaturated distribution of solute atoms through solution treatment, so that the difficulty is brought to the alloy production.
Disclosure of Invention
The invention aims to overcome the problems in the prior art, provides a low-cost, high-strength and environment-friendly elastic copper alloy and a preparation method thereof, and aims to meet the requirements of high performance and simple preparation process of alloy parts in industrial production.
In order to achieve the purpose, the invention provides a high-strength metastable elastic copper alloy which comprises, by mass, 9.5-10.5% of Al, 11.5-12.5% of Mn, 0.5-1.5% of Fe, and the balance of Cu, wherein a metallographic structure of the elastic copper alloy comprises a single metastable β phase structure.
Preferably, the tensile strength of the elastic copper alloy is more than or equal to 1000MPa, the elongation is more than or equal to 6%, and the softening resistance temperature exceeds 300 ℃.
By selecting the element content proportion of Al and Mn, the finished alloy product structure can have a single metastable β phase structure, and the control of the element proportion can ensure that the β phase has high thermal stability, so that the metastable β phase can be obtained by air cooling after the alloy is hot-processed, the structure foundation is laid for simplifying the production process, and the β phase can be orderly strengthened in the multistage aging process, so that the alloy has good mechanical properties.
The invention also provides a preparation method of the high-strength metastable elastic copper alloy, which comprises the following steps:
s1, batching according to the proportion of the alloy components;
s2, feeding and smelting to obtain alloy element melt;
s3, casting to obtain a billet;
s4, carrying out metastable state treatment on the billet to obtain an alloy sample containing a metastable state β phase;
s5, and then carrying out multi-stage aging treatment on the metastable β phase of the alloy sample to obtain the alloy finished product.
Preferably, the metastable state treatment of step S4 comprises a hot rolling or hot extrusion treatment.
Preferably, the step S2 includes:
1.1) melting copper, and completely covering the liquid level of the molten liquid with charcoal after the copper is melted;
1.2) wrapping the electrolytic manganese with copper foil and pressing the wrapped electrolytic manganese into the liquid below the liquid level to completely melt the electrolytic manganese below the liquid level and prevent the oxidation of the manganese;
1.3) then adding aluminum, immediately adding iron after adding aluminum, and melting iron by utilizing the rapid temperature rise caused by the heat of melting of aluminum.
Preferably, the conditions of the hot rolling include: the hot rolling heating temperature is 600-800 ℃, and the hot rolling heating time is 1-2 hours.
Further, the total processing rate of hot rolling is more than or equal to 80%, multi-pass hot rolling is carried out, the pass reduction is 30-40%, a sample after hot rolling is air-cooled without water quenching, and the final rolling temperature is not lower than 550 ℃ so as to obtain a metastable β phase structure.
Preferably, the conditions of the hot extrusion include:
the extrusion heating temperature is 650-700 ℃, the preheating temperature of an extrusion barrel is 400-500 ℃, and the high-strength metastable elastic copper alloy is obtained by air cooling after extrusion.
Preferably, the step S5 includes the step of carrying out multi-stage aging on the metastable β phase of the alloy sample at 200-250 ℃/3h + 300-350 ℃/1h to obtain the alloy finished product.
Through the technical scheme, the high-strength metastable elastic copper alloy and the preparation method thereof provided by the invention have the following advantages:
(1) compared with the existing high-strength elastic copper alloy, the alloy does not contain expensive metals such as Ni and Sn, and the prices of Al and Mn contained in the alloy are very low, so that the raw material cost of the alloy is very low;
(2) the alloy does not contain toxic substances such as Be and the like, and belongs to an environment-friendly elastic material;
(3) according to the preparation method, the content ratio of Al and Mn elements in the alloy and the metastable state treatment heat processing technology are controlled, so that the finished alloy structure is composed of a stable metastable state β phase, the alloy is not decomposed even if the alloy is air-cooled β phase after heat processing, and a structure foundation is laid for ordered reinforcement;
(4) the alloy contains high-content Al, and a layer of oxide film is formed on the surface of the melt when the Al is smelted, so that the melt is protected from air suction, and the alloy smelting can be carried out in an atmospheric environment; a small amount of Fe in the alloy can refine the structure, and further improve the mechanical property and the hot processing technology property of the material;
(5) the β phase of the alloy has high stability, and the supersaturated solid solution structure can be reserved without quenching after hot working, thereby saving the solid solution procedure in the preparation process of the alloy and further reducing the production cost;
(6) the β phase can be orderly strengthened after multistage aging, which saves the aging process and endows the alloy with high strength and elasticity by the orderly strengthening.
The final metallographic structure of the alloy is a fibrous processing structure, and the structure can obviously improve the plasticity of the material along the rolling direction or the extrusion direction. The mechanical property of the alloy is not reduced after long-term heat preservation at 350 ℃, so the alloy can be used in occasions with higher use temperature. And because the raw material price is low, the production process is simple, and the mechanical property is not lower than that of the existing high-strength elastic copper alloy, the copper alloy has high popularization value in related industrial application.
Drawings
FIG. 1 is a metallographic phase diagram showing a side metallographic structure of a finished elastic copper alloy plate according to example 1 of the present invention;
FIG. 2 is a schematic TEM microstructure of a finished sheet of an elastic copper alloy provided in example 1 of the present invention;
fig. 3 is a SAED spectrum of a finished sheet of resilient copper alloy provided in accordance with example 1 of the present invention.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating embodiments of the invention, are given by way of illustration and explanation only, not limitation.
The invention provides a high-strength metastable elastic copper alloy, which preferably comprises 9.5-10.5% of Al, 11.5-12.5% of Mn, 0.5-1.5% of Fe and the balance of Cu by mass percentage, wherein the metallographic structure of the elastic copper alloy comprises a single metastable β phase structure.
According to a preferred embodiment of the invention, the elongation of the resilient copper alloy is equal to or greater than 6%.
According to a preferred embodiment of the invention, the resilient copper alloy has a softening resistance temperature exceeding 300 ℃.
According to a preferred embodiment of the invention, the elastic copper alloy has a tensile strength of 1000MPa or more.
By selecting the element content ratio of Al to Mn, the finished alloy structure can have a single metastable β phase structure, and the control of the element ratio can ensure that the β phase has high thermal stability, so that the alloy can be subjected to air cooling after hot working to obtain a metastable β phase, the β phase is not decomposed during the air cooling after hot working, the structure foundation is laid for simplifying the production process, and the β phase can be orderly strengthened in the multistage aging process after hot working, so that the alloy is endowed with high mechanical properties.
The alloy does not contain expensive metals such as Ni and Sn, and the prices of Al and Mn contained in the alloy are very low, so the raw material cost of the alloy is very low; meanwhile, the alloy does not contain toxic substances such as Be and the like, belongs to an environment-friendly elastic material, contains high-content Al, and forms an oxide film on the surface of molten liquid during smelting of the Al, so that the molten liquid is protected from air suction, the alloy smelting can Be carried out in an atmospheric environment, and a small amount of Fe in the alloy can refine the structure, so that the mechanical property and the hot-working process property of the material are further improved.
Compared with the common high-strength elastic copper alloy, the elastic copper alloy prepared by the preparation method provided by the invention has the advantages of low cost, corrosion resistance and no elements harmful to the environment, the tensile strength of the elastic copper alloy is more than or equal to 1000MPa, the elongation is more than or equal to 6%, the softening resistance temperature of the alloy exceeds 300 ℃, and based on the characteristics, the copper alloy can be applied to occasions with higher requirements on strength, heat resistance and corrosion resistance, such as high-strength spring gaskets and contact springs for chemical equipment, and elastic elements in instruments and meters under a corrosion environment.
The preparation method is based on the strengthening mechanism of ordered strengthening, the metastable metal matrix is formed, and the elastic copper alloy is strengthened by ordering the matrix, and the preparation method is characterized in that the high-temperature metastable structure of the CuAlMn alloy can be reserved only by air cooling without solid solution and water cooling after hot processing by controlling alloy components and hot processing technology, so that the strengthening of the alloy is finally realized by forming the ordered structure in the multistage aging process.
The preparation method of the high-strength metastable elastic copper alloy comprises the following steps:
s1, batching according to the proportion of the alloy components;
s2, feeding and smelting to obtain alloy element melt;
s3, casting to obtain a billet;
s4, carrying out metastable state treatment on the billet to obtain an alloy sample containing a metastable state β phase;
s5, and then carrying out multi-stage aging treatment on the metastable β phase of the alloy sample to obtain the alloy finished product.
According to a preferred embodiment of the present invention, the melting process of step S2 preferably includes: the copper is melted first, and after the copper is melted, the liquid level of the solution is completely covered by charcoal. Then adding electrolytic manganese, wherein the electrolytic manganese is wrapped by copper foil, and then adding the electrolytic manganese to the molten liquid in batches. After the electrolytic manganese is added, the electrolytic manganese bag is pressed below the liquid level, so that the electrolytic manganese is completely melted below the liquid level, and the oxidation of the manganese is prevented. Then adding aluminum, immediately adding iron after adding aluminum, and melting the refractory iron by utilizing rapid melt temperature rise caused by the heat of melting of aluminum.
According to the present invention, the metastable state processing in said step S4 includes a hot rolling process or a hot extrusion process.
According to the preferred embodiment of the invention, the specific technological parameters in the hot rolling process are that the hot rolling heating temperature is 600-800 ℃, the hot rolling heating time is 1-2 hours, the alloy can be continuously rolled to the final thickness in multiple passes, the hot rolling heating temperature is selected on the basis of ensuring that the final rolling temperature is not lower than 550 ℃, so that the alloy can keep a metastable β phase structure, intermediate annealing is not needed in the hot rolling process, the total processing rate of hot rolling is more than or equal to 80%, the pass reduction is about 30-40%, and the hot rolling process is air-cooled.
According to a preferred embodiment of the present invention, the specific process parameters in the hot extrusion process are preferably as follows: heating the extruded billet at 650-700 deg.c, preheating the extruding cylinder at 400-500 deg.c, and air cooling the extruded workpiece.
Then carrying out multistage aging on the metastable β phase of the alloy sample at 200-250 ℃/3h and 300-350 ℃/1h to obtain an alloy finished product.
The preparation method of the invention controls the content proportion of Al and Mn elements in the alloy and the hot working process, so that the finished product structure of the alloy is composed of the metastable β phase which is very stable, the alloy is not decomposed even if the β phase is air-cooled after hot working, the structure foundation is laid for ordered reinforcement, the β phase composing the alloy has very high stability, the supersaturated solid solution structure can be kept without quenching after hot working, the solid solution procedure in the preparation process of the alloy is omitted, the production cost is further reduced, the β phase can be ordered reinforced in the multistage aging process, and the alloy is endowed with high strength and elasticity by ordered reinforcement.
The final metallographic structure obtained by the preparation method is a fibrous processing structure, the structure can obviously improve the plasticity of the material along the rolling direction or the extrusion direction, and the long-term heat-preservation mechanical property of the obtained elastic copper alloy at 350 ℃ is not reduced, so that the elastic copper alloy can be used for occasions with higher use temperature.
The present invention will be described in further detail with reference to specific examples.
Example 1
The alloy of this example comprises the following ingredients: 10% of Al, 12% of Mn, 1% of Fe and the balance of Cu.
In the embodiment, the preparation method of the high-strength metastable-state elastic copper alloy provided by the invention comprises the following specific preparation processes:
1. smelting: the copper is melted first, and after the copper is melted, the liquid level of the solution is completely covered by charcoal. Then adding electrolytic manganese, wherein the electrolytic manganese is wrapped by copper foil, and then adding the electrolytic manganese to the molten liquid in batches. After the electrolytic manganese is added, the electrolytic manganese bag is pressed below the liquid surface, so that the electrolytic manganese is completely melted below the liquid surface. Then adding aluminum, immediately adding iron after adding the aluminum, and simultaneously stirring the molten liquid to enable the Fe to be dissolved more quickly. And then, scattering a slagging agent on the surface of the melt, simultaneously carrying out 1100 ℃ heat preservation on the melt for 10min, after the heat preservation is finished, slagging off the melt, and then casting into a square ingot with the cross section of 20mm multiplied by 100 mm.
2. Milling the surface of the cast ingot by 1mm, and then carrying out hot rolling; specific conditions of the hot rolling process include: the hot rolling heating temperature is 750 ℃, and the heating time is 1 hour.
The hot rolling pass distribution is as follows: 18mm → 11mm → 6mm → 3mm → 2mm, hot rolling is carried out continuously in 4 passes without annealing treatment in the middle, the surface temperature of the hot rolled plate is 600 ℃, and then air cooling is carried out to the room temperature.
Referring to fig. 1-3, fig. 1 shows a sheet structure of air-cooled to room temperature, the sheet structure is a fibrous processed structure, fig. 2 and 3 show TEM structures and corresponding SAED patterns of the alloy at room temperature, the obtained alloy matrix is metastable β phase, and a large number of ordered domain structures are formed, thereby producing ordered strengthening.
Example 2
The alloy of this example comprises the following ingredients: 10% of Al, 12% of Mn, 1% of Fe and the balance of Cu.
In the embodiment, the preparation method of the high-strength metastable-state elastic copper alloy provided by the invention comprises the following specific preparation processes:
1. smelting: the copper is melted first, and after the copper is melted, the liquid level of the solution is completely covered by charcoal. Then adding electrolytic manganese, wherein the electrolytic manganese is wrapped by copper foil, and then adding the electrolytic manganese to the molten liquid in batches. After the electrolytic manganese is added, the electrolytic manganese bag is pressed below the liquid surface, so that the electrolytic manganese is completely melted below the liquid surface. Then adding aluminum, immediately adding iron after adding the aluminum, and simultaneously stirring the molten liquid to enable the Fe to be dissolved more quickly. Then, spreading a slag removing agent on the surface of the melt, simultaneously carrying out heat preservation on the melt at 1100 ℃ for 10min, slagging off the melt after the heat preservation is finished, and then casting the melt into round ingots with the diameter of 80 mm.
2. And milling the surface of the cast ingot by 1mm, and then carrying out hot extrusion. The specific conditions of the hot extrusion process are as follows: heating at 700 deg.C for 1 hr, heating at 400 deg.C with an extrusion cylinder, hot-extruding the cast ingot into round bar with diameter of 20mm, and air cooling the extruded bar without water quenching.
Table 1 shows the high-strength metastable elastic CuAlMn alloy and the common high-strength elastic copper alloy QBe obtained by the alloy preparation method of the embodiment of the invention2And the performance of CuNiMn.
TABLE 1
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, numerous simple modifications can be made to the technical solution of the invention, including combinations of the specific features in any suitable way, and the invention will not be further described in relation to the various possible combinations in order to avoid unnecessary repetition. Such simple modifications and combinations should be considered within the scope of the present disclosure as well.
Claims (9)
1. The high-strength metastable elastic copper alloy is characterized by comprising 9.5-10.5% of Al, 11.5-12.5% of Mn, 0.5-1.5% of Fe and the balance of Cu by mass percentage, and the metallographic structure of the elastic copper alloy comprises a single metastable β phase structure.
2. The elastic copper alloy according to claim 1, wherein the elastic copper alloy has a tensile strength of 1000MPa or more, an elongation of 6% or more, and a softening resistance temperature of 300 ℃ or more.
3. A method of producing a high strength metastable elastic copper alloy according to claim 1 or 2, characterized in that the method comprises the steps of:
s1, batching according to the proportion of the alloy components;
s2, feeding and smelting to obtain alloy element melt;
s3, casting to obtain a billet;
s4, carrying out metastable state treatment on the billet to obtain an alloy sample containing a metastable state β phase;
s5, and then carrying out multi-stage aging treatment on the metastable β phase of the obtained alloy sample to obtain an alloy finished product.
4. The production method according to claim 3, wherein the metastable treatment of step S4 includes a hot rolling or hot extrusion treatment.
5. The production method according to claim 3, wherein the step S2 includes:
1.1) melting copper, and completely covering the liquid level of the molten liquid with charcoal after the copper is melted;
1.2) wrapping the electrolytic manganese with copper foil and pressing the wrapped electrolytic manganese into the liquid below the liquid level to completely melt the electrolytic manganese below the liquid level and prevent the oxidation of the manganese;
1.3) then adding aluminum, immediately adding iron after adding aluminum, and melting iron by utilizing the rapid temperature rise caused by the heat of melting of aluminum.
6. The production method according to claim 4, wherein the conditions of the hot rolling include: the hot rolling heating temperature is 600-800 ℃, and the hot rolling heating time is 1-2 hours.
7. The preparation method of claim 6, wherein the total hot rolling processing rate is more than or equal to 80%, the hot rolling is carried out in multiple passes, the pass reduction is 30-40%, and a sample after the hot rolling is air-cooled without water quenching; the finishing temperature is not lower than 550 ℃.
8. The production method according to claim 4, wherein the conditions of the hot extrusion include:
the extrusion heating temperature is 650-700 ℃, the preheating temperature of the extrusion barrel is 400-500 ℃, and air cooling is carried out after extrusion.
9. The production method according to claim 3, wherein the step S5 includes:
and carrying out multistage aging on the metastable β phase of the alloy sample at 200-250 ℃/3h and 300-350 ℃/1h to obtain an alloy finished product.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002105559A (en) * | 2000-09-29 | 2002-04-10 | Tokin Corp | TWO-WAY ELEMENT MADE OF Cu-Al-Mn BASED ALLOY |
| CN105164289A (en) * | 2013-05-10 | 2015-12-16 | 国立大学法人东北大学 | Cu-Al-Mn-based bar material and plate material demonstrating stable superelasticity, method for manufacturing said bar material and plate material, seismic control member in which said bar material and plate material are used, and seismic control structure in which seismic control member is used |
| CN105408509A (en) * | 2013-07-16 | 2016-03-16 | 古河科技材料株式会社 | Expanded member comprising Cu-Al-Mn alloy material and exhibiting superior anti-stress corrosion properties, and use therefor |
| CN108998694A (en) * | 2018-07-06 | 2018-12-14 | 武汉理工大学 | A kind of preparation method of superelastic alloy local enhancement concrete anti-earthquake column |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002105559A (en) * | 2000-09-29 | 2002-04-10 | Tokin Corp | TWO-WAY ELEMENT MADE OF Cu-Al-Mn BASED ALLOY |
| CN105164289A (en) * | 2013-05-10 | 2015-12-16 | 国立大学法人东北大学 | Cu-Al-Mn-based bar material and plate material demonstrating stable superelasticity, method for manufacturing said bar material and plate material, seismic control member in which said bar material and plate material are used, and seismic control structure in which seismic control member is used |
| CN105408509A (en) * | 2013-07-16 | 2016-03-16 | 古河科技材料株式会社 | Expanded member comprising Cu-Al-Mn alloy material and exhibiting superior anti-stress corrosion properties, and use therefor |
| CN108998694A (en) * | 2018-07-06 | 2018-12-14 | 武汉理工大学 | A kind of preparation method of superelastic alloy local enhancement concrete anti-earthquake column |
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