CN116179889A - Copper alloy bar and preparation method thereof - Google Patents
Copper alloy bar and preparation method thereof Download PDFInfo
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- CN116179889A CN116179889A CN202310008766.3A CN202310008766A CN116179889A CN 116179889 A CN116179889 A CN 116179889A CN 202310008766 A CN202310008766 A CN 202310008766A CN 116179889 A CN116179889 A CN 116179889A
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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
- C22C9/04—Alloys based on copper with zinc as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0075—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for rods of limited length
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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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
- C22C9/10—Alloys based on copper with silicon as the next major constituent
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- 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
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Abstract
The invention discloses a copper alloy bar, which is characterized in that: the copper alloy comprises the following components in percentage by mass: 1.0 to 2.0wt percent, mn:0.3 to 0.8 weight percent of Zn:0.01 to 1.2 weight percent, less than or equal to 0.10 weight percent of Fe, less than or equal to 0.007 weight percent of Pb, and the balance of Cu and unavoidable impurities. The contents of Si, mn and Zn in the copper alloy are controlled, the proportion of MnSi brittle phases is controlled, and the excellent cold heading performance and mechanical property and tensile strength of the material are obtained: 360-450 Mpa, yield strength: 310-400 MPa, area shrinkage Z: 40-60%, hardness HV: 100-150.
Description
Technical Field
The invention belongs to the technical field of copper alloy, and particularly relates to a copper alloy bar and a preparation method thereof.
Background
Fasteners are a generic term for a type of mechanical part used when two or more parts are fastened together as a single piece. C65100 is a fastener which takes Si and Mn as main alloy elements, has good mechanical property and can be used for cold heading bolts, screws, nuts and the like. Cold heading is a processing method that utilizes plastic deformation of metal under the action of external force, and redistributes and transfers the volume of metal by means of a die, thereby forming the required part or blank. The cold heading process is most suitable for producing the fastener, replaces the cutting process, has high production efficiency and saves raw materials.
The good cold heading performance means that the copper alloy has lower deformation resistance, can withstand deformation to a great extent without generating cracks, and the reduction of area and the yield strength can reflect the good and bad cold heading performance of the material, and the larger the reduction of area is, the lower the yield strength is, which indicates that the better the cold heading performance of the material is. However, as the fastener, the torque test is required to pass, so that the strength is required to be kept high, and the fastener is prevented from deforming when being stressed.
Although C65100 has excellent cold deformation processing performance, when the cold heading is processed into fasteners such as screws, nuts and the like, small cracks which are invisible to naked eyes are easy to form because the deformation generally reaches 60-90%, and the small cracks expand and crack under the action of external force during the service period of the material, so that hidden danger is caused to the safe operation of equipment. The main reasons are as follows: the grain size is uneven, the difference between the minimum grain size and the maximum grain size reaches about 70 mu m, the grain orientation is disordered and has anisotropy, when the material is cold-headed and deformed due to structural defects, the deformation quantity and the stress state of each grain are different, the difference can be embodied in different parts of a macroscopic scale sample and also exist in the inside of the grains with different orientations, even in different areas of the same grain, the deformation quantity and the stress state are different, the stress distribution is extremely uneven, the tensile stress born by the part with the largest cold deformation is the largest, tiny cracks are most easily generated, and the fastener for C65100 silicon-manganese-copper processing on the market at present cannot be used in scenes with extremely high requirements on the safety performance of the material, so that the current silicon-manganese-copper component and processing technology need to be improved, the silicon-manganese-copper rod wire with uniform grain size and consistent orientation can be prepared, and the requirements of industries such as aviation, navigation, electric power and the like on silicon-manganese-copper are met.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a copper alloy bar with excellent cold heading performance.
The second technical problem to be solved by the invention is to provide a preparation method of a copper alloy bar.
The invention solves the first technical problem by adopting the technical scheme that: a copper alloy bar, characterized in that: the copper alloy comprises the following components in percentage by mass: 1.0 to 2.0wt percent, mn:0.3 to 0.8 weight percent of Zn:0.01 to 1.2 weight percent, less than or equal to 0.10 weight percent of Fe, less than or equal to 0.007 weight percent of Pb, and the balance of Cu and unavoidable impurities.
Si: si has the maximum solubility of 5.3% at 852 ℃, but decreases with the decrease of temperature, si can improve the hardness and strength of Cu, when the Si content is lower than 1%, the contradiction problem between alloy strength and forgeability can occur, the requirement of the fastener on the tensile strength of the Si-Mn-Cu rod wire being more than or equal to 350MPa can be met by increasing the processing rate of the rod wire stretching deformation, and the negative problem is that the forgeability of the Si-Mn-Cu is poor due to the strong processing hardening effect, and cracks are easy to generate during cold heading deformation; however, as the Si content increases, the Si content exceeds 2%, and the malleability of the silicomanganese copper starts to decrease, mainly because Si combines with Mn to form a MnSi brittle phase. Therefore, the Si content of the silicon-manganese-copper is controlled to be 1.0-2.0wt%.
Mn: mn is dissolved in copper in a solid solution mode, so that the softening temperature of the silicon-manganese-copper can be improved, and the mechanical property and the processing property of the silicon-manganese-copper can be improved. When the Mn content is lower than 0.3%, the softening temperature of the silicon-manganese-copper cannot reach more than 430 ℃ by adjusting the content of other alloy elements of the silicon-manganese-copper and the processing technology; when Mn exceeds 0.8%, mn which is not completely dissolved is combined with Si to form MnSi brittle phase, and the forgeability of the silicon-manganese-copper is reduced.
Zn: zn is better than Si and Mn, and a small amount of Zn can avoid SiO generated by combining oxygen with Si and Mn in the melt 2 And MnO 2 Oxides, avoiding Si and Mn oxides remained in the melt. Zn can also reduce the liquid-solid interval of the silicon-manganese-copper, and avoid the loose production in the cast ingot, so the lower limit of the effective action content of Zn is not less than 0.01 percent, but the maximum Zn is not more than 1.2 percent, otherwise, the corrosion resistance of the alloy is poor.
Fe: at normal temperature, fe exists in the form of hard particles in Cu basically, which can lead to the increase of the hardness of the silicon-manganese-copper and reduce the malleability of the silicon-manganese-copper, so that the Fe content in the alloy is controlled below 0.10 percent, and the malleability of the silicon-manganese-copper is little affected.
Pb: pb is almost insoluble in the silicon-manganese-copper, and Pb is distributed in a free state at a crystal boundary, so that the crystal boundary presents cold brittleness, and a crack source is easy to generate at the crystal boundary in the cold heading deformation process of the silicon bronze; in addition, when Pb in the Si-Mn-Cu alloy reaches more than 0.007%, pb in the grain boundary is hot brittle during hot working, so that the hot working cracks are caused, and therefore, the Pb impurity in the Si-Mn-Cu alloy is required to be strictly controlled below 0.007%.
Preferably, the microstructure of the copper alloy has an α -phase as a matrix phase, and the area ratio of the MnSi phase is 0.2% or less.
Preferably, the average grain size of the copper alloy is 30-50 mu m, the number of grains with the grain size larger than 70 mu m is less than or equal to 3%, and the number of grains with the grain size smaller than 10 mu m is less than or equal to 5%. The average grain size of the copper alloy is 30-50 mu m, because the control requirement of the internal structure of the cold heading Si-Mn-Cu is different from that of Si-Mn-Cu for other purposes, the grain size is too small, grain boundaries for preventing sliding are increased, the number of dislocation plugs at the grain boundaries in the deformation process is increased, the yield strength is increased, the deformation resistance is increased, the cold heading forming becomes difficult, and cracking is easy to occur; the grain size is too large, and the surface of the product after cold heading is rough, so that obvious wrinkles are generated. The number of crystal grains with the grain size larger than 70 mu m is less than or equal to 3 percent, and the number of crystal grains with the grain size smaller than 10 mu m is less than or equal to 5 percent, because the deformation of the metal during cold heading occurs due to the sliding of the crystal grains and the deformation of the crystal grains, the uniformity of the grain size is good, the deformation can be uniformly dispersed to each crystal grain, the stress concentration caused by the deformation is small, and the possibility of cracking is also reduced.
Preferably, the twin area in the copper alloy structure is not more than 10% of the total area of the crystal grains, and the deformation twin area is not more than 20% of the total area of the twin. The twinning area ratio is not more than 10% of the total area of the crystal grains, because after twinning, the twinning boundary can play a hardening role, and the plasticity of the alloy is reduced. The area ratio of the deformation twin crystals is not more than 20% of the total area of the twin crystals, because the annealing twin crystals are isotropic, and the deformation twin crystals can generate different preferred orientations due to different external stresses, so that the deformation twin crystals are anisotropic, and cracks are not easy to generate in the cold heading deformation process of the annealing twin crystals relative to the deformation twin crystals.
The invention solves the second technical problem by adopting the technical proposal that: the preparation method of the copper alloy bar is characterized in that the process flow of the copper alloy comprises the following steps: smelting, casting, extruding, coiling, annealing, pickling, stretching a finished product and annealing at a low temperature; the low-temperature annealing process adopts reducing atmosphere protection, and the annealing temperature is as follows: 200-350 ℃, and the heat preservation time is as follows: cooling to below 60 ℃ for 2-6 h, and discharging.
Preferably, the smelting is carried out in the sequence of red copper, copper-silicon intermediate alloy, copper-manganese intermediate alloy and zinc. Si in the alloy can reduce the solubility of H (hydrogen) in the melt, mn can improve the solubility of H in the melt, zn is most active and is easy to combine with oxygen, so that the final addition can reduce the oxides of Si and Mn in the melt and improve the metallurgical quality of the melt.
Preferably, the casting temperature of the casting: 1220-1270 ℃, and drawing and casting speed: 30-70 mm/min, primary cooling water flow: 10-20 m 3 And/h, secondary cooling water flow rate: 0.1-3 m 3 /h, cooling water pressure: 0.01-0.06 MPa. Because Si seriously reduces the heat conduction property of copper, the solidification speed is low when the alloy is cast, and for the alloy with poor heat conduction, the alloy is ensured to have enough solidification time, the situation that the core part is still in a molten state after the solidification of the outer surface layer of an ingot is still caused when the cooling strength is high is avoided, and the stress is easy to generateForce cracking, therefore, the casting of the silicomanganese copper of the invention requires weak secondary cooling and low-speed casting. The drawing and casting speed is too slow, the primary and secondary cooling water flows are too large, the liquid-solid interface moves upwards into the crystallizer, the contact area between the solidified shell and the inner wall of the crystallizer is increased, the friction resistance is increased, and the surface quality of the cast ingot is poor; the drawing and casting speed is too high, the flow rate of the primary and secondary cooling water is too low, the distance that the liquid-solid interface moves downwards to the lower part of the outlet of the crystallizer is prolonged, the liquid cavity is deepened, and the thin solidified shell layer is melted and broken by the high-temperature liquid copper water at the center to leak copper.
Preferably, the extruded ingot heating temperature: 820-900 ℃, extrusion speed: 9-14 mm/s, extrusion ratio: 80-200. The extrusion ratio is lower than 80, and the dynamic recrystallization driving force is small because of low extrusion deformation degree, and the grains of the extrusion blank are coarse; however, the extrusion ratio is too high and exceeds 200, the strong extrusion deformation is caused, the deformation energy of the crystal lattice is high, the dynamic recrystallization driving force is large, the recrystallized grains are small and less than 20 mu m, the grain boundary is increased, the grain boundary is a place with irregular atomic arrangement, the energy is very high, the grain size of the finished product is difficult to be increased to 30-50 mu m through process adjustment, when the extrusion speed is low, the whole ingot can be extruded only by a longer time, the temperature drop of the ingot is fast, the deformation resistance of the tail end of the ingot is increased, the extrusion of the whole ingot can not be successfully completed, when the extrusion speed is too fast, the extrusion force is rapidly increased and exceeds the limit pressure of the extruder, so that the extrusion rod is broken, and the alloy is suitable for extrusion at the speed of 9-14 mm/s.
Preferably, the processing rate of the coil drawing is controlled to be 20-60%, and the processing rate of the finished product drawing is controlled to be 3-17%. If the disc drawing processing rate is lower than 20%, the cold deformation degree is low, the caused lattice distortion is small, the atom dislocation degree is low, deformation twin crystals are easy to generate, after annealing, part of deformation twin crystals disappear, and new annealing twin crystals are formed; with the increase of the cold deformation degree, after the disc drawing processing rate exceeds 60%, the structure of each part of the blank is fully deformed, the original crystal grains of the extrusion blank are completely crushed, the number of recrystallized nuclei is obviously increased, the recrystallized crystal grains are tiny, the deformation resistance is increased, the cold heading forming becomes difficult, and the cracking is easy to occur. Based on the control of the mechanical properties of the finished product, the processing rate of the finished product is lower than 3%, and as the deformation of the wire blank after being stretched by the die is too small, the deformation only occurs on the surface layer of the wire blank, so that the flow rate of the surface layer metal is higher than that of the central layer metal, and the surface of the finished product can be subjected to stupefied printing; after the working rate exceeds 17%, the plasticity of the alloy is poor due to the work hardening effect, and the cold heading is easy to crack.
Preferably, the annealing temperature is 520-600 ℃, the temperature is raised from normal temperature, and after the temperature reaches the set temperature, the heat preservation time is as follows: 120-300 min. The annealing temperature is increased, the stronger the atom diffusion capability is, the more easily the crystal boundary is migrated, and the faster the crystal grain grows. The annealing temperature of the silicon-manganese-copper alloy is lower than 520 ℃, and deformation twin crystals generated by tensile deformation are difficult to disappear on one hand; on the other hand, the grain size of the recrystallization is small, the average grain size is lower than 30 mu m, the cold heading deformation resistance is large, and cracks are easy to occur; after the annealing temperature exceeds 600 ℃, grains start to become coarse, the average grain size exceeds 50 mu m, wrinkles are easily formed on the surface of a product after cold heading, copper adhesion of a stamping die is easily caused, and the service life of the die is reduced. The heat preservation time is short and is lower than 120min, the recrystallization is insufficient, and the method is more prominent particularly under the condition of large charging quantity; the heat preservation time is long, after the heat preservation time exceeds 300min, the grains are extremely easy to be coarse, and the annealed wire blank is cleaned from surface oxide skin by acid washing.
Compared with the prior art, the invention has the advantages that: the contents of Si, mn and Zn in the copper alloy are controlled, the proportion of MnSi brittle phases is controlled, and the excellent cold heading performance and mechanical property and tensile strength of the material are obtained: 360-450 Mpa, yield strength: 310-400 MPa, area shrinkage Z: 40-60%, hardness HV: 100-150.
Detailed Description
The present invention is described in further detail below with reference to examples.
The invention provides 6 examples and 2 comparative examples, the specific compositions are shown in Table 1.
The preparation procedure of the examples is as follows:
1) Smelting: the ingredients are mixed according to the required components, and the feeding sequence is as follows: red copper, copper-silicon intermediate alloy, copper-manganese intermediate alloy and zinc, and the smelting temperature is 1200-1280 ℃.
2) Casting: casting temperature:1220-1270 ℃, and drawing and casting speed: 30-70 mm/min, primary cooling water flow: 10-20 m 3 And/h, secondary cooling water flow rate: 0.1-3 m 3 /h, cooling water pressure: 0.01-0.06 MPa, and ingot sawing specification: phi 180-260 mm 500-800 mm.
3) Extruding: ingot heating temperature: 820-900 ℃, extrusion speed: 9-14 mm/s, extrusion ratio: 80-200, extruding the extrusion blank from a die, and coiling the wire.
4) And (3) disc pulling: the processing rate of the disc drawing is 20-60%;
5) Annealing and acid washing: the annealing temperature is 520-600 ℃, the temperature is raised from normal temperature, and after the temperature reaches the set temperature, the heat preservation time is as follows: 120-300 min.
6) And (3) stretching a finished product: the bar is drawn, straightened, polished and sawed into a straight bar by combined drawing, the bar is drawn into a wire rod by an inverted wire drawing machine, and the processing rate is as follows: 3 to 17 percent.
7) And (3) low-temperature annealing: by reducing atmosphere H 2 Protection, annealing temperature: 200-350 ℃, and the heat preservation time is as follows: cooling to below 60 ℃ for 2-6 h, and discharging.
8) The finished product is checked, and key technological parameter control is shown in tables 2 and 3.
Comparative example 1 is a commercially available C65100 phi 10.5 wire.
Comparative example 2 is a commercially available C65100 phi 17.5 bar.
The following test was performed on the microstructures of the examples and comparative examples, and the results are shown in table 4.
Observing the grain size, the different grain proportion and the brittle phase distribution quantity under a scanning electron microscope;
the following performance tests were performed on 6 examples and 2 comparative examples, and the results are recorded in table 5.
Tensile strength, yield strength Rp 0.2 And area reduction: according to GB/T228.1-2021 section 1 Metal tensile test: room temperature test method.
Hardness HV: according to GB/T4340.1-2009 Vickers hardness test of Metal materials part 1: test methods.
Upsetting test: the sample is prepared into a sample original with the height ofCylindrical shape 1.5 times the original diameter, and then flattening in an oil press until a first visually observable crack appears on the sample surface, the degree of compression
(H 0 : original height of cylindrical sample, H k : the height of the sample when the 1 st macroscopic crack appears on the side during the flattening of the sample) is shown in Table 5, ε c The larger the value, the better the forgeability of the test specimen.
Torque test: the breaking torque of the bolt or screw was measured according to the method of GB/T3098.13-1996 "torque test of mechanical bolt and screw of fastener and breaking torque nominal diameter 1-10 mm", and recorded in Table 5.
TABLE 1 Components per wt% of inventive and comparative examples
| Numbering device | Si | Mn | Zn | Fe | Pb | Cu |
| Example 1 | 1.68 | 0.49 | 0.025 | 0.011 | 0.0027 | Allowance of |
| Example 2 | 1.76 | 0.42 | 0.082 | 0.035 | 0.0030 | Allowance of |
| Example 3 | 1.92 | 0.33 | 0.31 | 0.022 | 0.0056 | Allowance of |
| Example 4 | 1.15 | 0.78 | 0.58 | 0.086 | 0.0015 | Allowance of |
| Example 5 | 1.30 | 0.57 | 0.90 | 0.065 | 0.0040 | Allowance of |
| Example 6 | 1.55 | 0.69 | 1.14 | 0.050 | 0.0068 | Allowance of |
| Comparative example 1 | 1.71 | 0.47 | 0.029 | 0.012 | 0.0027 | Allowance of |
| Comparative example 2 | 1.80 | 0.54 | 0.0078 | 0.029 | 0.012 | Allowance of |
TABLE 2 Key process parameter control for embodiments of the invention
3 key Process parameter control of embodiments of the present invention
TABLE 4 microstructure of examples and comparative examples of the present invention
TABLE 5 Properties of examples and comparative examples of the invention
Claims (10)
1. A copper alloy bar, characterized in that: the copper alloy comprises the following components in percentage by mass: 1.0 to 2.0wt percent, mn:0.3 to 0.8 weight percent of Zn:0.01 to 1.2 weight percent, less than or equal to 0.10 weight percent of Fe, less than or equal to 0.007 weight percent of Pb, and the balance of Cu and unavoidable impurities.
2. The copper alloy bar according to claim 1, wherein: the microstructure of the copper alloy takes an alpha phase as a matrix phase, and the area ratio of the MnSi phase is below 0.2 percent.
3. The copper alloy bar according to claim 1, wherein: the average grain size of the copper alloy is 30-50 mu m, the number of grains with the grain size larger than 70 mu m is less than or equal to 3%, and the number of grains with the grain size smaller than 10 mu m is less than or equal to 5%.
4. The copper alloy bar according to claim 1, wherein: the twin area ratio in the copper alloy structure is not more than 10% of the total area of the crystal grains, and the deformation twin area ratio is not more than 20% of the total area of the twin crystals.
5. A method for producing a copper alloy bar according to any one of claims 1 to 4, wherein the process flow of the copper alloy comprises: smelting, casting, extruding, coiling, annealing, pickling, stretching a finished product and annealing at a low temperature; the low-temperature annealing process adopts reducing atmosphere protection, and the annealing temperature is as follows: 200-350 ℃, and the heat preservation time is as follows: cooling to below 60 ℃ for 2-6 h, and discharging.
6. The method for producing a copper alloy bar according to claim 5, wherein: the smelting feeding sequence is red copper, copper-silicon intermediate alloy, copper-manganese intermediate alloy and zinc.
7. The method of producing copper alloy bar according to claim 5, wherein the casting temperature of the casting is: 1220-1270 ℃, and drawing and casting speed: 30-70 mm/min, primary cooling water flow: 10-20 m 3 And/h, secondary cooling water flow rate: 0.1-3 m 3 /h, cooling water pressure: 0.01-0.06 MPa.
8. The method for producing a copper alloy bar according to claim 5, wherein: the extruded ingot heating temperature: 820-900 ℃, extrusion speed: 9-14 mm/s, extrusion ratio: 80-200.
9. The method for producing a copper alloy bar according to claim 5, wherein: the processing rate of the coil drawing is controlled to be 20-60%, and the processing rate of the finished product drawing is controlled to be 3-17%.
10. The method for producing a copper alloy bar according to claim 5, wherein: the annealing temperature is 520-600 ℃, the temperature is raised from normal temperature, and after the temperature reaches the set temperature, the heat preservation time is as follows: 120-300 min.
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| CN117305649A (en) * | 2023-11-29 | 2023-12-29 | 中铝科学技术研究院有限公司 | Copper alloy material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117305649A (en) * | 2023-11-29 | 2023-12-29 | 中铝科学技术研究院有限公司 | Copper alloy material and preparation method thereof |
| CN117305649B (en) * | 2023-11-29 | 2024-02-27 | 中铝科学技术研究院有限公司 | Copper alloy material and preparation method thereof |
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