CN105177344A - Cu-Fe alloy wire and preparing method thereof - Google Patents
Cu-Fe alloy wire and preparing method thereof Download PDFInfo
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- CN105177344A CN105177344A CN201510459015.9A CN201510459015A CN105177344A CN 105177344 A CN105177344 A CN 105177344A CN 201510459015 A CN201510459015 A CN 201510459015A CN 105177344 A CN105177344 A CN 105177344A
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- 239000000956 alloy Substances 0.000 title claims abstract description 100
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 98
- 238000000034 method Methods 0.000 title claims abstract description 36
- 229910017827 Cu—Fe Inorganic materials 0.000 title abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 85
- 238000005266 casting Methods 0.000 claims abstract description 43
- 239000010949 copper Substances 0.000 claims abstract description 42
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 238000002844 melting Methods 0.000 claims abstract description 17
- 230000008018 melting Effects 0.000 claims abstract description 17
- 238000005242 forging Methods 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 8
- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 claims description 63
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 62
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 49
- 239000000203 mixture Substances 0.000 claims description 48
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 38
- 238000000137 annealing Methods 0.000 claims description 37
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 26
- 229910052802 copper Inorganic materials 0.000 claims description 22
- 238000002360 preparation method Methods 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 19
- 238000007670 refining Methods 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 16
- 229910052742 iron Inorganic materials 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 238000005554 pickling Methods 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000005098 hot rolling Methods 0.000 claims description 9
- 238000005096 rolling process Methods 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 230000006698 induction Effects 0.000 claims description 6
- 238000003801 milling Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 238000005482 strain hardening Methods 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- 102000002151 Microfilament Proteins Human genes 0.000 claims description 5
- 108010040897 Microfilament Proteins Proteins 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000007499 fusion processing Methods 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- 210000003632 microfilament Anatomy 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 230000009286 beneficial effect Effects 0.000 claims description 4
- 238000010622 cold drawing Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005204 segregation Methods 0.000 abstract description 11
- 239000006104 solid solution Substances 0.000 abstract description 5
- 229910002549 Fe–Cu Inorganic materials 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract 2
- 229910021652 non-ferrous alloy Inorganic materials 0.000 abstract 1
- 238000013461 design Methods 0.000 description 6
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- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 description 2
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- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910000846 In alloy Inorganic materials 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
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- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a Cu-Fe alloy wire and a preparing method thereof, and belongs to the technical field of non-ferrous alloy. The preparing method includes the steps that an intermediate alloy with even ingredients is used as parent materials, wherein the ingredients of the parent materials comprise 45% to 60% of Fe, 0.20% to 0.35% of Ni, not smaller than 0% of RE and the balance Cu; and then cathode copper and the intermediate alloy parent materials serve as raw materials, and a casting-state alloy ingot is obtained through vacuum melting and further machined into the Cu-Fe alloy wire, wherein the wire is prepared from 8.0% to 13.0% of Fe and the balance Cu and unavoidable impurities. When the prepared Cu-Fe alloy is in the casting state and the forging state, Fe-Cu solid solution is good, Fe elements are evenly distributed without segregation, and good machinability is achieved. The diameter phi of the further-machined finished wire ranges from 0.05 mm to 0.1 mm, the tensile strength of the finished wire is larger than or equal to 440 N/mm<2>, and the elongation of the finished wire is larger than or equal to 10%. The Cu-Fe alloy further has the excellent electromagnetic shielding effect.
Description
Technical field
The present invention relates to non-ferrous metal alloy technical field, be specifically related to a kind of copper-iron alloy silk material and preparation method thereof.
Background technology
Metallic substance has a wide range of applications scope, but it is few to the report of copper-iron alloy both at home and abroad, the Some features of Cu-Fe alloy can be predicted: (1) fusing point should higher than Cu lower than Fe by the knowledge of Metal Material Science, if be used as vacuum electric contact material to carry out alternative Cu alloy, then can improve its arc ablation resistance ability; (2) fine copper and pure iron all have good ductility, and therefore Cu-Fe alloy should also possess this performance; (3) cost of Cu material can be reduced with Fe Substitute For Partial Cu; (4) there is effectiveness.
Figure 1 shows that Cu-Fe binary alloy phase diagram, elementary solid solution theory is thought: atomic radius and the electrochemical properties of two kinds of elements are more similar, then more easily form sosoloid, but Fe-Cu system is exception, their atomic radius is almost equal, chemical affinity or electronegativity and other chemical property all very similar, but solubleness below fusing point is very little, only has 2.5% unlimited solid solution from metal phase diagram Fe in Cu.Along with the increase of Fe content, Cu-Fe alloy very easily forms the serious tissue of segregation in process of setting, namely the microstructure of alloy is mainly present in Cu matrix with nascent rich Fe dendritic form, Fe content is higher, α-Fe dendrite is thicker, because this characteristic of this alloy, greatly hinder production and the application of Cu-Fe alloy.
Alloy is in smelting process, and some elements add in the mode of master alloy.Utilize the mode that master alloy adds, the melting loss of alloying element can be reduced on the one hand, thus realize the accurate control of alloy chemical composition; On the other hand, while reduction smelting temperature, also shorten smelting time, be conducive to the life-span of improving melting equipment, and save energy.Separately there are some researches show, the factor such as composition, structure of master alloy also can produce material impact to the performance of prepared alloy.
Therefore, by adopting specific master alloy masterbatch in production Cu-Fe binary alloy process, to changing the solid solubility of prepared Cu-Fe binary alloy, optimizing its performance and expansive approach scope, becoming a kind of new Research Thinking.
Summary of the invention
The object of the present invention is to provide a kind of copper-iron alloy silk material and preparation method thereof, adopt the master alloy masterbatch of specific composition, in conjunction with specific technique, when the CuFe alloy casting state of preparation and forging state Fe and Cu solid solution good, Fe Elemental redistribution evenly, not segregation, there is good processibility.After being processed into a material further, there is excellent physical strength and unit elongation.
For achieving the above object, the technical solution adopted in the present invention is as follows:
A kind of copper-iron alloy silk material, weight percentage, this copper-iron alloy silk material chemical composition is: Fe is 8.0 ~ 13.0%, and surplus is Cu and inevitable impurity; The preferred chemical composition of this material is: Fe is 8.5 ~ 11.5%, and surplus is Cu and inevitable impurity; In its chemical composition: C≤0.03%, S≤0.01%, P≤0.01%.
This copper-iron alloy silk material final dimension tolerance grade is high, its diameter Ф 0.05 ~ 0.1mm, tensile strength>=440N/mm
2; Unit elongation>=10%; This material also has excellent effectiveness.
Described copper-iron alloy silk material is prepared in accordance with the following steps:
(1) raw material prepares and batching
By cathode copper and master alloy masterbatch surface successively through pickling, washing and drying and processing, guarantee that all raw materials clean, then in required ratio correct amount; Described pickling refers to: cathode copper adopts the sulfuric acid cleaned of concentration 30vol.%, and technically pure iron adopts the hydrochloric acid cleaning of concentration 30vol.%, and electrolytic nickel adopts the nitric acid cleaning of concentration 40vol.%; Described master alloy masterbatch is strip-like copper iron master alloy, weight percentage, and this master alloy chemistries is: Fe45 ~ 60%, Ni0.20 ~ 0.35%, and RE>0, Cu are surplus; Wherein: RE is lanthanide-indueed shift; This master alloy chemistries is preferably: Fe48 ~ 52%, Ni0.20 ~ 0.30%, La<0.02%, Ce<0.04%, Cu are surplus.
Described master alloy masterbatch is as the source of ferro element and part copper element, and described cathode copper is as the source of remainder copper; The preparation of described master alloy masterbatch comprises following (a)-(e) step:
A () raw material prepares: material choice cathode copper, technically pure iron and electrolytic nickel, successively through pickling, washing and drying and processing before raw material uses, to ensure that all raw materials clean; Described pickling refers to: cathode copper adopts the sulfuric acid cleaned of concentration 30vol.%, and technically pure iron adopts the hydrochloric acid cleaning of concentration 30vol.%, and electrolytic nickel adopts the nitric acid cleaning of concentration 40vol.%.Weight percentage, in raw material, each element percentage composition is: Fe45 ~ 60%, Ni0.20 ~ 0.35%, RE0.05 ~ 0.1%, and Cu is surplus; Wherein: RE is lanthanide-indueed shift; In raw material, each element percentage composition is preferably: Fe48 ~ 52%, Ni0.25 ~ 0.30%, La0.02 ~ 0.025%, Ce0.04 ~ 0.045%, Cu is surplus.
(b) vacuum induction melting:
According to element ratio batching each in raw material, then carry out vacuum induction melting, fusion process is specially: cathode copper, technically pure iron are loaded in crucible by proportioning, vacuumizes the fusing of rear power transmission, 1300 ~ 1550 DEG C of refining 20-30min in stove; To add after Ni and CaF refining 20-30min again; Finally add La and Ce, after 40 ~ 50 seconds, start charged casting; In fusion process, vacuum tightness≤8Pa, refining temperature controls at 1300 ~ 1550 DEG C; Casting obtains alloy cast ingot;
(c) ingot mill surface:
Remove the thick top layer of ingot casting surface 2-3mm with vertical milling machine, its objective is and the part that removing foreign matter content is high be beneficial to following process simultaneously;
(d) hot rolling cogging:
Rolling temperature 1000 ~ 1015 DEG C, be incubated 90 ~ 100 minutes, a rolling 6-7 passage, is hot-rolled down to 10 ~ 12mm, is then cold working to 5 ~ 6mm;
E the sheet material after () hot rolling cogging cleans, cleaning process is: the oxide skin first washing away plate surface with the sulfuric acid of concentration 30vol.%, then rinses well with the residual acid of clear water by surface; The strip-like copper iron intermediate alloy material of required specification is cut into after cleaning.
(2) vacuum melting
Load in crucible by cathode copper, master alloy masterbatch, refining 20-30min after power transmission fusing, then adds CaF, again refining 20-30min, then starts charged casting be filled with rare gas element Ar in stove after, namely obtain described copper-iron alloy ingot casting; In Vacuum Melting: refining temperature controls at 1200 ~ 1500 DEG C; Vacuum tightness≤2Pa; In prepared copper-iron alloy (ingot casting) Fe Elemental redistribution evenly, not segregation.
(3) alloy cast ingot car light:
By copper-iron alloy ingot casting surface car light.
(4) forge hot and forging rear car light:
Open die forging on 750Kg air hammer, heating by electric cooker temperature 850 ~ 875 DEG C, was incubated after 60 ~ 100 minutes, carried out two upsettings two and pulled out rear forging to Ф 42 ~ 50mm bar; Then car light is to Ф 40 ~ 45mm bar.
(5) hot rolling:
Heating by electric cooker temperature 845 ~ 855 DEG C, was incubated after 70 ~ 80 minutes, and rolling on Ф 250 × 350 pass milling train (stalk pressure) is to Ф 10 ~ 15mm bar.
(6) cold working and pilot process vacuum annealing:
Step (3) gained Ф 10 ~ 15mm bar is carried out successively dish circle, annealing and cold drawing process, repeat this process 3 ~ 5 times, after obtaining Ф 1.2 ~ 2.0mm silk material, carry out anneal again, annealing temperature 550 ~ 730 DEG C.
(7) microfilament drawing:
After vacuum annealing, soft state Ф 1.2 ~ 2.0mm silk material carries out repeatedly drawing process, and obtain diameter Ф 0.05 ~ 0.1mm copper-iron alloy silk material, detailed process is:
Ф 1.2 ~ 2.0mm silk material is drawn to Ф 0.8 ~ 1.2mm, every time working modulus 15%; Continuous hydrogen annealing furnace anneal: furnace temperature 740 DEG C, draws and gets between (machine) speed 70 ~ 80, silk material unit elongation >=25% after annealing; Ф 0.8 ~ 1.2mm silk material is drawn to Ф 0.3 ~ 0.5mm, every time working modulus 15%; Continuous hydrogen annealing furnace anneal: furnace temperature 740 DEG C, draws and gets between (machine) speed 70 ~ 80, silk material unit elongation >=25% after annealing; Ф 0.3 ~ 0.5mm silk material is drawn to Ф 0.15 ~ 0.2mm, every time working modulus 13%; Continuous hydrogen annealing furnace anneal: furnace temperature 740 DEG C, draws and gets between (machine) speed 70 ~ 80, silk material unit elongation >=20% after annealing; Ф 0.15 ~ 0.2mm silk material is drawn to Ф 0.05 ~ 0.1mm, every time working modulus 12%; Continuous hydrogen annealing furnace anneal: furnace temperature 740 DEG C, draws and gets between (machine) speed 70 ~ 80, silk material unit elongation >=10% after annealing.
Advantage of the present invention and beneficial effect as follows:
1, for producing high-strength high-tractility Cu-Fe alloy wire, CuFe master alloy masterbatch is adopted.Masterbatch ingot casting upper, middle and lower uniform composition, Fe Elemental redistribution evenly, not segregation; Adopt this masterbatch and coordinate the preparation technology of feature can reduce the fusing point of high ductibility Cu-Fe alloy, reducing the oxidation of Fe and scaling loss, and by secondary vacuum remelting, making being evenly distributed of Fe in high ductibility Cu-Fe alloy, not segregation.
2, for making the CuFe master alloy masterbatch of uniform composition, add rare-earth elements La (lanthanum) and the Ce (cerium) of specific proportioning, lanthanide-indueed shift has purification, impurity elimination effect, and act synergistically with other elements under specific process conditions, thus the crystal grain of abundant refinement Cu-Fe As-cast Microstructure, reduce the generation of segregation.
3, prepared high-strength high ductibility copper-iron alloy silk material chemical composition stability, Fe element being evenly distributed in the alloy, not segregation.
4, prepared high-strength, high ductibility copper-iron alloy silk material final dimension tolerance grade is high, microfilament diameter Ф can reach 0.05 ~ 0.1mm; Good mechanical performance, silk material tensile strength>=440N/mm
2, unit elongation>=10%; Copper-iron alloy silk material also has excellent effectiveness, and stable performance, cost performance is high, has very wide market outlook.
Accompanying drawing explanation
Fig. 1 is CuFe binary alloy phase diagram.
Fig. 2 is CuFe master alloy metallographic microscopic appearance figure prepared by embodiment 1.
Fig. 3 is metallographic microscopic appearance figure under the CuFe alloy casting state of embodiment 1 preparation.
Fig. 4 is metallographic microscopic appearance figure under the CuFe alloy forging state of embodiment 1 preparation.
Fig. 5 is that the CuFe alloy tensile of embodiment 1 preparation is to metallographic microscopic appearance figure during Ф 8.4mm.
Embodiment
Below in conjunction with drawings and Examples in detail the present invention is described in detail.
The masterbatch that the present invention is prepared using copper iron master alloy as Cu-Fe alloy wire, the preparation process of this master alloy is: raw material preparation → batching → vacuum melting → masterbatch component analysis → ingot mill surface → hot rolling → pickling, washing → shearing; Following examples are prepared in accordance with the following steps:
(1) raw material prepares
In raw material, each element proportioning is (wt.%): Fe45 ~ 60%, Ni0.20 ~ 0.35%, RE0.05 ~ 0.1%, and Cu is surplus; Wherein: RE is lanthanide-indueed shift; Preferred proportioning raw materials is: Fe48 ~ 52%, Ni0.25 ~ 0.30%, La0.02 ~ 0.025%, Ce0.04 ~ 0.045%, and Cu is surplus.
(2) prepare burden: weigh by element proportion speed each in raw material.By cathode copper, technically pure iron, electrolytic nickel surface through pickling, washing, drying and processing, guarantee that all raw materials clean.Acid cleaning process is: cathode copper adopts the sulfuric acid cleaned of concentration 30vol.%, and technically pure iron adopts the hydrochloric acid cleaning of concentration 30vol.%, and electrolytic nickel adopts the nitric acid cleaning of concentration 40vol.%.
(3) vacuum melting
Load in crucible by cathode copper, technically pure iron, electrolytic nickel and CaF load in loading hopper, and lanthanide-indueed shift loads in feeder; Banking vacuumizes, vacuum tightness≤8Pa (namely 6 × 10
-2mmHg); Refining 25min after power transmission fusing, then Ni (electrolytic nickel) and CaF refining 25min again, finally adds La and Ce, starts charged casting after 45 seconds, obtains alloy cast ingot.The vacuum induction furnace model that vacuum melting adopts: ZG-0.025; Refining temperature controls at 1300 ~ 1550 DEG C.
(4) masterbatch component analysis
Adopt ammonium bifluoride to cover Fe, then detect the content of the upper and lower Cu of masterbatch ingot casting with chemistry titration, precisely determine that in masterbatch, the production of Cu, Fe composition to next step CuFe system alloy is very important.
(5) ingot mill surface
Remove the high part of ingot surface foreign matter content (removing 2mm thickness top layer) with vertical milling machine, be beneficial to following process simultaneously.
(6) hot rolling cogging
Heating by electric cooker: temperature 1010 DEG C, is incubated 90 ~ 100 minutes, is hot-rolled down to 12mm, is cold working to 5 ~ 6mm.Equipment used: Φ 250 × 450 2 roller hot rolls.
(7) pickling, washing: wash away the oxide skin on masterbatch surface with sulfuric acid (30vol.%) and rinse well with the residual acid of clear water by surface.
(8) shear: masterbatch plate shears is cut into required specification strip master alloy stand-by.
Using the masterbatch of the strip master alloy of above-mentioned preparation as the high-strength high ductibility copper-iron alloy silk material of required preparation, the process for the preparation of high-strength high ductibility copper-iron alloy silk material is as follows:
(1) raw material prepares and batching
By cathode copper and strip master alloy masterbatch surface successively through pickling, washing and drying and processing, guarantee that all raw materials clean, described pickling refers to: cathode copper adopts the sulfuric acid cleaned of concentration 30vol.%, technically pure iron adopts the hydrochloric acid cleaning of concentration 30vol.%, and electrolytic nickel adopts the nitric acid cleaning of concentration 40vol.%;
Copper-iron alloy silk material chemical composition to be prepared is (wt.%): Fe is 8.0 ~ 13.0%, and surplus is Cu and inevitable impurity; Preferred chemical composition is (wt.%): Fe is 8.5 ~ 11.5%, and surplus is Cu and inevitable impurity; In alloy: C≤0.03%, S≤0.01%, P≤0.01%.
By the raw material after cleaning by required alloy proportion correct amount; Described master alloy masterbatch is as required source of preparing ferro element and part copper element in high ductibility copper-iron alloy, and described cathode copper is as the source of remainder copper;
(2) vacuum melting
In Vacuum Melting: refining temperature controls at 1200 ~ 1500 DEG C; Vacuum tightness≤2Pa (namely 1.5 × 10
-2mmHg); Vacuum melting equipment used: ZG-0.025 vacuum induction furnace, fusion process is:
Load in crucible by cathode copper, strip master alloy masterbatch, CaF loads in loading hopper, and banking vacuumizes, refining 20min after power transmission fusing, then adds CaF, again refining 20min, start charged casting after being filled with rare gas element Ar again in stove, namely obtain copper-iron alloy ingot casting.
(3) composition of the copper-iron alloy ingot casting upper, middle and lower Fe prepared by using plasma Atomic Emission SpectrometerAES (ICP-1000) detection.
(4) alloy cast ingot car light:
By copper-iron alloy ingot casting qualified for composition at CA6140 lathe upper surface car light.
(5) forge hot and forging rear car light:
Open die forging on 750Kg air hammer, heating by electric cooker temperature 860 DEG C, was incubated after 90 minutes, carried out two upsettings two and pulled out rear forging to Ф 45mm bar; Then car light is to Ф 42mm bar.
(6) hot rolling:
Heating by electric cooker temperature 850 DEG C, was incubated after 70 minutes, and rolling on Ф 250 × 350 pass milling train (stalk pressure) is to Ф 13mm bar.
(7) cold working and pilot process vacuum annealing:
Step (3) gained Ф 13mm bar is carried out successively dish circle, annealing (annealing temperature 550 ~ 730 DEG C) and cold drawing process, repeat this process 4 times, after obtaining Ф 1.5mm silk material, carry out the anneal under 550 ~ 730 DEG C of conditions again; Equipment used LS-20 ton chain drawbench in this step; 1/560,1/350,1/250 upright stretching machine; Ф 800 pit type annealing furnace etc.
(8) microfilament drawing:
After vacuum annealing, soft state Ф 1.5mm silk material carries out multi pass drawing process, and every time working modulus 15%, is drawn to Ф 0.9mm; Continuous annealing furnace anneal (hydrogen): furnace temperature 740 DEG C, draws and gets (machine) speed 80, silk material unit elongation >=25% after annealing; Ф 0.9mm silk material is carried out multi pass drawing process, and every time working modulus 15%, is drawn to Ф 0.4mm; Continuous annealing furnace anneal (hydrogen): furnace temperature 740 DEG C, draws and gets (machine) speed 70, silk material unit elongation >=25% after annealing; Ф 0.4mm silk material is drawn to Ф 0.18mm, every time working modulus 13%; Continuous hydrogen annealing furnace anneal: furnace temperature 740 DEG C, draws and gets (machine) speed 70, silk material unit elongation >=20% after annealing; Ф 0.18mm silk material is drawn to Ф 0.06mm, every time working modulus 12%; Continuous hydrogen annealing furnace anneal: furnace temperature 740 DEG C, draws and gets (machine) speed 70, silk material unit elongation >=10% after annealing.
Embodiment 1
1, the present embodiment prepares the concrete consumption of each raw material of copper iron master alloy masterbatch is (wt.%): Fe=48%; Ni=0.25%; La=0.02%; Ce=0.04%; Cu=51.69%; Gained master alloy masterbatch (1#) composition is in table 1, and this master alloy metallographic microscopic appearance figure is as Fig. 2, and as can be seen from Fig. 2 and table 1 data, copper iron master alloy chemistries prepared by the present invention is stablized, ingot casting upper, middle and lower uniform composition; Fe element is evenly distributed in master alloy, not segregation.
2, prepare high-strength high ductibility CuFe alloy, chemical composition design is (wt.%): Fe=8.8%, Cu=91.2%.Prepared copper-iron alloy ingot casting composition is as shown in table 2, and ingot chemistry is stablized, ingot casting upper, middle and lower uniform composition; Under as-cast condition, metallographic microscopic appearance figure as shown in Figure 3, can find out, Cu, Fe solid solution is good, still has the rich Fe of part unbound state to exist.As shown in Figure 4, rich Fe free under as cast condition obtains partial crushing through heating and forging to the metallographic microscopic appearance of ingot casting after forging.
3, CuFe alloy bar material is processed into a material, metallographic microscopic appearance when being stretched to Ф 8.4mm silk material is as Fig. 5, and as can be seen from the figure, through repeatedly heating, thermal treatment and after repeatedly obstructing pressure, stretch process, the distribution of Fe is more even, refinement.Finally be prepared into Ф 0.06mm silk material, after tested, this Ф 0.06mm silk material tensile strength 440N/mm
2; Unit elongation is 12.5%; This copper-iron alloy also has excellent effectiveness.
Embodiment 2
1, the present embodiment prepares copper iron master alloy masterbatch process with embodiment 1.
2, prepare high-strength high ductibility CuFe alloy, chemical composition design is (wt.%): Fe=9.0%, Cu=91.0%.Prepared copper-iron alloy ingot casting composition is as shown in table 2, and ingot chemistry is stablized, ingot casting upper, middle and lower uniform composition;
3, CuFe alloy cast ingot is processed into Ф 0.06mm silk material, after tested, this Ф 0.06mm silk material tensile strength 443N/mm
2; Unit elongation is 12%; This copper-iron alloy also has excellent effectiveness.
Embodiment 3
1, the present embodiment prepares copper iron master alloy masterbatch process with embodiment 1.
2, prepare high-strength high ductibility CuFe alloy, chemical composition design is (wt.%): Fe=9.5%, Cu=90.5%.Prepared copper-iron alloy ingot casting composition is as shown in table 2, and ingot chemistry is stablized, ingot casting upper, middle and lower uniform composition;
3, CuFe alloy cast ingot is processed into Ф 0.06mm silk material, after tested, this Ф 0.06mm silk material tensile strength 445N/mm
2; Unit elongation is 11.2%; This copper-iron alloy also has excellent effectiveness.
Embodiment 4
1, the present embodiment prepares copper iron master alloy masterbatch process with embodiment 1.
2, prepare high-strength high ductibility CuFe alloy, chemical composition design is (wt.%): Fe=10.2%, Cu=89.8%.Prepared copper-iron alloy ingot casting composition is as shown in table 2, and ingot chemistry is stablized, ingot casting upper, middle and lower uniform composition;
3, CuFe alloy cast ingot is processed into Ф 0.06mm silk material, after tested, this Ф 0.06mm silk material tensile strength 448N/mm
2; Unit elongation is 11%; This copper-iron alloy also has excellent effectiveness.
Embodiment 5
1, the present embodiment prepares the concrete consumption of each raw material of copper iron master alloy masterbatch is (wt.%): Fe=49%; Ni=0.26%; La=0.02%; Ce=0.04%; Cu=51.68%; Gained master alloy masterbatch (2#) composition is in table 1, and as can be seen from table 1 data, copper iron master alloy chemistries prepared by the present invention is stablized, ingot casting upper, middle and lower uniform composition; Fe element is evenly distributed in master alloy, not segregation.
2, prepare high-strength high ductibility CuFe alloy, chemical composition design is (wt.%): Fe=10.8%, Cu=89.2%.Prepared copper-iron alloy ingot casting composition is as shown in table 2, and ingot chemistry is stablized, ingot casting upper, middle and lower uniform composition;
3, CuFe alloy cast ingot is processed into Ф 0.06mm silk material, after tested, this Ф 0.06mm silk material tensile strength 452N/mm
2; Unit elongation is 10.3%; This copper-iron alloy also has excellent effectiveness.
Embodiment 6
1, the present embodiment prepares the concrete consumption of each raw material of copper iron master alloy masterbatch is (wt.%): Fe=50%; Ni=0.27%; La=0.02%; Ce=0.04%; Cu=49.67%; Gained master alloy masterbatch (3#) composition is in table 1, and as can be seen from table 1 data, copper iron master alloy chemistries prepared by the present invention is stablized, ingot casting upper, middle and lower uniform composition; Fe element is evenly distributed in master alloy, not segregation.
2, prepare high-strength high ductibility CuFe alloy, chemical composition design is (wt.%): Fe=11.2%, Cu=88.8%.Prepared copper-iron alloy ingot casting composition is as shown in table 2, and ingot chemistry is stablized, ingot casting upper, middle and lower uniform composition;
3, CuFe alloy cast ingot is processed into Ф 0.06mm silk material, after tested, this Ф 0.06mm silk material tensile strength 455N/mm
2; Unit elongation is 10%; This copper-iron alloy also has excellent effectiveness.
CuFe master alloy masterbatch (ingot casting) chemical composition measured value (analytical procedure: cover Fe with ammonium bifluoride, then volumetry surveys Cu content, surveys other constituent contents in conjunction with other elemental analysis method) as shown in table 1 in above-described embodiment.Prepared copper-iron alloy ingot chemistry measured value is as shown in table 2, the composition of the ingot casting upper, middle and lower Fe prepared by using plasma Atomic Emission SpectrometerAES (ICP-1000) detects.
Table 1CuFe master alloy masterbatch (ingot casting) chemical composition (wt.%)
Table 2CuFe alloy (ingot casting) chemical composition measured value (wt.%)
Claims (10)
1. a copper-iron alloy silk material, is characterized in that: weight percentage, and this material chemical composition is: Fe is 8.0 ~ 13.0%, and surplus is Cu and inevitable impurity.
2. copper-iron alloy silk material according to claim 1, is characterized in that: weight percentage, in this alloy composition: Fe is 8.5 ~ 11.5%, and surplus is Cu and inevitable impurity.
3. copper-iron alloy silk material according to claim 1 and 2, is characterized in that: weight percentage, in this alloy composition: C≤0.03%, and S≤0.01%, P≤0.01%.
4. copper-iron alloy silk material according to claim 1 and 2, is characterized in that: this material diameter Ф 0.05 ~ 0.1mm, tensile strength>=440N/mm
2, unit elongation>=10%; This copper-iron alloy silk material has effectiveness.
5. the preparation method of copper-iron alloy silk material according to claim 1 and 2, is characterized in that: the method comprises the steps:
(1) raw material prepares and batching:
By cathode copper and master alloy masterbatch surface successively through pickling, washing and drying and processing, guarantee that all raw materials clean, then in required ratio correct amount;
(2) vacuum melting:
Load in crucible by cathode copper, master alloy masterbatch, refining 20-30min after power transmission fusing, then adds CaF, again refining 20-30min, then starts charged casting be filled with rare gas element Ar in stove after, namely obtains copper-iron alloy ingot casting; In Vacuum Melting: refining temperature controls at 1200 ~ 1500 DEG C, vacuum tightness≤2Pa;
(3) alloy cast ingot car light:
To be got on the bus light at lathe in copper-iron alloy ingot casting surface;
(4) forge hot and forging rear car light:
Open die forging on 750Kg air hammer, heating by electric cooker temperature 850 ~ 875 DEG C, was incubated after 60 ~ 100 minutes, carried out two upsettings two and pulled out rear forging to Ф 42 ~ 50mm bar; Then car light is to Ф 40 ~ 45mm bar;
(5) hot rolling:
Heating by electric cooker temperature 845 ~ 855 DEG C, was incubated after 70 ~ 80 minutes, and Ф 250 × 350 pass milling train is rolling to Ф 10 ~ 15mm bar;
(6) cold working and pilot process vacuum annealing:
Step (3) gained Ф 10 ~ 15mm bar is carried out successively dish circle, annealing and cold drawing process, repeat this process 3 ~ 5 times, after obtaining Ф 1.2 ~ 2.0mm silk material, carry out anneal again, annealing temperature 550 ~ 730 DEG C;
(7) microfilament drawing:
After vacuum annealing, soft state Ф 1.2 ~ 2.0mm silk material carries out repeatedly drawing process, obtains diameter Ф 0.05 ~ 0.1mm copper-iron alloy silk material.
6. the preparation method of copper-iron alloy silk material according to claim 5, it is characterized in that: in step (1), described master alloy masterbatch is strip-like copper iron master alloy, weight percentage, this master alloy chemistries is: Fe45 ~ 60%, Ni0.20 ~ 0.35%, RE>0, Cu are surplus.
7. the preparation method of copper-iron alloy silk material according to claim 6, is characterized in that: in step (1), and described master alloy masterbatch is as the source of ferro element and part copper element, and described cathode copper is as the source of remainder copper; The preparation of described master alloy masterbatch comprises the steps:
A () raw material prepares: weight percentage, and in raw material, each element percentage composition is: Fe45 ~ 60%, Ni0.20 ~ 0.35%, RE0.05 ~ 0.1%, and Cu is surplus; Wherein: RE is lanthanide-indueed shift;
(b) vacuum induction melting:
According to element ratio batching each in raw material, then carry out vacuum induction melting, in fusion process, vacuum tightness≤8Pa, refining temperature controls at 1300 ~ 1550 DEG C; Casting obtains alloy cast ingot;
(c) ingot mill surface:
Remove the thick top layer of ingot casting surface 2-3mm with vertical milling machine, its objective is and the part that removing foreign matter content is high be beneficial to following process simultaneously;
(d) hot rolling cogging:
Rolling temperature 1000 ~ 1015 DEG C, be incubated 90 ~ 100 minutes, a rolling 6-7 passage, is hot-rolled down to 10 ~ 12mm, is then cold working to 5 ~ 6mm;
E the sheet material after () hot rolling cogging cleans, cleaning process is: the oxide skin first washing away plate surface with the sulfuric acid of concentration 30vol.%, then rinses well with the residual acid of clear water by surface; The strip-like copper iron intermediate alloy material of required specification is cut into after cleaning.
8. the preparation method of copper-iron alloy silk material according to claim 7, it is characterized in that: in step (b), fusion process is specially: cathode copper, technically pure iron are loaded in crucible by proportioning, the fusing of rear power transmission is vacuumized, 1300 ~ 1550 DEG C of refining 20-30min in stove; To add after Ni and CaF refining 20-30min again; Finally add La and Ce, start charged casting after 40 ~ 50 seconds and obtain alloy cast ingot.
9. the preparation method of copper-iron alloy silk material according to claim 8, is characterized in that: in raw material cathode copper, technically pure iron and electrolytic nickel surface use before successively through pickling, washing and drying and processing, with ensure all raw materials clean; Described pickling refers to: cathode copper adopts the sulfuric acid cleaned of concentration 30vol.%, and technically pure iron adopts the hydrochloric acid cleaning of concentration 30vol.%, and electrolytic nickel adopts the nitric acid cleaning of concentration 40vol.%.
10. the preparation method of copper-iron alloy silk material according to claim 5, is characterized in that: in step (7), microfilament drawing process is specific as follows:
Ф 1.2 ~ 2.0mm silk material is drawn to Ф 0.8 ~ 1.2mm, every time working modulus 15%; Continuous hydrogen annealing furnace anneal: furnace temperature 740 DEG C, draws between the speed of getting 70 ~ 80, silk material unit elongation >=25% after annealing; Ф 0.8 ~ 1.2mm silk material is drawn to Ф 0.3 ~ 0.5mm, every time working modulus 15%; Continuous hydrogen annealing furnace anneal: furnace temperature 740 DEG C, draws between the speed of getting 70 ~ 80, silk material unit elongation >=25% after annealing; Ф 0.3 ~ 0.5mm silk material is drawn to Ф 0.15 ~ 0.2mm, every time working modulus 13%; Continuous hydrogen annealing furnace anneal: furnace temperature 740 DEG C, draws between the speed of getting 70 ~ 80, silk material unit elongation >=20% after annealing; Ф 0.15 ~ 0.2mm silk material is drawn to Ф 0.05 ~ 0.1mm, every time working modulus 12%; Continuous hydrogen annealing furnace anneal: furnace temperature 740 DEG C, draws between the speed of getting 70 ~ 80, silk material unit elongation >=10% after annealing.
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