CN109371270B - Preparation method for CuFe master alloy material by vacuum induction melting - Google Patents
Preparation method for CuFe master alloy material by vacuum induction melting Download PDFInfo
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- CN109371270B CN109371270B CN201811316100.XA CN201811316100A CN109371270B CN 109371270 B CN109371270 B CN 109371270B CN 201811316100 A CN201811316100 A CN 201811316100A CN 109371270 B CN109371270 B CN 109371270B
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- 238000002844 melting Methods 0.000 title claims abstract description 25
- 230000008018 melting Effects 0.000 title claims abstract description 25
- 239000000956 alloy Substances 0.000 title claims abstract description 22
- 230000006698 induction Effects 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000003723 Smelting Methods 0.000 claims abstract description 34
- 238000005266 casting Methods 0.000 claims abstract description 22
- 229910052786 argon Inorganic materials 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 229910052802 copper Inorganic materials 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 238000007599 discharging Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 13
- 229910045601 alloy Inorganic materials 0.000 description 13
- 239000010949 copper Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- -1 conductivity Chemical compound 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910000640 Fe alloy Inorganic materials 0.000 description 4
- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 description 4
- 238000005204 segregation Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 235000010290 biphenyl Nutrition 0.000 description 3
- 239000004305 biphenyl Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000007712 rapid solidification Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
-
- 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
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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
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Crucibles And Fluidized-Bed Furnaces (AREA)
Abstract
The invention discloses a preparation method of a CuFe master alloy material by vacuum induction melting, which comprises the following steps: weighing raw materials of Cu and Fe according to a ratio, putting the raw materials into a crucible, putting the crucible into a vacuum smelting furnace, closing a furnace cover and an air release valve, and cleaning an observation window; step two, starting a mechanical pump and a low vacuum baffle valve, starting a Roots pump to pump vacuum until the pressure P in a vacuum melting furnace is less than or equal to 0.08MPa, starting the Roots pump to pump vacuum until the pressure P in the vacuum melting furnace is less than or equal to 4Pa, increasing the power of the vacuum melting furnace to 25KW, keeping the temperature for 8min, increasing the power of the vacuum melting furnace to 45KW, keeping the temperature for 8min, increasing the heating power of the vacuum melting furnace to 65KW, reducing the power to 20KW after raw materials in a crucible are uniform, filling argon into the furnace body, closing an argon filling gas valve when the pressure in the furnace is increased to 0.08 MPa; and step three, reducing the power of the vacuum smelting furnace to 40KW, keeping for 0.5min, starting casting into a casting mold, and cooling for 60min after casting is finished and then discharging.
Description
Technical Field
The invention belongs to the technical field of new material preparation, and particularly relates to a preparation method of a CuFe master alloy material by vacuum induction melting.
Background
With the wide application of high-strength and high-conductivity copper alloys in various industries, higher requirements are put on the use performance and manufacturing cost of the high-strength and high-conductivity copper alloys, the copper-iron alloys have unique and superior characteristics such as electromagnetic wave shielding property, elasticity, conductivity, heat release property, wear resistance, antibacterial property and the like due to the properties of copper such as conductivity, thermal conductivity, ductility, elasticity and the like and the properties of iron such as wear resistance, strength, hardness, magnetism and the like, and the copper-iron alloys can be processed into various physical forms such as bars, cables, plates, films, powders, tubes and the like, can be applied to various industrial fields, and have competitiveness and market prospect which cannot be surpassed.
However, as seen from the phase diagram of copper and iron, the two are almost completely immiscible at room temperature, the solubility at 300 ℃ is still zero, the solubility at 1094 ℃ is only about 5%, and the solubility of Fe in Cu is very low, so that the alloy is very easy to form a structure with serious segregation in the solidification process, and the application of the CuFe alloy is seriously influenced. The rapid solidification can refine grains, increase solid solubility and inhibit or relieve an effective way for forming a segregation structure in the solidification process of the CuFe alloy, so that the research on the rapid solidification behavior is more and more concerned by people.
The current method for producing CuFe alloy at home and abroad comprises the following steps: the invention provides a preparation method adopting vacuum induction melting, aiming at the defects of the prior art, and the preparation method adopts a vacuum induction melting method.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method for a CuFe master alloy material by vacuum induction melting.
The technical scheme of the invention is as follows: a preparation method for CuFe master alloy material by vacuum induction melting comprises the following steps:
step one, batching and charging
Weighing Cu and Fe raw materials according to the proportion of 1:1 in percentage by weight, uniformly mixing, putting the mixture into a crucible, putting the crucible into a vacuum smelting furnace, closing a vacuum smelting furnace cover, closing a gas release valve, and cleaning an observation window;
step two, vacuum induction melting
Starting a mechanical pump, opening a low-vacuum baffle valve to vacuumize, starting a Roots pump when the vacuum pressure P in a vacuum smelting furnace is less than or equal to 0.08MPa, heating and raising the temperature when the vacuum degree is less than or equal to 4Pa, raising the power of the vacuum smelting furnace to 20KW-30KW, preserving the heat for 5min-10min, raising the power of the vacuum smelting furnace to 40KW-50KW, preserving the heat for 5min-10min, raising the heating power of the vacuum smelting furnace to 60KW-70KW, reducing the power to 20KW after the raw materials in a crucible are uniformly lifted, opening an argon-filled air valve, slowly filling argon into the furnace body of the vacuum smelting furnace, closing the argon-filled air valve when the pressure in the furnace is raised to 0.08MPa, raising the power to 70KW +/-5 KW, and;
step three, casting and discharging
And reducing the power of the vacuum smelting furnace to 40KW +/-5 KW, keeping for 0.5min, starting to cast into the casting mold, closing heating after casting is finished, and discharging after cooling for 60 min.
Furthermore, a pressure sensor is arranged in the vacuum melting furnace and used for monitoring the pressure in the vacuum melting furnace in real time, an MAS intelligent controller is arranged in the pressure sensor in an integrated mode, the MAS intelligent controller is electrically connected with the roots pump, the heating device and the argon filling air valve respectively and used for intelligently controlling the starting and stopping of the roots pump, the heating device and the argon filling air valve, intelligent control is achieved, accuracy is high, manpower is saved, and melting efficiency is improved.
Furthermore, the crucible material is zirconia, the crucible selected during smelting must be a carbon-free crucible, carbon in the carbon-containing crucible seriously influences the smelting of the copper-iron alloy, and the casting mold is a steel film mold, so that the forming is fast, the cooling is easy, and the loss is low.
Furthermore, the purity of the Cu and Fe raw materials is more than 99.9%, the content of impurities in the raw materials is avoided, and the purity of the CuFe master alloy is ensured.
Further, the concentration of argon filled in the second step is 99.999%, and the higher the concentration is, the better the protection is.
Furthermore, the casting time t in the third step is less than or equal to 1min, the casting speed is in the order of slow, fast and slow, and the casting is easy to cause uneven casting due to long casting time.
Furthermore, the cooling mode in the third step is water-cooling, alkyl biphenyl heat transfer oil is adopted in the water-cooling, the water-cooling efficiency is higher than that of air cooling, and the adopted alkyl biphenyl heat transfer oil has the advantages of high boiling point, good thermal stability and no corrosiveness.
The invention has the beneficial effects that: compared with the prior art, the preparation method for smelting the CuFe master alloy material by adopting vacuum induction selects raw materials with higher purity, ensures the purity of the alloy from the source, simultaneously selects a carbon-free crucible as a smelting crucible, avoids carbon from influencing the smelting of the copper-iron alloy, and optimizes the smelting step.
Drawings
FIG. 1-2 is a schematic view of the metallographic structure of the CuFe alloy of the present invention.
Detailed Description
For the understanding of the technical solutions of the present invention, the following description is further illustrated with reference to fig. 1-2 and specific examples, which are not intended to limit the scope of the present invention.
Example 1
A preparation method for CuFe master alloy material by vacuum induction melting comprises the following steps:
step one, batching and charging
Weighing Cu and Fe raw materials with the purity of more than 99.9 percent according to the proportion of 1:1, uniformly mixing, putting the raw materials into a zirconia crucible, putting the zirconia crucible into a vacuum smelting furnace, closing a vacuum smelting furnace cover, closing a gas release valve, and cleaning an observation window;
step two, vacuum induction melting
Starting a mechanical pump, opening a low-vacuum baffle valve for vacuumizing, starting a roots pump when the vacuum pressure P in a vacuum smelting furnace is equal to 0.08MPa, heating and raising the temperature when the vacuum degree is increased to 4Pa, raising the power of the vacuum smelting furnace to 25KW, keeping the temperature for 8min, raising the power of the vacuum smelting furnace to 15KW, keeping the temperature for 8min, raising the heating power of the vacuum smelting furnace to 65KW, lowering the power to 20KW after the raw materials in a crucible are uniformly lifted, opening an argon filling valve, slowly filling argon with the concentration of 99.999% into the furnace body of the vacuum smelting furnace, closing the argon filling valve when the pressure in the furnace is increased to 0.08MPa, raising the power to 70KW, refining for 2min, arranging a pressure sensor in the vacuum smelting furnace for monitoring the pressure in the vacuum smelting furnace in real time, integrally arranging an MAS intelligent controller in the pressure sensor, and electrically connecting the MAS intelligent controller with the roots pump, the heating device and the argon filling valve respectively, the device is used for intelligently controlling the starting and stopping of the Roots pump, the heating device and the argon filling gas valve, intelligently controlling, having high accuracy, saving manpower and improving the smelting efficiency;
step three, casting and discharging
Reducing the power of a vacuum smelting furnace to 40KW, keeping 0.5min, starting to cast in a steel casting mold, wherein the casting time t is 1min, closing and heating after casting, discharging after cooling for 60min, and adopting alkyl biphenyl heat conduction oil for water cooling.
Example 2
The metallographic structure of the CuFe alloy prepared by the vacuum induction melting method of example 1 is shown in fig. 1-2:
in the figure 1-2, the gray part is an iron phase, and the white part is a copper phase, and as can be seen from the figure 1-2, the iron phase is mainly granular or dendritic and is uniformly dispersed in the copper matrix, and no obvious segregation phenomenon is observed.
And (4) conclusion: the CuFe alloy prepared by the vacuum induction melting method of example 1 had a uniform structure and no segregation.
Example 3
The chemical content of the CuFe master alloy prepared by the vacuum induction melting method in example 1 was measured as shown in table 1:
TABLE 1 chemical content detection table for CuFe master alloy
Fe(%) | O(ppm) | N(ppm) | C(ppm) | S(ppm) | |
CuFe master alloy | 50.18 | 60 | 14 | 16 | 37 |
And (4) conclusion: the CuFe alloy produced by the vacuum induction melting method of example 1 had a small amount of inclusions and a uniform texture component.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (1)
1. A preparation method for CuFe master alloy material by vacuum induction melting is characterized by comprising the following steps:
step one, batching and charging
Weighing Cu and Fe raw materials according to the proportion of 1:1 in percentage by weight, uniformly mixing, putting the mixture into a crucible, putting the crucible into a vacuum smelting furnace, closing a vacuum smelting furnace cover, closing a gas release valve, and cleaning an observation window;
step two, vacuum induction melting
Starting a mechanical pump, opening a low-vacuum baffle valve to vacuumize, starting a Roots pump when the vacuum pressure P in a vacuum smelting furnace is less than or equal to 0.08MPa, when the vacuum degree is less than or equal to 4Pa, increasing the power of a heating device to 20KW-30KW, preserving heat for 5min-10min, increasing the heating power of the heating device to 40KW-50KW, preserving heat for 5min-10min, increasing the heating power of the heating device to 60KW-70KW, reducing the heating power to 20KW after the raw materials in a crucible are uniform up and down, opening an argon filling air valve, slowly filling argon into the furnace body of the vacuum smelting furnace, closing the argon filling air valve when the pressure in the furnace is increased to 0.08MPa, increasing the power to 70KW +/-5 KW, and refining for 1min-2 min;
step three, casting and discharging
Reducing the power of a vacuum smelting furnace to 40KW +/-5 KW, keeping for 0.5min, starting casting into a casting mold, closing heating after casting is finished, and discharging after cooling for 60 min;
a pressure sensor is arranged in the vacuum smelting furnace and used for monitoring the pressure in the vacuum smelting furnace in real time, an intelligent controller is integrated in the pressure sensor, and the intelligent controller is electrically connected with the roots pump, the heating device and the argon filling air valve respectively and used for intelligently controlling the roots pump, the heating device and the argon filling air valve;
the crucible is made of zirconia, and the casting mold is a steel film mold;
the purity of the Cu and Fe raw materials is more than 99.9%;
argon is filled into the step two, wherein the concentration of the argon is 99.999 percent;
and the casting time t in the third step is less than or equal to 1 min.
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