CN116694957A - High-purity nickel-magnesium intermediate alloy and preparation method thereof - Google Patents
High-purity nickel-magnesium intermediate alloy and preparation method thereof Download PDFInfo
- Publication number
- CN116694957A CN116694957A CN202310559914.0A CN202310559914A CN116694957A CN 116694957 A CN116694957 A CN 116694957A CN 202310559914 A CN202310559914 A CN 202310559914A CN 116694957 A CN116694957 A CN 116694957A
- Authority
- CN
- China
- Prior art keywords
- magnesium
- nickel
- intermediate alloy
- less
- equal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000956 alloy Substances 0.000 title claims abstract description 76
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 74
- ATTFYOXEMHAYAX-UHFFFAOYSA-N magnesium nickel Chemical compound [Mg].[Ni] ATTFYOXEMHAYAX-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 40
- 239000011777 magnesium Substances 0.000 claims abstract description 40
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 19
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 19
- 238000003723 Smelting Methods 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 230000006698 induction Effects 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 13
- 238000007670 refining Methods 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000007664 blowing Methods 0.000 claims description 6
- 239000006260 foam Substances 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 239000011819 refractory material Substances 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 229910000601 superalloy Inorganic materials 0.000 abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 238000007712 rapid solidification Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000005485 electric heating Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 229910052785 arsenic Inorganic materials 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000005204 segregation Methods 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 229910052718 tin Inorganic materials 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 229910001018 Cast iron Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000009849 vacuum degassing Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D43/00—Mechanical cleaning, e.g. skimming of molten metals
- B22D43/001—Retaining slag during pouring molten metal
- B22D43/004—Retaining slag during pouring molten metal by using filtering means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D43/00—Mechanical cleaning, e.g. skimming of molten metals
- B22D43/005—Removing slag from a molten metal surface
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/06—Ingot moulds or their manufacture
- B22D7/064—Cooling the ingot moulds
-
- 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
- C22C1/023—Alloys based on nickel
-
- 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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The application discloses a high-purity nickel-magnesium intermediate alloy and a preparation method thereof, wherein main metal elements of the intermediate alloy comprise 9-17% of magnesium and less than or equal to 0.1% of nickel in percentage by weight, and the balance of nickel is the sum of impurities. The preparation method of the application is different from common induction smelting and vacuum induction smelting processes, but adopts a pressurized inert gas protection smelting process and a rapid solidification technology. The method provided by the application has the advantages of stable and reliable production and high yield. The obtained nickel-magnesium intermediate alloy has good consistency and high purity, fully ensures the high purity requirement of the smelting raw materials for nickel-base superalloys, and reduces the introduction of elements such as nitrogen, oxygen and the like and inclusions.
Description
Technical Field
The application relates to the technical field of alloys, in particular to a high-purity nickel-magnesium intermediate alloy and a preparation method thereof.
Background
The super alloy is used for the hot end parts of aeroengines or gas engines, belongs to key core materials, and has poor quality stability when used in critical conditions, especially in the aspect of long-term service life compared with foreign advanced enterprise products. Besides the problem of control values of alloy elements, the key point is that the purity of the material influences the service life of the material, and the magnesium element is generally added in the final step before finished products after refining in the superalloy preparation process, so that the purity of the nickel-magnesium intermediate alloy directly influences the performance quality of the superalloy master alloy material.
The common nickel-magnesium intermediate alloy is generally produced in an atmospheric environment by adopting an intermediate frequency furnace, and the quality of the prepared nickel-magnesium intermediate alloy is very poor due to the fact that magnesium is in contact with air to be burnt vigorously. Because the normal pressure boiling point of magnesium is only about 1170 ℃, the smelting temperature of 1250-1450 ℃ is adopted in the vacuum induction smelting of the nickel-magnesium intermediate alloy, the magnesium can be boiled and burned in a large quantity, and the accuracy and uniformity of the magnesium content of the alloy cannot be controlled. Therefore, the quality condition of the raw materials such as the nickel-magnesium intermediate alloy and the like is one of key factors influencing the production of special high-performance materials in China.
Disclosure of Invention
The application aims to: aiming at the defects in the prior art, the application provides the high-purity nickel-magnesium intermediate alloy for the superalloy and the preparation method thereof, and the obtained nickel-magnesium intermediate alloy has the advantages of good consistency, accurate components, low inclusion content and high yield, and fully ensures the high-quality requirement of smelting raw materials for nickel-based superalloy.
The technical scheme is as follows: the application provides a high-purity nickel-magnesium intermediate alloy which is characterized in that main metal elements of the intermediate alloy comprise 9-17% by weight of magnesium and less than or equal to 0.1% by weight of nickel, and the balance of nickel is impurities.
Specifically, the impurities: fe is less than or equal to 0.02 percent, si is less than or equal to 0.03 percent, C is less than or equal to 0.03 percent, ag is less than or equal to 0.001 percent, sn is less than or equal to 0.001 percent, as is less than or equal to 0.001 percent, N is less than or equal to 0.001 percent, and O is less than or equal to 0.001 percent.
The application also provides a preparation method of the high-purity nickel-magnesium intermediate alloy, which is characterized by comprising the following steps:
step 1, selecting electrolytic nickel and a primary magnesium ingot, polishing and cutting, then calculating ingredients according to the proportion, weighing and split charging after the ingredients are prepared;
step 2, loading the raw materials into smelting equipment, vacuumizing, carrying out power transmission heating, reducing power after the materials turn red, charging argon before melting, adjusting the temperature to 1250-1450 ℃ after all melting, blowing inert gas into an alloy melt after reducing power, stirring and refining for 1-5 minutes, and adjusting the temperature to 1200-1300 ℃ after refining;
step 3, adjusting an induction power supply to be stirring power, electromagnetically stirring, pouring refined alloy melt to one side of a chute, forming a molten pool with a certain height by the alloy melt through a baffle dam, removing scum by a flashboard, filtering impurities for the second time by a foam filter plate and a filter pipe in sequence, and finally flowing out from a pouring hole and pouring into a water-cooling crystallizer;
step 4, pouring the alloy melt to the working surface of the water-cooling crystallizer to form a quenching layer, and quickly solidifying; and forming an alloy ingot after complete solidification, and ejecting the nickel-magnesium alloy ingot by a hydraulic ejector rod at the bottom of the crystallizer through an ejection hole of a water tank.
Specifically, the raw materials are selected from electrolytic nickel with the specification of Ni9999 and above GB/T6516, and raw magnesium ingots with the specification of Mg9995 and above GB/T3499.
Specifically, the ratio is as follows: 9-17%, and the balance Ni is calculated and proportioned.
Specifically, in the step 2, vacuum is pumped to be less than or equal to 1Pa. The application removes volatile matters such as air, water and the like in the furnace body by vacuum and deaerates raw materials. In the step 2, argon is filled to 0.3-1.0 MPa. According to the application, inert gas argon is filled to positive pressure in the melting period, so that volatilization loss of elemental magnesium is inhibited, and the accuracy of alloy components is ensured.
Specifically, after the power is reduced, argon is blown into the alloy melt in the smelting equipment through a ventilation plug at the bottom of the smelting equipment to stir and refine for 1-5 minutes. Inert gas argon is blown into the bottom of the smelting equipment to generate a melt stirring effect, so that the homogenization of alloy components is promoted, and meanwhile, bubbles formed by the inert gas in the melt drive impurities to float up to achieve a purifying and refining effect.
Specifically, the casting is performed while electromagnetic stirring, and the uniformity of components is ensured by adopting electromagnetic stirring in the casting process.
Specifically, the chute is formed by pressing and sintering high-magnesium refractory materials. The chute consists of an overflow area and a filtering area, the overflow area is provided with a baffle, a flashboard is arranged between the overflow area and the filtering area, and the filter is provided with a filter plate and a filter pipe; the outside of the filter pipe is communicated with the inner space of the chute, and the inside of the filter pipe is communicated with the injection hole. The filter plate and the filter pipe are made of magnesium-based foam ceramic. The chute provided by the application has a filtering and purifying function to further purify the melt.
Specifically, the water-cooled crystallizer structure is provided with a tubular crystallizer, a bottom water tank, a working face, a top outlet and an ejection mechanism. The water-cooling crystallizer has the rapid solidification function, so that macroscopic segregation and microscopic segregation in the cooling process and the solidification process are reduced, and the uniformity of alloy components is further ensured.
The high-purity nickel-magnesium intermediate alloy guarantees the quality requirements of superalloy preparation on raw materials no matter the accuracy, uniformity and purity of components, and has the characteristics of high purity and low segregation.
The beneficial effects are that: according to the application, various refining and homogenizing measures such as vacuum degassing, atmosphere refining, melt blowing refining, electromagnetic stirring, rapid cooling and the like are adopted, uniformity and purity are effectively controlled, and the high-pressure argon atmosphere effectively inhibits volatilization of magnesium, so that the accuracy of alloy components and element recovery rate are ensured, the floating removal of inclusions is promoted by blowing at the bottom of a crucible, and element segregation in the solidification process is reduced by rapid cooling of a water-cooled crystallizer.
The production process is stable and reliable, the cost is low, the consistency of the obtained nickel-magnesium intermediate alloy is good, and the nickel-magnesium intermediate alloy is used for preparing superalloy materials and producing special functional materials such as solid hydrogen storage materials and the like, and is beneficial to the quality improvement and progress of domestic high-end alloy materials.
Drawings
FIG. 1 is a photograph showing the structure of a high purity nickel magnesium master alloy of example 1.
FIG. 2 is a photograph of a vacuum nickel-magnesium master alloy structure of comparative example 01.
FIG. 3 is a photograph of the structure of a common nickel-magnesium master alloy of comparative example 02.
FIG. 4 is a schematic diagram of a purge chute configuration.
In the figure: 1-a chute; 2-dam; 3-flashboard; 4-a filter plate; 5-a filter tube; 6-hole injection.
FIG. 5 is a schematic diagram of a water-cooled crystallizer.
In the figure: 21-water-cooling working face; 22-ejection hole.
Detailed Description
The technical scheme of the present application is described in detail by examples below, but the scope of the present application is not limited to the examples.
Example 1
The high-purity nickel-magnesium intermediate alloy is prepared according to the following method:
1. raw material pretreatment, namely cleaning the surface of the raw material according to a conventional method and processing the raw material into a size required by charging; after pretreatment of the raw materials, weighing: 2.2Kg of magnesium ingot and 17.8Kg of electrolytic nickel.
2. Electrolytic nickel and magnesium ingots are added into a crucible. And (3) vacuumizing the furnace to 0.02Pa, carrying out electric heating with the power of 80KW, carrying out electric heating with the power of 50KW after the material is red, stopping pumping and filling argon to 0.5MPa for complete melting, adjusting the temperature to 1250 ℃, reducing the power to 15KW, blowing argon into an alloy melt in a crucible, and refining for 3Min.
3. The temperature is regulated to 1220 ℃ in a power cut, the stirring power of 25KW is regulated, the crucible is tilted, the alloy is stirred and injected into a water-cooling crystallizer through a purifying chute, the alloy melt is rapidly cooled after contacting a water-cooling copper working surface, and after 40Min is completely solidified and cooled, a hydraulic ejector rod is started to send the alloy out of the crystallizer.
4. And after the alloy is taken out by breaking the air, sampling and detecting chemical components. The results were as follows: mg of The upper part of the ingot ：10.66％，Mg Middle part of ingot ：10.70％，Mg The lower part of the ingot ：10.68％，Fe:0.013％，Si:0.010％，C:0.007％，Ag:0.0001％，Sn:0.0001％，As:0.0001％，N:0.0003％，O:0.0002％。
| Magnesium element | Upper part | Middle part | Lower part | Maximum deviation |
| Component WT% | 10.66 | 10.70 | 10.68 | 0.04 |
Example 2
The high-purity nickel-magnesium intermediate alloy is prepared according to the following method:
1. raw material pretreatment, namely cleaning the surface of the raw material according to a conventional method and processing the raw material into a size required by charging; after pretreatment of the raw materials, weighing: 3.2Kg of magnesium ingot and 16.8Kg of electrolytic nickel.
2. Electrolytic nickel and magnesium ingots are added into a crucible. And (3) vacuumizing the furnace to 0.1Pa, carrying out electric heating with the power of 80KW, carrying out electric heating with the power of 50KW after the material is red, stopping pumping and filling argon to 0.8MPa for complete melting, adjusting the temperature to 1350 ℃, reducing the power to 15KW, blowing argon into an alloy melt in a crucible, and refining for 3Min.
3. The temperature is regulated to 1220 ℃ in a power cut, the stirring power of 25KW is regulated, the crucible is tilted, the alloy is stirred and injected into a water-cooling crystallizer through a purifying chute, the alloy melt is rapidly cooled after contacting a water-cooling copper working surface, and after 40Min is completely solidified and cooled, a hydraulic ejector rod is started to send the alloy out of the crystallizer.
4. After the alloy is taken out by breaking the air, 19.4kg of the alloy is cleaned and weighed, and the yield is 97%.
5. Sampling and detecting chemical components. The results were as follows: mg of The upper part of the ingot ：15.71％，Mg Middle part of ingot ：15.73％，Mg The lower part of the ingot ：15.72％，，Fe:0.011％，Si:0.010％，C:0.012％，Ag:0.0001％，Sn:0.0001％，As:0.0001％，N:0.0005％，O：0.0003％。
| Magnesium element | Upper part | Middle part | Lower part | Maximum deviation |
| Component WT% | 15.71 | 15.73 | 15.72 | 0.02 |
Comparative example 01
The present comparative example prepares a nickel-magnesium master alloy according to the following method (vacuum method):
1. raw material pretreatment, namely cleaning the surface of the raw material according to a conventional method and processing the raw material into a size required by charging; after pretreatment of the raw materials, weighing: 3.2Kg of magnesium ingot and 16.8Kg of electrolytic nickel.
2. Electrolytic nickel and magnesium ingots are added into a crucible. And (3) vacuumizing the furnace to 0.1Pa, carrying out electric heating with the power of 80KW, carrying out electric heating with the power of 50KW after the material is reddened, stopping pumping, and filling argon to-0.08 MPa for complete melting.
3. The temperature is regulated to 1200 ℃ in a power cut mode, the stirring power of 25KW is regulated, the crucible is tilted, and the alloy is poured into a cast iron mold while being stirred.
4. After the alloy is broken and taken out, the alloy is cleaned, 17.4kg of net weight is weighed, and the yield is calculated: 87% of
5. Sampling and detecting chemical components. The results were as follows: mg of The upper part of the ingot ：15.21％，Mg Middle part of ingot ：15.02％，Mg The lower part of the ingot ：14.02％，，Fe:0.25％，Si:0.03％，C:0.02％，Ag:0.0001％，Sn:0.0001％，As:0.0002％，N:0.0025％，O：0.0013％。
| Magnesium element | Upper part | Middle part | Lower part | Maximum deviation |
| Component WT% | 15.21 | 15.02 | 14.02 | 1.19 |
Comparative example 02
The present comparative example was prepared as a nickel-magnesium master alloy according to the following method (ordinary method):
1. raw material pretreatment, namely cleaning the surface of the raw material according to a conventional method and processing the raw material into a size required by charging; after pretreatment of the raw materials, weighing: 3.2Kg of magnesium ingot, 16.8Kg of electrolytic nickel, and 2Kg of covering agent is prepared according to 70% anhydrous magnesium chloride and 30% calcium fluoride.
2. Electrolytic nickel and magnesium ingots were charged into a crucible, and 0.4Kg of a covering agent was sprinkled on the upper portion. And the power of 80KW is used for power transmission and heating, and a covering agent is used for extinguishing fire when magnesium burns in the process until the magnesium is completely melted.
3. And (5) regulating the temperature to 1280 ℃ in power failure, tilting the crucible, and pouring into a cast iron mold.
4. And cooling, taking out the alloy, cleaning the surface dry slag by using a steel wire brush, and manually selecting and cleaning slag inclusion after crushing.
5 weighing 15.6kg of alloy net weight, and calculating yield 78%
6. Sampling and detecting chemical components. The results were as follows: mg of The upper part of the ingot ：13.3％，Mg Middle part of ingot ：12.2％，Mg The lower part of the ingot ：11.0％，Fe:0.3％，Si:0.2％，C:0.15％，Ag:0.0002％，Sn:0.0005％，As:0.0005％，N:0.07％，O：0.013％。
| Magnesium element | Upper part | Middle part | Lower part | Maximum deviation |
| Component WT% | 13.3 | 12.2 | 11.0 | 2.3 |
As can be seen from the finished product weighing, chemical component detection and microscopic examination comparison photographs (figures 1-3), the purity, uniformity and recovery rate of the high-purity nickel-magnesium intermediate alloy prepared by the method are far higher than those of vacuum and common nickel-magnesium intermediate alloy.
Claims (10)
1. The high-purity nickel-magnesium intermediate alloy is characterized in that main metal elements of the intermediate alloy comprise 9-17% by weight of magnesium and less than or equal to 0.1% by weight of nickel, and the balance of nickel is the total impurity.
2. The high purity nickel magnesium master alloy according to claim 1, wherein the impurities: fe is less than or equal to 0.02 percent, si is less than or equal to 0.03 percent, C is less than or equal to 0.03 percent, ag is less than or equal to 0.001 percent, sn is less than or equal to 0.001 percent, as is less than or equal to 0.001 percent, N is less than or equal to 0.001 percent, and O is less than or equal to 0.001 percent.
3. The preparation method of the high-purity nickel-magnesium intermediate alloy is characterized by comprising the following steps of:
step 1, selecting electrolytic nickel and a primary magnesium ingot, polishing and cutting, then calculating ingredients according to the proportion, weighing and split charging after the ingredients are prepared;
step 2, loading the raw materials into smelting equipment, vacuumizing, carrying out power transmission heating, reducing power after the materials turn red, charging argon before melting, adjusting the temperature to 1250-1450 ℃ after all melting, blowing inert gas into an alloy melt after reducing power, stirring and refining for 1-5 minutes, and adjusting the temperature to 1200-1300 ℃ after refining;
step 3, adjusting an induction power supply to be stirring power, electromagnetically stirring, pouring refined alloy melt to one side of a chute, forming a molten pool with a certain height by the alloy melt through a baffle dam, removing scum by a flashboard, filtering impurities for the second time by a foam filter plate and a filter pipe in sequence, and finally flowing out from a pouring hole and pouring into a water-cooling crystallizer;
step 4, pouring the alloy melt to the working surface of the water-cooling crystallizer to form a quenching layer, and quickly solidifying; and forming an alloy ingot after complete solidification, and ejecting the nickel-magnesium alloy ingot by a hydraulic ejector rod at the bottom of the crystallizer through an ejection hole of a water tank.
4. The method for producing a high purity nickel magnesium intermediate alloy according to claim 3, wherein the raw material is selected from electrolytic nickel of GB/T6516, ni9999 and above, and raw magnesium ingot of GB/T3499, mg9995 and above.
5. The method for preparing high purity nickel magnesium intermediate alloy according to claim 3, wherein the ratio is as follows: 9-17%, and the balance Ni is calculated and proportioned.
6. The method for preparing a high purity nickel magnesium intermediate alloy according to claim 3, wherein in step 2, vacuum is applied to a pressure of 1Pa or less; in the step 2, argon is filled to the positive pressure of 0.3-1.0 MPa.
7. The method for preparing the high-purity nickel-magnesium intermediate alloy according to claim 3, wherein the chute is formed by pressing and sintering a high-magnesium refractory material.
8. The method for preparing the high-purity nickel-magnesium intermediate alloy according to claim 3, wherein the chute consists of an overflow area and a filtering area, the overflow area is provided with a baffle, a flashboard is arranged between the overflow area and the filtering area, and the filter is provided with a filter plate and a filter pipe; the outside of the filter pipe is communicated with the inner space of the chute, and the inside of the filter pipe is communicated with the injection hole.
9. The method for preparing high purity nickel magnesium intermediate alloy according to claim 8, wherein the filter plate and the filter tube are made of magnesium-based foam ceramic.
10. The method for producing a high purity nickel magnesium intermediate alloy according to claim 3, wherein after the power is reduced, argon is blown into the alloy melt in the apparatus through a vent plug at the bottom of the melting apparatus to perform stirring refining for 1 to 5 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310559914.0A CN116694957A (en) | 2023-05-18 | 2023-05-18 | High-purity nickel-magnesium intermediate alloy and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310559914.0A CN116694957A (en) | 2023-05-18 | 2023-05-18 | High-purity nickel-magnesium intermediate alloy and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116694957A true CN116694957A (en) | 2023-09-05 |
Family
ID=87828442
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310559914.0A Pending CN116694957A (en) | 2023-05-18 | 2023-05-18 | High-purity nickel-magnesium intermediate alloy and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116694957A (en) |
-
2023
- 2023-05-18 CN CN202310559914.0A patent/CN116694957A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2021018203A1 (en) | Copper-iron alloy slab non-vacuum down-drawing continuous casting production process | |
| CN108546834B (en) | Purification smelting method for nickel-based high-temperature alloy master alloy | |
| CN109371271B (en) | Non-vacuum smelting and continuous casting process for copper-iron alloy | |
| CN110144472B (en) | Vacuum induction melting method of manganese-copper vibration-damping alloy | |
| CN109161697B (en) | Method for controlling non-metallic inclusions in powder metallurgy high-temperature alloy master alloy | |
| CN109913702B (en) | Preparation process of nickel-based high-temperature alloy with high content of refractory elements | |
| CN110396605B (en) | Preparation method of deformed high-temperature alloy ingot | |
| CN111593225B (en) | Preparation method for improving strength of chromium-zirconium-copper bar | |
| JP5048222B2 (en) | Method for producing long ingots of active refractory metal alloys | |
| CN108085546A (en) | A kind of 2024 aluminium alloy smelting casting methods | |
| CN109295330B (en) | Method for refining nitride inclusions in nickel-based wrought superalloy | |
| CN107686902A (en) | A kind of nuclear grade zirconium alloy cast ingot preparation method | |
| CN115094263B (en) | Alterant alloy for copper-chromium-zirconium series alloy, preparation method and application thereof | |
| CN112430767B (en) | Large-size hollow ingot casting and ingot casting method | |
| CN114318109B (en) | Method for smelting high-nitrogen die steel by using vacuum induction furnace and pressurized electroslag furnace | |
| CN104388756A (en) | Nickel-based alloy and preparation method thereof | |
| CN108660320A (en) | A kind of low-aluminium high titanium-type high temperature alloy electroslag remelting process | |
| CN112359251A (en) | Preparation method and application of nickel-chromium-tungsten intermediate alloy | |
| CN102069174A (en) | Method for producing centrifugal electroslag smelting and casting double-base composite roller | |
| CN110438378A (en) | A kind of 2 line aluminium alloy melting and casting methods | |
| CN114000020B (en) | Ingot for large-size die forging and preparation method thereof | |
| CN116694957A (en) | High-purity nickel-magnesium intermediate alloy and preparation method thereof | |
| JP2011173172A (en) | Method for producing long cast block of active high melting point metal alloy | |
| CN113549733B (en) | Bottom argon blowing method for high-temperature alloy master alloy purification smelting | |
| JP2011012300A (en) | Copper alloy and method for producing copper alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |