CN117127036A - Preparation method of strengthening NCu30-4-2-1 alloy by adding rare earth element Ce - Google Patents
Preparation method of strengthening NCu30-4-2-1 alloy by adding rare earth element Ce Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 152
- 239000000956 alloy Substances 0.000 title claims abstract description 152
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000005728 strengthening Methods 0.000 title abstract description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 64
- 238000005266 casting Methods 0.000 claims abstract description 50
- 238000007670 refining Methods 0.000 claims abstract description 50
- 239000002994 raw material Substances 0.000 claims abstract description 41
- 239000000155 melt Substances 0.000 claims abstract description 32
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 15
- 239000010439 graphite Substances 0.000 claims abstract description 15
- 229910052786 argon Inorganic materials 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims description 43
- 230000008018 melting Effects 0.000 claims description 43
- 239000012535 impurity Substances 0.000 claims description 22
- 229910000831 Steel Inorganic materials 0.000 claims description 20
- 238000005275 alloying Methods 0.000 claims description 20
- 239000010959 steel Substances 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229910052684 Cerium Inorganic materials 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000002893 slag Substances 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 8
- 229910052748 manganese Inorganic materials 0.000 claims description 8
- 230000005540 biological transmission Effects 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 230000001276 controlling effect Effects 0.000 abstract description 30
- 238000003723 Smelting Methods 0.000 abstract description 17
- 239000010949 copper Substances 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 13
- 230000006698 induction Effects 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 5
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 229910000881 Cu alloy Inorganic materials 0.000 abstract description 2
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000005496 eutectics Effects 0.000 description 28
- 210000001787 dendrite Anatomy 0.000 description 24
- 238000004458 analytical method Methods 0.000 description 20
- 239000000203 mixture Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 239000011159 matrix material Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 5
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 150000002910 rare earth metals Chemical group 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000007872 degassing Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- -1 rare earth compounds Chemical class 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000004781 supercooling Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the field of strengthening nickel-copper alloy, and particularly relates to a preparation method of strengthening NCu30-4-2-1 alloy by adding rare earth element Ce. Firstly, putting graphite, a Cu plate, a Ni plate and Fe blocks into a crucible by utilizing a vacuum induction smelting technology, refining the raw materials, wherein the vacuum degree in the refining period is 0.5-1.0 Pa, the refining temperature is 1480-1520 ℃, and the refining time is 20min; after the liquid surface of the melt is conjunctival, argon is filled into the furnace for 30000Pa to 40000Pa, then Si blocks and Mn sheets wrapped by nickel plates are added into the melt, and high-power stirring is carried out for 5min; and finally controlling the temperature of the melt at 1250-1300 ℃, adding the Ce block wrapped by the nickel plate into the melt, stirring for 5min under high power, and casting when the temperature is raised to 1360+/-10 ℃ by power supply, thus obtaining the cast ingot with high purity and uniform components. The invention determines the feeding mode and smelting process of alloy smelting and improves the yield of rare earth element Ce. In addition, the content of Ce element is regulated and controlled to obtain better strong plastic matching.
Description
Technical Field
The invention belongs to the field of strengthening nickel-copper alloy, and particularly relates to a preparation method of strengthening NCu30-4-2-1 alloy by adding rare earth element Ce.
Background
The NCu30-4-2-1 alloy is a high-wear-resistance nickel-based alloy which has high hardness, high strength, excellent wear resistance and anti-adhesion property and is used for manufacturing aviation fuel oil devices and other precise friction parts requiring stable operation. The outstanding problem in the smelting process of NCu30-4-2-1 alloy is that the alloy elements are easy to oxidize and have a tendency to suck air, so that effective measures must be taken in many ways to obtain a high-quality alloy melt with low gas content, few inclusions and uniform and qualified chemical composition. The NCu30-4-2-1 alloy is smelted mainly by using a vacuum induction furnace and a vacuum arc furnace, and elements such as Cu, si, mn and the like in the alloy components are easy to oxidize under the high-temperature smelting condition, so that a large amount of inclusions are generated on grain boundaries when the alloy is solidified, and the performance and the yield of the alloy are reduced.
The rare earth element can improve the performance of traditional materials such as steel, aluminum and the like, and plays a role in stone-firing and gold-forming. The addition of trace rare earth elements Ce to NCu30-4-2-1 alloy can form nonmetallic inclusions with O, N and S elements in steel, and can be used as dispersoids of pinning grain boundaries, which can refine the structure and improve the mechanical properties of the alloy. In addition, the larger radius of the rare earth atoms causes larger lattice distortion, thereby playing the role of solid solution strengthening. However, excessive O, N, S content in the melt not only affects the mechanical properties of the alloy, but also significantly affects the Ce yield. In addition, the feeding mode of Ce and the temperature of the melt also influence the yield of Ce; in order to improve the mechanical properties of the alloy, the invention mainly controls the content of rare earth element Ce by improving a feeding mode and a smelting process, and toughens the NCu30-4-2-1 alloy by adding the Ce element.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method for strengthening NCu30-4-2-1 alloy by adding rare earth element Ce. By adopting the feeding mode and the smelting process provided by the invention, the content of O in the NCu30-4-2-1 alloy prepared by smelting is less than or equal to 0.0030%, the content of N is less than or equal to 0.0010% and the content of S is less than or equal to 0.0015%. Meanwhile, the capability of regulating and controlling microstructure by the rare earth element is exerted by adjusting the Ce content, so that the prepared NCu30-4-2-1 alloy has good matching of high strength and high plasticity.
The technical scheme of the invention is as follows:
a preparation method of a strengthening NCu30-4-2-1 alloy by adding rare earth element Ce comprises the following components in percentage by weight: less than or equal to 0.03 percent of C, 30 to 32 percent of Cu, 3.9 to 4.3 percent of Si, 1.5 to 2.8 percent of Fe, 0.5 to 1.5 percent of Mn, 0.01 to 0.06 percent of Ce, and the balance of Ni and unavoidable impurity elements; in the impurity elements, the content of O is less than or equal to 0.0030 percent, the content of N is less than or equal to 0.0010 percent, and the content of S is less than or equal to 0.0015 percent;
the preparation method specifically comprises the following steps:
(1) Raw material selection: selecting a Ni plate, a Cu plate, a Si block, a Fe rod, a Mn sheet, a graphite rod and a Ce block as raw materials, and calculating and preparing raw materials of each element according to the component control requirement;
(2) And (2) charging: for the NCu30-4-2-1 alloy containing Ce, batch charging is carried out according to the factors of the melting point, the easy oxidation degree, the density, the adding quantity and the easy volatility of the raw materials; charging in a first batch, and sequentially loading graphite, a Cu plate, a Ni plate and Fe blocks into a crucible; charging in a second batch, and sequentially loading Si blocks and Mn sheets wrapped by nickel plates into a crucible; thirdly, charging in batches, and charging Ce blocks wrapped by nickel plates into a crucible;
(3) Melting period: when the vacuum degree in the melting period is less than or equal to 10Pa, power transmission is started, the power is gradually increased to 25-30 kW in the early melting period of the first batch, so that after a molten pool is formed, the power supply is reduced to 20+/-1 kW of melting materials, and the melting period time is ensured to be 35-45 min; after melting, heating to 1480-1520 ℃ and entering a refining period;
(4) Refining period: controlling the vacuum degree to be 0.5-1.0 Pa in the refining period, controlling the power range to be 13-17 kW, controlling the refining temperature to be 1480-1520 ℃ and the refining time to be 15-25 min;
(5) Alloying period: after refining, entering an alloying period, stopping power and forming a film, charging argon 30000-40000 Pa into a furnace, adding a second batch of materials into a melt, stirring for 4-6 min under high power, finally controlling the temperature of the melt to 1250-1300 ℃, adding a third batch of materials, stirring for 4-6 min under high power, heating to 1360+/-10 ℃ and casting;
(6) Casting: the inner wall of the ingot casting mould is cleaned by a steel shovel and a steel brush, the residual steel slag and oxide skin are removed by compressed air, the casting temperature is 1360+/-10 ℃, a pouring cup with the inner diameter of a lower opening of phi 20mm is used for controlling the casting speed, the casting time of each ingot casting is ensured to be 40-60 s, the yield of Ce element is stabilized at 85% -90%, and the ingot casting with high purity and uniform components is obtained.
In the preparation method of the strengthening NCu30-4-2-1 alloy by adding the rare earth element Ce, in the step (1), the total carried-in O content of the raw materials is less than or equal to 0.020 percent, and the S content is less than or equal to 0.0015 percent.
In the preparation method of the reinforced NCu30-4-2-1 alloy by adding the rare earth element Ce, in the step (1), all raw materials remove oxides, greasy dirt and impurities on the surface.
In the preparation method of the reinforced NCu30-4-2-1 alloy by adding the rare earth element Ce, in the step (1), si blocks and Mn sheets with industrial purity are adopted as raw materials, and the purity of the raw materials of the rest alloy elements is not lower than 99.9 wt%.
The preparation method of the strengthening NCu30-4-2-1 alloy by adding the rare earth element Ce comprises the steps of controlling the O content in a melt to be less than or equal to 0.0050%, the N content to be less than or equal to 0.0020% and the S content to be less than or equal to 0.0015% after the melting period in the step (3) and the refining period in the step (4).
In the preparation method of the reinforced NCu30-4-2-1 alloy by adding the rare earth element Ce, in the step (5), the high power is 30kW.
The design idea of the invention is as follows:
based on the technical scheme, the invention ensures that the total carried-in O content of the raw materials is less than or equal to 0.020 percent and the S content is less than or equal to 0.0015 percent, and reduces the reaction with Ce element to form oxysulfide by controlling the content of the charged O, S, thereby influencing the yield of the Ce element. All high-purity graphite is added into the first batch of material, so that the concentration of C in a molten pool is ensured, the C-O reaction in the melting process is promoted, and the degassing effect in the melting period is improved. The vacuum degree and time of the melting period and the vacuum degree and refining time of the refining period are controlled, good thermodynamic and kinetic conditions can be provided for the C-O reaction, the degassing in the vacuum induction process is promoted, and the alloying period is ensured after the O content is less than or equal to 0.0050%, the N content is less than or equal to 0.0020% and the S content is less than or equal to 0.0015%.
The alloying period of the invention adopts a mode of low temperature and argon filling, so that volatilization of Mn element is reduced. The Ce block is added at the lower temperature of 1250-1300 ℃, so that the burning loss can be reduced; the Mn sheet, the Si block and the Ce block are wrapped by the nickel plate, so that the elements can be quickly sunk in the melt. Meanwhile, the nickel plate is melted in the melt first, so that the oxidation burning loss of the elements is avoided when the elements are added into the melt. High-power stirring is adopted, so that Mn, si and Ce elements are quickly involved into the melt and are uniformly dissolved, the burning loss of the elements is further reduced, and an alloy cast ingot with uniform components is obtained.
The invention has the advantages and beneficial effects that:
(1) The invention reduces the pressure of O removal, N removal and S removal in the vacuum smelting process by controlling the contents of the furnace O, N and the S.
(2) The invention ensures that the O content is less than or equal to 0.0050 percent, the N content is less than or equal to 0.0020 percent and the S content is less than or equal to 0.0015 percent in melt entering an alloying period through process control in a charging period, a melting period and a refining period, and creates basic conditions for accurate and stable control of the Ce content.
(3) According to the invention, through a Ce feeding mode and a melt temperature and stirring process control, accurate and stable control of Ce content in NCu30-4-2-1 alloy vacuum induction smelting is realized, and the Ce yield is stabilized at 85% -90%.
(4) According to the invention, trace rare earth elements Ce are added to adsorb O, N, S and other impurity elements to form nonmetallic oxygen and sulfide pinning grain boundaries, so that grain boundary migration is hindered, the effects of refining tissues and removing impurities are achieved, and finally the strength and plasticity of NCu30-4-2-1 alloy are well matched.
(5) The preparation method of the strengthening NCu30-4-2-1 alloy by adding the rare earth element Ce provided by the invention has a simple process flow.
In a word, the invention determines the feeding mode and smelting process of alloy smelting, and improves the yield of rare earth element Ce. The addition of the rare earth element Ce can effectively degas and remove impurities, so that the metallurgical quality of the alloy is improved; in addition, the content of Ce element is regulated and controlled, the alloy is better matched with strong plasticity, and the performance index of the NCu30-4-2-1 alloy strengthened and toughened by adding the rare earth element Ce is as follows: alloy tensile Strength R m 910-980 MPa, yield strength R p0.2 550-590 MPa, elongation after fracture A of 9.0-13.5% and dendrite area volume fraction of 46-63%.
Description of the drawings:
FIG. 1 is an X-ray diffraction spectrum of an as-cast NCu30-4-2-1 alloy prepared in comparative example and example.
FIG. 2 shows the microstructure morphology of the as-cast NCu30-4-2-1 alloy prepared in the comparative example and the example. Wherein, (a) the Ce0 alloy shows dendrite morphology, (b) the Ce1 alloy shows dendrite morphology, (c) the Ce3 alloy shows dendrite morphology, and (d) the Ce6 alloy shows dendrite morphology, and the inset is a partial enlarged view.
FIG. 3 is a tensile engineering stress strain curve of the as-cast NCu30-4-2-1 alloy prepared in the comparative example and the example.
Detailed Description
In a specific implementation, the NCu30-4-2-1 alloy composition (wt.%) of the examples is as follows: less than or equal to 0.03 percent of C, 30 to 32 percent of Cu, 3.9 to 4.3 percent of Si, 1.5 to 2.8 percent of Fe, 0.5 to 1.5 percent of Mn, 0.01 to 0.06 percent of Ce, and the balance of Ni and unavoidable impurity elements; among the impurity elements, the content of O is less than or equal to 0.0030 percent, the content of N is less than or equal to 0.0010 percent, and the content of S is less than or equal to 0.0015 percent. The NCu30-4-2-1 alloy composition (wt.%) of the comparative example is as follows: c is less than or equal to 0.03, cu is 30-32, si is 3.9-4.3, fe is 1.5-2.8, mn is 0.5-1.5, ce is 0, and the balance is Ni and unavoidable impurity elements; among the impurity elements, the content of O is less than or equal to 0.0050%, the content of N is less than or equal to 0.0020%, and the content of S is less than or equal to 0.0015%.
Firstly, putting graphite, a Cu plate, a Ni plate and Fe blocks into a crucible by utilizing a vacuum induction smelting technology, refining the raw materials, wherein the vacuum degree in the refining period is 0.5-1.0 Pa, the refining temperature is 1480-1520 ℃, and the refining time is 20min; after the liquid surface of the melt is conjunctival, argon is filled into the furnace for 30000Pa to 40000Pa, then Si blocks and Mn sheets wrapped by nickel plates are added into the melt, and high-power stirring is carried out for 5min; and finally controlling the temperature of the melt at 1250-1300 ℃, adding the Ce block wrapped by the nickel plate into the melt, stirring for 5min under high power, and casting when the temperature is raised to 1360+/-10 ℃ by power supply, thus obtaining the cast ingot with high purity and uniform components.
Wherein, the raw materials adopt Si blocks with industrial purity (> 99.37 wt.%) and Mn sheets (> 97.45 wt.%) and the raw material purity of the rest alloy elements is not lower than 99.9wt.%. The recipe for the NCu30-4-2-1 alloy is shown in Table 1; the NCu30-4-2-1 alloy obtains the content of each element by a plasma emission spectrometer, an oxygen-nitrogen-hydrogen analyzer and a carbon-sulfur analyzer, and the content is shown in a table 2; the NCu30-4-2-1 alloy has the composition phase components obtained by a scanning electron microscope spectrometer, and the composition phase components are shown in a table 3.
TABLE 1 dosage unit for comparative and example alloys
Table 2 comparative and example alloys the content of each element was obtained by a plasma emission spectrometer, an oxygen nitrogen hydrogen analyzer and a carbon sulfur analyzer
Table 3 comparative and example alloys constituent phase compositions obtained by scanning electron microscopy spectroscopy
The technical scheme of the present invention will be described in further detail with reference to comparative examples and examples.
Comparative example 1
In the comparative example, the NCu30-4-2-1 alloy is not added with rare earth element Ce, which is called Ce0 alloy for short, 10kg of alloy is smelted in a single furnace, and 0wt.% of Ce element is added during batching, as shown in Table 1.
The preparation method of the NCu30-4-2-1 alloy comprises the following specific steps:
(1) Raw material selection: selecting Ni plate, cu plate, si block, fe rod, mn sheet and graphite as raw materials, ensuring that the total carried O content of the raw materials is less than or equal to 0.020% and the S content is less than or equal to 0.0015%, and calculating and preparing raw materials of each element according to the component control requirement; all raw materials remove oxides, greasy dirt and impurities on the surface;
(2) And (2) charging: the NCu30-4-2-1 alloy was charged in batches. Charging in a first batch, and sequentially loading graphite, a Cu plate, a Ni plate and Fe blocks into a crucible; charging in a second batch, namely charging Si blocks and Mn sheets wrapped by nickel plates into a crucible;
(3) Melting period: the power transmission is started when the vacuum degree in the melting period is 5Pa, the power is gradually increased to 28kW in the early melting period of the first batch, so that after a molten pool is formed, the power supply is reduced to 20+/-1 kW of melting materials, and the melting period time is ensured to be 40min; after melting, heating to 1500 ℃ to enter a refining period;
(4) Refining period: controlling the vacuum degree to be 0.8Pa, the power to be 15kW in the refining period, controlling the refining temperature to be 1500 ℃, refining for 20min, controlling the O content to be less than or equal to 0.0050%, the N content to be less than or equal to 0.0020% and the S content to be less than or equal to 0.0015% in the melt, and then entering an alloying period;
(5) Alloying period: after refining, entering an alloying period, stopping power and forming films, charging argon into a furnace for 35000Pa, adding a second batch of materials into a melt, stirring for 5min with high power of 30kW, then supplying power and heating to 1360+/-10 ℃ for casting;
(6) Casting: the inner wall of the ingot casting mould is cleaned by a steel shovel and a steel brush, the residual steel slag and oxide skin are removed by compressed air, the casting temperature is 1360+/-10 ℃, a pouring cup with the inner diameter of a lower opening of phi 20mm is used for controlling the casting speed, the casting time of each ingot casting is ensured to be 40-60 s, and NCu30-4-2-1 alloy ingot casting with uniform components is obtained.
Characterization of the microstructure of the as-cast Ce0 alloy. As shown in fig. 1, the XRD diffraction pattern of the Ce0 alloy has two phases, an alpha phase and a beta phase, which are both face-centered cubic structures; as shown in fig. 2 (a), the Ce0 alloy shows dendrite morphology, and both dendrites and inter-dendrites have matrix alpha phase and granular secondary beta phase that is dispersed and precipitated in the matrix, but the difference in color between the two regions is due to the difference in solid solution element content, i.e. the inter-dendrite Si element content is higher, as shown in table 3. In addition, there is eutectic (alpha+beta) phase between dendrites, and black spots are clearly visible on the eutectic beta phase, and the spots are eutectic alpha phase. Because the size of the eutectic alpha phase is small, the analysis result of the size limitation of the energy spectrometer of the scanning electron microscope can be greatly error, but the analysis result can show that the two-phase components are different. In contrast, the composition analysis of the eutectic beta phase is more accurate, and the chemical analysis result shows that the beta phase is enriched in Ni and Si elements, but depleted in Cu, fe and Mn elements; the composition analysis error of the eutectic alpha phase is larger, but the Si content is obviously lower than that of the eutectic beta phase, as shown in Table 3.
As shown in FIG. 3, from the tensile engineering stress-strain curve of Ce0 alloy, the tensile strength R of Ce0 alloy can be seen m 961MPa, yield strength R p0.2 591MPa, elongation after break A is 14.75%.
Example 1
In this example, 10kg of an alloy, abbreviated as Ce1 alloy, was single-furnace smelted by adding 0.01wt.% of a rare earth element Ce0.01 to toughen the NCu30-4-2-1 alloy. Considering the burning loss of rare earth element Ce in smelting, 0.0125wt.% of Ce element is added in the process of batching, and the table 1 is shown.
The preparation method of the NCu30-4-2-1 alloy comprises the following specific steps:
(1) Raw material selection: selecting Ni plates, cu plates, si blocks, fe rods, mn sheets, graphite and Ce blocks as raw materials, ensuring that the total carried-in O content of the raw materials is less than or equal to 0.020 percent and the S content is less than or equal to 0.0015 percent, and calculating and preparing raw materials of each element according to the component control requirement; all raw materials remove oxides, greasy dirt and impurities on the surface;
(2) And (2) charging: the Ce-containing NCu30-4-2-1 alloy was charged in batches. Charging in a first batch, and sequentially loading graphite, a Cu plate, a Ni plate and Fe blocks into a crucible; charging in a second batch, namely charging Si blocks and Mn sheets wrapped by nickel plates into a crucible; thirdly, charging in batches, and charging Ce blocks wrapped by nickel plates into a crucible;
(3) Melting period: the power transmission is started when the vacuum degree in the melting period is 5Pa, the power is gradually increased to 28kW in the early melting period of the first batch, so that after a molten pool is formed, the power supply is reduced to 20+/-1 kW of melting materials, and the melting period time is ensured to be 40min; after melting, heating to 1500 ℃ to enter a refining period;
(4) Refining period: controlling the vacuum degree to be 0.8Pa, the power to be 15kW in the refining period, controlling the refining temperature to be 1500 ℃, refining for 20min, controlling the O content to be less than or equal to 0.0050%, the N content to be less than or equal to 0.0020% and the S content to be less than or equal to 0.0015% in the melt, and then entering an alloying period;
(5) Alloying period: after refining, entering an alloying period, stopping power and forming a film, charging argon into a furnace for 35000Pa, adding a second batch of materials into a melt, stirring for 5min with high power of 30kW, finally controlling the temperature of the melt to 1270 ℃, adding Ce blocks wrapped by nickel plates, stirring for 5min with high power of 30kW, and heating to 1360+/-10 ℃ for casting;
(6) Casting: the inner wall of the ingot casting mould is cleaned by a steel shovel and a steel brush, the residual steel slag and oxide skin are removed by compressed air, the casting temperature is 1360+/-10 ℃, a pouring cup with the inner diameter of a lower opening of phi 20mm is used for controlling the casting speed, the casting time of each ingot casting is ensured to be 40-60 s, the yield of Ce element is stabilized at 85% -90%, and NCu30-4-2-1 alloy ingot casting with uniform components is obtained.
Characterization of the microstructure of the as-cast Ce1 alloy. As shown in fig. 1, the XRD diffraction pattern of the Ce1 alloy is the same as that of the Ce0 alloy, and the Ce1 alloy has two phases, an alpha phase and a beta phase, which are both face-centered cubic structures; as shown in fig. 2 (b), the Ce1 alloy exhibits a dendrite morphology, both dendrites and inter-dendrites have a matrix α phase, a granular secondary β phase is dispersed and precipitated in the matrix, and the secondary β phase in the inter-dendrite region has a larger particle size, mainly because the inter-dendrite region has a higher Si element content, as shown in table 3. Similarly, eutectic (alpha+beta) phases exist among dendrites, black spots are clearly visible on the eutectic beta phases, the spots are eutectic alpha phases, and the size of the eutectic alpha phases is small, so that the analysis result of the energy spectrometer of the scanning electron microscope is greatly error due to size limitation, but the analysis result can show that two-phase components are different. In contrast, the composition analysis of the eutectic beta phase is more accurate, and the chemical analysis result shows that the beta phase is enriched in Ni and Si elements, but depleted in Cu, fe and Mn elements; the composition analysis error of the eutectic alpha phase is larger, but the Si content is obviously lower than that of the eutectic beta phase, as shown in Table 3. Compared with the Ce0 alloy, 0.01wt.% of Ce element is added into the Ce1 alloy, the structure of the alloy is thinned, and dendrite segregation can be reduced. In addition, the addition of Ce can improve the metallurgical quality of the alloy. The main reason is that Ce element plays a role of modifier in the alloy, and after entering alloy liquid, ce element reacts with O, N, S and the like rapidly to generate a high-melting-point rare earth Ce-rich compound, the compound remains solid in the solidification process, and part of the compound enters a slag phase to be removed, so that the aim of removing impurities is fulfilled, and the impurity is shown in a table 2; in addition, a part of fine high-melting-point compound particles remain in the alloy liquid and are dispersed, and the alloy liquid becomes crystalline alloy when being solidified, so that non-spontaneous crystal nuclei are generated in the crystallization process, and the structure is refined.
As shown in FIG. 3, from the tensile engineering stress-strain curve of Ce1 alloy, the tensile strength R of Ce1 alloy can be seen m 918MPa, yield strength R p0.2 The elongation after break A was 9.08% at 567 MPa. Compared with the tensile property of the Ce0 alloy, the tensile strength, the yield strength and the elongation after break of the Ce1 alloy are reduced. The main reason is that the dendrite area volume fraction in the Ce1 alloy is smaller (about 59% Ce0 and about 46% Ce 1), which reduces the tensile properties of the alloy.
Example 2
In this example, 10kg of an alloy, abbreviated as Ce3 alloy, was single-furnace smelted by adding 0.03wt.% of a rare earth element Ce0.03wt.% of a strengthening NCu30-4-2-1 alloy. Considering the burning loss of rare earth element Ce in smelting, 0.0375wt.% of Ce element is added in the process of proportioning, see table 1.
The preparation method of the NCu30-4-2-1 alloy comprises the following specific steps:
(1) Raw material selection: selecting Ni plates, cu plates, si blocks, fe rods, mn sheets, graphite and Ce blocks as raw materials, ensuring that the total carried-in O content of the raw materials is less than or equal to 0.020 percent and the S content is less than or equal to 0.0015 percent, and calculating and preparing raw materials of each element according to the component control requirement; all raw materials remove oxides, greasy dirt and impurities on the surface;
(2) And (2) charging: the Ce-containing NCu30-4-2-1 alloy was charged in batches. Charging in a first batch, and sequentially loading graphite, a Cu plate, a Ni plate and Fe blocks into a crucible; charging in a second batch, namely charging Si blocks and Mn sheets wrapped by nickel plates into a crucible; thirdly, charging in batches, and charging Ce blocks wrapped by nickel plates into a crucible;
(3) Melting period: the power transmission is started when the vacuum degree in the melting period is 8Pa, the power is gradually increased to 26kW in the early melting period of the first batch, so that after a molten pool is formed, the power supply is reduced to 20+/-1 kW of melting materials, and the melting period time is ensured to be 35min; after melting, heating to 1480 ℃ and entering a refining period;
(4) Refining period: controlling the vacuum degree to be 0.5Pa, the power to be 13kW in the refining period, controlling the refining temperature to be 1480 ℃, refining time to be 20min, controlling the O content to be less than or equal to 0.0050%, the N content to be less than or equal to 0.0020% and the S content to be less than or equal to 0.0015% in the melt, and then entering an alloying period;
(5) Alloying period: after refining, entering an alloying period, stopping power and forming a film, charging argon 30000Pa into a furnace, adding a second batch of materials into a melt, stirring for 5min with high power of 30kW, finally controlling the temperature of the melt to 1250 ℃, adding Ce blocks wrapped by nickel plates, stirring for 5min with high power of 30kW, and heating to 1360+/-10 ℃ for casting;
(6) Casting: the inner wall of the ingot casting mould is cleaned by a steel shovel and a steel brush, the residual steel slag and oxide skin are removed by compressed air, the casting temperature is 1360+/-10 ℃, a pouring cup with the inner diameter of a lower opening of phi 20mm is used for controlling the casting speed, the casting time of each ingot casting is ensured to be 40-60 s, the yield of Ce element is stabilized at 85% -90%, and NCu30-4-2-1 alloy ingot casting with uniform components is obtained.
Characterization of the microstructure of the as-cast Ce3 alloy. As shown in FIG. 1, the XRD diffraction pattern of the Ce3 alloy is the same as that of Ce0 and Ce1 alloys, and the Ce3 alloy has two phases, namely an alpha phase and a beta phase, which are both in a face-centered cubic structure; as shown in fig. 2 (c), the Ce3 alloy exhibits a dendrite morphology, both dendrites and inter-dendrites have a matrix α phase, a granular secondary β phase is dispersed and precipitated in the matrix, and the secondary β phase in the inter-dendrite region has a larger particle size, mainly because the inter-dendrite region has a higher Si element content, as shown in table 3. Similarly, eutectic (alpha+beta) phases exist among dendrites, black spots are clearly visible on the eutectic beta phases, the spots are eutectic alpha phases, and the size of the eutectic alpha phases is small, so that the analysis result of the energy spectrometer of the scanning electron microscope is greatly error due to size limitation, but the analysis result can show that two-phase components are different. In contrast, the composition analysis of the eutectic beta phase is more accurate, and the chemical analysis result shows that the beta phase is enriched in Ni and Si elements, but depleted in Cu, fe and Mn elements; the composition analysis error of the eutectic alpha phase is larger, but the Si content is obviously lower than that of the eutectic beta phase, as shown in Table 3. Compared with the Ce1 alloy, when the Ce3 alloy content reaches 0.03 wt%, the morphology of dendrite tissue is coarsened. The main reasons are as follows: the Ce element is added into the alloy, so that the Ce element is alloyed with other elements beneficial to heterogeneous nucleation to form a large amount of rare earth compounds which are gathered and enter a slag phase in a block form to be removed; in addition, more Ce elements are added, so that the supercooling effect of rare earth Ce atomic components is reduced, and the overdeterioration phenomenon occurs. Compared with the content of O, N in the Ce1 alloy, the content of more Ce element in the alloy can further remove harmful impurities in the alloy, and has important significance for improving the metallurgical quality of the alloy, as shown in Table 2.
As shown in FIG. 3, from the tensile engineering stress-strain curve of the Ce3 alloy, the tensile strength R of the Ce3 alloy can be seen m 923MPa, yield strength R p0.2 565MPa, and elongation after break A is 10.12%. Compared with the Ce1 alloy, the tensile strength and the elongation after fracture of the Ce3 alloy are improved, while the yield strength is almost unchanged, and the main reason is that the volume fraction (about 54%) of dendrite areas in the Ce3 alloy is improved.
Example 3
In this example, 10kg of an alloy, abbreviated as Ce6 alloy, was single-furnace smelted by adding 0.06wt.% of rare earth element Ce0.06 to toughen the NCu30-4-2-1 alloy. Considering the burning loss of rare earth element Ce in smelting, 0.075wt.% of Ce element is added in the batching, see Table 1.
The preparation method of the NCu30-4-2-1 alloy comprises the following specific steps:
(1) Raw material selection: selecting Ni plates, cu plates, si blocks, fe rods, mn sheets, graphite and Ce blocks as raw materials, ensuring that the total carried-in O content of the raw materials is less than or equal to 0.020 percent and the S content is less than or equal to 0.0015 percent, and calculating and preparing raw materials of each element according to the component control requirement; all raw materials remove oxides, greasy dirt and impurities on the surface;
(2) And (2) charging: the Ce-containing NCu30-4-2-1 alloy was charged in batches. Charging in a first batch, and sequentially loading graphite, a Cu plate, a Ni plate and Fe blocks into a crucible; charging in a second batch, namely charging Si blocks and Mn sheets wrapped by nickel plates into a crucible; thirdly, charging in batches, and charging Ce blocks wrapped by nickel plates into a crucible;
(3) Melting period: the power transmission is started when the vacuum degree in the melting period is 2Pa, the power is gradually increased to 30kW in the early melting period of the first batch, so that after a molten pool is formed, the power supply is reduced to 20+/-1 kW of melting materials, and the time in the melting period is ensured to be 45min; after melting, heating to 1520 ℃ to enter a refining period;
(4) Refining period: controlling the vacuum degree to be 1.0Pa, the power to be 17kW in the refining period, controlling the refining temperature to 1520 ℃ and the refining time to be 20min, and controlling the O content to be less than or equal to 0.0050%, the N content to be less than or equal to 0.0020% and the S content to be less than or equal to 0.0015% in the melt and then entering an alloying period;
(5) Alloying period: after refining, entering an alloying period, stopping power and forming a film, charging argon gas 40000Pa into a furnace, adding a second batch of materials into a melt, stirring for 5min under high power, finally controlling the temperature of the melt to 1300 ℃, adding Ce blocks wrapped by nickel plates, stirring for 5min under high power, heating to 1360+/-10 ℃ and casting;
(6) Casting: the inner wall of the ingot casting mould is cleaned by a steel shovel and a steel brush, the residual steel slag and oxide skin are removed by compressed air, the casting temperature is 1360+/-10 ℃, a pouring cup with the inner diameter of a lower opening of phi 20mm is used for controlling the casting speed, the casting time of each ingot casting is ensured to be 40-60 s, the yield of Ce element is stabilized at 85% -90%, and NCu30-4-2-1 alloy ingot casting with uniform components is obtained.
Characterization of the microstructure of the as-cast Ce6 alloy. As shown in FIG. 1, the XRD diffraction pattern of the Ce6 alloy is the same as that of Ce0, ce1 and Ce3 alloys, and the Ce6 alloy has two phases, namely an alpha phase and a beta phase, which are both in a face-centered cubic structure; as shown in fig. 2 (d), the Ce6 alloy exhibits a dendrite morphology, both dendrites and inter-dendrites have a matrix α phase, a granular secondary β phase is dispersed and precipitated in the matrix, and the secondary β phase in the inter-dendrite region has a larger particle size, mainly because the inter-dendrite region has a higher Si element content, as shown in table 3. Similarly, eutectic (alpha+beta) phases exist among dendrites, black spots are clearly visible on the eutectic beta phases, the spots are eutectic alpha phases, and the size of the eutectic alpha phases is small, so that the analysis result of the energy spectrometer of the scanning electron microscope is greatly error due to size limitation, but the analysis result can show that two-phase components are different. In contrast, the composition analysis of the eutectic beta phase is more accurate, and the chemical analysis result shows that the beta phase is enriched in Ni and Si elements, but depleted in Cu, fe and Mn elements; the composition analysis error of the eutectic alpha phase is larger, but the Si content is obviously lower than that of the eutectic beta phase, as shown in Table 3. Compared with Ce1 and Ce3 alloys, when the Ce content of the series of alloys reaches 0.06 wt%, the dendrite structure coarsens again, and even exceeds the Ce0 alloy without adding Ce element. The main reasons are as follows: the addition of a large amount of Ce element to the alloy allows the Ce element to be alloyed with other elements beneficial to heterogeneous nucleation to form a large amount of rare earth compounds which are gathered and enter a slag phase in a block form to be removed; in addition, a large amount of Ce elements are added, so that the supercooling effect of rare earth Ce atomic components is reduced, and the phenomenon of overdeterioration occurs. Comparing the O, N content of Ce1, ce3 and Ce6 alloy, the increase of Ce element can further remove harmful impurity in alloy, and improve metallurgical quality of alloy, see table 2.
As shown in FIG. 3, from the tensile engineering stress-strain curve of Ce6 alloy, the tensile strength R of Ce6 alloy can be seen m 979MPa yield strength R p0.2 584MPa, and the elongation after break A is 13.46%. Compared with the tensile properties of Ce1 and Ce3 alloys, the tensile strength, yield strength and elongation after fracture of the Ce6 alloy are improved, and the main reason is that the volume fraction (about 63%) of dendrite regions in the Ce6 alloy is the largest.
In conclusion, the invention determines the feeding mode and the smelting process, and improves the yield of the rare earth element Ce. By adjusting the Ce content of the rare earth element, impurities and refined structures are effectively removed under the condition of not changing the phase types, so that the NCu30-4-2-1 alloy obtains good strength and plasticity matching. The research shows that the tensile property of the series of NCu30-4-2-1 alloys is mainly determined by the volume fraction of dendrite areas, and the higher the volume fraction is, the better the comprehensive tensile property of the alloy is; along with the increase of the content of Ce element, the O, N content of the alloy is reduced, and the metallurgical quality of the alloy is improved.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solution of the present invention, and not limiting thereof; although the 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 scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (6)
1. A preparation method of an NCu30-4-2-1 alloy strengthened by adding a rare earth element Ce is characterized in that the NCu30-4-2-1 alloy comprises the following components in percentage by weight: less than or equal to 0.03 percent of C, 30 to 32 percent of Cu, 3.9 to 4.3 percent of Si, 1.5 to 2.8 percent of Fe, 0.5 to 1.5 percent of Mn, 0.01 to 0.06 percent of Ce, and the balance of Ni and unavoidable impurity elements; in the impurity elements, the content of O is less than or equal to 0.0030 percent, the content of N is less than or equal to 0.0010 percent, and the content of S is less than or equal to 0.0015 percent;
the preparation method specifically comprises the following steps:
(1) Raw material selection: selecting a Ni plate, a Cu plate, a Si block, a Fe rod, a Mn sheet, a graphite rod and a Ce block as raw materials, and calculating and preparing raw materials of each element according to the component control requirement;
(2) And (2) charging: for the NCu30-4-2-1 alloy containing Ce, batch charging is carried out according to the factors of the melting point, the easy oxidation degree, the density, the adding quantity and the easy volatility of the raw materials; charging in a first batch, and sequentially loading graphite, a Cu plate, a Ni plate and Fe blocks into a crucible; charging in a second batch, and sequentially loading Si blocks and Mn sheets wrapped by nickel plates into a crucible; thirdly, charging in batches, and charging Ce blocks wrapped by nickel plates into a crucible;
(3) Melting period: when the vacuum degree in the melting period is less than or equal to 10Pa, power transmission is started, the power is gradually increased to 25-30 kW in the early melting period of the first batch, so that after a molten pool is formed, the power supply is reduced to 20+/-1 kW of melting materials, and the melting period time is ensured to be 35-45 min; after melting, heating to 1480-1520 ℃ and entering a refining period;
(4) Refining period: controlling the vacuum degree to be 0.5-1.0 Pa in the refining period, controlling the power range to be 13-17 kW, controlling the refining temperature to be 1480-1520 ℃ and the refining time to be 15-25 min;
(5) Alloying period: after refining, entering an alloying period, stopping power and forming a film, charging argon 30000-40000 Pa into a furnace, adding a second batch of materials into a melt, stirring for 4-6 min under high power, finally controlling the temperature of the melt to 1250-1300 ℃, adding a third batch of materials, stirring for 4-6 min under high power, heating to 1360+/-10 ℃ and casting;
(6) Casting: the inner wall of the ingot casting mould is cleaned by a steel shovel and a steel brush, the residual steel slag and oxide skin are removed by compressed air, the casting temperature is 1360+/-10 ℃, a pouring cup with the inner diameter of a lower opening of phi 20mm is used for controlling the casting speed, the casting time of each ingot casting is ensured to be 40-60 s, the yield of Ce element is stabilized at 85% -90%, and the ingot casting with high purity and uniform components is obtained.
2. The method for producing a tough NCu30-4-2-1 alloy by adding rare earth element Ce according to claim 1, wherein in step (1), the total O content of the raw material is 0.020% or less and the S content is 0.0015% or less.
3. The method for producing a tough NCu30-4-2-1 alloy by adding a rare earth element Ce according to claim 1, wherein in step (1), all the raw materials are freed from surface oxides, oil stains and impurities.
4. The method for producing a reinforced NCu30-4-2-1 alloy by adding a rare earth element Ce according to claim 1, wherein in the step (1), the raw material is an industrially pure Si block or Mn piece, and the raw material purity of the remaining alloying elements is not lower than 99.9wt.%.
5. The method for producing a tough NCu30-4-2-1 alloy by adding a rare earth element Ce according to claim 1, wherein the melt is controlled to have O content of 0.0050%, N content of 0.0020% or less and S content of 0.0015% or less after the melting phase in step (3) and the refining phase in step (4) and then the alloy is alloyed.
6. The method for producing a tough NCu30-4-2-1 alloy by adding a rare earth element Ce according to claim 1, wherein the high power in step (5) is 30kW.
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