CN117737486A - Manufacturing method of electrode blank for Ni-Cr-Mo based alloy electroslag remelting - Google Patents
Manufacturing method of electrode blank for Ni-Cr-Mo based alloy electroslag remelting Download PDFInfo
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Abstract
The invention discloses a manufacturing method of an electrode blank for Ni-Cr-Mo based alloy electroslag remelting, which adopts a smelting process of a non-vacuum induction furnace, an LF furnace and a VOD furnace, wherein the large-tonnage non-vacuum induction furnace has relatively loose requirements on raw material gas, carbon, silicon and impurity sulfur entering the furnace except strict requirements on raw material impurity phosphorus, has relatively low cost, is carried out at normal temperature and normal pressure, is relatively simple, convenient and rapid to operate, and has relatively high production efficiency. The purposes of decarburization, desilication, accurate control of alloy components and reduction of gas content are realized by utilizing LF furnace alloying and adopting two-step operation and refining function of VOD furnace. The invention has the beneficial effects that: an electrode blank for electroslag remelting of a low-gas-content low-carbon low-silicon Ni-Cr-Mo-based superalloy with the successful smelting hydrogen content of not more than 0.0002%, the oxygen content of not more than 0.0015%, the nitrogen content of not more than 0.0050%, the carbon content of not more than 0.008% and the silicon content of not more than 0.06%.
Description
Technical Field
The invention belongs to the field of corrosion-resistant alloy manufacturing, and particularly relates to a manufacturing method of an electrode blank for electroslag remelting of a Ni-Cr-Mo-based alloy, which is low in alloy gas, carbon and silicon content.
Background
The alloy is a Ni-Cr-Mo-based high-temperature alloy with low gas, low carbon and low silicon content, and still has a single face-centered cubic structure, namely a gamma structure under the condition that the alloy contains a large amount of Cr, mo and other elements. The low carbon (w (C) is less than or equal to 0.01 percent) can reduce the precipitation quantity of carbide in the alloy, and the low silicon (w (Si) is less than or equal to 0.08 percent) can reduce the precipitation quantity of intermetallic phases in the alloy, thereby improving the intergranular corrosion resistance of the alloy. The alloy has stronger corrosion resistance in both oxidizing medium and reducing medium, and is not only resistant to hypochlorite, wet chlorine, oxidizing chloride and chloride salt solution corrosion, but also resistant to corrosion by heat-resistant concentrated sulfuric acid solution, and is called as universal corrosion resistant alloy; is suitable for harsh medium environments in a plurality of fields such as nuclear fuel production, chemical manufacturing, flue gas desulfurization, papermaking, ocean development and the like. The alloy has high molybdenum content (w (Mo): 15% -17%) and poor plasticity, and the gas content is required to be low in order to improve forging plasticity; because of low silicon, the use requirement on deoxidizing elements is more severe; the low carbon has strict requirements on the carbon content in the raw materials and auxiliary materials, and if the quality control of the alloy electrode is not good, electroslag smelting is difficult to obtain an electroslag ingot with qualified components and stable quality. In order to ensure that alloy components and gases are qualified, the alloy is produced by adopting a vacuum induction smelting and vacuum consumable remelting or vacuum induction smelting and electroslag remelting process. The vacuum induction furnace smelting is carried out under high vacuum, so that the components and the gases are relatively stable, but the vacuum induction furnace has strict requirements on the oxygen, nitrogen and other gas contents of raw materials to be fed, the carbon and silicon contents, the sulfur and phosphorus contents of impurities, the surface quality and the like, and the raw material cost is relatively high; in addition, because the crucible of the vacuum induction furnace is relatively smaller, the iron loading times are more, the process seasoning, temperature measurement, sampling and the like are required to be repeatedly vacuumized on the charging chamber, the single-furnace smelting time is long, the production efficiency is relatively low, and the ton steel production cost is relatively high.
Disclosure of Invention
The invention discloses a manufacturing method of an electrode blank for Ni-Cr-Mo based alloy electroslag remelting, which solves the problems that the smelting cost of a vacuum induction furnace is high, the electrode blank for Ni-Cr-Mo based alloy electroslag remelting with low gas, low carbon and low silicon content is smelted under the atmosphere of the non-vacuum induction furnace, the degassing is difficult, the smelting control difficulty of carbon and silicon elements with narrow standard specifications is high, and the like by adopting a smelting process of a non-vacuum induction furnace, an LF furnace and a VOD furnace, so that a Ni-Cr-Mo based alloy electroslag remelting electrode with low gas content and qualified carbon and silicon elements is obtained.
The following process procedures are adopted to achieve the purposes: preparing materials, melting materials in a non-vacuum induction furnace, alloying in an LF furnace, refining in a VOD furnace, pouring and checking the result.
The specific technical scheme is as follows:
1. the chemical components (mass percent,%) of the electrode blank for alloy electroslag remelting are controlled: carbon no greater than 0.01, manganese no greater than 1.00, silicon no greater than 0.08, phosphorus no greater than 0.04, sulfur no greater than 0.03, chromium: 14.5 to 16.5, molybdenum: 15.0 to 17.0, iron: 4.0 to 7.0, cobalt is not more than 2.5, tungsten: 3.0 to 4.5, vanadium not more than 0.35, hydrogen not more than 2X 10 -6 Oxygen is not more than 15×10 -6 Nitrogen is not more than 50X 10 -6 The balance being nickel.
2. Melting materials in a non-vacuum induction furnace;
alloy return materials with the same or similar components, metal chromium, metal molybdenum, molybdenum iron, metal tungsten, tungsten iron, nickel plates and the like are selected as raw materials and melted into liquid in a non-vacuum induction furnace; sampling and full analysis are carried out when the temperature of molten steel is not lower than 1600 ℃, and the components meet the control targets (mass percent): carbon: 0.30 to 0.60 percent of chromium: 14.5 to 16.5, molybdenum: 15.0 to 17.0 percent, tungsten: 3.0 to 4.5, iron: 4.0-6.5, the temperature of molten steel is not lower than 1650 ℃ and tapping can be carried out.
LF furnace alloying:
firstly, after the non-vacuum induction furnace is discharged, the ladle is transported to an LF furnace, and oxygen blowing operation is carried out by adopting an oxygen blowing pipe according to silicon components in the furnace, so that the silicon content in the steel is reduced, and the silicon content is ensured to be not more than 0.06%.
Secondly, after oxygen-blown silicon is properly contained, slag skimming is carried out, carbon powder deoxidization and reduction are adopted, components are regulated, and the components meet control targets (mass percent): carbon: 0.30 to 0.60 percent of chromium: 15.0 to 16.2, molybdenum: 15.1 to 16.0, tungsten: 3.1 to 3.8, iron: 5.5 to 6.5, silicon is not more than 0.06, and steel can be tapped when the temperature of molten steel is not lower than 1700 ℃.
Refining in a VOD furnace:
the method comprises the steps of blowing oxygen to remove carbon, wherein the ultimate vacuum degree is not higher than 67Pa, the argon flow is not less than 40L/min during oxygen blowing, the stirring effect is ensured, the sampling carbon is not more than 0.008%, and deoxidization operation can be performed;
after oxygen blowing is finished, adding 10 kg/t-12 kg/t of high-quality lime and 8 kg/t-10 kg/t of high-quality fluorite, wherein in order to avoid the increase of the carbon content in molten steel, the carbon content in the high-quality lime is required to be not more than 0.25%; adding 4 kg/t-6 kg/t of aluminum block for deoxidization, vacuumizing to not higher than 67Pa, maintaining the argon flow to not lower than 40L/min for 15min, and performing deoxidization and reduction operation to ensure that aluminum is sampled after deoxidization: 0.10 to 0.16 percent.
Adding metal calcium and metal cerium for final deoxidization after aluminum deoxidization, adding 0.2kg/t of metal cerium, adding 0.05kg/t of metal calcium, and hanging out and casting at the temperature of 1510-1540 ℃.
5. Pouring:
pouring by adopting a pouring pit and a lifting vehicle for at least 30min before pouring, filling argon into the ingot mould and the middle pouring pipe, pouring molten steel under the protection of argon, demoulding for 30min after pouring at 1510-1540 ℃, and then air-cooling to room temperature.
The innovation points of the invention are as follows:
besides strict requirements on raw material impurity phosphorus, the large-tonnage non-vacuum induction furnace has relatively loose requirements on raw material gas, carbon, silicon, impurity sulfur, surface quality and the like, the raw material cost is relatively low, and the charging, temperature measurement, seasoning, sampling and the like are all carried out at normal temperature and normal pressure, so that the operation is relatively simple, convenient and quick, and the production efficiency is relatively high. However, because the non-vacuum induction furnace does not have a molten steel refining system such as an argon stirring system, a vacuum system and the like, alloy components are difficult to accurately control and the removal of hydrogen, oxygen and nitrogen gases is difficult, and the non-vacuum induction furnace has no decarburization and desilication capabilities, the purposes of decarburization, desilication, accurate control of alloy components and reduction of gas content are realized by utilizing the alloying of the LF furnace and the refining function of the VOD furnace.
1. Control of non-vacuum induction furnace material melting process parameters
Controlling tapping components (mass percent,%) of the non-vacuum induction furnace: carbon: 0.30 to 0.60 percent of chromium: 14.5 to 16.5, molybdenum: 15.0 to 17.0 percent, tungsten: 3.0 to 4.5, iron: 4.0 to 6.5 and other elements meet the standard requirements; before tapping, the main elements such as carbon, chromium, molybdenum, tungsten, iron and the like are controlled within the specification range.
Technological parameter control by adopting two-step operation method for LF furnace alloying
The method comprises the steps of firstly carrying out oxygen blowing operation after molten steel enters an LF furnace, and requiring that silicon in the molten steel is not more than 0.06%.
The LF furnace deoxidization and reduction operation can well desulfurize, so that the desulfurization pressure in the deoxidization and reduction period of the VOD furnace is reduced.
Thirdly, controlling tapping components (mass percent,%) of the LF furnace: chromium: 15.0 to 16.2, molybdenum: 15.1 to 16.0, tungsten: 3.1 to 3.8, iron: 5.5 to 6.0 percent, avoiding the readjustment of components in the VOD furnace, controlling the carbon according to 0.30 to 0.60 percent, effectively ensuring the sufficient carbon-oxygen reaction of the VOD furnace and improving the capability of removing hydrogen and nitrogen of the VOD furnace; the tapping temperature is above 1700 ℃, so that the secondary heating of VOD is avoided, the smelting time is long, and carbon in molten steel rises.
Control of VOD furnace Process parameters
The method has the advantages that the flow and the vacuum degree of argon are controlled during oxygen blowing, so that the carbon and oxygen in molten steel can react uniformly and fully, and the removal of carbon and gas hydrogen and nitrogen contents is facilitated.
The aluminum block is adopted for deoxidizing, the aluminum block is added at one time, deoxidizing is carried out according to the ratio of 4kg/t to 6kg/t, and meanwhile aluminum in molten steel is controlled to be 0.10% -0.16%, so that the deoxidizing effect of the molten steel can be ensured, and silicon in slag is prevented from exceeding the standard requirement due to reduction of silicon (SiO2+Al=Al2O3+Si) in the molten steel due to high aluminum content.
Controlling the argon gas flow, the extreme vacuum degree and the time kept under the extreme vacuum degree during deoxidation, so that the uniform and sufficient reduction reaction can be ensured, and the further removal of the hydrogen and nitrogen gas is facilitated; the high-quality white ash used in slag formation during reduction is 10 kg/t-12 kg/t, and the carbon content in the white ash is not more than 0.25%, so that the carbon expansion of molten steel is prevented and exceeds the standard requirement.
After deoxidizing, the ingredients are forbidden to be adjusted, firstly, the aim is to prevent the carbon content in the molten steel from rising due to the delay of material selection, weighing and charging time; secondly, the risk of silicon rising and carbon rising caused by reheating due to the fact that the temperature of molten steel is lower than the pouring temperature due to charging is prevented; and thirdly, preventing trace carbon in the metal material from being carried into molten steel. Adding aluminum for deoxidization, adding metal cerium and metal calcium for final deoxidization, adding 0.2kg/t of metal cerium, 0.05kg/t of metal calcium, and finally measuring the temperature and pouring.
4. Casting process control
The method has the advantages that the 1510-1540 ℃ casting is adopted for casting of the alloy, so that the fluidity of molten steel during casting can be guaranteed, and the quality risks of molten steel suction and refractory material inclusion erosion and the like can be reduced.
The argon is filled into the steel ingot mould 30min in advance before casting, measures such as argon protection casting are taken during casting, air suction during molten steel casting can be effectively reduced, and risks that the air does not meet standard requirements are reduced.
The invention has the beneficial effects that: by controlling the non-vacuum induction furnace melting material, the LF furnace alloying adopts a two-step method operation, the VOD furnace refining reasonably controls oxygen blowing and deoxidizing operation, adopts the implementation of measures such as argon filling in advance in a steel ingot mould, argon protection during casting and the like, and finally successfully smelts the electrode blank for the electroslag remelting of the low-gas-content low-carbon low-silicon Ni-Cr-Mo-based superalloy with the hydrogen content of not more than 0.0002%, the oxygen content of not more than 0.0015%, the nitrogen content of not more than 0.0050%, the carbon content of not more than 0.008% and the silicon content of not more than 0.06%.
Detailed Description
The present invention will be further specifically described with reference to three examples.
The furnace charge amounts of the examples were respectively: example 1:31.25t, example 2:32.7t, example 3:32.79t.
1. Tapping chemical composition and tapping temperature of the non-vacuum induction furnace:
the chemical composition (mass percent,%) of the tapping of a non-vacuum induction furnace is shown in table 1.
TABLE 1
The tapping temperature of the non-vacuum induction furnace is respectively: example 1:1662 ℃; example 2:1658 ℃; example 3:1660 ℃.
The LF furnace production process and tapping components are as follows:
the silicon composition (mass%) of the three examples after the oxygen blowing operation of the LF furnace is shown in table 2.
TABLE 2
| Batch of | Si |
| Example 1 | 0.05 |
| Example 2 | 0.03 |
| Example 3 | 0.04 |
After the deoxidizing operation of the LF furnace, the steel tapping components (mass percent,%) of the three embodiments are shown in Table 3.
TABLE 3 Table 3
Third, tapping temperatures of the LF furnace in the three embodiments are respectively as follows: example 1:1728 deg.C; example 2:1731 ℃; example 3:1725 ℃.
VOD furnace technological parameters
The main technological parameters of oxygen blowing and carbon removing operation of the VOD furnace are shown in table 4, the main technological parameters of reduction operation of the VOD furnace are shown in table 5, and the carbon content and final deoxidization adding amount of lime for slag formation of the VOD furnace are shown in table 6.
TABLE 4 Table 4
| Batch of | Argon flow (L/min) | Ultimate vacuum degree (Pa) | Endpoint carbon content (%) |
| Example 1 | 55 | 67 | 0.005 |
| Example 2 | 55 | 67 | 0.004 |
| Example 3 | 65 | 67 | 0.005 |
TABLE 5
TABLE 6
4. Casting process parameters
The main technological parameters of the pouring operation are shown in Table 7.
TABLE 7
5. Finished product component
The chemical composition (mass percent,%) of the finished electrode blank for alloy electroslag remelting is shown in Table 8, and the gas content (x 10) of the electrode blank for alloy electroslag remelting -6 ) See table 9.
TABLE 8
TABLE 9
| — | Hydrogen gas | Oxygen gas | Nitrogen and nitrogen |
| Standard requirements | ≤2 | ≤15 | ≤50 |
| Example 1 | 1.1 | 9 | 42 |
| Example 2 | 1.0 | 11 | 46 |
| Example 3 | 1.0 | 10 | 45 |
Claims (1)
1. The manufacturing method of the electrode blank for the electroslag remelting of the Ni-Cr-Mo based alloy is characterized by comprising the following steps of: preparing materials, melting materials in a non-vacuum induction furnace, alloying in an LF furnace, refining in a VOD furnace, pouring and checking results;
the chemical composition of the electrode blank for alloy electroslag remelting is controlled: carbon not greater than 0.01%, manganese not greater than 1.00%, silicon not greater than 0.08%, phosphorus not greater than 0.04%, sulfur not greater than 0.03%, chromium: 14.5 to 16.5 percent, molybdenum: 15.0 to 17.0 percent, iron: 4.0 to 7.0 percent, cobalt is not more than 2.5 percent, tungsten: 3.0 to 4.5 percent, vanadium is not more than 0.35 percent, and hydrogen is not more than 2 multiplied by 10 -6 Oxygen is not more than 15×10 -6 Nitrogen is not more than 50X 10 -6 The balance being nickel;
the material preparation and non-vacuum induction furnace material melting are carried out: alloy return materials with the same or similar components, metal chromium, metal molybdenum, molybdenum iron, metal tungsten, tungsten iron, nickel plates and the like are selected as raw materials and melted into liquid in a non-vacuum induction furnace; sampling and full analysis are carried out when the temperature of molten steel is not lower than 1600 ℃, and the components meet the control targets: carbon: 0.30 to 0.60 percent of chromium: 14.5 to 16.5 percent, molybdenum: 15.0 to 17.0 percent of tungsten: 3.0 to 4.5 percent of iron: 4.0 to 6.5 percent, and tapping can be carried out when the temperature of molten steel is not lower than 1650 ℃;
alloying the LF furnace: according to the silicon components in the furnace, an oxygen blowing pipe is adopted for oxygen blowing operation, so that the silicon content in steel is reduced, and silicon is ensured to be not more than 0.06%; after the oxygen-blown silicon components are proper, slag skimming is carried out, carbon powder deoxidization and reduction are adopted, the components are adjusted, and the components meet control targets: carbon: 0.30 to 0.60 percent of chromium: 15.0 to 16.2 percent of molybdenum: 15.1 to 16.0 percent of tungsten: 3.1 to 3.8 percent of iron: 5.5 to 6.5 percent, silicon is not more than 0.06 percent, and steel can be tapped when the temperature of molten steel is not lower than 1700 ℃;
refining the VOD furnace: the method comprises the steps of blowing oxygen to remove carbon, wherein the ultimate vacuum degree is not higher than 67Pa, the argon flow is not less than 40L/min during oxygen blowing, and the sampling carbon is not more than 0.008%, so that deoxidization operation can be performed; adding 10 kg/t-12 kg/t of high-quality lime and 8 kg/t-10 kg/t of high-quality fluorite after oxygen blowing is finished, wherein the carbon content in the high-quality lime is required to be not more than 0.25%; adding 4 kg/t-6 kg/t of aluminum block for deoxidization, vacuumizing to 67Pa or less, maintaining the argon flow at 40L/min or less for 15min, performing deoxidization and reduction operation, and sampling aluminum after deoxidization: 0.10 to 0.16 percent; thirdly, after aluminum is added for deoxidization, cerium metal is added according to 200g/t, calcium metal is added according to 50g/t for final deoxidization, and casting is carried out at 1510-1540 ℃.
And (3) pouring: argon is filled into the ingot mould and the middle injection pipe at least 30min before casting, casting is carried out by adopting a casting pit and a lifting car, casting temperature is 1510-1540 ℃, demoulding is carried out 30min after casting, and then air cooling is carried out to room temperature.
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