CN109112319B - Slag for nuclear-grade stainless steel electroslag remelting and method for electroslag remelting by using slag - Google Patents
Slag for nuclear-grade stainless steel electroslag remelting and method for electroslag remelting by using slag Download PDFInfo
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- 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
- C22B9/16—Remelting metals
- C22B9/18—Electroslag remelting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention relates to slag for nuclear-grade stainless steel electroslag remeltingThe slag comprises CaF as the component in percentage by weight2 40～70%、MgF2 1～10%、Al2O310-20% of CaO, 10-20% of MgO, 1-10% of BaO and 0-3% of BaO; the electroslag ingot preparation method mainly comprises the following steps: electrode bar preparation → slag preparation → electroslag remelting. The electroslag ingot prepared by the method has the advantages of low content of harmful elements such as Co, B, Pb, Sn, H, P, S and the like, good surface quality, uniform components, less segregation, fine and compact structure, and less than or equal to 2.0-level total non-metallic inclusions, and meets the metallurgical quality requirement of nuclear-grade stainless steel.
Description
Technical Field
The invention relates to a smelting method, in particular to slag for nuclear-grade stainless steel electroslag remelting and a method for electroslag remelting by adopting the slag.
Background
Electroslag remelting is a process of melting, refining and solidifying and forming a metal consumable electrode in a crystallizer by using resistance heat generated by liquid slag. The electroslag steel has the advantages of pure metal, compact structure, uniform components, excellent performance and the like, and the electroslag remelting technology is an important means for producing special alloy materials from the generation to the present.
Slag is an important raw material essential to the field of electroslag metallurgy, and the metallurgical quality of a final product is determined by the slag formula and the using method.
The electroslag remelting process technology comprises an electrical system, a slag system, a temperature system, a speed system, a starting technology, an electrode replacement technology, a stripping technology, a high-uniformity control technology, a low-hydrogen control technology, a low-oxygen control technology, a low-aluminum control technology, a slag analysis technology, a molten pool detection technology and the like, and the technologies are gradually optimized and improved and become more mature along with the improvement of equipment technologies and the accumulation of practical data.
Hydrogen is one of the main reasons for forging scrap and is often scrapped in batches, and once scrap occurs, the economic loss is large. It is generally required that the hydrogen content in the steel does not exceed 2ppm, and when the hydrogen content is too high, it is usually necessary to perform dehydrogenation annealing for a long time, thereby greatly increasing the cost. In the electroslag ingot smelted by the conventional method, the hydrogen content is usually over 2 ppm.
The uniformity is one of the main problems of metallurgical quality control, and electroslag ingots prepared by the common method usually have increased carbon content at the bottom and reduced contents of elements such as silicon, titanium, aluminum and the like, so that the components of the steel ingots are not uniform. On the other hand, in the electroslag remelting process, the decomposition of some components of the molten slag can cause the change of slag components, so that the metallurgical property and the process property of the molten slag are changed, and finally, the element distribution of the part of the ingot in the high direction is not uniform. The steel ingot has uneven components, which can cause uneven structure and performance of the final product, and can not be used in serious cases, thus causing product rejection.
At present, nuclear grade stainless steel produced by part of manufacturers has poor metallurgical quality, so that scrapping is caused sometimes, for example, the content of harmful elements exceeds the standard, nonmetallic inclusions exceed the standard, shrinkage cavities are serious, the content of the harmful elements is high, so that the performance is deteriorated, the uniformity of components is poor, so that the uniformity of the performance is poor or the performance is unqualified. The electroslag remelting technology is not over-closed or has not been subjected to an electroslag remelting process.
Disclosure of Invention
The invention aims to provide slag for nuclear-grade stainless steel electroslag remelting and a method for electroslag remelting by adopting the slag, and an electroslag ingot prepared by adopting the method has the advantages of low content of harmful elements such as Co, B, Pb, Sn, H, P, S and the like, good surface quality, uniform components, less segregation, fine and compact structure and less than or equal to 2.0-grade total non-metallic inclusions.
The technical scheme of the invention is as follows:
the slag used for the nuclear grade stainless steel electroslag remelting method comprises the components of CaF in percentage by weight2 40～70％、MgF2 1～10％、Al2O3 10～20％、CaO 10～20％、MgO 1～10％、BaO 0～3％，The slag charge has industrial purity, and [ Co ]]+[Nb]+[Ta]≤0.2％、[B]≤0.01％。
The better technical scheme is that the slag comprises the following components in percentage by weight: CaF2 55～60％、MgF2 6～8％、Al2O3 12～16％、CaO 10～15％、MgO 6～7％、BaO 0.5％。
Of the above slag components, MgF28-15% of MgO, 13-20% of CaO + BaO, and the content of CaO + BaO + MgO is not less than Al2O3The content of (a).
The nuclear grade stainless steel electroslag remelting method comprises the following steps:
1) electrode rod preparation
A vacuum ingot smelted by a vacuum induction smelting furnace is used as an electrode bar, oxide skin on the surface of the electrode bar is removed, and the electrode bar is welded with a false electrode;
2) slag preparation
Taking the components of the slag according to the proportion, baking the slag, uniformly mixing, gradually adding the slag into a crystallizer, electrifying to melt slag, continuously electrifying for 5-10 minutes after the slag is completely molten, then powering off, cooling the slag to room temperature, breaking the slag, and uniformly mixing to obtain pre-melted slag;
3) electroslag remelting
Gradually adding the pre-melted slag obtained in the step 2) into a crystallizer, melting the slag by using the electrode rod prepared in the step 1), adding a variable valence oxide after the pre-melted slag is melted, inserting the electrode rod, moving the electrode rod up and down for 3-5 times, stirring, and electrifying for remelting to obtain the nuclear-grade stainless steel electroslag ingot.
The shape of the cross section of the electrode rod in the step 1) corresponds to the shape of the cross section of the crystallizer.
The voltage and current corresponding to the specification of the crystallizer are as follows: 1) phi 300mm crystallizer: the voltage is 50-55V, and the current is 7000-9000A; 2) phi 600mm crystallizer: the voltage is 55-60V, and the current is 10000-15000A.
And 2) electrifying the slag under the voltage of 30-55V and at the current of 3000-6000A.
Step 2) baking the slag charge, wherein CaF2、MgF2、Al2O3、MgOThe BaO baking system is 600-900 ℃ multiplied by 4-6 h, and the CaO baking system is 900-950 ℃ multiplied by 6-8 h.
And in the step 3), the valence-variable oxide is one or more of MnO2, MnO, TiO2 and rare earth oxide, the dosage of the valence-variable oxide is 0.5-3% of the weight of the slag charge, and the purity of the valence-variable oxide is analytically pure.
The rare earth oxide is cerium oxide or yttrium oxide.
And 3) the speed of vertically moving the electrode rod is 5-30 mm/S.
And 3) the nuclear grade stainless steel electroslag ingot has the following characteristics that [ O ] is less than or equal to 20ppm, [ H ] is less than or equal to 2ppm, [ P ] is less than or equal to 60ppm, [ S ] is less than or equal to 10ppm, [ Co ] is less than or equal to 0.1%, and [ B ] is less than or equal to 0.005%.
And 3) electrifying and remelting, and selecting voltage and current according to the specification of the crystallizer.
The purity of the slag is industrial purity, and the [ Co ] + [ Nb ] + [ Ta ] in the slag is less than or equal to 0.2 percent, and the [ B ] is less than or equal to 0.01 percent.
The electrode bar in the step 1) can not contact with water, and if the electrode bar contacts with the water, baking is carried out at 200 ℃ for 4 h.
The total amount of non-metallic inclusions in the nuclear-grade stainless steel prepared by the electroslag ingot is less than or equal to 2.0 grade.
The chemical composition of the electrode bar is consistent with that of a finished electroslag ingot.
Compared with the conventional method, the nuclear-grade stainless steel electroslag ingot prepared by the method has the advantages of low content of harmful elements, uniform components, fine and compact structure, good surface quality, less segregation, less non-metallic inclusions, small size and uniform distribution, and can meet the requirement of the nuclear power field on the metallurgical quality of the stainless steel material.
In the slag charge of the invention, the main components have the following functions:
(1) CaF 2: can reduce the melting point, viscosity and surface tension of the slag. But the conductivity of CaF2 was higher compared to the other components.
(2) CaO: the slag alkalinity is increased by adding CaO into the slag, the desulfurization efficiency is improved, and the conductivity of the slag can be reduced by adding CaO. However, CaO has strong water absorption and is easy to carry hydrogen and oxygen, so that the steel is increased in hydrogen and oxygen, and therefore, the steel needs to be baked at high temperature before use.
(3) Al2O 3: can obviously reduce the conductivity of the slag, reduce the power consumption and improve the productivity. However, the increase of Al2O3 in the slag will increase the melting temperature and viscosity of the slag and will reduce the desulfurization effect of the slag, and in addition, the remelting process is difficult to establish and stabilize.
(4) MgO: the slag contains proper MgO, so that a layer of semi-solidified film is formed on the surface of the slag pool, the hydrogen absorption of the slag pool can be prevented, and the oxygen supply of the slag to the metal molten pool by the valence oxide can be prevented, thereby reducing the contents of oxygen, hydrogen and nitrogen in the cast ingot. Meanwhile, the solidified film can reduce the heat loss of the slag surface to the atmosphere radiation. However, MgO tends to increase the viscosity of the slag.
(5) MgF 2: similar to CaF2, the slag modifier is used as an auxiliary agent, so that the melting point of the slag is greatly reduced, and the viscosity, the surface tension and the conductivity of the slag can also be reduced.
(6) BaO: the alkalinity of the slag is improved, and the content of P, S elements in the steel is reduced.
According to the method, the variable valence oxide can balance C, O, H elements in a slag pool in the remelting process, so that the content of harmful elements is reduced, and the uniformity is improved.
The invention improves the component uniformity of the electroslag ingot, eliminates the metallurgical defects of porosity, air holes and the like, reduces the contents of harmful elements such as Co, B, Pb, Sn, H, P, S and the like and meets the metallurgical quality requirement of the nuclear grade stainless steel by controlling the aspects of an electrical system, a slag system, raw materials, a process flow and the like.
Detailed Description
EXAMPLE 1 preparation of 316L stainless Steel electroslag ingot
1) Electrode rod preparation
Smelting by adopting a 500kg vacuum induction smelting furnace, pouring the molten steel shown in the table 1 into an electrode bar with the diameter of phi 170mm, removing oxide scales on the surface of the electrode bar by sanding, and then welding the electrode bar and a dummy electrode together.
Table 1 the main elemental composition of the steel is given in the following table:
2) slag preparation
The slag charge ratio is (weight percentage): CaF2 60％、MgF2 6％、Al2O316 percent of CaO, 10.5 percent of MgO, 0.5 percent of BaO, and the total weight of the slag charge is 30 kg. Mixing CaF2、MgF2、Al2O3And uniformly mixing MgO and BaO, and then baking at 800 ℃ for 5h, independently baking CaO at 930 ℃ for 6 h. And (2) melting slag by using the electrode rod in the step 1), gradually adding the premixed slag (adding the slag in batches, adding the next batch after the added slag is melted) into a crystallizer, electrifying to start arcing, gradually increasing the voltage to 50V, gradually increasing the current to 5000A, reducing the current to 3500A after the slag is completely melted, keeping for 5 minutes, and breaking after the slag is cooled to room temperature to obtain the pre-melted slag.
3) Electroslag remelting
Gradually adding the pre-melted slag prepared in the step 2) into a copper crystallizer with the specification of phi 300mm, melting the slag by adopting the electrode rod in the step 1, and adding a valence-variable oxide (MnO) after melting the slag2)0.2kg, then inserting an electrode rod, moving the electrode rod up and down for 5 times to stir, then gradually increasing the power transmission power, starting to increase the voltage to 35V and the current to 3000A, and increasing the voltage to 51-55V and the current to 7800-8200A in 1-2 minutes. And (3) performing feeding before remelting is finished, wherein the feeding adopts a power successive subtraction method, the current reduction rate is 0.005-0.007 kA/S, and the feeding initial current is the electroslag remelting finishing current, so that the nuclear-grade stainless steel electroslag ingot is obtained.
The stainless steel electroslag ingot prepared by the method has the main indexes that: 15ppm of [ O ], 2ppm of [ H ], 50ppm of [ P ], 7ppm of [ S ], 13ppm of [ B ], 0.02% of [ Co ] and +/-0.005% of uniformity of carbon elements in steel ingots; the grade of the non-metallic inclusion is as follows: class A detail class 0, class B detail class 0, class C detail class 0, class D detail class 1.0; the components are uniform, no loose and no air holes exist, and the surface quality is good.
EXAMPLE 2 preparation of Gr.B8M stainless Steel electroslag ingot
1) Electrode rod preparation
Smelting by adopting a 500kg vacuum induction smelting furnace, pouring the molten steel shown in the table 2 into an electrode bar with the diameter of phi 170mm, removing oxide scales on the surface of the electrode bar by sanding, and then welding the electrode bar and a dummy electrode together.
Table 2 the main elemental composition of the steel is given in the following table:
2) slag preparation
The slag charge ratio is (weight percentage): CaF260％、MgF26％、Al2O312 percent of CaO, 15 percent of MgO, 6.5 percent of MgO, 0.5 percent of BaO, and the total weight of the slag charge is 30 kg. Mixing CaF2、MgF2、Al2O3And uniformly mixing MgO and BaO, and then baking at 800 ℃ for 5h, and independently baking CaO at 930 ℃ for 6 h. And (2) melting slag by using the electrode rod in the step 1), gradually adding the premixed slag (adding the slag in batches, adding the next batch after the added slag is melted) into a crystallizer, electrifying to start arcing, gradually increasing the voltage to 50V, gradually increasing the current to 5000A, reducing the current to 3500A after the slag is completely melted, keeping for 5 minutes, and breaking after the slag is cooled to room temperature to obtain the pre-melted slag.
3) Electroslag remelting
Gradually adding the pre-melted slag prepared in the step 2) into a copper crystallizer, wherein the specification of the crystallizer is phi 300mm, melting the slag by adopting the electrode rod in the step 1), adding 0.2kg of valence-change oxide (MnO) after melting the slag, then inserting the electrode rod, moving the electrode rod up and down for 5 times to stir, then gradually increasing the power transmission power, starting the voltage of 35V and the current of 3000A, and increasing the voltage to the normal smelting voltage of 51-55V and the current of 7800-8200A within 1-2 minutes. And (3) performing feeding before remelting is finished, wherein the feeding adopts a power successive subtraction method, the current reduction rate is 0.005-0.007 kA/S, and the feeding initial current is the electroslag remelting finishing current, so that the nuclear-grade stainless steel electroslag ingot is obtained.
The stainless steel electroslag ingot prepared by the method has the main indexes that: 14ppm of [ O ], 2ppm of [ H ], 52ppm of [ P ], 6ppm of [ S ], 18ppm of [ B ], 0.02% of [ Co ] and +/-0.005% of uniformity of carbon elements in steel ingots; the grade of the non-metallic inclusion is as follows: class A detail class 0, class B detail class 0, class C detail class 0, class D detail class 1.0; the components are uniform, no loose and no air holes exist, and the surface quality is good.
EXAMPLE 3 preparation of 304 stainless Steel electroslag ingot
1) Electrode rod preparation
Smelting by adopting a 3000kg vacuum induction smelting furnace, pouring the molten steel shown in the table 3 into an electrode rod with the diameter of 400mm, removing oxide scales on the surface of the electrode rod by sanding, and then welding the electrode rod and a dummy electrode together.
Table 3 the main elemental composition of the steel is given in the following table:
2) slag preparation
The slag charge ratio is (weight percentage): CaF255％、MgF28％、Al2O315 percent of CaO, 15 percent of MgO, and 7 percent of MgO, wherein the total weight of the slag is 100 kg. Mixing CaF2、MgF2、Al2O3And uniformly mixing MgO, baking at 800 ℃ for 5h, and independently baking CaO at 930 ℃ for 6 h. And (2) melting slag by using the electrode rod in the step 1), gradually adding the premixed slag (adding the slag in batches, adding the next batch after the added slag is melted) into a crystallizer, electrifying to start arcing, gradually increasing the voltage to 50V, gradually increasing the current to 5000A, reducing the current to 3500A after the slag is completely melted, keeping for 5 minutes, and breaking after the slag is cooled to room temperature to obtain the pre-melted slag.
3) Electroslag remelting
Gradually adding the pre-melted slag prepared in the step 2) into a copper crystallizer, wherein the specification of the crystallizer is phi 600mm, melting the slag by adopting the electrode rod in the step 1), adding 1kg of variable valence oxide (cerium oxide) after melting the slag, then inserting the electrode rod, moving the electrode rod up and down for 5 times to stir, then gradually increasing the power transmission power, starting the voltage to be 40V and the current to be 5000A, and increasing the voltage to be 55-60V and the current to be 10000-13000A after 1-2 minutes. And (3) performing feeding before remelting is finished, wherein the feeding adopts a power successive subtraction method, the current reduction rate is 0.007-0.009 kA/S, and the feeding initial current is the electroslag remelting finishing current, so that the nuclear-grade stainless steel electroslag ingot is obtained.
The stainless steel electroslag ingot prepared by the method has the main indexes that: 18ppm of [ O ], 2ppm of [ H ], 59ppm of [ P ], 6ppm of [ S ], 20ppm of [ B ], 0.02% of [ Co ] and +/-0.005% of uniformity of carbon elements in steel ingots; the grade of the non-metallic inclusion is as follows: class A detail class 0, class B detail class 0, class C detail class 0, class D detail class 1.0; the components are uniform, no loose and no air holes exist, and the surface quality is good.
Claims (6)
1. An electroslag remelting method for nuclear grade stainless steel is characterized by comprising the following steps:
1) electrode rod preparation
A vacuum ingot smelted by a vacuum induction smelting furnace is used as an electrode bar, oxide skin on the surface of the electrode bar is removed, and the electrode bar is welded with a false electrode;
2) slag preparation
The slag for the nuclear-grade stainless steel electroslag remelting comprises CaF2 40～70%、MgF2 1～10%、Al2O310-20% of CaO, 10-20% of MgO, 0-3% of BaO, and the slag has industrial purity of [ Co ]]+[Nb]+[Ta]≤0.2%、[B]≤0.01%；
In the components of the slag, MgF28-15% of MgO, 13-20% of CaO + BaO, and the content of CaO + BaO + MgO is not less than Al2O3The content of (A);
taking the components of the slag according to the proportion, baking the slag, uniformly mixing, gradually adding the slag into a crystallizer, electrifying to melt slag, continuously electrifying for 5-10 minutes after the slag is completely molten, then powering off, cooling the slag to room temperature, breaking the slag, and uniformly mixing to obtain pre-melted slag;
3) electroslag remelting
Gradually adding the pre-melted slag obtained in the step 2) into a crystallizer, melting the slag by using the electrode rod prepared in the step 1), adding a valence-variable oxide after the pre-melted slag is melted, moving the electrode rod up and down for 3-5 times to stir, and carrying out energization remelting to obtain a nuclear-grade stainless steel electroslag ingot;
the variable valence oxide is one or more of MnO2, MnO, TiO2 and rare earth oxide, and the using amount of the variable valence oxide is 0.5-3% of the weight of the slag charge;
the nuclear-grade stainless steel electroslag ingot comprises 14-18 ppm of [ O ], less than or equal to 2ppm of [ H ], less than or equal to 60ppm of [ P ], less than or equal to 10ppm of [ S ], less than or equal to 0.1% of [ Co ] and less than or equal to 0.005% of [ B ].
2. The electroslag remelting method for nuclear grade stainless steel according to claim 1, wherein the slag components in step 2) are in the following weight percentage: CaF2 55～60%、 MgF2 6～8%、 Al2O3 12～16%、 CaO 10～15%、 MgO 6～7%，BaO 0.5%。
3. The electroslag remelting process for a nuclear grade stainless steel according to claim 1, wherein: the shape of the cross section of the electrode rod in the step 1) corresponds to the shape of the cross section of the crystallizer.
4. The electroslag remelting process for a nuclear grade stainless steel according to claim 1, wherein: and 2) electrifying the slag under the voltage of 30-55V and at the current of 3000-6000A.
5. The electroslag remelting process for a nuclear grade stainless steel according to claim 1, wherein: step 2) baking the slag charge, wherein CaF2、MgF2、Al2O3The baking schedule of MgO and BaO is 600-900 ℃ multiplied by 4-6 h, and the baking schedule of CaO is 900-950 ℃ multiplied by 6-8 h.
6. The electroslag remelting process for a nuclear grade stainless steel according to claim 1, wherein: and 3) the rare earth oxide is cerium oxide or yttrium oxide.
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| CN109777919A (en) * | 2019-03-05 | 2019-05-21 | 河南中原特钢装备制造有限公司 | Reduce the remelting method and remelting slag system of ESR ingot oxygen content |
| CN111118302B (en) * | 2019-12-31 | 2022-04-19 | 浙江正达模具有限公司 | Crystallizer for metal electroslag remelting, electroslag remelting device and electroslag remelting method |
| CN111378848B (en) * | 2020-04-07 | 2022-03-15 | 中国航发北京航空材料研究院 | Pre-melted slag for electroslag remelting for improving purity of GH4169 alloy return and preparation method thereof |
| CN111748696A (en) * | 2020-05-22 | 2020-10-09 | 重庆材料研究院有限公司 | Nuclear-grade stainless steel electroslag remelting slag for high-level waste glass curing container and method for remelting electroslag |
| CN111575575B (en) * | 2020-06-24 | 2021-12-07 | 西安建筑科技大学 | Y for electroslag remelting ODS steel2O3Reinforced particles and methods of making and using the same |
| CN111876609B (en) * | 2020-07-29 | 2022-03-01 | 西安建筑科技大学 | Oxide-reinforced low-activation steel, electroslag remelting slag system and smelting method |
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| CN115216639A (en) * | 2022-07-29 | 2022-10-21 | 江苏星火特钢集团有限公司 | Production process capable of improving surface quality of electroslag ingot |
| CN115232921A (en) * | 2022-07-29 | 2022-10-25 | 江苏星火特钢集团有限公司 | Titanium content control method of titanium-containing steel |
| CN116607015A (en) * | 2023-04-11 | 2023-08-18 | 宝立合金有限公司 | Slag pool dynamic balancing method in electroslag smelting process |
| CN117305611B (en) * | 2023-11-27 | 2024-03-26 | 成都先进金属材料产业技术研究院股份有限公司 | Nickel-copper alloy electroslag remelting method |
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| JP2007302954A (en) * | 2006-05-11 | 2007-11-22 | Daido Steel Co Ltd | Method for electrically remelting slag in vacuum and apparatus for electrically remelting slag in vacuum |
| RU2487173C1 (en) * | 2011-12-29 | 2013-07-10 | Антон Васильевич Рощин | Flux for electroslag remelting |
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