CN117845145A - Super-purity 316LVV stainless steel cast ingot, triple smelting process and application thereof - Google Patents
Super-purity 316LVV stainless steel cast ingot, triple smelting process and application thereof Download PDFInfo
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- CN117845145A CN117845145A CN202311687894.1A CN202311687894A CN117845145A CN 117845145 A CN117845145 A CN 117845145A CN 202311687894 A CN202311687894 A CN 202311687894A CN 117845145 A CN117845145 A CN 117845145A
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- 238000003723 Smelting Methods 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000010935 stainless steel Substances 0.000 title claims abstract description 36
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 36
- 239000002893 slag Substances 0.000 claims abstract description 48
- 238000002844 melting Methods 0.000 claims abstract description 27
- 230000008018 melting Effects 0.000 claims abstract description 27
- 230000006698 induction Effects 0.000 claims abstract description 23
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 21
- 239000010959 steel Substances 0.000 claims abstract description 21
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 239000004065 semiconductor Substances 0.000 claims abstract description 8
- 238000004381 surface treatment Methods 0.000 claims abstract description 6
- 238000007670 refining Methods 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 11
- 238000005266 casting Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 6
- 238000005275 alloying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 239000011651 chromium Substances 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 239000011572 manganese Substances 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- 229910018505 Ni—Mg Inorganic materials 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 238000010079 rubber tapping Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 239000003999 initiator Substances 0.000 claims 1
- 229910052702 rhenium Inorganic materials 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 6
- 230000003749 cleanliness Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000008186 active pharmaceutical agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/10—Handling in a vacuum
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides an ultra-purity 316LVV stainless steel cast ingot, a triple smelting process and application thereof, wherein the ultra-purity 316LVV stainless steel cast ingot comprises the following components in percentage by mass: c is less than or equal to 0.01%, si is less than or equal to 0.05%, mn is less than or equal to 0.05%, ni: 14.50-15.00%, cr: 16.50-17.00%, mo: 2.2-2.5%, nb less than or equal to 0.5% and Fe in balance. The ultra-purity 316LVV stainless steel cast ingot is manufactured by adopting a triple smelting process, (1) an induction electrode is manufactured by adopting a vacuum induction smelting process; (2) The induction electrode is subjected to surface treatment and then electroslag smelting, (3) is subjected to surface treatment after being subjected to electroslag smelting treatment, then is subjected to vacuum consumable smelting, the induction electrode manufactured by the vacuum induction smelting process is subjected to electroslag smelting, the temperature of a slag pool is lowered in a mode of lowering the melting speed of the consumable electrode by lowering the power supply, and the purpose of reducing the shrinkage cavity depth is achieved, so that the yield of finished products of bars is improved, the content of nonmetallic inclusion and the content of C, O, N element are low, the purity of steel is improved, and the induction electrode can be well applied to semiconductors.
Description
Technical Field
The invention relates to the technical field of metal processing, in particular to an ultra-purity 316LVV stainless steel cast ingot, and a triple smelting process and application thereof.
Background
The 316LVV stainless steel has the advantages of high corrosion resistance, temperature resistance, strength, weldability and the like, can meet the high strength and corrosion resistance requirements used in most industrial environments, and is widely applied to the fields of semiconductors, parts, medical industry, LCD-TFT industry and the like. Process cleanliness is one of the most interesting problems in the semiconductor industry, and the material purity of the components of the fluid system is critical to achieving the required process cleanliness, so that in order to ensure the purity of the materials in the semiconductor industry, higher requirements are put on harmful impurities and nonmetallic inclusions of 316LVV stainless steel produced in a smelting plant.
Currently, 316L VV stainless steel generally adopts a Vacuum Induction Melting (VIM) +vacuum consumable remelting (VAM) double-vacuum smelting process, and the process has the defects in controlling bulk nonmetallic inclusions, harmful contents and the like. The vacuum induction melting cast electrode has more secondary inclusions, bright shrinkage cavities and dark shrinkage cavities and poorer electrode compactness; the vacuum consumable remelting finished product has defects at the position where shrinkage holes are generated, meanwhile, the S removing effect is poor, the S element content in the finished product bar is too high, and the performance of the material is seriously affected. Therefore, the purity of the product produced by the existing smelting method cannot meet the requirements of the industries such as semiconductors.
Disclosure of Invention
Based on the current situation, in order to solve the problems and defects existing in the process of smelting 316LVV stainless steel ingot, the invention aims to provide an ultrapure 316LVV stainless steel ingot and a triple smelting process thereof, and the triple smelting process is adopted to produce the ultrapure 316LVV stainless steel ingot.
In order to achieve the above purpose, the invention discloses an ultrapure 316LVV stainless steel ingot, which comprises the following components in percentage by mass: c is less than or equal to 0.01%, si is less than or equal to 0.05%, mn is less than or equal to 0.05%, ni: 14.50-15.00%, cr: 16.50-17.00%, mo: 2.2-2.5%, nb less than or equal to 0.5% and Fe in balance.
As a preferred mode, the triple smelting process of the ultra-purity 316LVV stainless steel ingot casting comprises the following steps:
(1) Adopting a vacuum induction smelting process to prepare an induction electrode;
(2) After the surface treatment of the induction electrode, protective atmosphere electroslag smelting is carried out, and the specific steps are as follows:
2.1 stage of slag preparation
Providing slag, and loading the slag into a slag adding bin;
2.2 arc striking and slag forming stage
An arc striking agent is put into the water-cooling crystallizer, and a current loop is formed between the consumable electrode and the water-cooling dummy ingot bottom plate through the arc striking agent;
the secondary side current range is controlled to be 4000A, the secondary side voltage range is controlled to be 56V, and the slag melting time is more than or equal to 30min;
arc striking stage: controlling the current range of the secondary side to be 8000A, the voltage range of the secondary side to be 59V, and the arcing time to be more than or equal to 60min;
2.3 Stable smelting stage
Controlling the melting speed and slag pendulum by adopting the melting speed of 240-360 kg/h and the slag pendulum of 0.15-0.36 mohm, and introducing argon under the pressure of 0.2bar for protection;
2.4 Heat seal topping stage
The power is controlled by adopting the power plus slag resistance, the power is slowly reduced from the steady-state power to 35-46% of the steady smelting stage, and the slag resistance is gradually increased from the steady-state slag resistance to 150-170% of the steady smelting stage;
(3) After electroslag smelting treatment, surface treatment is carried out, and then vacuum consumable smelting is carried out.
Preferably, the slag is selected from CaF 2 、Al 2 O 3 And CaO. Wherein CaF 2 The melting point, viscosity and surface tension of the slag can be reduced; al (Al) 2 O 3 The conductivity can be reduced, and the energy consumption is reduced; caO can improve the alkalinity and the desulfurization effect.
As a preferred mode, the arc striking agent comprises CaF 2 And TiO 2 Is a mixture of (a) and (b).
As a preferred mode, the vacuum induction melting comprises the following steps:
1.1 preparation of raw materials
Providing raw materials according to the required proportion of the product;
1.2 charging
Roasting the raw materials at a low temperature of 200 ℃, preserving heat for 3 hours, and adding the raw materials into a crucible according to the proportion of alloy components of the product;
1.3 vacuum pumping
The power supply and the vacuum valve are turned on, the vacuum is pumped to 9Pa, then the power is supplied for heating, the power is set to 90KW, and the furnace burden is ensured to be uniformly melted;
1.4 refining
Controlling the vacuum degree to be less than or equal to 1Pa in the refining period, and controlling the refining temperature to be 1630+/-10 ℃ in the refining period for not less than 40 minutes;
1.5 alloying
Heating the molten steel to 1570-1590 ℃ for alloying;
1.6 casting
Casting the molten steel treated in the steps, measuring the temperature of the molten steel, controlling the temperature of the molten steel to be 1000-1500 ℃, deoxidizing after refining is finished, and casting to obtain an induction electrode;
in the preferred mode, in the step 1.4 refining, volatile and easily burnt small materials are added before tapping, so that the depth of shrinkage holes of the electrode is not more than 300mm, the volatile and easily burnt small materials comprise Ni-Mg, re and the like, and electromagnetic stirring is also preferred, so that the uniformity of the components and the temperature of molten steel can be promoted.
As a preferred mode, the raw materials comprise high-purity metallic chromium JCr-A, metallic molybdenum Mo-2, electrolytic nickel Ni9996, industrial pure iron YT1, cathode copper Cu-CATH-1 and metallic manganese.
As a preferred mode, the steps of vacuum consumable smelting are as follows:
3.1, adopting a copper crystallizer with the diameter of phi 550 mm;
3.2 arc striking and slag forming stage
The current and the molten drop are adopted for control, the current is 1.0-6kA, the voltage is 22-25V, and the time of an arcing stage is about 6min;
3.3 Stable smelting stage
Adopting melting speed and droplet control, wherein the melting speed is 3.5+/-0.3 kg/min, introducing helium and controlling the pressure in the furnace to be 300-500 Pa;
3.4 feeding stage
And (3) adopting current and molten drop control, gradually reducing the current to 0.7-1.2kA from a stable smelting stage, wherein the voltage is 18-20V, closing an inlet gas channel and an outlet gas channel after smelting, and cooling for 3-4 hours under the protection of argon gas for discharging, thereby obtaining the ultra-purity 316LVV stainless steel cast ingot.
Correspondingly, the invention also provides application of the ultra-pure 316LVV stainless steel cast ingot in semiconductors.
Correspondingly, the invention also provides application of the ultra-pure 316LVV stainless steel ingot prepared by the triple smelting process of the ultra-pure 316LVV stainless steel ingot in semiconductors.
The invention has the beneficial effects that:
(1) In the ultra-purity 316LVV stainless steel cast ingot prepared by the triple smelting process, the induction electrode prepared by the vacuum induction smelting process is subjected to electroslag smelting, the temperature of a slag pool is reduced in a mode of reducing the melting speed of a consumable electrode by reducing the power supply, and the purpose of reducing the shrinkage cavity depth is achieved, so that the yield of finished products of bars is improved, the content of nonmetallic inclusion and the content of C, O, N element are low, and the purity of steel is improved;
(2) In the ultra-purity 316LVV stainless steel cast ingot prepared by the triple smelting process, the class A, class B, class C, class D and DS inclusions are 0, which indicates that the product reaches the cleanliness level of a zero inclusion product;
(3) The invention controls the vacuum degree to be less than or equal to 1Pa in the refining period, the time is not less than 40 minutes, the refining temperature is 1630+/-10 ℃, and the uniformity of the components and the temperature of molten steel can be promoted.
Drawings
FIG. 1 is a diagram of metallographic inclusions of the product of the example.
Description of the embodiments
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention. It should be noted that the following embodiments and features in the embodiments may be combined with each other without conflict.
Examples
The invention provides an ultra-purity 316LVV stainless steel cast ingot, which comprises the following components in percentage by mass: c is less than or equal to 0.01%, si is less than or equal to 0.05%, mn is less than or equal to 0.05%, ni: 14.50-15.00%, cr: 16.50-17.00%, mo: 2.2-2.5%, nb less than or equal to 0.5% and Fe in balance.
The ultra-purity 316LVV stainless steel cast ingot is prepared by a triple smelting process, and comprises the following specific steps:
(1) Vacuum induction melting VIM
1.1 preparation of raw materials
Raw materials (high-purity metal chromium JCr-A, metal molybdenum Mo-2, electrolytic nickel Ni9996, industrial pure iron YT1, cathode copper Cu-CATH-1, metal manganese and the like) are provided according to the required proportion of the product;
1.2 charging
Baking the raw materials at low temperature of 200deg.C, maintaining the temperature for 3 hours, keeping the raw materials dry for standby, and storing in open air for no more than 24 hours; adding raw materials such as high-purity metallic chromium JCr-A, metallic molybdenum Mo-2, electrolytic nickel Ni9996, industrial pure iron YT1, cathode copper Cu-CATH-1, metallic manganese and the like into a crucible according to the alloy component proportion of the product;
1.3 vacuum pumping
The power supply and the vacuum valve are turned on, the vacuum is pumped to 9Pa, then the power is supplied for heating, the power is set to 90KW, and the furnace burden is ensured to be uniformly melted; entering a melting period, and simultaneously strengthening electromagnetic stirring, thereby being beneficial to carbon-oxygen reaction; reducing power after furnace burden is melted, carrying out secondary charging, continuously increasing power until furnace burden is melted down, stopping vacuumizing, reducing power, and filling argon gas for sampling;
1.4 refining
Controlling the vacuum degree to be less than or equal to 1Pa in the refining period, controlling the time to be not less than 40 minutes, controlling the refining temperature to 1630+/-10 ℃, adding volatile and easily burnt small materials (such as Ni-Mg, re and the like) before tapping, and controlling the electrode shrinkage cavity depth to be not more than 300mm;
1.5 alloying
Heating the molten steel to 1570-1590 ℃ for alloying;
1.6 casting
Casting the molten steel treated in the steps, measuring the temperature of the molten steel, controlling the temperature of the molten steel to be 1000-1500 ℃, deoxidizing after refining is finished, and casting to obtain an induction electrode;
(2) Protective atmosphere electroslag smelting ESR
2.1 stage of slag preparation
Providing slag, and loading the slag into a slag adding bin;
slag is selected from CaF 2 、Al 2 O 3 Firstly, loading slag into a slag adding bin and setting slag adding process parameters;
2.2 arc striking and slag forming stage
Placing an arc starting agent (CaF) in a water-cooled crystallizer 2 And TiO 2 The mixture) and a current loop is formed between the consumable electrode and the water-cooled dummy ingot bottom plate through an arc striking agent;
wherein the slag melting stage:
controlling the current range of the secondary side to 4000A, the voltage range of the secondary side to 56V, and the slag melting time to be more than or equal to 30min;
arc striking stage: controlling the current range of the secondary side to be 8000A, the voltage range of the secondary side to be 59V, and the arcing time to be more than or equal to 60min;
2.3 Stable smelting stage
Controlling the melting speed and slag pendulum, wherein the melting speed is 240-360 kg/h, the slag pendulum is 0.15-0.36 mohm, and argon with the pressure of 0.2bar is introduced for protection, so that molten steel is prevented from contacting oxygen and nitrogen in air, and oxidation of steel is prevented;
2.4 Heat seal topping stage
The power and slag resistance control is adopted, the power is slowly reduced from the steady-state power to 35-46% of the steady smelting stage, the slag resistance is gradually increased from the steady-state slag resistance to 150-170% of the steady smelting stage, the temperature of the slag pool is reduced in a mode of reducing the melting speed of the consumable electrode by reducing the power supply, and the purpose of reducing the shrinkage cavity depth is achieved;
(3) Var for vacuum consumable smelting
3.1, adopting a copper crystallizer with the diameter of phi 550 mm;
3.2 arc striking and slag forming stage
The current and the molten drop are adopted for control, the current is 1.0-6kA, the voltage is 22-25V, the time of the arcing phase is about 6min, the current adopts the trend of firstly increasing rapidly and then reducing slowly in order to ensure the stability of the arcing phase, and the setting rule of the voltage is matched with the current;
3.3 Stable smelting stage
The melting speed is 3.5+/-0.3 kg/min by adopting melting speed and droplet control, helium is introduced, the pressure in the furnace is controlled to be 300-500Pa, the cooling effect is enhanced, and impurities can be discharged in time;
3.4 feeding stage
By adopting current and molten drop control, the current is gradually reduced to 0.7-1.2kA from a stable smelting stage, the voltage is 18-20V, the temperature of a slag pool is reduced in a mode of reducing the melting speed of a consumable electrode by reducing the power supply, the purpose of reducing the shrinkage cavity depth is achieved, the yield of the ingot is improved, an inlet and outlet gas circuit is closed after smelting is finished, and the ingot is cooled for 3-4 hours under the protection of argon and discharged, so that the ultra-purity 316LVV stainless steel ingot is obtained.
Comparative example
The comparative example uses a double vacuum melting process of Vacuum Induction Melting (VIM) +vacuum consumable remelting (VAM), i.e. the process of step (2) without examples, the remainder being the same as examples.
In the production process of the product, oxygen in the solution reacts with carbon to generate bubbles in the solidification process; meanwhile, in the cooling process, oxygen can be separated out from the solution in the form of FeO, mnO or other oxide inclusions, so that the ductility, toughness, fatigue strength and machining performance of the steel are weakened, and when the hydrogen content in the steel is more than 2ppm, the phenomena of internal cracking and fracture can occur in the cooling process after rolling and forging. Therefore, the gas content in the product has a large influence on the quality thereof, and for this purpose, the gas contents of the products obtained in examples and comparative examples were tested, and the results are shown in Table 1:
table 1 results of gas content of examples and comparative examples products
| Gas element | O ppm | N ppm | H ppm |
| Comparative example | 15 | 50 | 1.6 |
| Examples | 8 | 25 | 0.5 |
As can be seen from the data in Table 1, the hydrogen content of the comparative example product is less than 2, and the hydrogen content of the product prepared by the triple smelting process of the invention is only 0.5 ppm, and the product has lower gas content, which indicates that the product has better ductility, toughness, fatigue strength and machining property, and also indicates that the nonmetallic inclusion content and C, O, N element content in the product are lower, so that the purity of the steel is greatly improved.
Referring to fig. 1, fig. 1 is a metallographic inclusion diagram of an example product, and as can be seen from the metallographic inclusion diagram, class a, class B, class C, class D, and class DS inclusions are 0, which indicates that the product has reached the "zero inclusion" product cleanliness level.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. Equivalent variations are therefore contemplated as falling within the scope of the claimed invention.
Claims (10)
1. An ultrapure 316LVV stainless steel ingot, characterized by comprising, in mass percent: c is less than or equal to 0.01%, si is less than or equal to 0.05%, mn is less than or equal to 0.05%, ni: 14.50-15.00%, cr: 16.50-17.00%, mo: 2.2-2.5%, nb less than or equal to 0.5% and Fe in balance.
2. The triple smelting process of ultra-purity 316LVV stainless steel ingot according to claim 1, comprising the steps of:
(1) Adopting a vacuum induction smelting process to prepare an induction electrode;
(2) After the surface treatment of the induction electrode, electroslag smelting is carried out, and the specific steps are as follows:
2.1 stage of slag preparation
Providing slag, and loading the slag into a slag adding bin;
2.2 arc striking and slag forming stage
An arc striking agent is put into the water-cooling crystallizer, and a current loop is formed between the consumable electrode and the water-cooling dummy ingot bottom plate through the arc striking agent;
the secondary side current range is controlled to be 4000A, the secondary side voltage range is controlled to be 56V, and the slag melting time is more than or equal to 30min; controlling the current range of the secondary side at 8000A, the voltage range of the secondary side at 59V and the arcing time at 60min or more in the arcing stage;
2.3 Stable smelting stage
Controlling the melting speed and slag pendulum by adopting the melting speed of 240-360 kg/h and the slag pendulum of 0.15-0.36 mohm, and introducing argon under the pressure of 0.2bar for protection;
2.4 Heat seal topping stage
The power is controlled by adopting the power plus slag resistance, the power is slowly reduced from the steady-state power to 35-46% of the steady smelting stage, and the slag resistance is gradually increased from the steady-state slag resistance to 150-170% of the steady smelting stage;
(3) After electroslag smelting treatment, surface treatment is carried out, and then vacuum consumable smelting is carried out.
3. The triple smelting process for ultra-purity 316LVV stainless steel ingot according to claim 2, wherein the slag is selected from CaF 2 、Al 2 O 3 And CaO.
4. The triple smelting process of ultra-purity 316LVV stainless steel ingot according to claim 2, wherein the arc initiator comprises CaF 2 And TiO 2 Is a mixture of (a) and (b).
5. The triple smelting process of ultra-purity 316LVV stainless steel ingot according to claim 2, wherein the vacuum induction smelting comprises the steps of:
1.1 preparation of raw materials
Providing raw materials according to the required proportion of the product;
1.2 charging
Roasting the raw materials at a low temperature of 200 ℃, preserving heat for 3 hours, and adding the raw materials into a crucible according to the proportion of alloy components of the product;
1.3 vacuum pumping
The power supply and the vacuum valve are turned on, the vacuum is pumped to 9Pa, then the power is supplied for heating, the power is set to 90KW, and the furnace burden is ensured to be uniformly melted;
1.4 refining
Controlling the vacuum degree to be less than or equal to 1Pa in the refining period, and controlling the refining temperature to be 1630+/-10 ℃ in the refining period for not less than 40 minutes;
1.5 alloying
Heating the molten steel to 1570-1590 ℃ for alloying;
1.6 casting
Casting the molten steel treated in the steps, measuring the temperature of the molten steel, controlling the temperature of the molten steel to be 1000-1500 ℃, deoxidizing after refining is finished, and casting to obtain the induction electrode.
6. The triple smelting process of the ultra-purity 316LVV stainless steel ingot according to claim 2, wherein the raw materials comprise high-purity metal chromium JCr-A, metal molybdenum Mo-2, electrolytic nickel Ni9996, industrial pure iron YT1, cathode copper Cu-CATH-1 and metal manganese.
7. The triple smelting process of ultra-purity 316LVV stainless steel ingot according to claim 2, wherein the step of vacuum consumable smelting comprises the steps of:
3.1, adopting a copper crystallizer with the diameter of phi 550 mm;
3.2 arc striking and slag forming stage
The current and the molten drop are adopted for control, the current is 1.0-6kA, the voltage is 22-25V, and the time of an arcing stage is 6min;
3.3 Stable smelting stage
Adopting melting speed and droplet control, wherein the melting speed is 3.5+/-0.3 kg/min, introducing helium and controlling the pressure in the furnace to be 300-500 Pa;
3.4 feeding stage
And (3) adopting current and molten drop control, gradually reducing the current to 0.7-1.2kA from a stable smelting stage, wherein the voltage is 18-20V, closing an inlet gas channel and an outlet gas channel after smelting, and cooling for 3-4 hours under the protection of argon gas for discharging, thereby obtaining the ultra-purity 316LVV stainless steel cast ingot.
8. The triple smelting process of ultra-purity 316LVV stainless steel ingot according to claim 2, wherein in the step 1.4 refining, a volatile and easily burnt small material is added before tapping, so that the electrode shrinkage depth is not more than 300mm.
9. The triple smelting process for ultra-pure 316LVV stainless steel ingot according to claim 8, wherein the volatile and burnable minor material comprises Ni-Mg or Re.
10. Use of an ultrapure 316LVV stainless steel ingot as defined in claim 1 or an ultrapure 316LVV stainless steel ingot as defined in any one of claims 2-9 in a semiconductor manufactured by a triple smelting process of an ultrapure 316LVV stainless steel ingot.
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