CN118207471B - Preparation method of hydrogen-resistant stainless steel master alloy bar and hydrogen storage container - Google Patents
Preparation method of hydrogen-resistant stainless steel master alloy bar and hydrogen storage container Download PDFInfo
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- CN118207471B CN118207471B CN202410624723.2A CN202410624723A CN118207471B CN 118207471 B CN118207471 B CN 118207471B CN 202410624723 A CN202410624723 A CN 202410624723A CN 118207471 B CN118207471 B CN 118207471B
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 86
- 239000001257 hydrogen Substances 0.000 title claims abstract description 84
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000000956 alloy Substances 0.000 title claims abstract description 69
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 68
- 238000003860 storage Methods 0.000 title claims abstract description 31
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 25
- 239000010935 stainless steel Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005242 forging Methods 0.000 claims abstract description 65
- 238000002844 melting Methods 0.000 claims abstract description 48
- 230000008018 melting Effects 0.000 claims abstract description 48
- 230000006698 induction Effects 0.000 claims abstract description 32
- 238000003723 Smelting Methods 0.000 claims abstract description 29
- 238000005096 rolling process Methods 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 238000010891 electric arc Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 49
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 39
- 229910000831 Steel Inorganic materials 0.000 claims description 34
- 239000010959 steel Substances 0.000 claims description 34
- 238000005266 casting Methods 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 21
- 239000002994 raw material Substances 0.000 claims description 21
- 229910052742 iron Inorganic materials 0.000 claims description 20
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- ATTFYOXEMHAYAX-UHFFFAOYSA-N magnesium nickel Chemical compound [Mg].[Ni] ATTFYOXEMHAYAX-UHFFFAOYSA-N 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims description 10
- 238000007670 refining Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 238000010079 rubber tapping Methods 0.000 claims description 8
- 229910000519 Ferrosilicon Inorganic materials 0.000 claims description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 7
- 229910018487 Ni—Cr Inorganic materials 0.000 claims description 7
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 claims description 7
- 239000011572 manganese Substances 0.000 claims description 7
- 239000011733 molybdenum Substances 0.000 claims description 7
- 238000009792 diffusion process Methods 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- 238000005422 blasting Methods 0.000 claims description 5
- 239000011651 chromium Substances 0.000 claims description 5
- 238000007689 inspection Methods 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 238000003466 welding Methods 0.000 abstract description 5
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 description 11
- 238000007599 discharging Methods 0.000 description 10
- 230000008569 process Effects 0.000 description 6
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
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- 238000005498 polishing Methods 0.000 description 4
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- 239000012535 impurity Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 238000001914 filtration Methods 0.000 description 2
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- 238000000265 homogenisation Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
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- 238000005204 segregation Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000010583 slow cooling Methods 0.000 description 2
- 238000005275 alloying Methods 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 239000000446 fuel Substances 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
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- 230000002035 prolonged effect Effects 0.000 description 1
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Classifications
-
- 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
- C22C33/06—Making ferrous alloys by melting using master alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/002—Hybrid process, e.g. forging following casting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/22—Moulds for peculiarly-shaped castings
-
- 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
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- 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
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the field of metallurgy, and discloses a preparation method of a hydrogen-resistant stainless steel master alloy bar and a hydrogen storage container, wherein the master alloy bar is used for being remelted and integrally cast into a cylinder of the hydrogen storage container, and the preparation method of the master alloy bar comprises the following steps: sequentially carrying out vacuum induction melting, vacuum consumable melting, forging cogging and rolling to obtain a master alloy bar; wherein, carry out vacuum consumable smelting and include: in the initial melting stage, forming a molten pool within 1h by adopting high current; in the stable smelting stage, the electric arc is kept stable, the vacuum degree is controlled to be 0.08-0.4 Pa, the metal melting speed is 3.4-5.6 kg/min, and the number of molten drops is 3.5-5.2 drops/s. The invention can prepare the hydrogen-resistant stainless steel master alloy bar which is suitable for being integrally cast and molded into the cylinder body of the hydrogen storage container after remelting, thereby reducing or eliminating the welding joint to the greatest extent and improving the hydrogen embrittlement resistance of the hydrogen storage container under the hydrogen condition.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a preparation method of a hydrogen-resistant stainless steel master alloy bar and a hydrogen storage container.
Background
The hydrogen energy is a pollution-free renewable and circulating green energy source, and can effectively reduce carbon dioxide emission caused by the traditional petrochemical fuel. With the continuous development of hydrogen energy technology, such as hydrogen-based steelmaking, hydrogen station construction and hydrogen storage pressure vessel development, the problem of damage tolerance of materials in a hydrogen service environment must be considered. Because of its better hydrogen embrittlement resistance, the research on hydrogen embrittlement of 316L austenitic stainless steel under conditions of high pressure, low temperature, etc. is becoming a research focus.
In order to meet the requirements of a complex structure and a large-size container, welding is an indispensable processing process, for example, a cylinder body of a high-temperature high-pressure hydrogen storage container is welded by austenitic stainless steel. The weld structure includes a weld, a heat affected zone, and a matrix parent metal. The inventors of the present application have recognized that, under the influence of thermal cycling during welding, the heat affected zone (particularly the coarse grain heat affected zone) has a more complex microstructure than the parent material, and under rapid cooling conditions, a martensitic structure is produced that is more susceptible to hydrogen embrittlement. In addition, the tensile residual stress introduced in the welding process can accelerate the diffusion and enrichment of hydrogen in the material, improve the hydrogen embrittlement sensitivity of the weldment, and lead to cracking failure in the subsequent service process of the material.
Therefore, there is a need to develop an improvement in the hydrogen embrittlement resistance of hydrogen storage vessels.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a hydrogen-resistant stainless steel master alloy bar and a hydrogen storage container, so as to solve the problem that the hydrogen storage container is difficult to meet the service requirement in a hydrogen environment because of the hydrogen embrittlement sensitivity of a welded joint in the hydrogen environment.
According to one aspect of the invention, a preparation method of a hydrogen-resistant stainless steel master alloy bar is provided, wherein the master alloy bar is used for being integrally cast and molded into a cylinder of a hydrogen storage container after remelting; the master alloy bar comprises the following components in percentage by mass: p is less than or equal to 0.006%, S is less than or equal to 0.004%, O is less than or equal to 0.004%, and N is less than or equal to 0.005%; after ultrasonic nondestructive inspection, the master alloy bar meets the A-level requirement in GB/T4162-2022; the method comprises the following steps:
sequentially carrying out vacuum induction melting, vacuum consumable melting, forging cogging and rolling to obtain a master alloy bar;
wherein, carry out vacuum consumable smelting and include: in the initial melting stage, forming a molten pool within 1h by adopting a large current of 8-12 kA; in the stable smelting stage, keeping the electric arc stable, controlling the vacuum degree to be 0.08-0.4 Pa, the metal melting speed to be 3.4-5.6 kg/min, and the number of molten drops to be 3.5-5.2 drops/s;
The master alloy bar comprises the following components in percentage by mass: less than or equal to 0.03 percent of C, less than or equal to 0.90 percent of Si, less than or equal to 1.85 percent of Mn, less than or equal to 0.006 percent of P, less than or equal to 0.004 percent of S, less than or equal to 0.004 percent of O, less than or equal to 0.005 percent of N, less than or equal to 16 percent of Cr, less than or equal to 17.5 percent of 12 percent of Ni, less than or equal to 14 percent of 12 percent, less than or equal to 2.3 percent of Mo, less than or equal to 3.0 percent of Fe and the balance of Fe;
performing vacuum induction melting includes:
Sequentially loading nickel-chromium intermediate alloy, carbon blocks, ferrosilicon, electrolytic manganese, molybdenum strips and pure iron into a vacuum induction furnace, wherein the content of P brought in by raw materials is controlled to be less than or equal to 0.006wt% and the content of S is controlled to be less than or equal to 0.004wt%;
When the vacuum degree in the vacuum induction furnace is less than 5Pa, starting to electrify and melt, heating to 1550+/-20 ℃ after raw materials are melted, starting to keep warm and refine, and electromagnetically stirring for at least 30min and controlling the vacuum degree to be less than 0.3Pa during refining;
When the sampling analysis is carried out and the N content is less than or equal to 0.005wt% and the O content is less than or equal to 0.004wt%, inert gas is filled to ensure that the pressure in the vacuum induction furnace is 10000-13000 Pa, nickel-magnesium alloy is added for continuous deoxidization, electrified tapping is carried out after electromagnetic stirring is carried out for 10min, the tapping temperature is 1530+/-10 ℃, and then the molten steel is cast into steel ingots;
Forging cogging includes:
Forging by fire: the self-consumption ingot obtained after vacuum self-consumption is subjected to heat preservation at 1170 ℃ for 45-55 min, then is upset to 45-55% of the height of the self-consumption ingot, and then is drawn to be an octagonal forging material with phi 410+/-10 mm;
Secondary forging: the octagonal forging material with phi 410 plus or minus 10mm is upsetted to 45 to 55 percent of the height of a consumable ingot after heat preservation for 45 to 55 minutes at 1170 ℃, and then is drawn to be the octagonal forging material with phi 265 plus or minus 10 mm;
Forging with three times of fire: the octagonal forging material with phi 265 plus or minus 10mm is heated for 45-55 min at 1170 ℃ and then is drawn to be the octagonal forging material with phi 200 plus or minus 10 mm;
Forging four times: and (3) preserving heat of the octagonal forging material with phi 200+/-10 mm for 45-55 min at 1170 ℃ and then drawing the octagonal forging material to a square forging material with the cross section side length of 150-160 mm, wherein the final forging temperature is more than or equal to 830 ℃.
According to one embodiment of the invention, performing vacuum induction melting comprises: performing surface shot blasting treatment on the pure iron rod to remove oxide skin; the oxidized portion of the nickel-magnesium alloy is removed.
According to one embodiment of the invention, performing vacuum induction melting comprises: before casting, the ingot mould is scalded by molten iron, and the molten steel is filtered in the casting process.
According to one embodiment of the present invention, performing forging cogging includes: the consumable ingot was diffusion annealed at 1180.+ -. 20 ℃ for at least 24 hours and then kept at 1130.+ -. 15 ℃ for 3 hours before being forged over a fire.
According to one embodiment of the invention, performing rolling into a product comprises: and heating the square forging material to 1130+/-15 ℃ and preserving heat for 3 hours, then rolling, wherein the initial rolling temperature is more than or equal to 1060 ℃, and rolling into bars with the specification of phi 65-75 mm through 6 passes.
According to one embodiment of the invention, performing rolling into a product comprises: and (3) carrying out surface finishing processing on the bar with the specification of phi 65-75 mm to obtain the hydrogen-resistant stainless steel master alloy bar.
According to one embodiment of the invention, the grain size of the master alloy bar is not less than 7 grades, and the grain size difference is not more than 1 grade.
According to one embodiment of the invention, performing vacuum consumable smelting comprises: in the beginning of the melting stage, a molten pool is formed within 1h by adopting a large current of 8 kA; in the stable smelting stage, the electric arc is kept stable, the vacuum degree is controlled to be 0.08-0.22 Pa, the metal melting speed is 3.4-4.3 kg/min, and the number of molten drops is 3.5-4.2 drops/s.
According to one embodiment of the invention, performing vacuum consumable smelting comprises: in the initial melting stage, a molten pool is formed within 1h by adopting a large current of 12 kA; in the stable smelting stage, the electric arc is kept stable, the vacuum degree is controlled to be 0.22-0.4 Pa, the metal melting speed is controlled to be 4.3-5.6 kg/min, and the number of molten drops is controlled to be 4.2-5.2 drops/s.
According to another aspect of the present invention, there is provided a hydrogen storage container, wherein the cylinder of the hydrogen storage container is obtained by remelting and integrally casting the hydrogen-resistant stainless steel master alloy bar prepared by the method as described above.
According to the technical scheme, the steps of vacuum induction melting, vacuum consumable melting, forging cogging, rolling into a material and the like are adopted, and specific means and parameters of each step are designed, so that the hydrogen-resistant stainless steel master alloy bar with uniform component structure, low impurity elements and basically no defects can be prepared, and the master alloy bar is suitable for being integrally cast and formed into a cylinder body of the hydrogen storage container after remelting, so that welded joints are reduced or eliminated to the greatest extent, and the hydrogen embrittlement resistance of the hydrogen storage container under the hydrogen condition is improved.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 shows a flow chart of a method of preparing a hydrogen resistant stainless steel master alloy bar according to an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments of the present invention will be described in further detail with reference to the accompanying drawings.
It should be noted that, in the embodiments of the present invention, all the expressions "first" and "second" are used to distinguish two entities with the same name but different entities or different parameters, and it is noted that the "first" and "second" are only used for convenience of expression, and should not be construed as limiting the embodiments of the present invention, and the following embodiments are not described one by one.
As mentioned in the background section above, the inventors of the present application have recognized that the barrels of hydrogen storage vessels are typically welded from austenitic stainless steel in the prior art, and that welded joints have a higher susceptibility to hydrogen embrittlement, which can affect the performance of the hydrogen storage vessel in a hydrogen environment.
The inventors have further recognized that master alloy is a refined alloy material for remelting casting. As a casting base material, many characteristics of the master alloy (such as chemical composition, precipitated phase distribution, grain size, mechanical properties, corrosion properties, etc.) are inherited to the relevant work pieces after remelting casting. The master alloy simplifies the control of smelting process, has low carbon emission and higher quality stability.
Thus, the inventors have realized that if a master alloy is used as a raw material, workpieces such as a cylinder of a hydrogen storage container, etc., are directly produced by integral casting molding, the welded joint can be reduced or eliminated to the maximum extent, thereby improving the hydrogen embrittlement resistance of the workpiece under the hydrogen-critical condition.
Based on the above recognition, the present application provides, in one or more embodiments to be described below, a method of manufacturing a hydrogen resistant stainless steel master alloy bar capable of manufacturing a master alloy bar suitable for being remelted and integrally cast into a cylinder of a hydrogen storage container, and a hydrogen storage container.
The invention provides a preparation method of a hydrogen-resistant stainless steel master alloy bar, wherein the master alloy bar is used for being remelted and integrally cast to form a cylinder of a hydrogen storage container; the master alloy bar comprises the following components in percentage by mass: p is less than or equal to 0.006%, S is less than or equal to 0.004%, O is less than or equal to 0.004%, and N is less than or equal to 0.005%; after ultrasonic nondestructive inspection, the master alloy bar meets the A-level requirement in GB/T4162-2022; referring to fig. 1, the preparation method includes: sequentially carrying out vacuum induction melting, vacuum consumable melting, forging cogging and rolling to obtain a master alloy bar; wherein, carry out vacuum consumable smelting and include: in the initial melting stage, forming a molten pool within 1h by adopting high current; in the stable smelting stage, the electric arc is kept stable, the vacuum degree is controlled to be 0.08-0.4 Pa, the metal melting speed is controlled to be 3.4-5.6 kg/min, and the number of molten drops is controlled to be 3.5-5.2 drops/s (which means that 3.5-5.2 drops of molten steel fall down per second).
In an embodiment of the present invention, vacuum induction melting may include operations of heating melting, refining, alloying/deoxidizing, casting, etc., in order to complete preliminary melting of the steel ingot, remove harmful elements C, O, N, H, etc. The vacuum consumable smelting may include a start-up smelting stage, a normal smelting stage, and a fill smelting stage, with the aim of further improving the purity and compactness of the material, such as deoxidizing denitrification. The forging cogging can comprise two basic working procedures of upsetting and drawing, and the as-cast structure can be effectively broken through repeated upsetting and drawing, so that grains are refined, and the grains are uniformly distributed. The rolled product can further improve the distribution of bar crystal grains and the mechanical property.
In the embodiment of the invention, the steps of vacuum induction melting, vacuum consumable melting, forging cogging, rolling into a material and the like are adopted, and specific means and parameters of each step are designed, so that the hydrogen-resistant stainless steel master alloy bar with uniform composition structure (the grain size is not lower than 7 levels, the grain size difference is not more than 1 level) and low impurity elements and basically no defects can be prepared, and the master alloy bar is suitable for being integrally cast into a barrel of a hydrogen storage container after remelting, thereby reducing or eliminating welding joints to the greatest extent and improving the hydrogen embrittlement resistance of the hydrogen storage container under the hydrogen condition. Specifically, the master alloy bar has better hydrogen resistance, and can inherit the property to a hydrogen storage container prepared by taking the master alloy bar as a raw material. The grains of the master alloy bar are refined and uniformly distributed, and can be inherited into a casting structure, the finer the grains are, and the better the hydrogen embrittlement resistance of an austenite structure is; after twice vacuum melting, the purity of the master alloy bar is greatly improved, the content of harmful elements C, O, N, H is reduced, and the segregation of impurity elements in the subsequent casting process is reduced. For example, carbon element segregation can form carbides which are unevenly distributed and can interact with hydrogen, so that the probability of initiating hydrogen induced cracks is increased; after the twice vacuum melting, the density of the material is also improved, the occurrence of defects in the casting process, such as tiny holes, is reduced, and the casting quality is improved.
In some embodiments, the master alloy bar may, for example, employ a basic composition of 316L stainless steel, the composition of the master alloy bar being, in mass percent: less than or equal to 0.03 percent of C, less than or equal to 0.90 percent of Si, less than or equal to 1.85 percent of Mn, less than or equal to 0.006 percent of P, less than or equal to 0.004 percent of S, less than or equal to 0.004 percent of O, less than or equal to 0.005 percent of N, less than or equal to 16 percent of Cr, less than or equal to 17.5 percent of 12 percent of Ni, less than or equal to 14 percent of 2.3 percent of Mo, less than or equal to 3.0 percent of Fe and the balance.
In some embodiments, performing vacuum induction melting comprises:
Sequentially loading nickel-chromium intermediate alloy, carbon blocks, ferrosilicon, electrolytic manganese, molybdenum strips and pure iron into a vacuum induction furnace, wherein the content of P brought in by raw materials is controlled to be less than or equal to 0.006wt% and the content of S is controlled to be less than or equal to 0.004wt%;
When the vacuum degree in the vacuum induction furnace is less than 5Pa, starting to electrify and melt, heating to 1550+/-20 ℃ after raw materials are melted, starting to keep warm and refine, and electromagnetically stirring for at least 30min and controlling the vacuum degree to be less than 0.3Pa during refining;
when the content of N in the molten steel is less than or equal to 0.005wt% and the content of O is less than or equal to 0.004wt%, filling inert gas to ensure that the pressure in the vacuum induction furnace is 10000-13000 Pa, adding nickel-magnesium alloy for continuous deoxidization, carrying out electromagnetic stirring for 10min, carrying out electrified tapping, wherein the tapping temperature is 1530+/-10 ℃, and casting the molten steel into steel ingots.
In some embodiments, performing vacuum induction melting comprises: performing surface shot blasting treatment on the pure iron rod to remove oxide skin; the oxidized portion of the nickel-magnesium alloy is removed.
In some embodiments, performing vacuum induction melting comprises: before casting, the ingot mould is scalded by molten iron, and the molten steel is filtered in the casting process.
In some embodiments, performing the forging cogging includes:
Forging by fire: the self-consumption ingot obtained after vacuum self-consumption is subjected to heat preservation at 1170 ℃ for 45-55 min, then is upset to 45-55% of the height of the self-consumption ingot, and then is drawn to be an octagonal forging material with phi 410+/-10 mm;
Secondary forging: the octagonal forging material with phi 410 plus or minus 10mm is upsetted to 45 to 55 percent of the height of a consumable ingot after heat preservation for 45 to 55 minutes at 1170 ℃, and then is drawn to be the octagonal forging material with phi 265 plus or minus 10 mm;
Forging with three times of fire: the octagonal forging material with phi 265 plus or minus 10mm is heated for 45-55 min at 1170 ℃ and then is drawn to be the octagonal forging material with phi 200 plus or minus 10 mm;
Forging four times: and (3) preserving heat of the octagonal forging material with phi 200+/-10 mm for 45-55 min at 1170 ℃ and then drawing the octagonal forging material to a square forging material with the cross section side length of 150-160 mm, wherein the final forging temperature is more than or equal to 830 ℃.
In some embodiments, performing the forging cogging includes: the consumable ingot was diffusion annealed at 1180.+ -. 20 ℃ for at least 24 hours and then kept at 1130.+ -. 15 ℃ for 3 hours before being forged over a fire.
In some embodiments, performing the rolling into a log comprises: and heating the square forging material to 1130+/-15 ℃ and preserving heat for 3 hours, then rolling, wherein the initial rolling temperature is more than or equal to 1060 ℃, and rolling into bars with the specification of phi 65-75 mm through 6 passes.
In some embodiments, performing the rolling into a log comprises: and (3) carrying out surface finishing processing on the bar with the specification of phi 65-75 mm to obtain the hydrogen-resistant stainless steel master alloy bar.
The invention also provides a hydrogen storage container, and the cylinder of the hydrogen storage container is obtained by remelting the hydrogen-resistant stainless steel master alloy bar prepared by the method and then integrally casting and forming.
In summary, the invention develops a cast master alloy bar for the hydrogen-resistant stainless steel aiming at the typical brand 316L in the austenitic stainless steel, which is mainly used as a smelting raw material for integrated casting. By mother alloy smelting and integrated casting, the number of welded joints can be greatly reduced while high-quality workpieces with complex shapes are obtained, and the crack initiation probability of austenitic stainless steel in a hydrogen environment is reduced, so that the service life of the material in the complex hydrogen environment is prolonged.
The following description is made with reference to specific examples.
Example 1
The embodiment provides a preparation method of a hydrogen-resistant stainless steel master alloy bar, which comprises the following detailed steps:
(1) Selecting raw materials including carbon blocks, pure iron bars, ferrosilicon, nickel-chromium intermediate alloy, molybdenum bars, electrolytic manganese and nickel-magnesium intermediate alloy, wherein the P content and the S content of the raw material are controlled to be 60ppm and 40ppm respectively. Performing surface shot blasting treatment on the pure iron rod to remove oxide skin; and removing the off-white oxidized part of the nickel-magnesium alloy.
(2) Sequentially loading nickel-chromium intermediate alloy, carbon blocks, ferrosilicon, electrolytic manganese, molybdenum strips and pure iron into a vacuum induction furnace in order, so as to avoid raw material bridging; a crucible with the diameter of 1.5t is adopted, and the diameter of the ingot mould is 360mm; and vacuumizing the induction furnace smelting chamber, and when the vacuum degree is less than 5Pa, starting to heat the furnace burden by feeding electricity, and linearly increasing the feeding power to gradually melt the metal raw material.
(3) Heating the raw materials to 1550+/-20 ℃ after melting the raw materials, and starting heat preservation refining, wherein electromagnetic stirring is performed for at least 30min in the refining process; the vacuum degree is less than 0.3Pa during refining, good degassing effect is maintained, when the content of N in the molten steel is 50ppm and the content of O is 40ppm in the sampling analysis, high-purity argon is filled until the pressure in the vacuum induction furnace is 10000-13000 Pa, nickel-magnesium alloy is added for continuous deoxidation, the steel is charged after electromagnetic stirring for 10min, and the steel tapping temperature is 1530+/-10 ℃.
(4) Adopting three-stage baffles to carry out filtering casting, scalding the ingot mould before casting by molten iron, keeping the surface of the ingot mould clean and free from oxidation, allowing breaking of air (breaking the vacuum state in the furnace) after furnace cooling for 3 hours after casting, and demoulding after slow cooling for at least 2 hours after breaking of air; cutting off the head and the tail of the vacuum induction electrode rod, and cleaning the surface of the steel ingot until the steel ingot is bright.
(5) And (3) putting the treated electrode rod into a vacuum consumable furnace with the diameter phi of 410mm of a crystallizer for remelting, and forming a molten pool within 1h by adopting high current (8 kA) at the beginning of the melting stage. Entering a stable smelting stage, keeping an electric arc stable, keeping the vacuum degree at 0.08-0.22 Pa, the metal melting speed at 3.4-4.3 kg/min, and the number of molten drops at 3.5-4.2 drops/s; cooling for 2h along with the furnace after smelting; and after the molten steel is completely solidified, discharging the molten steel from the furnace for air cooling, and polishing the surface of the cast ingot for standby after the molten steel is cooled to room temperature.
(6) Carrying out high-temperature diffusion annealing on the vacuum consumable ingot at 1180+/-20 ℃ for 24 hours to promote homogenization of steel ingot components; then the temperature is adjusted to 1130+/-15 ℃ for 3 hours, and then the cogging is carried out. After the steel ingot is discharged from the furnace, the whole steel ingot is deformed by light pressure along the radial direction, the clamp is arranged at the dead head end, the tail end is cut off by 120mm, the furnace is returned for heat preservation for 55min, and the furnace temperature is 1170 ℃.
(7) Upsetting the ingot to 45% of the initial height of a consumable ingot after discharging the ingot from the furnace by fire, then drawing the ingot to a phi 410+/-10 mm octagonal shape, returning the furnace to heat preservation for 55min, and keeping the furnace temperature at 1170 ℃; and upsetting again to half the height of the cast ingot after discharging from the furnace by the second fire, then drawing to be in an octagonal shape with phi 265 plus or minus 10mm, returning to the furnace, preserving heat for 55min, and keeping the furnace temperature at 1170 ℃.
(8) Drawing out the phi 265 plus or minus 10mm octagonal section bar to phi 200 plus or minus 10mm octagonal shape after discharging the three-fire furnace, returning the furnace to keep the temperature for 55min, and keeping the furnace temperature at 1170 ℃; and drawing the octagonal forging material with phi of 200+/-10 mm to square forging material with the cross section of 150 multiplied by 150mm after the four-fire furnace is taken out, cutting off pliers handles, and placing the square forging material in a pebble field, spreading out and air cooling to room temperature.
(9) Heating a square forged material with the length of 150 multiplied by 150mm to 1130+/-15 ℃, preserving heat for 3 hours, starting rolling at 1080 ℃, discharging, performing 6 passes on the forged material with the length of 150mm by one fire, and rolling into a bar with the specification of phi 65 mm; the head and tail of the hot saw bar are respectively about 50mm, the bar is placed in a pebble field for spreading and air cooling to room temperature, the diameter of the bar is measured by roundness, and the head and tail errors are all less than 4%; and polishing the hot rolled bar by a machine tool to obtain the hydrogen-resistant stainless steel casting master alloy bar with the specification phi of 60 mm.
In the embodiment, the master alloy rod has uniform structure (the grain size is 8 grade, the grade difference is 1 grade), and the purity is well controlled, wherein the P content is 60ppm, the S content is 38ppm, the O content is 33ppm, the N content is 42ppm, the C content is 0.03%, the Si content is 0.9%, the Mn content is 1.85%, the Cr content is 17.5%, the Ni content is 14%, and the Mo content is 3.0%; the surface quality of the bar is good, and the ultrasonic nondestructive inspection meets the A-level requirement in GB/T4162-2022.
Example 2
The embodiment provides a preparation method of a hydrogen-resistant stainless steel master alloy bar, which comprises the following detailed steps:
(1) Selecting raw materials including carbon blocks, pure iron bars, ferrosilicon, nickel-chromium intermediate alloy, molybdenum bars, electrolytic manganese and nickel-magnesium intermediate alloy, and controlling the P content and the S content of the raw material carrying-in amount to be 58ppm and 39ppm. Performing surface shot blasting treatment on the pure iron rod to remove oxide skin; and removing the off-white oxidized part of the nickel-magnesium alloy.
(2) Sequentially loading nickel-chromium intermediate alloy, carbon blocks, ferrosilicon, electrolytic manganese, molybdenum strips and pure iron into a vacuum induction furnace in order, so as to avoid raw material bridging; a crucible with the diameter of 1.5t is adopted, and the diameter of the ingot mould is 360mm; and vacuumizing the induction furnace smelting chamber, and when the vacuum degree is less than 5Pa, starting to heat the furnace burden by feeding electricity, and linearly increasing the feeding power to gradually melt the metal raw material.
(3) Heating the raw materials to 1550+/-20 ℃ after melting the raw materials, and starting heat preservation refining, wherein electromagnetic stirring is performed for at least 30min in the refining process; the vacuum degree is less than 0.3Pa during refining, good degassing effect is maintained, when the N content in the molten steel is 48ppm and the O content is 38ppm in the sampling analysis, 10000-13000 Pa of high-purity argon is filled, nickel-magnesium alloy is added for continuous deoxidization, the steel is charged after electromagnetic stirring for 10min, and the steel tapping temperature is 1530+/-10 ℃.
(4) Adopting three-stage baffles to carry out filtration casting, scalding the ingot mould before casting by molten iron, keeping the surface of the ingot mould clean and free from oxidation, allowing breaking the blank after 3 hours of furnace cooling after casting, and demoulding after at least 2 hours of slow cooling after breaking the blank; cutting off the head and the tail of the vacuum induction electrode rod, and cleaning the surface of the steel ingot until the steel ingot is bright.
(5) And (3) putting the treated electrode rod into a vacuum consumable furnace with the diameter of phi 410 mm of a crystallizer for remelting, and forming a molten pool within 1h by adopting high current (12 kA) at the beginning of the melting stage. Entering a stable smelting stage, keeping an electric arc stable, keeping the vacuum degree at 0.22-0.4 Pa, the metal melting speed at 4.3-5.6 kg/min, and the number of molten drops at 4.2-5.2 drops/s; cooling for 2h along with the furnace after smelting; and after the molten steel is completely solidified, discharging the molten steel from the furnace for air cooling, and polishing the surface of the cast ingot for standby after the molten steel is cooled to room temperature.
(6) Carrying out high-temperature diffusion annealing on the vacuum consumable ingot at 1180+/-20 ℃ for 24 hours to promote homogenization of steel ingot components; then the temperature is adjusted to 1130+/-15 ℃ for 3 hours, and then the cogging is carried out. After the steel ingot is discharged from the furnace, the whole steel ingot is deformed by light pressure along the radial direction, the clamp is arranged at the riser end, the tail end is cut off by 140mm, the furnace is returned for heat preservation for 45min, and the furnace temperature is 1170 ℃.
(7) Upsetting the ingot to 55% of the initial height of a consumable ingot after discharging the ingot from the furnace by fire, then drawing the ingot to phi 410+/-10 mm octagonal, returning the furnace to heat preservation for 45min, and keeping the furnace temperature at 1170 ℃; and upsetting again to about half of the height of the cast ingot after discharging from the furnace by the second fire, then drawing to be in an octagonal shape with phi 275+/-10 mm, returning to the furnace, preserving heat for 45min, and keeping the furnace temperature at 1170 ℃.
(8) Drawing out the phi 275+/-10 mm octagonal section bar to be in a phi 210+/-10 mm octagonal shape after discharging the three fires, returning the furnace to keep the temperature for 45min, and keeping the furnace temperature at 1170 ℃; and drawing the octagonal forging material with phi 210+/-10 mm out of the furnace by four fires until the cross section of the octagonal forging material is 160 multiplied by 160mm, cutting off pliers handles, and placing the square forging material in a pebble field for spreading and air cooling to room temperature.
(9) Heating a 160X 160mm square forging material to 1130+/-15 ℃ and preserving heat for 3 hours, wherein the initial rolling temperature is 1071 ℃, discharging the square forging material, and performing 6 passes on the square forging material with the primary fire, and rolling the square forging material into bars with phi 75mm specifications; the head and tail of the hot saw bar are respectively about 50mm, the bar is placed in a pebble field for spreading and air cooling to room temperature, the diameter of the bar is measured by roundness, and the head and tail errors are all less than 4%; and polishing the hot rolled bar by a machine tool to obtain the hydrogen-resistant stainless steel casting master alloy bar with the specification phi of 70 mm.
In the embodiment, the master alloy rod has uniform structure (the grain size is 7 grade, the grade difference is 1 grade), and the purity is well controlled, wherein the P content is 58ppm, the S content is 37ppm, the O content is 31ppm, and the N content is 40ppm; 0.025% of C, 0.81% of Si, 1.73% of Mn, 16% of Cr, 12% of Ni and 2.3% of Mo; the surface quality of the bar is good, and the ultrasonic nondestructive inspection meets the A-level requirement in GB/T4162-2022.
Those of ordinary skill in the art will appreciate that: the above discussion of any embodiment is merely exemplary and is not intended to imply that the scope of the disclosure of embodiments of the invention, including the claims, is limited to such examples; combinations of features of the above embodiments or in different embodiments are also possible within the idea of an embodiment of the invention, and there are many other variations of the different aspects of the embodiments of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, equivalent substitutions, improvements, and the like, which are made within the spirit and principles of the embodiments of the invention, are included within the scope of the embodiments of the invention.
Claims (10)
1. The preparation method of the hydrogen-resistant stainless steel master alloy bar is characterized in that the master alloy bar is used for being integrally cast and molded into a cylinder of a hydrogen storage container after remelting; the master alloy bar comprises the following components in percentage by mass: p is less than or equal to 0.006%, S is less than or equal to 0.004%, O is less than or equal to 0.004%, and N is less than or equal to 0.005%; after ultrasonic nondestructive inspection, the master alloy bar meets the A-level requirement in GB/T4162-2022; the method comprises the following steps:
Sequentially carrying out vacuum induction melting, vacuum consumable melting, forging cogging and rolling to obtain a master alloy bar;
wherein, carry out vacuum consumable smelting and include: in the initial melting stage, forming a molten pool within 1h by adopting a large current of 8-12 kA; in the stable smelting stage, keeping the electric arc stable, controlling the vacuum degree to be 0.08-0.4 Pa, the metal melting speed to be 3.4-5.6 kg/min, and the number of molten drops to be 3.5-5.2 drops/s;
The master alloy bar comprises the following components in percentage by mass: less than or equal to 0.03 percent of C, less than or equal to 0.90 percent of Si, less than or equal to 1.85 percent of Mn, less than or equal to 0.006 percent of P, less than or equal to 0.004 percent of S, less than or equal to 0.004 percent of O, less than or equal to 0.005 percent of N, less than or equal to 16 percent of Cr, less than or equal to 17.5 percent of 12 percent of Ni, less than or equal to 14 percent of 12 percent, less than or equal to 2.3 percent of Mo, less than or equal to 3.0 percent of Fe and the balance of Fe;
performing vacuum induction melting includes:
Sequentially loading nickel-chromium intermediate alloy, carbon blocks, ferrosilicon, electrolytic manganese, molybdenum strips and pure iron into a vacuum induction furnace, wherein the content of P brought in by raw materials is controlled to be less than or equal to 0.006wt% and the content of S is controlled to be less than or equal to 0.004wt%;
When the vacuum degree in the vacuum induction furnace is less than 5Pa, starting to electrify and melt, heating to 1550+/-20 ℃ after raw materials are melted, starting to keep warm and refine, and electromagnetically stirring for at least 30min and controlling the vacuum degree to be less than 0.3Pa during refining;
When the sampling analysis is carried out and the N content is less than or equal to 0.005wt% and the O content is less than or equal to 0.004wt%, inert gas is filled to ensure that the pressure in the vacuum induction furnace is 10000-13000 Pa, nickel-magnesium alloy is added for continuous deoxidization, electrified tapping is carried out after electromagnetic stirring is carried out for 10min, the tapping temperature is 1530+/-10 ℃, and then the molten steel is cast into steel ingots;
Forging cogging includes:
Forging by fire: the self-consumption ingot obtained after vacuum self-consumption is subjected to heat preservation at 1170 ℃ for 45-55 min, then is upset to 45-55% of the height of the self-consumption ingot, and then is drawn to be an octagonal forging material with phi 410+/-10 mm;
Secondary forging: the octagonal forging material with phi 410 plus or minus 10mm is upsetted to 45 to 55 percent of the height of a consumable ingot after heat preservation for 45 to 55 minutes at 1170 ℃, and then is drawn to be the octagonal forging material with phi 265 plus or minus 10 mm;
Forging with three times of fire: the octagonal forging material with phi 265 plus or minus 10mm is heated for 45-55 min at 1170 ℃ and then is drawn to be the octagonal forging material with phi 200 plus or minus 10 mm;
Forging four times: and (3) preserving heat of the octagonal forging material with phi 200+/-10 mm for 45-55 min at 1170 ℃ and then drawing the octagonal forging material to a square forging material with the cross section side length of 150-160 mm, wherein the final forging temperature is more than or equal to 830 ℃.
2. The method of claim 1, wherein performing vacuum induction melting comprises: performing surface shot blasting treatment on the pure iron rod to remove oxide skin; the oxidized portion of the nickel-magnesium alloy is removed.
3. The method of claim 1, wherein performing vacuum induction melting comprises: before casting, the ingot mould is scalded by molten iron, and the molten steel is filtered in the casting process.
4. The method of claim 1, wherein performing forging cogging comprises: the consumable ingot was diffusion annealed at 1180.+ -. 20 ℃ for at least 24 hours and then kept at 1130.+ -. 15 ℃ for 3 hours before being forged over a fire.
5. The method of claim 1, wherein performing a rolling pass comprises: and heating the square forging material to 1130+/-15 ℃ and preserving heat for 3 hours, then rolling, wherein the initial rolling temperature is more than or equal to 1060 ℃, and rolling into bars with the specification of phi 65-75 mm through 6 passes.
6. The method of claim 5, wherein performing a rolling pass comprises: and (3) carrying out surface finishing processing on the bar with the specification of phi 65-75 mm to obtain the hydrogen-resistant stainless steel master alloy bar.
7. The method according to claim 1, wherein the master alloy bar has a grain size of not less than 7 grades and a grain size difference of not more than 1 grade.
8. The method of claim 1, wherein performing vacuum consumable smelting comprises: in the beginning of the melting stage, a molten pool is formed within 1h by adopting a large current of 8 kA; in the stable smelting stage, the electric arc is kept stable, the vacuum degree is controlled to be 0.08-0.22 Pa, the metal melting speed is 3.4-4.3 kg/min, and the number of molten drops is 3.5-4.2 drops/s.
9. The method of claim 1, wherein performing vacuum consumable smelting comprises: in the initial melting stage, a molten pool is formed within 1h by adopting a large current of 12 kA; in the stable smelting stage, the electric arc is kept stable, the vacuum degree is controlled to be 0.22-0.4 Pa, the metal melting speed is controlled to be 4.3-5.6 kg/min, and the number of molten drops is controlled to be 4.2-5.2 drops/s.
10. A hydrogen storage container, characterized in that a cylinder of the hydrogen storage container is obtained by remelting and integrally casting a hydrogen-resistant stainless steel master alloy bar prepared by the method of any one of claims 1 to 9.
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