CN113263173A - Manufacturing process for high-strength hydrogen embrittlement-resistant additive manufacturing stainless steel - Google Patents
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 50
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 50
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 41
- 239000010935 stainless steel Substances 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 239000000654 additive Substances 0.000 title claims abstract description 24
- 230000000996 additive effect Effects 0.000 title claims abstract description 24
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- 238000010438 heat treatment Methods 0.000 claims abstract description 18
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- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 238000010146 3D printing Methods 0.000 claims abstract description 4
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 4
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 4
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 229910000963 austenitic stainless steel Inorganic materials 0.000 claims description 6
- 238000002474 experimental method Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000005429 filling process Methods 0.000 claims description 2
- 238000000861 blow drying Methods 0.000 claims 1
- 238000004140 cleaning Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 238000005498 polishing Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 3
- 239000007769 metal material Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 5
- 239000011733 molybdenum Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
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- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 229910003178 Mo2C Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
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- 238000007669 thermal treatment Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- B22F1/0003—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/20—Post-treatment, e.g. curing, coating or polishing
-
- 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
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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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
- C22C38/02—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
-
- 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
- C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/247—Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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Abstract
The invention discloses a manufacturing process of high-strength hydrogen embrittlement-resistant additive manufacturing stainless steel, and belongs to the field of additive manufacturing of metal materials. The additive manufacturing stainless steel comprises the following chemical components in percentage by weight: c: less than or equal to 0.03 percent, less than or equal to 2 percent of Mn, less than or equal to 0.045 percent of P, less than or equal to 0.03 percent of S, less than or equal to 0.75 percent of Si, 15-17 percent of Cr, 12-14 percent of Ni, 3-3.5 percent of Mo, N: 0.2-0.3%, and the balance of Fe and inevitable impurities. The manufacturing process comprises the following steps: 3D printing process and heat treatment process. The high-strength hydrogen embrittlement-resistant stainless steel material has the advantages that compared with the traditional stainless steel material, the high-strength hydrogen embrittlement-resistant stainless steel material can realize high strength and hydrogen embrittlement resistance, and compared with the traditional material increase manufacturing stainless steel material, the high-strength hydrogen embrittlement-resistant stainless steel material has the performance in both aspects.
Description
Technical Field
The invention belongs to the field of additive manufacturing of metal materials, and particularly relates to a manufacturing process of high-strength hydrogen embrittlement-resistant additive manufacturing stainless steel.
Background
In the nuclear power field, many key parts have the characteristics of complex structure, high manufacturing difficulty, high bearing load, harsh service environment and the like, and the traditional manufacturing technology is difficult to simultaneously meet the comprehensive requirements of the parts in various aspects such as structural complexity, strong plasticity, hydrogen embrittlement resistance and the like. Therefore, it is urgently needed to develop a novel manufacturing technology which can process a complex structure and obtain high strength and hydrogen embrittlement resistance.
Selective Laser Melting (SLM) is a mature metal additive manufacturing technology, and the austenitic stainless steel prepared by the SLM has the advantages of high processing freedom, excellent printing quality and the like, and is suitable for manufacturing complex parts. At present, the mechanical properties of the SLM stainless steel are far beyond those of the traditional process materials, which provides possibility for the application of the austenitic stainless steel in the complex parts through additive manufacturing. However, the corrosion resistance and the performance stability of the prior additive manufactured austenitic stainless steel are poor, and many research results show that the corrosion resistance of the SLM stainless steel is weaker than that of the SLM stainless steel material prepared by the traditional process with the same components, and the hydrogen brittleness performance of the SLM stainless steel under different printing conditions has great difference, so that the application hidden danger of the SLM stainless steel in the fields of nuclear power, hydrogen energy and the like is greatly increased. It can be seen that the problem of corrosion resistance of SLM stainless steels is an important obstacle limiting their application in high pressure, high hydrogen embrittlement environments.
The hydrogen embrittlement resistance of SLM austenitic stainless steel is closely related to its microstructure, including the trans-scale interfaces (bath boundaries, grain boundaries, dislocation-rich cellular boundaries, etc.), elemental segregation and microscopic defects. The cross-scale interface affects hydrogen embrittlement sensitivity on one hand and strong plasticity on the other hand, so that the cross-scale interface can be used as an intermediate bridge for obtaining high-strength hydrogen embrittlement resistance in stainless steel additive manufacturing, the structure of the cross-scale interface is complex, the influence of the cross-scale interface on hydrogen embrittlement behavior is not known, and factors influencing the cross-scale interface are more, which brings great difficulty to effective regulation and control. Therefore, the influence mechanism of the cross-scale interface structure of the additive manufacturing stainless steel on the hydrogen embrittlement behavior and the high-strength hydrogen embrittlement resistance regulation mechanism are the key problems to be solved at present.
Disclosure of Invention
The invention aims to overcome the defects in the background technology and provides a method for developing high-strength hydrogen embrittlement-resistant additive manufacturing stainless steel.
The additive manufacturing stainless steel comprises the following chemical components in percentage by weight: c: less than or equal to 0.03 percent, less than or equal to 2 percent of Mn, less than or equal to 0.045 percent of P, less than or equal to 0.03 percent of S, less than or equal to 0.75 percent of Si, 15-17 percent of Cr, 12-14 percent of Ni, 3-3.5 percent of Mo, and N: 0.2-0.3%, and the balance of Fe and inevitable impurities.
Therefore, compared with the chemical components of the traditional stainless steel metal powder, the alloy element molybdenum is added, and a certain nitrogen content is added. The main functions and the proportion are as follows:
molybdenum: on the one hand, molybdenum can improve the corrosion resistance of a matrix structure, and particularly the pitting corrosion resistance of the material. On the other hand, in the case of a liquid,fe can be precipitated in the aging process2Mo、Ni3Mo、Mo2C and the like, thereby improving the tempering stability and the secondary hardening effect of the steel. But too high a molybdenum content may promote
Ferrite formation adversely affects the performance. Comprehensively, the molybdenum content of the invention is 2-3%.
Nitrogen: first, in terms of texture properties, the effect of nitrogen on the texture of stainless steel substrates is strong. This effect of nitrogen makes it possible to replace part of the nickel in stainless steels, to reduce the ferrite content of the steel, to make the austenite more stable, to prevent the precipitation of harmful intermetallic phases and to avoid martensitic transformation even under cold working conditions. In the aspect of mechanical property, nitrogen does not reduce the plasticity and toughness of the material while obviously improving the strength of the stainless steel. Finally, the beneficial effects of nitrogen on the corrosion resistance of stainless steel in the aspect of hydrogen embrittlement resistance are shown in intergranular hydrogen embrittlement resistance, point hydrogen embrittlement resistance and gap hydrogen embrittlement resistance.
The process involved in the invention is as follows:
1. the powder parameters are C: less than or equal to 0.03 percent, less than or equal to 2 percent of Mn, less than or equal to 0.045 percent of P, less than or equal to 0.03 percent of S, less than or equal to 0.75 percent of Si, 15-17 percent of Cr, 12-14 percent of Ni, 3-3.5 percent of Mo, 0.10 percent of N, and the balance of Fe and inevitable impurities, wherein the powder granularity meets the following requirements: d10: 17.99, D50: 31.8, D90: 53.3, no hollow powder, the sphericity of more than 95 percent, the fluidity of 17.18S/50g determined by Hall experiment, no inclusion detected and the oxygen content of 186 PPM.
The 2.3D printing process adopts EOS M290 equipment, a Yb-fiber laser, 400W of power 300-.
3. Heat treatment process SLM additive manufactured 316L austenitic stainless steel was made into required size samples with wire cutting equipment and the experiments were placed in a muffle furnace filled with argon (argon is used to protect the samples from oxidation). The heating rate of the heat treatment is 10 ℃ per minute until the temperature is raised to 500 ℃ and 1100 ℃, and the temperature is kept for 4 hours.
The invention has the following advantages:
1. compared with the traditional stainless steel material, can realize high strength and hydrogen embrittlement resistance
The mechanical property indexes are as follows: after the 316L stainless steel is subjected to heat treatment, the yield strength is not lower than 450MPa, the tensile strength is higher than 700MPa, and the elongation exceeds 35%. The product of strength and elongation is 2 times more than that of common 316L stainless steel.
Hydrogen embrittlement resistance performance index: in the environment of 5 percent NaCl, the relative elongation of the stainless steel manufactured by additive manufacturing after heat treatment and hydrogen charging is 76.03 percent,
compared with the traditional additive manufacturing stainless steel material, the high-strength hydrogen embrittlement-resistant stainless steel material has the advantages of high strength and hydrogen embrittlement resistance.
In sum, the SLM SS316L subjected to subcritical heat treatment at 950 ℃ has excellent mechanical properties and hydrogen embrittlement resistance.
Drawings
FIG. 1 mechanical property curves for a non-heat treated SLM SS316L pattern;
FIG. 2 mechanical property curves of a heat treated SLM SS316L pattern.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
Example 1
1. The powder parameters are C: 0.025 percent, Mn 2 percent, P0.04 percent, S0.03 percent, Si 0.65 percent, Cr 17 percent, Ni 12 percent,
3.4% of Mo, 0.10% of N, and the balance of Fe and inevitable impurities, wherein the powder granularity meets the following requirements: d10: 17.99, D50: 31.8, D90: 53.3, no hollow powder, the sphericity of more than 95 percent, the fluidity of 17.18S/50g determined by Hall experiment, no inclusion detected and the oxygen content of 186 PPM.
The 2.3D printing process adopts EOS M290 equipment, a Yb-fiber optical fiber laser, 400W of power, 250um of spot diameter, 200W of scanning power, 0.08mm of scanning interval, 950mm/s of scanning speed and 0.04mm of powder laying and settling thickness.
3. Thermal treatment process, the experiment was placed in a muffle furnace filled with argon (argon is used to protect the sample from oxidation). The heating rate of the heat treatment is 10 ℃ per min until the temperature is raised to 950 ℃, and the temperature is kept for 4 hours.
4. The hydrogen filling process is to mechanically polish (remove oxide layer) the sample after heat treatment at 950 ℃, ultrasonically clean with alcohol or acetone, and blow-dry. Placing into a hydrogen-filled kettle, vacuumizing for 30min, introducing hydrogen, heating to 300 deg.C (25 deg.C, and filling hydrogen 9.4 Mpa). Finally, charging hydrogen at 18MPa for 14 days. (calculation according to PV = NRT)
Example 2
Example 2 is identical to example 1 in powder composition and printing process, except that this example does not carry out hydrogen charging, and the other contents are identical to those of example 1.
Example 3
Example 3 is different from example 1 in that this example does not perform heat treatment and hydrogen charging, and the other contents are the same as those of example 1.
Example 4
Forged specimens of the same dimensions as in examples 1,2 and 3.
As can be seen from FIG. 1, the elongation of both the normal 316L stainless steel and the SLM316L stainless steel is reduced after charging hydrogen, which indicates that the plasticity is also reduced. As can be seen from FIG. 2, the elongation of the non-charged 950 ℃ heat-treated sample exceeds 100%, and the sample has excellent plasticity, while the elongation of the two groups of the non-charged 950 ℃ heat-treated samples after charging hydrogen is reduced compared with that of the non-charged sample, but the reduction ratio is not large, which indicates that the SLM316L stainless steel subjected to 950 ℃ heat treatment in air and 5% NaCl solution after charging hydrogen still has excellent plasticity, and further indicates that the heat treatment can improve the hydrogen embrittlement resistance of the SLM316L stainless steel.
Claims (6)
1. A manufacturing process of high-strength hydrogen embrittlement-resistant additive manufactured stainless steel comprises the following steps:
(1) raw material powders were prepared as follows,
c: less than or equal to 0.03 percent, less than or equal to 2 percent of Mn, less than or equal to 0.045 percent of P, less than or equal to 0.03 percent of S, less than or equal to 0.75 percent of Si, 15-17 percent of Cr, 12-14 percent of Ni, 3-3.5 percent of Mo, N: 0.2-0.3%, the balance being Fe and inevitable impurities, the powder particle size satisfying: d10: 17.99, D50: 31.8, D90: 53.3, no hollow powder, the sphericity of more than 95 percent, the fluidity of 17.18S/50g determined by Hall experiment, and the oxygen content of 186 PPM;
(2) 3D printing process
EOS M290 equipment and a Yb-fiber laser are adopted, the power is 300-;
(3) heat treatment process
Manufacturing 316L austenitic stainless steel by SLM additive manufacturing into a sample with a required size by using linear cutting equipment, and putting an experiment into a muffle furnace filled with argon;
(4) hydrogen filling process
Mechanically polishing the sample subjected to heat treatment at 950 ℃, ultrasonically cleaning the sample by using alcohol or acetone, blow-drying the sample, putting the sample into a hydrogen filling kettle, vacuumizing the kettle, introducing hydrogen, starting to heat up the kettle, and heating to 300 ℃.
2. The process for manufacturing a high-strength hydrogen embrittlement resistant additive manufactured stainless steel according to claim 1, wherein:
the temperature rise rate of the heat treatment in the step (3) is 10 ℃ per minute.
3. The process for manufacturing a high-strength hydrogen embrittlement resistant additive manufactured stainless steel according to claim 1, wherein:
in the step (3), the temperature is raised to 500-1100 ℃.
4. The process for manufacturing a high-strength hydrogen embrittlement resistant additive manufactured stainless steel according to claim 1, wherein:
keeping the temperature constant for 4 hours in the step (3).
5. The process for manufacturing a high-strength hydrogen embrittlement resistant additive manufactured stainless steel according to claim 1, wherein:
and (4) vacuumizing for 30 min.
6. The process for manufacturing a high-strength hydrogen embrittlement resistant additive manufactured stainless steel according to claim 1, wherein:
and (4) in the step (4), at the normal temperature of 25 ℃, the charging pressure is 9.4Mpa, the final charging is 18Mpa, and the charging time is 14 days.
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| CN114592158A (en) * | 2022-03-09 | 2022-06-07 | 上海理工大学 | Preparation method of novel 304L stainless steel material with strong proton irradiation resistance |
| CN114700499A (en) * | 2022-06-06 | 2022-07-05 | 北京煜鼎增材制造研究院有限公司 | Additive manufacturing method of nitrogen-controlled stainless steel |
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