CN115446331B - Method for preparing high-nitrogen stainless steel by laser melting of pure metal powder through selected area - Google Patents

Method for preparing high-nitrogen stainless steel by laser melting of pure metal powder through selected area Download PDF

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CN115446331B
CN115446331B CN202211153022.2A CN202211153022A CN115446331B CN 115446331 B CN115446331 B CN 115446331B CN 202211153022 A CN202211153022 A CN 202211153022A CN 115446331 B CN115446331 B CN 115446331B
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powder
nitrogen
printing
percent
stainless steel
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CN115446331A (en
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赵定国
孙鑫
任建彪
王亚超
王书桓
倪国龙
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North China University of Science and Technology
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North China University of Science and Technology
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Priority to PCT/CN2023/089856 priority patent/WO2024060607A1/en
Priority to ZA2023/05299A priority patent/ZA202305299B/en
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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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • 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
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium 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
    • C22C38/38—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of 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
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Abstract

The invention discloses a method for preparing high-nitrogen stainless steel by laser melting of pure metal powder through a selected area, which comprises the following steps: preparing a powder mixing raw material according to the chemical composition of a target product; putting the mixed powder raw materials into a ball mill for ball milling and mixing to obtain blended powder; placing the mixed powder into a powder bin of a laser 3D printer; vacuumizing the cavity of the laser 3D printer, then filling nitrogen, and beginning printing after the substrate is preheated; and taking out the sample after printing is finished, namely the high-nitrogen stainless steel. The high-nitrogen printing powder is obtained by a powder preparation method through a powder preparation selecting laser melting method, so that the nitrogen content in the product is ensured, and the cost for preparing the high-nitrogen steel printing powder is reduced; the reaction pressure is not required to be increased in the reaction process, so that the printing reaction cost is reduced, and the safety is improved; through adjusting the content of the mixed powder raw material elements, various high-nitrogen steel printing powder can be prepared, and the feasibility of 3D printing of the high-nitrogen steel is improved.

Description

Method for preparing high-nitrogen stainless steel by laser melting of pure metal powder through selected area
Technical Field
The invention relates to the technical field of ferrous metallurgy, in particular to a method for preparing high-nitrogen stainless steel by laser melting of a pure metal powder passing through a selected area.
Background
The high-nitrogen stainless steel is considered as one of the most promising novel engineering materials by virtue of excellent corrosion resistance, good comprehensive mechanical properties and excellent processability in various corrosive media. The method is widely applied to the fields of bioenergy industry, aerospace industry, petrochemical industry, ocean engineering, biomedical industry and the like. At present, the method for preparing the high-nitrogen steel at home and abroad comprises the following steps: nitrogen pressure smelting, powder metallurgy and surface nitriding; the nitrogen pressure melting method is a method for producing high nitrogen steel, which is excellent in product quality, but is limited by high pressure production costs, complicated equipment, and the like.
The metal additive manufacturing technology is a preparation processing technology based on a digital model and capable of processing powder materials by a high-energy heat source and rapidly accumulating and forming layer by layer, and is a major breakthrough in the field of world manufacturing technology in recent 30 years, and is regarded as a new technology for promoting the third industrial revolution of human beings. Selective Laser Melting (SLM) is an important branch of metal additive manufacturing, and the SLM process is a process in which high-power laser and metal powder materials are melted and solidified at high speed and are interacted in a selective and layer-by-layer mode.
The selective laser melting is applied to preparing high-nitrogen stainless steel, the nitrogen content of which meets the standard cannot be directly obtained due to nitrogen element overflow in the printing process, the nitrogen overflow is usually restrained by adopting a pressurizing mode, but conventional 3D printing equipment does not have the pressurizing function. The solubility of nitrogen in liquid steel at atmospheric pressure is very low, traditional smelting of high nitrogen steel is not as easy as that of other steel, and the SLM process is difficult to directly produce high nitrogen stainless steel by using conventional nitrogen-containing metal powder at normal pressure.
Therefore, the method for 3D printing of high-nitrogen stainless steel by using the high-N-content powder solves the problem that the nitrogen content in the steel printed under normal pressure is low, and the technical problem to be solved by the person skilled in the art is needed to be solved.
Disclosure of Invention
Therefore, the invention provides a method for preparing high-nitrogen stainless steel by adopting pure metal powder passing selective laser melting on the basis of the powder process and the selective laser melting technology.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for preparing high-nitrogen stainless steel by laser melting of pure metal powder through a selected area comprises the following steps:
(1) Preparing a powder mixing raw material according to the chemical composition of a target product;
(2) Putting the mixed powder raw materials into a ball mill for ball milling and mixing to obtain blended powder;
(3) Placing the mixed powder into a powder bin of a laser 3D printer;
(4) Vacuumizing the cavity of the laser 3D printer, then filling nitrogen, and beginning printing after the substrate is preheated to 145-150 ℃;
(5) And taking out the sample after printing is finished, namely the high-nitrogen stainless steel.
Further, in the step (1), the chemical components of the target product by mass percent are as follows: less than or equal to 0.1 percent of C, 18 to 23 percent of Cr, 0.8 to 2.0 percent of N, 8 to 12 percent of Mn, 2 to 3.5 percent of Mo, less than or equal to 0.01 percent of Ni, less than or equal to 0.1 percent of Si, less than or equal to 0.01 percent of P, less than or equal to 0.01 percent of S, and the balance being Fe.
The beneficial effect of adopting above-mentioned further scheme lies in: the key points of the laser melting method of the powder selection area of the over-distribution in the scheme are that firstly, a proper amount of over-distribution powder is prepared by a pure metal over-distribution method, the overflow amount of nitrogen is accurately calculated according to a nitrogen escape rate experiment, the nitrogen content after printing is ensured, and in order to obtain a product with the nitrogen content of 1 percent, the over-distribution powder with the over-distribution ratio of 1.4 is adopted, and the over-distribution powder with the nitrogen content of 1.4 percent is prepared; 2. and a reasonable selective laser melting and solidifying process is formulated, so that the segregation of nitrogen is reduced. In order to obtain accurate nitrogen content and ensure even distribution of nitrogen in steel, the overflow rate of nitrogen in the selective laser melting process is calculated, so that the over-matched powder component is obtained. The reasonably selected area laser melting process is obtained through an experimental method.
Further, the powder mixture raw materials comprise iron powder, chromium nitride, chromium powder, manganese powder and molybdenum powder.
Further, the iron powder, the chromium powder and the molybdenum powder are spherical powder, and the chromium nitride powder and the manganese powder are irregular powder.
The purities of the iron powder, the chromium nitride, the chromium powder, the manganese powder and the molybdenum powder are all more than or equal to 99.0 percent.
The beneficial effect of adopting above-mentioned further scheme lies in: according to the invention, the mass percentage accuracy of chemical components of the powder target product is improved, so that the introduction of impurities is avoided.
Further, the particle size of the powder mixture raw material is 15-53 mu m.
The beneficial effect of adopting above-mentioned further scheme lies in: because the powder preparation method and the selective laser melting method are dependent on the powder preparation method and the selective laser melting method, certain requirements are imposed on the particle size and the fluidity of the powder, and the particle size is the optimal particle size for the selective laser melting.
Further, the ball milling rotating speed of the rotary ball mill in the step (2) is 400-420r/min, and the ball milling time is 4-5h.
The beneficial effect of adopting above-mentioned further scheme lies in: the operation can fully and uniformly mix the powder, enhance the fluidity and uniformity of the powder after being matched, and reduce printing segregation.
Further, the printing parameters of the laser 3D printer in the step (4) are: the laser power is 200W-300W, the scanning speed is 1000mm/s, the scanning interval is 0.08mm, and the thickness of the powder layer is 0.03mm.
The invention has the beneficial effects that: the invention adopts the selective laser melting method of the powder, adopts manganese and nitrogen to replace nickel, reduces the cost, improves the nitrogen content and the controllability of the nitrogen content of the high-nitrogen steel prepared by the selective laser melting method, effectively improves the performances of pitting corrosion resistance, stress corrosion resistance and the like of the stainless steel material, and has higher yield and tensile strength.
According to the invention, the high-nitrogen stainless steel is prepared under the conventional 3D printing condition by using the mixed powder and the selective laser melting method, so that the nitrogen content of the complex parts can be effectively improved.
Compared with other high-nitrogen steel preparation processes, the high-nitrogen printing powder is obtained by a powder preparation method through a powder preparation selecting laser melting method, so that the nitrogen content in the product is ensured, and the cost for preparing the high-nitrogen steel printing powder is reduced; the reaction pressure is not required to be increased in the reaction process, so that the printing reaction cost is reduced, and the safety is improved; through adjusting the content of the mixed powder raw material elements, various high-nitrogen steel printing powder can be prepared, and the feasibility of 3D printing of the high-nitrogen steel is improved.
Drawings
FIG. 1 is a schematic drawing of the dimensions of a tensile specimen provided by the present invention;
fig. 2 is a diagram of a molded article according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) The target chemical composition of the high nitrogen stainless steel powder is shown in table 1;
TABLE 1 target chemical composition elemental composition (mass%)
Cr N Mn Mo Fe
18～19 1.4～1.5 11～12 3～3.5 Bal
(2) The powder is prepared according to the target chemical composition.
Weighing Fe, crN, mn, cr, mo metal powder according to the mass ratio of the components in the required steel, wherein each 100 g of powder Fe: crN: mn: cr: mo=66: 10:11:10:3.
(3) And (3) carrying out preliminary mixing on various weighed powder in proportion, fully and uniformly mixing the powder by using a planetary ball mill for 4 hours at the rotating speed of 400r/min to obtain the prepared powder. The powder composition is shown in table 2 below:
TABLE 2 chemical composition (mass%) of high nitrogen nickel-free stainless steel powder
Si Cr N Mn Mo Ni C O S P Fe
0.04 18.64 1.472 9.06 3.23 0.006 0.069 0.002 0.005 0.03 Bal
(4) Placing the powder subjected to the distribution into a sorting bin of a selective laser melting experimental device, and preheating a base plate to 150 ℃ under the protection of nitrogen. The process parameters for forming the selected laser melted blocks and drawn pieces are shown in table 3, the block forming size was 5X 5mm. The tensile sample dimensions are shown in figure 1. The molded object is shown in FIG. 2.
TABLE 3 Selective laser melting Block Forming parameters
Process parameters Parameter selection
Laser power (W) 200、225、250、275、300
Scanning speed (mm/s) 800
Scanning interval (mm) 0.08
Powder spreading thickness (mm) 0.03
(5) Testing of the formed part for Nitrogen content
TABLE 4 Selective laser melting Block Forming parameters
power/W 200 225 250 275 300
Nitrogen content wt% 0.991 0.982 0.974 0.965 0.956
(6) Testing of formed part Performance
power/W 200 225 250 275 300
Tensile strength/MPa 927.9 976.3 992.1 1001.7 961.2
Yield strength/MPa 322.9 300.9 364.4 363.8 269.5
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.

Claims (3)

1. A method for preparing high-nitrogen stainless steel by laser melting of pure metal powder through a selected area is characterized in that,
the method comprises the following steps:
(1) Preparing a powder mixing raw material according to the chemical composition of a target product; the chemical components of the target product in percentage by mass are: less than or equal to 0.1 percent of C, 18 to 23 percent of Cr, 0.8 to 2.0 percent of N, 8 to 12 percent of Mn, 2 to 3.5 percent of Mo, 0.01 percent of Ni, 0.1 percent of Si, 0.01 percent of P, 0.01 percent of S and the balance of Fe; preparing powder by a pure metal overdistribution method, accurately calculating the nitrogen overflow amount according to a nitrogen escape rate experiment, ensuring the nitrogen content after printing, and preparing the overdistribution powder with the nitrogen content of 1.4% by adopting the overdistribution ratio of 1.4 to obtain a product with the nitrogen content of 1%; the mixed powder raw materials comprise iron powder, chromium nitride, chromium powder, manganese powder and molybdenum powder; the iron powder, the chromium powder and the molybdenum powder are spherical powder, and the chromium nitride powder and the manganese powder are irregular powder;
(2) Putting the mixed powder raw materials into a ball mill for ball milling and mixing to obtain blended powder;
(3) Placing the mixed powder into a powder bin of a laser 3D printer;
(4) Vacuumizing the cavity of the laser 3D printer, then filling nitrogen, and starting printing after the substrate is preheated to 145-150 ℃ without increasing reaction pressure in the reaction process; the printing parameters of the laser 3D printer are as follows: the laser power is 200-300W, the scanning speed is 1000mm/s, the scanning interval is 0.08mm, and the thickness of the powder layer is 0.03mm;
(5) And taking out the sample after printing is finished, namely the high-nitrogen stainless steel.
2. The method for preparing high-nitrogen stainless steel by laser melting of pure metal powder through a powder selection area according to claim 1, wherein the granularity of the powder mixing raw material is 15-53 microns.
3. The method for preparing high-nitrogen stainless steel by laser melting of pure metal powder passing through a powder selection area according to claim 1, wherein the ball milling speed of the ball mill in the step (2) is 400-420r/min, and the ball milling time is 4-5h.
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PCT/CN2023/089856 WO2024060607A1 (en) 2022-09-21 2023-04-21 Method for preparing high-nitrogen stainless steel by selective laser melting of pure metal prepared powder
ZA2023/05299A ZA202305299B (en) 2022-09-21 2023-05-15 Method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-matched powder

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