CN115446331A - Method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder - Google Patents

Method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder Download PDF

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CN115446331A
CN115446331A CN202211153022.2A CN202211153022A CN115446331A CN 115446331 A CN115446331 A CN 115446331A CN 202211153022 A CN202211153022 A CN 202211153022A CN 115446331 A CN115446331 A CN 115446331A
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powder
nitrogen
mixed powder
stainless steel
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CN115446331B (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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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
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    • 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
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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Abstract

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

Description

Method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder
Technical Field
The invention relates to the technical field of ferrous metallurgy, in particular to a method for preparing high-nitrogen stainless steel by pure metal powder selective laser melting.
Background
High nitrogen stainless steel is considered to be one of the most promising new engineering materials by virtue of its excellent corrosion resistance in various corrosion media, good comprehensive mechanical properties and excellent processability. The method is widely applied to various fields of bioenergy industry, aerospace, petrochemical industry, ocean engineering, biomedicine and the like. At present, the methods for preparing high-nitrogen steel at home and abroad comprise the following steps: nitrogen pressure melting, powder metallurgy, and surface nitriding; the nitrogen pressure smelting method is a method for preparing high-nitrogen steel, which has excellent product quality, but is limited by high-pressure manufacturing cost, complex equipment and the like.
The metal additive manufacturing technology is a preparation and processing technology which is based on a digital model and processes powder materials through a high-energy heat source to quickly build and form layer by layer, and a major breakthrough in the world manufacturing technical field in the last 30 years is regarded as a new technology for promoting the third industrial revolution of human beings. The Selective Laser Melting (SLM) technology is an important branch of metal additive manufacturing, and the SLM technology is a technological process in which high-power laser and metal powder materials are melted and solidified at a high speed and selective area-by-area superposition interaction is carried out.
Selective laser melting is applied to preparation high nitrogen stainless steel and can't directly obtain the high nitrogen stainless steel that nitrogen content is up to standard because of the nitrogen element spills over among the printing process, adopts the pressure boost mode to restrain nitrogen and spills over usually, but conventional 3D printing apparatus does not possess the pressure boost function. The solubility of nitrogen in liquid steel under atmospheric pressure is very low, the traditional smelting of high-nitrogen steel is not easy to carry out like other steels, and the direct production of high-nitrogen stainless steel by using conventional nitrogen-containing metal powder under normal pressure by an SLM (selective laser melting) process is difficult.
Therefore, a method for 3D printing of high-nitrogen stainless steel by using high-N-content powder is provided, and the problem of low nitrogen content in steel printed under normal pressure is a technical problem that needs to be solved by those skilled in the art.
Disclosure of Invention
In view of this, the invention provides a method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder on the basis of a powder process and a selective laser melting technology.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder comprises the following steps:
(1) Preparing a mixed powder 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 a over-mixed powder body;
(3) Putting 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 ℃;
(5) And taking out the sample after printing is finished, namely obtaining the high-nitrogen stainless steel.
Further, the target product in the step (1) comprises the following chemical components in percentage by mass: 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 0.01 percent of Ni, less than 0.1 percent of Si, less than 0.01 percent of P, less than 0.01 percent of S, and the balance of Fe.
The beneficial effect of adopting the above-mentioned further scheme lies in: the key points of the selective laser melting method for the over-mixed powder in the scheme of the invention are two aspects, namely, preparing a proper amount of over-mixed powder by a pure metal over-mixing method, accurately calculating the nitrogen overflow amount according to a nitrogen escape rate experiment, ensuring the nitrogen content after printing, and in order to obtain a product with the nitrogen content of 1%, the over-mixed powder with the over-mixed ratio of 1.4 is adopted, and the over-mixed powder with the nitrogen content of 1.4 is prepared; 2. and a reasonable selective laser melting solidification process is formulated, so that the segregation of nitrogen is reduced. In order to obtain accurate nitrogen content and ensure that nitrogen is uniformly distributed in steel, the overflow rate of nitrogen in the selective laser melting process is calculated, so that the over-mixed powder component is obtained. The reasonable selective laser melting process is obtained through an experimental method.
Further, the mixed powder raw materials comprise iron powder, chromium nitride, chromium powder, manganese powder and molybdenum powder.
Furthermore, 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 the above-mentioned further scheme lies in: the invention avoids the introduction of impurities by improving the accuracy of the mass percent of chemical components of the target product of the over-blended powder.
Furthermore, the particle size of the mixed powder raw material is 15-53 mu m.
The beneficial effect of adopting the above-mentioned further scheme lies in: because the over-mixed powder selective laser melting method depends on the over-mixed powder preparation method and the selective laser melting method, certain requirements are made on the particle size and the fluidity of the powder, and the particle size is the optimal particle size of selective laser melting.
Further, the ball milling rotation 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 the above-mentioned further scheme lies in: the operation can fully and uniformly mix the powder, enhance the fluidity and uniformity of the over-prepared powder and reduce the printing segregation.
Further, the printing parameters of the laser 3D printer in 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 over-matched powder to replace nickel with manganese and nitrogen, 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 pitting corrosion resistance, the stress corrosion resistance and other properties of the stainless steel material, and has higher yield and tensile strength.
The high-nitrogen stainless steel is prepared by using a mixed powder and selective laser melting method under the conventional 3D printing condition, and the nitrogen content of 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 mode through a powder preparation selective laser melting method, so that the nitrogen content in a product is ensured, and the cost for preparing the high-nitrogen steel printing powder is reduced; reaction pressure does not need to be increased in the reaction process, so that the printing reaction cost is reduced, and the safety is improved; by adjusting the element content of the mixed powder raw material, various high-nitrogen steel printing powder can be prepared, and the feasibility of high-nitrogen steel 3D printing 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 object provided by the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) The high nitrogen stainless steel powder target chemical composition is shown in table 1;
TABLE 1 elemental ratio (mass%) of target chemical components
Cr N Mn Mo Fe
18～19 1.4～1.5 11～12 3～3.5 Bal
(2) The overpreparation powder is prepared according to the target chemical component.
Weighing Fe, crN, mn, cr and Mo metal powder according to the mass ratio of the components in the required steel, wherein each 100 g of powder is mixed with Fe: crN: mn: cr: mo =66:10:11:10:3.
(3) And (3) preliminarily mixing the various powder weighed in proportion, and 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 over-mixed powder. The powder components are as follows in table 2:
TABLE 2 chemical composition (% by 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) And putting the over-prepared powder into a sub-bin of selective laser melting experimental equipment, preheating the substrate to 150 ℃, and using nitrogen as protective atmosphere. The process parameters of selective laser melting the block and forming the stretching piece are shown in the table 3, and the forming size of the block is 5 multiplied by 5mm. The tensile specimen dimensions are shown in figure 1. The figure of the formed object is shown in figure 2.
TABLE 3 Selective laser melting Block Forming parameters
Technological parameters Parameter selection
Laser power (W) 200、225、250、275、300
Scanning speed (mm/s) 800
Scanning interval (mm) 0.08
Powder thickness (mm) 0.03
(5) Testing of shaped articles 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 the Properties of shaped articles
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
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (7)

1. A method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder is characterized by comprising the following steps:
(1) Preparing a mixed powder 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 a over-mixed powder body;
(3) Putting the mixed over-prepared 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 ℃;
(5) And taking out the sample after printing is finished, thus obtaining the high-nitrogen stainless steel.
2. The method for preparing the high-nitrogen stainless steel by selective laser melting of the pure metal over-mixed powder according to claim 1, wherein the target product in the step (1) comprises the following chemical components in percentage by mass: 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 0.01 percent of Ni, less than 0.1 percent of Si, less than 0.01 percent of P, less than 0.01 percent of S, and the balance of Fe.
3. The method for preparing the high-nitrogen stainless steel by selective laser melting of the pure metal over-mixed powder according to claim 2, wherein the mixed powder raw materials comprise iron powder, chromium nitride, chromium powder, manganese powder and molybdenum powder.
4. The method for preparing the high-nitrogen stainless steel by selective laser melting of the pure metal over-mixed powder according to claim 3, wherein 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.
5. The method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder according to claim 3, wherein the particle size of the mixed powder raw material is 15-53 μm.
6. The method for preparing the high-nitrogen stainless steel through selective laser melting of the pure metal over-mixed powder according to claim 1, wherein the ball milling rotation speed of the rotary ball mill in the step (2) is 400-420r/min, and the ball milling time is 4-5h.
7. The method for preparing the high-nitrogen stainless steel by selective laser melting of the pure metal over-mixed powder according to claim 1, wherein the printing parameters of the laser 3D printer in the step (4) are as follows: 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.
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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
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WO2024060607A1 (en) * 2022-09-21 2024-03-28 华北理工大学 Method for preparing high-nitrogen stainless steel by selective laser melting of pure metal prepared powder

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