WO2024060607A1 - Method for preparing high-nitrogen stainless steel by selective laser melting of pure metal prepared powder - Google Patents

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

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WO2024060607A1
WO2024060607A1 PCT/CN2023/089856 CN2023089856W WO2024060607A1 WO 2024060607 A1 WO2024060607 A1 WO 2024060607A1 CN 2023089856 W CN2023089856 W CN 2023089856W WO 2024060607 A1 WO2024060607 A1 WO 2024060607A1
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powder
nitrogen
stainless steel
laser melting
selective laser
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PCT/CN2023/089856
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French (fr)
Chinese (zh)
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孙鑫
赵定国
任建彪
王亚超
王书桓
倪国龙
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华北理工大学
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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

Definitions

  • the invention relates to the technical field of iron and steel metallurgy, and specifically to a method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-matched powder.
  • High-nitrogen stainless steel is considered to be one of the most promising new engineering materials due to its excellent corrosion resistance, good comprehensive mechanical properties and excellent processing performance in a variety of corrosive media. It has been widely used in the bioenergy industry, aerospace, petrochemical industry, marine engineering, biomedical and other fields. At present, the methods used to prepare high-nitrogen steel at home and abroad include: nitrogen pressure smelting method, powder metallurgy method and surface nitriding method. Nitrogen pressure smelting method is a method for preparing high-nitrogen steel. The product quality is excellent, but because of its high The high-voltage manufacturing cost and equipment complexity are limited.
  • Metal additive manufacturing technology is a preparation and processing technology that is based on digital models and uses high-energy heat sources to process powder materials to rapidly accumulate layer by layer. It has been a major breakthrough in the world's manufacturing technology field in the past 30 years and is regarded as promoting the third generation of centuries. New technologies of the sub-industrial revolution. Selective laser melting technology (SLM) is an important branch of metal additive manufacturing.
  • SLM process is a process in which high-power laser and metal powder materials melt and solidify at high speed and selectively superimpose layer by layer.
  • Selective laser melting is used to prepare high-nitrogen stainless steel. Due to the overflow of nitrogen during the printing process, high-nitrogen stainless steel with up-to-standard nitrogen content cannot be directly obtained. Pressurization is usually used to suppress nitrogen overflow, but conventional 3D printing equipment does not have a pressurization function. The solubility of nitrogen in liquid steel under atmospheric pressure is very low. Traditional smelting of high-nitrogen steel is not as easy as other steels. Similarly, it is difficult for the SLM process to directly produce high-nitrogen stainless steel using conventional nitrogen-containing metal powders under normal pressure.
  • a method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder including the following steps:
  • the chemical composition of the target product described in step (1) is as follows in percentage by mass: C ⁇ 0.1%, Cr 18-23%, N 0.8-2.0%, Mn 8-12%, Mo 2-3.5%, Ni ⁇ 0.01%, Si ⁇ 0.1%, P ⁇ 0.01%, S ⁇ 0.01%, and the remainder is Fe.
  • the key to the selective laser melting method of over-matched powder in the above-mentioned solution of the present invention lies in two aspects.
  • the nitrogen escape rate experiment Accurately calculate the amount of nitrogen overflow to ensure the nitrogen content after printing.
  • the present invention uses an overmixing ratio of 1.4 powder and configures an overmixed powder with a nitrogen content of 1.4%; 2.
  • Formulate a reasonable selected laser Melting and solidification process reduces nitrogen segregation.
  • the nitrogen overflow rate during the selective laser melting process was calculated to obtain the overmixed powder composition. A reasonable selective laser melting process was obtained through experimental methods.
  • the powder mixing raw materials include iron powder, chromium nitride, chromium powder, manganese powder and molybdenum powder.
  • the iron powder, chromium powder and molybdenum powder are spherical powders, and the chromium nitride and manganese powder are irregular powders.
  • the purity of the iron powder, chromium nitride, chromium powder, manganese powder and molybdenum powder are all ⁇ 99.0%.
  • the beneficial effect of adopting the above further solution is that the present invention avoids the introduction of impurities by improving the accuracy of the mass percentage of chemical components of the over-formulated powder target product.
  • the particle size of the mixed powder raw material is 15-53 ⁇ m.
  • the beneficial effect of adopting the above further solution is that since the over-formulation powder selective laser melting method relies on the over-formulation method to prepare powder and the selective laser melting method, it has certain requirements for the particle size and fluidity of the powder.
  • This particle size is the selective laser melting method.
  • the ball milling speed of the rotary ball mill described in step (2) is 400-420r/min, and the ball milling time is 4-5h.
  • the beneficial effect of adopting the above further solution is that the above operations can fully mix the powder evenly, enhance the fluidity and uniformity of the over-mixed powder, and reduce printing segregation.
  • the printing parameters of the laser 3D printer in step (4) are: laser power of 200W to 300W, scanning speed of 1000mm/s, scanning interval of 0.08mm, and powder layer thickness of 0.03mm.
  • the present invention adopts the selective laser melting method of over-mixed powder to prepare, and replaces nickel with manganese and nitrogen, thereby reducing the cost and improving the nitrogen content and controllability of the nitrogen content of high-nitrogen steel prepared by the selective laser melting method. , effectively improve the pitting corrosion resistance, stress corrosion resistance and other properties of stainless steel materials, and have high yield and tensile strength.
  • the present invention uses powder mixing and selective laser melting methods to prepare high-nitrogen stainless steel under conventional 3D printing conditions, which can effectively increase the nitrogen content of complex parts.
  • the over-mixed powder selective laser melting method obtains high-nitrogen printing powder through powder mixing, ensuring the nitrogen content in the product and reducing the cost of preparing high-nitrogen steel printing powder; reaction process There is no need to increase reaction pressure, which reduces printing reaction costs and improves safety; by adjusting The element content of the mixed powder raw materials can be used to prepare a variety of high-nitrogen steel printing powders, which increases the feasibility of high-nitrogen steel 3D printing.
  • Figure 1 is a schematic diagram of the dimensions of the tensile specimen provided by the present invention.
  • Figure 2 is a diagram of the actual molding provided by the present invention.
  • the Fe, CrN, Mn, Cr and Mo metal powders are weighed according to the mass ratio of the components in the required steel, and the ratio of Fe:CrN:Mn:Cr:Mo to 100 grams of powder is 66:10:11:10:3.

Abstract

Disclosed in the present invention is a method for preparing high-nitrogen stainless steel by selective laser melting of pure metal prepared powder, comprising the steps of: preparing a mixed powder raw material according to chemical components of a target product; putting the mixed powder raw material into a ball mill for ball milling and mixing to obtain prepared powder; putting the mixed prepared powder into a laser 3D printer powder container; vacuumizing a cavity of the laser 3D printer, then introducing nitrogen, and preheating a substrate to start printing; and after the printing is completed, taking out a sample to obtain high-nitrogen stainless steel. In the prepared powder selective laser melting method, high-nitrogen printing powder is obtained by a powder preparation mode, the content of nitrogen in the product is guaranteed, and the cost of preparation for high-nitrogen steel printing powder is reduced; the reaction pressure does not need to be increased in a reaction process, the printing reaction cost is reduced, and the safety is improved; by adjusting the content of elements in 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

一种纯金属过配粉体选区激光熔化制备高氮不锈钢的方法A method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-matched powder 技术领域Technical field
本发明涉及钢铁冶金技术领域，具体的说涉及一种纯金属过配粉体选区激光熔化制备高氮不锈钢的方法。The invention relates to the technical field of iron and steel metallurgy, and specifically to a method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-matched powder.
背景技术Background technique
高氮不锈钢凭借其具有在多种腐蚀介质中优秀的耐腐蚀性能、良好的综合力学性能和优良的加工性能，被认为是最有发展前景的新型工程材料之一。在生物能源行业、航空航天、石油化工行业、海洋工程、生物医用等多方领域获得了广泛的应用。目前，国内外用于制备高氮钢的方法有：氮气加压熔炼法、粉末冶金法和表面渗氮法；氮气加压熔炼法是制备高氮钢的方法中产品质量优异，但因其较高的高压制造成本、装备复杂等受到限制。High-nitrogen stainless steel is considered to be one of the most promising new engineering materials due to its excellent corrosion resistance, good comprehensive mechanical properties and excellent processing performance in a variety of corrosive media. It has been widely used in the bioenergy industry, aerospace, petrochemical industry, marine engineering, biomedical and other fields. At present, the methods used to prepare high-nitrogen steel at home and abroad include: nitrogen pressure smelting method, powder metallurgy method and surface nitriding method. Nitrogen pressure smelting method is a method for preparing high-nitrogen steel. The product quality is excellent, but because of its high The high-voltage manufacturing cost and equipment complexity are limited.
金属增材制造技术是一种以数字化模型为基础，通过高能热源加工粉体材料快速逐层堆积成型的制备加工技术，近30年来世界制造技术领域的一次重大突破，被视为推动人类第三次工业革命的新技术。选区激光熔化技术(SLM)是金属增材制造的一个重要分支，SLM工艺是高功率激光与金属粉体材料发生高速熔化凝固并选区逐层叠加交互作用的一个工艺过程。Metal additive manufacturing technology is a preparation and processing technology that is based on digital models and uses high-energy heat sources to process powder materials to rapidly accumulate layer by layer. It has been a major breakthrough in the world's manufacturing technology field in the past 30 years and is regarded as promoting the third generation of mankind. New technologies of the sub-industrial revolution. Selective laser melting technology (SLM) is an important branch of metal additive manufacturing. The SLM process is a process in which high-power laser and metal powder materials melt and solidify at high speed and selectively superimpose layer by layer.
选区激光熔化应用于制备高氮不锈钢因打印过程中氮元素溢出而无法直接得到氮含量达标的高氮不锈钢，通常采用增压方式抑制氮溢出，但常规3D打印设备不具备增压功能。大气压力下氮在液态钢中的溶解度很低，高氮钢的传统冶炼不像其它钢那样容易进行，同样SLM工艺在常压下使用常规含氮金属粉体也难以直接生产出高氮不锈钢。Selective laser melting is used to prepare high-nitrogen stainless steel. Due to the overflow of nitrogen during the printing process, high-nitrogen stainless steel with up-to-standard nitrogen content cannot be directly obtained. Pressurization is usually used to suppress nitrogen overflow, but conventional 3D printing equipment does not have a pressurization function. The solubility of nitrogen in liquid steel under atmospheric pressure is very low. Traditional smelting of high-nitrogen steel is not as easy as other steels. Similarly, it is difficult for the SLM process to directly produce high-nitrogen stainless steel using conventional nitrogen-containing metal powders under normal pressure.
因此，提供一种高N含量粉体用于3D打印高氮不锈钢的方法，解决常压 下打印出的钢中氮含量较低的问题是本领域技术人员亟需解决的技术问题。Therefore, a method of using high N content powder for 3D printing of high nitrogen stainless steel is provided to solve the problem of normal pressure The problem of low nitrogen content in the steel printed below is a technical problem that those skilled in the art urgently need to solve.
发明内容Contents of the invention
有鉴于此，本发明粉工艺和选区激光熔化技术基础上，提供一种采用纯金属过配粉体选区激光熔化制备高氮不锈钢的方法。In view of this, based on the powder process and selective laser melting technology of the present invention, a method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder is provided.
为了实现上述目的，本发明采用如下技术方案：In order to achieve the above objects, the present invention adopts the following technical solutions:
一种纯金属过配粉体选区激光熔化制备高氮不锈钢的方法，包括以下步骤：A method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder, including the following steps:
(1)按照目标产品化学成分组成配置混粉原料；(1) Configure powder mixing raw materials according to the chemical composition of the target product;
(2)将混粉原料放入球磨机内球磨混合，得到过配粉体；(2) Put the mixed powder raw materials into a ball mill and ball-mill and mix to obtain over-blended powder;
(3)将混合好的过配粉体放入激光3D打印机粉仓内；(3) Place the mixed powder into the powder bin of the laser 3D printer;
(4)将激光3D打印机腔室内抽真空，然后充入氮气，基板预热至145-150℃后开始打印；(4) Evacuate the laser 3D printer chamber, then fill it with nitrogen, preheat the substrate to 145-150°C and then start printing;
(5)待打印完成后将试样取出，即为高氮不锈钢。(5) After printing is completed, take out the sample, which is high nitrogen stainless steel.
进一步，步骤(1)中所述目标产品化学成分质量百分比组成为：C≤0.1％，Cr 18～23％，N 0.8～2.0％，Mn 8～12％，Mo 2～3.5％，Ni<0.01％，Si<0.1％，P<0.01％，S<0.01％，余量为Fe。Furthermore, the chemical composition of the target product described in step (1) is as follows in percentage by mass: C≤0.1%, Cr 18-23%, N 0.8-2.0%, Mn 8-12%, Mo 2-3.5%, Ni<0.01%, Si<0.1%, P<0.01%, S<0.01%, and the remainder is Fe.
采用上述进一步方案的有益效果在于：本发明上述方案中过配粉体选区激光熔化法关键在于两个方面，一、通过纯金属过配法配置适量的过配粉体，根据氮逸出率实验精准计算氮的溢出量，保证打印后氮的含量，为得到氮含量1％制品，本发明采用过配比为1.4配粉，配置氮含量1.4％过配粉体；二、制定合理的选区激光熔化凝固工艺，减少氮的偏析。为获得精确的氮含量，保证氮在钢中均匀分布，对选区激光熔化过程中氮的溢出率进行了计算，从而得到过配粉体成分。通过实验法得到合理地选区激光熔化工艺。The beneficial effect of adopting the above further solution is that the key to the selective laser melting method of over-matched powder in the above-mentioned solution of the present invention lies in two aspects. First, an appropriate amount of over-matched powder is configured through the pure metal over-matching method. According to the nitrogen escape rate experiment Accurately calculate the amount of nitrogen overflow to ensure the nitrogen content after printing. In order to obtain a product with a nitrogen content of 1%, the present invention uses an overmixing ratio of 1.4 powder and configures an overmixed powder with a nitrogen content of 1.4%; 2. Formulate a reasonable selected laser Melting and solidification process reduces nitrogen segregation. In order to obtain accurate nitrogen content and ensure uniform distribution of nitrogen in the steel, the nitrogen overflow rate during the selective laser melting process was calculated to obtain the overmixed powder composition. A reasonable selective laser melting process was obtained through experimental methods.
进一步，所述混粉原料包括铁粉、氮化铬、铬粉、锰粉和钼粉。 Further, the powder mixing raw materials include iron powder, chromium nitride, chromium powder, manganese powder and molybdenum powder.
更进一步，所述铁粉、铬粉和钼粉为球形粉体，所述氮化铬和锰粉为不规则粉体。Furthermore, the iron powder, chromium powder and molybdenum powder are spherical powders, and the chromium nitride and manganese powder are irregular powders.
所述铁粉、氮化铬、铬粉、锰粉和钼粉的纯度均≥99.0％。The purity of the iron powder, chromium nitride, chromium powder, manganese powder and molybdenum powder are all ≥99.0%.
采用上述进一步方案的有益效果在于：本发明通过提高过配粉体目标产品化学成分质量百分比精确度，避免杂质引入。The beneficial effect of adopting the above further solution is that the present invention avoids the introduction of impurities by improving the accuracy of the mass percentage of chemical components of the over-formulated powder target product.
更进一步，所述混粉原料的粒度为15～53μm。Furthermore, the particle size of the mixed powder raw material is 15-53 μm.
采用上述进一步方案的有益效果在于：由于过配粉体选区激光熔化法依赖于过配法制备粉体和选区激光熔化法，对粉体粒径和流动性有一定要求，此粒度为选区激光熔化最佳粒度。The beneficial effect of adopting the above further solution is that since the over-formulation powder selective laser melting method relies on the over-formulation method to prepare powder and the selective laser melting method, it has certain requirements for the particle size and fluidity of the powder. This particle size is the selective laser melting method. Optimal granularity.
进一步，步骤(2)中所述转球磨机的球磨转速为400-420r/min，球磨时间为4-5h。Further, the ball milling speed of the rotary ball mill described in step (2) is 400-420r/min, and the ball milling time is 4-5h.
采用上述进一步方案的有益效果在于：上述操作可使粉末充分混合均匀，增强过配粉体流动性和粉体均匀性，减少打印偏析。The beneficial effect of adopting the above further solution is that the above operations can fully mix the powder evenly, enhance the fluidity and uniformity of the over-mixed powder, and reduce printing segregation.
进一步，步骤(4)中所述激光3D打印机的打印参数为：激光功率为200W～300W，扫描速度为1000mm/s，扫描间隔为0.08mm，粉层厚度为0.03mm。Furthermore, the printing parameters of the laser 3D printer in step (4) are: laser power of 200W to 300W, scanning speed of 1000mm/s, scanning interval of 0.08mm, and powder layer thickness of 0.03mm.
本发明的有益效果在于：本发明采用过配粉体选区激光熔化方法进行制备，以锰、氮代镍，降低成本，提高选区激光熔化法制备高氮钢的氮含量和氮含量的可控性，有效提高不锈钢材料的耐点蚀、耐应力腐蚀等性能，具有较高的屈服和拉伸强度。The beneficial effects of the present invention are: the present invention adopts the selective laser melting method of over-mixed powder to prepare, and replaces nickel with manganese and nitrogen, thereby reducing the cost and improving the nitrogen content and controllability of the nitrogen content of high-nitrogen steel prepared by the selective laser melting method. , effectively improve the pitting corrosion resistance, stress corrosion resistance and other properties of stainless steel materials, and have high yield and tensile strength.
本发明利用混粉和选区激光熔化方法高氮钢，在常规3D打印条件下制备高氮不锈钢，能有效提高复杂零部件的氮含量。The present invention uses powder mixing and selective laser melting methods to prepare high-nitrogen stainless steel under conventional 3D printing conditions, which can effectively increase the nitrogen content of complex parts.
与其他高氮钢制备工艺相比，过配粉体选区激光熔化法通过配粉的方式得到高氮打印粉体，保证制品中氮的含量，降低了制备高氮钢打印粉体成本；反应过程无需增加反应压力，降低了打印反应成本，提高了安全性；通过调 整混粉原料元素含量，可以制备多种高氮钢打印粉体，增加了高氮钢3D打印提可行性。Compared with other high-nitrogen steel preparation processes, the over-mixed powder selective laser melting method obtains high-nitrogen printing powder through powder mixing, ensuring the nitrogen content in the product and reducing the cost of preparing high-nitrogen steel printing powder; reaction process There is no need to increase reaction pressure, which reduces printing reaction costs and improves safety; by adjusting The element content of the mixed powder raw materials can be used to prepare a variety of high-nitrogen steel printing powders, which increases the feasibility of high-nitrogen steel 3D printing.
附图说明Description of drawings
图1为本发明提供的拉伸试样尺寸示意图；Figure 1 is a schematic diagram of the dimensions of the tensile specimen provided by the present invention;
图2为本发明提供的成型实物图。Figure 2 is a diagram of the actual molding provided by the present invention.
具体实施方式Detailed ways
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present invention.
实施例1Example 1
(1)高氮不锈钢粉体目标化学成分，如表1所示；(1) Target chemical composition of high nitrogen stainless steel powder, as shown in Table 1;
表1目标化学成分元素配比(质量％)
Table 1 Target chemical composition element ratio (mass %)
(2)根据目标化学成分配备过配粉体。(2) Prepare the formulated powder according to the target chemical composition.
将Fe、CrN、Mn、Cr、Mo金属粉体按所需钢中成份进行质量配比称重，每100克过配粉体Fe：CrN：Mn：Cr：Mo＝66：10：11：10：3。The Fe, CrN, Mn, Cr and Mo metal powders are weighed according to the mass ratio of the components in the required steel, and the ratio of Fe:CrN:Mn:Cr:Mo to 100 grams of powder is 66:10:11:10:3.
(3)将配比称重好的各种粉体先进行初步混合，使用行星式球磨机对其充分混匀，时长为4h，球磨机转速400r/min，得到过配粉体。粉体成分如下表2：(3) Preliminarily mix the various proportioned and weighed powders, and mix them thoroughly using a planetary ball mill for 4 hours, with the ball mill rotating at 400 r/min to obtain the over-mixed powder. The powder ingredients are as follows in Table 2:
表2高氮无镍不锈钢粉体化学成分(质量％)
Table 2 Chemical composition of high nitrogen nickel-free stainless steel powder (mass %)
(4)将过配粉体放入选区激光融化实验设备分仓中，设置基板预热为150℃，保护气氛为氮气。选区激光熔化块体和拉伸件成形工艺参数如表3示，块体成形尺寸为5×5×5mm。拉伸试样尺寸如图1所示。成型实物图如图2所示。(4) Place the over-mixed powder into the compartment of the selective laser melting experimental equipment, set the substrate preheating to 150°C, and the protective atmosphere to nitrogen. The process parameters of the selective laser melting block and drawn parts forming are shown in Table 3. The block forming size is 5×5×5mm. The tensile specimen dimensions are shown in Figure 1. The actual molding picture is shown in Figure 2.
表3选区激光熔化块体成形参数
Table 3 Selected laser melting block forming parameters
(5)测试成形件氮含量(5) Test the nitrogen content of formed parts
表4选区激光熔化块体成形参数
Table 4 Selected laser melting block forming parameters
(6)测试成形件性能
(6) Test the performance of formed parts
尽管上面已经示出和描述了本发明的实施例，可以理解的是，上述实施例是示例性的，不能理解为对本发明的限制，本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。 Although the embodiments of the present invention have been shown and described above, it can be understood that the above-mentioned embodiments are illustrative and should not be construed as limitations of the present invention. Those of ordinary skill in the art can make modifications to the above-mentioned embodiments within the scope of the present invention. The embodiments are subject to changes, modifications, substitutions and variations.

Claims (7)

  1. 一种纯金属过配粉体选区激光熔化制备高氮不锈钢的方法，其特征在于，包括以下步骤：A method for preparing high-nitrogen stainless steel through selective laser melting of pure metal over-mixed powder, which is characterized by including the following steps:
    (1)按照目标产品化学成分组成配置混粉原料；(1) Configure powder mixing raw materials according to the chemical composition of the target product;
    (2)将混粉原料放入球磨机内球磨混合，得到过配粉体；(2) Put the mixed powder raw materials into a ball mill and ball-mill and mix to obtain over-blended powder;
    (3)将混合好的过配粉体放入激光3D打印机粉仓内；(3) Place the mixed powder into the powder bin of the laser 3D printer;
    (4)将激光3D打印机腔室内抽真空，然后充入氮气，基板预热至145-150℃后开始打印；(4) Evacuate the laser 3D printer chamber, then fill it with nitrogen, preheat the substrate to 145-150°C and then start printing;
    (5)待打印完成后将试样取出，即为高氮不锈钢。(5) After printing is completed, take out the sample, which is high nitrogen stainless steel.
  2. 根据权利要求1所述一种纯金属过配粉体选区激光熔化制备高氮不锈钢的方法，其特征在于，步骤(1)中所述目标产品化学成分质量百分比组成为：C≤0.1％，Cr 18～23％，N 0.8～2.0％，Mn8～12％，Mo 2～3.5％，Ni<0.01％，Si<0.1％，P<0.01％，S<0.01％，余量为Fe。According to the method for preparing high nitrogen stainless steel by selective laser melting of pure metal over-matched powder as described in claim 1, it is characterized in that the chemical composition mass percentage of the target product described in step (1) is: C≤0.1%, Cr 18-23%, N 0.8-2.0%, Mn8-12%, Mo 2-3.5%, Ni<0.01%, Si<0.1%, P<0.01%, S<0.01%, and the remainder is Fe.
  3. 根据权利要求2所述一种纯金属过配粉体选区激光熔化制备高氮不锈钢的方法，其特征在于，所述混粉原料包括铁粉、氮化铬、铬粉、锰粉和钼粉。A method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder according to claim 2, wherein the powder mixing raw materials include iron powder, chromium nitride, chromium powder, manganese powder and molybdenum powder.
  4. 据权利要求3所述一种纯金属过配粉体选区激光熔化制备高氮不锈钢的方法，其特征在于，所述铁粉、铬粉和钼粉为球形粉体，所述氮化铬和锰粉为不规则粉体。A method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-matched powder according to claim 3, characterized in that the iron powder, chromium powder and molybdenum powder are spherical powders, and the chromium nitride and manganese The powder is irregular powder.
  5. 据权利要求3所述一种纯金属过配粉体选区激光熔化制备高氮不锈钢的方法，其特征在于，所述混粉原料的粒度为15～53μm。A method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder according to claim 3, characterized in that the particle size of the powder mixed raw material is 15 to 53 μm.
  6. 根据权利要求1所述一种纯金属过配粉体选区激光熔化制备高氮不锈钢的方法，其特征在于，步骤(2)中所述转球磨机的球磨转速为400-420r/min，球磨时间为4-5h。A method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-mixed powder according to claim 1, characterized in that the ball milling speed of the ball mill in step (2) is 400-420r/min, and the ball milling time is 4-5h.
  7. 根据权利要求1所述一种纯金属过配粉体选区激光熔化制备高氮不锈钢的方法，其特征在于，步骤(4)中所述激光3D打印机的打印参数为：激光 功率为200w～300W，扫描速度为1000mm/s，扫描间隔为0.08mm，粉层厚度为0.03mm。 A method for preparing high-nitrogen stainless steel by selective laser melting of pure metal over-matched powder according to claim 1, characterized in that the printing parameters of the laser 3D printer in step (4) are: laser The power is 200w~300W, the scanning speed is 1000mm/s, the scanning interval is 0.08mm, and the powder layer thickness is 0.03mm.
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