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CN116213751A - A kind of 316L stainless steel surface treatment method - Google Patents

A kind of 316L stainless steel surface treatment method Download PDF

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CN116213751A
CN116213751A CN202211594978.6A CN202211594978A CN116213751A CN 116213751 A CN116213751 A CN 116213751A CN 202211594978 A CN202211594978 A CN 202211594978A CN 116213751 A CN116213751 A CN 116213751A
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stainless steel
shot peening
surface treatment
treatment method
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张超
吴建雄
祝毅
张军辉
徐兵
纵怀志
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Zhejiang University ZJU
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Abstract

本发明公开了一种316L不锈钢表面处理方法,用于解决激光粉末床熔融快速成形的316L不锈钢由于表面质量差,孔隙多,残余应力大和抗腐蚀性不强等缺点而造成应用性能差的技术问题。该方法是首先采用激光粉末床熔融技术对316L不锈钢进行快速成形处理,并将成形后的316L进行去应力退火处理,将退火后的LPBF 316L不锈钢放入高能喷丸室中,对LPBF 316L不锈钢表面进行喷丸处理。由于对表面进行了高能喷丸处理,引入了高应变和高应变速率的剧烈塑性变形,致使316L表面出现梯度纳米化结构,不再出现原有的熔池结构。经测试,316L不锈钢表面形成的纳米晶层可以达到212μm。

Figure 202211594978

The invention discloses a surface treatment method of 316L stainless steel, which is used to solve the technical problem of poor application performance caused by the disadvantages of poor surface quality, many pores, large residual stress and weak corrosion resistance of 316L stainless steel rapidly formed by laser powder bed fusion . The method is to firstly use laser powder bed fusion technology to perform rapid prototyping treatment on 316L stainless steel, and perform stress relief annealing on the formed 316L stainless steel, put the annealed LPBF 316L stainless steel into a high-energy shot blasting chamber, and treat the surface of LPBF 316L stainless steel Perform shot peening. Due to the high-energy shot peening treatment on the surface, severe plastic deformation with high strain and high strain rate was introduced, resulting in the gradient nanostructure on the surface of 316L, and the original molten pool structure no longer appeared. After testing, the nanocrystalline layer formed on the surface of 316L stainless steel can reach 212 μm.

Figure 202211594978

Description

一种316L不锈钢表面处理方法A kind of 316L stainless steel surface treatment method

技术领域technical field

本发明涉及不锈钢表面处理领域,尤其涉及一种316L不锈钢表面处理方法。The invention relates to the field of stainless steel surface treatment, in particular to a 316L stainless steel surface treatment method.

背景技术Background technique

LPBF 316L不锈钢具有良好的耐腐蚀性、耐高温和抗蠕变性能,在航空航天领域、机器人、工程机械等领域得到广泛的应用,由于LPBF 316L不锈钢多服役于高温、高压等严苛的工作环境,故对其表面性能和使用可靠性提出了更高的要求。纳米晶具有尺寸小、界面密度高、晶界结构和普通大角度晶界相似等特点,相对于LPBF 316L原始晶粒,纳米晶可以显著改善材料性能,为改善LPBF 316L不锈钢的整体性能和服役寿命创造了条件。LPBF 316L stainless steel has good corrosion resistance, high temperature resistance and creep resistance, and is widely used in aerospace, robotics, construction machinery and other fields. Because LPBF 316L stainless steel is mostly used in harsh working environments such as high temperature and high pressure , so higher requirements are put forward for its surface performance and reliability. Nanocrystals have the characteristics of small size, high interface density, and grain boundary structure similar to ordinary high-angle grain boundaries. Compared with LPBF 316L original grains, nanocrystals can significantly improve material properties. In order to improve the overall performance and service life of LPBF 316L stainless steel conditions are created.

文献1“吴佳豪,选区激光熔化成形316L不锈钢组织及性能研究[J].兵器材料科学与工程”报道了采用选区激光熔化(SLM)技术成形316L不锈钢试样,对垂直/平行打印方向的两个面进行组织结构和机械性能的对比研究,结果表明:受晶粒尺寸和孔隙率的影响,垂直面的机械性能优于平行面。文献2“马春宇,装饰用316L不锈钢粉末高速压制成形过程中的孪晶行为[J].锻压技术,2022,47(08)”报道了高速压制316L粉末成形过程中冲击能量对孪晶组织的影响,而孪晶组织的致密度决定了316L不锈钢的耐腐蚀性能,结果发现:在较高的冲击能量下,可以获得更大密度的孪晶组织,可以提高其耐腐蚀性能,有助于降低腐蚀速率。文献3“朱德荣,固溶时效对SLM成形316L不锈钢块体件显微组织及硬度的影响[J].金属热处理,2022,47(08)”报道了关于选区激光熔化技术采用不同的时效工艺对成形后的316L不锈钢显微组织以及硬度的影响,结果表明:SLM成形316L不锈钢块体件显微组织主要由细小的柱状晶和蜂窝状晶粒组成,“层-层”和“道-道”熔池边界清晰可见,但是经过固溶时效后边界消失,晶界清晰可见,在较高的时效温度时,试样晶界处产生M23C6,显微硬度得到显著提升。Document 1 "Wu Jiahao, Research on Microstructure and Properties of 316L Stainless Steel Formed by Selective Laser Melting [J]. Weapon Materials Science and Engineering" reported that 316L stainless steel samples were formed by selective laser melting (SLM) technology. The results show that the mechanical properties of vertical planes are better than those of parallel planes due to the influence of grain size and porosity. Document 2 "Ma Chunyu, Twin crystal behavior during high-speed compaction of 316L stainless steel powder for decoration [J]. Forging Technology, 2022, 47(08)" reported the effect of impact energy on twin crystal structure during high-speed compaction of 316L powder , and the density of the twin structure determines the corrosion resistance of 316L stainless steel. It was found that under higher impact energy, a denser twin structure can be obtained, which can improve its corrosion resistance and help reduce corrosion. rate. Document 3 "Zhu Derong, Effect of solution aging on the microstructure and hardness of 316L stainless steel blocks formed by SLM [J]. Metal Heat Treatment, 2022, 47 (08)" reported that different aging processes were used in selective laser melting technology The influence on the microstructure and hardness of 316L stainless steel after forming, the results show that: the microstructure of 316L stainless steel block formed by SLM is mainly composed of fine columnar grains and honeycomb grains, "layer-layer" and "road-road "The molten pool boundary is clearly visible, but after solid solution aging, the boundary disappears and the grain boundary is clearly visible. At a higher aging temperature, M 23 C 6 is generated at the grain boundary of the sample, and the microhardness is significantly improved.

一般来说,表面晶粒尺度越小,剧烈塑性变形层厚度越大,316L不锈钢的机械性能越优越。此外,引入高应变和高应变速率是改变316L不锈钢表面性能的有效措施。上述方法中,虽然制备了316L不锈钢结构,但是制备的316L不锈钢表面晶粒尺度较大,剧烈塑性变形层比小,制约了其有效应用。Generally speaking, the smaller the surface grain size and the greater the thickness of the severe plastic deformation layer, the better the mechanical properties of 316L stainless steel. In addition, the introduction of high strain and high strain rate is an effective measure to change the surface properties of 316L stainless steel. In the above method, although the 316L stainless steel structure is prepared, the surface grain size of the prepared 316L stainless steel is relatively large, and the severe plastic deformation layer ratio is small, which restricts its effective application.

发明内容Contents of the invention

为了改善LPBF成形的316L不锈钢的表面性能,拓展其实际应用的技术问题,本发明提供以一种增材制造316L不锈钢表面强化方法。该方法将LPBF 316L不锈钢进行去应力退火处理,然后在高压下对其表面进行喷丸处理,经过较长时间的喷丸处理,使LPBF 316L不锈钢表层发生大应变和应变高速率的剧烈塑性变形,实现表面梯度纳米结构。In order to improve the surface properties of 316L stainless steel formed by LPBF and expand the technical problems of its practical application, the present invention provides a surface strengthening method for additively manufacturing 316L stainless steel. In this method, LPBF 316L stainless steel is subjected to stress relief annealing treatment, and then its surface is shot peened under high pressure. After a long period of shot peening, the surface of LPBF 316L stainless steel undergoes severe plastic deformation with large strain and high strain rate. Achieve surface gradient nanostructures.

本发明解决其技术问题所采用的技术方案包括以下步骤:一种316L不锈钢表面处理方法,该方法包括以下步骤:The technical scheme that the present invention adopts to solve its technical problem comprises the following steps: a kind of 316L stainless steel surface treatment method, this method comprises the following steps:

(1)对316L不锈钢粉末进行激光粉末床熔融快速成形,得到316L不锈钢样件;(1) Perform laser powder bed fusion rapid prototyping on 316L stainless steel powder to obtain 316L stainless steel samples;

(2)对成形后的316L不锈钢样件进行去应力退火处理;(2) Perform stress relief annealing on the formed 316L stainless steel sample;

(3)对去应力退火处理后的316L不锈钢样件进行喷丸处理,实现表面梯度纳米结构,所述喷丸条件为空气压力为0.3或0.4MPa,喷丸时间为30或45mim。(3) Shot peening is performed on the 316L stainless steel sample after the stress relief annealing treatment to realize the surface gradient nanostructure. The shot peening conditions are that the air pressure is 0.3 or 0.4 MPa, and the shot peening time is 30 or 45 min.

进一步地,步骤(1)中,所述316L不锈钢粉末按照质量分数计算,粉末的具体成分为:C为0.03%,Mn为0.02%,Ni为12.5%~13.0%,Cu为0.50%,Si为0.75%,P为0.025%,Cr为17.5%~18.0%,Mo为2.25%~2.50%,余量为Fe。Further, in step (1), the 316L stainless steel powder is calculated according to the mass fraction, and the specific composition of the powder is: C is 0.03%, Mn is 0.02%, Ni is 12.5%~13.0%, Cu is 0.50%, and Si is 0.75%, P is 0.025%, Cr is 17.5%~18.0%, Mo is 2.25%~2.50%, and the balance is Fe.

进一步地,步骤(1)中,扫描策略为Meader,工艺参数选择如下:Further, in step (1), the scanning strategy is Meader, and the process parameters are selected as follows:

层厚:50μm,光斑大小:70μm,扫描间距:110μm,激光功率:200W,点距:60μm,曝光时间:80μs,扫面速度,750mm/s。Layer thickness: 50μm, spot size: 70μm, scanning pitch: 110μm, laser power: 200W, spot pitch: 60μm, exposure time: 80μs, scanning speed, 750mm/s.

进一步地,步骤(2)中, 去应力退火处理条件为:退火温度为1280℃,保温时间为60min,空冷至室温。Further, in step (2), the stress relief annealing treatment conditions are as follows: the annealing temperature is 1280° C., the holding time is 60 minutes, and air cooling to room temperature.

进一步地,步骤(3)中,采用直径为0.6mm的ASH230弹丸对316L不锈钢样件进行高能喷丸处理。Further, in step (3), the 316L stainless steel sample was subjected to high-energy shot peening using ASH230 projectiles with a diameter of 0.6 mm.

与现有技术相比,本发明的有益结果是:Compared with prior art, beneficial result of the present invention is:

本发明制备的316L不锈钢表面晶粒尺度大大减小,同时增大了其表面的剧烈塑性形变层厚度。该不锈钢表面的纳米晶尺寸在25nm,已达到超细晶尺度,塑性变形层厚度可以达到212μm,比背景技术中的晶粒尺度减小很多,变形层厚度明显增大。The grain size on the surface of the 316L stainless steel prepared by the invention is greatly reduced, and the thickness of the severe plastic deformation layer on the surface is increased at the same time. The nanocrystal size on the surface of the stainless steel is 25nm, which has reached the ultra-fine grain scale, and the thickness of the plastic deformation layer can reach 212 μm, which is much smaller than the grain size in the background technology, and the thickness of the deformed layer is obviously increased.

附图说明Description of drawings

为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图做简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动前提下,还可以根据这些附图获得其他附图。In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only These are some embodiments of the present invention. Those skilled in the art can also obtain other drawings based on these drawings without creative work.

图1为实施例1制备316L不锈钢表面纳米梯度结构示意图。Figure 1 is a schematic diagram of the nanogradient structure on the surface of 316L stainless steel prepared in Example 1.

图2为激光粉末床熔融快速成形技术扫描策略和成形试样。Figure 2 shows the scanning strategy and forming samples of laser powder bed fusion rapid prototyping technology.

图3为实施例1制备316L不锈钢表面纳米结构的透射电镜明场、暗场和电子衍射照片。Fig. 3 is the transmission electron microscope bright field, dark field and electron diffraction photos of the surface nanostructures of 316L stainless steel prepared in Example 1.

图4为实施例2制备316L不锈钢表面纳米结构塑性变形层照片。Fig. 4 is the photo of the nanostructure plastic deformation layer on the surface of 316L stainless steel prepared in Example 2.

图5为实施例3和实施例1塑性变形层厚度对比照片。Fig. 5 is a photograph comparing the thickness of the plastically deformed layer of Example 3 and Example 1.

具体实施方式Detailed ways

以下结合附图对本发明具体实施方式作进一步详细说明。The specific embodiments of the present invention will be described in further detail below in conjunction with the accompanying drawings.

实施例1:本发明提供了一种316L不锈钢表面处理方法,具体步骤如下:Embodiment 1: the present invention provides a kind of 316L stainless steel surface treatment method, concrete steps are as follows:

(1)对316L不锈钢粉末进行激光粉末床熔融(Laser powder bed fusion,LPBF)快速成形处理,所用的316L不锈钢粉末是由气体雾化形成的球形状颗粒,粒度直径在20~65μm之间,平均直径大约50μm;316L不锈钢粉末按照质量分数计算,粉末的具体成分为:C为0.03%,Mn为0.02%,Ni为12.5%~13.0%,Cu为0.50%,Si为0.75%,P为0.025%,Cr为17.5%~18.0%,Mo为2.25%~2.50%,余量为Fe。(1) Laser powder bed fusion (LPBF) rapid prototyping treatment is performed on 316L stainless steel powder. The 316L stainless steel powder used is a spherical particle formed by gas atomization, with a particle size diameter between 20 and 65 μm. The diameter is about 50 μm; 316L stainless steel powder is calculated according to the mass fraction. The specific composition of the powder is: C is 0.03%, Mn is 0.02%, Ni is 12.5%~13.0%, Cu is 0.50%, Si is 0.75%, and P is 0.025%. , Cr is 17.5%~18.0%, Mo is 2.25%~2.50%, and the balance is Fe.

扫描策略为Meader,每一层的扫描路线如图2中的(a)所示,具体加工工艺参数如表1所示,每打印一层316L不锈钢之后,旋转67°继续保持扫描路线,最终形成70×19×4mm3的平板316L不锈钢试样如图2中的(b)所示;The scanning strategy is Meader. The scanning route of each layer is shown in (a) in Figure 2. The specific processing parameters are shown in Table 1. After printing each layer of 316L stainless steel, rotate 67° to continue to maintain the scanning route, and finally form The flat 316L stainless steel sample of 70×19×4mm 3 is shown in (b) in Figure 2;

表1Table 1

Figure 246166DEST_PATH_IMAGE001
Figure 246166DEST_PATH_IMAGE001

(2)对成形后的316L不锈钢样件进行去应力退火处理,退火温度为1280℃,保温时间为60min,空冷至室温;(2) Perform stress-relieving annealing treatment on the formed 316L stainless steel sample, the annealing temperature is 1280°C, the holding time is 60min, and air-cooled to room temperature;

(3)采用直径为0.6mm的ASH230铸钢弹丸对去应力退火后的316L不锈钢样件进行高能喷丸处理,实现表面梯度纳米结构,如图1所示,喷丸处理条件为空气压力为0.40MPa,喷丸时间为45min;(3) ASH230 cast steel projectiles with a diameter of 0.6 mm were used to perform high-energy shot peening on the 316L stainless steel sample after stress relief annealing to achieve surface gradient nanostructures. As shown in Figure 1, the shot peening condition was that the air pressure was 0.40 MPa, the shot peening time is 45min;

图3中的(a)为实施例1制备316L不锈钢表面纳米晶的透射电镜明场,图3中的(b)为实施例1制备316L不锈钢表面纳米晶的暗场,图3中的(c)为实施例1制备316L不锈钢表面纳米晶的对应明场的电子衍射花样。从明场和暗场像可以看出,316L不锈钢试样表面的晶粒极其细小;由暗场图晶粒尺寸范围可以看出,316L不锈钢试样表面的晶粒已经细化为超细纳米晶,最小晶粒尺寸为25nm。图5中的(b)可以看出实施例1的塑性变形层可以达到231μm,同时塑性变形层熔池结构基本消除。(a) in Fig. 3 is that embodiment 1 prepares the transmission electron microscope bright field of 316L stainless steel surface nanocrystal, (b) among Fig. 3 is the dark field that embodiment 1 prepares 316L stainless steel surface nanocrystal, (c among Fig. 3 ) is the electron diffraction pattern corresponding to the bright field of the nanocrystals on the surface of 316L stainless steel prepared in Example 1. It can be seen from the bright field and dark field images that the grains on the surface of the 316L stainless steel sample are extremely small; from the grain size range of the dark field image, it can be seen that the grains on the surface of the 316L stainless steel sample have been refined into ultrafine nanocrystals , the minimum grain size is 25nm. It can be seen from (b) in Figure 5 that the plastic deformation layer in Example 1 can reach 231 μm, and at the same time, the molten pool structure of the plastic deformation layer is basically eliminated.

实施例2Example 2

根据实施例1的强化方法,改变步骤(3)中喷丸时间为30min,喷丸空气压力为0.3MPa,对实施例1中已经成形的316L不锈钢进行表面强化,如图4所示,该不锈钢的剧烈塑性变形层厚度达到212μm,而且塑性变形层熔池结构基本消除。According to the strengthening method of Example 1, the shot peening time in step (3) is changed to 30min, and the shot peening air pressure is 0.3MPa, and the surface of the 316L stainless steel that has been formed in Example 1 is strengthened, as shown in Figure 4, the stainless steel The thickness of the severe plastic deformation layer reaches 212μm, and the molten pool structure of the plastic deformation layer is basically eliminated.

实施例3Example 3

根据实施例1的强化方法,选取步骤(1)和步骤(2)对316L不锈钢进行处理,如图5中的(a)所示,可以发现LPBF成形的316L不锈钢表面没有塑性变形层,而且LPBF成形时表面的熔池结构在基本没有消除。According to the strengthening method of Example 1, step (1) and step (2) are selected to treat 316L stainless steel, as shown in (a) in Figure 5, it can be found that the surface of 316L stainless steel formed by LPBF has no plastic deformation layer, and LPBF The molten pool structure on the surface is basically not eliminated during forming.

以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书及附图内容所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。The above is only an embodiment of the present invention, and does not limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made by using the description of the present invention and the contents of the accompanying drawings, or directly or indirectly used in other related technologies fields, are all included in the scope of patent protection of the present invention in the same way.

Claims (5)

1.一种316L不锈钢表面处理方法,其特征在于,该方法包括以下步骤:1. a 316L stainless steel surface treatment method is characterized in that the method may further comprise the steps: (1)对316L不锈钢粉末进行激光粉末床熔融快速成形,得到316L不锈钢样件;(1) Perform laser powder bed fusion rapid prototyping on 316L stainless steel powder to obtain 316L stainless steel samples; (2)对成形后的316L不锈钢样件进行去应力退火处理;(2) Perform stress relief annealing on the formed 316L stainless steel sample; (3)对去应力退火处理后的316L不锈钢样件进行喷丸处理,实现表面梯度纳米结构,所述喷丸条件为空气压力为0.3或0.4MPa,喷丸时间为30或45mim。(3) Shot peening is performed on the 316L stainless steel sample after the stress relief annealing treatment to realize the surface gradient nanostructure. The shot peening conditions are that the air pressure is 0.3 or 0.4 MPa, and the shot peening time is 30 or 45 min. 2.根据权利要求1所示的一种316L不锈钢表面处理方法,其特征在于,步骤(1)中,所述316L不锈钢粉末按照质量分数计算,粉末的具体成分为:C为0.03%,Mn为0.02%,Ni为12.5%~13.0%,Cu为0.50%,Si为0.75%,P为0.025%,Cr为17.5%~18.0%,Mo为2.25%~2.50%,余量为Fe。2. A 316L stainless steel surface treatment method according to claim 1, characterized in that, in step (1), the 316L stainless steel powder is calculated according to the mass fraction, and the specific composition of the powder is: C is 0.03%, and Mn is 0.02%, Ni is 12.5%~13.0%, Cu is 0.50%, Si is 0.75%, P is 0.025%, Cr is 17.5%~18.0%, Mo is 2.25%~2.50%, and the balance is Fe. 3.根据权利要求1所示的一种316L不锈钢表面处理方法,其特征在于,步骤(1)中,扫描策略为Meader,工艺参数选择如下:3. A 316L stainless steel surface treatment method according to claim 1, characterized in that, in step (1), the scanning strategy is Meader, and the process parameters are selected as follows: 层厚:50μm,光斑大小:70μm,扫描间距:110μm,激光功率:200W,点距:60μm,曝光时间:80μs,扫面速度,750mm/s。Layer thickness: 50μm, spot size: 70μm, scanning pitch: 110μm, laser power: 200W, spot pitch: 60μm, exposure time: 80μs, scanning speed, 750mm/s. 4.根据权利要求1所示的一种316L不锈钢表面处理方法,其特征在于,步骤(2)中, 去应力退火处理条件为:退火温度为1280℃,保温时间为60min,空冷至室温。4. A method for surface treatment of 316L stainless steel according to claim 1, characterized in that in step (2), the stress relief annealing treatment conditions are as follows: annealing temperature is 1280°C, holding time is 60 minutes, and air cooling to room temperature. 5.根据权利要求1所示的一种316L不锈钢表面处理方法,其特征在于,步骤(3)中,采用直径为0.6mm的ASH230弹丸对316L不锈钢样件进行高能喷丸处理。5. A 316L stainless steel surface treatment method according to claim 1, characterized in that in step (3), the 316L stainless steel sample is subjected to high-energy shot peening using ASH230 projectiles with a diameter of 0.6 mm.
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