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CN115679247A - A preparation method of low-friction and wear-resistant composite coating containing boronizing layer and textured surface - Google Patents

A preparation method of low-friction and wear-resistant composite coating containing boronizing layer and textured surface Download PDF

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CN115679247A
CN115679247A CN202211098950.3A CN202211098950A CN115679247A CN 115679247 A CN115679247 A CN 115679247A CN 202211098950 A CN202211098950 A CN 202211098950A CN 115679247 A CN115679247 A CN 115679247A
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boronizing
workpiece
friction
layer
wear
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吴红星
尹绍冲
李跃辉
史俊勤
王琳
花珂
王海丰
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Northwestern Polytechnical University
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Abstract

The invention discloses a preparation method of a low-friction wear-resistant composite coating containing a boronizing layer and a texture surface, which comprises the following steps: carrying out boronizing strengthening treatment, preparing a boronizing strengthening layer on the surface of a workpiece, and then removing residues on the surface of the workpiece after the boronizing treatment; step (2), carrying out surface texturing treatment on the workpiece subjected to boronizing treatment to form pits on the surface of the workpiece; and (3) coating the two-dimensional material dispersion liquid on the surface of the workpiece, drying, and repeating the coating and drying operation until a solid self-lubricating coating based on the boronizing strengthening layer and the textured surface is obtained. The solid lubricating layer is made of a two-dimensional material, and the wear-resistant and friction-reducing capability of the two-dimensional material is fully exerted depending on the adhesion effect of the boronizing strengthening layer and the storage effect of the textured surface, so that the lubricating behavior of long service life and low friction and wear is realized.

Description

一种含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法A preparation method of low-friction and wear-resistant composite coating containing boronizing layer and textured surface

技术领域technical field

本发明属于固体润滑涂层和材料技术领域,尤其涉及一种含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法。The invention belongs to the technical field of solid lubricating coatings and materials, in particular to a method for preparing a low-friction and wear-resistant composite coating containing a boronized layer and a textured surface.

背景技术Background technique

据报道,每年摩擦磨损所造成的能源损耗占全球能源损耗的1/3,过度摩擦所导致的机械设备及零部件失效可达总量的80%,造成的机械设备恶性事故超过50%。降低摩擦磨损、提升机械部件服役寿命以及减少能源损耗已经成为当前世界亟需解决的难题。然而,随着我国工业和尖端技术的迅猛发展,航空、航天、航海以及高铁等高端制造走向“更高、更深、更快、更安全”,传统液体润滑剂已经无法满足现代工业高速、重载、高温高压等极端环境条件下的应用需求。According to reports, the energy loss caused by friction and wear accounts for 1/3 of the global energy loss every year, and the failure of mechanical equipment and parts caused by excessive friction can reach 80% of the total, and the serious accidents of mechanical equipment caused by it exceed 50%. Reducing friction and wear, improving the service life of mechanical components and reducing energy consumption have become problems that need to be solved urgently in the current world. However, with the rapid development of my country's industry and cutting-edge technology, high-end manufacturing such as aviation, aerospace, navigation, and high-speed rail is moving towards "higher, deeper, faster, and safer". Application requirements under extreme environmental conditions such as high temperature and high pressure.

作为另一重要润滑形式,固体润滑具有着高承载、高耐磨、低摩擦以及优异的环境适应性等优势,被广泛应用于空间环境、航空工业和先进能源装备等领域。近年来,固体润滑涂层相关技术已获得研究工作者的广泛关注。CN110064575A公开了一种二维材料固体润滑薄膜及其制备方法,将二维材料分散液涂覆于工件表面,并借助热压、热退火等附着力提升处理,制备出稳定性高、摩擦性能好的固体润滑薄膜。CN114000106A公开了一种低摩擦系数二硫化钼基复合固体润滑涂层及其制备方法,通过磁控溅射制备在工件表面制备出低摩擦、抗磨损的MoS2基复合涂层。然而,固体润滑涂层技术普遍存在着制备工艺复杂、制备条件苛刻、生产成本高以及与基底结合性能差、服役寿命短等缺点,严重限制了它们的研究和应用。As another important form of lubrication, solid lubrication has the advantages of high load capacity, high wear resistance, low friction and excellent environmental adaptability, and is widely used in space environment, aviation industry and advanced energy equipment and other fields. In recent years, technologies related to solid lubricating coatings have received extensive attention from researchers. CN110064575A discloses a two-dimensional material solid lubricating film and its preparation method. The two-dimensional material dispersion is coated on the surface of the workpiece, and the adhesion is improved by hot pressing, thermal annealing, etc. to prepare a film with high stability and good friction performance. solid lubricating film. CN114000106A discloses a low-friction molybdenum disulfide-based composite solid lubricating coating and a preparation method thereof. A low-friction, wear-resistant MoS2 - based composite coating is prepared on the surface of a workpiece by magnetron sputtering. However, solid lubricating coating technologies generally have disadvantages such as complex preparation process, harsh preparation conditions, high production cost, poor bonding performance with the substrate, and short service life, which severely limit their research and application.

发明内容Contents of the invention

为解决上述背景技术中提出的技术难题,本发明提出了一种含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,该复合涂层涉及渗硼强化层、织构化表面以及固体润滑层三部分,该方法制备的固体涂层不仅结合性能好、稳定性高、服役寿命长以及润滑性能出色,而且还具有涂层厚度可控、制备工艺简单、成本低廉、适于大面积快速制备等优点,在实际的工业生产和应用中展现出良好的前景。In order to solve the technical problems raised in the above-mentioned background technology, the present invention proposes a method for preparing a low-friction and wear-resistant composite coating containing a boronizing layer and a textured surface. The composite coating involves a boronizing strengthening layer, textured Surface and solid lubricating layer, the solid coating prepared by this method not only has good bonding performance, high stability, long service life and excellent lubricating performance, but also has controllable coating thickness, simple preparation process, low cost, suitable for The advantages of large-area rapid preparation show good prospects in actual industrial production and application.

具体的,本发明提供一种含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,包括如下步骤:Specifically, the present invention provides a method for preparing a low-friction and wear-resistant composite coating containing a boronized layer and a textured surface, comprising the following steps:

步骤(1)进行渗硼强化处理,在工件表面上制备渗硼强化层,然后去除渗硼处理后工件表面的残留物;Step (1) performing boronizing strengthening treatment, preparing a boronizing strengthening layer on the surface of the workpiece, and then removing the residue on the surface of the workpiece after boriding treatment;

步骤(2)对渗硼处理后的工件进行表面织构化处理,使工件表面形成凹坑;Step (2) performing surface texturing treatment on the workpiece after boriding treatment, so that pits are formed on the surface of the workpiece;

步骤(3)将二维材料分散液涂覆于工件表面,并进行干燥处理,重复所述涂覆及所述干燥处理操作,直至获得基于渗硼强化层与织构化表面的固体自润滑涂层。Step (3) Coating the two-dimensional material dispersion on the surface of the workpiece, and performing drying treatment, repeating the coating and drying treatment operations until a solid self-lubricating coating based on a boronizing strengthening layer and a textured surface is obtained. layer.

作为本发明的进一步说明,所述工件为钢、钛合金、多主元合金中的一种。As a further description of the present invention, the workpiece is one of steel, titanium alloy, and multi-principal alloy.

作为本发明的进一步说明,步骤(1)中所述渗硼强化处理采用固体渗硼工艺或熔盐电解渗硼工艺中的一种。As a further description of the present invention, the boronizing strengthening treatment in step (1) adopts one of solid boronizing process or molten salt electrolytic boronizing process.

作为本发明的进一步说明,步骤(1)中进行所述渗硼强化处理前需对工件表面进行清洗;且采用超声清洗去除渗硼处理后工件表面的残留物。As a further illustration of the present invention, the surface of the workpiece needs to be cleaned before the boronizing strengthening treatment in step (1); and ultrasonic cleaning is used to remove the residues on the surface of the workpiece after boronizing treatment.

作为本发明的进一步说明,步骤(2)中所述表面织构化处理包括压刻加工处理、磨料气射流加工处理、电解加工处理、反应离子刻蚀加工处理、激光表面织构处理中的一种。As a further illustration of the present invention, the surface texturing treatment in step (2) includes one of embossing processing, abrasive gas jet processing, electrolytic processing, reactive ion etching processing, and laser surface texturing. kind.

作为本发明的进一步说明,步骤(2)中工件表面形成的所述凹坑为微圆柱凹坑,且所述凹坑直径为20-300 μm,深度为20-500 μm,面积密度为5%-35%。As a further illustration of the present invention, the pits formed on the surface of the workpiece in step (2) are micro-cylindrical pits, and the pits have a diameter of 20-300 μm, a depth of 20-500 μm, and an area density of 5% -35%.

作为本发明的进一步说明,步骤(3)中所述二维材料包括石墨烯、氧化石墨烯、二硫化钼、二硫化钨、二硒化钼以及六方氮化硼中的一种或多种。As a further description of the present invention, the two-dimensional material in step (3) includes one or more of graphene, graphene oxide, molybdenum disulfide, tungsten disulfide, molybdenum diselenide and hexagonal boron nitride.

作为本发明的进一步说明,步骤(3)中所述二维材料分散液的溶剂包括水、烷基胺、聚乙烯亚胺、聚丙烯酸、聚乙二醇中的一种或多种。As a further description of the present invention, the solvent of the two-dimensional material dispersion in step (3) includes one or more of water, alkylamine, polyethyleneimine, polyacrylic acid, and polyethylene glycol.

作为本发明的进一步说明,步骤(3)中所述涂覆的方法包括滴涂、喷涂、旋涂、电泳沉积中的一种。As a further description of the present invention, the coating method in step (3) includes one of drop coating, spray coating, spin coating, and electrophoretic deposition.

作为本发明的进一步说明,步骤(3)中所述涂覆及所述干燥处理操作重复至少三次。As a further description of the present invention, the coating and drying operations in step (3) are repeated at least three times.

与现有技术相比,本发明具有以下有益的技术效果:Compared with the prior art, the present invention has the following beneficial technical effects:

本发明中织构化表面对二维材料具有很好的储存能力,可显著提升固体润滑层的使用寿命;The textured surface of the present invention has a good storage capacity for two-dimensional materials, which can significantly improve the service life of the solid lubricating layer;

本发明中渗硼强化层与工件表面为冶金结合,结合强度大,不易剥落,其具有较高的硬度、较好地承载能力、优异的耐磨性以及较强的粘附作用,可对织构化表面起到很好的保护作用以及显著改善工件与固体润滑层之间的结合强度;In the present invention, the boronizing strengthening layer is metallurgically bonded to the surface of the workpiece, the bonding strength is high, and it is not easy to peel off. It has high hardness, good bearing capacity, excellent wear resistance and strong adhesion, and can The textured surface plays a very good protective role and significantly improves the bonding strength between the workpiece and the solid lubricating layer;

本发明中固体润滑层由二维材料组成,依赖于渗硼强化层的粘附作用及织构化表面的储存作用,充分发挥二维材料的抗磨减摩能力,实现长寿命与低摩擦磨损的润滑行为;In the present invention, the solid lubricating layer is composed of two-dimensional materials, relying on the adhesion of the boronizing strengthening layer and the storage function of the textured surface, fully exerting the anti-wear and friction-reducing capabilities of the two-dimensional materials, and realizing long life and low friction and wear lubrication behavior;

本发明中固体润滑层的制备工艺简单,成本低廉,且对设备无特殊要求,可在大气环境下实现所述的固体润滑技术,适于工业应用中快速大面积的制备;且所述固体润滑层的制备工艺适用范围广,可应用于各类钢材、钛合金、锆合金及多主元合金表面。The preparation process of the solid lubricating layer in the present invention is simple, low in cost, and has no special requirements for equipment, and the solid lubricating technology can be realized in an atmospheric environment, which is suitable for rapid and large-area preparation in industrial applications; and the solid lubricating The preparation process of the layer has a wide range of applications, and can be applied to the surfaces of various steel materials, titanium alloys, zirconium alloys and multi-principal alloys.

附图说明Description of drawings

图1是本发明实施例1中渗硼强化层的SEM图。FIG. 1 is an SEM image of a boronizing strengthening layer in Example 1 of the present invention.

图2是本发明实施例1中织构化表面的光学图片。Figure 2 is an optical picture of the textured surface in Example 1 of the present invention.

图3是本发明实施例1制备的固体润滑层的摩擦测试结果。Fig. 3 is the friction test result of the solid lubricating layer prepared in Example 1 of the present invention.

图4是本发明实施例2制备的固体润滑层的摩擦测试结果。Fig. 4 is the friction test result of the solid lubricating layer prepared in Example 2 of the present invention.

图5是对比例1制备的固体润滑层的摩擦测试结果。Fig. 5 is the friction test result of the solid lubricating layer prepared in Comparative Example 1.

图6是对比例2制备的固体润滑层的摩擦测试结果。Fig. 6 is the friction test result of the solid lubricating layer prepared in Comparative Example 2.

图7是对比例3制备的固体润滑层的摩擦测试结果。Fig. 7 is the friction test result of the solid lubricating layer prepared in Comparative Example 3.

具体实施方式Detailed ways

为了能够更清楚地理解本发明的上述目的、特征和优点,下面结合附图和具体实施例对本发明进行详细描述。需要说明的是,在不冲突的情况下,本发明的实施例及实施例中的特征可以相互组合。In order to more clearly understand the above objects, features and advantages of the present invention, the present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments. It should be noted that, in the case of no conflict, the embodiments of the present invention and the features in the embodiments can be combined with each other.

除非另有定义,本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的,不是旨在于限制本发明。Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the technical field of the invention. The terms used herein in the description of the present invention are for the purpose of describing specific embodiments only, and are not intended to limit the present invention.

实施例1:Example 1:

一种含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,该方法包括以下步骤:A method for preparing a low-friction and wear-resistant composite coating containing a boronizing layer and a textured surface, the method comprising the following steps:

S1:渗硼强化层的制备-将轴承钢圆盘工件放入熔盐电解炉中,于900 ℃、20 A的条件下保温30 min,完成渗硼强化层的制备;待工件冷却后,将其放入沸水中,去除工件表面残留的熔盐,随后,对工件进行超声清洗,并放入烘箱干燥,以得到具有渗硼强化层的轴承钢工件,渗硼强化层的SEM图如图1所示。S1: Preparation of boronizing strengthening layer - put the bearing steel disk workpiece into a molten salt electrolytic furnace, and keep it warm for 30 min at 900 °C and 20 A to complete the preparation of boronizing strengthening layer; after the workpiece is cooled, put Put it into boiling water to remove the residual molten salt on the surface of the workpiece, then ultrasonically clean the workpiece and dry it in an oven to obtain a bearing steel workpiece with a boronizing strengthening layer. The SEM image of the boronizing strengthening layer is shown in Figure 1 shown.

其中,渗硼方法还可为固体渗硼或气体渗硼,具体渗硼操作并不局限于本实施例所提到的方式。Wherein, the boronizing method may also be solid boronizing or gas boronizing, and the specific boronizing operation is not limited to the method mentioned in this embodiment.

S2:织构化表面的制备—将S1中带有渗硼强化层的直径30 mm、厚5 mm的轴承钢圆盘工件放置在激光打标机工作台上,通过Ezcad软件控制激光路径,在工件表面得到微圆柱凹坑纹理,凹坑直径100微米,深度120微米,面积密度为16%;表面织构化处理后,使用目数为2000#的砂纸进行磨抛,去除表面残留废屑,将带有织构化表面的工件超声清洗后放入烘箱干燥,得到表面洁净的织构化表面,织构化表面的光学图片如图2所示。S2: Preparation of textured surface—Place the 30 mm diameter and 5 mm thick bearing steel disk workpiece with boronizing strengthening layer in S1 on the laser marking machine workbench, and control the laser path through Ezcad software. Micro-cylindrical pit texture is obtained on the surface of the workpiece. The pit diameter is 100 microns, the depth is 120 microns, and the area density is 16%. The workpiece with the textured surface was ultrasonically cleaned and dried in an oven to obtain a clean textured surface. The optical picture of the textured surface is shown in Figure 2.

其中,表面织构化处理技术还可为压刻加工技术、磨料气射流加工技术、电解加工技术或反应离子刻蚀加工技术,具体表面织构化处理并不局限于本实施例中所提到的方式。Among them, the surface texture treatment technology can also be embossing processing technology, abrasive gas jet processing technology, electrolytic processing technology or reactive ion etching processing technology, and the specific surface texturing treatment is not limited to the ones mentioned in this embodiment. The way.

S3:二维材料分散液的制备-将0.2 g氧化石墨烯与0.2 g二硫化钼分别加入试剂瓶中,添加去离子水至100 g,在超声作用下,获得分散均匀的0.2 wt%氧化石墨烯和0.2wt%二硫化钼混合二维材料分散液。S3: Preparation of two-dimensional material dispersion - add 0.2 g graphene oxide and 0.2 g molybdenum disulfide to the reagent bottle respectively, add deionized water to 100 g, and obtain uniformly dispersed 0.2 wt% graphite oxide under the action of ultrasound Alkene and 0.2wt% molybdenum disulfide mixed two-dimensional material dispersion.

其中,二维材料还可为石墨烯、氧化石墨烯、二硫化钼、二硫化钨、二硒化钼以及六方氮化硼中的一种或多种。Wherein, the two-dimensional material may also be one or more of graphene, graphene oxide, molybdenum disulfide, tungsten disulfide, molybdenum diselenide and hexagonal boron nitride.

S4:固体润滑层的制备-使用滴涂法将S3中的二维材料分散液涂覆在S2中的工件表面,并放入干燥箱中于60℃进行干燥处理;待干燥完成后,重复上述操作5次,获得基于渗硼强化层与织构化表面的固体润滑层。S4: Preparation of solid lubricating layer - use the drop coating method to coat the two-dimensional material dispersion in S3 on the surface of the workpiece in S2, and put it in a drying oven at 60°C for drying treatment; after the drying is completed, repeat the above The operation was performed 5 times to obtain a solid lubricating layer based on a boronizing strengthening layer and a textured surface.

S5:摩擦测试-将经过上述固体润滑技术处理过的工件置于多功能摩擦磨损试验机上进行摩擦测试,施加10 N荷载、6 mm/s线速度,在200℃下,获得了稳定的超低摩擦状态(cof=0.025),摩擦测试结果如图3所示。S5: Friction test - put the workpiece treated by the above solid lubrication technology on a multi-functional friction and wear testing machine for friction test, apply a load of 10 N, a line speed of 6 mm/s, and obtain a stable ultra-low temperature at 200 °C. Friction state (cof=0.025), friction test results are shown in Figure 3.

实施例2:Example 2:

一种含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,该方法包括以下步骤:A method for preparing a low-friction and wear-resistant composite coating containing a boronizing layer and a textured surface, the method comprising the following steps:

S1:渗硼强化层的制备-将轴承钢圆盘工件放入熔盐电解炉中,于900 ℃、20 A的条件下保温30 min,完成渗硼强化层的制备;待工件冷却后,将其放入沸水中,去除工件表面残留的熔盐,随后,对工件进行超声清洗,并放入烘箱干燥,以得到具有渗硼强化层的轴承钢工件。S1: Preparation of boronizing strengthening layer - put the bearing steel disk workpiece into a molten salt electrolytic furnace, and keep it warm for 30 min at 900 °C and 20 A to complete the preparation of boronizing strengthening layer; after the workpiece is cooled, put It is placed in boiling water to remove residual molten salt on the surface of the workpiece, and then the workpiece is ultrasonically cleaned and dried in an oven to obtain a bearing steel workpiece with a boronizing strengthening layer.

其中,渗硼方法还可为固体渗硼或气体渗硼,具体渗硼操作并不局限于本实施例所提到的方式。Wherein, the boronizing method may also be solid boronizing or gas boronizing, and the specific boronizing operation is not limited to the method mentioned in this embodiment.

S2:织构化表面的制备—将S1中带有渗硼强化层的直径30 mm、厚5 mm的轴承钢圆盘工件放置在激光打标机工作台上,通过Ezcad软件控制激光路径,在工件表面得到微圆柱凹坑纹理,凹坑直径100 μm,深度120 μm,面积密度为16%;表面织构化处理后,使用目数为2000#的砂纸进行磨抛,去除表面残留废屑,将带有织构化表面的工件超声清洗后放入烘箱干燥,以得到带有渗硼强化层与织构化表面的待涂覆工件。S2: Preparation of textured surface—Place the 30 mm diameter and 5 mm thick bearing steel disk workpiece with boronizing strengthening layer in S1 on the laser marking machine workbench, and control the laser path through Ezcad software. Micro-cylindrical pit texture was obtained on the surface of the workpiece. The pit diameter was 100 μm, the depth was 120 μm, and the area density was 16%. The workpiece with the textured surface is ultrasonically cleaned and then dried in an oven to obtain a workpiece to be coated with a boronizing strengthening layer and a textured surface.

其中,表面织构化处理技术还可为压刻加工技术、磨料气射流加工技术、电解加工技术或反应离子刻蚀加工技术,具体表面织构化处理并不局限于本实施例中所提到的方式。Among them, the surface texture treatment technology can also be embossing processing technology, abrasive gas jet processing technology, electrolytic processing technology or reactive ion etching processing technology, and the specific surface texturing treatment is not limited to the ones mentioned in this embodiment. The way.

S3:二维材料分散液的制备-将0.2 g氧化石墨烯与0.2 g二硫化钼分别加入试剂瓶中,添加去离子水至100g,在超声作用下,获得分散均匀的0.2 wt%氧化石墨烯和0.2 wt%二硫化钼混合二维材料分散液。S3: Preparation of two-dimensional material dispersion - add 0.2 g graphene oxide and 0.2 g molybdenum disulfide to the reagent bottle respectively, add deionized water to 100 g, and obtain uniformly dispersed 0.2 wt% graphene oxide under the action of ultrasound Mix the two-dimensional material dispersion with 0.2 wt% molybdenum disulfide.

其中,二维材料还可为石墨烯、氧化石墨烯、二硫化钼、二硫化钨、二硒化钼以及六方氮化硼中的一种或多种。Wherein, the two-dimensional material may also be one or more of graphene, graphene oxide, molybdenum disulfide, tungsten disulfide, molybdenum diselenide and hexagonal boron nitride.

S4:固体润滑层的制备-使用滴涂法将S3中的二维材料分散液涂覆在S2中的工件表面,并放入干燥箱中于60℃进行干燥处理;待干燥完成后,重复上述操作5次,获得基于渗硼强化层与织构化表面的固体润滑层。S4: Preparation of solid lubricating layer - use the drop coating method to coat the two-dimensional material dispersion in S3 on the surface of the workpiece in S2, and put it in a drying oven at 60°C for drying treatment; after the drying is completed, repeat the above The operation was performed 5 times to obtain a solid lubricating layer based on a boronizing strengthening layer and a textured surface.

S5:摩擦测试-将经过上述固体润滑技术处理过的工件置于多功能摩擦磨损试验机上进行摩擦测试,施加10 N荷载、6 mm/s线速度,在室温下,获得了长时稳定低摩擦状态,摩擦测试结果如图4所示。S5: Friction test - put the workpiece treated by the above solid lubrication technology on a multi-functional friction and wear testing machine for friction test, apply a load of 10 N, and a line speed of 6 mm/s. At room temperature, a long-term stable low friction is obtained. state, the friction test results are shown in Fig. 4.

对比例1:Comparative example 1:

一种测试不含渗硼层与织构表面的复合涂层摩擦学行为的方法,该方法包括以下步骤:A method for testing the tribological behavior of a composite coating not containing a boronizing layer and a textured surface, the method comprising the following steps:

S1:二维材料分散液的制备-将0.2 g氧化石墨烯与0.2 g二硫化钼分别加入试剂瓶中,添加去离子水至100g,在超声作用下,获得分散均匀的0.2 wt%氧化石墨烯和0.2 wt%二硫化钼混合二维材料分散液。S1: Preparation of two-dimensional material dispersion - add 0.2 g graphene oxide and 0.2 g molybdenum disulfide to the reagent bottle respectively, add deionized water to 100 g, and obtain uniformly dispersed 0.2 wt% graphene oxide under the action of ultrasound Mix the two-dimensional material dispersion with 0.2 wt% molybdenum disulfide.

其中,二维材料还可为石墨烯、氧化石墨烯、二硫化钼、二硫化钨、二硒化钼以及六方氮化硼中的一种或多种。Wherein, the two-dimensional material may also be one or more of graphene, graphene oxide, molybdenum disulfide, tungsten disulfide, molybdenum diselenide and hexagonal boron nitride.

S2:固体润滑层的制备-使用滴涂法将S1中的二维材料分散液涂覆在原始轴承钢工件表面,并放入干燥箱中于60℃进行干燥处理;待干燥完成后,重复上述操作5次,获得涂覆有固体润滑层的轴承钢工件。S2: Preparation of solid lubricating layer - use the drop coating method to coat the two-dimensional material dispersion in S1 on the surface of the original bearing steel workpiece, and put it in a drying oven at 60°C for drying treatment; after the drying is completed, repeat the above The operation was performed 5 times to obtain a bearing steel workpiece coated with a solid lubricating layer.

S3:摩擦测试-将经过涂覆有固体润滑层的工件置于多功能摩擦磨损试验机上进行摩擦测试,施加10 N荷载、6 mm/s线速度,在室温下并未获得稳定的低摩擦状态(摩擦系数于0.4附近波动),摩擦测试结果如图5所示。S3: Friction test - the workpiece coated with a solid lubricant layer was placed on a multi-functional friction and wear testing machine for friction testing, a load of 10 N was applied and a line speed of 6 mm/s was applied, and a stable low friction state was not obtained at room temperature (The friction coefficient fluctuates around 0.4), and the friction test results are shown in Figure 5.

对比例2:Comparative example 2:

一种测试仅含织构表面的复合涂层摩擦学行为的方法,该方法包括以下步骤:A method of testing the tribological behavior of composite coatings containing only textured surfaces, the method comprising the steps of:

S1:织构化表面的制备—将直径30 mm、厚5 mm的轴承钢圆盘工件放置在激光打标机工作台上,通过Ezcad软件控制激光路径,在工件表面得到微圆柱凹坑纹理,凹坑直径100μm,深度120 μm,面积密度为16%;表面织构化处理后,使用目数为2000#的砂纸进行磨抛,去除表面残留废屑,将带有织构化表面的工件超声清洗后放入烘箱干燥,得到表面洁净的织构化表面。S1: Preparation of textured surface—place a bearing steel disk workpiece with a diameter of 30 mm and a thickness of 5 mm on the workbench of a laser marking machine, and control the laser path through Ezcad software to obtain a micro-cylindrical pit texture on the surface of the workpiece. The diameter of the pit is 100 μm, the depth is 120 μm, and the area density is 16%. After the surface texture treatment, sandpaper with a mesh number of 2000# is used for grinding and polishing to remove residual waste on the surface, and the workpiece with the textured surface is ultrasonically After cleaning, it is placed in an oven to dry to obtain a textured surface with a clean surface.

其中,表面织构化处理技术还可为压刻加工技术、磨料气射流加工技术、电解加工技术或反应离子刻蚀加工技术,具体表面织构化处理并不局限于本实施例中所提到的方式。Among them, the surface texture treatment technology can also be embossing processing technology, abrasive gas jet processing technology, electrolytic processing technology or reactive ion etching processing technology, and the specific surface texturing treatment is not limited to the ones mentioned in this embodiment. The way.

S2:二维材料分散液的制备-将0.2 g氧化石墨烯与0.2 g二硫化钼分别加入试剂瓶中,添加去离子水至100g,在超声作用下,获得分散均匀的0.2 wt%氧化石墨烯和0.2 wt%二硫化钼混合二维材料分散液。S2: Preparation of two-dimensional material dispersion - add 0.2 g graphene oxide and 0.2 g molybdenum disulfide to the reagent bottle respectively, add deionized water to 100 g, and obtain uniformly dispersed 0.2 wt% graphene oxide under the action of ultrasound Mix the two-dimensional material dispersion with 0.2 wt% molybdenum disulfide.

其中,二维材料还可为石墨烯、氧化石墨烯、二硫化钼、二硫化钨、二硒化钼以及六方氮化硼中的一种或多种。Wherein, the two-dimensional material may also be one or more of graphene, graphene oxide, molybdenum disulfide, tungsten disulfide, molybdenum diselenide and hexagonal boron nitride.

S3:固体润滑层的制备-使用滴涂法将S3中的二维材料分散液涂覆在带有织构化表面的工件上,并放入干燥箱中于60℃进行干燥处理;待干燥完成后,重复上述操作5次,获得基于织构化表面的固体润滑层。S3: Preparation of solid lubricating layer - use the drop coating method to coat the two-dimensional material dispersion in S3 on the workpiece with a textured surface, and put it in a drying oven at 60°C for drying treatment; wait for the drying to complete Finally, the above operation was repeated 5 times to obtain a solid lubricating layer based on the textured surface.

S4:摩擦测试-将经过上述固体润滑技术处理过的工件置于多功能摩擦磨损试验机上进行摩擦测试,施加10 N荷载、6 mm/s线速度,在室温下,摩擦系数在0.1附近仅维持了100 s的时间,便升高至0.4附近,未能获得稳定的超低摩擦状态,摩擦测试结果如图6所示。S4: Friction test - put the workpiece treated by the above solid lubrication technology on a multi-functional friction and wear testing machine for friction test, apply a load of 10 N, and a line speed of 6 mm/s. At room temperature, the friction coefficient is only maintained at around 0.1 After 100 s, it rises to around 0.4, failing to obtain a stable ultra-low friction state. The friction test results are shown in Figure 6.

对比例3:Comparative example 3:

一种测试仅基于渗硼层的复合涂层摩擦学行为的方法,该方法包括以下步骤:A method of testing the tribological behavior of composite coatings based solely on boronizing layers, the method comprising the following steps:

S1:渗硼强化层的制备-将直径30 mm、厚5 mm的轴承钢圆盘工件放入熔盐电解炉中,于900 ℃、20 A的条件下保温30 min,完成渗硼强化层的制备;待工件冷却后,将其放入沸水中,去除工件表面残留的熔盐,随后,对工件进行超声清洗,并放入烘箱干燥,以得到带有渗硼强化层的待涂覆工件。S1: Preparation of boronizing strengthening layer - put a bearing steel disc workpiece with a diameter of 30 mm and a thickness of 5 mm into a molten salt electrolytic furnace, and keep it warm for 30 min at 900 °C and 20 A to complete the boronizing strengthening layer. Preparation: After the workpiece is cooled, put it into boiling water to remove the molten salt remaining on the surface of the workpiece, then ultrasonically clean the workpiece and dry it in an oven to obtain a workpiece to be coated with a boronizing strengthening layer.

其中,渗硼方法还可为固体渗硼或气体渗硼,具体渗硼操作并不局限于本实施例所提到的方式。Wherein, the boronizing method may also be solid boronizing or gas boronizing, and the specific boronizing operation is not limited to the method mentioned in this embodiment.

S2:二维材料分散液的制备-将0.2 g氧化石墨烯与0.2 g二硫化钼分别加入试剂瓶中,添加去离子水至100g,在超声作用下,获得分散均匀的0.2 wt%氧化石墨烯和0.2 wt%二硫化钼混合二维材料分散液。S2: Preparation of two-dimensional material dispersion - add 0.2 g graphene oxide and 0.2 g molybdenum disulfide to the reagent bottle respectively, add deionized water to 100 g, and obtain uniformly dispersed 0.2 wt% graphene oxide under the action of ultrasound Mix the two-dimensional material dispersion with 0.2 wt% molybdenum disulfide.

其中,二维材料还可为石墨烯、氧化石墨烯、二硫化钼、二硫化钨、二硒化钼以及六方氮化硼中的一种或多种。Wherein, the two-dimensional material may also be one or more of graphene, graphene oxide, molybdenum disulfide, tungsten disulfide, molybdenum diselenide and hexagonal boron nitride.

S3:固体润滑层的制备-使用滴涂法将S2中的二维材料分散液涂覆在S1中带有渗硼强化层的工件表面,并放入干燥箱中于60℃进行干燥处理;待干燥完成后,重复上述操作5次,获得基于渗硼强化层的固体润滑层。S3: Preparation of solid lubricating layer - use the drop coating method to coat the two-dimensional material dispersion in S2 on the surface of the workpiece with boronizing strengthening layer in S1, and put it in a drying oven at 60°C for drying treatment; After the drying was completed, the above operation was repeated 5 times to obtain a solid lubricating layer based on the boronizing strengthening layer.

S4:摩擦测试-将经过上述固体润滑技术处理过的工件置于多功能摩擦磨损试验机上进行摩擦测试,施加10 N荷载、6 mm/s线速度,在室温下,并未获得稳定的低摩擦状态,摩擦测试结果如图7所示。S4: Friction test - put the workpiece treated by the above solid lubrication technology on a multi-functional friction and wear testing machine for friction test, apply a load of 10 N, and a line speed of 6 mm/s. At room temperature, stable low friction was not obtained state, the friction test results are shown in Fig. 7.

最后应说明的是,以上实施例仅用以说明本发明的技术方案而非限制,尽管参照较佳实施例对本发明进行了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或等同替换,而不脱离本发明技术方案的精神和范围。Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention without limitation. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be Modifications or equivalent replacements can be made without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1.一种含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,其特征在于,包括如下步骤:1. a preparation method of a low-friction and wear-resistant composite coating containing a boronized layer and texture surface, is characterized in that, comprises the steps: 步骤(1)进行渗硼强化处理,在工件表面上制备渗硼强化层,然后去除渗硼处理后工件表面的残留物;Step (1) performing boronizing strengthening treatment, preparing a boronizing strengthening layer on the surface of the workpiece, and then removing the residue on the surface of the workpiece after boriding treatment; 步骤(2)对渗硼处理后的工件进行表面织构化处理,使工件表面形成凹坑;Step (2) performing surface texturing treatment on the boronized workpiece to form pits on the surface of the workpiece; 步骤(3)将二维材料分散液涂覆于工件表面,并进行干燥处理,重复所述涂覆及所述干燥处理操作,直至获得基于渗硼强化层与织构化表面的固体自润滑涂层。Step (3) Coating the two-dimensional material dispersion on the surface of the workpiece, and performing drying treatment, repeating the coating and drying treatment operations until a solid self-lubricating coating based on a boronizing strengthening layer and a textured surface is obtained. layer. 2.根据权利要求1所述的含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,其特征在于,所述工件为钢、钛合金、多主元合金中的一种。2. the preparation method of the low-friction and wear-resistant composite coating containing boronizing layer and textured surface according to claim 1, is characterized in that, described workpiece is a kind of in steel, titanium alloy, multi-principal element alloy . 3.根据权利要求1所述的含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,其特征在于,步骤(1)中所述渗硼强化处理采用固体渗硼工艺或熔盐电解渗硼工艺中的一种。3. The preparation method of the low-friction and wear-resistant composite coating containing boronizing layer and textured surface according to claim 1, characterized in that, the boronizing strengthening treatment in step (1) adopts solid boronizing process or One of the molten salt electrolytic boronizing processes. 4.根据权利要求1所述的含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,其特征在于,步骤(1)中进行所述渗硼强化处理前需对工件表面进行清洗;且采用超声清洗去除渗硼处理后工件表面的残留物。4. The preparation method of the low-friction and wear-resistant composite coating containing boronizing layer and textured surface according to claim 1, characterized in that, before performing the boronizing strengthening treatment in step (1), the workpiece surface needs to be cleaning; and ultrasonic cleaning is used to remove the residues on the surface of the workpiece after boriding treatment. 5.根据权利要求1所述的含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,其特征在于,步骤(2)中所述表面织构化处理包括压刻加工处理、磨料气射流加工处理、电解加工处理、反应离子刻蚀加工处理、激光表面织构处理中的一种。5. The method for preparing a low-friction and wear-resistant composite coating containing a boronized layer and a textured surface according to claim 1, wherein the surface texturing treatment in step (2) includes embossing processing , abrasive gas jet processing, electrolytic processing, reactive ion etching processing, and laser surface texturing. 6.根据权利要求1所述的含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,其特征在于,步骤(2)中工件表面形成的所述凹坑为微圆柱凹坑,且所述凹坑直径为20-300 μm,深度为20-500 μm,面积密度为5%-35%。6. The method for preparing a low-friction and wear-resistant composite coating containing a boronized layer and a textured surface according to claim 1, wherein the pits formed on the surface of the workpiece in step (2) are microcylindrical pits pits, and the pits have a diameter of 20-300 μm, a depth of 20-500 μm, and an area density of 5%-35%. 7.根据权利要求1所述的含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,其特征在于,步骤(3)中所述二维材料包括石墨烯、氧化石墨烯、二硫化钼、二硫化钨、二硒化钼以及六方氮化硼中的一种或多种。7. The method for preparing a low-friction and wear-resistant composite coating containing a boronizing layer and a textured surface according to claim 1, wherein the two-dimensional material in step (3) includes graphene, graphene oxide One or more of , molybdenum disulfide, tungsten disulfide, molybdenum diselenide and hexagonal boron nitride. 8.根据权利要求1所述的含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,其特征在于,步骤(3)中所述二维材料分散液的溶剂包括水、烷基胺、聚乙烯亚胺、聚丙烯酸、聚乙二醇中的一种或多种。8. The method for preparing a low-friction and wear-resistant composite coating containing a boronized layer and a textured surface according to claim 1, wherein the solvent of the two-dimensional material dispersion in step (3) includes water, One or more of alkylamine, polyethyleneimine, polyacrylic acid, polyethylene glycol. 9.根据权利要求1所述的含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,其特征在于,步骤(3)中所述涂覆的方法包括滴涂、喷涂、旋涂、电泳沉积中的一种。9. The preparation method of the low-friction and wear-resistant composite coating containing boronizing layer and textured surface according to claim 1, characterized in that the coating method in step (3) includes drip coating, spray coating, One of spin coating and electrophoretic deposition. 10.根据权利要求1所述的含渗硼层与织构表面的低摩擦耐磨复合涂层的制备方法,其特征在于,步骤(3)中所述涂覆及所述干燥处理操作重复至少三次。10. The method for preparing a low-friction and wear-resistant composite coating containing a boronized layer and a textured surface according to claim 1, wherein the coating and drying operations in step (3) are repeated for at least three times.
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