CN115612965A - A kind of preparation method of completely amorphous coating - Google Patents
A kind of preparation method of completely amorphous coating Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及一种完全非晶涂层的制备方法，属于超音速火焰喷涂技术领域。The invention relates to a preparation method of a completely amorphous coating, which belongs to the technical field of supersonic flame spraying.
背景技术Background technique
块体非晶合金的出现，实现了用常规铸造方法制备大尺寸非晶合金，并使非晶合金作为结构材料的应用成为可能。非晶合金在许多方面呈现出较常规合金材料更优异的性能，如高硬度、高弹性模量、高耐磨性以及优异的耐腐蚀性能。在对材料的各种性能要求日益苛刻的21世纪，非晶合金材料有望成为最重要的新型工程材料之一。The emergence of bulk amorphous alloys has realized the preparation of large-size amorphous alloys by conventional casting methods, and made it possible to use amorphous alloys as structural materials. Amorphous alloys exhibit better performance than conventional alloy materials in many aspects, such as high hardness, high elastic modulus, high wear resistance and excellent corrosion resistance. In the 21st century, when the various properties of materials are increasingly demanding, amorphous alloy materials are expected to become one of the most important new engineering materials.
然而，块体非晶合金的塑性很差，这严重限制了其实际应用。由于在微米尺度下，非晶合金的脆性会大大改善，将非晶合金微粉末喷涂到韧性基体上制成非晶涂层是一个有效改善脆性并发挥其耐磨耐蚀特性的方法。热喷涂方法制备的非晶合金涂层，呈现出高强度、高耐磨性及优异的耐腐蚀性能，在海洋、电力、石化等国家重大领域关键部件上具有重要应用前景。然而，热喷涂涂层使役过程中一个突出问题是其易于发生分层或局部开裂，最终导致涂层失效，这与涂层制备过程中形成的氧化物及孔隙等缺陷密切相关。涂层中氧化物和孔隙的形成由喷涂过程粉末粒子的速度和温度变化规律决定，而粒子的速度和温度特性与超音速火焰喷涂喷嘴结构息息相关。因而，超音速火焰喷涂喷嘴结构特性是制备高致密度、低氧化缺陷、高性能非晶合金涂层的关键。However, the poor plasticity of bulk amorphous alloys severely limits their practical applications. Since the brittleness of amorphous alloys will be greatly improved at the micron scale, it is an effective method to improve brittleness and exert its wear and corrosion resistance characteristics by spraying amorphous alloy micropowders on tough substrates to form amorphous coatings. The amorphous alloy coating prepared by thermal spraying method shows high strength, high wear resistance and excellent corrosion resistance, and has important application prospects in key components in major national fields such as marine, electric power, and petrochemical. However, a prominent problem in the service process of thermal spray coatings is that they are prone to delamination or local cracking, which eventually leads to coating failure, which is closely related to defects such as oxides and pores formed during the coating preparation process. The formation of oxides and pores in the coating is determined by the velocity and temperature variation of the powder particles during the spraying process, and the velocity and temperature characteristics of the particles are closely related to the structure of the supersonic flame spraying nozzle. Therefore, the structural characteristics of supersonic flame spraying nozzles are the key to the preparation of high-density, low-oxidation defects, and high-performance amorphous alloy coatings.
发明内容Contents of the invention
本发明的目的在于提供一种超音速火焰喷涂喷嘴优化方法及高性能非晶涂层的制备方法，所述方法为优化超音速火焰喷涂喷嘴结构，具体为：超音速火焰喷涂喷嘴采用拉瓦尔喷嘴，通过优化设计拉瓦尔喷嘴收缩段和发散段，使非晶粉末在撞击基板的速度高且处于半熔化状态，之后在基板上形成铁基完全非晶涂层。The object of the present invention is to provide a method for optimizing a supersonic flame spraying nozzle and a method for preparing a high-performance amorphous coating. The method is to optimize the structure of a supersonic flame spraying nozzle, specifically: the supersonic flame spraying nozzle adopts Laval nozzle , by optimizing the design of the contraction section and divergence section of the Laval nozzle, the amorphous powder hits the substrate at a high speed and is in a semi-molten state, and then forms a completely amorphous iron-based coating on the substrate.
一种完全非晶涂层的制备方法，所述方法为超音速火焰喷涂法，其中，原料为非晶粉末，所采用的超音速火焰喷涂装置的喷嘴为拉瓦尔喷嘴，所述拉瓦尔喷嘴由发散段和收缩段组成，其中，A preparation method of a completely amorphous coating, the method is a supersonic flame spraying method, wherein the raw material is an amorphous powder, and the nozzle of the supersonic flame spraying device adopted is a Laval nozzle, and the Laval nozzle is composed of consists of a divergent segment and a contractive segment, where,
所述收缩段长度为21～56mm，收缩段线型采用维托辛斯基曲线设计法；The length of the shrinkage section is 21 to 56mm, and the line shape of the shrinkage section adopts the Witoshinski curve design method;
所述发散段长度为170～200mm，喉口部直径12～16mm。The length of the diverging section is 170-200 mm, and the diameter of the throat is 12-16 mm.
本发明所述拉瓦尔喷嘴口与燃烧室相接，其尺寸与燃烧室入口相匹配。优选，本发明所述拉瓦尔喷嘴的喷嘴口处直径为71mm。The opening of the Laval nozzle of the present invention is connected with the combustion chamber, and its size matches the entrance of the combustion chamber. Preferably, the diameter of the nozzle opening of the Laval nozzle of the present invention is 71mm.
本发明所述完全非晶涂层的制备方法中所使用的超音速火焰喷涂装置为现有技术公开的超音速火焰喷涂装置，可商业购得。The supersonic flame spraying device used in the preparation method of the completely amorphous coating in the present invention is a supersonic flame spraying device disclosed in the prior art, which is commercially available.
本发明所述超音速火焰喷涂装置与现有技术的差别主要在于喷嘴的设计与使用。The difference between the supersonic flame spraying device of the present invention and the prior art mainly lies in the design and use of the nozzle.
本发明所完全非晶涂层的制备方法中，所得涂层为完全非晶合金涂层，孔隙率低于2.1％，氧含量低于1.8％。In the preparation method of the completely amorphous coating of the present invention, the obtained coating is a completely amorphous alloy coating, the porosity is lower than 2.1%, and the oxygen content is lower than 1.8%.
优选地，所述非晶粉末粒子在撞击基板之前熔化指数小于1。Preferably, the amorphous powder particles have a melting index of less than 1 before impacting the substrate.
优选地，所述非晶粉末的直径为10～60μm；进一步优选地，所述非晶粉末的直径为20～30μm。Preferably, the diameter of the amorphous powder is 10-60 μm; further preferably, the diameter of the amorphous powder is 20-30 μm.
优选地，所述超音速火焰喷涂法中，所述超音速火焰喷涂法中，喷涂距离为150～200mm；空气压力为850～940KPa；丙烷压力为900～980KPa；氮气压力为700～800KPa。Preferably, in the supersonic flame spraying method, in the supersonic flame spraying method, the spraying distance is 150-200mm; the air pressure is 850-940KPa; the propane pressure is 900-980KPa; the nitrogen pressure is 700-800KPa.
本发明通过上述超音速火焰喷涂拉瓦尔喷嘴的优化，喷涂过程中，非晶粉末获得较高的速度，在撞击基板前非晶粉末处于半熔化状态，粉末粒子的驻留时间短，降低涂层中孔隙和氧化的缺陷数量。In the present invention, through the optimization of the Laval nozzle for supersonic flame spraying, during the spraying process, the amorphous powder obtains a higher speed, and the amorphous powder is in a semi-melted state before hitting the substrate, and the residence time of the powder particles is short, reducing the coating Number of defects in mesopores and oxidation.
本发明的有益效果为：本发明提供一种超音速火焰喷涂喷嘴优化方法及高性能非晶涂层的制备方法，超音速火焰喷涂喷嘴采用拉瓦尔喷嘴，优化拉瓦尔喷发散段和收缩段结构，促使粉末粒子在撞击基板之前处于半熔化状态、较高的撞击速度、较短的驻留时间，从而减少所制备铁基非晶涂层中的孔隙和氧化缺陷，增加与基体结合强度，防止涂层开裂。The beneficial effects of the present invention are: the present invention provides a supersonic flame spraying nozzle optimization method and a preparation method of a high-performance amorphous coating, the supersonic flame spraying nozzle adopts a Laval nozzle, and optimizes the structure of the diverging section and the contracting section of Laval spraying , so that the powder particles are in a semi-melted state, higher impact velocity, and shorter residence time before impacting the substrate, thereby reducing the pores and oxidation defects in the prepared iron-based amorphous coating, increasing the bonding strength with the substrate, and preventing Coating cracked.
与现有技术相比，本发明具有下述特点：Compared with prior art, the present invention has following characteristics:
(1)本发明方法通过优化超音速喷嘴结构，解决了以往喷涂工艺参数优化过程中大量资源浪费问题，降低了非晶涂层制备成本，并获得了低孔隙率、低氧化缺陷的铁基非晶涂层，提高铁基非晶涂层与基体的结合力及耐腐蚀性能，推动其更广泛的应用。(1) By optimizing the structure of the supersonic nozzle, the method of the present invention solves the problem of waste of a large amount of resources in the optimization process of the previous spraying process parameters, reduces the preparation cost of the amorphous coating, and obtains an iron-based amorphous coating with low porosity and low oxidation defects. Crystal coating, improve the bonding force and corrosion resistance of iron-based amorphous coating and substrate, and promote its wider application.
(2)超音速火焰喷涂的拉瓦尔喷嘴收缩段型线采用维托辛斯基曲线设计方法，与传统的收缩段采用直线型线相比，维氏曲线具有进口收缩较快、中后部收缩与进口处相比要小、出口速度与加速性都比较均匀的优点，因此收缩段维氏曲线具有均匀的速度和温度分布特点，收缩段焰流的温度场和速度场增加地更加均匀，粉末粒子获得更高的冲击速度，更重要的是粉末粒子在喷涂过程中的驻留时间大大降低，从而降低涂层氧化缺陷的产生。此外，拉瓦尔喷嘴收缩段长度的优化，有效地控制粉末粒子的熔化状态，减少涂层中的孔隙缺陷，提高涂层致密性以及与基体结合强度。(2) The contraction section of the Laval nozzle for supersonic flame spraying adopts the Vitoshinski curve design method. Compared with the traditional contraction section using a straight line, the Vickers curve has a faster inlet contraction and a middle and rear contraction. Compared with the inlet, it has the advantages of being smaller, and the outlet velocity and acceleration are relatively uniform, so the Vickers curve of the contraction section has uniform velocity and temperature distribution characteristics, and the temperature field and velocity field of the contraction section flame flow increase more uniformly, and the powder The particles get a higher impact velocity, and more importantly, the residence time of the powder particles in the spraying process is greatly reduced, thereby reducing the generation of coating oxidation defects. In addition, the optimization of the length of the shrinking section of the Laval nozzle can effectively control the melting state of powder particles, reduce pore defects in the coating, and improve the compactness of the coating and the bonding strength with the substrate.
附图说明Description of drawings
图1(a)是拉瓦尔喷嘴结构示意图；(b)是对比例1中拉瓦尔喷嘴收缩段线型为直线的喷嘴结构示意图；Fig. 1 (a) is the structure schematic diagram of Laval nozzle; (b) is the nozzle structure schematic diagram of the contraction section line type of Laval nozzle in comparative example 1;
图2是实施例1制备的涂层XRD图；Fig. 2 is the coating XRD figure that embodiment 1 prepares;
图3是不同直径的粉末颗子飞行过程中熔化特性图；Fig. 3 is a diagram of melting characteristics during flight of powder particles of different diameters;
图4为不同直径的粉末颗子飞行过程中速度变化图。Fig. 4 is a diagram of velocity variation of powder particles with different diameters during flight.
图5为实施例1制备的涂层表面和截面SEM照片；其中：(a)表面；(b)截面。Fig. 5 is the SEM photo of the coating surface and cross-section prepared in Example 1; wherein: (a) surface; (b) cross-section.
具体实施方式detailed description
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明，但不以任何方式限制本发明。The following non-limiting examples can enable those skilled in the art to understand the present invention more fully, but do not limit the present invention in any way.
下述实施例中所述试验方法，如无特殊说明，均为常规方法；所述试剂和材料，如无特殊说明，均可从商业途径获得。The test methods described in the following examples, unless otherwise specified, are conventional methods; the reagents and materials, unless otherwise specified, can be obtained from commercial sources.
下述实施例中，所用用超音速火焰喷涂装置为KERMETICO公司的AK07。。In the following examples, the supersonic flame spraying device used is AK07 of KERMETICO Company. .
实施例1Example 1
采用超音速火焰喷涂技术制备铁基非晶涂层，其中：选取拉瓦尔喷嘴收缩段线型为维托辛斯基曲线，收缩段长度：50mm，拉瓦尔喷嘴发散段长度：190mm，喉口部直径14mm，如图1所示。所用非晶粉末尺寸为20-30μm，喷涂距离为180mm，空气压力为900KPa；丙烷压力为950KPa；氮气压力为760KPa。据此制备的铁基非晶涂层，由图2表明所制备的涂层为完全非晶特征。图3是不同直径的粉末颗子飞行过程中熔化特性，其中，直径为10μm和20μm粉末粒子熔化指数小于1，处于半熔化状态，图4为不同直径的粉末颗子飞行过程中速度变化特性，由图5(a)可以看出涂层的表面熔化的状态良好，没有未熔颗粒和熔化过度现象，根据图5(b)计算获得涂层的孔隙率为1.1％，涂层氧含量为0.75％。Supersonic flame spraying technology is used to prepare iron-based amorphous coatings. Among them: the line shape of the contraction section of the Laval nozzle is selected as the Witousinski curve, the length of the contraction section: 50mm, the length of the divergence section of the Laval nozzle: 190mm, and the throat part 14mm in diameter, as shown in Figure 1. The size of the amorphous powder used is 20-30 μm, the spraying distance is 180mm, the air pressure is 900KPa; the propane pressure is 950KPa; the nitrogen pressure is 760KPa. According to the prepared iron-based amorphous coating, Figure 2 shows that the prepared coating is completely amorphous. Figure 3 shows the melting characteristics of powder particles with different diameters during flight. Among them, the melting index of powder particles with a diameter of 10 μm and 20 μm is less than 1, and they are in a semi-melted state. Figure 4 shows the velocity change characteristics of powder particles with different diameters during flight. It can be seen from Figure 5(a) that the surface of the coating is in a good state of melting, without unmelted particles and excessive melting. According to Figure 5(b), the porosity of the coating is 1.1%, and the oxygen content of the coating is 0.75 %.
实施例2Example 2
采用超音速火焰喷涂技术制备铁基非晶涂层，其中：选取拉瓦尔喷嘴收缩段线型为维托辛斯基曲线，收缩段长度：21mm，拉瓦尔喷嘴发散段长度：190mm，喉口部直径14mm。所用非晶粉末尺寸为20-30μm，喷涂距离为180mm，空气压力为900KPa；丙烷压力为950KPa；氮气压力为760KPa。据此制备的铁基非晶涂层，涂层的孔隙率为2.0％，涂层氧含量为1.03％。Supersonic flame spraying technology is used to prepare iron-based amorphous coatings. Among them: the line shape of the Laval nozzle contraction section is selected as the Witousinski curve, the length of the contraction section: 21mm, the length of the divergence section of the Laval nozzle: 190mm, and the throat part 14mm in diameter. The size of the amorphous powder used is 20-30 μm, the spraying distance is 180mm, the air pressure is 900KPa; the propane pressure is 950KPa; the nitrogen pressure is 760KPa. According to the prepared iron-based amorphous coating, the porosity of the coating is 2.0%, and the oxygen content of the coating is 1.03%.
实施例3Example 3
采用超音速火焰喷涂技术制备铁基非晶涂层，其中：选取拉瓦尔喷嘴收缩段线型为维托辛斯基曲线，收缩段长度：28mm，拉瓦尔喷嘴发散段长度：190mm，喉口部直径14mm。所用非晶粉末尺寸为20-30μm，喷涂距离为180mm，空气压力为900KPa；丙烷压力为950KPa；氮气压力为760KPa。据此制备的铁基非晶涂层，涂层的孔隙率为1.8％，涂层氧含量为1.33％。Supersonic flame spraying technology was used to prepare iron-based amorphous coatings. Among them: the line shape of the Laval nozzle contraction section was selected as the Witousinski curve, the length of the contraction section: 28mm, the length of the divergence section of the Laval nozzle: 190mm, and the throat part 14mm in diameter. The size of the amorphous powder used is 20-30 μm, the spraying distance is 180mm, the air pressure is 900KPa; the propane pressure is 950KPa; the nitrogen pressure is 760KPa. According to the prepared iron-based amorphous coating, the porosity of the coating is 1.8%, and the oxygen content of the coating is 1.33%.
实施例4Example 4
采用超音速火焰喷涂技术制备铁基非晶涂层，其中：选取拉瓦尔喷嘴收缩段线型为维托辛斯基曲线，收缩段长度：36mm，拉瓦尔喷嘴发散段长度：190mm，喉口部直径14mm。所用非晶粉末尺寸为20-30μm，喷涂距离为180mm，空气压力为900KPa；丙烷压力为950KPa；氮气压力为760KPa。据此制备的铁基非晶涂层，涂层的孔隙率为1.7％，涂层氧含量为1.59％。Supersonic flame spraying technology is used to prepare iron-based amorphous coatings. Among them: the line shape of the Laval nozzle contraction section is selected as the Witousinski curve, the length of the contraction section: 36mm, the length of the divergence section of the Laval nozzle: 190mm, and the throat part 14mm in diameter. The size of the amorphous powder used is 20-30 μm, the spraying distance is 180mm, the air pressure is 900KPa; the propane pressure is 950KPa; the nitrogen pressure is 760KPa. According to the prepared iron-based amorphous coating, the porosity of the coating is 1.7%, and the oxygen content of the coating is 1.59%.
实施例5Example 5
采用超音速火焰喷涂技术制备铁基非晶涂层，其中：选取拉瓦尔喷嘴收缩段线型为维托辛斯基曲线，收缩段长度：56mm，拉瓦尔喷嘴发散段长度：190mm，喉口部直径14mm。所用非晶粉末尺寸为20-30μm，喷涂距离为180mm，空气压力为900KPa；丙烷压力为950KPa；氮气压力为760KPa。据此制备的铁基非晶涂层，涂层的孔隙率为1.4％，涂层氧含量为1.71％。Supersonic flame spraying technology was used to prepare iron-based amorphous coatings. Among them: the line shape of the contraction section of the Laval nozzle was selected as the Witousinski curve, the length of the contraction section: 56mm, the length of the divergence section of the Laval nozzle: 190mm, and the throat part 14mm in diameter. The size of the amorphous powder used is 20-30 μm, the spraying distance is 180mm, the air pressure is 900KPa; the propane pressure is 950KPa; the nitrogen pressure is 760KPa. According to the prepared iron-based amorphous coating, the porosity of the coating is 1.4%, and the oxygen content of the coating is 1.71%.
对比例1Comparative example 1
与实施例1的不同之处在于：拉瓦尔喷嘴收缩段线型为直线，收缩段长度60mm，拉瓦尔喷嘴发散段长度210mm，喉口部直径17mm。结果：所制备的完全非晶合金涂层孔隙率为3.33％，涂层氧含量为5.31％，高于实施例1。The difference from Example 1 is that the contraction section of the Laval nozzle is straight, the length of the contraction section is 60mm, the length of the divergence section of the Laval nozzle is 210mm, and the diameter of the throat is 17mm. Results: The porosity of the prepared completely amorphous alloy coating is 3.33%, and the oxygen content of the coating is 5.31%, which is higher than that of Example 1.
对比例2Comparative example 2
与实施例1的不同之处在于：拉瓦尔喷嘴收缩段线型为直线，收缩段长度19mm，拉瓦尔喷嘴发散段长度210mm，喉口部直径17mm。结果：所制备的完全非晶合金涂层孔隙率为5.01％，涂层氧含量为4.09％，高于实施例1。The difference from Example 1 is that the contraction section of the Laval nozzle is straight, the length of the contraction section is 19 mm, the length of the divergence section of the Laval nozzle is 210 mm, and the diameter of the throat is 17 mm. Results: The porosity of the prepared completely amorphous alloy coating was 5.01%, and the oxygen content of the coating was 4.09%, which was higher than that of Example 1.
对比例3Comparative example 3
与实施例1的不同之处在于：拉瓦尔喷嘴收缩段线型为直线，收缩段长度60mm，拉瓦尔喷嘴发散段长度110mm，喉口部直径17mm。结果：所制备的完全非晶合金涂层孔隙率为6.13％，涂层氧含量为3.01％，高于实施例1。The difference from Example 1 is that the contraction section of the Laval nozzle is straight, the length of the contraction section is 60 mm, the length of the divergence section of the Laval nozzle is 110 mm, and the diameter of the throat is 17 mm. Results: The porosity of the prepared completely amorphous alloy coating is 6.13%, and the oxygen content of the coating is 3.01%, which is higher than that of Example 1.
对比例4Comparative example 4
与实施例1的不同之处在于：拉瓦尔喷嘴收缩段线型为直线，收缩段长度19mm，拉瓦尔喷嘴发散段长度110mm，喉口部直径17mm。结果：所制备的完全非晶合金涂层孔隙率为6.94％，涂层氧含量为2.47％，高于实施例1。The difference from Example 1 is that the contraction section of the Laval nozzle is straight, the length of the contraction section is 19 mm, the length of the divergence section of the Laval nozzle is 110 mm, and the diameter of the throat is 17 mm. Results: The porosity of the prepared completely amorphous alloy coating was 6.94%, and the oxygen content of the coating was 2.47%, which was higher than that of Example 1.
对比例5Comparative example 5
与实施例1的不同之处在于：拉瓦尔喷嘴收缩段线型为直线，收缩段长度60mm，拉瓦尔喷嘴发散段长度210mm，喉口部直径11mm。结果：所制备的完全非晶合金涂层孔隙率为2.98％，涂层氧含量为6.03％，高于实施例1。The difference from Example 1 is that the contraction section of the Laval nozzle is straight, the length of the contraction section is 60mm, the length of the divergence section of the Laval nozzle is 210mm, and the diameter of the throat is 11mm. Results: The porosity of the prepared completely amorphous alloy coating is 2.98%, and the oxygen content of the coating is 6.03%, which is higher than that of Example 1.
对比例6Comparative example 6
与实施例1的不同之处在于：拉瓦尔喷嘴收缩段线型为直线，收缩段长度19mm，拉瓦尔喷嘴发散段长度210mm，喉口部直径11mm。结果：所制备的完全非晶合金涂层孔隙率为4.49％，涂层氧含量为5.04％，高于实施例1。The difference from Example 1 is that the contraction section of the Laval nozzle is straight, the length of the contraction section is 19 mm, the length of the divergence section of the Laval nozzle is 210 mm, and the diameter of the throat is 11 mm. Results: The porosity of the prepared completely amorphous alloy coating was 4.49%, and the oxygen content of the coating was 5.04%, which was higher than that of Example 1.
对比例7Comparative example 7
与实施例1的不同之处在于：拉瓦尔喷嘴收缩段线型为直线，收缩段长度60mm，拉瓦尔喷嘴发散段长度110mm，喉口部直径11mm。结果：所制备的完全非晶合金涂层孔隙率为5..89％，涂层氧含量为3.49％，高于实施例1。The difference from Example 1 is that the contraction section of the Laval nozzle is straight, the length of the contraction section is 60mm, the length of the divergence section of the Laval nozzle is 110mm, and the diameter of the throat is 11mm. Results: The porosity of the prepared completely amorphous alloy coating is 5..89%, and the oxygen content of the coating is 3.49%, which is higher than that of Example 1.
对比例8Comparative example 8
与实施例1的不同之处在于：拉瓦尔喷嘴收缩段线型为直线，收缩段长度19mm，拉瓦尔喷嘴发散段长度110mm，喉口部直径11mm。结果：所制备的完全非晶合金涂层孔隙率为6.71％，涂层氧含量为3.07％，高于实施例1。The difference from Example 1 is that the contraction section of the Laval nozzle is straight, the length of the contraction section is 19 mm, the length of the divergence section of the Laval nozzle is 110 mm, and the diameter of the throat is 11 mm. Results: The porosity of the prepared completely amorphous alloy coating was 6.71%, and the oxygen content of the coating was 3.07%, which was higher than that of Example 1.
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