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CN106191854A - A kind of preparation method of control pore Ni-based coating - Google Patents

A kind of preparation method of control pore Ni-based coating Download PDF

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CN106191854A
CN106191854A CN201610644126.1A CN201610644126A CN106191854A CN 106191854 A CN106191854 A CN 106191854A CN 201610644126 A CN201610644126 A CN 201610644126A CN 106191854 A CN106191854 A CN 106191854A
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cladding
powder
magnetic field
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CN106191854B (en
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王梁
胡勇
姚建华
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Zhejiang University of Technology ZJUT
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00Coating starting from inorganic powder
    • C23C24/08Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/10Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
    • C23C24/103Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • C23C24/106Coating with metal alloys or metal elements only

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
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  • Laser Beam Processing (AREA)
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Abstract

The present invention relates to the preparation method of a kind of control pore Ni-based coating, comprise the steps: A: polish, clean, scrubbing;B: laser melting coating: use coaxial powder feeding device that nickel base powder is sent into matrix surface, forms laser melting coating molten bath, successively carries out laser melting coating with laser scanning and make cladding molten bath form bubble;C: Lorentz force body force couples: formed in bubble at cladding bath described in step B, being simultaneously introduced adjustable gradient Lorentz force, the bubble forming step B process carries out pore that profile adjustment forms it in cladding layer by surface to the inside depth direction distribution gradient or be evenly distributed.The magnetic field intensity gradient of DC current size and weld pool surface that the inventive method is applied to substrate surface by adjustment affects the downward gradient of Lorentz force.It is not only does this apply to laser fusion covered nickel base coating, welding, laser melting etc. can be suitable for simultaneously and produce the form processing in molten bath, applied widely.

Description

一种可控孔隙镍基涂层的制备方法A kind of preparation method of controllable porosity nickel base coating

技术领域technical field

本发明涉及一种镍基涂层的制备方法,特别涉及一种隙孔隙可调的镍基涂层的制备方法。The invention relates to a preparation method of a nickel-based coating, in particular to a preparation method of a nickel-based coating with adjustable porosity.

背景技术Background technique

激光熔覆技术作为一种新型的制造技术,已越来越多的应用于工业生产中。在熔覆的过程中,由于环境中的水分、载气或者熔覆材料存在C,Ti等元素,熔覆层经常不可避免随机产生气孔。但随着使用条件的日益苛刻,对涂层的性能要求也越来越高。在某些应用场合中,在满足力学性能要求同时,需对熔覆层的抗震性、热传导性提出要求。根据相关文献的研究表明涂层中气孔的数量及分布对上述性能产生重要的影响,因此需对熔覆层中气孔进行调节。但单纯依靠改变激光熔覆工艺参数或者粉末工艺,很难对熔覆层中气孔含量及分布进行定量控制,为解决上述问题本发明提供了一种孔隙可调的镍基涂层制备方法。As a new type of manufacturing technology, laser cladding technology has been more and more used in industrial production. During the cladding process, due to the moisture in the environment, the carrier gas or the presence of C, Ti and other elements in the cladding material, the cladding layer often inevitably generates pores randomly. However, with the increasingly harsh conditions of use, the performance requirements of the coating are also getting higher and higher. In some applications, while meeting the requirements of mechanical properties, it is necessary to set requirements for the shock resistance and thermal conductivity of the cladding layer. According to the relevant literature, the number and distribution of pores in the coating have an important impact on the above properties, so the pores in the cladding layer need to be adjusted. However, it is difficult to quantitatively control the content and distribution of pores in the cladding layer simply by changing the parameters of the laser cladding process or the powder process. To solve the above problems, the present invention provides a method for preparing a nickel-based coating with adjustable pores.

关于外加磁场对激光焊接和熔覆过程的调控技术,国内外学者已经开展了一系列的研究。如德国的Bachmann等通过静态磁场改善了铝合金焊接熔池形貌,不莱梅实验室的Gatzen M等研究发现交变磁场对元素分布产生影响,但上述学者所采用的洛仑兹力均为自身感应洛仑兹力,而非外加洛仑兹力且未对气孔进行研究。国内也有众多学者对其展开研究,如公开的文件(CN102899661)提出了一种采用磁场辅助激光熔覆的方法,该方法特点是仅采用单纯磁场作用激光熔覆熔池得到晶粒取向一致,细腻均匀的涂层。公开的文件(CN102703897)提出了一种旋转磁场辅助激光熔覆制备Fe60复合涂层的方法,因该方法采用了旋转磁场,这也使得内部洛伦兹力是呈周期性变化,其作用结果往往使得熔覆层组织、元素、颗粒等分布更加均匀,不能调控气孔、颗粒等的定向运动,且未涉及熔覆工艺与磁场的组合调控;公开的文件(CN104195541),提出一种电磁复合场辅助激光熔覆的方法及装置,文件中所提供方法主要采用电磁复合场调控对象为组织、颗粒、元素、表面形貌,未涉及激光熔覆气泡的生成工艺以及对气泡运动调控,国内外针对外场的发明或者研究大多其中于材料的组织、性能、熔池运动,而往往将气孔作为缺陷避免其产生。Scholars at home and abroad have carried out a series of research on the control technology of laser welding and cladding process by external magnetic field. For example, Bachmann in Germany improved the morphology of aluminum alloy welding pool through static magnetic field, and Gatzen M in Bremen laboratory found that alternating magnetic field affects the distribution of elements, but the Lorentz force used by the above-mentioned scholars is The Lorentz force is induced by itself, not the external Lorentz force and the stomata are not studied. Many domestic scholars have also conducted research on it. For example, the public document (CN102899661) proposed a method of magnetic field-assisted laser cladding. Uniform coating. The published document (CN102703897) proposes a method for preparing Fe60 composite coatings by rotating magnetic field-assisted laser cladding, because the method uses a rotating magnetic field, which also makes the internal Lorentz force change periodically, and the result is often It makes the distribution of cladding layer structure, elements, particles, etc. more uniform, and cannot control the directional movement of pores, particles, etc., and does not involve the combined regulation of cladding process and magnetic field; the open document (CN104195541) proposes an electromagnetic composite field assisted The method and device of laser cladding, the method provided in the document mainly adopts the electromagnetic compound field to control the objects such as tissue, particles, elements, and surface morphology, and does not involve the generation process of laser cladding bubbles and the control of bubble movement. Most of the inventions or researches are based on the structure, performance and molten pool movement of materials, and pores are often regarded as defects to avoid their generation.

发明内容Contents of the invention

本发明要克服现有激光熔覆技术不能对气孔分布调控的缺陷,提供一种可控孔隙镍基涂层的制备方法。The invention overcomes the defect that the existing laser cladding technology cannot control the distribution of pores, and provides a method for preparing a nickel-based coating with controllable pores.

本发明所述的一种可控孔隙镍基涂层的制备方法,包括如下步骤:The preparation method of a kind of controllable pore nickel-based coating of the present invention comprises the following steps:

A:抛光、清洗、除污:对基材表面进行打磨处理,直至表面光亮达到表面粗糙度小于Ra1.6,再使用丙酮或者酒精进行擦拭清洗将表面油污去除,并在通风处晾干;A: Polishing, cleaning, and decontamination: Polish the surface of the substrate until the surface is bright and the surface roughness is less than Ra1.6, then wipe and clean with acetone or alcohol to remove the surface oil, and dry in a ventilated place;

B:激光熔覆:使用同轴送粉器将镍基粉末送入基材表面,形成激光熔覆熔池,逐层用激光扫描进行激光熔覆使熔覆熔池形成气泡,按以下参数调整镍基粉末Ti、C含量、粉末粒径、粉末球形度、保护气中的水分含量并结合激光工艺参数控制熔覆层气孔数量;B: Laser cladding: Use a coaxial powder feeder to send nickel-based powder into the surface of the substrate to form a laser cladding molten pool, and use laser scanning to perform laser cladding layer by layer to form bubbles in the cladding molten pool. Adjust according to the following parameters Nickel-based powder Ti, C content, powder particle size, powder sphericity, moisture content in the shielding gas and combined with laser process parameters to control the number of pores in the cladding layer;

所述的镍基粉末质量分数为:Ni 50.0~55.0%,Cr 12.0~17.10%,C 0.08~0.2%,Si 0~0.35%,Mn0~0.35%,S 0~0.018%,P0~0.015%,Al 0.30~0.70%,Ti1.10~2%,Mo 2.8~3.30%,Nb 4.75~5.50%,余量为Fe;The mass fraction of the nickel-based powder is: Ni 50.0-55.0%, Cr 12.0-17.10%, C 0.08-0.2%, Si 0-0.35%, Mn0-0.35%, S 0-0.018%, P0-0.015%, Al 0.30~0.70%, Ti1.10~2%, Mo 2.8~3.30%, Nb 4.75~5.50%, the balance is Fe;

所述粉末粒径d=50~150μm;The particle size of the powder d=50-150 μm;

所述粉末球形度为0.6~0.9;The powder sphericity is 0.6~0.9;

所述保护气中水分含量质量分数为0.05~2%;The moisture content mass fraction in the protective gas is 0.05-2%;

所述激光工艺参数控制在激光功率为800~1800W;扫描速度为6~15mm/s;保护气流量为10~80HF/min;送粉量8~20g/min;The laser process parameters are controlled at a laser power of 800-1800W; a scanning speed of 6-15mm/s; a shielding gas flow rate of 10-80HF/min; a powder feeding volume of 8-20g/min;

通常在上述条件下,所述熔覆层产生的气孔形状为球形,直径范围为5μm~100μm,所述熔覆层气孔的总体积为熔覆层总体积的0.1~5%;Usually under the above conditions, the shape of the pores in the cladding layer is spherical, the diameter ranges from 5 μm to 100 μm, and the total volume of the pores in the cladding layer is 0.1 to 5% of the total volume of the cladding layer;

C:洛伦兹力体积力耦合:在B步骤让所述熔覆熔池内部形成气泡基础上(也就是通常所说的“起泡”),同时引入可调梯度洛伦兹力,对步骤B过程形成的气泡进行分布调节使气泡形成的气孔在熔覆层中由表面至里面深度方向呈梯度分布或呈均匀分布,这里起初在液态流体中的气泡,在激光扫描过程中气泡被凝固前沿捕获,保留在熔覆层中形成气孔;所述的洛伦兹力调节方法为:在基体通入平行于基材表面的直流电流,直至扫描结束,电流密度大小为0~106A/m2,同时,将基体置于梯度稳态磁场中,直至扫描结束,使得熔池表面的磁场强度为0~2T,磁场强度随着熔池的深度增加而均匀降低,磁场强度下降的梯度为0.01~0.06T/mm。通常所述的保护气为惰性气体,如氩气。C: Coupling of Lorentz force and body force: In step B, on the basis of forming bubbles inside the cladding pool (also known as "bubbling"), an adjustable gradient Lorentz force is introduced at the same time, for the step The distribution of the bubbles formed in the B process is adjusted so that the pores formed by the bubbles are distributed in a gradient or evenly distributed in the depth direction from the surface to the inside in the cladding layer. Here, the bubbles in the liquid fluid are initially solidified during the laser scanning process. Trapped and retained in the cladding layer to form pores; the Lorentz force adjustment method is as follows: a direct current parallel to the surface of the substrate is passed through the substrate until the end of the scan, and the current density is 0-10 6 A/m 2. At the same time, place the substrate in the gradient steady-state magnetic field until the end of scanning, so that the magnetic field strength on the surface of the molten pool is 0-2T, and the magnetic field strength decreases uniformly with the increase of the depth of the molten pool, and the gradient of the magnetic field strength decline is 0.01 ~0.06T/mm. Usually the protective gas is an inert gas, such as argon.

进一步,所述基体在激光熔覆以前与可提供直流电流的外接电源连接以待连通。Further, the substrate is connected to an external power supply that can provide direct current before laser cladding to be connected.

通常所述直流电流为稳态直流电流,由低压大额定电流蓄电池提供,即外接电源为低压大额定电流蓄电池,所述低压大额定电流蓄电池的电压为2~6V,放电能力:300~600Ah。Usually, the DC current is a steady state DC current provided by a low-voltage high-rated current battery, that is, the external power supply is a low-voltage high-rated current battery, the voltage of the low-voltage high-rated current battery is 2-6V, and the discharge capacity is 300-600Ah.

本发明优选所述镍基粉末质量分数为:Ni 52.5%,Cr 15%,C 0.1%,Si 0.3%,Mn 0.3%,S 0.01%,P 0.01%,Al 0.4%,Ti 1.5%,Mo 3%,Nb 5%,Fe 21.88%。In the present invention, the mass fraction of the nickel-based powder is preferably: Ni 52.5%, Cr 15%, C 0.1%, Si 0.3%, Mn 0.3%, S 0.01%, P 0.01%, Al 0.4%, Ti 1.5%, Mo 3 %, Nb 5%, Fe 21.88%.

再进一步,所述磁场由电磁铁提供,磁场方向与熔覆熔池表面平行,同时垂直于所述激光扫描方向,磁场梯度调节通过改变双侧接触矩形磁极长度和\或宽度来实现,所述的所述矩形磁极的宽度为10mm~40mm,所述的长度为80~120mm。Still further, the magnetic field is provided by an electromagnet, and the direction of the magnetic field is parallel to the surface of the cladding pool and perpendicular to the scanning direction of the laser. The adjustment of the magnetic field gradient is realized by changing the length and/or width of the rectangular magnetic poles in contact with both sides. The width of the rectangular magnetic poles is 10mm-40mm, and the length is 80-120mm.

更进一步,所述洛仑兹力的方向通过改变通入电流方向或者磁场方向进行调节。Furthermore, the direction of the Lorentz force is adjusted by changing the direction of the current or the direction of the magnetic field.

为具体地,所述的可控孔隙镍基涂层的制备方法,推存所述的激光功率为1600W,扫描速度为10mm/s,送粉量为10g/min,保护气流量20HF/min,熔覆层形成球形气孔,按以上操作,所产生的熔覆层球形气孔直径范围为5μm~100μm,产生气孔总体积占熔覆层体积的0.1~0.2%,且气孔无规则分布,并且熔覆层形貌良好,无裂纹。本方案在步骤B工艺及粉末条件下,所述的熔覆层是指通过激光熔化覆盖在基体表面的材料并与之形成冶金结合的涂层。Specifically, for the preparation method of the controllable pore nickel-based coating, the recommended laser power is 1600W, the scanning speed is 10mm/s, the powder feeding rate is 10g/min, and the shielding gas flow rate is 20HF/min. The cladding layer forms spherical pores. According to the above operation, the diameter range of the spherical pores of the cladding layer is 5 μm to 100 μm, and the total volume of the generated pores accounts for 0.1 to 0.2% of the volume of the cladding layer, and the pores are distributed randomly. The layer morphology is good without cracks. In this solution, under the process of step B and powder conditions, the cladding layer refers to a coating layer that is melted by laser to cover the material on the surface of the substrate and forms a metallurgical bond with it.

区别于其他激光涂层制备方法,本方法所针对的调控对象为气孔,主要粉末及保护气优选内容还包括:通过调整镍基粉末Ti,C含量分别为1.5%与0.1%,控制保护气中的水分含量为2%,为起泡提供原料以产生CO,CO2等气体,控制镍基粉末粒径(50~75μm)及球形度(0.8~0.9),提高粉末与保护气中水分的结合能力,对熔覆层进行“起泡”,并在气泡形核,长大过程中施加洛伦兹力,以加速或者抑制气泡运动,从而对熔覆层中气泡数量及分布进行调节。Different from other laser coating preparation methods, this method targets pores, and the main powder and shielding gas optimization content also includes: by adjusting the Ti and C contents of the nickel-based powder to 1.5% and 0.1%, respectively, to control the The moisture content is 2%, providing raw materials for foaming to generate CO, CO 2 and other gases, controlling the particle size (50-75μm) and sphericity (0.8-0.9) of nickel-based powder, and improving the combination of powder and moisture in the protective gas The ability to "bubble" the cladding layer, and apply Lorentz force during the nucleation and growth of the bubbles to accelerate or suppress the movement of the bubbles, thereby adjusting the number and distribution of the bubbles in the cladding layer.

通常,本发明通过步骤C调节磁场强度使其为1~2T,电流密度为105~106A/m2,同时使得洛仑兹力方向与熔覆熔池表面垂直向内,这会使得气泡溢出数量增加,得到熔覆层中残留气孔体积百分比0~0.1%且分布于熔覆层上部;这样可以得到的无气孔或气孔含量极少的镍基涂层。Usually, the present invention adjusts the magnetic field intensity to 1-2T through step C, and the current density is 10 5 -10 6 A/m 2 , and at the same time makes the direction of the Lorentz force perpendicular to the surface of the cladding pool, which will make The number of bubbles overflowing increases, so that the volume percentage of residual pores in the cladding layer is 0-0.1% and distributed on the upper part of the cladding layer; in this way, a nickel-based coating with no pores or very little pores can be obtained.

如果我们在步骤C调节磁场强度使其为1~2T,电流密度为105~106A/m2,同时使得洛伦兹力方向与熔覆熔池表面垂直向外,会使得气泡溢出数量减少,熔覆层中残留气孔体积百分比5~20%,且分布于熔覆层底部。这样可以得到的镍基涂层残留气孔较多,并且大多分布在涂层的较底层。If we adjust the magnetic field strength in step C to 1-2T, the current density is 10 5 ~10 6 A/m 2 , and at the same time make the direction of the Lorentz force perpendicular to the surface of the cladding pool, the number of bubbles will overflow The volume percentage of residual pores in the cladding layer is 5-20%, and they are distributed at the bottom of the cladding layer. The nickel-based coating that can be obtained in this way has more residual pores, and most of them are distributed in the lower layer of the coating.

如果,我们调节磁场强度为0.1~0.5T,电流密度大小为0~105A/m2,同时使得洛伦兹力方向垂直熔覆熔池表面向内,这会使得气泡形核的能量降低,所述熔覆熔池中气泡增多,此时洛仑兹力较小,流体的拖曳力占主导,气泡受到流体搅拌作用而使得熔覆层气孔变得均匀。If we adjust the magnetic field strength to 0.1-0.5T, the current density to 0-10 5 A/m 2 , and at the same time make the direction of the Lorentz force perpendicular to the surface of the cladding pool inward, this will reduce the energy of bubble nucleation , the number of bubbles in the cladding pool increases. At this time, the Lorentz force is small, and the drag force of the fluid dominates. The bubbles are stirred by the fluid to make the pores of the cladding layer uniform.

具体的,所述的可控孔隙镍基涂层的制备方法为:所述的洛伦兹力是在熔覆熔池区域由磁场与电场相互耦合产生,方向与熔覆熔池表面垂直向内或垂直向外,通过调节电流密度值0~106A/m2与磁场值0~2T,使得洛仑兹力值大小范围为0~2×106N/m3,调节磁场梯度0.01~0.06T/mm,使得洛仑兹力从表面至里面深度方向并呈负梯度分布,洛仑兹力下降的梯度为102~105N/mm。Specifically, the preparation method of the controllable pore nickel-based coating is as follows: the Lorentz force is generated by the mutual coupling of the magnetic field and the electric field in the cladding pool area, and the direction is perpendicular to the surface of the cladding pool and inward. Or vertically outward, by adjusting the current density value of 0-10 6 A/m 2 and the magnetic field value of 0-2T, the Lorentz force value ranges from 0 to 2×10 6 N/m 3 , and the magnetic field gradient is adjusted from 0.01 to 0.06T/mm, so that the Lorentz force is distributed in a negative gradient from the surface to the depth direction, and the gradient of the Lorentz force decrease is 10 2 -10 5 N/mm.

本发明方法具有以下优点:The inventive method has the following advantages:

1、本发明将镍基粉末材料含量(C和/或Ti含量)、粉末特性及保护气含水量与洛仑兹力相调节结合,将定向洛伦兹力间接作用于气泡,以物理形式调节气孔分布,尽可能的保留了原有涂层的力学性能及组织特点,可得到不同孔隙的涂层。1. The present invention adjusts the nickel-based powder material content (C and/or Ti content), powder characteristics and protective gas water content with the Lorentz force, and the directional Lorentz force acts indirectly on the air bubbles to adjust in physical form Pore distribution, the mechanical properties and organizational characteristics of the original coating are retained as much as possible, and coatings with different pores can be obtained.

2、本发明采用梯度洛伦兹力体积力,既可增加对熔池表面这一气泡溢出关键界面区域的控制能力,以显著提高控制效果,又可减少洛伦兹力对熔池底部气泡析出过程的影响。2. The present invention adopts the gradient Lorentz force body force, which can not only increase the control ability of the key interface area of the bubble overflow on the surface of the molten pool, so as to significantly improve the control effect, but also reduce the Lorentz force on the bubble precipitation at the bottom of the molten pool process impact.

3、本发明可以通过调整施加在基材表面的直流电流大小及熔池表面的磁场强度来影响洛仑兹力的下降梯度,从而调整镍基涂层内的孔隙,以适应不同的加工要求。这不仅适用于激光熔覆镍基涂层,可同时适用焊接、激光熔凝等产生熔池的加工形式,适用范围广。3. The present invention can affect the descending gradient of the Lorentz force by adjusting the magnitude of the direct current applied to the surface of the substrate and the strength of the magnetic field on the surface of the molten pool, thereby adjusting the pores in the nickel-based coating to meet different processing requirements. This is not only applicable to laser cladding nickel-based coatings, but also applicable to welding, laser melting and other processing forms that generate molten pools, and has a wide range of applications.

附图说明Description of drawings

图1一种可控孔隙镍基涂层的制备装置工作状态结构图Fig. 1 The working state structure diagram of the preparation device of a kind of controllable pore nickel-based coating

图2实施例1条件下熔覆层纵截面气孔分布图Fig. 2 Pore distribution in the longitudinal section of the cladding layer under the conditions of Example 1

图3实施例2条件下熔覆层纵截面气孔分布图Fig. 3 distribution diagram of pores in longitudinal section of cladding layer under the conditions of Example 2

图4实施例3条件下熔覆层纵截面气孔分布图Fig. 4 The distribution diagram of pores in the longitudinal section of the cladding layer under the conditions of Example 3

图5实施例4条件下熔覆层纵截面气孔分布图Fig. 5 distribution of pores in longitudinal section of the cladding layer under the conditions of Example 4

图6实施例5洛伦兹力向上条件下(磁场梯度0.01T/mm)熔覆层纵截面气孔分布图Fig. 6 The pore distribution diagram of the longitudinal section of the cladding layer under the condition of upward Lorentz force in Example 5 (magnetic field gradient 0.01T/mm)

图7实施例6洛伦兹力向下条件下(磁场梯度0.06T/mm)熔覆层纵截面气孔分布图Fig. 7 Distribution of air holes in the longitudinal section of the cladding layer under the condition of downward Lorentz force in Example 6 (magnetic field gradient 0.06T/mm)

图8实施例7洛伦兹力向上条件下熔覆层纵截面气孔分布图Fig. 8 The pore distribution diagram of the longitudinal section of the cladding layer under the condition of upward Lorentz force in Example 7

图9实施例8洛仑兹力条件熔覆层纵截面气孔均匀分布图Figure 9 Example 8 Lorentz force condition cladding layer longitudinal section uniform distribution of pores

具体实施方式detailed description

下面结合附图,对本发明作进一步阐述,但本发明的保护范围不限于所述内容。The present invention will be further elaborated below in conjunction with the accompanying drawings, but the protection scope of the present invention is not limited to the content described.

本案的实施例匀由以下装置实现,如附图1所示,所述的装置包括:1-激光器、2-激光传输通道、3-送粉头、4-工件夹持器、5-导线、6-低压大额定电流电源、7—线圈绕组、8—矩形磁极头、9—基体、10—线圈绕组电源。The embodiment of this case is realized by the following devices, as shown in Figure 1, the device includes: 1-laser, 2-laser transmission channel, 3-powder feeding head, 4-workpiece holder, 5-wire, 6—low voltage and high rated current power supply, 7—coil winding, 8—rectangular magnetic pole head, 9—substrate, 10—coil winding power supply.

具体连接方式:激光器1与激光传输通道2可通过柔性光纤或飞行光路连接,送粉头3与激光传输通道2同轴组合,送粉头3位于基体9正上方,低压大额定电流电源6通过导线5及工件夹持器4与基体9相连接,矩形磁极头8位于基体两侧与线圈绕组7组合,线圈绕组与线圈绕组电源10连接。Specific connection method: the laser 1 and the laser transmission channel 2 can be connected through a flexible optical fiber or a flying optical path, the powder feeding head 3 is coaxially combined with the laser transmission channel 2, the powder feeding head 3 is located directly above the substrate 9, and the low-voltage high-rated current power supply 6 passes through The wire 5 and the workpiece holder 4 are connected to the base body 9 , the rectangular magnetic pole head 8 is located on both sides of the base body and combined with the coil winding 7 , and the coil winding is connected to the coil winding power supply 10 .

具体实施方式:首先将基体与工件夹持器相连,使基体处于水平位置,选取合适的矩形磁极头(根据不同磁场梯度选取形状尺寸),调节双磁头相对位置直至各极头与基体侧面距离约0.5mm。打开直流电源开关,调节电流,在基体中通入所需电流值,打开线圈绕组电源并调节电流值,使极头产生所需磁场值。准备完毕后,开始激光熔覆,送粉头按所设定的轨迹在基材表面熔覆,通电、通磁直至熔覆结束,将所加工的基体取出。Specific implementation method: at first base body is connected with workpiece holder, makes base body be in horizontal position, selects suitable rectangular magnetic pole head (choose shape size according to different magnetic field gradients), adjusts the relative position of double magnetic head until each pole head and base body side distance about 0.5mm. Turn on the DC power switch, adjust the current, pass the required current value into the matrix, turn on the coil winding power supply and adjust the current value, so that the pole head can generate the required magnetic field value. After the preparation is completed, laser cladding starts, and the powder feeding head cladding on the surface of the substrate according to the set trajectory, energizes and magnetizes until the cladding is completed, and the processed substrate is taken out.

实施例1Example 1

激光熔覆基材为316奥氏体不锈钢,机械加工成100×10×10mm的金属试样,表面经除油、除锈、打磨处理后,粗糙度小于Ra1.6,再用丙酮清洗将表面油污去除。熔覆粉末为镍基合金粉末,将所述粉末放于干燥箱内,设置温度100℃,干燥时间为60min。待粉末冷却后,将其放入送粉器中,将待熔覆的试样水平放置于工作台上,开启激光发生器(功率为1600W)、气体保护装置(保护气为氩气,流量为20HF/min,水分含量0.05%)和送粉器(送粉量为10g/min),10mm/s的扫描速度按照预设熔覆轨迹进行熔覆。粉末粒径为50~75μm,球形度0.8~0.9,其中所述镍基粉末质量分数为为:Ni 52.5%,Cr 15%,C 0.1%,Si 0.3%,Mn0.3%,S 0.01%,P 0.01%,Al 0.4%,Ti 1.5%,Mo 3%,Nb 5%,Fe 21.88%。图2为上述工艺条件下熔覆层气孔分布图,直径范围为60μm~100μm,所述熔覆层气孔的总体积为熔覆层总体积的约为0.2%。The base material of laser cladding is 316 austenitic stainless steel, which is machined into a metal sample of 100×10×10mm. Grease removal. The cladding powder is nickel-based alloy powder, and the powder is placed in a drying oven with a set temperature of 100° C. and a drying time of 60 minutes. After the powder is cooled, put it into the powder feeder, place the sample to be clad horizontally on the workbench, turn on the laser generator (the power is 1600W), the gas protection device (the protection gas is argon, the flow rate is 20HF/min, moisture content 0.05%) and powder feeder (powder feeding amount 10g/min), 10mm/s scan speed to carry out cladding according to the preset cladding trajectory. The particle size of the powder is 50-75 μm, and the sphericity is 0.8-0.9, wherein the mass fraction of the nickel-based powder is: Ni 52.5%, Cr 15%, C 0.1%, Si 0.3%, Mn0.3%, S 0.01%, P 0.01%, Al 0.4%, Ti 1.5%, Mo 3%, Nb 5%, Fe 21.88%. Fig. 2 is a distribution diagram of pores in the cladding layer under the above process conditions, the diameter ranges from 60 μm to 100 μm, and the total volume of the pores in the cladding layer is about 0.2% of the total volume of the cladding layer.

实施例1的熔覆层纵截面气孔分布图见附图2。The pore distribution diagram of the longitudinal section of the cladding layer in Example 1 is shown in Figure 2.

实施例2Example 2

该例为对比例,将实施例1中保护气中含水量降低为0.04%,粉末化学成分(质量分数,%)与实施例1中一致:Ni 52.5%,Cr 15%,C 0.1%,Si 0.3%,Mn 0.3%,S 0.01%,P 0.01%,Al 0.4%,Ti 1.5%,Mo 3%,Nb 5%,Fe 21.88%。保证其他工艺参数与实施例1一致,得到熔覆层纵截面气孔分布图(图3所示),其中熔覆层气孔形状为球形,直径范围为5~10μm,所述熔覆层气孔的总体积为熔覆层总体积的约为0.05%;对比图2可以发现熔覆层气孔数量与气孔直径明显减小,说明保护气中水分含量降低,使得熔覆层中氧含量减少,气孔含量明显减少。This example is a comparative example, and the water content in the shielding gas in Example 1 is reduced to 0.04%, and the powder chemical composition (mass fraction, %) is consistent with Example 1: Ni 52.5%, Cr 15%, C 0.1%, Si 0.3%, Mn 0.3%, S 0.01%, P 0.01%, Al 0.4%, Ti 1.5%, Mo 3%, Nb 5%, Fe 21.88%. Ensure that other process parameters are consistent with Example 1, obtain the cladding layer vertical section pore distribution diagram (shown in Figure 3), wherein the cladding layer pore shape is spherical, the diameter range is 5 ~ 10 μm, the total number of cladding layer pores The volume is about 0.05% of the total volume of the cladding layer; comparing Figure 2, it can be found that the number of pores and the diameter of the pores in the cladding layer are significantly reduced, indicating that the moisture content in the shielding gas is reduced, which reduces the oxygen content in the cladding layer and the pore content is obvious. reduce.

实施例3Example 3

该例为对比例,仅按实施例1中条件,将镍基粉末粒径增加到150μm至180μm时,球形度0.8~0.9,保持激光工艺及粉末化学成分实施例1一致,得到了熔覆层纵截面气孔分布图(图4所示)。从图中可以得到当粒径增加到大于150μm,熔覆层表面有微气孔,熔覆层气孔的总体积为熔覆层总体积的约为0.05%,说明粒径的增大使得颗粒表面的载气能力降低,从而导致气孔含量降低。This example is a comparative example. Only according to the conditions in Example 1, when the particle size of the nickel-based powder is increased to 150 μm to 180 μm, the sphericity is 0.8 to 0.9, and the laser process and powder chemical composition are kept consistent with Example 1, and the cladding layer is obtained. Pore distribution diagram in longitudinal section (shown in Figure 4). It can be seen from the figure that when the particle size increases to more than 150 μm, there are micropores on the surface of the cladding layer, and the total volume of the pores in the cladding layer is about 0.05% of the total volume of the cladding layer, indicating that the increase in particle size makes the particle surface The gas-carrying capacity is reduced, resulting in a lower porosity.

实施例4Example 4

参照图5。该例为对比例,按实施例1中条件,将镍基粉末颗粒球形度增加到约0.98,并保持粉末化学成分、粒径与实施例1一致,即粉末粒径为50~75μm,球形度0.8~0.9,其中熔覆粉末化学成分(质量分数,%)为:Ni 52.5%,Cr 15%,C 0.1%,Si 0.3%,Mn0.3%,S 0.01%,P 0.01%,Al 0.4%,Ti 1.5%,Mo 3%,Nb 5%,Fe 21.88%。将粉末放于干燥箱内,设置温度100℃,干燥时间为60min。保证其他工艺参数与实施例1一致,得到了熔覆层纵截面气孔分布图(图5所示)。从图中可以得到当球形度增加,尽管存在微气孔,但气孔数量较实施例1明显减少,其原因是粉末球形度增加,载气结合能力降低,从而导致外界气体进入熔池的含量发生变化,使得气孔尺寸及数量减小。综合实施例3、4可得,粒径超出150μm以及球形度大于0.9时,不利于熔覆层“起泡”。Refer to Figure 5. This example is a comparative example. According to the conditions in Example 1, the sphericity of the nickel-based powder particles is increased to about 0.98, and the chemical composition and particle size of the powder are kept consistent with Example 1, that is, the powder particle size is 50-75 μm, and the sphericity 0.8~0.9, wherein the cladding powder chemical composition (mass fraction, %) is: Ni 52.5%, Cr 15%, C 0.1%, Si 0.3%, Mn0.3%, S 0.01%, P 0.01%, Al 0.4% , Ti 1.5%, Mo 3%, Nb 5%, Fe 21.88%. Put the powder in a drying oven, set the temperature at 100°C, and dry for 60 minutes. Ensure that other process parameters are consistent with those in Example 1, and obtain the pore distribution diagram of the longitudinal section of the cladding layer (as shown in FIG. 5 ). It can be seen from the figure that when the sphericity increases, although there are micropores, the number of pores is significantly reduced compared with Example 1. The reason is that the powder sphericity increases and the binding ability of the carrier gas decreases, which leads to changes in the content of external gas entering the molten pool. , so that the size and number of pores are reduced. Combining Examples 3 and 4, it can be obtained that when the particle size exceeds 150 μm and the sphericity is greater than 0.9, it is not conducive to "bubbling" of the cladding layer.

实施例5Example 5

参照图6。通过对比实施例1与实施例2,实施例1与实施例3,实施例1与实施例4可知,调整保护气含水量与粉末成分,粉末球形度以及粉末粒径将对气孔数量与大小产生影响,但是仅依靠工艺,往往很难对其分布进行控制,因此本发明在实施例1成功气泡基础上同时外加洛仑兹力体积力来改变气泡的等效浮力,以达到定量调控分布的目的。本实施例中激光熔覆基材为316奥氏体不锈钢,机械加工成100×10×10mm的金属试样,表面经除油、除锈、打磨处理后,再用丙酮清洗。所述基体在激光熔覆以前与可提供直流电流的外接电源连接以待连通,所述直流电流为稳态直流电流,外接电源为低压大额定电流蓄电池(电池规格为:6V,600Ah)。Refer to Figure 6. By comparing Example 1 and Example 2, Example 1 and Example 3, and Example 1 and Example 4, it can be seen that adjusting the water content of the shielding gas and powder composition, powder sphericity and powder particle size will have a significant impact on the number and size of pores. influence, but only relying on the process, it is often difficult to control its distribution. Therefore, on the basis of the successful bubbles in Example 1, the present invention simultaneously adds Lorentz force and body force to change the equivalent buoyancy of the bubbles, so as to achieve the purpose of quantitatively regulating the distribution. . In this embodiment, the laser cladding base material is 316 austenitic stainless steel, which is machined into a metal sample of 100×10×10 mm, and the surface is cleaned with acetone after degreasing, derusting and grinding. Before laser cladding, the substrate is connected to an external power supply that can provide direct current. The direct current is a steady-state direct current, and the external power supply is a low-voltage high-rated current battery (battery specification: 6V, 600Ah).

将镍基合金粉末放于干燥箱内,设置温度100℃,干燥时间60min。待粉末冷却后,将其放入送粉器中,合金粉末化学成分(质量分数,%)为:Ni 52.5%,Cr 15%,C 0.1%,Si0.3%,Mn 0.3%,S 0.01%,P 0.01%,Al 0.4%,Ti 1.5%,Mo 3%,Nb 5%,Fe 21.88%。粉末粒径为50~75μm,球形度0.8~0.9。开启激光发生器(功率为1400W)、气体保护装置(氩气流量为10L/h,水分含量2%)和送粉器(送粉量为10g/min),用7mm/s的扫描速度按照预设熔覆轨迹进行熔覆。同时,在基体中通入106A/m2的电流密度,基体两侧磁场强度为2T,磁场强度下降的梯度为0.01T/mm,在熔覆熔池区域形成垂直熔覆熔池表面向外的梯度洛伦兹力,其下降梯度值从熔池表面至底部105N/m4。由于洛仑兹力的影响,气泡受到额外向下的力,抑制气泡向上排出,最终大部分气孔集中分布在熔覆涂层的底部,如图6所示,图中气孔孔径范围为10~120μm,所述熔覆层气孔的总体积为熔覆层总体积的约为8%。Put the nickel-based alloy powder in a drying oven, set the temperature at 100°C, and dry for 60 minutes. After the powder is cooled, put it into the powder feeder. The chemical composition (mass fraction, %) of the alloy powder is: Ni 52.5%, Cr 15%, C 0.1%, Si0.3%, Mn 0.3%, S 0.01% , P 0.01%, Al 0.4%, Ti 1.5%, Mo 3%, Nb 5%, Fe 21.88%. The particle size of the powder is 50-75 μm, and the sphericity is 0.8-0.9. Turn on the laser generator (power is 1400W), gas protection device (argon gas flow rate is 10L/h, moisture content is 2%) and powder feeder (powder feed rate is 10g/min), and the scan speed is 7mm/s according to the preset Set the cladding trajectory for cladding. At the same time, a current density of 10 6 A/m 2 is passed into the substrate, the magnetic field strength on both sides of the substrate is 2T, and the gradient of the magnetic field strength drop is 0.01T/mm, and a vertical cladding molten pool surface is formed in the cladding molten pool area. The external gradient Lorentz force has a descending gradient value of 10 5 N/m 4 from the molten pool surface to the bottom. Due to the influence of the Lorentz force, the bubbles are subjected to an additional downward force, which inhibits the upward discharge of the bubbles, and finally most of the pores are concentrated and distributed at the bottom of the cladding coating, as shown in Figure 6. The pore size range in the figure is 10-120 μm , the total volume of pores in the cladding layer is about 8% of the total volume of the cladding layer.

实施例6Example 6

参照图7熔覆层纵截面气孔分布图。该例仅将实施例5中磁场强度下降的梯度为0.06T/mm,其他激光工艺参数、粉末参数、保护气、电流大小以及磁场大小与实施例5保持一致,得到如图7所示的气孔分布图。从图中可以气孔孔径范围为10~120μm,较图6气孔数量有所减少,总体积占熔覆层总体积的约为6%。Refer to Figure 7 for the distribution diagram of pores in the longitudinal section of the cladding layer. In this example, only the gradient of the magnetic field intensity drop in Example 5 is 0.06T/mm, and other laser process parameters, powder parameters, shielding gas, current and magnetic field are kept consistent with Example 5, and the pores shown in Figure 7 are obtained. Distribution. It can be seen from the figure that the pore diameter ranges from 10 to 120 μm, and the number of pores is reduced compared with that in Figure 6, and the total volume accounts for about 6% of the total volume of the cladding layer.

实施例7Example 7

参照图8。该例仅将实施例5中的洛伦兹力方向变为垂直熔池表面向内,其他激光工艺参数、粉末参数、保护气、电流大小以及磁场大小与实施例5保持一致,得到如图8所示的气孔分布图。从图中可以发现气孔数量较图2、6和7明显减少,得到致密的熔覆层,总体积占熔覆层总体积的约为0。Refer to Figure 8. In this example, only the direction of the Lorentz force in Example 5 is changed to be vertical to the surface of the molten pool inward, and other laser process parameters, powder parameters, shielding gas, current and magnetic field are consistent with Example 5, as shown in Figure 8 The pore distribution diagram shown. It can be seen from the figure that the number of pores is significantly reduced compared with Figures 2, 6 and 7, and a dense cladding layer is obtained, and the total volume accounts for about 0% of the total volume of the cladding layer.

实施例8Example 8

参照图9。本实施例在实施例5基础上,在基体中施加电流密度大小为105A/m2,磁场强度0.4T,磁场强度下降的梯度为0.01T/mm形成洛仑兹力的方向垂直熔池液面向里,其下降梯度值从熔池表面至底部为400N/mm4。激光熔覆基材为316奥氏体不锈钢,机械加工成100×10×10mm的金属试样,表面经除油、除锈、打磨处理至Ra1.6,再用乙醇清洗。将镍基合金粉末放于干燥箱内,设置温度100℃,干燥时间60min。待粉末冷却后,将其放入送粉器中,合金粉末化学成分(质量分数,%)为:Ni 52.5%,Cr 15%,C 0.1%,Si 0.3%,Mn 0.3%,S0.01%,P 0.01%,Al 0.4%,Ti 1.5%,Mo 3%,Nb 5%,Fe 21.88%,与实施例1保持一致。开启激光发生器(功率为1400W)、气体保护装置(氩气流量为10L/h,水分含量2%)和送粉器(送粉量为10g/min),用10mm/s的扫描速度按照预设熔覆轨迹进行熔覆,得到如图9所示的气孔均匀分布图,气孔直径10~100μm,气孔总体积占熔覆层总体积约6%。Refer to Figure 9. In this example, on the basis of Example 5, a current density of 10 5 A/m 2 is applied to the substrate, a magnetic field strength is 0.4T, and the gradient of magnetic field strength drop is 0.01T/mm to form a molten pool perpendicular to the direction of Lorentz force The liquid surface is inward, and its descending gradient value is 400N/mm 4 from the molten pool surface to the bottom. The laser cladding base material is 316 austenitic stainless steel, which is machined into a metal sample of 100×10×10 mm. The surface is degreased, derusted, and polished to Ra1.6, and then cleaned with ethanol. Put the nickel-based alloy powder in a drying oven, set the temperature at 100°C, and dry for 60 minutes. After the powder is cooled, put it into the powder feeder, the chemical composition (mass fraction, %) of the alloy powder is: Ni 52.5%, Cr 15%, C 0.1%, Si 0.3%, Mn 0.3%, S0.01% , P 0.01%, Al 0.4%, Ti 1.5%, Mo 3%, Nb 5%, Fe 21.88%, consistent with Example 1. Turn on the laser generator (power is 1400W), gas protection device (argon gas flow rate is 10L/h, moisture content is 2%) and powder feeder (powder feed rate is 10g/min), and scan speed is 10mm/s according to the preset Set up the cladding trajectory for cladding, and obtain the uniform distribution of pores as shown in Figure 9. The diameter of the pores is 10-100 μm, and the total volume of the pores accounts for about 6% of the total volume of the cladding layer.

Claims (10)

1. a preparation method for control pore Ni-based coating, comprises the steps:
A: polish, clean, scrubbing: substrate surface is carried out grinding process, until surface-brightening reaches surface roughness and is less than Ra1.6, re-uses acetone or ethanol carries out wiping and cleans surface and oil contaminant removal, and dries in ventilation;
B: laser melting coating: use coaxial powder feeding device that nickel base powder is sent into matrix surface, forms laser melting coating molten bath, successively with swashing Photoscanning carry out laser melting coating makes cladding molten bath formed bubble, by following parameter adjustment nickel base powder Ti, C content, powder diameter, Powder sphericity, protection gas in moisture and combine laser technical parameters control cladding layer pore quantity;
Described nickel base powder mass fraction is: Ni 50.0~55.0%, Cr 12.0~17.10%, C 0.08~0.2%, Si 0~0.35%, Mn0~0.35%, S 0~0.018%, P0~0.015%, Al 0.30~0.70%, Ti 1.10~ 2%, Mo 2.8~3.30%, Nb 4.75~5.50%, surplus is Fe;Described powder diameter d=50~150 μm;
Described powder sphericity is 0.6~0.9;
In described protection gas, moisture mass fraction is 0.05~2%;
It is 800~1800W that described laser technical parameters controls in laser power;Scanning speed is 6~15mm/s;Protection throughput It is 10~80HF/min;Powder sending quantity 8~20g/min;
C: Lorentz force body force couples: is formed in bubble at cladding bath described in step B, is simultaneously introduced adjustable ladder Degree Lorentz force, the bubble forming step B process carries out pore that profile adjustment forms it in cladding layer by surface extremely The inside depth direction distribution gradient or be evenly distributed;Described Lorentz force control method is: be passed through at described matrix Being parallel to the DC current of described matrix surface until the end of scan, electric current density size is 0~106A/m2, meanwhile, by described Matrix be placed in gradient steady magnetic field until the end of scan so that the magnetic field intensity of weld pool surface is 0~2T, magnetic field intensity with The degree of depth molten bath increases and uniformly reduces, and the gradient that magnetic field intensity declines is 0.01~0.06T/mm.
2. the preparation method of control pore Ni-based coating as claimed in claim 1, it is characterised in that: described matrix melts at laser Being connected to wait to connect coated with external power supply that is front and that can provide DC current, described DC current is steady-state DC electric current, external Power supply is the big specified electric current accumulators of low pressure.
3. the preparation method of control pore Ni-based coating as claimed in claim 1, it is characterised in that: described magnetic field is by electric magnet Thering is provided, magnetic direction is parallel with cladding weld pool surface, both perpendicular to described laser scanning direction, by changing double sided contacts Rectangular shaped poles length and or width realize magnetic field gradient regulation, the width of described rectangular shaped poles is 10mm~40mm, described square A length of the 80 of shape magnetic pole~120mm.
4. the preparation method of control pore Ni-based coating as claimed in claim 1, it is characterised in that: the side of described Lorentz force To being passed through the sense of current by change or magnetic direction is adjusted.
5. the preparation method of the control pore Ni-based coating as described in one of Claims 1 to 4, it is characterised in that described swashs Luminous power is 1600W, and laser scanning speed is 10mm/s, and powder sending quantity is 10g/min, and protection throughput 20HF/min obtains cladding Layer spherical porosity.
6. the preparation method of the control pore Ni-based coating as described in one of Claims 1 to 4, it is characterised in that: adjust described Nickel base powder in the mass fraction of C be C 0.1% or and adjustment described in nickel base powder in the mass fraction of Ti be Ti 1.5%, the moisture controlled in protection gas is 2%, provides raw material to produce CO, CO for bubbling2Deng gas, control described powder End particle diameter d=50~75 μm, controlling described sphericity is 0.8~0.9, improves powder and the binding ability of moisture in protection gas.
7. the preparation method of the control pore Ni-based coating as described in one of Claims 1 to 4, is characterised by: step C regulation magnetic Field intensity is 1~2T, and electric current density is 105~106A/m2, make Lorentz force direction hang down with cladding weld pool surface simultaneously Straight inwardly bubble overflows quantity to be increased, and obtains in cladding layer remaining pore percent by volume 0~0.1% and be distributed in cladding layer Top;Described cladding layer refers to covered at the material of matrix surface by laser fusion and form the painting of metallurgical binding therewith Layer.
8. the preparation method of the control pore Ni-based coating as described in one of Claims 1 to 4, is characterised by: step C regulation magnetic Field intensity is 1~2T, and electric current density is 105~106A/m2, make Lorentz force direction hang down with cladding weld pool surface simultaneously Straight outside, bubble overflows quantity to be reduced, remaining pore percent by volume 5~20% in cladding layer, and is distributed in bottom cladding layer.
9. the preparation method of the control pore Ni-based coating as described in one of Claims 1 to 4, it is characterised in that: step C regulates Magnetic field intensity is 0.1~0.5T, and electric current density size is 0~105A/m2, make Lorentz force direction and cladding molten bath table simultaneously Face is perpendicularly inward so that the energy of bubble forming core reduces, and increased air bubble in described cladding molten bath, bubble is by fluid agitation effect And make cladding layer pore become uniform.
10. the preparation method of the control pore Ni-based coating as described in one of Claims 1 to 4, it is characterised in that: described Lip river Lun Zili is to intercouple generations, described Lorentz force direction and cladding weld pool surface by magnetic field and electric field in cladding molten bath zone Perpendicularly inward or vertically outside, by regulation current density value 0~106A/m2With magnetic field value 0~2T so that Lorentz lorentz's force value is big Little scope is 0~2 × 106N/m3, adjusting magnetic gradient 0.01~0.06T/mm so that Lorentz force is from a surface to the inside degree of depth Direction is also distributed in negative gradient, and the gradient that Lorentz force declines is 102~105N/mm4
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