激光熔覆制备超细陶瓷复合涂层的组织与性能研究
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摘要
激光表面复合强化处理作为一种高性能表面的制备方法,是当今研究热点之一。该技术有望在机车、重大装备、航空航天及工模具等领域的核心部件的高性能制造中有起着关键作用,有着巨大的应用前景。本文以激光熔覆技术为基础,结合化学沉积技术、溶胶凝胶化学合成技术以及纳米陶瓷增强技术等,制备了高性能陶瓷复合涂层,克服了单一的传统表面强化技术和激光熔覆技术存在的缺点,优势互补,是激光表面强化技术的继承和发展。
论文研究工作围绕下列几个方面展开：首先分别采用预置法、化学镀复合法及溶胶凝胶复合法三种粉体制备方法,将微纳米材料进行有效组装,进而采用脉冲Nd:YAG激光辐照,以在金属基体上制备强化层；建立了工艺参数优化模型,获得了高性能的超细陶瓷复合强化涂层；研究了各涂层的微观组织、硬度分布规律及磨损性能之间的关系,详细分析了陶瓷强化相的作用和涂层强化机理,并对不同方法制备涂层的特点和应用进行系统分析。主要结果如下：
(1)在激光作用下利用预置法熔覆镍包纳米Al2O3制备了Al2O3复合陶瓷涂层,通过优化试验,可获得硬度较高、无裂纹涂层的工艺参数组合是：50%Ni+50%Al2O3,电流强度150A,扫描速度300mm/min,脉冲宽度2ms,脉冲频率30Hz。该参数下获得了厚度为0.6mm和最高硬度为672Hv0.2的强化涂层,耐磨性提高1.5倍。该方法操作方便灵活,适用于复杂部件的局部强化,如模具型腔、内壁、刀具等。
(2)采用复合化学镀法制备了Ni-P-Al2O3复合强化镀层,利用高能脉冲激光对镀层进行强化处理,建立了基于神经网络的工艺参数预测模型,单道脉冲激光处理复合镀层的优化工艺参数为：电流强度200～240A；脉宽2.1～2.3ms；脉冲频率21～23Hz；扫描速率450mm/min。在该参数下,获得了厚度为0.2～0.3mm、硬度为840Hv0.2的强化涂层,耐磨性提高6倍。该方法涂层均匀性好,适用于要求较高的重要部件局部强化,如刀具刃口、叶片、轴颈等。
(3)采用激光与溶胶－凝胶化学合成反应复合法,制备了钛化物(TiC/TiN/TiB2复合强化涂层,制备TiC涂层优化的工艺参数为：TiO2和C的摩尔比为1：5,预置层厚度0.2mm,电流强度250A,脉宽2.5ms,频率18Hz,激光扫描速率50mm/min。在该参数下,获得了厚度为0.3～0.4mm,硬度达1150Hv0.1的强化涂层,耐磨性提高了12.5倍。该方法制备的涂层硬度高,耐磨性能良好,方便灵活,适用于各类工具刃部的强化。
(4)陶瓷强化相作用和涂层强化机理研究表明：由于纳米Al2O3异质相粒子的存在提高了熔体过冷度,改变了晶体生长形态,熔化表层从柱状晶向胞状晶转变,从而极大的促进了细晶组织的形成。晶粒细化和生成的A12O3、Al5FeNi、FeNi、 Fe0.64Ni0.36等高度弥散硬质相,是实现涂层强化的主要原因。而对于溶胶凝胶法,主要依靠激光与溶胶凝胶体(TiO2·2H2O+C+BN)的合成反应,获得TiC、TiB2和TiN为主要强化相的强化层。
综上所述,三种不同的复合方法都获得了不同效果的强化涂层,分别适用于复杂部件的局部强化、各类工具刃部强化及要求较高的重要部件局部强化,为获得高性能强化涂层提供了一条新途径。通过前期在医疗器械和机械装备上的初步应用试验表明,该技术在医疗微创手术器械和工模具领域有着广泛的应用前景和巨大的应用潜力。
As a high-performance coating preparation method, the hybrid laser surface strengthening technology has become a research focus, because it shows great application prospects in manufacturing key components for locomotive, magnitude equipment, aeroplane, giant tools and molds. In this paper, the high-performance ceramic composite coatings were prepared by combining laser cladding technology, chemical deposition technology, sol-gel chemical synthesis and nano-ceramics together. The hybrid laser surface strengthening technique is expected to obtain the complementary advantages of each technology, and to avoid the shortcomings of the traditional surface strengthening technology and laser cladding technology, which is considered as the inheritance and development of the laser surface strengthening technology.
The research in this paper was carried on around the following aspects. At first, the three kinds of powder preparation methods:presetting, electroless plating and sol-gel method, were adopted to assemble micro-and nano-materials effectively on the surface of the sample, and the pulsed Nd:YAG laser was used to produce hardening coatings on the metallic substrate. Secondly, with the help of the process parameters optimization model, the ultrafine ceramic reinforced composite coatings with high performances were prepared. Thirdly, the relations between the microstructure, microhardness distribution and the wear properties were investigated, the function of ceramic phases and the strengthening mechanism of the coatings were analyzed, and the characteristics and applications of different preparation methods were discussed as well. The main results are as follows:
(1) The Al2O3ceramic composite coatings were achieved by laser cladding preseted Ni-coated nano-Al2O3. The optimal processing parameters for crack-free coating with high hardness are under the condition of50%Ni+50%Al2O3, current intensity of150A, scanning speed of300mm/min, pulse width of2ms and pulse frequency of30Hz. With the optimal processing parameter, the coating with maximum hardness of672Hv0.2and hardening layer thickness of0.6mm can be obtained, and its wear resistance increases by1.5times with respect to that of the substrate. This method is convenient and flexible, which is suitable for local strengthening of the complex parts, such as the cavity and inner wall of mold, and tools.
(2) The Ni-P-Al2O3electroless plating coatings were strengthened by the pulsed Nd:YAG laser. A process parameters prediction model based on neural network was established, and the optimal strengthening parameters for single track are under the conditions including current intensity of200to240A, pulse width of2.1to2.3ms, pulse frequency of21to23Hz, scanning speed of450mm/min. With the optimal processing parameters, the coating with maximum hardness of840Hv0.2and hardening layer thickness of0.2-0.3mm can be obtained, and its wear resistance increases by6times relative to that of the substrate. This method is featured with nice homogeneity and is suitable for local strengthening of the key components with high propertied requirement, such as the cutting edge of cutters, turbine blades and shaft neck.
(3) The titanium compound (TiC/TiN/TiB2) strengthening coatings were achieved by chemical synthesis reaction via laser action and sol-gel. The optimal processing parameters are under the condition of TiO2and C molar ratio of1:5, the preseted layer thickness of0.2mm, the current intensity of250A, the pulse width of2.5ms, the pulse frequency of18Hz, and the laser scanning speed of50mm/min. With the optimal processing parameters, the coating with maximum hardness of1150Hv0.2and hardening layer thickness of0.3~0.4mm can be obtained and its wear resistance increases by12.5times from that of the substrate. This method is convenient and flexible, and can produce coatings with high hardness and wear resistance, which is suitable for the hardening of tools blade.
(4) The research results on the function of ceramic phases and the hardening mechanism show that, due to the presence of nano-Al2O3heterogeneous phase particles, the melt supercooling degree increases, and thus changes the crystal growth morphology as a consequence. The columnar grains change to cellular dendrite in the upper layer of the coating, which greatly promotes the formation of the fine grain structures. The grain refinement and the generation of highly dispersed hard phases such as Al2O3, Al5FeNi, FeNi and Fe0.64Ni0.36are the main factor causing the coating strengthening. As to the sol-gel compound laser hardening method, it is the synthesis reactions of laser and TiO2·2H2O+C+BN sol-gel to produce the hardening coating with TiC, TiB2and TiN ceramic reinforced phases.
In conclusion, different enhanced coatings with different functional characteristics were obtained thought the three different composite methods mentioned above. The three hybrid methods are suitable for the local hardening of complex parts, tools blade and local strengthening of the critical parts, respectively, which provides a new way to obtain high-performance strengthening coating. The preliminary application tests in the medical devices and mechanized equipment show that the technology has broad application prospects and great potential for the application in medical minimally invasive surgical instruments and the fields of tool and die.
论文研究工作围绕下列几个方面展开：首先分别采用预置法、化学镀复合法及溶胶凝胶复合法三种粉体制备方法,将微纳米材料进行有效组装,进而采用脉冲Nd:YAG激光辐照,以在金属基体上制备强化层；建立了工艺参数优化模型,获得了高性能的超细陶瓷复合强化涂层；研究了各涂层的微观组织、硬度分布规律及磨损性能之间的关系,详细分析了陶瓷强化相的作用和涂层强化机理,并对不同方法制备涂层的特点和应用进行系统分析。主要结果如下：
(1)在激光作用下利用预置法熔覆镍包纳米Al2O3制备了Al2O3复合陶瓷涂层,通过优化试验,可获得硬度较高、无裂纹涂层的工艺参数组合是：50%Ni+50%Al2O3,电流强度150A,扫描速度300mm/min,脉冲宽度2ms,脉冲频率30Hz。该参数下获得了厚度为0.6mm和最高硬度为672Hv0.2的强化涂层,耐磨性提高1.5倍。该方法操作方便灵活,适用于复杂部件的局部强化,如模具型腔、内壁、刀具等。
(2)采用复合化学镀法制备了Ni-P-Al2O3复合强化镀层,利用高能脉冲激光对镀层进行强化处理,建立了基于神经网络的工艺参数预测模型,单道脉冲激光处理复合镀层的优化工艺参数为：电流强度200～240A；脉宽2.1～2.3ms；脉冲频率21～23Hz；扫描速率450mm/min。在该参数下,获得了厚度为0.2～0.3mm、硬度为840Hv0.2的强化涂层,耐磨性提高6倍。该方法涂层均匀性好,适用于要求较高的重要部件局部强化,如刀具刃口、叶片、轴颈等。
(3)采用激光与溶胶－凝胶化学合成反应复合法,制备了钛化物(TiC/TiN/TiB2复合强化涂层,制备TiC涂层优化的工艺参数为：TiO2和C的摩尔比为1：5,预置层厚度0.2mm,电流强度250A,脉宽2.5ms,频率18Hz,激光扫描速率50mm/min。在该参数下,获得了厚度为0.3～0.4mm,硬度达1150Hv0.1的强化涂层,耐磨性提高了12.5倍。该方法制备的涂层硬度高,耐磨性能良好,方便灵活,适用于各类工具刃部的强化。
(4)陶瓷强化相作用和涂层强化机理研究表明：由于纳米Al2O3异质相粒子的存在提高了熔体过冷度,改变了晶体生长形态,熔化表层从柱状晶向胞状晶转变,从而极大的促进了细晶组织的形成。晶粒细化和生成的A12O3、Al5FeNi、FeNi、 Fe0.64Ni0.36等高度弥散硬质相,是实现涂层强化的主要原因。而对于溶胶凝胶法,主要依靠激光与溶胶凝胶体(TiO2·2H2O+C+BN)的合成反应,获得TiC、TiB2和TiN为主要强化相的强化层。
综上所述,三种不同的复合方法都获得了不同效果的强化涂层,分别适用于复杂部件的局部强化、各类工具刃部强化及要求较高的重要部件局部强化,为获得高性能强化涂层提供了一条新途径。通过前期在医疗器械和机械装备上的初步应用试验表明,该技术在医疗微创手术器械和工模具领域有着广泛的应用前景和巨大的应用潜力。
As a high-performance coating preparation method, the hybrid laser surface strengthening technology has become a research focus, because it shows great application prospects in manufacturing key components for locomotive, magnitude equipment, aeroplane, giant tools and molds. In this paper, the high-performance ceramic composite coatings were prepared by combining laser cladding technology, chemical deposition technology, sol-gel chemical synthesis and nano-ceramics together. The hybrid laser surface strengthening technique is expected to obtain the complementary advantages of each technology, and to avoid the shortcomings of the traditional surface strengthening technology and laser cladding technology, which is considered as the inheritance and development of the laser surface strengthening technology.
The research in this paper was carried on around the following aspects. At first, the three kinds of powder preparation methods:presetting, electroless plating and sol-gel method, were adopted to assemble micro-and nano-materials effectively on the surface of the sample, and the pulsed Nd:YAG laser was used to produce hardening coatings on the metallic substrate. Secondly, with the help of the process parameters optimization model, the ultrafine ceramic reinforced composite coatings with high performances were prepared. Thirdly, the relations between the microstructure, microhardness distribution and the wear properties were investigated, the function of ceramic phases and the strengthening mechanism of the coatings were analyzed, and the characteristics and applications of different preparation methods were discussed as well. The main results are as follows:
(1) The Al2O3ceramic composite coatings were achieved by laser cladding preseted Ni-coated nano-Al2O3. The optimal processing parameters for crack-free coating with high hardness are under the condition of50%Ni+50%Al2O3, current intensity of150A, scanning speed of300mm/min, pulse width of2ms and pulse frequency of30Hz. With the optimal processing parameter, the coating with maximum hardness of672Hv0.2and hardening layer thickness of0.6mm can be obtained, and its wear resistance increases by1.5times with respect to that of the substrate. This method is convenient and flexible, which is suitable for local strengthening of the complex parts, such as the cavity and inner wall of mold, and tools.
(2) The Ni-P-Al2O3electroless plating coatings were strengthened by the pulsed Nd:YAG laser. A process parameters prediction model based on neural network was established, and the optimal strengthening parameters for single track are under the conditions including current intensity of200to240A, pulse width of2.1to2.3ms, pulse frequency of21to23Hz, scanning speed of450mm/min. With the optimal processing parameters, the coating with maximum hardness of840Hv0.2and hardening layer thickness of0.2-0.3mm can be obtained, and its wear resistance increases by6times relative to that of the substrate. This method is featured with nice homogeneity and is suitable for local strengthening of the key components with high propertied requirement, such as the cutting edge of cutters, turbine blades and shaft neck.
(3) The titanium compound (TiC/TiN/TiB2) strengthening coatings were achieved by chemical synthesis reaction via laser action and sol-gel. The optimal processing parameters are under the condition of TiO2and C molar ratio of1:5, the preseted layer thickness of0.2mm, the current intensity of250A, the pulse width of2.5ms, the pulse frequency of18Hz, and the laser scanning speed of50mm/min. With the optimal processing parameters, the coating with maximum hardness of1150Hv0.2and hardening layer thickness of0.3~0.4mm can be obtained and its wear resistance increases by12.5times from that of the substrate. This method is convenient and flexible, and can produce coatings with high hardness and wear resistance, which is suitable for the hardening of tools blade.
(4) The research results on the function of ceramic phases and the hardening mechanism show that, due to the presence of nano-Al2O3heterogeneous phase particles, the melt supercooling degree increases, and thus changes the crystal growth morphology as a consequence. The columnar grains change to cellular dendrite in the upper layer of the coating, which greatly promotes the formation of the fine grain structures. The grain refinement and the generation of highly dispersed hard phases such as Al2O3, Al5FeNi, FeNi and Fe0.64Ni0.36are the main factor causing the coating strengthening. As to the sol-gel compound laser hardening method, it is the synthesis reactions of laser and TiO2·2H2O+C+BN sol-gel to produce the hardening coating with TiC, TiB2and TiN ceramic reinforced phases.
In conclusion, different enhanced coatings with different functional characteristics were obtained thought the three different composite methods mentioned above. The three hybrid methods are suitable for the local hardening of complex parts, tools blade and local strengthening of the critical parts, respectively, which provides a new way to obtain high-performance strengthening coating. The preliminary application tests in the medical devices and mechanized equipment show that the technology has broad application prospects and great potential for the application in medical minimally invasive surgical instruments and the fields of tool and die.
引文
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