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CN101323900A - High speed processing method for realizing superfine crystal grain structure on metallic material surface - Google Patents

High speed processing method for realizing superfine crystal grain structure on metallic material surface Download PDF

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CN101323900A
CN101323900A CNA2007100117246A CN200710011724A CN101323900A CN 101323900 A CN101323900 A CN 101323900A CN A2007100117246 A CNA2007100117246 A CN A2007100117246A CN 200710011724 A CN200710011724 A CN 200710011724A CN 101323900 A CN101323900 A CN 101323900A
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grain structure
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李文利
陶乃镕
卢柯
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Institute of Metal Research of CAS
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Abstract

本发明涉及纳米结构的金属材料表面高速变形的处理方法,特别提供了一种在金属材料表层实现超细晶粒组织结构的高速加工方法。在室温或低温条件下,通过高速塑性变形的机械处理方法,使金属材料表层微米级粗大晶粒结构细化成近于等轴的亚微米晶粒或纳米晶粒,在金属材料表层形成超细晶粒组织结构。随距离处理表面深度的增加,微观结构尺寸呈梯度变化,由纳米级、亚微米尺寸增大至微米级。本发明的高速加工方法与现有形成表面超细晶粒结构的处理方法相比,被处理的金属材料表面粗糙度明显减小,变形层厚度增加,而且处理方法简单,工作效率高。The invention relates to a processing method for high-speed deformation of the surface of a metal material with a nanostructure, and in particular provides a high-speed processing method for realizing an ultrafine grain structure on the surface of the metal material. At room temperature or low temperature, through the mechanical treatment method of high-speed plastic deformation, the micron-scale coarse grain structure on the surface of the metal material is refined into nearly equiaxed submicron grains or nano-grains, and ultra-fine grains are formed on the surface of the metal material granular structure. With the increase of the depth from the treated surface, the size of the microstructure changes in a gradient, from nanometer and submicron to micron. Compared with the existing processing method for forming superfine grain structure on the surface, the high-speed processing method of the present invention obviously reduces the surface roughness of the processed metal material, increases the thickness of the deformed layer, and has simple processing method and high working efficiency.

Description

在金属材料表层实现超细晶粒组织结构的高速加工方法 A high-speed machining method for realizing ultra-fine grain structure on the surface of metal materials

技术领域 technical field

本发明涉及纳米结构的金属材料表面高速变形的处理方法,特别提供了一种在金属材料表层实现超细晶粒组织结构的高速加工方法,在金属材料表层形成纳米尺寸、亚微米尺寸的超细晶粒组织结构。The invention relates to a treatment method for high-speed deformation of the surface of a metal material with a nanostructure, and in particular provides a high-speed processing method for realizing an ultra-fine grain structure on the surface of a metal material, forming nano-sized and sub-micron-sized ultra-fine particles on the surface of the metal material. Grain structure.

背景技术 Background technique

纳米材料是由结构尺寸小于100nm的亚结构组成的单相或多相晶体材料,由于纳米材料晶界占有很大的比例,纳米材料通常具有不同于、而且常常优越于普通多晶体材料的优异性能,例如高强度,高扩散系数,良好的电学、磁学等性能。Nanomaterials are single-phase or multi-phase crystalline materials composed of substructures with a structural size less than 100nm. Since the grain boundaries of nanomaterials occupy a large proportion, nanomaterials usually have excellent properties that are different from and often superior to ordinary polycrystalline materials. , such as high strength, high diffusion coefficient, good electrical and magnetic properties.

目前,纳米结构材料领域的研究主要针对块体纳米结构材料的合成、制备、结构特征、热稳定性等方面。从已有的方法来看,气相冷凝、机械球磨等方法难以消除所制备材料中的孔洞,污染等缺陷的不良影响;而等通道挤压(ECAP),叠层轧制接合(ARB)等严重塑性变形方法弥补了前述方法的缺点,但设备损耗大,工作效率低,成本高;处理的材料其形状、尺寸都有很大的局限性,难以实现工业应用。At present, research in the field of nanostructured materials mainly focuses on the synthesis, preparation, structural characteristics, and thermal stability of bulk nanostructured materials. From the existing methods, methods such as gas phase condensation and mechanical ball milling are difficult to eliminate the adverse effects of defects such as holes and pollution in the prepared materials; The plastic deformation method makes up for the shortcomings of the above-mentioned methods, but the equipment loss is large, the work efficiency is low, and the cost is high; the shape and size of the processed materials have great limitations, and it is difficult to realize industrial application.

事实上,材料的失效大多发生在材料的表面,因此材料表面结构性能的好坏直接影响工程金属材料的综合性能指标。将常规工程材料表面层微观结构尺寸细化至纳米、亚微米尺度,利用纳米结构材料的优异性能来改善材料表面的结构、性能,尤其是疲劳性能,腐蚀性能和摩擦、磨损性能等,从而提高工程材料的综合性能及服役行为。In fact, the failure of materials mostly occurs on the surface of the material, so the quality of the surface structure of the material directly affects the comprehensive performance indicators of engineering metal materials. The microstructure size of the surface layer of conventional engineering materials is refined to the nanometer and submicron scale, and the excellent performance of nanostructure materials is used to improve the structure and performance of the material surface, especially the fatigue performance, corrosion performance, friction and wear performance, etc., thereby improving Comprehensive performance and service behavior of engineering materials.

现有的金属材料表面处理的方法主要有:(1)表面涂层。利用涂层和沉积技术如PVD、CVD、溅射镀膜、电镀等方法在基体材料表面生成一层纳米结构层。这种技术的关键是涂层与基体之间以及涂层粒子之间的结合力,最容易也最常发生的失效是涂层的剥离或脱落。另外,设备投资较大,生产成本较高,不适用于数量巨大的工程金属材料表面处理;(2)表面机械处理法。利用表面机械研磨处理技术,在外加载荷的重复作用下,材料表面的粗晶组织经过不同方向产生的强烈塑性变形而逐渐碎化至纳米量级。然而目前这种处理技术得到的样品表面粗糙度较大,无法满足实际应用的要求,限制了其在工业中的推广,处理的样品形状也有很大的局限性。此外,操作程序比较繁琐,研磨使用的托盘和球丸消耗大,导致成本增加。The existing metal material surface treatment methods mainly include: (1) surface coating. Using coating and deposition techniques such as PVD, CVD, sputter coating, electroplating and other methods to generate a nanostructure layer on the surface of the base material. The key to this technology is the bonding force between the coating and the substrate and between the coating particles. The easiest and most frequent failure is the peeling or falling off of the coating. In addition, the investment in equipment is large and the production cost is high, so it is not suitable for the surface treatment of a large number of engineering metal materials; (2) surface mechanical treatment. Using the surface mechanical grinding treatment technology, under the repeated action of external load, the coarse-grained structure on the surface of the material undergoes strong plastic deformation in different directions and gradually fragments to the nanometer level. However, the surface roughness of the sample obtained by this processing technology is relatively large at present, which cannot meet the requirements of practical applications, which limits its promotion in industry, and the shape of the processed sample also has great limitations. In addition, the operating procedures are relatively cumbersome, and the consumption of trays and pellets used for grinding is large, resulting in increased costs.

发明内容 Contents of the invention

本发明的目的在于提供一种新型金属材料表面高速变形处理方法,其投资少,操作简单,工业上易于实现,用其制备的纳米、亚微米结构层不易脱落,并且可以通过控制各种条件来处理复杂形状的工件,同时保证较低的表面粗糙度,还能够使用比较成熟的机械加工冷却技术,从而为全面提高工程金属材料的表面性能提供可能。The purpose of the present invention is to provide a new type of metal material surface high-speed deformation treatment method, which has low investment, simple operation, and easy industrial realization. The nano and submicron structure layers prepared by it are not easy to fall off, and can be controlled by various conditions. It handles workpieces with complex shapes while ensuring low surface roughness, and can also use relatively mature machining cooling technology, thus providing the possibility to comprehensively improve the surface properties of engineering metal materials.

本发明的技术方案是:Technical scheme of the present invention is:

本发明提供了一种金属材料表面高速变形处理方法,该处理方法装置由工件高速运动机构,刀具进给机构和冷却机构组成。本发明采用一定曲率半径的刀具做轴向进给运动,被处理工件做高速旋转运动,选择不同的冷却介质进行冷却来控制处理时金属材料表面的温度。其中,刀具的曲率半径优选范围为4mm---8mm;刀具的轴向进给速度优选范围为150mm/min---250mm/min;被处理工件转速优选范围为600rpm---1000rpm;被处理工件的金属材料表面温度优选范围为-100℃---20℃;冷却介质可以为高压油雾、液氮气体。The invention provides a high-speed deformation treatment method for the surface of metal materials. The treatment method device is composed of a workpiece high-speed movement mechanism, a tool feed mechanism and a cooling mechanism. The invention adopts a tool with a certain radius of curvature to perform axial feed movement, and the workpiece to be processed performs high-speed rotational movement, and selects different cooling media for cooling to control the surface temperature of the metal material during processing. Among them, the preferred range of the radius of curvature of the tool is 4mm---8mm; the preferred range of the axial feed speed of the tool is 150mm/min---250mm/min; the preferred range of the workpiece speed to be processed is 600rpm---1000rpm; The surface temperature of the metal material of the workpiece preferably ranges from -100°C to 20°C; the cooling medium can be high-pressure oil mist or liquid nitrogen gas.

本发明所依据的原理是通过高速变形导致金属材料表面产生严重塑性变形,使表面晶粒通过位错增殖、运动、湮灭、重排等过程细化至纳米尺寸。因而任何可使刀具和工件呈现高速相对运动的设备均可作为本发明结构,如各种车床,磨床等。The principle of the present invention is to cause serious plastic deformation on the surface of metal materials through high-speed deformation, so that the surface grains are refined to nanometer size through processes such as dislocation proliferation, movement, annihilation, and rearrangement. Therefore any equipment that can cause the tool and the workpiece to exhibit high-speed relative motion can be used as the structure of the present invention, such as various lathes, grinding machines and the like.

利用高速变形技术,对工件表面进行低温多次变形处理,工艺参数:Using high-speed deformation technology, low-temperature multiple deformation treatment is performed on the surface of the workpiece. Process parameters:

变形应变速率:103-106s-1Deformation strain rate: 10 3 -10 6 s -1 ;

变形应变量:总变形量大于2.9(计算方法: ϵ = γ / 3 , ε为变形量,γ为剪应变);Deformation strain: the total deformation is greater than 2.9 (calculation method: ϵ = γ / 3 , ε is the amount of deformation, γ is the shear strain);

变形温度:-196℃---100℃。Deformation temperature: -196°C---100°C.

本发明具有如下优点:The present invention has the following advantages:

1.处理方法简单。本发明利用高速变形技术,处理方法简单,易于控制好变形工艺参数和变形温度。对目前传统的切削技术进行必要的改进,优化工艺参数和变形温度,即可得到表面细化结构层。1. The processing method is simple. The invention utilizes high-speed deformation technology, has a simple processing method, and is easy to control deformation process parameters and deformation temperature. Necessary improvements are made to the current traditional cutting technology, and the process parameters and deformation temperature are optimized to obtain a refined surface structure layer.

2.适用性强。适用于各种复杂工件的表面处理,并且是在不改变材料的化学成分的情况下,只通过调整材料的微观结构来强化金属及合金。2. Strong applicability. It is suitable for the surface treatment of various complex workpieces, and only adjusts the microstructure of the material to strengthen metals and alloys without changing the chemical composition of the material.

3.处理后表面质量高。本方法的处理方式保证了整个表面处理的均匀性,从而得到较低的表面粗糙度,变形层厚度增加,并且处理完成后很容易通过各种常规的工业手段对表面进行修整。3. High surface quality after treatment. The treatment method of the method ensures the uniformity of the entire surface treatment, thereby obtaining a lower surface roughness, increasing the thickness of the deformed layer, and after the treatment is completed, it is easy to repair the surface by various conventional industrial means.

本发明是通过对金属材料的表面进行高速变形处理,在材料表面形成一定厚度的纳米、亚微米组织结构,而保持材料的表层与整体成分不变。晶粒尺寸分布:沿深度方向,表层一定厚度(厚度大约为20μm---300μm)内为纳米、亚微米尺寸的细化结构、变形组织层和基体的粗大晶粒组织。由于材料的破坏起源于材料的表面,因此表面结构的优化有利于材料基本性能的提高,如在抑制裂纹生长方面,细小晶粒优于粗大晶粒。反之,在抵制裂纹扩展方面,粗大晶粒优于细小晶粒。这样,细小晶粒表层与粗大晶粒基体的理想组合,对延长材料的使用寿命更加有利。总之,本发明将纳米材料的优异性能与工程金属材料相结合,给传统的金属材料赋予特殊性能,这在基础研究和工程应用方面均有十分广阔的前景。In the present invention, through high-speed deformation treatment on the surface of the metal material, a nanometer and submicron tissue structure with a certain thickness is formed on the surface of the material, while the surface layer and the overall composition of the material remain unchanged. Grain size distribution: Along the depth direction, within a certain thickness of the surface layer (thickness is about 20μm---300μm), there are nanometer and submicron-sized refined structures, deformed structure layers and coarse grain structures of the matrix. Since the damage of the material originates from the surface of the material, the optimization of the surface structure is beneficial to the improvement of the basic properties of the material. For example, fine grains are better than coarse grains in inhibiting crack growth. Conversely, coarser grains are better than finer grains in resisting crack propagation. In this way, the ideal combination of the fine grain surface layer and the coarse grain matrix is more beneficial to prolong the service life of the material. In a word, the present invention combines the excellent properties of nanomaterials with engineering metal materials, endowing traditional metal materials with special properties, which has very broad prospects in both basic research and engineering applications.

附图说明 Description of drawings

图1为利用本发明技术处理的纯铜材料表层透射电镜照片(主轴转速:600rpm)。Fig. 1 is the transmission electron microscope photo (spindle speed: 600rpm) of the surface layer of pure copper material processed by the technology of the present invention.

图2为利用本发明技术处理的纯铜材料的表层透射电镜照片(主轴转速:1000rpm)。Fig. 2 is a transmission electron microscope photograph of the surface layer of the pure copper material processed by the technology of the present invention (spindle speed: 1000rpm).

图3(a)-(c)为利用本发明技术处理的纯铜材料的表层透射电镜明(a)、暗(b)场像、衍射(c)照片(主轴转速:600rpm)。Figure 3(a)-(c) is the surface TEM bright (a), dark (b) field image and diffraction (c) photo of the pure copper material processed by the technology of the present invention (spindle speed: 600rpm).

图4为本发明处理方法所采用装置结构示意图。图中,1工件夹持及旋转机构;2刀具夹持及进给机构;3油雾冷却喷嘴;4冷却介质;5工件;6刀具。Fig. 4 is a schematic structural diagram of the device used in the treatment method of the present invention. In the figure, 1 workpiece clamping and rotating mechanism; 2 tool clamping and feeding mechanism; 3 oil mist cooling nozzle; 4 cooling medium; 5 workpiece; 6 tool.

具体实施方式 Detailed ways

如图4所示,本发明处理方法所采用装置由工件夹持及旋转机构1、刀具夹持及进给机构2、油雾冷却喷嘴3、冷却介质4、工件5、刀具6组成,其工作过程如下:本发明采用一定曲率半径的刀具6,在刀具夹持及进给机构2的带动下做轴向进给运动,被处理工件5在工件夹持及旋转机构1的带动下做高速旋转运动,选择不同的冷却介质进行冷却来控制处理时金属材料表面的温度,冷却喷嘴3喷出的高压油雾(喷油机供气气压大于80psi),以及液氮冷却气体作为冷却介质4。其中,刀具的曲率半径优选范围为4mm---8mm;刀具的轴向进给速度优选范围为150mm/min---250mm/min;被处理工件转速优选范围为600rpm---1000rpm;被处理工件的金属材料表面温度优选范围为-100℃---20℃。As shown in Figure 4, the device used in the processing method of the present invention is composed of a workpiece clamping and rotating mechanism 1, a tool clamping and feeding mechanism 2, an oil mist cooling nozzle 3, a cooling medium 4, a workpiece 5, and a tool 6. The process is as follows: the present invention uses a tool 6 with a certain radius of curvature to perform axial feed motion driven by the tool clamping and feeding mechanism 2, and the processed workpiece 5 is driven by the workpiece clamping and rotating mechanism 1 to perform high-speed rotation Movement, choose different cooling media for cooling to control the temperature of the metal material surface during processing, the high-pressure oil mist sprayed from the cooling nozzle 3 (the air supply pressure of the fuel injector is greater than 80psi), and liquid nitrogen cooling gas as the cooling medium 4. Among them, the preferred range of the radius of curvature of the tool is 4mm---8mm; the preferred range of the axial feed speed of the tool is 150mm/min---250mm/min; the preferred range of the workpiece speed to be processed is 600rpm---1000rpm; The surface temperature of the metal material of the workpiece preferably ranges from -100°C to 20°C.

下面通过实施例详述本发明。The present invention is described in detail below by way of examples.

实施例1Example 1

利用表面高速变形技术处理纯铜材料:Treatment of pure copper materials using surface high-speed deformation technology:

设备:表面高速变形处理设备;Equipment: Surface high-speed deformation treatment equipment;

主轴转速:600rpm;Spindle speed: 600rpm;

变形应变速率:103-104s-1Deformation strain rate: 10 3 -10 4 s -1 ;

变形应变量:3-5;Deformation strain: 3-5;

变形温度:20℃;Deformation temperature: 20°C;

处理道次:8;Processing passes: 8;

纯铜材料:纯度99.97%(重量百分比),经600℃退火3小时,晶粒尺寸20μm。Pure copper material: purity 99.97% (weight percent), annealed at 600° C. for 3 hours, grain size 20 μm.

处理得到表层细化的纯铜材料,如图1,表层厚度约为60μm,其微观结构主要特征是接近等轴的亚微米晶粒/亚晶粒,短轴尺寸为164nm,长轴尺寸为351nm。The pure copper material with a refined surface layer is obtained after treatment, as shown in Figure 1, the surface layer thickness is about 60 μm, and the main characteristics of its microstructure are submicron grains/subgrains that are close to equiaxes, the short axis size is 164nm, and the long axis size is 351nm .

实施例2Example 2

利用表面高速变形技术处理纯铜材料:Treatment of pure copper materials using surface high-speed deformation technology:

设备:表面高速变形处理设备;Equipment: Surface high-speed deformation treatment equipment;

主轴转速:1000rpm;Spindle speed: 1000rpm;

变形应变速率:103-104s-1Deformation strain rate: 10 3 -10 4 s -1 ;

变形应变量:3-5;Deformation strain: 3-5;

变形温度:20℃;Deformation temperature: 20°C;

处理道次:8;Processing passes: 8;

纯铜材料:纯度99.97%,经600℃退火3小时,晶粒尺寸20μm。Pure copper material: purity 99.97%, annealed at 600°C for 3 hours, grain size 20μm.

处理得到的表层结构如图2,表层厚度约为30μm,短轴尺寸为178nm,长轴尺寸为587nm。The surface structure obtained after the treatment is shown in Figure 2, the surface thickness is about 30 μm, the short axis size is 178 nm, and the long axis size is 587 nm.

实施例3Example 3

利用表面高速变形技术处理纯铜材料:Treatment of pure copper materials using surface high-speed deformation technology:

设备:表面高速变形处理设备;Equipment: Surface high-speed deformation processing equipment;

主轴转速:600rpm;Spindle speed: 600rpm;

变形应变速率:103-104s-1Deformation strain rate: 10 3 -10 4 s -1 ;

变形应变量:3-5;Deformation strain: 3-5;

变形温度:20℃;Deformation temperature: 20°C;

处理道次:6;Processing passes: 6;

纯铜材料:纯度99.97%,经600℃退火3小时,晶粒尺寸20μm。Pure copper material: purity 99.97%, annealed at 600°C for 3 hours, grain size 20μm.

处理得到的表层厚度约为30μm,短轴尺寸为158nm,长轴尺寸为604nm。The thickness of the treated surface layer is about 30 μm, the short axis dimension is 158nm, and the long axis dimension is 604nm.

实施例4Example 4

利用表面高速变形技术处理纯铜材料:Treatment of pure copper materials using surface high-speed deformation technology:

设备:表面高速变形处理设备;Equipment: Surface high-speed deformation treatment equipment;

主轴转速:600rpm;Spindle speed: 600rpm;

变形应变速率:103-104s-1Deformation strain rate: 10 3 -10 4 s -1 ;

变形应变量:3-5;Deformation strain: 3-5;

变形温度:-100℃;Deformation temperature: -100°C;

处理道次:6;Processing passes: 6;

纯铜材料:纯度99.97%,经600℃退火3小时,晶粒尺寸20μm。Pure copper material: purity 99.97%, annealed at 600°C for 3 hours, grain size 20μm.

处理得到的表层是接近等轴的纳米晶,最表层5μm内晶粒短轴尺寸为19nm,长轴尺寸为38nm,纳米层厚度约为20μm,如图3(a)-(c)所示,利用本发明技术处理的纯铜材料的表层透射电镜明、暗场像、衍射照片。The treated surface layer is nearly equiaxed nanocrystals, the minor axis size of the crystal grains within 5 μm of the outermost layer is 19 nm, the major axis size is 38 nm, and the thickness of the nanolayer is about 20 μm, as shown in Figure 3(a)-(c), The surface transmission electron microscope bright and dark field images and diffraction photos of the pure copper material processed by the technology of the present invention.

比较例1Comparative example 1

等通道挤压(ECAP)处理8道次后纯铜的层片间距为290±160nm,本发明的方法与该方法根本区别在于本方法采用了低温高应变速率变形技术,可以使纯铜表层晶粒尺寸减小到纳米尺寸。The lamellar spacing of pure copper after 8 passes of equal channel extrusion (ECAP) is 290 ± 160nm. The fundamental difference between the method of the present invention and this method is that the method adopts a low temperature high strain rate deformation technology, which can make the pure copper surface crystal The particle size is reduced to nanometer size.

比较例2Comparative example 2

纯铜的表面机械研磨处理5分钟后表层的平均晶粒/位错胞尺寸为160nm。本发明的方法相对表面机械研磨处理方法的优越性在于:沿表面方向微观结构更均匀及表面粗糙度明显减小。The average grain/dislocation cell size of the surface layer was 160nm after the surface mechanical grinding treatment of pure copper for 5 minutes. Compared with the surface mechanical grinding treatment method, the method of the present invention has the advantages that the microstructure is more uniform along the surface direction and the surface roughness is obviously reduced.

Claims (8)

1. high-speed processing method of realizing superfine crystal grain structure on the metallic substance top layer is characterized in that: utilize the high speed relative movement on cutter and processed workpiece surface, workpiece surface is carried out repeatedly deformation process of low temperature, processing parameter:
Deformation strain speed: 10 3---10 6s -1
The deformation strain amount: total deformation is greater than 2.9, method of calculation: ϵ = γ / 3 , ε is a deflection, and γ is tangential strain;
Texturing temperature :-196 ℃ to 100 ℃.
2. according to the described high-speed processing method of realizing superfine crystal grain structure on the metallic substance top layer of claim 1, it is characterized in that: deformation strain amount preferable range is 3-5.
3. according to the described high-speed processing method of realizing superfine crystal grain structure on the metallic substance top layer of claim 1, it is characterized in that: cutter is done axial feed motion, processed workpiece rotates, and adopts heat-eliminating medium to cool off the temperature of controlling metal material surface when handling.
4. according to the described high-speed processing method of realizing superfine crystal grain structure on the metallic substance top layer of claim 3, it is characterized in that: the radius-of-curvature preferable range of cutter is 4mm---8mm.
5. according to the described high-speed processing method of realizing superfine crystal grain structure on the metallic substance top layer of claim 3, it is characterized in that: the axial feed velocity preferable range of cutter is 150mm/min---250mm/min.
6. according to the described high-speed processing method of realizing superfine crystal grain structure on the metallic substance top layer of claim 3, it is characterized in that: processed workpiece rotating speed preferable range is 600rpm---1000rpm.
7. according to the described high-speed processing method of realizing superfine crystal grain structure on the metallic substance top layer of claim 3, it is characterized in that: the metal material surface temperature preferable range of processed workpiece is-100 ℃---20 ℃.
8. according to the described high-speed processing method of realizing superfine crystal grain structure on the metallic substance top layer of claim 3, it is characterized in that: heat-eliminating medium is high pressure mist of oil, liquid nitrogen gas.
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