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CN111320487A - Silicon Nitride Ceramic Surface Modification Assisted Direct Diffusion Bonding Method - Google Patents

Silicon Nitride Ceramic Surface Modification Assisted Direct Diffusion Bonding Method Download PDF

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CN111320487A
CN111320487A CN202010146123.1A CN202010146123A CN111320487A CN 111320487 A CN111320487 A CN 111320487A CN 202010146123 A CN202010146123 A CN 202010146123A CN 111320487 A CN111320487 A CN 111320487A
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silicon nitride
ceramic
nitride ceramic
metal
surface modification
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刘多
宋延宇
胡胜鹏
宋晓国
曹健
冯吉才
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Harbin Institute of Technology Weihai
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B37/00Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/02Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
    • C04B37/021Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles in a direct manner, e.g. direct copper bonding [DCB]
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics

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Abstract

The invention provides a silicon nitride ceramic surface modification auxiliary direct diffusion bonding method, which comprises the steps of firstly pretreating the surface of silicon nitride ceramic to remove surface oil stains and impurities, and then carrying out laser irradiation treatment on the surface of silicon nitride ceramic under the protection of vacuum or inert gas; assembling the treated materials according to the sequence of the silicon nitride ceramics and the metal materials, placing the materials in a vacuum diffusion connecting device for pressurizing, heating and preserving heat for a period of time, utilizing the modified silicon nitride ceramics and the metal materials to generate a local eutectic liquid phase through eutectic reaction, and then solidifying the eutectic liquid phase to realize the connection of the ceramics and the metal. The method solves the problems of higher cost and less selection range of brazing filler metal in the existing active metal brazing method. The invention can be widely applied to the high-quality connection of ceramics and metals.

Description

氮化硅陶瓷表面改性辅助直接扩散连接方法Silicon Nitride Ceramic Surface Modification Assisted Direct Diffusion Bonding Method

技术领域technical field

本发明涉及陶瓷与金属连接技术领域,特别是涉及一种氮化硅陶瓷表面改性辅助直接扩散连接方法。The invention relates to the technical field of ceramic and metal connection, in particular to a method for direct diffusion connection assisted by surface modification of silicon nitride ceramics.

背景技术Background technique

随着当前新能源汽车、可再生能源以及电子元器件等领域的快速发展,对功率电子器件的性能也提出了更高的要求。绝缘栅双极晶体管(IGBT)作为电力电子领域中最重要的大功率器件,已广泛应用于电动汽车、智能电网和轨道交通等领域,其中,用于封装功率模块的基板材料作为支撑体、绝缘体以及导热通道是模块中的关键基础材料。目前常用的IGBT模块基板材料为陶瓷基板,主要包括氧化铝、氮化铝和氮化硅陶瓷基板,其中氮化硅陶瓷相对于氧化铝和氮化铝两种陶瓷材料,氮化硅陶瓷具有良好的机械性能、抗热震性和耐高温氧化及抗化学腐蚀性能等优点,同时还具备抵抗热冷冲击的特点,在空气中加热到1000℃以上,急剧冷却再急剧加热也不会碎裂,因此采用氮化硅陶瓷作为功率模块中的基板材料对于推进大功率器件在极端条件以及复杂的力学环境中的应用具有重要的意义。With the current rapid development of new energy vehicles, renewable energy, and electronic components, higher requirements are placed on the performance of power electronic devices. As the most important high-power device in the field of power electronics, insulated gate bipolar transistors (IGBTs) have been widely used in electric vehicles, smart grids, and rail transit. And the heat conduction channel is the key base material in the module. At present, the commonly used IGBT module substrate materials are ceramic substrates, mainly including alumina, aluminum nitride and silicon nitride ceramic substrates. Compared with the two ceramic materials of alumina and aluminum nitride, silicon nitride ceramics have better performance. It has the advantages of excellent mechanical properties, thermal shock resistance, high temperature oxidation resistance and chemical corrosion resistance, and also has the characteristics of resistance to thermal and cold shock. It will not break when heated to above 1000 ℃ in the air, and it will not be broken after rapid cooling and rapid heating. Therefore, the use of silicon nitride ceramics as substrate materials in power modules is of great significance for promoting the application of high-power devices in extreme conditions and complex mechanical environments.

在模块封装技术方面,主要采用表面镀铜技术、直接覆铜工艺及活性金属钎焊工艺。目前,氮化硅陶瓷基板与铜的连接方法主要为活性金属钎焊法,该方法是通过采用熔点比母材低的金属材料作为钎料,将焊接温度加热到高于钎料并低于母材熔点的温度,利用液态钎料中活性元素与母材发生冶金反应从而促使液态钎料润湿母材,从而实现连接的一种方法。In terms of module packaging technology, surface copper plating technology, direct copper cladding technology and active metal brazing technology are mainly used. At present, the connection method between silicon nitride ceramic substrate and copper is mainly active metal brazing method. This method is to use metal material with a lower melting point than the base metal as the brazing filler metal, and heat the welding temperature to a temperature higher than that of the brazing filler metal and lower than that of the mother metal. The temperature of the melting point of the material is a method of using the metallurgical reaction between the active elements in the liquid solder and the base metal to promote the liquid solder to wet the base metal, so as to realize the connection.

然而,现有的活性金属钎焊法存在成本较高、钎料选择范围少的问题,且钎焊过程中液态钎料与母材之间不可避免的发生反应形成界面反应层,该界面反应层以及中间金属间化合物严重影响了基板的热传导性,导致焊后陶瓷-金属复合基板在热循环过程中易于产生开裂问题,这样就严重影响了功率模块的可靠性,因此,本发明提供一种简单高效的氮化硅陶瓷表面改性辅助直接扩散连接方法,解决现有的氮化硅陶瓷基板与铜的连接方法存在的以上技术问题。However, the existing active metal brazing method has the problems of high cost and limited selection of brazing filler metals, and the reaction between the liquid brazing filler metal and the base metal inevitably occurs during the brazing process to form an interface reaction layer. And the intermediate intermetallic compound seriously affects the thermal conductivity of the substrate, causing the ceramic-metal composite substrate to be prone to cracking during the thermal cycle after welding, which seriously affects the reliability of the power module. Therefore, the present invention provides a simple The efficient silicon nitride ceramic surface modification assisted direct diffusion connecting method solves the above technical problems existing in the existing connecting method of silicon nitride ceramic substrate and copper.

发明内容SUMMARY OF THE INVENTION

本发明就是为了解决现有活性金属钎焊法由于该方法成本较高、钎料选择范围较少,且钎焊过程中液态钎料与母材之间不可避免的发生反应形成界面反应层,该界面反应层以及中间金属间化合物严重影响了基板的热传导性,导致焊后陶瓷-金属复合基板在热循环过程中易于产生开裂,严重影响了功率模块的可靠性的技术问题,提供一种利用脉冲激光照射氮化硅陶瓷表面对其进行表面改性预处理,通过改变陶瓷表面微观结构和应力分布状态等特性,实现氮化硅陶瓷基板与铜金属的直接连接,该工艺方法获得的陶瓷-金属复合基板具有高强度、抗冲击能力强、承载电流能力强、导热性好及可靠性高等优点。The present invention is to solve the problem that the existing active metal brazing method has higher cost, less selection range of brazing material, and the inevitable reaction between the liquid brazing material and the base metal during the brazing process to form an interface reaction layer. The interface reaction layer and the intermediate intermetallic compound seriously affect the thermal conductivity of the substrate, which leads to the easy cracking of the ceramic-metal composite substrate after welding during the thermal cycle, which seriously affects the technical problem of the reliability of the power module. The surface of the silicon nitride ceramic is irradiated by laser to carry out surface modification pretreatment, and the direct connection between the silicon nitride ceramic substrate and the copper metal is realized by changing the characteristics of the ceramic surface microstructure and stress distribution state. The ceramic-metal obtained by this process The composite substrate has the advantages of high strength, strong impact resistance, strong current carrying capacity, good thermal conductivity and high reliability.

为此,本发明一种氮化硅陶瓷表面改性辅助直接扩散连接方法,包括以下步骤:To this end, the present invention provides a silicon nitride ceramic surface modification assisted direct diffusion connection method, comprising the following steps:

(1)将氮化硅陶瓷放入丙酮溶液中超声清洗10min-20min,去除表面油污和杂质,然后分别采用600#、1200#、2000#的砂盘对氮化硅陶瓷表面逐级打磨并抛光;(1) Put the silicon nitride ceramics into the acetone solution for ultrasonic cleaning for 10min-20min to remove the surface oil and impurities, and then use 600#, 1200#, 2000# sand discs to grind and polish the surface of the silicon nitride ceramics step by step. ;

(2)将步骤(1)中得到的氮化硅陶瓷放置在加热平台上,在真空或惰性气体保护状态下进行加热,控制加热温度为100℃-300℃,随后将加热后的氮化硅陶瓷置于激光加工平台上,在真空或惰性气体保护状态下对氮化硅陶瓷表面进行激光照射,即实现陶瓷表面的改性;(2) The silicon nitride ceramic obtained in step (1) is placed on a heating platform, heated under vacuum or inert gas protection state, and the heating temperature is controlled to be 100°C-300°C, and then the heated silicon nitride is heated. The ceramic is placed on the laser processing platform, and the surface of the silicon nitride ceramic is irradiated by laser under the protection of vacuum or inert gas, that is, the modification of the ceramic surface is realized;

(3)将金属材料进行机械加工,得到待连接金属材料试样,再将金属材料放入丙酮溶液中超声清洗10min-20min,然后将金属材料的待焊连接面分别采用400#、800#、1200#、2000#的砂纸逐级打磨并抛光;(3) Machining the metal material to obtain a sample of the metal material to be connected, then put the metal material into the acetone solution for ultrasonic cleaning for 10min-20min, and then use 400#, 800#, 400#, 800#, 1200#, 2000# sandpaper is polished and polished step by step;

(4)将步骤(2)中得到的表面改性的氮化硅陶瓷与步骤(3)中得到的金属材料按照陶瓷-金属材料的次序装配并置于真空扩散连接装置中,抽真空,对连接结构加压、加热进行连接,冷却至室温,即实现氮化硅陶瓷与金属材料的直接扩散连接。(4) Assembling the surface-modified silicon nitride ceramic obtained in step (2) and the metal material obtained in step (3) in the order of ceramic-metal material and placing it in a vacuum diffusion connection device, vacuuming, The connection structure is pressurized and heated for connection, and cooled to room temperature, that is, the direct diffusion connection between the silicon nitride ceramic and the metal material is realized.

优选地,步骤(2)中加热温度为100℃-250℃,加热过程在真空或惰性气体保护状态下进行。Preferably, in step (2), the heating temperature is 100°C-250°C, and the heating process is carried out under the protection of vacuum or inert gas.

优选地,步骤(2)中所述激光电流为320A-350A,激光脉宽为1.8ms-2.5ms,激光频率为3Hz-5Hz,激光扫描速度为50mm/min-250mm/min。Preferably, the laser current in step (2) is 320A-350A, the laser pulse width is 1.8ms-2.5ms, the laser frequency is 3Hz-5Hz, and the laser scanning speed is 50mm/min-250mm/min.

优选地,步骤(2)中惰性气体为氦气或者氩气中任意一种作为保护气体。Preferably, in step (2), the inert gas is any one of helium or argon as the protective gas.

优选地,步骤(3)中的金属材料为铜。Preferably, the metal material in step (3) is copper.

优选地,步骤(4)中连接过程中扩散连接装置内真空度为1.5×10-3Pa-6.5×10- 3Pa。Preferably, in the connection process in step (4), the degree of vacuum in the diffusion connection device is 1.5×10 -3 Pa-6.5× 10 -3 Pa.

优选地,步骤(4)中陶瓷和铜的组合件施加的轴向压力为2MPa-5MPa。Preferably, the axial pressure applied by the ceramic and copper composite in step (4) is 2MPa-5MPa.

优选地,步骤(4)中加热过程为,首先控制升温速率为10℃/min-20℃/min升温至750℃并保温10min,然后控制升温速率为5℃/min-10℃/min升温至850℃-1000℃,保温30min-120min,最后再控制5℃/min-10℃/min的冷却速率降温至300℃后随炉冷却。Preferably, in the step (4), the heating process is as follows: firstly, the temperature increase rate is controlled to be 10°C/min-20°C/min to be heated to 750°C and kept for 10 minutes, and then the temperature increase rate is controlled to be 5°C/min-10°C/min and heated to 750°C for 10 minutes. 850℃-1000℃, heat preservation for 30min-120min, and finally control the cooling rate of 5℃/min-10℃/min to cool down to 300℃ and then cool with the furnace.

优选地,步骤(4)中加热过程为,首先控制升温速率为10℃±1℃/min升温至750℃±1℃保温10min,然后控制升温速率为5℃±0.5℃/min升温至900℃,保温60min,最后再控制5℃±0.5℃/min的冷却速率降温至300℃后随炉冷却。Preferably, the heating process in step (4) is as follows: firstly, the temperature increase rate is controlled to be 10°C ± 1°C/min to be heated to 750°C ± 1°C for 10 minutes, and then the temperature increase rate is controlled to be 5°C ± 0.5°C/min to be heated to 900°C , hold for 60min, and finally control the cooling rate of 5℃±0.5℃/min to cool down to 300℃ and then cool with the furnace.

本发明的有益效果是,由于采用脉冲激光对氮化硅陶瓷表面进行改性处理,一方面利用陶瓷表面改性后氮化硅分解形成硅单质,利用硅铜共晶反应形成局部液相从而在较低温度下实现陶瓷与金属的直接连接,减少现有氮化硅陶瓷与金属连接中钎料金属与母材反应形成大量金属间化合物,影响接头的性能;同时由于氮化硅陶瓷表面改性后引起表面微观结构和状态的改变,有效促进了连接过程中原子的扩散以及两种材料的结合,提高了陶瓷与金属之间的连接强度。The beneficial effect of the present invention is that, due to the use of pulsed laser to modify the surface of silicon nitride ceramics, on the one hand, silicon nitride is decomposed to form silicon element after the ceramic surface is modified, and a local liquid phase is formed by silicon-copper eutectic reaction, so that the The direct connection between the ceramic and the metal is realized at a lower temperature, which reduces the reaction between the solder metal and the base metal in the existing silicon nitride ceramic and metal connection to form a large number of intermetallic compounds, which affects the performance of the joint; at the same time, due to the surface modification of the silicon nitride ceramic After that, the surface microstructure and state are changed, which effectively promotes the diffusion of atoms during the connection process and the combination of the two materials, and improves the connection strength between the ceramic and the metal.

附图说明Description of drawings

图1是本发明氮化硅陶瓷表面改性过程示意图;Fig. 1 is the schematic diagram of the surface modification process of silicon nitride ceramics of the present invention;

图2是本发明氮化硅陶瓷表面改性前后的宏观照片和扫描电子显微镜照片;Fig. 2 is the macroscopic photograph and scanning electron microscope photograph before and after the surface modification of silicon nitride ceramics of the present invention;

图3是本发明其中一个实施例的氮化硅陶瓷与金属铜的连接界面扫描电子显微镜照片。FIG. 3 is a scanning electron microscope photograph of the connection interface between silicon nitride ceramics and metallic copper according to one embodiment of the present invention.

具体实施方式Detailed ways

实施例1Example 1

如图1-图3所示,是本实施例的一种氮化硅陶瓷表面改性辅助直接扩散连接方法得出的样品的照片,其中图1是本实施例氮化硅陶瓷表面改性过程示意图,图2是本实施例氮化硅陶瓷表面改性前后的宏观照片和扫描电子显微镜照片,图3是本实施例的氮化硅陶瓷与金属铜的连接界面扫描电子显微镜照片。该实施例一种氮化硅陶瓷表面改性辅助直接扩散连接方法,包括以下步骤:As shown in Figures 1 to 3, it is a photo of a sample obtained by the method of direct diffusion connection assisted by surface modification of silicon nitride ceramics in this embodiment, wherein Figure 1 is the surface modification process of silicon nitride ceramics in this embodiment Schematic diagram, FIG. 2 is a macroscopic photo and a scanning electron microscope photo before and after the surface modification of the silicon nitride ceramic in this embodiment, and FIG. 3 is a scanning electron microscope photo of the connection interface between the silicon nitride ceramic and metallic copper in this embodiment. In this embodiment, a silicon nitride ceramic surface modification assisted direct diffusion connection method includes the following steps:

(1)将氮化硅陶瓷放入丙酮溶液中超声清洗10min-20min,去除表面油污和杂质,然后分别采用600#、1200#、2000#的砂盘对氮化硅陶瓷表面逐级打磨并抛光;(1) Put the silicon nitride ceramics into the acetone solution for ultrasonic cleaning for 10min-20min to remove the surface oil and impurities, and then use 600#, 1200#, 2000# sand discs to grind and polish the surface of the silicon nitride ceramics step by step. ;

(2)将步骤一中得到的氮化硅陶瓷放置加热平台上,在氩气气体保护状态下进行加热,控制加热温度为200℃,随后将加热后的氮化硅陶瓷置于激光加工平台上,在氩气气体保护状态下对氮化硅陶瓷表面进行激光照射,其中激光电流为340A,激光脉宽为1.8ms,激光频率为4Hz,激光扫描速度为100mm/min,即实现陶瓷表面的改性;(2) Place the silicon nitride ceramic obtained in step 1 on a heating platform, heat it under the protection of argon gas, and control the heating temperature to be 200°C, and then place the heated silicon nitride ceramic on the laser processing platform. , under the protection of argon gas, the surface of silicon nitride ceramics is irradiated by laser, the laser current is 340A, the laser pulse width is 1.8ms, the laser frequency is 4Hz, and the laser scanning speed is 100mm/min, that is, the improvement of the ceramic surface is realized. sex;

(3)将金属铜进行机械加工,得到待连接金属材料试样,再将金属铜放入丙酮溶液中超声清洗10min-20min,然后将金属铜的待焊连接面分别采用400#、800#、1200#、2000#的砂纸逐级打磨并抛光;(3) The metal copper is mechanically processed to obtain a sample of the metal material to be connected, and then the metal copper is put into the acetone solution for ultrasonic cleaning for 10min-20min, and then the metal copper joint surfaces to be welded are respectively 400#, 800#, 1200#, 2000# sandpaper is polished and polished step by step;

(4)将步骤(2)中得到的表面改性的氮化硅陶瓷与步骤(3)中得到的金属铜按照陶瓷-金属材料的次序装配并置于真空扩散连接装置中,对陶瓷和铜的组合件施加5MPa的轴向压力,待真空度达到1.5×10-3Pa时进行加热,首先控制升温速率为10℃/min升温至750℃保温10min,然后控制升温速率为5℃/min升温至900℃,保温60min,最后再控制5℃/min的冷却速率降温至300℃后随炉冷却,即实现氮化硅陶瓷与金属铜的直接扩散连接。(4) The surface-modified silicon nitride ceramic obtained in step (2) and the metallic copper obtained in step (3) are assembled in the order of ceramic-metal material and placed in a vacuum diffusion bonding device. The assembly is subjected to an axial pressure of 5MPa, and heated when the vacuum degree reaches 1.5×10 -3 Pa. First, the heating rate is controlled to be 10°C/min to 750°C for 10 minutes, and then the heating rate is controlled to be 5°C/min. To 900 ℃, keep the temperature for 60 minutes, and finally control the cooling rate of 5 ℃/min to cool down to 300 ℃ and then cool with the furnace, that is, to realize the direct diffusion connection between silicon nitride ceramics and metal copper.

本实施例将激光改性技术与瞬时液相扩散连接方法相结合,有效去除了陶瓷表面惰性层并实现了陶瓷表面化学成分及表面状态的改变,同时激光改性促进了扩散连接过程中的原子间的扩散,在较低的温度下实现了陶瓷与金属的高质量连接。In this embodiment, the laser modification technology is combined with the instantaneous liquid phase diffusion connection method, which effectively removes the inert layer on the ceramic surface and realizes the change of the chemical composition and surface state of the ceramic surface. The diffusion between the ceramics and the metal achieves a high-quality connection at a lower temperature.

由于该实施例采用脉冲激光对氮化硅陶瓷表面进行改性处理,一方面利用陶瓷表面改性后氮化硅分解形成硅单质,利用硅铜共晶反应形成局部液相从而在较低温度下实现陶瓷与金属的直接连接,减少现有氮化硅陶瓷与金属连接中钎料金属与母材反应形成大量金属间化合物,影响接头的性能;同时由于氮化硅陶瓷表面改性后引起表面微观结构和状态的改变,有效促进了连接过程中原子的扩散以及两种材料的结合,提高了陶瓷与金属之间的连接强度。In this embodiment, pulsed laser is used to modify the surface of silicon nitride ceramics. On the one hand, silicon nitride is decomposed to form silicon element after the ceramic surface is modified, and a local liquid phase is formed by silicon-copper eutectic reaction, so that at a lower temperature Realize the direct connection between ceramic and metal, and reduce the reaction between the solder metal and the base metal to form a large number of intermetallic compounds in the existing silicon nitride ceramic and metal connection, which affects the performance of the joint; at the same time, the surface microscopic surface is caused by the surface modification of the silicon nitride ceramic. The change of structure and state effectively promotes the diffusion of atoms and the combination of the two materials during the connection process, and improves the connection strength between the ceramic and the metal.

实施例2Example 2

本实施例的一种氮化硅陶瓷表面改性辅助直接扩散连接方法,包括以下步骤:A method for direct diffusion connection assisted by surface modification of silicon nitride ceramics in this embodiment includes the following steps:

(1)将氮化硅陶瓷放入丙酮溶液中超声清洗10min-20min,去除表面油污和杂质,然后分别采用600#、1200#、2000#的砂盘对氮化硅陶瓷表面逐级打磨并抛光;(1) Put the silicon nitride ceramics into the acetone solution for ultrasonic cleaning for 10min-20min to remove the surface oil and impurities, and then use 600#, 1200#, 2000# sand discs to grind and polish the surface of the silicon nitride ceramics step by step. ;

(2)将步骤(1)中得到的氮化硅陶瓷放置加热平台上,在氩气气体保护状态下进行加热,控制加热温度为200℃,随后将加热后的氮化硅陶瓷置于激光加工平台上,在氩气气体保护状态下对氮化硅陶瓷表面进行激光照射,其中激光电流为335A,激光脉宽为1.8ms,激光频率为4Hz,激光扫描速度为80mm/min,即实现陶瓷表面的改性;(2) The silicon nitride ceramic obtained in step (1) is placed on a heating platform, heated under the protection of argon gas, and the heating temperature is controlled to be 200°C, and then the heated silicon nitride ceramic is placed on the laser processing On the platform, the surface of silicon nitride ceramics is irradiated by laser under the protection of argon gas, the laser current is 335A, the laser pulse width is 1.8ms, the laser frequency is 4Hz, and the laser scanning speed is 80mm/min, that is, the ceramic surface is realized. modification;

(3)将金属铜进行机械加工,得到待连接金属材料试样,再将金属铜放入丙酮溶液中超声清洗10min-20min,然后将金属铜的待焊连接面分别采用400#、800#、1200#、2000#的砂纸逐级打磨并抛光;(3) The metal copper is mechanically processed to obtain a sample of the metal material to be connected, and then the metal copper is put into the acetone solution for ultrasonic cleaning for 10min-20min, and then the metal copper joint surfaces to be welded are respectively 400#, 800#, 1200#, 2000# sandpaper is polished and polished step by step;

(4)将步骤(2)中得到的表面改性的氮化硅陶瓷与步骤(3)中得到的金属铜按照陶瓷-金属材料的次序装配并置于真空扩散连接装置中,对陶瓷和铜的组合件施加4MPa的轴向压力,待真空度达到1.5×10-3Pa时进行加热,首先控制升温速率为10℃/min升温至750℃保温10min,然后控制升温速率为5℃/min升温至850℃,保温90min,最后再控制5℃/min的冷却速率降温至300℃后随炉冷却,即实现氮化硅陶瓷与金属铜的直接扩散连接。(4) The surface-modified silicon nitride ceramic obtained in step (2) and the metallic copper obtained in step (3) are assembled in the order of ceramic-metal material and placed in a vacuum diffusion bonding device. The assembly is subjected to an axial pressure of 4MPa, and heated when the degree of vacuum reaches 1.5×10 -3 Pa. First, the heating rate is controlled to be 10°C/min to 750°C for 10 minutes, and then the heating rate is controlled to be 5°C/min. To 850 ℃, keep the temperature for 90 minutes, and finally control the cooling rate of 5 ℃/min to cool down to 300 ℃ and then cool with the furnace, that is, to realize the direct diffusion connection between silicon nitride ceramics and metal copper.

经过试验,该实施例中的部分工艺参数相对于实施例1中的参数进行了调整,也可以达到预期的目标。After experiments, some process parameters in this example have been adjusted relative to those in Example 1, and the expected goal can also be achieved.

实施例3Example 3

本实施例的一种氮化硅陶瓷表面改性辅助直接扩散连接方法,包括以下步骤:A method for direct diffusion connection assisted by surface modification of silicon nitride ceramics in this embodiment includes the following steps:

(1)将氮化硅陶瓷放入丙酮溶液中超声清洗10min-20min,去除表面油污和杂质,然后分别采用600#、1200#、2000#的砂盘对氮化硅陶瓷表面逐级打磨并抛光;(1) Put the silicon nitride ceramics into the acetone solution for ultrasonic cleaning for 10min-20min to remove the surface oil and impurities, and then use 600#, 1200#, 2000# sand discs to grind and polish the surface of the silicon nitride ceramics step by step. ;

(2)将步骤一中得到的氮化硅陶瓷放置加热平台上,在氩气气体保护状态下进行加热,控制加热温度为200℃,随后将加热后的氮化硅陶瓷置于激光加工平台上,在氩气气体保护状态下对氮化硅陶瓷表面进行激光照射,其中激光电流为320A,激光脉宽为1.8ms,激光频率为3Hz,激光扫描速度为200mm/min,即实现陶瓷表面的改性;(2) Place the silicon nitride ceramic obtained in step 1 on a heating platform, heat it under the protection of argon gas, and control the heating temperature to be 200°C, and then place the heated silicon nitride ceramic on the laser processing platform. , Under the protection of argon gas, the surface of silicon nitride ceramics is irradiated by laser, the laser current is 320A, the laser pulse width is 1.8ms, the laser frequency is 3Hz, and the laser scanning speed is 200mm/min, that is, the improvement of the ceramic surface is realized. sex;

(3)将金属铜进行机械加工,得到待连接金属材料试样,再将金属铜放入丙酮溶液中超声清洗10min-20min,然后将金属铜的待焊连接面分别采用400#、800#、1200#、2000#的砂纸逐级打磨并抛光;(3) The metal copper is mechanically processed to obtain a sample of the metal material to be connected, and then the metal copper is put into the acetone solution for ultrasonic cleaning for 10min-20min, and then the metal copper joint surfaces to be welded are respectively 400#, 800#, 1200#, 2000# sandpaper is polished and polished step by step;

(4)将步骤二中得到的表面改性的氮化硅陶瓷与步骤三中得到的金属铜按照陶瓷-金属材料的次序装配并置于真空扩散连接装置中,对陶瓷和铜的组合件施加2MPa的轴向压力,待真空度达到5×10-3Pa时进行加热,首先控制升温速率为10℃/min升温至750℃保温10min,然后控制升温速率为5℃/min升温至900℃,保温60min,最后再控制5℃/min的冷却速率降温至300℃后随炉冷却,即实现氮化硅陶瓷与金属铜的直接扩散连接。(4) Assemble the surface-modified silicon nitride ceramic obtained in step 2 and the metallic copper obtained in step 3 in the order of ceramic-metal material and place them in a vacuum diffusion bonding device, and apply The axial pressure of 2MPa is heated when the vacuum degree reaches 5×10 -3 Pa. First, the heating rate is controlled to be 10°C/min to 750°C for 10 minutes, and then the temperature rise rate is controlled to be 5°C/min to be heated to 900°C. Hold for 60 minutes, and finally control the cooling rate of 5 °C/min to cool down to 300 °C and then cool with the furnace, that is, to realize the direct diffusion connection between silicon nitride ceramics and metal copper.

经过试验,该实施例中的部分工艺参数相对于实施例1中的参数进行了调整,也可以达到预期的目标。After experiments, some process parameters in this example have been adjusted relative to those in Example 1, and the expected goal can also be achieved.

实施例4Example 4

本实施例的一种氮化硅陶瓷表面改性辅助直接扩散连接方法,包括以下步骤:A method for direct diffusion connection assisted by surface modification of silicon nitride ceramics in this embodiment includes the following steps:

(1)将氮化硅陶瓷放入丙酮溶液中超声清洗10min-20min,去除表面油污和杂质,然后分别采用600#、1200#、2000#的砂盘对氮化硅陶瓷表面逐级打磨并抛光;(1) Put the silicon nitride ceramics into the acetone solution for ultrasonic cleaning for 10min-20min to remove the surface oil and impurities, and then use 600#, 1200#, 2000# sand discs to grind and polish the surface of the silicon nitride ceramics step by step. ;

(2)将步骤(1)中得到的氮化硅陶瓷放置加热平台上,在氩气气体保护状态下进行加热,控制加热温度为200℃,随后将加热后的氮化硅陶瓷置于激光加工平台上,在氩气气体保护状态下对氮化硅陶瓷表面进行激光照射,其中激光电流为340A,激光脉宽为4ms,激光频率为4Hz,激光扫描速度为100mm/min,即实现陶瓷表面的改性;(2) The silicon nitride ceramic obtained in step (1) is placed on a heating platform, heated under the protection of argon gas, and the heating temperature is controlled to be 200°C, and then the heated silicon nitride ceramic is placed on the laser processing On the platform, the surface of silicon nitride ceramics is irradiated by laser under the protection of argon gas, where the laser current is 340A, the laser pulse width is 4ms, the laser frequency is 4Hz, and the laser scanning speed is 100mm/min, that is, the ceramic surface is irradiated. modified;

(3)将金属铜进行机械加工,得到待连接金属材料试样,再将金属铜放入丙酮溶液中超声清洗10min-20min,然后将金属铜的待焊连接面分别采用400#、800#、1200#、2000#的砂纸逐级打磨并抛光;(3) The metal copper is mechanically processed to obtain a sample of the metal material to be connected, and then the metal copper is put into the acetone solution for ultrasonic cleaning for 10min-20min, and then the metal copper joint surfaces to be welded are respectively 400#, 800#, 1200#, 2000# sandpaper is polished and polished step by step;

(4)将步骤(2)中得到的表面改性的氮化硅陶瓷与步骤(3)中得到的金属铜按照陶瓷-金属材料的次序装配并置于真空扩散连接装置中,对陶瓷和铜的组合件施加5MPa的轴向压力,待真空度达到5×10-3Pa时进行加热,首先控制升温速率为10℃/min升温至750℃保温10min,然后控制升温速率为5℃/min升温至950℃,保温30min,最后再控制5℃/min的冷却速率降温至300℃后随炉冷却,即实现氮化硅陶瓷与金属铜的直接扩散连接。(4) The surface-modified silicon nitride ceramic obtained in step (2) and the metallic copper obtained in step (3) are assembled in the order of ceramic-metal material and placed in a vacuum diffusion bonding device. The assembly is subjected to an axial pressure of 5MPa, and heated when the degree of vacuum reaches 5×10 -3 Pa. First, the heating rate is controlled to be 10°C/min to 750°C for 10 minutes, and then the heating rate is controlled to be 5°C/min. To 950 ℃, keep the temperature for 30 minutes, and finally control the cooling rate of 5 ℃/min to cool down to 300 ℃ and then cool with the furnace, that is, to realize the direct diffusion connection between silicon nitride ceramics and metal copper.

经过试验,该实施例中的部分工艺参数相对于实施例1中的参数进行了调整,也可以达到预期的目标。After experiments, some process parameters in this example have been adjusted relative to those in Example 1, and the expected goal can also be achieved.

实施例5Example 5

本实施例的一种氮化硅陶瓷表面改性辅助直接扩散连接方法,包括以下步骤:A method for direct diffusion connection assisted by surface modification of silicon nitride ceramics in this embodiment includes the following steps:

(1)将氮化硅陶瓷放入丙酮溶液中超声清洗10min-20min,去除表面油污和杂质,然后分别采用600#、1200#、2000#的砂盘对氮化硅陶瓷表面逐级打磨并抛光;(1) Put the silicon nitride ceramics into the acetone solution for ultrasonic cleaning for 10min-20min to remove the surface oil and impurities, and then use 600#, 1200#, 2000# sand discs to grind and polish the surface of the silicon nitride ceramics step by step. ;

(2)将步骤一中得到的氮化硅陶瓷放置加热平台上,在氩气气体保护状态下进行加热,控制加热温度为200℃,随后将加热后的氮化硅陶瓷置于激光加工平台上,在氩气气体保护状态下对氮化硅陶瓷表面进行激光照射,其中激光电流为340A,激光脉宽为1.8ms,激光频率为4Hz,激光扫描速度为200mm/min,即实现陶瓷表面的改性;(2) Place the silicon nitride ceramic obtained in step 1 on a heating platform, heat it under the protection of argon gas, and control the heating temperature to be 200°C, and then place the heated silicon nitride ceramic on the laser processing platform. , Under the protection of argon gas, the surface of silicon nitride ceramics is irradiated by laser, the laser current is 340A, the laser pulse width is 1.8ms, the laser frequency is 4Hz, and the laser scanning speed is 200mm/min, that is, the improvement of the ceramic surface is realized. sex;

(3)将金属铜进行机械加工,得到待连接金属材料试样,再将金属铜放入丙酮溶液中超声清洗10min-20min,然后将金属铜的待焊连接面分别采用400#、800#、1200#、2000#的砂纸逐级打磨并抛光;(3) The metal copper is mechanically processed to obtain a sample of the metal material to be connected, and then the metal copper is put into the acetone solution for ultrasonic cleaning for 10min-20min, and then the metal copper joint surfaces to be welded are respectively 400#, 800#, 1200#, 2000# sandpaper is polished and polished step by step;

(4)将步骤(2)中得到的表面改性的氮化硅陶瓷与步骤(3)中得到的金属铜按照陶瓷-金属材料的次序装配并置于真空扩散连接装置中,对陶瓷和铜的组合件施加5MPa的轴向压力,待真空度达到5×10-3Pa时进行加热,首先控制升温速率为10℃/min升温至750℃保温10min,然后控制升温速率为5℃/min升温至840℃,保温120min,最后再控制5℃/min的冷却速率降温至300℃后随炉冷却,即实现氮化硅陶瓷与金属铜的直接扩散连接。(4) The surface-modified silicon nitride ceramic obtained in step (2) and the metallic copper obtained in step (3) are assembled in the order of ceramic-metal material and placed in a vacuum diffusion bonding device. The assembly is subjected to an axial pressure of 5MPa, and heated when the degree of vacuum reaches 5×10 -3 Pa. First, the heating rate is controlled to be 10°C/min to 750°C for 10 minutes, and then the heating rate is controlled to be 5°C/min. To 840 ℃, hold the temperature for 120 minutes, and finally control the cooling rate of 5 ℃/min to cool down to 300 ℃ and then cool with the furnace, that is, to realize the direct diffusion connection between silicon nitride ceramics and metal copper.

实施例6Example 6

本实施例的一种氮化硅陶瓷表面改性辅助直接扩散连接方法,包括以下步骤:A method for direct diffusion connection assisted by surface modification of silicon nitride ceramics in this embodiment includes the following steps:

(1)将氮化硅陶瓷放入丙酮溶液中超声清洗10min-20min,去除表面油污和杂质,然后分别采用600#、1200#、2000#的砂盘对氮化硅陶瓷表面逐级打磨并抛光;(1) Put the silicon nitride ceramics into the acetone solution for ultrasonic cleaning for 10min-20min to remove the surface oil and impurities, and then use 600#, 1200#, 2000# sand discs to grind and polish the surface of the silicon nitride ceramics step by step. ;

(2)将步骤(1)中得到的氮化硅陶瓷放置加热平台上,在氩气气体保护状态下进行加热,控制加热温度为200℃,随后将加热后的氮化硅陶瓷置于激光加工平台上,在氩气气体保护状态下对氮化硅陶瓷表面进行激光照射,其中激光电流为340A,激光脉宽为4ms,激光频率为4Hz,激光扫描速度为100mm/min,即实现陶瓷表面的改性;(2) The silicon nitride ceramic obtained in step (1) is placed on a heating platform, heated under the protection of argon gas, and the heating temperature is controlled to be 200°C, and then the heated silicon nitride ceramic is placed on the laser processing On the platform, the surface of silicon nitride ceramics is irradiated by laser under the protection of argon gas, where the laser current is 340A, the laser pulse width is 4ms, the laser frequency is 4Hz, and the laser scanning speed is 100mm/min, that is, the ceramic surface is irradiated. modified;

(3)将金属铜进行机械加工,得到待连接金属材料试样,再将金属铜放入丙酮溶液中超声清洗10min-20min,然后将金属铜的待焊连接面分别采用400#、800#、1200#、2000#的砂纸逐级打磨并抛光;(3) The metal copper is mechanically processed to obtain a sample of the metal material to be connected, and then the metal copper is put into the acetone solution for ultrasonic cleaning for 10min-20min, and then the metal copper joint surfaces to be welded are respectively 400#, 800#, 1200#, 2000# sandpaper is polished and polished step by step;

(4)将步骤(2)中得到的表面改性的氮化硅陶瓷与步骤(3)中得到的金属铜按照陶瓷-金属材料的次序装配并置于真空扩散连接装置中,对陶瓷和铜的组合件施加2MPa的轴向压力,待真空度达到5×10-3Pa时进行加热,首先控制升温速率为10℃/min升温至750℃保温10min,然后控制升温速率为5℃/min升温至1000℃,保温60min,最后再控制5℃/min的冷却速率降温至300℃后随炉冷却,即实现氮化硅陶瓷与金属铜的直接扩散连接。(4) The surface-modified silicon nitride ceramic obtained in step (2) and the metallic copper obtained in step (3) are assembled in the order of ceramic-metal material and placed in a vacuum diffusion bonding device. The assembly is subjected to an axial pressure of 2MPa, and heated when the vacuum degree reaches 5×10 -3 Pa. First, control the heating rate to be 10°C/min to 750°C for 10 minutes, and then control the heating rate to 5°C/min. To 1000 ℃, hold for 60 minutes, and finally control the cooling rate of 5 ℃/min to cool down to 300 ℃ and then cool with the furnace, that is, to realize the direct diffusion connection between silicon nitride ceramics and metal copper.

实施例7Example 7

本实施例的一种氮化硅陶瓷表面改性辅助直接扩散连接方法,包括以下步骤:A method for direct diffusion connection assisted by surface modification of silicon nitride ceramics in this embodiment includes the following steps:

(1)将氮化硅陶瓷放入丙酮溶液中超声清洗10min-20min,去除表面油污和杂质,然后分别采用600#、1200#、2000#的砂盘对氮化硅陶瓷表面逐级打磨并抛光;(1) Put the silicon nitride ceramics into the acetone solution for ultrasonic cleaning for 10min-20min to remove the surface oil and impurities, and then use 600#, 1200#, 2000# sand discs to grind and polish the surface of the silicon nitride ceramics step by step. ;

(2)将步骤(1)中得到的氮化硅陶瓷放置加热平台上,在真空状态下进行加热,控制加热温度为150℃,随后将加热后的氮化硅陶瓷置于激光加工平台上,在真空状态下对氮化硅陶瓷表面进行激光照射,其中激光电流为345A,激光脉宽为1.8ms,激光频率为4Hz,激光扫描速度为100mm/min,即实现陶瓷表面的改性;(2) placing the silicon nitride ceramic obtained in step (1) on a heating platform, heating in a vacuum state, and controlling the heating temperature to be 150° C., and then placing the heated silicon nitride ceramic on a laser processing platform, The surface of the silicon nitride ceramics is irradiated with laser light in a vacuum state, the laser current is 345A, the laser pulse width is 1.8ms, the laser frequency is 4Hz, and the laser scanning speed is 100mm/min, that is, the modification of the ceramic surface is realized;

(3)将金属铜进行机械加工,得到待连接金属材料试样,再将金属铜放入丙酮溶液中超声清洗10min-20min,然后将金属铜的待焊连接面分别采用400#、800#、1200#、2000#的砂纸逐级打磨并抛光;(3) The metal copper is mechanically processed to obtain a sample of the metal material to be connected, and then the metal copper is put into the acetone solution for ultrasonic cleaning for 10min-20min, and then the metal copper joint surfaces to be welded are respectively 400#, 800#, 1200#, 2000# sandpaper is polished and polished step by step;

(4)将步骤(2)中得到的表面改性的氮化硅陶瓷与步骤(3)中得到的金属铜按照陶瓷-金属材料的次序装配并置于真空扩散连接装置中,对陶瓷和铜的组合件施加5MPa的轴向压力,待真空度达到1.5×10-3Pa时进行加热,首先控制升温速率为10℃/min升温至750℃保温10min,然后控制升温速率为5℃/min升温至880℃,保温60min,最后再控制5℃/min的冷却速率降温至300℃后随炉冷却,即实现氮化硅陶瓷与金属铜的直接扩散连接。(4) The surface-modified silicon nitride ceramic obtained in step (2) and the metallic copper obtained in step (3) are assembled in the order of ceramic-metal material and placed in a vacuum diffusion bonding device. The assembly is subjected to an axial pressure of 5MPa, and heated when the vacuum degree reaches 1.5×10 -3 Pa. First, the heating rate is controlled to be 10°C/min to 750°C for 10 minutes, and then the heating rate is controlled to be 5°C/min. To 880 ℃, hold the temperature for 60 minutes, and finally control the cooling rate of 5 ℃/min to cool down to 300 ℃ and then cool with the furnace, that is, to realize the direct diffusion connection between silicon nitride ceramics and metal copper.

本发明技术方案不局限于以上所举例的具体实施方式,还包括各具体实施方式之间的任意组合,以上实施例由于采用脉冲激光对氮化硅陶瓷表面进行改性处理,一方面利用陶瓷表面改性后氮化硅分解形成硅单质,利用硅铜共晶反应形成局部液相从而在较低温度下实现陶瓷与金属的直接连接,减少现有氮化硅陶瓷与金属连接中钎料金属与母材反应形成大量金属间化合物,影响接头的性能;同时由于氮化硅陶瓷表面改性后引起表面微观结构和状态的改变,有效促进了连接过程中原子的扩散以及两种材料的结合,提高了陶瓷与金属之间的连接强度。The technical solution of the present invention is not limited to the specific embodiments exemplified above, but also includes any combination of specific embodiments. The above embodiments use pulsed lasers to modify the surface of silicon nitride ceramics, on the one hand, use the ceramic surface After modification, silicon nitride is decomposed to form silicon element, and the silicon-copper eutectic reaction is used to form a local liquid phase, so as to realize the direct connection between ceramic and metal at a lower temperature, and reduce the solder metal and metal in the existing silicon nitride ceramic and metal connection. The base metal reacts to form a large number of intermetallic compounds, which affect the performance of the joint; at the same time, due to the change of the surface microstructure and state after the surface modification of the silicon nitride ceramic, it effectively promotes the diffusion of atoms and the combination of the two materials during the connection process. The strength of the connection between ceramic and metal.

Claims (9)

1.一种氮化硅陶瓷表面改性辅助直接扩散连接方法,其特征是包括以下步骤:1. a silicon nitride ceramic surface modification assistant direct diffusion connecting method is characterized in that comprising the following steps: (1)将氮化硅陶瓷放入丙酮溶液中超声清洗10min-20min,去除表面油污和杂质,然后分别采用600#、1200#、2000#的砂盘对氮化硅陶瓷表面逐级打磨并抛光;(1) Put the silicon nitride ceramics into the acetone solution for ultrasonic cleaning for 10min-20min to remove the surface oil and impurities, and then use 600#, 1200#, 2000# sand discs to grind and polish the surface of the silicon nitride ceramics step by step. ; (2)将步骤(1)中得到的氮化硅陶瓷放置在加热平台上,在真空或惰性气体保护状态下进行加热,控制加热温度为100℃-300℃,随后将加热后的氮化硅陶瓷置于激光加工平台上,在真空或惰性气体保护状态下对氮化硅陶瓷表面进行激光照射,即实现陶瓷表面的改性;(2) The silicon nitride ceramic obtained in step (1) is placed on a heating platform, heated under vacuum or inert gas protection state, and the heating temperature is controlled to be 100°C-300°C, and then the heated silicon nitride is heated. The ceramic is placed on the laser processing platform, and the surface of the silicon nitride ceramic is irradiated by laser under the protection of vacuum or inert gas, that is, the modification of the ceramic surface is realized; (3)将金属材料进行机械加工,得到待连接金属材料试样,再将金属材料放入丙酮溶液中超声清洗10min-20min,然后将金属材料的待焊连接面分别采用400#、800#、1200#、2000#的砂纸逐级打磨并抛光;(3) Machining the metal material to obtain a sample of the metal material to be connected, then put the metal material into the acetone solution for ultrasonic cleaning for 10min-20min, and then use 400#, 800#, 400#, 800#, 1200#, 2000# sandpaper is polished and polished step by step; (4)将步骤(2)中得到的表面改性的氮化硅陶瓷与步骤(3)中得到的金属材料按照陶瓷-金属材料的次序装配并置于真空扩散连接装置中,抽真空,对连接结构加压、加热进行连接,冷却至室温,即实现氮化硅陶瓷与金属材料的直接扩散连接。(4) Assembling the surface-modified silicon nitride ceramic obtained in step (2) and the metal material obtained in step (3) in the order of ceramic-metal material and placing it in a vacuum diffusion connection device, vacuuming, The connection structure is pressurized and heated for connection, and cooled to room temperature, that is, the direct diffusion connection between the silicon nitride ceramic and the metal material is realized. 2.根据权利要求1所述的氮化硅陶瓷表面改性辅助直接扩散连接方法,其特征在于:所述步骤(2)中加热温度为100℃-250℃,加热过程在真空或惰性气体保护状态下进行。2. The silicon nitride ceramic surface modification-assisted direct diffusion bonding method according to claim 1, characterized in that: in the step (2), the heating temperature is 100°C-250°C, and the heating process is protected by vacuum or inert gas. state. 3.根据权利要求1所述的氮化硅陶瓷表面改性辅助直接扩散连接方法,其特征在于:所述步骤(2)中所述激光电流为320A-350A,激光脉宽为1.8ms-2.5ms,激光频率为3Hz-5Hz,激光扫描速度为50mm/min-250mm/min。3. The silicon nitride ceramic surface modification-assisted direct diffusion connection method according to claim 1, wherein the laser current in the step (2) is 320A-350A, and the laser pulse width is 1.8ms-2.5 ms, the laser frequency is 3Hz-5Hz, and the laser scanning speed is 50mm/min-250mm/min. 4.根据权利要求1所述的氮化硅陶瓷表面改性辅助直接扩散连接方法,其特征在于:所述步骤(2)中惰性气体为氦气或者氩气中任意一种作为保护气体。4 . The method for surface modification assisted direct diffusion connection of silicon nitride ceramics according to claim 1 , wherein in the step (2), the inert gas is any one of helium or argon as the protective gas. 5 . 5.根据权利要求1所述的氮化硅陶瓷表面改性辅助直接扩散连接方法,其特征在于:所述步骤(3)中的金属材料为铜。5 . The method of claim 1 , wherein the metal material in the step (3) is copper. 6 . 6.根据权利要求1所述的氮化硅陶瓷表面改性辅助直接扩散连接方法,其特征在于:所述步骤(4)中连接过程中扩散连接装置内真空度为1.5×10-3Pa-6.5×10-3Pa。6 . The method for assisted direct diffusion bonding by surface modification of silicon nitride ceramics according to claim 1 , wherein the vacuum degree in the diffusion bonding device during the connecting process in the step (4) is 1.5×10 -3 Pa- 6.5×10 -3 Pa. 7.根据权利要求1所述的氮化硅陶瓷表面改性辅助直接扩散连接方法,其特征在于:所述步骤(4)中陶瓷和铜的组合件施加的轴向压力为2MPa-5MPa。7 . The method for assisted direct diffusion bonding of silicon nitride ceramic surface modification according to claim 1 , wherein in the step (4), the axial pressure exerted by the ceramic and copper assembly is 2MPa-5MPa. 8 . 8.根据权利要求1所述的氮化硅陶瓷表面改性辅助直接扩散连接方法,其特征在于:所述步骤(4)中加热过程为,首先控制升温速率为10℃/min-20℃/min升温至750℃并保温10min,然后控制升温速率为5℃/min-10℃/min升温至850℃-1000℃,保温30min-120min,最后再控制5℃/min-10℃/min的冷却速率降温至300℃后随炉冷却。8. The silicon nitride ceramic surface modification-assisted direct diffusion bonding method according to claim 1, characterized in that: in the step (4), the heating process is, firstly, the heating rate is controlled to be 10°C/min-20°C/ Min heating up to 750°C and holding for 10min, then control the heating rate to 5°C/min-10°C/min, heat up to 850°C-1000°C, hold for 30min-120min, and finally control the cooling at 5°C/min-10°C/min The rate is cooled to 300 ℃ and then cooled with the furnace. 9.根据权利要求1所述的氮化硅陶瓷表面改性辅助直接扩散连接方法,其特征在于:所述步骤(4)中加热过程为,首先控制升温速率为10℃±1℃/min升温至750℃±1℃保温10min,然后控制升温速率为5℃±0.5℃/min升温至900℃,保温60min,最后再控制5℃±0.5℃/min的冷却速率降温至300℃后随炉冷却。9. The silicon nitride ceramic surface modification-assisted direct diffusion bonding method according to claim 1, characterized in that: in the step (4), the heating process is, firstly, the temperature increase rate is controlled to be 10°C ± 1°C/min. Keep the temperature at 750℃±1℃ for 10min, then control the heating rate to be 5℃±0.5℃/min, heat up to 900℃, keep the temperature for 60min, and finally control the cooling rate of 5℃±0.5℃/min to cool down to 300℃ and then cool with the furnace .
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