WO2023065666A1 - Preparation method for nanowire silver film for packaging and interconnection of large-size power semiconductor integrated circuit - Google Patents

Preparation method for nanowire silver film for packaging and interconnection of large-size power semiconductor integrated circuit Download PDF

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WO2023065666A1
WO2023065666A1 PCT/CN2022/095116 CN2022095116W WO2023065666A1 WO 2023065666 A1 WO2023065666 A1 WO 2023065666A1 CN 2022095116 W CN2022095116 W CN 2022095116W WO 2023065666 A1 WO2023065666 A1 WO 2023065666A1
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silver
nanowire
film
preparation
mother liquor
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PCT/CN2022/095116
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French (fr)
Chinese (zh)
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余翠娟
叶益聪
堵永国
王震
彭泳潜
倪子琪
徐元曦
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国防科技大学
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00

Definitions

  • the invention relates to the technical field of electronic packaging, in particular to a method for preparing a nanowire silver film for packaging and interconnecting large-scale power semiconductor integrated circuits.
  • Nano-silver films on the market are mostly prepared by nano-silver particles, and the film-forming property of particle raw materials is poor.
  • organic substances such as film-forming agents and dispersants need to be added, and films are prepared by casting methods, coating methods and other processes.
  • the content of nano-silver particles in the silver film is as high as 99%, the content of organic matter is still relatively high, about 1%.
  • the silver film prepared by nano-silver particles has shortcomings in terms of process adaptability and performance in the packaging and interconnection process.
  • the silver film transfer process is complicated and requires special equipment for implementation: the strength of the nano-particle silver film is very low and cannot be transferred directly.
  • To the surface of the chip or substrate it is usually necessary to attach the chip to the silver film with custom-made equipment, perform pre-sintering to realize the initial bonding of the chip and the silver film, and then transfer it to the substrate for hot-press sintering to obtain the chip and the silver film.
  • the thermal conductivity and connection strength of the packaging interconnection layer are low.
  • the remaining organic matter in the sintered layer of the silver film is difficult to remove during the hot-pressing sintering process of the packaging interconnection, and the silver nanoparticles are almost in point contact, and the sintered layer will form more interfaces and pores.
  • the microstructure characteristics of the silver film sintered layer are not conducive to the improvement of the thermal conductivity, electrical conductivity and connection strength of the film layer, and it is difficult to meet the requirements of high thermal conductivity and high connection strength for packaging and interconnection of
  • the invention provides a method for preparing a nanowire silver film for encapsulation and interconnection of large-scale power semiconductor integrated circuits, which is used to overcome defects such as insufficient process adaptability and service performance in the prior art.
  • the present invention proposes a method for preparing a nanowire silver film for encapsulating and interconnecting large-scale power semiconductor integrated circuits, comprising the following steps:
  • the beneficial effect of the present invention has:
  • the preparation method of the nanowire silver film for encapsulation and interconnection of large-scale power semiconductor integrated circuits requires large-scale equipment such as casting machines and coating machines compared to the nanoparticle silver film, and the nanowire silver film only needs to be pressed. Filtration or suction filtration is enough, the equipment and process are simple, the performance is stable, and it can be mass-produced.
  • the content of organic matter in the nanowire silver film is lower (less than 0.3%), and the hot-pressed sintering layer of the nanowire silver film has less residual carbon, lower porosity, high thermal conductivity, and better electrical conductivity.
  • the connection strength is higher.
  • the silver film sintering layer has a porous structure, and the porous silver film structure can buffer the stress generated during sintering and improve the reliability of the device. That is, the microstructure of the nanowire silver film prepared by the present invention can reduce the thermomechanical stress caused by the thermal mismatch between the chip and the substrate, and improve the reliability of the device during service.
  • Fig. 1 is the scanning electron micrograph of silver nanowire in embodiment 1;
  • Fig. 2 is the scanning electron micrograph of nanowire silver film in embodiment 1;
  • FIG. 3 is a physical diagram of the nanowire silver film in Example 1.
  • the present invention proposes a method for preparing a nanowire silver film for encapsulating and interconnecting large-scale power semiconductor integrated circuits, comprising the following steps:
  • step S1 the dilution is specifically:
  • the silver nanowire mother liquor is diluted 2 to 20 times with a diluent.
  • the purpose of dilution is to dissolve the organic matter coated on the surface of the silver nanowires into diluents such as water and ethanol to achieve the purpose of purification.
  • the diluent is ethanol, deionized water or other alcoholic low-boiling organic solvents.
  • the surface of the silver nanowires prepared by the alcohol thermal method is coated with a layer of organic matter, which can be alcohol-soluble or water-soluble. Subsequent pressure filtration requires low-temperature drying after film formation, so water or low-boiling point alcohol solvents must be used.
  • step S1 the purification is specifically:
  • the diluted silver nanowire mother liquor is placed in a 30-60° C. water bath and stirred for 0.5-2 hours to obtain a silver nanowire dispersion.
  • the principle of purification is that the organic matter on the surface of silver nanowires can be dissolved in water or alcohol, and by adding a sufficient amount of diluent, the organic matter coating layer on the surface of silver nanowires can be thinned until there is no more.
  • the purpose of purification is that the organic coating layer on the surface of silver nanowires will affect the electrical and thermal conductivity of the packaged device, and it must be cleaned to meet the requirements of high-power devices.
  • the pressure of the pressure filtration or suction filtration is 0.5-2 MPa.
  • the purpose of pressure filtration or suction filtration is to extract the silver nanowires in the mother liquor, the solid silver nanowires are left on the pressure filtration membrane or suction filtration membrane, and other liquid substances are filtered out through the pressure filtration membrane or suction filtration membrane to achieve The purpose of solid-liquid separation.
  • the size of silver nanowires is small, as low as 20nm, and the pressure of pressure filtration or suction filtration is small, and it is difficult for the mother liquor to pass through the pressure filtration membrane or suction filtration membrane, and the purpose of solid-liquid separation cannot be achieved.
  • the pressure filter membrane or suction filter membrane made of organic material will rupture.
  • step S3 the drying is specifically:
  • nanowire silver film transferring the wet nanowire silver film to a plastic film, and drying at 40-80° C. for 1-3 hours to obtain the nanowire silver film.
  • the reason for the transfer to plastic film is that the thickness of nano-silver film is very small, generally 30-70 ⁇ m, and its strength is very low. It needs to be placed on a carrier to facilitate transportation and use.
  • the plastic film is one of polyethylene, polypropylene, polyvinyl chloride, polystyrene and polyethylene terephthalate.
  • Different plastic materials have different surface tensions and have different adsorption forces to nanowire wet films. If the tension is too large, the silver film is easy to transfer; if the tension is too small, the adsorption force between the silver film and the plastic film is large, and the water or alcohol solvent between the films is not easy to volatilize during drying.
  • the nanowire silver film has a thickness of 30-70 ⁇ m, and the content of impurities such as organic matter is less than 0.3%.
  • the silver nanowires in the silver nanowire mother liquor have a diameter of 20-200 nm and a length of 5-50 ⁇ m.
  • the preparation method of the nanowire silver film for encapsulation and interconnection of high-power semiconductor integrated circuits provided by the invention adopts the silver nanowire to prepare the silver film.
  • the silver nanowire has a small diameter, has a low melting point effect, and can be sintered by low-temperature hot pressing.
  • the melting point of the sintered body (film layer) is close to that of bulk silver (961°C), and it can be used at high temperature, with good thermal and electrical conductivity and high shear strength.
  • the preparation method provided by the present invention uses silver nanowires to prepare films, the length of the silver nanowires is 5-50 ⁇ m, and the silver nanowires are interspersed and overlapped, making it easier to form a film, the structural integrity of the silver film is good, and the thickness is thinner and uniform controllable.
  • the silver nanowire mother liquor is prepared by a conventional alcohol thermal method; the mass fraction of the silver nanowire in the silver nanowire mother liquor is 0.5-0.6%.
  • Example 1 the mass fraction of the silver nanowire in the silver nanowire mother liquor is 0.5-0.6%.
  • This embodiment provides a method for preparing a nanowire silver film for encapsulation and interconnection of large-scale power semiconductor integrated circuits, including the following steps:
  • a silver nanowire mother liquor is prepared by a conventional alcohol-thermal method.
  • the silver nanowire in the silver nanowire mother liquor is shown in FIG. 1 , with a diameter of 100-150 nm and a length of 25-35 ⁇ m.
  • the beaker was placed in a 30°C water bath and stirred for 2 hours at a stirring speed of 500r/min to obtain a silver nanowire dispersion.
  • the filter press membrane in this embodiment is a hydrophilic polytetrafluoroethylene microporous filter membrane with a pore size of 0.45 ⁇ m.
  • the carrier of the wet nanowire silver film is a polyethylene terephthalate film.
  • the nanowire silver film prepared by this embodiment has a thickness of 45 ⁇ m and an organic matter content of 0.22%.
  • This embodiment provides a method for preparing a nanowire silver film for encapsulation and interconnection of large-scale power semiconductor integrated circuits, including the following steps:
  • a silver nanowire mother liquor is prepared by a conventional alcohol-thermal method, and the silver nanowire mother liquor has a diameter of 50-80 nm and a length of 20-33 ⁇ m.
  • the beaker was placed in a water bath at 50° C. and stirred for 0.5 h at a stirring speed of 500 r/min to obtain a silver nanowire dispersion.
  • the filter press membrane in this embodiment is a hydrophilic polytetrafluoroethylene microporous filter membrane with a pore size of 1 ⁇ m.
  • the carrier of the wet nanowire silver film is a polypropylene plastic film.
  • S3 Put the wet silver nanowire film in a vacuum oven at 50°C to dry for 1 hour to obtain a silver nanowire film.
  • the silver nanowire film has good structural integrity, and the silver nanowires in the silver nanowire film are interspersed and overlapped. catch.
  • the thickness of the silver film of silver nanowires prepared in this example is 57 ⁇ m, and the content of organic matter is 0.24%.
  • This embodiment provides a method for preparing a nanowire silver film for encapsulation and interconnection of large-scale power semiconductor integrated circuits, including the following steps:
  • a silver nanowire mother liquor is prepared by a conventional alcohol-thermal method, and the silver nanowire mother liquor has a diameter of 160-200 nm and a length of 5-18 ⁇ m.
  • the beaker was placed in a 60° C. water bath and stirred for 0.7 h at a stirring speed of 500 r/min to obtain a silver nanowire dispersion.
  • the filter press membrane in this embodiment is a hydrophilic polytetrafluoroethylene microporous filter membrane with a pore size of 1 ⁇ m.
  • the carrier of the wet nanowire silver film is a polystyrene film.
  • S3 Put the wet silver nanowire film in a vacuum oven at 80°C for 1.2 hours to dry to obtain a silver nanowire film.
  • the silver nanowire film has good structural integrity, and the silver nanowires in the silver nanowire film are interspersed with each other. lap.
  • the thickness of the silver film of silver nanowires prepared in this embodiment is 30 ⁇ m, and the content of organic matter is 0.21%.
  • This embodiment provides a method for preparing a nanowire silver film for encapsulation and interconnection of large-scale power semiconductor integrated circuits, including the following steps:
  • a silver nanowire mother liquor is prepared by a conventional alcohol-thermal method, and the silver nanowire mother liquor has a diameter of 20-45 nm and a length of 35-50 ⁇ m.
  • the beaker was placed in a 40° C. water bath and stirred for 2 hours at a stirring speed of 500 r/min to obtain a silver nanowire dispersion.
  • the filter press membrane in this embodiment is a hydrophilic polytetrafluoroethylene microporous filter membrane with a pore size of 0.5 ⁇ m.
  • the carrier of the wet nanowire silver film is a polystyrene film.
  • S3 Put the wet silver nanowire film in a vacuum oven at 70°C for 2.1 hours to dry to obtain a silver nanowire film.
  • the silver nanowire film has good structural integrity, and the silver nanowires in the silver nanowire film are interspersed with each other. lap.
  • the thickness of the silver film of silver nanowires prepared in this embodiment is 70 ⁇ m, and the content of organic matter is 0.23%.

Abstract

Disclosed in the present invention is a preparation method for a nanowire silver film for packaging and interconnection of a large-size power semiconductor integrated circuit, comprising: diluting and purifying a silver nanowire mother liquor, carrying out pressure filtration or suction filtration, and drying to obtain a nanowire silver film. The preparation method provided in the present invention is simple in process, low in cost, and controllable in film layer thickness. The nanowire silver film prepared in the present invention has the advantages of easy film formation, less impurities such as organic matters, relatively high structural strength, low-temperature sintering, convenient and efficient use, and high reliability, and after hot-pressing and sintering, the film layer has the characteristics such as high thermal conductivity, high electrical conductivity, and low porosity.

Description

一种大尺寸功率半导体集成电路封装互连用纳米线银膜的制备方法A preparation method of nanowire silver film for packaging and interconnection of large-scale power semiconductor integrated circuits 技术领域technical field
本发明涉及电子封装技术领域，尤其是一种大尺寸功率半导体集成电路封装互连用纳米线银膜的制备方法。The invention relates to the technical field of electronic packaging, in particular to a method for preparing a nanowire silver film for packaging and interconnecting large-scale power semiconductor integrated circuits.
背景技术Background technique
目前大功率半导体集成电路的芯片基板互连多采用纳米银膜实现。市面上纳米银膜多采用纳米银颗粒制备，颗粒原料的成膜性差，通常需要添加成膜剂、分散剂等有机物，采用流延法、涂布法等工艺制备成膜。虽然银膜中纳米银颗粒含量高达99％，但有机物含量仍然较高，约为1％。由纳米银颗粒制备的银膜在封装互连工艺中存在工艺适应性及使用性能等方面的不足，一是银膜转移工艺复杂，需专用设备实施：纳米颗粒银膜强度很低，无法直接转移至芯片或基板表面，通常需用定制设备先将芯片贴附在银膜，进行预烧结实现芯片与银膜的初步粘接，然后再将其转移至基板上实施热压烧结，以获得芯片与基板的封装互连。二是封装互连层的热导率及连接强度较低。银膜烧结层中残存的有机物在封装互连热压烧结过程中难以去除，且纳米银颗粒之间几乎均为点接触，烧结层会形成更多的界面和孔隙。该银膜烧结层的显微组织特征不利于膜层热导率、电导率及连接强度等性能的提高，难以满足大功率器件封装互连高导热导电、高连接强度等使用性能的要求。At present, the chip-substrate interconnection of high-power semiconductor integrated circuits is mostly realized by nano-silver film. Nano-silver films on the market are mostly prepared by nano-silver particles, and the film-forming property of particle raw materials is poor. Usually, organic substances such as film-forming agents and dispersants need to be added, and films are prepared by casting methods, coating methods and other processes. Although the content of nano-silver particles in the silver film is as high as 99%, the content of organic matter is still relatively high, about 1%. The silver film prepared by nano-silver particles has shortcomings in terms of process adaptability and performance in the packaging and interconnection process. First, the silver film transfer process is complicated and requires special equipment for implementation: the strength of the nano-particle silver film is very low and cannot be transferred directly. To the surface of the chip or substrate, it is usually necessary to attach the chip to the silver film with custom-made equipment, perform pre-sintering to realize the initial bonding of the chip and the silver film, and then transfer it to the substrate for hot-press sintering to obtain the chip and the silver film. Substrate package interconnection. Second, the thermal conductivity and connection strength of the packaging interconnection layer are low. The remaining organic matter in the sintered layer of the silver film is difficult to remove during the hot-pressing sintering process of the packaging interconnection, and the silver nanoparticles are almost in point contact, and the sintered layer will form more interfaces and pores. The microstructure characteristics of the silver film sintered layer are not conducive to the improvement of the thermal conductivity, electrical conductivity and connection strength of the film layer, and it is difficult to meet the requirements of high thermal conductivity and high connection strength for packaging and interconnection of high-power devices.
发明内容Contents of the invention
本发明提供一种大尺寸功率半导体集成电路封装互连用纳米线 银膜的制备方法，用于克服现有技术中工艺适应性及使用性能的不足等缺陷。The invention provides a method for preparing a nanowire silver film for encapsulation and interconnection of large-scale power semiconductor integrated circuits, which is used to overcome defects such as insufficient process adaptability and service performance in the prior art.
为实现上述目的，本发明提出一种大尺寸功率半导体集成电路封装互连用纳米线银膜的制备方法，包括以下步骤：In order to achieve the above object, the present invention proposes a method for preparing a nanowire silver film for encapsulating and interconnecting large-scale power semiconductor integrated circuits, comprising the following steps:
S1：对银纳米线母液进行稀释和提纯，得到银纳米线分散液；S1: diluting and purifying the silver nanowire mother liquor to obtain a silver nanowire dispersion;
S2：对所述银纳米线分散液进行压滤或抽滤，得到湿纳米线银膜；S2: performing pressure filtration or suction filtration on the silver nanowire dispersion to obtain a wet nanowire silver film;
S3：对所述湿纳米线银膜进行干燥，得到纳米线银膜。S3: drying the wet nanowire silver film to obtain a nanowire silver film.
与现有技术相比，本发明的有益效果有：Compared with prior art, the beneficial effect of the present invention has:
1、本发明提供的大尺寸功率半导体集成电路封装互连用纳米线银膜的制备方法，相比于纳米颗粒银膜需要流延机、涂布机等大型设备，纳米线银膜只需压滤或抽滤即可，设备与工艺简单，性能稳定，可批量生产。1. The preparation method of the nanowire silver film for encapsulation and interconnection of large-scale power semiconductor integrated circuits provided by the present invention requires large-scale equipment such as casting machines and coating machines compared to the nanoparticle silver film, and the nanowire silver film only needs to be pressed. Filtration or suction filtration is enough, the equipment and process are simple, the performance is stable, and it can be mass-produced.
2、本发明提供的制备方法，纳米线银膜中有机物含量更低(小于0.3％)，纳米线银膜热压烧结层残碳更少，孔隙率更低，热导率高、导电性更好、连接强度更高。2. In the preparation method provided by the present invention, the content of organic matter in the nanowire silver film is lower (less than 0.3%), and the hot-pressed sintering layer of the nanowire silver film has less residual carbon, lower porosity, high thermal conductivity, and better electrical conductivity. Well, the connection strength is higher.
3、烧结过程中芯片与基板的热胀冷缩不匹配，容易产生应力，应力的存在对器件的耐候性、可靠性等不利。本发明提供的制备方法，银膜烧结层具有多孔结构，该多孔的银膜结构可以缓冲烧结时产生的应力，提高器件的可靠性。即本发明制备的纳米线银膜的显微结构可以减轻由于芯片和基板之间热失配引起的热机械应力，提高器件在服役过程中的可靠性。3. During the sintering process, the thermal expansion and contraction of the chip and the substrate do not match, and stress is likely to occur. The existence of stress is detrimental to the weather resistance and reliability of the device. According to the preparation method provided by the invention, the silver film sintering layer has a porous structure, and the porous silver film structure can buffer the stress generated during sintering and improve the reliability of the device. That is, the microstructure of the nanowire silver film prepared by the present invention can reduce the thermomechanical stress caused by the thermal mismatch between the chip and the substrate, and improve the reliability of the device during service.
附图说明Description of drawings
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而 易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图示出的结构获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only These are some embodiments of the present invention. For those skilled in the art, other drawings can also be obtained according to the structures shown in these drawings without creative effort.
图1为实施例1中银纳米线的扫描电子显微镜图；Fig. 1 is the scanning electron micrograph of silver nanowire in embodiment 1;
图2为实施例1中纳米线银膜的扫描电子显微镜图；Fig. 2 is the scanning electron micrograph of nanowire silver film in embodiment 1;
图3为实施例1中纳米线银膜的实物图。FIG. 3 is a physical diagram of the nanowire silver film in Example 1. FIG.
本发明目的的实现、功能特点及优点将结合实施例，参照附图做进一步说明。The realization of the purpose of the present invention, functional characteristics and advantages will be further described in conjunction with the embodiments and with reference to the accompanying drawings.
具体实施方式Detailed ways
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明的一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without creative efforts fall within the protection scope of the present invention.
另外，本发明各个实施例之间的技术方案可以相互结合，但是必须是以本领域普通技术人员能够实现为基础，当技术方案的结合出现相互矛盾或无法实现时应当认为这种技术方案的结合不存在，也不在本发明要求的保护范围之内。In addition, the technical solutions of the various embodiments of the present invention can be combined with each other, but it must be based on the realization of those skilled in the art. When the combination of technical solutions is contradictory or cannot be realized, it should be considered as a combination of technical solutions. Does not exist, nor is it within the scope of protection required by the present invention.
无特殊说明，所使用的药品/试剂均为市售。Unless otherwise specified, the drugs/reagents used were all commercially available.
本发明提出一种大尺寸功率半导体集成电路封装互连用纳米线银膜的制备方法，包括以下步骤：The present invention proposes a method for preparing a nanowire silver film for encapsulating and interconnecting large-scale power semiconductor integrated circuits, comprising the following steps:
S1：对银纳米线母液进行稀释和提纯，得到银纳米线分散液；S1: diluting and purifying the silver nanowire mother liquor to obtain a silver nanowire dispersion;
S2：对所述银纳米线分散液进行压滤或抽滤，得到湿纳米线银膜；S2: performing pressure filtration or suction filtration on the silver nanowire dispersion to obtain a wet nanowire silver film;
S3：对所述湿纳米线银膜进行干燥，得到纳米线银膜。S3: drying the wet nanowire silver film to obtain a nanowire silver film.
优选地，在步骤S1中，所述稀释具体为：Preferably, in step S1, the dilution is specifically:
采用稀释剂将银纳米线母液稀释2～20倍。稀释是为了将银纳米线表面包覆的有机物溶解到水、乙醇等稀释剂中，达到提纯的目的。The silver nanowire mother liquor is diluted 2 to 20 times with a diluent. The purpose of dilution is to dissolve the organic matter coated on the surface of the silver nanowires into diluents such as water and ethanol to achieve the purpose of purification.
优选地，所述稀释剂为乙醇、去离子水或其他醇类低沸点有机溶剂。醇热法制备的银纳米线表面包覆一层有机物，该有机物可醇溶或水溶。后续压滤成膜后需低温烘干，所以须选用水或低沸点醇类溶剂。Preferably, the diluent is ethanol, deionized water or other alcoholic low-boiling organic solvents. The surface of the silver nanowires prepared by the alcohol thermal method is coated with a layer of organic matter, which can be alcohol-soluble or water-soluble. Subsequent pressure filtration requires low-temperature drying after film formation, so water or low-boiling point alcohol solvents must be used.
优选地，在步骤S1中，所述提纯具体为：Preferably, in step S1, the purification is specifically:
将稀释后的银纳米线母液置于30～60℃的水浴锅中搅拌0.5～2h，得到银纳米线分散液。提纯原理是银纳米线表层有机物可水溶或醇溶，通过添加足够量的稀释剂，即可将银纳米线表层的有机物包覆层减薄直至没有。The diluted silver nanowire mother liquor is placed in a 30-60° C. water bath and stirred for 0.5-2 hours to obtain a silver nanowire dispersion. The principle of purification is that the organic matter on the surface of silver nanowires can be dissolved in water or alcohol, and by adding a sufficient amount of diluent, the organic matter coating layer on the surface of silver nanowires can be thinned until there is no more.
提纯的目的在于银纳米线表面有机物包覆层会影响封装后器件的导电导热性能，须将其清洗干净才能满足大功率器件的使用要求。The purpose of purification is that the organic coating layer on the surface of silver nanowires will affect the electrical and thermal conductivity of the packaged device, and it must be cleaned to meet the requirements of high-power devices.
优选地，在步骤S2中，所述压滤或抽滤的压力为0.5～2MPa。压滤或抽滤的目的是为了将母液中的银纳米线提取出来，固态银纳米线留在压滤膜或抽滤膜上，其他的液态物质通过压滤膜或抽滤膜过滤掉，达到固液分离的目的。银纳米线尺寸较小，低至20nm，压滤或抽滤压力小时，母液很难通过压滤膜或抽滤膜，达不到固液分离的目的。压力太大时，有机材质的压滤膜或抽滤膜会破裂。Preferably, in step S2, the pressure of the pressure filtration or suction filtration is 0.5-2 MPa. The purpose of pressure filtration or suction filtration is to extract the silver nanowires in the mother liquor, the solid silver nanowires are left on the pressure filtration membrane or suction filtration membrane, and other liquid substances are filtered out through the pressure filtration membrane or suction filtration membrane to achieve The purpose of solid-liquid separation. The size of silver nanowires is small, as low as 20nm, and the pressure of pressure filtration or suction filtration is small, and it is difficult for the mother liquor to pass through the pressure filtration membrane or suction filtration membrane, and the purpose of solid-liquid separation cannot be achieved. When the pressure is too high, the pressure filter membrane or suction filter membrane made of organic material will rupture.
优选地，在步骤S3中，所述干燥具体为：Preferably, in step S3, the drying is specifically:
将湿纳米线银膜转移至塑料薄膜上，在40～80℃的条件下干燥1～3h，得纳米线银膜。转移至塑料薄膜的原因在于纳米银膜的厚度很小，一般为30～70μm，强度很低，需要放置在承载物上方便运输和使用。transferring the wet nanowire silver film to a plastic film, and drying at 40-80° C. for 1-3 hours to obtain the nanowire silver film. The reason for the transfer to plastic film is that the thickness of nano-silver film is very small, generally 30-70 μm, and its strength is very low. It needs to be placed on a carrier to facilitate transportation and use.
优选地，所述塑料薄膜为聚乙烯、聚丙烯、聚氯乙烯、聚苯乙烯和聚对苯二甲酸乙二醇酯中的一种。不同的塑料材质，其表面张力不同，对纳米线湿膜的吸附力也不同。张力太大，银膜容易转移；张力太小，银膜与塑料薄膜间的吸附力较大，干燥时膜之间的水或醇类溶剂不易挥发。Preferably, the plastic film is one of polyethylene, polypropylene, polyvinyl chloride, polystyrene and polyethylene terephthalate. Different plastic materials have different surface tensions and have different adsorption forces to nanowire wet films. If the tension is too large, the silver film is easy to transfer; if the tension is too small, the adsorption force between the silver film and the plastic film is large, and the water or alcohol solvent between the films is not easy to volatilize during drying.
优选地，所述纳米线银膜的厚度为30～70μm，有机物等杂质含量小于0.3％。Preferably, the nanowire silver film has a thickness of 30-70 μm, and the content of impurities such as organic matter is less than 0.3%.
优选地，所述银纳米线母液中银纳米线的直径为20～200nm，长度为5～50μm。Preferably, the silver nanowires in the silver nanowire mother liquor have a diameter of 20-200 nm and a length of 5-50 μm.
本发明提供的大功率半导体集成电路封装互连用纳米线银膜的制备方法采用银纳米线制备银膜，银纳米线直径小，具有低熔点效应，可低温热压烧结。烧结体(膜层)的熔点接近块体银(961℃)，可高温服役，导热导电性能好，剪切强度高。The preparation method of the nanowire silver film for encapsulation and interconnection of high-power semiconductor integrated circuits provided by the invention adopts the silver nanowire to prepare the silver film. The silver nanowire has a small diameter, has a low melting point effect, and can be sintered by low-temperature hot pressing. The melting point of the sintered body (film layer) is close to that of bulk silver (961°C), and it can be used at high temperature, with good thermal and electrical conductivity and high shear strength.
本发明提供的制备方法采用银纳米线制备成膜，银纳米线长度为5～50μm，银纳米线之间穿插交互搭接，更易成膜，银膜的结构完整性佳，厚度更薄且均匀可控。The preparation method provided by the present invention uses silver nanowires to prepare films, the length of the silver nanowires is 5-50 μm, and the silver nanowires are interspersed and overlapped, making it easier to form a film, the structural integrity of the silver film is good, and the thickness is thinner and uniform controllable.
优选地，所述银纳米线母液采用常规醇热法制备得到；所述银纳米线母液中银纳米线的质量分数为0.5～0.6％。实施例1Preferably, the silver nanowire mother liquor is prepared by a conventional alcohol thermal method; the mass fraction of the silver nanowire in the silver nanowire mother liquor is 0.5-0.6%. Example 1
本实施例提供一种大尺寸功率半导体集成电路封装互连用纳米线银膜的制备方法，包括以下步骤：This embodiment provides a method for preparing a nanowire silver film for encapsulation and interconnection of large-scale power semiconductor integrated circuits, including the following steps:
S1：采用常规醇热法制备银纳米线母液，该银纳米线母液中银纳米线如图1所示，直径为100～150nm、长度为25～35μm。S1: A silver nanowire mother liquor is prepared by a conventional alcohol-thermal method. The silver nanowire in the silver nanowire mother liquor is shown in FIG. 1 , with a diameter of 100-150 nm and a length of 25-35 μm.
取0.5L银纳米线母液置于烧杯中，按与银纳米线母液1:10的比例取常温去离子水，并加入烧杯中对银纳米线母液进行稀释；Take 0.5L of silver nanowire mother liquor and place it in a beaker, take normal temperature deionized water in a ratio of 1:10 with the silver nanowire mother liquor, and add it to the beaker to dilute the silver nanowire mother liquor;
将烧杯置于30℃水浴中搅拌2h，搅拌速度为500r/min，得到银 纳米线分散液。The beaker was placed in a 30°C water bath and stirred for 2 hours at a stirring speed of 500r/min to obtain a silver nanowire dispersion.
S2：将银纳米线分散液在0.5MPa的压力下压滤成湿纳米线银膜。本实施例的压滤膜为亲水性聚四氟乙烯微孔滤膜，孔径为0.45μm。本实施例湿纳米线银膜的承载物为聚对苯二甲酸乙二醇酯膜。S2: filter the silver nanowire dispersion liquid under a pressure of 0.5 MPa to form a wet nanowire silver film. The filter press membrane in this embodiment is a hydrophilic polytetrafluoroethylene microporous filter membrane with a pore size of 0.45 μm. In this embodiment, the carrier of the wet nanowire silver film is a polyethylene terephthalate film.
S3：将湿纳米线银膜放入温度为40℃的真空炉中干燥2h，得到纳米线银膜，如图2和3所示，纳米线银膜中银纳米线之间相互搭接在一起，且纳米线银膜整体性较好。S3: Put the wet nanowire silver film into a vacuum oven at a temperature of 40° C. to dry for 2 hours to obtain a nanowire silver film. As shown in Figures 2 and 3, the silver nanowires in the nanowire silver film are overlapped with each other. And the integrity of the nanowire silver film is better.
由本实施例制备得到的纳米线银膜厚度为45μm，有机物含量为0.22％。The nanowire silver film prepared by this embodiment has a thickness of 45 μm and an organic matter content of 0.22%.
实施例2Example 2
本实施例提供一种大尺寸功率半导体集成电路封装互连用纳米线银膜的制备方法，包括以下步骤：This embodiment provides a method for preparing a nanowire silver film for encapsulation and interconnection of large-scale power semiconductor integrated circuits, including the following steps:
S1：采用常规醇热法制备银纳米线母液，该银纳米线母液中银纳米线直径为50～80nm、长度为20～33μm。S1: A silver nanowire mother liquor is prepared by a conventional alcohol-thermal method, and the silver nanowire mother liquor has a diameter of 50-80 nm and a length of 20-33 μm.
取0.7L银纳米线母液置于烧杯中，按与银纳米线母液1:16的比例取常温去离子水，并加入烧杯中对银纳米线母液进行稀释；Take 0.7L of silver nanowire mother liquor and place it in a beaker, take normal temperature deionized water in a ratio of 1:16 with the silver nanowire mother liquor, and add it into the beaker to dilute the silver nanowire mother liquor;
将烧杯置于50℃水浴中搅拌0.5h，搅拌速度为500r/min，得到银纳米线分散液。The beaker was placed in a water bath at 50° C. and stirred for 0.5 h at a stirring speed of 500 r/min to obtain a silver nanowire dispersion.
S2：将银纳米线分散液在0.5MPa的压力下压滤成湿纳米线银膜。本实施例的压滤膜为亲水性聚四氟乙烯微孔滤膜，孔径为1μm。本实施例湿纳米线银膜的承载物为聚丙烯塑料膜。S2: filter the silver nanowire dispersion liquid under a pressure of 0.5 MPa to form a wet nanowire silver film. The filter press membrane in this embodiment is a hydrophilic polytetrafluoroethylene microporous filter membrane with a pore size of 1 μm. In this embodiment, the carrier of the wet nanowire silver film is a polypropylene plastic film.
S3：将湿纳米线银膜放入温度为50℃的真空炉中干燥1h，得到纳米线银膜，该纳米线银膜结构完整性好，该纳米线银膜中银纳米线之间穿插交互搭接。S3: Put the wet silver nanowire film in a vacuum oven at 50°C to dry for 1 hour to obtain a silver nanowire film. The silver nanowire film has good structural integrity, and the silver nanowires in the silver nanowire film are interspersed and overlapped. catch.
由本实施例制备得到的银纳米线银膜厚度为57μm，有机物含量为 0.24％。The thickness of the silver film of silver nanowires prepared in this example is 57 μm, and the content of organic matter is 0.24%.
实施例3Example 3
本实施例提供一种大尺寸功率半导体集成电路封装互连用纳米线银膜的制备方法，包括以下步骤：This embodiment provides a method for preparing a nanowire silver film for encapsulation and interconnection of large-scale power semiconductor integrated circuits, including the following steps:
S1：采用常规醇热法制备银纳米线母液，该银纳米线母液中银纳米线直径为160～200nm、长度为5～18μm。S1: A silver nanowire mother liquor is prepared by a conventional alcohol-thermal method, and the silver nanowire mother liquor has a diameter of 160-200 nm and a length of 5-18 μm.
取1L银纳米线母液置于烧杯中，按与银纳米线母液1:2的比例取乙醇，并加入烧杯中对银纳米线母液进行稀释；Get 1L of silver nanowire mother liquor and place it in a beaker, take ethanol in a ratio of 1:2 with the silver nanowire mother liquor, and add it to the beaker to dilute the silver nanowire mother liquor;
将烧杯置于60℃水浴中搅拌0.7h，搅拌速度为500r/min，得到银纳米线分散液。The beaker was placed in a 60° C. water bath and stirred for 0.7 h at a stirring speed of 500 r/min to obtain a silver nanowire dispersion.
S2：将银纳米线分散液在1MPa的压力下压滤成湿纳米线银膜。本实施例的压滤膜为亲水性聚四氟乙烯微孔滤膜，孔径为1μm。本实施例湿纳米线银膜的承载物为聚苯乙烯膜。S2: filter the silver nanowire dispersion under a pressure of 1 MPa to form a wet nanowire silver film. The filter press membrane in this embodiment is a hydrophilic polytetrafluoroethylene microporous filter membrane with a pore size of 1 μm. In this embodiment, the carrier of the wet nanowire silver film is a polystyrene film.
S3：将湿纳米线银膜放入温度为80℃的真空炉中干燥1.2h，得到纳米线银膜，该纳米线银膜结构完整性好，该纳米线银膜中银纳米线之间穿插交互搭接。S3: Put the wet silver nanowire film in a vacuum oven at 80°C for 1.2 hours to dry to obtain a silver nanowire film. The silver nanowire film has good structural integrity, and the silver nanowires in the silver nanowire film are interspersed with each other. lap.
由本实施例制备得到的银纳米线银膜厚度为30μm，有机物含量为0.21％。The thickness of the silver film of silver nanowires prepared in this embodiment is 30 μm, and the content of organic matter is 0.21%.
实施例4Example 4
本实施例提供一种大尺寸功率半导体集成电路封装互连用纳米线银膜的制备方法，包括以下步骤：This embodiment provides a method for preparing a nanowire silver film for encapsulation and interconnection of large-scale power semiconductor integrated circuits, including the following steps:
S1：采用常规醇热法制备银纳米线母液，该银纳米线母液中银纳米线直径为20～45nm、长度为35～50μm。S1: A silver nanowire mother liquor is prepared by a conventional alcohol-thermal method, and the silver nanowire mother liquor has a diameter of 20-45 nm and a length of 35-50 μm.
取0.2L银纳米线母液置于烧杯中，按与银纳米线母液1:20的比例取乙醇，并加入烧杯中对银纳米线母液进行稀释；Get 0.2L of silver nanowire mother liquor and place it in a beaker, take ethanol in a ratio of 1:20 with the silver nanowire mother liquor, and add it into the beaker to dilute the silver nanowire mother liquor;
将烧杯置于40℃水浴中搅拌2h，搅拌速度为500r/min，得到银纳米线分散液。The beaker was placed in a 40° C. water bath and stirred for 2 hours at a stirring speed of 500 r/min to obtain a silver nanowire dispersion.
S2：将银纳米线分散液在2MPa的压力下压滤成湿纳米线银膜。本实施例的压滤膜为亲水性聚四氟乙烯微孔滤膜，孔径为0.5μm。本实施例湿纳米线银膜的承载物为聚苯乙烯膜。S2: filter the silver nanowire dispersion under a pressure of 2 MPa to form a wet nanowire silver film. The filter press membrane in this embodiment is a hydrophilic polytetrafluoroethylene microporous filter membrane with a pore size of 0.5 μm. In this embodiment, the carrier of the wet nanowire silver film is a polystyrene film.
S3：将湿纳米线银膜放入温度为70℃的真空炉中干燥2.1h，得到纳米线银膜，该纳米线银膜结构完整性好，该纳米线银膜中银纳米线之间穿插交互搭接。S3: Put the wet silver nanowire film in a vacuum oven at 70°C for 2.1 hours to dry to obtain a silver nanowire film. The silver nanowire film has good structural integrity, and the silver nanowires in the silver nanowire film are interspersed with each other. lap.
由本实施例制备得到的银纳米线银膜厚度为70μm，有机物含量为0.23％。The thickness of the silver film of silver nanowires prepared in this embodiment is 70 μm, and the content of organic matter is 0.23%.
以上所述仅为本发明的优选实施例，并非因此限制本发明的专利范围，凡是在本发明的发明构思下，利用本发明说明书及附图内容所作的等效结构变换，或直接/间接运用在其他相关的技术领域均包括在本发明的专利保护范围内。The above is only a preferred embodiment of the present invention, and does not limit the patent scope of the present invention. Under the inventive concept of the present invention, the equivalent structural transformation made by using the description of the present invention and the contents of the accompanying drawings, or direct/indirect use All other relevant technical fields are included in the patent protection scope of the present invention.

Claims (10)

  1. 一种大尺寸功率半导体集成电路封装互连用纳米线银膜的制备方法，其特征在于，包括以下步骤：A method for preparing a nanowire silver film for encapsulating and interconnecting large-scale power semiconductor integrated circuits, characterized in that it comprises the following steps:
    S1：对银纳米线母液进行稀释和提纯，得到银纳米线分散液；S1: diluting and purifying the silver nanowire mother liquor to obtain a silver nanowire dispersion;
    S2：对所述银纳米线分散液进行压滤或抽滤，得到湿纳米线银膜；S2: performing pressure filtration or suction filtration on the silver nanowire dispersion to obtain a wet nanowire silver film;
    S3：对所述湿纳米线银膜进行干燥，得到纳米线银膜。S3: drying the wet nanowire silver film to obtain a nanowire silver film.
  2. 如权利要求1所述的制备方法，其特征在于，在步骤S1中，所述稀释具体为：The preparation method according to claim 1, wherein in step S1, the dilution is specifically:
    采用稀释剂将银纳米线母液稀释2～20倍。The silver nanowire mother liquor is diluted 2 to 20 times with a diluent.
  3. 如权利要求2所述的制备方法，其特征在于，所述稀释剂为乙醇、去离子水或其他醇类低沸点有机溶剂。The preparation method according to claim 2, wherein the diluent is ethanol, deionized water or other alcoholic low-boiling organic solvents.
  4. 如权利要求1～3任一项所述的制备方法，其特征在于，在步骤S1中，所述提纯具体为：The preparation method according to any one of claims 1 to 3, characterized in that, in step S1, the purification is specifically:
    将稀释后的银纳米线母液置于30～60℃的水浴锅中搅拌0.5～2h，得到银纳米线分散液。The diluted silver nanowire mother liquor is placed in a 30-60° C. water bath and stirred for 0.5-2 hours to obtain a silver nanowire dispersion.
  5. 如权利要求1所述的制备方法，其特征在于，在步骤S2中，所述压滤或抽滤的压力为0.5～2MPa。The preparation method according to claim 1, characterized in that, in step S2, the pressure of the pressure filtration or suction filtration is 0.5-2 MPa.
  6. 如权利要求1所述的制备方法，其特征在于，在步骤S3中，所述干燥具体为：The preparation method according to claim 1, characterized in that, in step S3, the drying is specifically:
    将湿纳米线银膜转移至塑料薄膜上，在40～80℃的条件下干燥1～3h，得纳米线银膜。transferring the wet nanowire silver film to a plastic film, and drying at 40-80° C. for 1-3 hours to obtain the nanowire silver film.
  7. 如权利要求6所述的制备方法，其特征在于，所述塑料薄膜为聚乙烯、聚丙烯、聚氯乙烯、聚苯乙烯和聚对苯二甲酸乙二醇酯中的一种。The preparation method according to claim 6, wherein the plastic film is one of polyethylene, polypropylene, polyvinyl chloride, polystyrene and polyethylene terephthalate.
  8. 如权利要求1所述的制备方法，其特征在于，所述纳米线银膜的厚度为30～70μm，有机物等杂质含量小于0.3％。The preparation method according to claim 1, characterized in that the thickness of the nanowire silver film is 30-70 μm, and the content of impurities such as organic matter is less than 0.3%.
  9. 如权利要求1所述的制备方法，其特征在于，所述银纳米线母液中银纳米线的直径为20～200nm，长度为5～50μm。The preparation method according to claim 1, characterized in that, the silver nanowires in the silver nanowire mother liquor have a diameter of 20-200 nm and a length of 5-50 μm.
  10. 如权利要求1所述的制备方法，其特征在于，所述银纳米线母液采用常规醇热法制备得到；所述银纳米线母液中银纳米线的质量分数为0.5～0.6％。The preparation method according to claim 1, characterized in that, the silver nanowire mother liquor is prepared by conventional alcohol thermal method; the mass fraction of the silver nanowire in the silver nanowire mother liquor is 0.5-0.6%.
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