CN111761827A - A kind of carbon fiber reinforced resin matrix composite material joining process method - Google Patents

A kind of carbon fiber reinforced resin matrix composite material joining process method Download PDF

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CN111761827A
CN111761827A CN202010517164.7A CN202010517164A CN111761827A CN 111761827 A CN111761827 A CN 111761827A CN 202010517164 A CN202010517164 A CN 202010517164A CN 111761827 A CN111761827 A CN 111761827A
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carbon fiber
ultrasonic vibration
reinforced resin
fiber reinforced
composite material
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CN111761827B (en
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陈一哲
黄开
华林
王辉
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Wuhan University of Technology WUT
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/48Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00General aspects of processes or apparatus for joining preformed parts
    • B29C66/01General aspects dealing with the joint area or with the area to be joined
    • B29C66/02Preparation of the material, in the area to be joined, prior to joining or welding
    • B29C66/028Non-mechanical surface pre-treatments, i.e. by flame treatment, electric discharge treatment, plasma treatment, wave energy or particle radiation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00General aspects of processes or apparatus for joining preformed parts
    • B29C66/70General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/72General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the structure of the material of the parts to be joined
    • B29C66/721Fibre-reinforced materials

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  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Lining Or Joining Of Plastics Or The Like (AREA)

Abstract

本发明公开了一种碳纤维增强树脂基复合材料连接工艺方法,使用紫外脉冲激光束扫描碳纤维增强树脂基复合材料粘接面,去除表面树脂层并暴露碳纤维层,并进行清洗、晾干处理;对粘接面涂胶并进行粘接;通过超声振动工具头对粘接面的垂直方向施加频率为15KHz~25KHz的超声波振动,振动前通过超声振动工具头施加1MPa~5MPa预压力,结束保持压力15~30min;将胶接件在40℃~80℃加热固化1~20h。本发明首次将超声振动辅助胶接与激光表面处理和使用碳纳米管对胶粘剂改性结合起来,有效解决了实际工程中碳纤维胶粘连接产生的胶粘质量不好、胶粘质量不均、胶粘前表面处理使碳纤维丝断裂的问题。The invention discloses a connection process method for carbon fiber reinforced resin-based composite materials. Ultraviolet pulsed laser beams are used to scan the bonding surface of carbon fiber-reinforced resin-based composite materials, the surface resin layer is removed, the carbon fiber layer is exposed, and cleaning and drying are performed; Apply glue on the bonding surface and carry out bonding; apply ultrasonic vibration with a frequency of 15KHz to 25KHz to the vertical direction of the bonding surface through the ultrasonic vibration tool head, apply a pre-pressure of 1MPa to 5MPa through the ultrasonic vibration tool head before vibration, and end the holding pressure of 15 ~30min; heat and cure the glued parts at 40℃~80℃ for 1~20h. The invention combines ultrasonic vibration-assisted bonding with laser surface treatment and modification of the adhesive by using carbon nanotubes for the first time, and effectively solves the problems of poor bonding quality, uneven bonding quality, and adhesive bonding caused by carbon fiber bonding in practical engineering. The problem of carbon fiber filaments breaking due to surface treatment before sticking.

Description

一种碳纤维增强树脂基复合材料连接工艺方法A kind of carbon fiber reinforced resin matrix composite material joining process method

技术领域technical field

本发明属于材料技术领域,具体涉及一种碳纤维增强树脂基复合材料连接工艺方法。The invention belongs to the technical field of materials, and in particular relates to a connection process method for carbon fiber reinforced resin-based composite materials.

背景技术Background technique

随着汽车工业的大力发展,节能、环保被越来越多的考虑到汽车生产制造过程中,研究表明,汽车减重1%,油耗降低0.7%,汽车整备质量每降低100kg,百公里燃油消耗量可降低0.3~0.6L,同时废气排放也相应减少。With the vigorous development of the automobile industry, energy saving and environmental protection are more and more taken into account in the manufacturing process of automobiles. Research shows that the weight of the automobile is reduced by 1%, and the fuel consumption is reduced by 0.7%. The volume can be reduced by 0.3 to 0.6L, and the exhaust emission is also reduced accordingly.

碳纤维增强树脂基复合材料由于其强度高、密度小、热稳定性能好、可制备性能好,近年来在多个工程领域内得到了广泛应用,成为新材料的研究重点。与传统的复合材料机械连接(螺栓连接、铆接)方式相比,胶连接借助胶接剂将零件连接,无对复合材料的损伤、无开孔应力集中,具有承载能力强、应力分布均匀、防止电化学腐蚀等优点。因此,胶连接比机械连接更广泛地应用于碳纤维先进复合材料的连接设计中,成为实现汽车轻量化的关键技术之一。但是胶接质量不高和胶接强度分布不均的问题一直没有得到较好的解决。Carbon fiber reinforced resin matrix composites have been widely used in many engineering fields in recent years due to their high strength, low density, good thermal stability, and good preparation performance, and have become the focus of new material research. Compared with the traditional mechanical connection of composite materials (bolt connection, riveting), the glue connection uses the adhesive to connect the parts, without damage to the composite material, without the stress concentration of openings, with strong bearing capacity, uniform stress distribution, preventing The advantages of electrochemical corrosion, etc. Therefore, glue connection is more widely used in the connection design of carbon fiber advanced composite materials than mechanical connection, and it has become one of the key technologies to realize the lightweight of automobiles. However, the problems of poor bonding quality and uneven distribution of bonding strength have not been well resolved.

超声振动辅助胶接技术成为近年来广泛关注的研究方向,与传统的胶粘工艺相比,超声振动在液相中产生的空化效应具有诱导填缝和界面增润作用能显著提高胶接质量,改善胶接强度分布不均的问题。Ultrasonic vibration-assisted bonding technology has become a research direction of extensive attention in recent years. Compared with the traditional bonding process, the cavitation effect generated by ultrasonic vibration in the liquid phase has the effect of inducing seam filling and interfacial moisturization, which can significantly improve the bonding quality. , to improve the problem of uneven distribution of bonding strength.

目前提高碳纤维增强树脂基复合材料粘接强度的方法主要是通过改进粘接表面处理工艺,比如打磨、喷砂、喷丸、偶联等,改善粘接剂的组分配比,以及改变粘接剂固化工艺等。但是在胶粘过程中人为因素影响很大,打磨不均、涂胶不均匀等工艺因素会使样件粘接强度差异性较大,喷砂、喷丸、偶联等工序繁杂增加成本,同时难以施加均匀的成型压力使粘接剂能充分润湿待粘接表面,这些因素都使获得稳定可靠的高粘合强度的粘接试样成为难题。At present, the method to improve the bonding strength of carbon fiber reinforced resin matrix composites is mainly by improving the bonding surface treatment process, such as grinding, sandblasting, shot peening, coupling, etc., improving the component ratio of the adhesive, and changing the adhesive. curing process, etc. However, human factors have a great influence on the gluing process. Process factors such as uneven grinding and uneven gluing will cause large differences in the bonding strength of the samples. Sandblasting, shot peening, coupling and other processes are complicated and increase costs. It is difficult to apply uniform molding pressure so that the adhesive can sufficiently wet the surfaces to be bonded, and these factors make it difficult to obtain stable and reliable bonded samples with high bond strength.

发明内容SUMMARY OF THE INVENTION

本发明目的在于提供一种碳纤维增强树脂基复合材料连接工艺方法,旨在提高碳纤维增强树脂基复合材料粘接面表面质量,提高粘接剂与粘接面的接触面积,进而提高超声振动辅助胶接强度和质量。The purpose of the present invention is to provide a connection process method of carbon fiber reinforced resin matrix composite materials, which aims to improve the surface quality of the bonding surface of carbon fiber reinforced resin matrix composite materials, improve the contact area between the adhesive and the bonding surface, and then improve the ultrasonic vibration auxiliary glue connection strength and quality.

为达到上述目的,采用技术方案如下:In order to achieve the above purpose, the technical solutions are as follows:

一种碳纤维增强树脂基复合材料连接工艺方法,包括以下步骤:A carbon fiber reinforced resin matrix composite material connection process method, comprising the following steps:

1)使用紫外脉冲激光束扫描碳纤维增强树脂基复合材料粘接面,去除表面树脂层并暴露碳纤维层,并进行清洗、晾干处理;1) Scan the bonding surface of the carbon fiber reinforced resin matrix composite material with an ultraviolet pulsed laser beam, remove the surface resin layer and expose the carbon fiber layer, and carry out cleaning and drying treatment;

2)将激光处理过的碳纤维增强树脂基复合材料固定后对粘接面涂胶并进行粘接;所用粘接剂制备方法如下:将碳纳米管与乙酸乙酯混合超声振动分散45min~90min,加入环氧树脂组分继续超声振动分散45min~90min后去除乙酸乙酯,加入环氧树脂固化剂并混合均匀;2) After fixing the laser-treated carbon fiber reinforced resin-based composite material, apply glue to the bonding surface and carry out bonding; the adhesive preparation method used is as follows: the carbon nanotubes are mixed with ethyl acetate and dispersed by ultrasonic vibration for 45min-90min, Add epoxy resin components and continue to disperse by ultrasonic vibration for 45min-90min, then remove ethyl acetate, add epoxy resin curing agent and mix evenly;

3)通过超声振动工具头对粘接面的垂直方向施加频率为15KHz~25KHz的超声波振动,振动前通过超声振动工具头施加1MPa~5MPa预压力,超声波振动结束保持压力15min~30min;3) Apply ultrasonic vibration with a frequency of 15KHz to 25KHz to the vertical direction of the bonding surface through the ultrasonic vibration tool head, apply a pre-pressure of 1MPa to 5MPa through the ultrasonic vibration tool head before the vibration, and maintain the pressure for 15min to 30min after the ultrasonic vibration;

4)将胶接件在40℃~80℃加热固化1~20h。4) Heat and cure the glued parts at 40℃~80℃ for 1~20h.

按上述方案,步骤1所用紫外脉冲激光为波长为193nm~355nm的紫外激光,光子能量为3.49eV~6.44eV,平均功率为15w~200w,重复频率为1MH~2MHz,光斑直径为1.3mm~1.5mm,扫描速度为50mm/s~1500mm/s。According to the above scheme, the ultraviolet pulsed laser used in step 1 is an ultraviolet laser with a wavelength of 193nm~355nm, the photon energy is 3.49eV~6.44eV, the average power is 15w~200w, the repetition frequency is 1MH~2MHz, and the spot diameter is 1.3mm~1.5 mm, the scanning speed is 50mm/s~1500mm/s.

按上述方案,步骤1所述紫外脉冲激光束扫描方向与所述碳纤维增强树脂基复合材料最外层纤维方向呈45°。According to the above scheme, the scanning direction of the ultraviolet pulsed laser beam in step 1 and the direction of the outermost fiber of the carbon fiber reinforced resin matrix composite material are at 45°.

按上述方案,步骤2所述粘接剂制备过程中,每隔15min停止超声振动分散并搅拌5min,温度保持在25℃~35℃;碳纳米管在粘接剂中的质量百分数为0.2%-1%。According to the above scheme, during the preparation process of the adhesive described in step 2, the ultrasonic vibration dispersion was stopped every 15 minutes and the stirring was carried out for 5 minutes, and the temperature was kept at 25°C to 35°C; the mass percentage of carbon nanotubes in the adhesive was 0.2%- 1%.

按上述方案,步骤2中胶层厚度在0.7mm~0.8mm之间。According to the above scheme, the thickness of the adhesive layer in step 2 is between 0.7mm and 0.8mm.

按上述方案,步骤2中超声波振动幅值为10μm~100μm,振幅百分比为50%~100%。According to the above scheme, in step 2, the ultrasonic vibration amplitude is 10 μm to 100 μm, and the amplitude percentage is 50% to 100%.

本发明的有益效果在于:The beneficial effects of the present invention are:

本发明的一种碳纤维增强树脂基复合材料连接工艺方法首次将超声振动辅助胶接与激光表面处理和使用碳纳米管对粘接剂改性结合起来,有效解决了实际工程中碳纤维胶粘连接产生的胶粘质量不好、胶粘质量不均、胶粘前表面处理使碳纤维丝断裂的问题。A carbon fiber reinforced resin-based composite material connection process method of the present invention combines ultrasonic vibration-assisted bonding with laser surface treatment and modification of the adhesive with carbon nanotubes for the first time, which effectively solves the problem of carbon fiber bonding in practical engineering. The adhesive quality is not good, the adhesive quality is uneven, and the carbon fiber filament is broken by the surface treatment before the adhesive.

本发明精度高,表面质量稳定,通过超声振动使碳纤维丝的空间排布产生变化,同时碳纤维丝在超声振动的作用下也会产生一定程度的振动,使碳纳米管在碳纤维丝间隙聚集形成交联网状的机械栓锁结构,从而使粘接剂能更好的碳纤维丝粘合;另外,通过超声振动还改变了胶层流场方向,使碳纳米管产生取向排布,碳纳米管表面的游离基团与环氧树脂粘接剂分子之间形成共价键,增强粘接剂性能,提高粘接强度提高胶接强度。The invention has high precision and stable surface quality, and changes the spatial arrangement of the carbon fiber filaments through ultrasonic vibration. At the same time, the carbon fiber filaments will also vibrate to a certain extent under the action of ultrasonic vibration, so that the carbon nanotubes gather in the gaps of the carbon fiber filaments to form crossovers. The networked mechanical latch structure enables the adhesive to better bond the carbon fiber filaments; in addition, the ultrasonic vibration also changes the direction of the flow field of the adhesive layer, so that the carbon nanotubes are oriented and arranged, and the surface of the carbon nanotubes is arranged. Covalent bonds are formed between the free groups and the epoxy resin adhesive molecules, which enhances the performance of the adhesive, improves the bonding strength and improves the bonding strength.

该方法适合自动化、工业化生产。The method is suitable for automated and industrialized production.

具体实施方式Detailed ways

以下实施例进一步阐释本发明的技术方案,但不作为对本发明保护范围的限制。The following examples further illustrate the technical solutions of the present invention, but are not intended to limit the protection scope of the present invention.

本发明所述碳纤维增强树脂基复合材料连接工艺方法流程如下:The process flow of the carbon fiber reinforced resin matrix composite material connection process method of the present invention is as follows:

步骤S100,将碳纤维增强树脂基复合材料表面进行清洁处理,通过皮秒激光处理清洁过的碳纤维增强树脂基复合材料胶接区域以除去表面树脂并暴露内层碳纤维层。In step S100, the surface of the carbon fiber reinforced resin matrix composite material is cleaned, and the cleaned bonding area of the carbon fiber reinforced resin matrix composite material is treated by picosecond laser to remove the surface resin and expose the inner carbon fiber layer.

步骤S200,采用溶液混合法向粘接剂中添加一定质量分数的碳纳米管。Step S200, adding a certain mass fraction of carbon nanotubes to the adhesive by using a solution mixing method.

步骤S300,碳纤维增强树脂基复合材料放入定位夹具中,进行粘接表面涂胶处理。Step S300, the carbon fiber reinforced resin matrix composite material is put into the positioning fixture, and the adhesive surface is treated with glue.

步骤S400,通过超声振动工具头对碳纤维增强树脂基复合材料施加一定频率的超声波振动。In step S400, ultrasonic vibration of a certain frequency is applied to the carbon fiber reinforced resin matrix composite material by an ultrasonic vibration tool head.

步骤S500,停止超声波振动,上升超声振动工具头,将胶接件放入烘箱中加热固化。In step S500, the ultrasonic vibration is stopped, the ultrasonic vibration tool head is raised, and the adhesive joint is placed in an oven for heating and curing.

实施例1Example 1

步骤一:使用紫外脉冲激光束扫描碳纤维增强树脂基复合材料粘接面,去除表面树脂层并暴露碳纤维层,并进行清洗、晾干处理。相关激光参数为:波长355nm,光子能量为3.49ev,平均功率30w,重复频率1MHz,光斑直径1.3mm,扫描速度1500mm/s,扫描方向与所述碳纤维增强树脂基复合材料最外层纤维方向呈45°。Step 1: Scan the bonding surface of the carbon fiber reinforced resin matrix composite material with an ultraviolet pulsed laser beam, remove the surface resin layer and expose the carbon fiber layer, and perform cleaning and drying treatment. The relevant laser parameters are: wavelength 355nm, photon energy 3.49ev, average power 30w, repetition frequency 1MHz, spot diameter 1.3mm, scanning speed 1500mm/s, and the scanning direction is in the direction of the outermost fiber of the carbon fiber reinforced resin matrix composite material. 45°.

步骤二:将占粘接剂质量0.2wt%碳纳米管与乙酸乙酯混合超声振动分散45min,加入环氧树脂组分继续超声振动分散45min后放入真空干燥箱去除乙酸乙酯,加入环氧树脂固化剂并混合均匀。Step 2: Mix 0.2wt% carbon nanotubes and ethyl acetate for 45min by ultrasonic vibration dispersion, add epoxy resin components and continue ultrasonic vibration dispersion for 45min, put into a vacuum drying box to remove ethyl acetate, add epoxy resin resin curing agent and mix well.

步骤三:将碳纤维增强树脂基复合材料放入定位夹具中,进行粘接表面涂胶处理,胶层厚度为0.7mm。Step 3: Put the carbon fiber reinforced resin-based composite material into the positioning fixture, and apply glue on the bonding surface, and the thickness of the glue layer is 0.7mm.

步骤四:通过超声振动工具头对碳纤维增强树脂基复合材料施加一定频率的超声波振动。其中,超声频率为15KHz,幅值为10μm,振幅百分比为70%,振动前通过超声振动工具头向碳纤维增强树脂基复合材料施加1MPa的预压力,振动结束后保持压力15min。Step 4: applying ultrasonic vibration of a certain frequency to the carbon fiber reinforced resin matrix composite material through the ultrasonic vibration tool head. Among them, the ultrasonic frequency is 15KHz, the amplitude is 10μm, and the amplitude percentage is 70%. Before the vibration, a pre-pressure of 1MPa is applied to the carbon fiber reinforced resin matrix composite material through the ultrasonic vibration tool head, and the pressure is maintained for 15min after the vibration.

步骤五:停止超声波振动,上升超声振动工具头,将胶接件放入烘箱中,在40℃下加热固化20h。Step 5: Stop the ultrasonic vibration, raise the ultrasonic vibration tool head, put the glue joint into the oven, and heat and cure it at 40°C for 20h.

根据ASTM D5868-01,对单搭接试样进行拉伸实验,得到试样剪切强度为12.08MPa。According to ASTM D5868-01, the tensile test was performed on the single lap specimen, and the shear strength of the specimen was 12.08 MPa.

实施例2Example 2

步骤一:使用紫外脉冲激光束扫描碳纤维增强树脂基复合材料粘接面,去除表面树脂层并暴露碳纤维层,并进行清洗、晾干处理。相关激光参数为:波长193nm,光子能量为6.44ev,平均功率15w,重复频率1.2MHz,光斑直径1.5mm,扫描速度800mm/s,扫描方向与所述碳纤维增强树脂基复合材料最外层纤维方向呈45°。Step 1: Scan the bonding surface of the carbon fiber reinforced resin matrix composite material with an ultraviolet pulsed laser beam, remove the surface resin layer and expose the carbon fiber layer, and perform cleaning and drying treatment. The relevant laser parameters are: wavelength 193nm, photon energy 6.44ev, average power 15w, repetition frequency 1.2MHz, spot diameter 1.5mm, scanning speed 800mm/s, scanning direction and the outermost fiber direction of the carbon fiber reinforced resin matrix composite material at 45°.

步骤二:将占粘接剂质量0.5wt%碳纳米管与乙酸乙酯混合超声振动分散60min,加入环氧树脂组分继续超声振动分散60min后放入真空干燥箱去除乙酸乙酯,加入环氧树脂固化剂并混合均匀。Step 2: Mix 0.5wt% carbon nanotubes and ethyl acetate for 60 minutes of ultrasonic vibration dispersion, add epoxy resin components, continue ultrasonic vibration dispersion for 60 minutes, put into a vacuum drying box to remove ethyl acetate, add epoxy resin resin curing agent and mix well.

步骤三:将碳纤维增强树脂基复合材料放入定位夹具中,进行粘接表面涂胶处理,胶层厚度为0.7mm。Step 3: Put the carbon fiber reinforced resin-based composite material into the positioning fixture, and apply glue on the bonding surface, and the thickness of the glue layer is 0.7mm.

步骤四:通过超声振动工具头对碳纤维增强树脂基复合材料施加一定频率的超声波振动。其中,超声频率为15KHz,幅值为32μm,振幅百分比为70%,振动前通过超声振动工具头向碳纤维增强树脂基复合材料施加1MPa的预压力,振动结束后保持压力15min。Step 4: applying ultrasonic vibration of a certain frequency to the carbon fiber reinforced resin matrix composite material through the ultrasonic vibration tool head. Among them, the ultrasonic frequency is 15KHz, the amplitude is 32μm, and the amplitude percentage is 70%. Before the vibration, a pre-pressure of 1MPa is applied to the carbon fiber reinforced resin matrix composite material through the ultrasonic vibration tool head, and the pressure is maintained for 15min after the vibration.

步骤五:停止超声波振动,上升超声振动工具头,将胶接件放入烘箱中,在40℃下加热固化20h。Step 5: Stop the ultrasonic vibration, raise the ultrasonic vibration tool head, put the glue joint into the oven, and heat and cure it at 40°C for 20h.

根据ASTM D5868-01,对单搭接试样进行拉伸实验,得到试样剪切强度为8.93MPa。According to ASTM D5868-01, the tensile test was performed on the single lap specimen, and the shear strength of the specimen was 8.93 MPa.

实施例3Example 3

步骤一:使用紫外脉冲激光束扫描碳纤维增强树脂基复合材料粘接面,去除表面树脂层并暴露碳纤维层,并进行清洗、晾干处理。相关激光参数为:波长355nm,光子能量为3.49ev,平均功率30w,重复频率1MHz,光斑直径1.5mm,扫描速度50mm/s,扫描方向与所述碳纤维增强树脂基复合材料最外层纤维方向呈45°。Step 1: Scan the bonding surface of the carbon fiber reinforced resin matrix composite material with an ultraviolet pulsed laser beam, remove the surface resin layer and expose the carbon fiber layer, and perform cleaning and drying treatment. The relevant laser parameters are: wavelength 355nm, photon energy 3.49ev, average power 30w, repetition frequency 1MHz, spot diameter 1.5mm, scanning speed 50mm/s, and the scanning direction is in the direction of the outermost fiber of the carbon fiber reinforced resin matrix composite material. 45°.

步骤二:将占粘接剂质量0.75wt%碳纳米管与乙酸乙酯混合超声振动分散75min,加入环氧树脂组分继续超声振动分散75min后放入真空干燥箱去除乙酸乙酯,加入环氧树脂固化剂并混合均匀。Step 2: Mix 0.75 wt% carbon nanotubes and ethyl acetate for 75 minutes of ultrasonic vibration dispersion, add epoxy resin components, continue ultrasonic vibration dispersion for 75 minutes, put into a vacuum drying box to remove ethyl acetate, add epoxy resin resin curing agent and mix well.

步骤三:将碳纤维增强树脂基复合材料放入定位夹具中,进行粘接表面涂胶处理,胶层厚度为0.76mm。Step 3: Put the carbon fiber reinforced resin-based composite material into the positioning fixture, and apply glue on the bonding surface, and the thickness of the glue layer is 0.76mm.

步骤四:通过超声振动工具头对碳纤维增强树脂基复合材料施加一定频率的超声波振动。其中,超声频率为15KHz,幅值为24μm,振幅百分比为70%,振动前通过超声振动工具头向碳纤维增强树脂基复合材料施加5MPa的预压力,振动结束后保持压力15min。Step 4: applying ultrasonic vibration of a certain frequency to the carbon fiber reinforced resin matrix composite material through the ultrasonic vibration tool head. Among them, the ultrasonic frequency is 15KHz, the amplitude is 24μm, and the amplitude percentage is 70%. Before the vibration, a pre-pressure of 5MPa is applied to the carbon fiber reinforced resin matrix composite material through the ultrasonic vibration tool head, and the pressure is maintained for 15min after the vibration.

步骤五:停止超声波振动,上升超声振动工具头,将胶接件放入烘箱中,在80℃下加热固化3h。Step 5: Stop the ultrasonic vibration, raise the ultrasonic vibration tool head, put the glue joint into the oven, and heat and cure it at 80°C for 3 hours.

根据ASTM D5868-01,对单搭接试样进行拉伸实验,得到试样剪切强度为24.48MPa。According to ASTM D5868-01, the tensile test was carried out on the single lap specimen, and the shear strength of the specimen was 24.48MPa.

实施例4Example 4

步骤一:使用紫外脉冲激光束扫描碳纤维增强树脂基复合材料粘接面,去除表面树脂层并暴露碳纤维层,并进行清洗、晾干处理。相关激光参数为:波长355nm,光子能量为3.49ev,平均功率200w,重复频率2MHz,光斑直径1.5mm,扫描速度300mm/s,扫描方向与所述碳纤维增强树脂基复合材料最外层纤维方向呈45°。Step 1: Scan the bonding surface of the carbon fiber reinforced resin matrix composite material with an ultraviolet pulsed laser beam, remove the surface resin layer and expose the carbon fiber layer, and perform cleaning and drying treatment. The relevant laser parameters are: wavelength 355nm, photon energy 3.49ev, average power 200w, repetition frequency 2MHz, spot diameter 1.5mm, scanning speed 300mm/s, and the scanning direction is in the direction of the outermost fiber of the carbon fiber reinforced resin matrix composite material. 45°.

步骤二:将占粘接剂质量0.75wt%碳纳米管与乙酸乙酯混合超声振动分散60min,加入环氧树脂组分继续超声振动分散75min后放入真空干燥箱去除乙酸乙酯,加入环氧树脂固化剂并混合均匀。Step 2: Mix 0.75wt% carbon nanotubes and ethyl acetate for 60 minutes of ultrasonic vibration dispersion, add epoxy resin components, continue ultrasonic vibration dispersion for 75 minutes, put into a vacuum drying box to remove ethyl acetate, add epoxy resin resin curing agent and mix well.

步骤三:将碳纤维增强树脂基复合材料放入定位夹具中,进行粘接表面涂胶处理,胶层厚度为0.8mm。Step 3: Put the carbon fiber reinforced resin-based composite material into the positioning fixture, and apply glue on the bonding surface, and the thickness of the glue layer is 0.8mm.

步骤四:通过超声振动工具头对碳纤维增强树脂基复合材料施加一定频率的超声波振动。其中,超声频率为20KHz,幅值为20μm,振幅百分比为50%,振动前通过超声振动工具头向碳纤维增强树脂基复合材料施加3MPa的预压力,振动结束后保持压力20min。Step 4: applying ultrasonic vibration of a certain frequency to the carbon fiber reinforced resin matrix composite material through the ultrasonic vibration tool head. Among them, the ultrasonic frequency is 20KHz, the amplitude is 20μm, and the amplitude percentage is 50%. Before the vibration, a pre-pressure of 3MPa is applied to the carbon fiber reinforced resin matrix composite material through the ultrasonic vibration tool head, and the pressure is maintained for 20min after the vibration.

步骤五:停止超声波振动,上升超声振动工具头,将胶接件放入烘箱中,在80℃下加热固化1h。Step 5: Stop the ultrasonic vibration, raise the ultrasonic vibration tool head, put the adhesive part into the oven, and heat and cure it at 80°C for 1 hour.

根据ASTM D5868-01,对单搭接试样进行拉伸实验,得到试样剪切强度为22.58MPa。According to ASTM D5868-01, the tensile test was carried out on the single lap specimen, and the shear strength of the specimen was 22.58MPa.

实施例5Example 5

步骤一:使用紫外脉冲激光束扫描碳纤维增强树脂基复合材料粘接面,去除表面树脂层并暴露碳纤维层,并进行清洗、晾干处理。相关激光参数为:波长248nm,光子能量为4.96ev,平均功率100w,重复频率1.6MHz,光斑直径1.4mm,扫描速度200mm/s,扫描方向与所述碳纤维增强树脂基复合材料最外层纤维方向呈45°。Step 1: Scan the bonding surface of the carbon fiber reinforced resin matrix composite material with an ultraviolet pulsed laser beam, remove the surface resin layer and expose the carbon fiber layer, and perform cleaning and drying treatment. The relevant laser parameters are: wavelength 248nm, photon energy 4.96ev, average power 100w, repetition frequency 1.6MHz, spot diameter 1.4mm, scanning speed 200mm/s, scanning direction and the outermost fiber direction of the carbon fiber reinforced resin matrix composite material at 45°.

步骤二:将占粘接剂质量1wt%碳纳米管与乙酸乙酯混合超声振动分散90min,加入环氧树脂组分继续超声振动分散90min后放入真空干燥箱去除乙酸乙酯,加入环氧树脂固化剂并混合均匀。Step 2: Mix 1 wt % of the adhesive mass of carbon nanotubes with ethyl acetate for ultrasonic vibration dispersion for 90 minutes, add epoxy resin components and continue ultrasonic vibration dispersion for 90 minutes, put them in a vacuum drying box to remove ethyl acetate, add epoxy resin hardener and mix well.

步骤三:将碳纤维增强树脂基复合材料放入定位夹具中,进行粘接表面涂胶处理,胶层厚度为0.8mm。Step 3: Put the carbon fiber reinforced resin-based composite material into the positioning fixture, and apply glue on the bonding surface, and the thickness of the glue layer is 0.8mm.

步骤四:通过超声振动工具头对碳纤维增强树脂基复合材料施加一定频率的超声波振动。其中,超声频率为25KHz,幅值为100μm,振幅百分比为100%,振动前通过超声振动工具头向碳纤维增强树脂基复合材料施加5MPa的预压力,振动结束后保持压力15min。Step 4: applying ultrasonic vibration of a certain frequency to the carbon fiber reinforced resin matrix composite material through the ultrasonic vibration tool head. Among them, the ultrasonic frequency is 25KHz, the amplitude is 100 μm, and the amplitude percentage is 100%. Before the vibration, a pre-pressure of 5 MPa is applied to the carbon fiber reinforced resin matrix composite material through the ultrasonic vibration tool head, and the pressure is maintained for 15 min after the vibration.

步骤五:停止超声波振动,上升超声振动工具头,将胶接件放入烘箱中,在60℃下加热固化8h。Step 5: Stop the ultrasonic vibration, raise the ultrasonic vibration tool head, put the glue joint into the oven, and heat and cure it at 60°C for 8 hours.

根据ASTM D5868-01,对单搭接试样进行拉伸实验,得到试样剪切强度为16.34MPa。According to ASTM D5868-01, the tensile test was carried out on the single lap specimen, and the shear strength of the specimen was 16.34 MPa.

根据上述实施例结果可知,实施例三的单搭接接头剪切强度最大,为24.48MPa,以下结合针对实施例三的对比例,进一步说明本工艺方法对粘接强度的促进作用。According to the results of the above examples, the shear strength of the single lap joint of Example 3 is the largest, which is 24.48MPa. The following is a further description of the promoting effect of this process method on bonding strength in conjunction with the comparative example of Example 3.

对比例1Comparative Example 1

相对于实施例三,对比例1未添加碳纳米管,步骤一、三、四、五与实施例中的相应步骤完全相同,根据ASTM D5868-01,对单搭接试样进行拉伸实验,得到试样剪切强度为5.38MPa。添加一定质量分数的碳纳米管使剪切强度提高约350%。Relative to Example 3, Comparative Example 1 did not add carbon nanotubes, and steps 1, 3, 4, and 5 were exactly the same as the corresponding steps in the embodiment. According to ASTM D5868-01, a tensile test was performed on the single-lap sample, The shear strength of the obtained sample was 5.38 MPa. Adding a certain mass fraction of carbon nanotubes increases the shear strength by about 350%.

对比例2Comparative Example 2

相对于实施例三,对比例二未对粘接面进行激光扫描处理,步骤二、三、四、五与实施例中的相应步骤完全相同,根据ASTM D5868-01,对单搭接试样进行拉伸实验,得到试样剪切强度为7.01MPa。对粘接面进行激光扫描处理使剪切强度提高约250%。Compared with Example 3, in Comparative Example 2, no laser scanning treatment was performed on the bonding surface, and steps 2, 3, 4, and 5 were exactly the same as the corresponding steps in the embodiment. The tensile test showed that the shear strength of the sample was 7.01MPa. Laser scanning treatment of the bonded surface increased shear strength by approximately 250%.

对比例3Comparative Example 3

相对于实施例三,对比例二未对待粘接试样进行超声振动处理,步骤一、二、三、五与实施例中的相应步骤完全相同,根据ASTM D5868-01,对单搭接试样进行拉伸实验,得到试样剪切强度为17.75MPa。对待粘接试样进行超声振动处理使剪切强度提高约38%。Compared with Example 3, in Comparative Example 2, the sample to be bonded is not subjected to ultrasonic vibration treatment, and steps 1, 2, 3, and 5 are exactly the same as the corresponding steps in the embodiment. According to ASTM D5868-01, the single-lap sample is The tensile test was carried out, and the shear strength of the sample was obtained as 17.75MPa. Ultrasonic vibration treatment of the samples to be bonded increases the shear strength by about 38%.

以上所述实例仅为本发明的一种实施方式,在不脱离本发明构思的前提下,还可做出若干改进和优化,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。The above-mentioned example is only an embodiment of the present invention, and several improvements and optimizations can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the appended claims.

Claims (6)

1.一种碳纤维增强树脂基复合材料连接工艺方法,其特征在于包括以下步骤:1. a carbon fiber reinforced resin matrix composite material connection process method is characterized in that comprising the following steps: 1)使用紫外脉冲激光束扫描碳纤维增强树脂基复合材料粘接面,去除表面树脂层并暴露碳纤维层,并进行清洗、晾干处理;1) Scan the bonding surface of the carbon fiber reinforced resin matrix composite material with an ultraviolet pulsed laser beam, remove the surface resin layer and expose the carbon fiber layer, and carry out cleaning and drying treatment; 2)将激光处理过的碳纤维增强树脂基复合材料固定后对粘接面涂胶并进行粘接;所用粘接剂制备方法如下:将碳纳米管与乙酸乙酯混合超声振动分散45min~90min,加入环氧树脂组分继续超声振动分散45min~90min后去除乙酸乙酯,加入环氧树脂固化剂并混合均匀;2) After fixing the laser-treated carbon fiber reinforced resin-based composite material, apply glue to the bonding surface and carry out bonding; the adhesive preparation method used is as follows: the carbon nanotubes are mixed with ethyl acetate and dispersed by ultrasonic vibration for 45min-90min, Add epoxy resin components and continue to disperse by ultrasonic vibration for 45min-90min, then remove ethyl acetate, add epoxy resin curing agent and mix evenly; 3)通过超声振动工具头对粘接面的垂直方向施加频率为15KHz~25KHz的超声波振动,振动前通过超声振动工具头施加1MPa~5MPa预压力,超声波振动结束保持压力15min~30min;3) Apply ultrasonic vibration with a frequency of 15KHz to 25KHz to the vertical direction of the bonding surface through the ultrasonic vibration tool head, apply a pre-pressure of 1MPa to 5MPa through the ultrasonic vibration tool head before the vibration, and maintain the pressure for 15min to 30min after the ultrasonic vibration; 4)将胶接件在40℃~80℃加热固化1~20h。4) Heat and cure the glued parts at 40℃~80℃ for 1~20h. 2.如权利要求1所述碳纤维增强树脂基复合材料连接工艺方法,其特征在于步骤1所用紫外脉冲激光为波长为193nm~355nm的紫外激光,光子能量为3.49eV~6.44eV,平均功率为15w~200w,重复频率为1MH~2MHz,光斑直径为1.3mm~1.5mm,扫描速度为50mm/s~1500mm/s。2. The carbon fiber reinforced resin-based composite material connection process method according to claim 1, wherein the ultraviolet pulse laser used in step 1 is an ultraviolet laser with a wavelength of 193nm~355nm, the photon energy is 3.49eV~6.44eV, and the average power is 15w ~200w, repetition frequency is 1MH~2MHz, spot diameter is 1.3mm~1.5mm, scanning speed is 50mm/s~1500mm/s. 3.如权利要求1所述碳纤维增强树脂基复合材料连接工艺方法,其特征在于步骤1所述紫外脉冲激光束扫描方向与所述碳纤维增强树脂基复合材料最外层纤维方向呈45°。3 . The method for connecting carbon fiber reinforced resin matrix composite materials according to claim 1 , wherein the scanning direction of the ultraviolet pulsed laser beam in step 1 and the direction of the outermost fiber of the carbon fiber reinforced resin matrix composite material are at 45°. 4 . 4.如权利要求1所述碳纤维增强树脂基复合材料连接工艺方法,其特征在于步骤2所述粘接剂制备过程中,每隔15min停止超声振动分散并搅拌5min,温度保持在25℃~35℃;碳纳米管在粘接剂中的质量百分数为0.2%-1%。4. The carbon fiber reinforced resin matrix composite material connection process method according to claim 1, characterized in that in the preparation process of the adhesive in step 2, the ultrasonic vibration is stopped every 15min to disperse and stir for 5min, and the temperature is maintained at 25 ℃~35 ℃. ℃; the mass percentage of carbon nanotubes in the adhesive is 0.2%-1%. 5.如权利要求1所述碳纤维增强树脂基复合材料连接工艺方法,其特征在于步骤2中胶层厚度在0.7mm~0.8mm之间。5 . The carbon fiber reinforced resin matrix composite material connection process method according to claim 1 , wherein the thickness of the adhesive layer in step 2 is between 0.7 mm and 0.8 mm. 6 . 6.如权利要求1所述碳纤维增强树脂基复合材料连接工艺方法,其特征在于步骤3中超声波振动幅值为10μm~100μm,振幅百分比为50%~100%。6 . The method for connecting carbon fiber reinforced resin matrix composite materials according to claim 1 , wherein the ultrasonic vibration amplitude in step 3 is 10 μm to 100 μm, and the amplitude percentage is 50% to 100%. 7 .
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