CN116835994A - Low-temperature connection method of alumina ceramic and 1060 pure aluminum - Google Patents
Low-temperature connection method of alumina ceramic and 1060 pure aluminum Download PDFInfo
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Abstract
本发明提供了一种氧化铝陶瓷与1060纯铝的低温连接方法,以Bi2O3、B2O3、ZnO、MgO和TiO2为原料制成铋酸盐玻璃粉,再以铋酸盐玻璃粉与有机载体制成的玻璃焊膏为钎料,将氧化铝陶瓷与1060纯铝形成待焊连接件,在420~500℃的温度下钎焊处理,实现氧化铝陶瓷与1060纯铝的低温可靠连接;与现有技术相比,本发明的铋酸盐玻璃粉具有较低的玻璃化转变温度、玻璃软化温度和热膨胀系数,降低了其与纯铝的焊接温度,实现了氧化铝陶瓷与1060纯铝的低温连接,同时其热膨胀系数与氧化铝陶瓷更为接近,降低了焊缝的残余应力,提高了接头的强度;本发明工艺简单、成本低、变形小、绿色环保,属于异种材料焊接技术领域。
The invention provides a low-temperature connection method between alumina ceramics and 1060 pure aluminum. Bi2O3 , B2O3 , ZnO, MgO and TiO2 are used as raw materials to prepare bismuthate glass powder, and then bismuthate glass powder is used as raw materials. The glass solder paste made of glass powder and organic carrier is used as solder. The alumina ceramics and 1060 pure aluminum are formed into joints to be welded. The soldering process is carried out at a temperature of 420 to 500°C to achieve the bonding between alumina ceramics and 1060 pure aluminum. Reliable connection at low temperature; compared with the existing technology, the bismuthate glass powder of the present invention has a lower glass transition temperature, glass softening temperature and thermal expansion coefficient, reduces its welding temperature with pure aluminum, and realizes alumina ceramics It is connected to 1060 pure aluminum at low temperature, and its thermal expansion coefficient is closer to that of alumina ceramics, which reduces the residual stress of the weld and improves the strength of the joint; the invention has simple process, low cost, small deformation, green and environmental protection, and is a heterogeneous Material welding technology field.
Description
技术领域Technical field
本发明涉及异种材料焊接技术领域,尤其是涉及一种氧化铝陶瓷与1060纯铝的低温连接方法。The invention relates to the technical field of dissimilar material welding, and in particular to a low-temperature connection method between alumina ceramics and 1060 pure aluminum.
背景技术Background technique
氧化铝陶瓷具有高硬度、优异的耐磨性和耐腐蚀性等优点,使之成为最广泛使用的工业陶瓷之一。纯铝作为一种仅次于钢铁被广泛应用的金属材料,具有轻质、高导电性能和高导热性能的优势。目前,氧化铝陶瓷与纯铝或铝合金的连接件已经被广泛应用于电子器件、汽车包装和轻量化零件制造等领域,例如,全铝汽车发动机中的陶瓷活塞和陶瓷挺柱就是氧化铝陶瓷与铝合金的连接件,因此,研究氧化铝陶瓷与纯铝或铝合金的连接技术具有重大的意义。Alumina ceramics have the advantages of high hardness, excellent wear resistance and corrosion resistance, making them one of the most widely used industrial ceramics. As a widely used metal material after steel, pure aluminum has the advantages of light weight, high electrical conductivity and high thermal conductivity. At present, the connectors between alumina ceramics and pure aluminum or aluminum alloys have been widely used in fields such as electronic devices, automobile packaging, and lightweight parts manufacturing. For example, ceramic pistons and ceramic tappets in all-aluminum automobile engines are alumina ceramics. Connectors with aluminum alloys, therefore, it is of great significance to study the connection technology between alumina ceramics and pure aluminum or aluminum alloys.
先前的研究表明,对陶瓷和纯铝进行连接时,需要先在陶瓷表面进行预金属化处理,形成金属薄膜,然后以金属薄膜为钎料,通过钎焊将两者连接起来,形成可靠的接头。然而,铝表面易形成一层致密的氧化铝薄膜,这会阻碍钎料在铝表面的润湿,从而降低焊接效率和焊接质量;此外,由于铝的熔点较低,仅为660℃,传统的活性金属钎焊方法所需要的焊接温度较高,不适合用于二者的连接;再者,氧化铝陶瓷与纯铝的热膨胀系数相差约3倍,这容易导致焊缝界面产生较大的残余应力,影响接头的强度。基于此,迫切需要研究一种合适的氧化铝陶瓷与纯铝的连接方法。Previous research has shown that when connecting ceramics and pure aluminum, it is necessary to pre-metallize the ceramic surface to form a metal film, and then use the metal film as a solder to connect the two through soldering to form a reliable joint. . However, the aluminum surface easily forms a dense aluminum oxide film, which will hinder the wetting of the solder on the aluminum surface, thus reducing the welding efficiency and welding quality; in addition, due to the low melting point of aluminum, which is only 660°C, traditional The active metal brazing method requires a high welding temperature and is not suitable for the connection between the two. Furthermore, the thermal expansion coefficients of alumina ceramics and pure aluminum are about three times different, which can easily lead to large residues at the weld interface. Stress affects the strength of the joint. Based on this, there is an urgent need to study a suitable connection method between alumina ceramics and pure aluminum.
发明内容Contents of the invention
为解决上述技术问题,本申请采用的技术方案是提供一种氧化铝陶瓷与1060纯铝的低温连接方法,以解决现有的陶瓷与纯铝的连接方法存在的焊接效率较低、焊接质量较差、焊接温度较高、接头强度较低的技术问题。In order to solve the above technical problems, the technical solution adopted in this application is to provide a low-temperature connection method between alumina ceramics and 1060 pure aluminum to solve the problems of low welding efficiency and poor welding quality in the existing connection methods of ceramics and pure aluminum. Technical problems include poor performance, higher welding temperature, and lower joint strength.
本申请实施例提供了一种氧化铝陶瓷与1060纯铝的低温连接方法,包括以下步骤:The embodiment of the present application provides a low-temperature connection method between alumina ceramics and 1060 pure aluminum, which includes the following steps:
(1)将Bi2O3、B2O3、ZnO、MgO和TiO2粉末混合均匀,经加热保温、水淬、研磨后,得到铋酸盐玻璃粉;(1) Mix Bi 2 O 3 , B 2 O 3 , ZnO, MgO and TiO 2 powders evenly, and obtain bismuth acid salt glass powder after heating and insulation, water quenching and grinding;
(2)对1060纯铝的待焊接面进行打磨、清洗、烘干,然后加热保温对其进行预氧化处理;(2) The surface to be welded of 1060 pure aluminum is polished, cleaned, dried, and then heated and insulated for pre-oxidation treatment;
(3)对氧化铝陶瓷的待焊接面进行机械打磨、抛光、清洗、烘干;(3) Mechanically grind, polish, clean and dry the surface to be welded of alumina ceramics;
(4)将铋酸盐玻璃粉与有机载体混合均匀制成玻璃焊膏,并均匀涂敷在氧化铝陶瓷及1060纯铝的待焊接面上,随后对向接触放置,得到待焊连接件;(4) Mix bismuthate glass powder and organic carrier evenly to make glass solder paste, and evenly apply it on the surfaces to be welded of alumina ceramics and 1060 pure aluminum, and then place them in opposite contact to obtain the connector to be welded;
(5)将待焊连接件加热至焊接温度后进行保温处理,然后冷却,最终得到氧化铝陶瓷-1060纯铝焊接接头。(5) Heat the joint to be welded to the welding temperature, perform heat preservation treatment, and then cool it to finally obtain an alumina ceramic-1060 pure aluminum welded joint.
优选的,步骤(1)中,所述铋酸盐玻璃粉包括如下质量百分数的组分:Bi2O3的含量为50~60%,B2O3的含量为30~35%,ZnO的含量为5~10%,MgO的含量为1~5%,TiO2的含量为1~5%。Preferably, in step (1), the bismuthate glass powder includes the following mass percentage components: the content of Bi 2 O 3 is 50 to 60%, the content of B 2 O 3 is 30 to 35%, and the content of ZnO is 30 to 35%. The content is 5 to 10%, the content of MgO is 1 to 5%, and the content of TiO 2 is 1 to 5%.
优选的,步骤(1)中,加热至1150~1200℃,保温60min。Preferably, in step (1), heat to 1150-1200°C and keep warm for 60 minutes.
优选的,步骤(1)中,研磨后经过300目过筛,得到直径为46~50μm的铋酸盐玻璃粉。Preferably, in step (1), after grinding, the powder is sieved with 300 mesh to obtain bismuthate glass powder with a diameter of 46 to 50 μm.
优选的,步骤(2)中,清洗的方式为超声波振动清洗,将1060纯铝依次置于丙酮溶液和无水乙醇中进行超声波振动清洗,清洗时间为10~15min。Preferably, in step (2), the cleaning method is ultrasonic vibration cleaning. 1060 pure aluminum is sequentially placed in acetone solution and absolute ethanol for ultrasonic vibration cleaning. The cleaning time is 10 to 15 minutes.
优选的,步骤(2)中,以10℃/min的加热速率加热至400~550℃,保温1~4h。Preferably, in step (2), the mixture is heated to 400-550°C at a heating rate of 10°C/min and maintained for 1-4 hours.
优选的,步骤(3)中,抛光至氧化铝陶瓷待焊接面的表面粗糙度为0.08~0.10μm;清洗的方式为超声波振动清洗,将氧化铝陶瓷依次置于丙酮溶液和无水乙醇中进行超声波振动清洗,清洗时间为10~15min。Preferably, in step (3), the surface roughness of the surface to be welded of the alumina ceramic is polished to 0.08-0.10 μm; the cleaning method is ultrasonic vibration cleaning, and the alumina ceramic is sequentially placed in an acetone solution and absolute ethanol. Ultrasonic vibration cleaning, cleaning time is 10 to 15 minutes.
优选的,步骤(4)中,所述有机载体由松油醇、乙基纤维素、乙酸乙酯、1-2丙二醇、大豆卵磷脂按照质量比65:5:15:7.5:7.5混合而成,所述铋酸盐玻璃粉与所述有机载体的质量比为7.5:1。Preferably, in step (4), the organic carrier is mixed with terpineol, ethyl cellulose, ethyl acetate, 1-2 propylene glycol, and soybean lecithin in a mass ratio of 65:5:15:7.5:7.5 , the mass ratio of the bismuthate glass powder to the organic carrier is 7.5:1.
优选的,步骤(4)中,玻璃焊膏的涂覆厚度为90~120μm。Preferably, in step (4), the coating thickness of the glass solder paste is 90-120 μm.
优选的,步骤(5)中,焊接前先对待焊连接件进行预热处理,以5~8℃/min的升温速率加热至250℃,保温10~60min;焊接时以5~8℃/min的升温速率加热至420~500℃,在焊接温度下保温10~40min。Preferably, in step (5), the joints to be welded are preheated before welding, heated to 250°C at a heating rate of 5 to 8°C/min, and kept for 10 to 60 minutes; Heating to 420~500℃ at a high heating rate, and holding at the welding temperature for 10~40min.
本发明提供了一种氧化铝陶瓷与1060纯铝的低温连接方法,以Bi2O3、B2O3、ZnO、MgO和TiO2为原料制成铋酸盐玻璃粉,再以铋酸盐玻璃粉与有机载体制成的玻璃焊膏为钎料,将氧化铝陶瓷与1060纯铝形成待焊连接件,在420~500℃的温度下钎焊处理,实现氧化铝陶瓷与1060纯铝的低温可靠连接;The invention provides a low-temperature connection method between alumina ceramics and 1060 pure aluminum. Bi2O3 , B2O3 , ZnO, MgO and TiO2 are used as raw materials to prepare bismuthate glass powder, and then bismuthate glass powder is used as raw materials. The glass solder paste made of glass powder and organic carrier is used as solder. The alumina ceramics and 1060 pure aluminum are formed into joints to be welded. The soldering process is carried out at a temperature of 420 to 500°C to achieve the bonding between alumina ceramics and 1060 pure aluminum. Reliable connection at low temperature;
与现有技术相比,本发明的有益效果为:Compared with the prior art, the beneficial effects of the present invention are:
(1)本发明的铋酸盐玻璃粉具有较低的玻璃化转变温度(Tg=320℃)、玻璃软化温度(Tf=355℃)和热膨胀系数(7.5~10×10-6K-1),降低了其与纯铝的焊接温度,实现了氧化铝陶瓷与1060纯铝的低温连接,同时其热膨胀系数与氧化铝陶瓷更为接近,降低了焊缝的残余应力,提高了接头的强度;(1) The bismuthate glass powder of the present invention has a low glass transition temperature (T g =320°C), glass softening temperature (T f =355°C) and thermal expansion coefficient (7.5~10×10 -6 K - 1 ), lowering the welding temperature with pure aluminum, achieving low-temperature connection between alumina ceramics and 1060 pure aluminum, and at the same time, its thermal expansion coefficient is closer to that of alumina ceramics, reducing the residual stress of the weld and improving the joint strength strength;
(2)本发明的铋酸盐玻璃粉增加了MgO和TiO2两种原料,TiO2中的钛在玻璃网络中以Ti4+的形式存在,增大了玻璃中氧原子的堆积密度,提高了玻璃网络结构的紧密性,从而提高了玻璃的热稳定性;MgO的存在能提高玻璃的化学稳定性和机械强度,并能降低玻璃的结晶倾向,避免玻璃由于析晶而变脆;MgO和TiO2的添加提高了接头的强度,实现了氧化铝陶瓷与1060纯铝的可靠连接;(2) The bismuthate glass powder of the present invention adds two raw materials, MgO and TiO 2. The titanium in TiO 2 exists in the form of Ti 4+ in the glass network, which increases the packing density of oxygen atoms in the glass and improves It improves the tightness of the glass network structure, thereby improving the thermal stability of the glass; the presence of MgO can improve the chemical stability and mechanical strength of the glass, and can reduce the crystallization tendency of the glass and prevent the glass from becoming brittle due to crystallization; MgO and The addition of TiO 2 improves the strength of the joint and achieves a reliable connection between alumina ceramics and 1060 pure aluminum;
(3)本发明通过对1060纯铝进行预氧化处理,提高了钎料在铝表面的润湿,解决金属表面氧化膜对钎焊过程产生不利影响的技术问题,提升了1060纯铝与玻璃钎料的封接工艺的密封性,从而提高了焊接效率和焊接质量;(3) By pre-oxidizing 1060 pure aluminum, the present invention improves the wetting of the solder material on the aluminum surface, solves the technical problem of the adverse impact of the oxide film on the metal surface on the brazing process, and improves the performance of the soldering process between 1060 pure aluminum and glass. The sealing of the material sealing process improves the welding efficiency and welding quality;
(4)本发明通过对待焊连接件进行预热处理,使得有机载体能充分挥发,避免焊接接头中产生气孔,提高接头的质量和强度;(4) In the present invention, by preheating the joints to be welded, the organic carrier can be fully volatilized, avoiding the generation of pores in the welded joints, and improving the quality and strength of the joints;
(5)本发明工艺简单、成本低、变形小、绿色环保,氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度为14~24MPa,钎焊接头组织致密,保证了氧化铝陶瓷与1060纯铝连接的可靠性。(5) The process of the present invention is simple, low in cost, small in deformation, and environmentally friendly. The room temperature shear strength of the alumina ceramic-1060 pure aluminum welded joint is 14 to 24 MPa. The brazed joint has a dense structure, ensuring that the alumina ceramic and 1060 pure aluminum welded joints are Reliability of aluminum connections.
附图说明Description of the drawings
为了更清楚地说明本申请实施例中的技术方案,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申请的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the embodiments or description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only for the purpose of the present application. For some embodiments, for those of ordinary skill in the art, other drawings can be obtained based on these drawings without exerting creative efforts.
图1为本申请实施例10中氧化铝陶瓷-1060纯铝焊接接头的微观组织图;Figure 1 is a microstructure diagram of the alumina ceramic-1060 pure aluminum welded joint in Example 10 of the present application;
图2为本申请对比例1中氧化铝陶瓷-1060纯铝焊接接头的微观组织图。Figure 2 is a microstructure diagram of the alumina ceramic-1060 pure aluminum welded joint in Comparative Example 1 of the present application.
图中符号说明:Explanation of symbols in the figure:
1.氧化铝陶瓷;2.1060纯铝。1. Alumina ceramic; 2.1060 pure aluminum.
具体实施方式Detailed ways
为了使本申请所要解决的技术问题、技术方案及有益效果更加清楚明白,以下结合附图及实施例,对本申请进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本申请,并不用于限定本申请。本发明中所使用的原料和装置,如无特殊规定,均为常规的市售产品;所使用的方法,如无特殊规定,均为常规的方法。In order to make the technical problems, technical solutions and beneficial effects to be solved by this application more clear, this application will be further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the present application and are not used to limit the present application. The raw materials and devices used in the present invention, unless otherwise specified, are all conventional commercially available products; the methods used, unless otherwise specified, are conventional methods.
实施例1Example 1
本实施例提供了一种氧化铝陶瓷与1060纯铝的低温连接方法,包括以下步骤:This embodiment provides a low-temperature connection method between alumina ceramics and 1060 pure aluminum, which includes the following steps:
(1)按照质量百分数分别称取50%Bi2O3、35%B2O3、5%ZnO、5%MgO和5%TiO2粉末,并置于滚筒式球磨机中混合均匀,然后将混合后的粉末放置于马弗炉中,加热至1150~1200℃保温60min,得到熔融态的玻璃,对熔融态的玻璃进行水淬,得到玻璃颗粒,将玻璃颗粒研磨后经过300目过筛,得到直径为46~50μm的铋酸盐玻璃粉;(1) Weigh 50% Bi 2 O 3 , 35% B 2 O 3 , 5% ZnO, 5% MgO and 5% TiO 2 powder respectively according to mass percentage, and mix them evenly in a drum ball mill, and then mix The final powder is placed in a muffle furnace, heated to 1150~1200°C and kept for 60 minutes to obtain molten glass. The molten glass is quenched with water to obtain glass particles. The glass particles are ground and sieved through 300 mesh to obtain Bismuthate glass powder with a diameter of 46 to 50 μm;
(2)使用砂纸对1060纯铝的待焊接面进行打磨,然后将1060纯铝依次置于丙酮溶液和无水乙醇中进行超声波振动清洗,清洗时间为10~15min,清洗完毕后将1060纯铝烘干,然后将其放置于马弗炉中,以10℃/min的加热速率加热至400℃,保温1h对其进行预氧化处理,然后随炉冷却;(2) Use sandpaper to polish the surface to be welded of 1060 pure aluminum, and then place the 1060 pure aluminum in an acetone solution and absolute ethanol for ultrasonic vibration cleaning. The cleaning time is 10 to 15 minutes. After cleaning, remove the 1060 pure aluminum. Dry it, then place it in a muffle furnace, heat it to 400°C at a heating rate of 10°C/min, keep it for 1 hour to pre-oxidize, and then cool it in the furnace;
(3)使用金刚石沙盘对氧化铝陶瓷的待焊接面进行机械打磨,并抛光至氧化铝陶瓷待焊接面的表面粗糙度为0.08~0.10μm,然后将氧化铝陶瓷依次置于丙酮溶液和无水乙醇中进行超声波振动清洗,清洗时间为10~15min,清洗完毕后将氧化铝陶瓷烘干;(3) Use a diamond sand table to mechanically grind the surface of the alumina ceramic to be welded, and polish it until the surface roughness of the surface to be welded is 0.08-0.10 μm, and then place the alumina ceramic in an acetone solution and anhydrous solution in sequence. Carry out ultrasonic vibration cleaning in ethanol, the cleaning time is 10 to 15 minutes, and dry the alumina ceramics after cleaning;
(4)将松油醇、乙基纤维素、乙酸乙酯、1-2丙二醇、大豆卵磷脂按照质量比65:5:15:7.5:7.5混合均匀,得到有机载体,再将铋酸盐玻璃粉与有机载体按照质量比7.5:1混合,并置于行星式重力搅拌机中混合均匀,制成玻璃焊膏,将玻璃焊膏均匀涂敷在氧化铝陶瓷及1060纯铝的待焊接面上,涂覆厚度为90~120μm,随后将氧化铝陶瓷与1060纯铝对向接触放置,得到待焊连接件;(4) Mix terpineol, ethyl cellulose, ethyl acetate, 1-2 propylene glycol, and soy lecithin according to the mass ratio of 65:5:15:7.5:7.5 to obtain an organic carrier, and then add bismuth acid salt glass The powder and organic carrier are mixed according to the mass ratio of 7.5:1, and placed in a planetary gravity mixer to mix evenly to form a glass solder paste. The glass solder paste is evenly applied on the surfaces to be welded of alumina ceramics and 1060 pure aluminum. The coating thickness is 90-120 μm, and then the alumina ceramics and 1060 pure aluminum are placed in opposing contact to obtain the connector to be welded;
(5)将待焊连接件放置于马弗炉中,先对待焊连接件进行预热处理,以5~8℃/min的升温速率加热至250℃,保温30min,然后对焊接件进行焊接,以5~8℃/min的升温速率加热至420℃,保温10min,随炉冷却,最终得到氧化铝陶瓷-1060纯铝焊接接头。(5) Place the joints to be welded in the muffle furnace, preheat the joints to be welded first, heat to 250°C at a heating rate of 5 to 8°C/min, keep the heat for 30 minutes, and then weld the welded parts. Heating to 420°C at a heating rate of 5 to 8°C/min, holding for 10 minutes, and then cooling in the furnace, finally obtaining an alumina ceramic-1060 pure aluminum welded joint.
对实施例1的氧化铝陶瓷-1060纯铝焊接接头进行力学性能测试,测得其室温抗剪强度如表1所示。The mechanical properties of the alumina ceramic-1060 pure aluminum welded joint in Example 1 were tested, and the measured room temperature shear strength is shown in Table 1.
实施例2Example 2
本实施方法和实施例1不同的是:步骤(1)中,按照质量百分数分别称取55%Bi2O3、32%B2O3、7%ZnO、3%MgO和3%TiO2粉末,其他步骤相同,最终得到氧化铝陶瓷-1060纯铝焊接接头,测得其室温抗剪强度如表1所示。The difference between this implementation method and Example 1 is that in step (1), 55% Bi 2 O 3 , 32% B 2 O 3 , 7% ZnO, 3% MgO and 3% TiO 2 powders are weighed according to mass percentages. , other steps are the same, and the alumina ceramic-1060 pure aluminum welded joint is finally obtained. The measured room temperature shear strength is shown in Table 1.
实施例3Example 3
本实施方法和实施例1不同的是:步骤(1)中,按照质量百分数分别称取60%Bi2O3、30%B2O3、8%ZnO、1%MgO和1%TiO2粉末,其他步骤相同,最终得到氧化铝陶瓷-1060纯铝焊接接头,测得其室温抗剪强度如表1所示。The difference between this implementation method and Example 1 is that in step (1), 60% Bi 2 O 3 , 30% B 2 O 3 , 8% ZnO, 1% MgO and 1% TiO 2 powder are respectively weighed according to mass percentages. , other steps are the same, and the alumina ceramic-1060 pure aluminum welded joint is finally obtained. The measured room temperature shear strength is shown in Table 1.
表1实施例1~3的焊接接头的工艺参数和室温抗剪强度Table 1 Process parameters and room temperature shear strength of the welded joints of Examples 1 to 3
请参阅表1,当铋酸盐玻璃粉中各原料的含量不同时,氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度也随之变化,Bi2O3/B2O3的数值越高,氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度就越高。Please refer to Table 1. When the content of each raw material in the bismuthate glass powder is different, the room temperature shear strength of the alumina ceramic-1060 pure aluminum welded joint also changes accordingly. The higher the value of Bi 2 O 3 /B 2 O 3 The higher the room temperature shear strength of the alumina ceramic-1060 pure aluminum welded joint.
实施例4Example 4
本实施方法和实施例3不同的是:步骤(2)中,以10℃/min的加热速率加热至480℃,其他步骤相同,最终得到氧化铝陶瓷-1060纯铝焊接接头,测得其室温抗剪强度如表2所示。The difference between this implementation method and Example 3 is that in step (2), the heating rate is 10°C/min to 480°C. The other steps are the same. Finally, an alumina ceramic-1060 pure aluminum welded joint is obtained, and its room temperature is measured. The shear strength is shown in Table 2.
实施例5Example 5
本实施方法和实施例3不同的是:步骤(2)中,以10℃/min的加热速率加热至550℃,其他步骤相同,最终得到氧化铝陶瓷-1060纯铝焊接接头,测得其室温抗剪强度如表2所示。The difference between this implementation method and Example 3 is that in step (2), it is heated to 550°C at a heating rate of 10°C/min. The other steps are the same. Finally, an alumina ceramic-1060 pure aluminum welded joint is obtained, and its room temperature is measured. The shear strength is shown in Table 2.
表2实施例3~5的焊接接头的工艺参数和室温抗剪强度Table 2 Process parameters and room temperature shear strength of the welded joints of Examples 3 to 5
请参阅表2,随着预氧化处理过程中温度的升高,氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度逐渐升高,当温度为550℃时,氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度最高,达到16.43MPa;因此,预氧化处理过程中的温度优选为550℃。Please refer to Table 2. As the temperature increases during the pre-oxidation treatment, the room temperature shear strength of the alumina ceramic-1060 pure aluminum welded joint gradually increases. When the temperature is 550°C, the room temperature shear strength of the alumina ceramic-1060 pure aluminum welded joint increases. The room temperature shear strength of the joint is the highest, reaching 16.43MPa; therefore, the temperature during the pre-oxidation treatment is preferably 550°C.
实施例6Example 6
本实施方法和实施例5不同的是:步骤(2)中,保温2.5h对其进行预氧化处理,其他步骤相同,最终得到氧化铝陶瓷-1060纯铝焊接接头,测得其室温抗剪强度如表3所示。The difference between this implementation method and Example 5 is that in step (2), it is pre-oxidized by holding it for 2.5 hours. The other steps are the same. Finally, an alumina ceramic-1060 pure aluminum welded joint is obtained, and its room temperature shear strength is measured. as shown in Table 3.
实施例7Example 7
本实施方法和实施例5不同的是:步骤(2)中,保温4h对其进行预氧化处理,其他步骤相同,最终得到氧化铝陶瓷-1060纯铝焊接接头,测得其室温抗剪强度如表3所示。The difference between this implementation method and Example 5 is that in step (2), it is pre-oxidized by holding it for 4 hours, and the other steps are the same. Finally, an alumina ceramic-1060 pure aluminum welded joint is obtained, and its room temperature shear strength is measured as follows As shown in Table 3.
表3实施例5~7的焊接接头的工艺参数和室温抗剪强度Table 3 Process parameters and room temperature shear strength of the welded joints of Examples 5 to 7
请参阅表3,随着预氧化处理过程中保温时间的延长,氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度先升高后趋于稳定,当保温时间为2.5h时,氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度最高,达到17.36MPa;因此,预氧化处理过程中的保温时间优选为2.5h。Please refer to Table 3. As the holding time increases during the pre-oxidation treatment, the room temperature shear strength of the alumina ceramic-1060 pure aluminum welded joint increases first and then becomes stable. When the holding time is 2.5h, the room temperature shear strength of the alumina ceramic-1060 pure aluminum welded joint increases. -1060 pure aluminum welded joints have the highest room temperature shear strength, reaching 17.36MPa; therefore, the holding time during the pre-oxidation process is preferably 2.5h.
实施例8Example 8
本实施方法和实施例6不同的是:步骤(5)中,焊接温度为460℃,其他步骤相同,最终得到氧化铝陶瓷-1060纯铝焊接接头,测得其室温抗剪强度如表4所示。The difference between this implementation method and Example 6 is that in step (5), the welding temperature is 460°C, and other steps are the same. Finally, an alumina ceramic-1060 pure aluminum welded joint is obtained, and its room temperature shear strength is measured as shown in Table 4. Show.
实施例9Example 9
本实施方法和实施例6不同的是:步骤(5)中,焊接温度为500℃,其他步骤相同,最终得到氧化铝陶瓷-1060纯铝焊接接头,测得其室温抗剪强度如表4所示。The difference between this implementation method and Example 6 is that in step (5), the welding temperature is 500°C, and other steps are the same. Finally, an alumina ceramic-1060 pure aluminum welded joint is obtained, and its room temperature shear strength is measured as shown in Table 4. Show.
表4实施例6、8~9的焊接接头的工艺参数和室温抗剪强度Table 4 Process parameters and room temperature shear strength of the welded joints of Examples 6, 8-9
请参阅表4,随着焊接过程中温度的升高,氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度先升高后降低,当温度为460℃时,氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度最高,达到19.28MPa;因此,焊接过程中的温度优选为460℃。Please refer to Table 4. As the temperature increases during the welding process, the room temperature shear strength of the alumina ceramic-1060 pure aluminum welded joint first increases and then decreases. When the temperature is 460°C, the room temperature shear strength of the alumina ceramic-1060 pure aluminum welded joint The room temperature shear strength of the joint is the highest, reaching 19.28MPa; therefore, the temperature during the welding process is preferably 460°C.
实施例10Example 10
本实施方法和实施例8不同的是:步骤(5)中,焊接过程中保温30min,其他步骤相同,最终得到氧化铝陶瓷-1060纯铝焊接接头,测得其室温抗剪强度如表5所示。The difference between this implementation method and Example 8 is that in step (5), the temperature is maintained for 30 minutes during the welding process. The other steps are the same. Finally, an alumina ceramic-1060 pure aluminum welded joint is obtained. The room temperature shear strength is measured as shown in Table 5. Show.
实施例11Example 11
本实施方法和实施例8不同的是:步骤(5)中,焊接过程中保温40min,其他步骤相同,最终得到氧化铝陶瓷-1060纯铝焊接接头,测得其室温抗剪强度如表5所示。The difference between this implementation method and Example 8 is that in step (5), the temperature is maintained for 40 minutes during the welding process. The other steps are the same. Finally, an alumina ceramic-1060 pure aluminum welded joint is obtained. The measured room temperature shear strength is as shown in Table 5. Show.
表5实施例8、10~11的焊接接头的工艺参数和室温抗剪强度Table 5 Process parameters and room temperature shear strength of the welded joints of Examples 8, 10-11
请参阅表5,随着焊接过程中保温时间的升高,氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度先升高后降低,当保温时间为30min时,氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度最高,达到23.39MPa;因此,焊接过程中的保温时间优选为30min。Please refer to Table 5. As the holding time increases during the welding process, the room temperature shear strength of the alumina ceramic-1060 pure aluminum welded joint first increases and then decreases. When the holding time is 30 minutes, the room temperature shear strength of the alumina ceramic-1060 pure aluminum welded joint increases. The room temperature shear strength of the welded joint is the highest, reaching 23.39MPa; therefore, the holding time during the welding process is preferably 30 minutes.
综上所述,氧化铝陶瓷与1060纯铝的钎焊工艺的较佳条件为:预氧化处理过程中的温度为550℃,保温时间为2.5h,预热处理过程中的温度为250℃,保温时间为30min,焊接过程中的温度为460℃,保温时间为30min;通过扫描电子显微镜(SEM)对实施例10的氧化铝陶瓷-1060纯铝焊接接头进行微观观察,得到其微观组织图如图1所示,由图1可知,氧化铝陶瓷-1060纯铝焊接接头组织致密,未出现未焊合的地方,未出现裂纹。In summary, the optimal conditions for the brazing process of alumina ceramics and 1060 pure aluminum are: the temperature during the pre-oxidation treatment is 550°C, the holding time is 2.5h, and the temperature during the preheating treatment is 250°C. The holding time is 30 minutes, the temperature during the welding process is 460°C, and the holding time is 30 minutes; the alumina ceramic-1060 pure aluminum welded joint of Example 10 is microscopically observed through a scanning electron microscope (SEM), and the microstructure diagram is obtained as follows: As shown in Figure 1, it can be seen from Figure 1 that the alumina ceramic-1060 pure aluminum welded joint has a dense structure, no unwelded areas, and no cracks.
对比例1Comparative example 1
本实施方法和实施例10不同的是:步骤(2)中,将1060纯铝烘干后,不对其进行预氧化处理,其他步骤相同,最终得到氧化铝陶瓷-1060纯铝焊接接头,其微观组织图如图2所示,测得其室温抗剪强度如表6所示。The difference between this implementation method and Example 10 is that in step (2), after drying the 1060 pure aluminum, no pre-oxidation treatment is performed. The other steps are the same, and finally an alumina ceramic-1060 pure aluminum welded joint is obtained. The microscopic The tissue diagram is shown in Figure 2, and the measured room temperature shear strength is shown in Table 6.
表6实施例10与对比例1的焊接接头的工艺参数和室温抗剪强度Table 6 Process parameters and room temperature shear strength of the welded joints of Example 10 and Comparative Example 1
请参阅表6,当不对1060纯铝进行预氧化处理时,得到的氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度明显降低;请参阅图2,对比例1的氧化铝陶瓷-1060纯铝焊接接头出现了明显的裂纹,由此可知,对1060纯铝表面的预氧化处理有助于提升其与玻璃钎料的封接工艺的密封性,解决金属表面氧化膜对钎焊过程产生不利影响的技术问题,从而提高焊缝的质量,提高接头的室温抗剪强度。Please refer to Table 6. When the 1060 pure aluminum is not pre-oxidized, the room temperature shear strength of the obtained alumina ceramic-1060 pure aluminum welded joint is significantly reduced; please refer to Figure 2, the alumina ceramic-1060 pure aluminum in Comparative Example 1 There are obvious cracks in the aluminum welded joints. It can be seen that the pre-oxidation treatment on the surface of 1060 pure aluminum can help improve the sealing performance of the sealing process with the glass solder and solve the problem of the oxide film on the metal surface that is detrimental to the brazing process. affect the technical issues, thereby improving the quality of the weld and improving the room temperature shear strength of the joint.
本发明提供了一种氧化铝陶瓷与1060纯铝的低温连接方法,以Bi2O3、B2O3、ZnO、MgO和TiO2为原料制成铋酸盐玻璃粉,再以铋酸盐玻璃粉与有机载体制成的玻璃焊膏为钎料,将氧化铝陶瓷与1060纯铝形成待焊连接件,在420~500℃的温度下钎焊处理,实现氧化铝陶瓷与1060纯铝的低温可靠连接;The invention provides a low-temperature connection method between alumina ceramics and 1060 pure aluminum. Bi2O3 , B2O3 , ZnO, MgO and TiO2 are used as raw materials to prepare bismuthate glass powder, and then bismuthate glass powder is used as raw materials. The glass solder paste made of glass powder and organic carrier is used as solder. The alumina ceramics and 1060 pure aluminum are formed into joints to be welded. The soldering process is carried out at a temperature of 420 to 500°C to achieve the bonding between alumina ceramics and 1060 pure aluminum. Reliable connection at low temperature;
与现有技术相比,(1)本发明的铋酸盐玻璃粉具有较低的玻璃化转变温度(Tg=320℃)、玻璃软化温度(Tf=355℃)和热膨胀系数(7.5~10×10-6K-1),降低了其与纯铝的焊接温度,实现了氧化铝陶瓷与1060纯铝的低温连接,同时其热膨胀系数与氧化铝陶瓷更为接近,降低了焊缝的残余应力,提高了接头的强度;(2)本发明的铋酸盐玻璃粉增加了MgO和TiO2两种原料,TiO2中的钛在玻璃网络中以Ti4+的形式存在,增大了玻璃中氧原子的堆积密度,提高了玻璃网络结构的紧密性,从而提高了玻璃的热稳定性;MgO的存在能提高玻璃的化学稳定性和机械强度,并能降低玻璃的结晶倾向,避免玻璃由于析晶而变脆;MgO和TiO2的添加提高了接头的强度,实现了氧化铝陶瓷与1060纯铝的可靠连接;(3)本发明通过对1060纯铝进行预氧化处理,提高了钎料在铝表面的润湿,解决金属表面氧化膜对钎焊过程产生不利影响的技术问题,提升了1060纯铝与玻璃钎料的封接工艺的密封性,从而提高了焊接效率和焊接质量;(4)本发明通过对待焊连接件进行预热处理,使得有机载体能充分挥发,避免焊接接头中产生气孔,提高接头的质量和强度;(5)本发明工艺简单、成本低、变形小、绿色环保,氧化铝陶瓷-1060纯铝焊接接头的室温抗剪强度为14~24MPa,钎焊接头组织致密,保证了氧化铝陶瓷与1060纯铝连接的可靠性;可广泛应用于异种材料焊接技术领域。Compared with the prior art, (1) the bismuthate glass powder of the present invention has a lower glass transition temperature (T g =320°C), glass softening temperature (T f =355°C) and thermal expansion coefficient (7.5~ 10×10 -6 K -1 ), which reduces the welding temperature with pure aluminum and realizes the low-temperature connection between alumina ceramics and 1060 pure aluminum. At the same time, its thermal expansion coefficient is closer to that of alumina ceramics, reducing the welding seam. Residual stress improves the strength of the joint; (2) The bismuthate glass powder of the present invention adds two raw materials: MgO and TiO 2. The titanium in TiO 2 exists in the form of Ti 4+ in the glass network, increasing the The packing density of oxygen atoms in the glass improves the tightness of the glass network structure, thereby improving the thermal stability of the glass; the presence of MgO can improve the chemical stability and mechanical strength of the glass, and can reduce the crystallization tendency of the glass and prevent the glass from crystallizing. It becomes brittle due to crystallization; the addition of MgO and TiO 2 improves the strength of the joint and realizes a reliable connection between alumina ceramics and 1060 pure aluminum; (3) The present invention improves the brazing efficiency by pre-oxidizing 1060 pure aluminum. The wetting of the material on the aluminum surface solves the technical problem of the negative impact of the oxide film on the metal surface on the brazing process, and improves the sealing performance of the sealing process between 1060 pure aluminum and glass brazing material, thus improving the welding efficiency and welding quality; (4) In the present invention, by preheating the joints to be welded, the organic carrier can be fully volatilized, avoiding the generation of pores in the welded joints, and improving the quality and strength of the joints; (5) The present invention has simple process, low cost, small deformation, Green and environmentally friendly, the room temperature shear strength of the alumina ceramic-1060 pure aluminum welded joint is 14-24MPa, and the brazed joint has a dense structure, ensuring the reliability of the connection between alumina ceramics and 1060 pure aluminum; it can be widely used in dissimilar material welding technology field.
需要说明的是:上述实施例中,预热处理过程中的保温时间设置为30min,仅作为较佳实施例,在实际生产中,预热处理过程中的保温时间可以设置为10~60min,在范围内即可。It should be noted that in the above embodiment, the holding time during the preheating process is set to 30 minutes. This is only a preferred embodiment. In actual production, the holding time during the preheating process can be set to 10 to 60 minutes. Just within the range.
以上所述实施例仅用以说明本申请的技术方案,而非对其限制;尽管参照前述实施例对本申请进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本申请各实施例技术方案的精神和范围,均应包含在本申请的保护范围之内。The above-described embodiments are only used to illustrate the technical solutions of the present application, but not to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still implement the above-mentioned implementations. The technical solutions described in the examples are modified, or some of the technical features are equivalently replaced; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions in the embodiments of this application, and should be included in within the protection scope of this application.
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