CN103058700A - Insulating sealed metal air pipe as well as sealed connection method of metal pipes and ceramic pipe - Google Patents
Insulating sealed metal air pipe as well as sealed connection method of metal pipes and ceramic pipe Download PDFInfo
- Publication number
- CN103058700A CN103058700A CN2013100432617A CN201310043261A CN103058700A CN 103058700 A CN103058700 A CN 103058700A CN 2013100432617 A CN2013100432617 A CN 2013100432617A CN 201310043261 A CN201310043261 A CN 201310043261A CN 103058700 A CN103058700 A CN 103058700A
- Authority
- CN
- China
- Prior art keywords
- metal
- sealing layer
- pipe
- wall
- ceramic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Ceramic Products (AREA)
Abstract
本发明提供一种绝缘密封金属气管,包括:第一金属管、第二金属管和陶瓷管;所述陶瓷管的内壁与所述第一金属管的外壁形成第一空间,所述第一空间的两端设置有氧化物密封层,所述第一空间内部填充有金属密封层;所述陶瓷管的内壁与所述第二金属管的外壁形成第二空间,所述第二空间的两端设置有氧化物密封层,所述第二空间内部填充有金属密封层。本发明还涉及金属管与陶瓷管的绝缘密封方法为:在陶瓷管内壁形成第一金属密封层和第二金属密封层;在所述第一金属密封层的两端及第二金属密封层两端分别涂覆氧化物密封浆料;将两个金属管分别与金属密封层焊接。所述绝缘密封金属气管适用于高温情况下的各种环境气氛。The present invention provides an insulated and sealed metal air pipe, comprising: a first metal pipe, a second metal pipe and a ceramic pipe; the inner wall of the ceramic pipe and the outer wall of the first metal pipe form a first space, and the first space The two ends of the ceramic tube are provided with an oxide sealing layer, and the inside of the first space is filled with a metal sealing layer; the inner wall of the ceramic tube and the outer wall of the second metal tube form a second space, and the two ends of the second space An oxide sealing layer is provided, and the second space is filled with a metal sealing layer. The present invention also relates to a method for insulating and sealing metal pipes and ceramic pipes: forming a first metal sealing layer and a second metal sealing layer on the inner wall of the ceramic pipe; The ends are respectively coated with oxide sealing slurry; the two metal pipes are respectively welded to the metal sealing layer. The insulated and sealed metal gas pipe is suitable for various ambient atmospheres under high temperature conditions.
Description
技术领域technical field
本发明涉及金属连接领域,特别涉及绝缘密封金属气管及金属管与陶瓷管的密封连接方法。The invention relates to the field of metal connection, in particular to an insulated and sealed metal air pipe and a method for sealing connection between the metal pipe and the ceramic pipe.
背景技术Background technique
金属与陶瓷封接是一种使用陶瓷介质与金属连接的技术,该技术使高温下工作的金属保持了绝缘性,主要应用于真空电子器件、半导体、集成电路、电光源、激光原子能、化工、冶金、电力设备等行业。Metal and ceramic sealing is a technology that uses ceramic media to connect metals. This technology keeps metals working at high temperatures insulated. It is mainly used in vacuum electronic devices, semiconductors, integrated circuits, electric light sources, laser atomic energy, chemical industry, Metallurgy, power equipment and other industries.
金属与陶瓷之间的封接方法主要有三种:There are three main methods of sealing between metal and ceramics:
一种为氧化物焊料法,又称玻璃焊料法,即利用焊料熔化形成玻璃向陶瓷渗透并浸润金属表面,从而完成陶瓷与金属的封接。One is the oxide solder method, also known as the glass solder method, which uses the melting of solder to form glass that penetrates into the ceramic and infiltrates the metal surface, thereby completing the sealing of the ceramic and the metal.
一种是烧结金属粉末法,即首先将在还原型气氛中用高温在陶瓷上烧结一层金属层,使陶瓷表面带有金属性质,然后再将其与金属进行焊接,从而完成陶瓷与金属的封接。One is the sintered metal powder method, that is, firstly, a metal layer is sintered on the ceramic at high temperature in a reducing atmosphere, so that the surface of the ceramic has metallic properties, and then it is welded with the metal to complete the bonding between the ceramic and the metal. seal.
一种是活性金属法,即利用钛、锆、铪等过渡金属元素与铜、镍、银等金属在低于各自熔点的温度下形成合金,这些合金在液相态下与陶瓷表面发生反应并浸润各种金属,从而完成陶瓷与金属的封接。One is the active metal method, which uses transition metal elements such as titanium, zirconium, and hafnium to form alloys with metals such as copper, nickel, and silver at temperatures lower than their respective melting points. These alloys react with the ceramic surface in the liquid phase and Infiltration of various metals to complete the sealing of ceramics and metals.
由于烧结金属粉末法或活性金属法涉及适用金属,如铜、镍、钛等金属,这些金属在高温下会发生氧化反应,容易使封接处出现老化,因此烧结金属粉末法或活性金属法在高温下只能工作于中性或还原型气氛中,而不能工作于氧化气氛中。Since the sintered metal powder method or active metal method involves applicable metals, such as copper, nickel, titanium and other metals, these metals will undergo oxidation reactions at high temperatures, which will easily cause aging of the seal, so the sintered metal powder method or active metal method in It can only work in neutral or reducing atmosphere at high temperature, but not in oxidizing atmosphere.
发明内容Contents of the invention
本发明解决的技术问题在于提供一种绝缘密封金属气管及金属管与陶瓷管的密封连接方法,适用于高温情况下的各种环境气氛。The technical problem to be solved by the present invention is to provide an insulated and sealed metal air pipe and a method for sealing connection between the metal pipe and the ceramic pipe, which is suitable for various ambient atmospheres under high temperature conditions.
本发明提供了一种绝缘密封金属气管,包括:第一金属管、第二金属管和内壁分别与所述第一金属管的外壁和第二金属管的外壁相连的陶瓷管;The present invention provides an insulated and sealed metal air pipe, comprising: a first metal pipe, a second metal pipe and a ceramic pipe whose inner wall is respectively connected to the outer wall of the first metal pipe and the outer wall of the second metal pipe;
所述陶瓷管的内壁与所述第一金属管的外壁形成第一空间,所述第一空间的两端设置有氧化物密封层,所述第一空间内部填充有金属密封层;The inner wall of the ceramic tube and the outer wall of the first metal tube form a first space, both ends of the first space are provided with an oxide sealing layer, and the inside of the first space is filled with a metal sealing layer;
所述陶瓷管的内壁与所述第二金属管的外壁形成第二空间,所述第二空间的两端设置有氧化物密封层,所述第二空间内部填充有金属密封层。The inner wall of the ceramic tube and the outer wall of the second metal tube form a second space, both ends of the second space are provided with an oxide sealing layer, and the inside of the second space is filled with a metal sealing layer.
优选的,所述金属密封层包括Mo,Mn,W,Cu,Ti,Ag,Au,Ni,Zr,Nb,Be,V,Zn,Sn和Pb中的一种或多种。Preferably, the metal sealing layer includes one or more of Mo, Mn, W, Cu, Ti, Ag, Au, Ni, Zr, Nb, Be, V, Zn, Sn and Pb.
优选的,所述氧化物密封层包括SiO2、Al2O3、B2O3、ZnO、RO和A2O中的一种或多种,所述RO为MgO、CaO、SrO或BaO,所述A2O为K2O、Na2O或Li2O。Preferably, the oxide sealing layer includes one or more of SiO 2 , Al 2 O 3 , B 2 O 3 , ZnO, RO and A 2 O, and the RO is MgO, CaO, SrO or BaO, The A 2 O is K 2 O, Na 2 O or Li 2 O.
优选的,所述第一金属管和第二金属管的膨胀系数大于陶瓷管的热膨胀系数。Preferably, the expansion coefficients of the first metal tube and the second metal tube are greater than the thermal expansion coefficient of the ceramic tube.
优选的,所述陶瓷管内各处的横截面积一致。Preferably, the cross-sectional area of each place in the ceramic tube is consistent.
优选的,所述陶瓷管内两端的横截面积大于中部的横截面积。Preferably, the cross-sectional area of the two ends of the ceramic tube is larger than the cross-sectional area of the middle part.
本发明还提供了一种金属管与陶瓷管的绝缘密封方法,包括以下步骤:The present invention also provides a method for insulating and sealing metal pipes and ceramic pipes, comprising the following steps:
(A)在陶瓷管内壁的两端分别涂覆金属密封浆料,进行烧结,形成第一金属密封层和第二金属密封层;(A) Coating metal sealing slurry on both ends of the inner wall of the ceramic tube, and sintering to form the first metal sealing layer and the second metal sealing layer;
(B)在所述第一金属密封层的两端涂覆氧化物密封浆料使所述第一金属密封层的两端与空气隔绝;(B) Coating oxide sealing slurry on both ends of the first metal sealing layer to isolate both ends of the first metal sealing layer from air;
在所述第二金属密封层的两端分别涂覆氧化物密封浆料,使第二金属密封层的两端与空气隔绝;Coating oxide sealing slurry on both ends of the second metal sealing layer, so that the two ends of the second metal sealing layer are isolated from the air;
(C)将第一金属管与第一金属密封层焊接,使第一金属密封层与空气隔绝;将第二金属管与第二金属密封层焊接,使第二金属密封层与空气隔绝。(C) welding the first metal tube to the first metal sealing layer to isolate the first metal sealing layer from the air; welding the second metal tube to the second metal sealing layer to isolate the second metal sealing layer from the air.
优选的,所述步骤(A)中,所述烧结的温度为1400~1600℃,所述烧结时间为50~70分钟。Preferably, in the step (A), the sintering temperature is 1400-1600° C., and the sintering time is 50-70 minutes.
优选的,在步骤(A)后还包括在第一金属层和第二金属层上镀镍。Preferably, nickel plating on the first metal layer and the second metal layer is also included after the step (A).
优选的,所述步骤(C)中,所述焊接的方法为钎焊,所述钎焊的温度为1000~1200℃。Preferably, in the step (C), the welding method is brazing, and the brazing temperature is 1000-1200°C.
与现有技术相比,本发明的绝缘密封金属气管包括:第一金属管、第二金属管和内壁分别与所述第一金属管的外壁和第二金属管的外壁相连的陶瓷管;所述陶瓷管的内壁与所述第一金属管的外壁形成第一空间,所述第一空间的两端设置有氧化物密封层,所述第一空间内部填充有金属密封层;所述陶瓷管的内壁与所述第二金属管的外壁形成第二空间,所述第二空间的两端设置有氧化物密封层,所述第一空间内部填充有金属密封层。Compared with the prior art, the insulating and sealed metal air pipe of the present invention comprises: a first metal pipe, a second metal pipe and a ceramic pipe whose inner wall is connected to the outer wall of the first metal pipe and the outer wall of the second metal pipe respectively; The inner wall of the ceramic tube and the outer wall of the first metal tube form a first space, the two ends of the first space are provided with an oxide sealing layer, and the inside of the first space is filled with a metal sealing layer; the ceramic tube The inner wall of the second metal tube and the outer wall of the second metal pipe form a second space, and the two ends of the second space are provided with an oxide sealing layer, and the inside of the first space is filled with a metal sealing layer.
由于金属管与陶瓷管的连接处既有氧化密封层又具有金属密封层,连接紧密,不易脱开,密封优良。而且由于金属密封层填充于氧化物密封料之间,金属密封层不与空气直接接触,不易在高温下发生氧化反应,老化速度慢,因此适用于高温情况下的各种环境气氛,而不再仅仅限用于中性或还原型气氛中。Since the connection between the metal tube and the ceramic tube has both an oxidized sealing layer and a metal sealing layer, the connection is tight, it is not easy to disengage, and the sealing is excellent. And because the metal sealing layer is filled between the oxide sealing materials, the metal sealing layer is not in direct contact with the air, it is not easy to oxidize at high temperature, and the aging speed is slow, so it is suitable for various ambient atmospheres under high temperature conditions, and no longer For use in neutral or reducing atmospheres only.
附图说明Description of drawings
图1为陶瓷管内壁为圆柱型的绝缘密封金属气管的剖面图;Fig. 1 is the cross-sectional view of the insulated and sealed metal air pipe of the cylindrical shape for the inner wall of the ceramic pipe;
图2为陶瓷管内壁为“工”型的绝缘密封金属气管的剖面图。Fig. 2 is a cross-sectional view of an insulated and sealed metal air pipe whose inner wall of the ceramic pipe is "I" type.
具体实施方式Detailed ways
为了进一步理解本发明,下面结合实施例对本发明优选实施方案进行描述,但是应当理解,这些描述只是为进一步说明本发明的特征和优点,而不是对本发明权利要求的限制。In order to further understand the present invention, the preferred embodiments of the present invention are described below in conjunction with examples, but it should be understood that these descriptions are only to further illustrate the features and advantages of the present invention, rather than limiting the claims of the present invention.
本发明实施例公开了一种绝缘密封金属气管,包括:第一金属管、第二金属管和内壁分别与所述第一金属管的外壁和第二金属管的外壁相连的陶瓷管;The embodiment of the present invention discloses an insulated and sealed metal air pipe, comprising: a first metal pipe, a second metal pipe, and a ceramic pipe whose inner walls are respectively connected to the outer wall of the first metal pipe and the outer wall of the second metal pipe;
所述陶瓷管的内壁与所述第一金属管的外壁形成第一空间,所述第一空间的两端设置有氧化物密封层,所述第一空间内部填充有金属密封层;The inner wall of the ceramic tube and the outer wall of the first metal tube form a first space, both ends of the first space are provided with an oxide sealing layer, and the inside of the first space is filled with a metal sealing layer;
所述陶瓷管的内壁与所述第二金属管的外壁形成第二空间,所述第二空间的两端设置有氧化物密封层,所述第二空间内部填充有金属密封层。The inner wall of the ceramic tube and the outer wall of the second metal tube form a second space, both ends of the second space are provided with an oxide sealing layer, and the inside of the second space is filled with a metal sealing layer.
本发明中,绝缘密封金属气管,包括:第一金属管、第二金属管和内壁分别与所述第一金属管的外壁和第二金属管的外壁相连的陶瓷管。In the present invention, the insulated and sealed metal gas pipe includes: a first metal pipe, a second metal pipe and a ceramic pipe whose inner wall is connected to the outer wall of the first metal pipe and the outer wall of the second metal pipe respectively.
所述第一金属管插入陶瓷管的一端,其外壁与陶瓷管的内壁连接,第二金属管插入陶瓷管的另外一端,第二金属管的外壁与陶瓷的内壁连接。第一金属管和第二金属管的末端不接触,第一金属管、陶瓷管和第二金属管的内管依次相通。The first metal tube is inserted into one end of the ceramic tube, and its outer wall is connected to the inner wall of the ceramic tube; the second metal tube is inserted into the other end of the ceramic tube, and the outer wall of the second metal tube is connected to the inner wall of the ceramic tube. The ends of the first metal tube and the second metal tube are not in contact, and the inner tubes of the first metal tube, the ceramic tube and the second metal tube communicate in sequence.
本发明对于第一金属管和第二金属管的材质没有特殊限制,其膨胀系数优选大于陶瓷管的膨胀系数。在高温使用过程中,金属密封层受到金属管和陶瓷管之间延径向的压应力,有利于密封。The present invention has no special limitation on the materials of the first metal pipe and the second metal pipe, and the expansion coefficient thereof is preferably greater than that of the ceramic pipe. During high-temperature use, the metal sealing layer is subjected to radial compressive stress between the metal tube and the ceramic tube, which is conducive to sealing.
陶瓷管将第一金属管和第二金属管连接起来,由于陶瓷在600~1000℃下不导电,因此其可以起到绝缘连接的作用。本发明对陶瓷管内壁的形状没有特殊限制,优选为“工”型或者圆柱型。所述“工”型即为陶瓷管两端的横截面积大于中部的横截面积;所述圆柱型即为陶瓷管内各处的横截面积一致。The ceramic tube connects the first metal tube and the second metal tube, and since the ceramic is non-conductive at 600-1000°C, it can function as an insulating connection. The present invention has no special limitation on the shape of the inner wall of the ceramic tube, preferably "I" shape or cylindrical shape. The "I" type means that the cross-sectional area at both ends of the ceramic tube is larger than the cross-sectional area in the middle; the cylindrical type means that the cross-sectional area of each place in the ceramic tube is consistent.
所述陶瓷管的内壁与所述第一金属管的外壁形成第一空间,所述第一空间围绕第一金属管外壁一周,为了保证密封性,因此在所述第一空间的两端设置有氧化物密封层,所述第一空间内部填充有金属密封层。所述陶瓷管的内壁与所述第二金属管的外壁形成第二空间,为了保证密封性,所述第二空间的两端同样设置有氧化物密封层,所述第二空间内部填充有金属密封层。The inner wall of the ceramic tube and the outer wall of the first metal tube form a first space, and the first space surrounds the outer wall of the first metal tube. In order to ensure the tightness, there are two ends of the first space An oxide sealing layer, the inside of the first space is filled with a metal sealing layer. The inner wall of the ceramic tube and the outer wall of the second metal tube form a second space. In order to ensure airtightness, both ends of the second space are also provided with an oxide sealing layer, and the inside of the second space is filled with metal Sealing layer.
在本发明中,金属管通过金属密封层和氧化物密封层与陶瓷管连接。在第一空间和第二空间中,氧化物密封层均将金属密封层包覆在中间,使金属密封层与空气隔绝,防止金属密封层在氧化环境中被氧化。In the present invention, the metal pipe is connected with the ceramic pipe through the metal sealing layer and the oxide sealing layer. In both the first space and the second space, the oxide sealing layer wraps the metal sealing layer in the middle to isolate the metal sealing layer from air and prevent the metal sealing layer from being oxidized in an oxidizing environment.
本发明的绝缘密封金属气管具体结构参见图1和图2。图1为陶瓷管内壁为圆柱型的绝缘密封金属气管的剖面图,包括第一金属管1、陶瓷管2、金属密封层3、氧化物密封层4a、氧化物密封层4b和第二金属管5;陶瓷管2内壁为圆柱型,所述陶瓷管2的内壁与所述第一金属管1的外壁形成第一空间,所述第一空间的一端即陶瓷管顶端与第一金属管相连的部位设置有氧化物密封层4a,所述第一空间的另一端,即陶瓷管中部与第一金属管1外壁的底部相连的部位设置有氧化物密封层4b。氧化物密封层4a和氧化物密封层4b之间填充有金属密层3。第二金属管5与陶瓷的连接方式与第一金属管4与陶瓷管2的连接方式相同,第二金属管5与第一金属管1不接触。在高温环境下,金属密封层3受到金属管1和陶瓷管2之间延径向的压应力,有利于密封。Refer to Fig. 1 and Fig. 2 for the specific structure of the insulated and sealed metal gas pipe of the present invention. Figure 1 is a cross-sectional view of a cylindrical insulated and sealed metal gas pipe with a ceramic tube inner wall, including a
图2为陶瓷管内壁为“工”型的绝缘密封金属气管的剖面图,包括第一金属管1、陶瓷管2、金属密封层3、氧化物密封层4a、氧化物密封层4b和第二金属管5;陶瓷管2内壁为“工”型,两端的横截面积大于中部的横截面积,第一金属管1内壁的横截面积与陶瓷管2内壁中部的横截面积相等。第一金属管1的外壁与陶瓷管2的内壁连接,形成第一空间,所述第一空间一端,即陶瓷管顶端与第一金属管相连的部位设置有氧化物密封层4a,所述第一空间的另一端,即陶瓷管中部与第一金属管1外壁的底部相连的部位设置有氧化物密封层4b。氧化物密封层4a和氧化物密封层4b之间填充有金属密封层3。第二金属管5与陶瓷的连接方式与第一金属管4与陶瓷管2的连接方式相同,第二金属管5与第一金属管1不接触。在高温环境下,金属密封层3受到金属管1和陶瓷管2之间延径向的压应力,有利于密封。Figure 2 is a sectional view of an insulating and sealed metal gas pipe whose inner wall is an "I" type of ceramic tube, including a
图1与图2的区别在于,氧化物密封层4b的形状不同。本发明对氧化物密封层4b的形状没有限制,能够使金属密封层3与空气隔绝即可。The difference between FIG. 1 and FIG. 2 is that the shape of the
所述第一空间内部填充的金属密封层和第二空间内部填充的金属密封层密可以选用相同的金属密封料,也可以选用不同的金属密封料,优选为两者相同。所述金属密封层优选包括Mo,Mn,W,Cu,Ti,Ag,Au,Ni,Zr,Nb,Be,V,Zn,Sn和Pb中的一种或多种,更优选包括Mo和Mn。金属密封层可紧密连接金属管与陶瓷管,结合力较高。而且金属密封层位于氧化物密封层之间,不与空气接触,从而保证其在高温下,处于氧化气氛中时,不会发生氧化。The metal sealing layer filled in the first space and the metal sealing layer filled in the second space may use the same metal sealing material, or different metal sealing materials, preferably both are the same. The metal sealing layer preferably includes one or more of Mo, Mn, W, Cu, Ti, Ag, Au, Ni, Zr, Nb, Be, V, Zn, Sn and Pb, more preferably Mo and Mn . The metal sealing layer can tightly connect the metal tube and the ceramic tube, and has a high bonding force. Moreover, the metal sealing layer is located between the oxide sealing layers and is not in contact with the air, so as to ensure that it will not be oxidized when it is in an oxidizing atmosphere at a high temperature.
所述第一空间两端的氧化物密封层和第二空间两端的氧化物密封层可以选用相同的氧化物密封料,也可以选用不同的氧化物密封料,优选为两者相同。所述氧化物密封层优选包括SiO2、Al2O3、B2O3、ZnO、RO和A2O中的一种或多种,所述RO为MgO、CaO、SrO或BaO,A2O为K2O、Na2O或Li2O,更优选包括SiO2、Al2O3和B2O3。The oxide sealing layer at both ends of the first space and the oxide sealing layer at both ends of the second space may use the same oxide sealing material, or different oxide sealing materials, preferably both are the same. The oxide sealing layer preferably includes one or more of SiO 2 , Al 2 O 3 , B 2 O 3 , ZnO, RO and A 2 O, and the RO is MgO, CaO, SrO or BaO, A 2 O is K 2 O, Na 2 O or Li 2 O, and more preferably includes SiO 2 , Al 2 O 3 and B 2 O 3 .
本发明还提供了一种金属管与陶瓷管的绝缘密封方法,包括以下步骤:The present invention also provides a method for insulating and sealing metal pipes and ceramic pipes, comprising the following steps:
(A)在陶瓷管内壁的两端分别涂覆金属密封浆料,进行烧结,形成第一金属密封层和第二金属密封层;(A) Coating metal sealing slurry on both ends of the inner wall of the ceramic tube, and sintering to form the first metal sealing layer and the second metal sealing layer;
(B)在所述第一金属密封层的两端涂覆氧化物密封浆料使所述第一金属密封层的两端与空气隔绝;(B) Coating oxide sealing slurry on both ends of the first metal sealing layer to isolate both ends of the first metal sealing layer from air;
在所述第二金属密封层的两端涂覆氧化物密封浆料,使第二金属密封层的两端与空气隔绝;Coating oxide sealing slurry on both ends of the second metal sealing layer to isolate the two ends of the second metal sealing layer from air;
(C)将第一金属管与第一金属层焊接,使第一金属层与空气隔绝;将第二金属管与第二金属层焊接,使第二金属层与空气隔绝。(C) welding the first metal tube to the first metal layer to isolate the first metal layer from the air; welding the second metal tube to the second metal layer to isolate the second metal layer from the air.
在本发明中,首先在陶瓷管内壁的一端涂覆金属密封浆料,进行烧结,形成第一金属密封层。本发明对涂覆金属密封浆料的面积没有特殊限制,本领域技术人员可根据金属管与陶瓷管的连接情况进行选择。所述金属密封浆料的制备方法优选为将金属粉末与有机溶剂及均匀混合,经过研磨得到金属浆料。所述金属粉末优选为Mo,Mn,W,Cu,Ti,Ag,Au,Ni,Zr,Nb,Be,V,Zn,Sn和Pb中的一种或多种,更优选为Mo和Mn。所述金属粉末总还可以添加其他种类的粉末以辅助烧结,优选添加氧化铝粉末。所述有机溶剂优选为以及纤维素和松油醇。本发明对金属粉末与有机溶剂的混合比例没有特殊限制,本领域技术人员可以根据熟知的比例进行混合。本发明对研磨的方式也没有特殊限制,可优选用三辊研磨机进行研磨。In the present invention, firstly, the metal sealing slurry is coated on one end of the inner wall of the ceramic tube, and then sintered to form the first metal sealing layer. The present invention has no special limitation on the area coated with the metal sealing slurry, which can be selected by those skilled in the art according to the connection between the metal tube and the ceramic tube. The method for preparing the metal sealing slurry is preferably uniformly mixing metal powder with an organic solvent, and grinding to obtain a metal slurry. The metal powder is preferably one or more of Mo, Mn, W, Cu, Ti, Ag, Au, Ni, Zr, Nb, Be, V, Zn, Sn and Pb, more preferably Mo and Mn. The metal powder can always be added with other types of powders to assist sintering, preferably alumina powders. The organic solvent is preferably cellulose and terpineol. The present invention has no special limitation on the mixing ratio of the metal powder and the organic solvent, and those skilled in the art can mix according to well-known ratios. The present invention has no special limitation on the grinding method, and a three-roll mill is preferably used for grinding.
所述第一金属层环绕陶瓷管内部一周。所述烧结优选在氢气气氛中进行;所述烧结的温度优选为1400~1600℃,更优选为1450~1550℃;所述烧结时间优选为50~70分钟,更优选为55~65分钟。The first metal layer surrounds the inside of the ceramic tube. The sintering is preferably carried out in a hydrogen atmosphere; the sintering temperature is preferably 1400-1600°C, more preferably 1450-1550°C; the sintering time is preferably 50-70 minutes, more preferably 55-65 minutes.
形成第一金属密封层后,优选在第一金属密封层上镀镍,所述镍的厚度为4~10μm,镀镍层可以改善焊料在金属层的流散情况,减缓接头中的残余应力,提高连接强度。After the first metal sealing layer is formed, it is preferable to plate nickel on the first metal sealing layer. The thickness of the nickel is 4-10 μm. The nickel-plated layer can improve the flow of solder in the metal layer, slow down the residual stress in the joint, and improve connection strength.
在本发明中,陶瓷管内形成第一金属密封层后,在所述第一金属层的两端涂覆氧化物密封浆料,使第一金属密封层的两端与空气隔绝。所述氧化物密封浆料为氧化物粉末与溶剂的混合物,其制备方法优选为:In the present invention, after the first metal sealing layer is formed in the ceramic tube, oxide sealing slurry is coated on both ends of the first metal layer to isolate the two ends of the first metal sealing layer from the air. The oxide sealing slurry is a mixture of oxide powder and solvent, and its preparation method is preferably:
将氧化物粉末球磨混合均匀,熔融,冷却后得到玻璃;The oxide powder is ball milled and mixed evenly, melted and cooled to obtain glass;
将所述玻璃粉碎后与有机溶剂混合,研磨,得到氧化物密封浆料。The glass is pulverized, mixed with an organic solvent, and ground to obtain an oxide sealing slurry.
所述氧化物粉末优选为SiO2、Al2O3、B2O3、ZnO、RO和A2O中的一种或多种,所述RO为MgO、CaO、SrO或BaO,A2O为K2O、Na2O或Li2O,更优选为SiO2、Al2O3和B2O3。所述熔融温度优选为1300~1500℃,更优选为1350~1450℃。The oxide powder is preferably one or more of SiO 2 , Al 2 O 3 , B 2 O 3 , ZnO, RO and A 2 O, and the RO is MgO, CaO, SrO or BaO, A 2 O is K 2 O, Na 2 O or Li 2 O, more preferably SiO 2 , Al 2 O 3 and B 2 O 3 . The melting temperature is preferably 1300-1500°C, more preferably 1350-1450°C.
所述有机溶剂优选为以及纤维素和松油醇。本发明对金属粉末与有机溶剂的混合比例没有特殊限制,本领域技术人员可以根据熟知的比例进行混合。本发明对研磨的方式也没有特殊限制,可优选用三辊研磨机进行研磨。The organic solvent is preferably cellulose and terpineol. The present invention has no special limitation on the mixing ratio of the metal powder and the organic solvent, and those skilled in the art can mix according to well-known ratios. The present invention has no special limitation on the grinding method, and a three-roll mill is preferably used for grinding.
在本发明中,所述第一金属层的两端与空气隔绝后将第一金属管与第一金属密封层焊接,使第一金属密封层与空气隔绝。经过焊接,第一金属管的外壁与陶瓷管内壁通过第一金属密封层连接,第一金属密封层的两端为氧化物密封层。由于焊接的温度较高,因此氧化物密封浆料干燥后,与陶瓷管内壁紧密封接。所述焊接优选为钎焊,所述钎焊优选利用铜焊料环,所述钎焊优选在氢气气氛中进行,所述钎焊的温度优选为1000~1200℃,更优选为1050~1150℃。In the present invention, after the two ends of the first metal layer are isolated from the air, the first metal tube is welded to the first metal sealing layer, so that the first metal sealing layer is isolated from the air. After welding, the outer wall of the first metal tube is connected to the inner wall of the ceramic tube through the first metal sealing layer, and both ends of the first metal sealing layer are oxide sealing layers. Due to the high welding temperature, the oxide sealing slurry is tightly sealed with the inner wall of the ceramic tube after drying. The welding is preferably brazing, the brazing preferably uses a copper solder ring, the brazing is preferably performed in a hydrogen atmosphere, and the brazing temperature is preferably 1000-1200°C, more preferably 1050-1150°C.
焊接完成后,第一金属管即与陶瓷管绝缘密封连接。After the welding is completed, the first metal tube is insulated and hermetically connected to the ceramic tube.
第二金属管与陶瓷管的密封连接方法与上述第一金属管与陶瓷管的密封连接方法相同。在陶瓷管内壁的另一端涂覆金属密封浆料,进行烧结,形成第二金属密封层。本发明对涂覆金属密封浆料的面积没有特殊限制,本领域技术人员可根据金属管与陶瓷管的连接情况进行选择。第二金属密封层选用的金属密封浆料可以与第一密封层选用的金属密封浆料相同,也可以不同。第二金属密封层的制备方法与第一密封层的制备方法相同。The sealing connection method of the second metal tube and the ceramic tube is the same as the above-mentioned sealing connection method of the first metal tube and the ceramic tube. The other end of the inner wall of the ceramic tube is coated with a metal sealing slurry and sintered to form a second metal sealing layer. The present invention has no special limitation on the area coated with the metal sealing slurry, which can be selected by those skilled in the art according to the connection between the metal tube and the ceramic tube. The metal sealing slurry selected for the second metal sealing layer may be the same as the metal sealing slurry selected for the first sealing layer, or may be different. The preparation method of the second metal sealing layer is the same as that of the first sealing layer.
所述第二金属层环绕陶瓷管内部一周。所述烧结优选在氢气气氛中进行;所述烧结的温度优选为1400~1600℃,更优选为1450~1550℃;所述烧结时间优选为50~70分钟,更优选为55~65分钟。The second metal layer surrounds the inside of the ceramic tube. The sintering is preferably carried out in a hydrogen atmosphere; the sintering temperature is preferably 1400-1600°C, more preferably 1450-1550°C; the sintering time is preferably 50-70 minutes, more preferably 55-65 minutes.
形成第二金属密封层后,优选在第一金属密封层上镀镍,所述镍的厚度为4~10μm,镀镍层可以改善焊料在金属层的流散情况,减缓接头中的残余应力,提高连接强度。After forming the second metal sealing layer, it is preferable to plate nickel on the first metal sealing layer. The thickness of the nickel is 4-10 μm. The nickel plating layer can improve the flow of solder in the metal layer, slow down the residual stress in the joint, and improve connection strength.
在本发明中,陶瓷管内形成第二金属密封层后,在所述第二金属层的两端涂覆氧化物密封浆料,使第二金属密封层的两端与空气隔绝。所述氧化物密封浆料为氧化物粉末与溶剂的混合物,其制备方法优选为:In the present invention, after the second metal sealing layer is formed in the ceramic tube, oxide sealing slurry is coated on both ends of the second metal layer to isolate the two ends of the second metal sealing layer from the air. The oxide sealing slurry is a mixture of oxide powder and solvent, and its preparation method is preferably:
将氧化物粉末球磨混合均匀,熔融,冷却后得到玻璃;The oxide powder is ball milled and mixed evenly, melted and cooled to obtain glass;
将所述玻璃粉碎后与有机溶剂混合,研磨,得到氧化物密封浆料。The glass is pulverized, mixed with an organic solvent, and ground to obtain an oxide sealing slurry.
所述氧化物粉末优选为SiO2、Al2O3、B2O3、ZnO、RO和A2O中的一种或多种,所述RO为MgO、CaO、SrO或BaO,A2O为K2O、Na2O或Li2O,更优选为SiO2、Al2O3和B2O3。所述熔融温度优选为1300~1500℃,更优选为1350~1450℃。The oxide powder is preferably one or more of SiO 2 , Al 2 O 3 , B 2 O 3 , ZnO, RO and A 2 O, and the RO is MgO, CaO, SrO or BaO, A 2 O is K 2 O, Na 2 O or Li 2 O, more preferably SiO 2 , Al 2 O 3 and B 2 O 3 . The melting temperature is preferably 1300-1500°C, more preferably 1350-1450°C.
所述有机溶剂优选为以及纤维素和松油醇。本发明对金属粉末与有机溶剂的混合比例没有特殊限制,本领域技术人员可以根据熟知的比例进行混合。本发明对研磨的方式也没有特殊限制,可优选用三辊研磨机进行研磨。The organic solvent is preferably cellulose and terpineol. The present invention has no special limitation on the mixing ratio of the metal powder and the organic solvent, and those skilled in the art can mix according to well-known ratios. The present invention has no special limitation on the grinding method, and a three-roll mill is preferably used for grinding.
在本发明中,所述第二金属层的两端与空气隔绝后将第二金属管与第二金属密封层焊接,使第二金属密封层与空气隔绝。经过焊接,第一金属管的外壁与陶瓷管内壁通过第一金属密封层连接,第一金属密封层的两端为氧化物密封层。由于焊接的温度较高,因此氧化物密封浆料干燥后,与陶瓷管内壁紧密封接。所述焊接优选为钎焊,所述钎焊优选利用铜焊料环,所述钎焊优选在氢气气氛中进行,所述钎焊的温度优选为1000~1200℃,更优选为1050~1150℃。In the present invention, after the two ends of the second metal layer are isolated from the air, the second metal tube is welded to the second metal sealing layer, so that the second metal sealing layer is isolated from the air. After welding, the outer wall of the first metal tube is connected to the inner wall of the ceramic tube through the first metal sealing layer, and both ends of the first metal sealing layer are oxide sealing layers. Due to the high welding temperature, the oxide sealing slurry is tightly sealed with the inner wall of the ceramic tube after drying. The welding is preferably brazing, the brazing preferably uses a copper solder ring, the brazing is preferably performed in a hydrogen atmosphere, and the brazing temperature is preferably 1000-1200°C, more preferably 1050-1150°C.
在实际操作当中,为了操作简便,可以在陶瓷管内壁的两端同时涂覆金属密封浆料,进行烧结后,分别得到第一金属密封层和第二金属密封层。然后在陶瓷管内壁的第一金属层的两端和第二金属层的两端分别涂覆氧化物密封浆料。最后将第一金属管和第二金属管分别套入陶瓷管的两端进行焊接。In actual operation, for the sake of simple operation, the metal sealing slurry can be coated on both ends of the inner wall of the ceramic tube at the same time, and after sintering, the first metal sealing layer and the second metal sealing layer are respectively obtained. Then, the two ends of the first metal layer and the two ends of the second metal layer on the inner wall of the ceramic tube are respectively coated with oxide sealing slurry. Finally, the first metal tube and the second metal tube are inserted into the two ends of the ceramic tube respectively for welding.
对所述绝缘密封方法得到的绝缘密封金属气管进行绝缘性及密封性测试,结果表明,金属管两端的绝缘电阻为1.8×1012~2.2×1012欧姆,而且密封性良好。The insulation and airtightness test of the insulated and sealed metal air pipe obtained by the insulating and sealing method shows that the insulation resistance at both ends of the metal pipe is 1.8×10 12 to 2.2×10 12 ohms, and the airtightness is good.
为了进一步理解本发明,下面结合实施例对本发明提供的绝缘密封金属气管及金属管与陶瓷管的密封连接方法进行说明,本发明的保护范围不受以下实施例的限制。In order to further understand the present invention, the insulated and sealed metal air pipe provided by the present invention and the sealing connection method between the metal pipe and the ceramic pipe are described below in conjunction with the examples, and the scope of protection of the present invention is not limited by the following examples.
实施例1Example 1
将20克SiO2、55克B2O3、25克Al2O3球磨混合均匀,在1400℃下熔融,倒入冷水中形成玻璃。将玻璃破碎并过40目筛,得到玻璃密封填充剂粉末。将80克玻璃密封填充剂粉末、1克乙基纤维素、19克松油醇混合均匀并通过三辊研磨机研磨,制成氧化物密封浆料。20 grams of SiO 2 , 55 grams of B 2 O 3 , and 25 grams of Al 2 O 3 were ball milled and mixed uniformly, melted at 1400°C, and poured into cold water to form a glass. The glass is crushed and passed through a 40-mesh sieve to obtain glass sealing filler powder. 80 grams of glass sealing filler powder, 1 gram of ethyl cellulose, and 19 grams of terpineol were uniformly mixed and ground by a three-roll mill to prepare an oxide sealing slurry.
将52克Mo粉、14克Mn粉、14克Al2O3粉、1克乙基纤维素、19克松油醇混合均匀并通过三辊研磨机研磨,制成金属密封浆料。Mix 52 grams of Mo powder, 14 grams of Mn powder, 14 grams of Al 2 O 3 powder, 1 gram of ethyl cellulose, and 19 grams of terpineol and grind them with a three-roll mill to make a metal sealing slurry.
将陶瓷管内壁清洁干净,在陶瓷管内壁的两端分别均匀涂覆所述金属密封浆料,然后在氢气气氛中1500℃烧结60分钟,得到第一金属层和第二金属层。The inner wall of the ceramic tube is cleaned, and the two ends of the inner wall of the ceramic tube are uniformly coated with the metal sealing slurry, and then sintered at 1500° C. for 60 minutes in a hydrogen atmosphere to obtain the first metal layer and the second metal layer.
将上述烧结好第一金属层和第二层的陶瓷管抛光后在金属化内壁镀上5um左右的镍层。After polishing the ceramic tube with the sintered first metal layer and the second layer, a nickel layer of about 5 μm is plated on the metallized inner wall.
在第一金属管和第二金属管的外壁均套上铜焊料环,在所述第一金属层的两端和第二金属层的两端分别涂覆氧化物密封浆料,使所述第一金属层的两端和第二金属层的两端均与空气隔绝。然后将第一金属管和第二金属管分别套入陶瓷管内并用夹具固定,第一金属管与第一金属层在氢气气氛中1100℃条件下钎焊,使第一金属层与空气隔绝;第二金属管与第二金属层在氢气气氛中1100℃条件下钎焊,使第二金属层与空气隔绝。Copper solder rings are placed on the outer walls of the first metal pipe and the second metal pipe, and the two ends of the first metal layer and the two ends of the second metal layer are respectively coated with oxide sealing paste, so that the first metal layer Both ends of the first metal layer and the second metal layer are isolated from air. Then put the first metal tube and the second metal tube into the ceramic tube respectively and fix them with a clamp. The first metal tube and the first metal layer are brazed at 1100°C in a hydrogen atmosphere, so that the first metal layer is isolated from the air; the second The two metal tubes and the second metal layer are brazed in a hydrogen atmosphere at 1100°C, so that the second metal layer is isolated from the air.
在830℃温度下,分别通入空气、氮气、氢气,进口和出口用水循环冷却,用绝缘测试仪测量金属管两端绝缘电阻,测量时间为30秒,用气体流量计测量进气和出气气流流量。实验结果参见表1,表1为在各种气氛中绝缘密封金属气管的密封绝缘性能。At a temperature of 830°C, air, nitrogen, and hydrogen are introduced respectively, and the inlet and outlet are cooled by water circulation. Use an insulation tester to measure the insulation resistance at both ends of the metal pipe. The measurement time is 30 seconds. Use a gas flowmeter to measure the airflow of the inlet and outlet. flow. See Table 1 for the experimental results. Table 1 shows the sealing and insulating performance of insulating and sealing metal gas pipes in various atmospheres.
表1各种气氛中绝缘密封金属气管的密封绝缘性能Table 1 Sealing and insulating properties of insulating and sealing metal gas pipes in various atmospheres
由表1可知,本发明得到的绝缘密封金属气管的绝缘情况良好,密封情况良好。It can be known from Table 1 that the insulating and sealed metal air pipe obtained by the present invention has good insulation and good sealing.
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求的保护范围内。The descriptions of the above embodiments are only used to help understand the method and core idea of the present invention. It should be pointed out that for those skilled in the art, without departing from the principle of the present invention, some improvements and modifications can be made to the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.
对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的,本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下,在其它实施例中实现。因此,本发明将不会被限制于本文所示的这些实施例,而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。The above description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the present invention will not be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310043261.7A CN103058700B (en) | 2013-01-31 | 2013-01-31 | Insulating sealed metal air pipe as well as sealed connection method of metal pipes and ceramic pipe |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310043261.7A CN103058700B (en) | 2013-01-31 | 2013-01-31 | Insulating sealed metal air pipe as well as sealed connection method of metal pipes and ceramic pipe |
Publications (2)
Publication Number | Publication Date |
---|---|
CN103058700A true CN103058700A (en) | 2013-04-24 |
CN103058700B CN103058700B (en) | 2014-11-05 |
Family
ID=48101635
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201310043261.7A Active CN103058700B (en) | 2013-01-31 | 2013-01-31 | Insulating sealed metal air pipe as well as sealed connection method of metal pipes and ceramic pipe |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN103058700B (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103819213A (en) * | 2013-12-31 | 2014-05-28 | 吉世尔(合肥)能源科技有限公司 | Multi-layer brazing structure of metal and ceramic, and brazing method |
CN112145824A (en) * | 2019-06-28 | 2020-12-29 | 国家能源投资集团有限责任公司 | Pipe fitting joint sealing structure and joint protection method |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101942864A (en) * | 2010-09-10 | 2011-01-12 | 江苏科技大学 | Composited tube node and production method |
CN102570157A (en) * | 2011-12-29 | 2012-07-11 | 航天时代电子技术股份有限公司 | Connector with sealing function |
-
2013
- 2013-01-31 CN CN201310043261.7A patent/CN103058700B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101942864A (en) * | 2010-09-10 | 2011-01-12 | 江苏科技大学 | Composited tube node and production method |
CN102570157A (en) * | 2011-12-29 | 2012-07-11 | 航天时代电子技术股份有限公司 | Connector with sealing function |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103819213A (en) * | 2013-12-31 | 2014-05-28 | 吉世尔(合肥)能源科技有限公司 | Multi-layer brazing structure of metal and ceramic, and brazing method |
CN103819213B (en) * | 2013-12-31 | 2015-11-25 | 吉世尔(合肥)能源科技有限公司 | A kind of metal and ceramic multi-layered brazing structure and method for welding |
CN112145824A (en) * | 2019-06-28 | 2020-12-29 | 国家能源投资集团有限责任公司 | Pipe fitting joint sealing structure and joint protection method |
Also Published As
Publication number | Publication date |
---|---|
CN103058700B (en) | 2014-11-05 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP3352233B1 (en) | Thermoelectric conversion module and thermoelectric conversion device | |
JP6350126B2 (en) | Lead-free low-melting glass composition, glass frit for low-temperature sealing containing the same, glass paste for low-temperature sealing, conductive material and conductive glass paste, and glass sealing parts and electric / electronic parts using the same | |
JP5741883B2 (en) | Multilayer coil component and manufacturing method thereof | |
CN105788779B (en) | A kind of sub- package casing of glass ceramics compound type insulating and preparation method thereof | |
CN105612019B (en) | The method being welded to connect for realizing metal-ceramic | |
KR20110135855A (en) | Manufacturing method of thermoelectric device | |
WO2009135387A1 (en) | Ceramic grain reinforced composite braziing filler metal | |
JP5470278B2 (en) | Sealing mechanism for high temperature fuel cell stacks | |
CN100541944C (en) | A method of manufacturing an electric heater connector plug | |
CN102557759B (en) | High-temperature metallization method of aluminum nitride ceramic | |
CN103058700B (en) | Insulating sealed metal air pipe as well as sealed connection method of metal pipes and ceramic pipe | |
CN104220396A (en) | Ceramic body and method for producing same | |
CN104387103B (en) | A brazing method for zirconia ceramics and metal materials | |
CN107785471A (en) | The method for packing and UVLED base of ceramic encapsulating structures of a kind of UVLED base of ceramic | |
CN104276838B (en) | Pottery vitrified method for sealing two with metal | |
CN108276019B (en) | Precision vacuum rotor spherical cavity device and sealing method for ceramic electrode lead pins | |
CN111266590B (en) | Ceramic metallizing raw material, ceramic metallizing method and metallized ceramic | |
TW202045456A (en) | Ceramic member and method for manufacturing same | |
CN208057243U (en) | A kind of aero-engine ignition device component | |
CN118867729A (en) | A ceramic brazing vacuum electrical connector and a preparation method thereof | |
CN104347788B (en) | Skutterudite-based thermoelectric element equipment and preparation method thereof | |
CN208368489U (en) | sealing structure | |
CN109860005A (en) | A kind of no magnetic pigtail splice and its manufacturing method | |
CN103113127B (en) | Insulated and sealed metal air tube | |
JP2003288867A (en) | Ceramic terminal |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant |