CN113666766B - Method for connecting zirconia ceramics by glass solder infiltration - Google Patents

Method for connecting zirconia ceramics by glass solder infiltration Download PDF

Info

Publication number
CN113666766B
CN113666766B CN202111071504.9A CN202111071504A CN113666766B CN 113666766 B CN113666766 B CN 113666766B CN 202111071504 A CN202111071504 A CN 202111071504A CN 113666766 B CN113666766 B CN 113666766B
Authority
CN
China
Prior art keywords
glass
solder
glass solder
ball milling
joint
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.)
Active
Application number
CN202111071504.9A
Other languages
Chinese (zh)
Other versions
CN113666766A (en
Inventor
朱巍巍
唐木
邹豪豪
冉旭
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changchun University of Technology
Original Assignee
Changchun University of Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Changchun University of Technology filed Critical Changchun University of Technology
Priority to CN202111071504.9A priority Critical patent/CN113666766B/en
Publication of CN113666766A publication Critical patent/CN113666766A/en
Application granted granted Critical
Publication of CN113666766B publication Critical patent/CN113666766B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B37/00Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/003Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/24Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/02Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
    • C04B2237/10Glass interlayers, e.g. frit or flux

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Ceramic Products (AREA)

Abstract

The invention discloses a method for connecting zirconia ceramics by glass solder in a penetrating way, belonging to the technical field of welding. The method comprises the steps of grinding and polishing the surfaces of two pieces of zirconia ceramics to be weldedLeveling; preparing glass solder powder according to the route of ball milling, drying, melting, water quenching, ball milling, drying and sieving, pressing the glass solder powder into sheets, and presintering for densification; placing a glass solder sheet between two ceramics to be welded for assembly; and (4) putting the assembled sample into a muffle furnace, heating to a welding temperature, preserving heat for a certain time, and cooling along with the furnace. The glass solder comprises the following components: caO:30 to 38 percent of TiO 2 :20%~26%,REO:5%~10%,B 2 O 3 :1‑5%,SiO 2 :34 to 44 percent. The invention can eliminate brazing seams existing in the traditional glass connection method, realize the uniform mixing of glass solder and ceramic grains, and further improve the strength, the thermal shock resistance and the high temperature resistance of the joint.

Description

Method for connecting zirconia ceramics by glass solder in penetrating way
Technical Field
The invention relates to the technical field of welding, in particular to a method for connecting zirconia ceramics by glass solder in a penetrating way.
Background
The zirconia ceramic has the advantages of high hardness, high strength, high toughness, good corrosion resistance and the like, and is widely applied to the fields of machinery, chemical engineering, aerospace and the like. However, due to the inherent brittleness and difficulty of machining of ceramic materials, joining techniques are often required to construct ceramic components of complex shapes and large sizes.
Among various ceramic material joining methods, glass joining is more suitable for joining of ceramics itself because of good chemical compatibility between glass solder and ceramics. However, the principle of the traditional glass connection method is similar to that of brazing, the texture structure and the physical and chemical properties of a weld seam are greatly different from those of a base material, for example, the thermal expansion coefficient, the elastic modulus, the softening temperature and the like of the weld seam are greatly different from those of a ceramic base material, and further, the thermal shock resistance and the high temperature resistance of a joint are insufficient. The invention provides a method for connecting zirconia ceramics by infiltration based on glass solder according to the infiltration principle of liquid into polycrystalline solid.
Disclosure of Invention
The invention aims to obtain a joint connecting layer with a structure similar to that of a ceramic base material, so that the strength, the thermal shock resistance and the use temperature of a joint are improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for infiltrating and connecting zirconia ceramics by glass solders is used for infiltrating and connecting zirconia ceramic base materials, and the glass solders comprise the following components in percentage by weight:
CaO:30%~38%,TiO 2 :20%~26%,REO:5%~10%,B 2 O 3 :1-5%,Li 2 O: 1-5%;SiO 2 :34%~44%。
preferably, the REO is La 2 O 3 、Y 2 O 3 、Nd 2 O 3 、Dy 2 O 3 And Ho 2 O 3 One or more of them.
The method for the glass solder infiltration connection of the zirconia ceramics specifically comprises the following steps:
(1) Preparing materials: and (3) grinding and polishing the surface of the zirconia ceramic to be welded, carrying out ultrasonic cleaning for 5-20min by taking acetone as a medium, and drying for later use.
(2) Preparing glass solder: weighing the oxide raw materials according to the composition of the glass solder, uniformly mixing, and preparing glass solder powder by adopting a melting-water quenching method;
(3) Pre-sintering of solder: adding polyvinyl alcohol into glass powder, uniformly stirring, then putting into a tabletting mold, pressing into a flaky structure with a certain thickness, and putting into a muffle furnace for pre-sintering to obtain a glass solder sheet;
(4) Assembling a joint: cutting the pre-sintered glass solder sheet into a shape with the same size as the surface of the ceramic to be welded, and then placing the glass solder sheet between two pieces of polished zirconia ceramics to form a sandwich assembly structure, wherein no pressure is used in the connection process;
(5) Connecting a joint: and (4) placing the joint assembled in the step (4) into a muffle furnace in an air atmosphere for rapidly heating to a welding temperature, wherein the purpose of rapid heating is to prevent the glass solder from excessively permeating before heat preservation. Heating to the welding temperature and preserving heat for a long enough time to ensure that the glass solder is uniformly mixed with the ceramic crystal grains; and after the heat preservation is finished, cooling the joint to the room temperature along with the furnace.
In the step (1), the grinding and polishing method comprises the steps of sequentially grinding with 400#, 800#, and 1200# sandpaper, and then sequentially polishing with diamond polishing pastes with the particle sizes of 2.5 μm, 1.5 μm, and 0.5 μm.
In the step (2), the preparation process of the glass solder comprises the following steps: putting the weighed oxide raw material powder into a polytetrafluoroethylene ball milling tank, and taking alcohol as a ball milling medium and ZrO 2 Performing ball milling on the grinding balls, wherein the ball milling rotation speed is 400-500 r/min, and the ball milling time is 2-5h; drying the composite powder after ball milling is finished, pouring the dried material into a platinum crucible, putting the platinum crucible into a muffle furnace in an air atmosphere, heating to 1500-1600 ℃, preserving heat for 1-3h, and pouring the obtained glass melt into deionized water to obtain glass fragments; putting the glass fragments into an agate ball milling tank, carrying out ball milling by taking agate as a milling ball, wherein the ball milling rotation speed is 400-500 r/min, the ball milling time is 2-5h, drying after the ball milling is finished, and sieving by a 200-mesh sieve to obtain the glass powder.
In the step (3), the weight of the added polyvinyl alcohol is 1-5% of the weight of the glass powder. The pressing process comprises the following steps: the pressure is 20-40MPa, and the pressure maintaining time is 1-5min. The sintering process comprises the following steps: the heating rate is 5-10 ℃/min, the heat preservation temperature is 750-850 ℃, and the heat preservation time is 30-60min. The purpose of pre-sintering is to sinter and densify the glass solder sheet and reduce the content of gas wrapped in the solder powder.
In the step (3), the thickness of the obtained glass solder sheet is 0.1-0.3mm, and the thermal expansion coefficient is 7-10 multiplied by 10 -6 The wetting angle of the solder on the surface of the zirconia ceramic is less than 10 degrees centigrade.
In the step (5), the heating speed of the assembled structure in a muffle furnace is 30-60min/min, the joint connection temperature is 1350-1500 ℃, and the heat preservation time is 40-90min.
In the step (5), after the joint is cooled to room temperature, the joint can be heated to the crystallization temperature of 900-1100 ℃ again, and the temperature is kept for 1-4h, so as to promote the crystallization of the glass phase between the ceramic grains of the parent metal at the joint connection area.
The design mechanism and the beneficial effects of the invention are as follows:
1. the invention designs a glass solder which has a thermal expansion coefficient close to that of zirconia ceramic and has good wettability and permeability on the surface of the zirconia ceramic. The glass solder of the component has smaller interfacial tension, good wettability and faster permeation speed with zirconia ceramics after being melted. When σ is shown in FIG. 1 SSSL When the glass is more than 2, the liquid glass can permeate into the polycrystalline zirconia ceramics. The glass solder and the zirconia ceramic have small solid-liquid interfacial tension, so the glass solder has good permeability.
2. In the presintering process of the glass solder sheet, the glass solder sheet is heated to 750-850 ℃ at the heating rate of 5-10 ℃/min, and the temperature is kept for 30-60min. The purpose of pre-sintering is to sinter and densify the glass solder sheet and reduce the content of gas wrapped in the solder powder.
3. In the process of connecting the joints, the assembled joints are placed into a muffle furnace for heating and are rapidly heated to the welding temperature, and the purpose of rapid heating is to prevent the glass solder from excessively permeating before heat preservation. The temperature is maintained for a sufficient period of time after heating to the welding temperature. In the heat preservation process, on one hand, the glass solder permeates into the ceramic base material, and meanwhile, the ceramic base material crystal grains can move under the action of buoyancy and gravity, so that the uniform mixing of the glass solder and the ceramic crystal grains can be guaranteed only under the combined action of the glass solder and the ceramic crystal grains, and further the permeating connection is realized.
4. The penetration connection method provided by the invention can eliminate brazing seams existing in the traditional glass connection method, can obtain a joint connection layer consisting of base material crystal grains and glass solder, and the physical and chemical properties of the joint connection layer, such as the organization structure, the thermal expansion coefficient, the elastic modulus and the like, are very close to those of a ceramic base material. Therefore, the invention can obtain the zirconia ceramic joint with high strength, low stress, high thermal shock resistance and high heat resistance.
Drawings
FIG. 1 is a schematic of the interfacial tension of the infiltration process.
FIG. 2 is a photograph of the microstructure of the zirconia ceramic joint obtained in example 1; wherein (a) and (b) are different magnifications.
FIG. 3 is a photograph of the microstructure of the zirconia ceramic joint obtained in comparative example 1.
FIG. 4 is a photograph of a microstructure of a zirconia ceramic joint obtained in comparative example 2; wherein (a) and (b) are different magnifications.
Detailed Description
The present invention is further described below in conjunction with the drawings and the embodiments so that those skilled in the art can better understand the present invention and can carry out the present invention, but the embodiments are not to be construed as limiting the present invention.
Example 1
The embodiment is a method for infiltrating and connecting zirconia ceramics by glass solder, which comprises the following steps:
(1) Preparing materials: and sequentially grinding the surfaces of the zirconia ceramics to be welded by 400#, 800# and 1200# sandpaper, and then sequentially polishing the surfaces of the ceramics to be welded by diamond polishing pastes with the particle sizes of 2.5 mu m, 1.5 mu m and 0.5 mu m. And ultrasonically cleaning the polished zirconia ceramic for 20min by taking acetone as a medium, and then drying for later use.
(2) Preparing glass solder: the glass solder comprises the following components in percentage by mass: caO:32% of TiO 2 : 23%,Dy 2 O 3 :5%,B 2 O 3 :3%,SiO 2 : and 37 percent. Weighing the oxide raw materials according to the proportion, and putting the oxide raw materials into a polytetrafluoroethylene ball milling tank to take alcohol as a ball milling medium, wherein ZrO is 2 Ball milling is carried out on the grinding balls, the ball milling rotating speed is 450 r/min, and the ball milling time is 4h. And drying the ball-milled product in a vacuum drying oven at 70 ℃ for 2 hours. The dried raw materials are poured into a platinum crucible and put into a muffle furnace to be heated to 1550 ℃. And pouring the glass melt into deionized water after the temperature is kept for 2 hours, and further obtaining glass fragments. And (3) putting the glass fragments into an agate ball-milling tank for ball-milling, wherein the ball-milling rotating speed is 500 r/min, and the ball-milling time is 4h. And drying after ball milling is finished, and sieving with a 200-mesh sieve for later use.
(3) Pre-sintering of solder: adding 2 percent of polyvinyl alcohol by weight into the glass powder, uniformly stirring, then putting into a tabletting mold, pressing into a sheet with the thickness of 0.2mm, then putting into a muffle furnace, heating to 800 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, sintering and densifying the solder, and finally cooling to room temperature along with the furnace for later use.
(4) Assembling a joint: the presintered glass solder sheet is cut into a shape with the same size as the surface of the ceramic to be welded, and then is placed between two pieces of polished zirconia ceramics to form a sandwich structure, and no pressure is used in the connection process.
(5) Connecting a joint: and (3) putting the assembled joint into a muffle furnace with an air atmosphere for heating, wherein no pressure is used in the connecting process. Rapidly heating to 1400 ℃ at the heating rate of 30 ℃/min and preserving the heat for 50min. And after the heat preservation is finished, cooling the joint to the room temperature along with the furnace.
FIG. 2 is a photograph showing the microstructure of the zirconia ceramic joint obtained in example 1, and it can be seen that the glass solder has completely penetrated into the base material and a good connection is formed. The joint has no defects such as holes and cracks. From the joint central area to the base material side, the content of the glass phase is gradually reduced, the content of the base material crystal grains is gradually increased, and a gradient transition structure is formed.
Example 2
The embodiment is a method for infiltrating and connecting zirconia ceramics by glass solder, which comprises the following steps:
(1) Preparing materials: and sequentially grinding the surfaces of the zirconia ceramics to be welded by 400#, 800# and 1200# sandpaper, and then sequentially polishing the surfaces of the ceramics to be welded by diamond polishing pastes with the particle sizes of 2.5 mu m, 1.5 mu m and 0.5 mu m. And ultrasonically cleaning the polished zirconia ceramic for 20min by taking acetone as a medium, and then drying for later use.
(2) Preparing glass solder powder: the glass solder comprises the following components in percentage by mass: caO:32% of TiO 2 :23%,Nd 2 O 3 :5%,B 2 O 3 :3%,SiO 2 :37 percent. Weighing the oxide raw materials according to the proportion, and putting the oxide raw materials into a polytetrafluoroethylene ball milling tank to take alcohol as a ball milling medium, wherein ZrO is 2 Ball milling is carried out on the grinding balls, the ball milling rotating speed is 450 r/min, and the ball milling time is 4h. And drying the ball-milled product in a vacuum drying oven at 70 ℃ for 2 hours. The dried raw materials are poured into platinumThe crucible was placed in a muffle furnace and heated to 1550 ℃. And pouring the glass melt into deionized water after the temperature is kept for 2 hours, and further obtaining glass fragments. And putting the glass fragments into an agate ball milling tank for ball milling, wherein the ball milling rotating speed is 500 r/min, and the ball milling time is 4h. And drying after ball milling, and sieving with a 200-mesh sieve to obtain the glass solder powder.
(3) Pre-sintering solder: adding polyvinyl alcohol into glass powder, stirring uniformly, then putting into a tabletting mold, pressing into a sheet with the thickness of 0.2mm, then putting into a muffle furnace, heating to 800 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, sintering and densifying the solder, and finally cooling to room temperature along with the furnace to obtain the glass solder sheet.
(4) Assembling a joint: the presintered glass solder sheet is cut into the shape with the same size as the surface of the ceramic to be welded, and then is placed between two pieces of polished zirconia ceramics to form a sandwich structure, and no pressure is used in the connection process.
(5) Connecting a joint: and (3) putting the assembled joint into a muffle furnace with an air atmosphere for heating, wherein no pressure is used in the connecting process. Rapidly heating to 1400 ℃ at the heating rate of 30 ℃/min and preserving the heat for 40min. And after the heat preservation is finished, cooling the joint to room temperature along with the furnace to obtain the glass solder permeable connection zirconia ceramic.
Example 3
The embodiment is a method for infiltrating and connecting zirconia ceramics by glass solder, which comprises the following steps:
(1) Preparing materials: and sequentially grinding the surfaces of the zirconia ceramics to be welded by 400#, 800# and 1200# sandpaper, and then sequentially polishing the surfaces of the ceramics to be welded by diamond polishing pastes with the particle sizes of 2.5 mu m, 1.5 mu m and 0.5 mu m. And ultrasonically cleaning the polished zirconia ceramic for 20min by taking acetone as a medium, and then drying for later use.
(2) Preparing glass solder powder: the glass solder comprises the following components in percentage by mass: caO:38% of TiO 2 :20%,Nd 2 O 3 :5%,B 2 O 3 :1%,SiO 2 :36 percent. Weighing the oxide raw materials according to the proportion, and putting the oxide raw materials into a polytetrafluoroethylene ball milling tank to be ball-milled by using alcoholMedium, zrO 2 Ball milling is carried out on the grinding balls, the ball milling rotating speed is 450 r/min, and the ball milling time is 4h. And drying the ball-milled product in a vacuum drying oven at 70 ℃ for 2 hours. The dried raw materials are poured into a platinum crucible and put into a muffle furnace to be heated to 1550 ℃. And pouring the glass melt into deionized water after the temperature is kept for 2 hours, and further obtaining glass fragments. And putting the glass fragments into an agate ball milling tank for ball milling, wherein the ball milling rotating speed is 500 r/min, and the ball milling time is 4h. And drying after ball milling is finished, and sieving with a 200-mesh sieve to obtain the glass solder powder.
(3) Pre-sintering solder: adding polyvinyl alcohol into glass powder, stirring uniformly, then putting into a tabletting mold, pressing into a sheet with the thickness of 0.2mm, then putting into a muffle furnace, heating to 800 ℃ at the heating rate of 10 ℃/min, preserving heat for 30min, sintering and densifying the solder, and finally cooling to room temperature along with the furnace to obtain the glass solder sheet.
(4) Assembling a joint: the presintered glass solder sheet is cut into the shape with the same size as the surface of the ceramic to be welded, and then is placed between two pieces of polished zirconia ceramics to form a sandwich structure, and no pressure is used in the connection process.
(5) Connecting a joint: the assembled joint is placed in a muffle furnace with air atmosphere for heating, and no pressure is used in the connection process. Rapidly heating to 1450 deg.C at a heating rate of 30 deg.C/min, and maintaining for 40min. And after the heat preservation is finished, cooling the joint to room temperature along with the furnace to obtain the glass solder permeable connection zirconia ceramic.
Comparative example 1
The holding time in step (5) was 10min, and the other steps were the same as in example 1. Due to the short holding time, the solder does not completely penetrate into the zirconia ceramic, and a glassy brazing seam is formed, as shown in fig. 3.
Comparative example 2
The temperature rise rate in the step (5) was 5 ℃/min, and the other steps were the same as in example 1. Due to the slow rate of temperature rise, the glass solder has penetrated into the zirconia ceramic matrix during the heating process, which leads to failure of effective connection at the joint, and the microstructure of the joint is shown in fig. 4. Therefore, a higher heating speed is needed to be adopted, and the existence of liquid solder in the welding line is ensured in the heat preservation process, so that the base material crystal grains and the solder can generate relative motion and further uniformly mix to form reliable connection.
The mechanical properties of the joints obtained in examples 1, 2, 3, 1 and 2 are shown in table 1. As can be seen from the table, examples 1, 2, and 3 all obtained excellent room temperature strength, high temperature strength, and strength after thermal shock cycle. Comparative example 1 the high temperature strength was significantly reduced due to the glassy weld obtained. Meanwhile, the thermal expansion coefficient between the base material and the solder is not matched, so that the strength of the joint after thermal shock circulation is low. Comparative example 2 the joint had the lowest room temperature strength, high temperature strength, and strength after thermal shock cycling because no effective joint was formed.
TABLE 1 bending Strength data of joints of examples and comparative examples
Figure BDA0003260536680000081

Claims (10)

1. A method for infiltrating and connecting zirconia ceramics by glass solder is characterized in that: the method adopts glass solder to perform infiltration connection on a zirconia ceramic base material, and the glass solder comprises the following raw materials in percentage by weight:
CaO:30%~38%,TiO 2 :20%~26%,REO:5%~10%,B 2 O 3 :1-5%,SiO 2 :34%~44%。
2. the method for glass-solder-infiltrated connection of zirconia ceramics according to claim 1, wherein: the REO is La 2 O 3 、Y 2 O 3 、Nd 2 O 3 、Dy 2 O 3 And Ho 2 O 3 One or more of them.
3. The method for glass-solder-infiltrated connection of zirconia ceramics according to claim 1, wherein: the method specifically comprises the following steps:
(1) Preparing materials: after the surface of the zirconia ceramic to be welded is ground and polished, ultrasonic cleaning is carried out for 5-20min by taking acetone as a medium, and the zirconia ceramic is dried for standby;
(2) Preparing glass solder: weighing the oxide raw materials according to the composition of the glass solder, uniformly mixing, and preparing glass solder powder by adopting a melting-water quenching method;
(3) Pre-sintering of solder: adding polyvinyl alcohol into the glass solder powder, uniformly stirring, then putting the glass solder powder into a tabletting mold, pressing the glass solder powder into a sheet structure with a certain thickness, and putting the sheet structure into a muffle furnace for pre-sintering to obtain a glass solder sheet;
(4) Assembling a joint: cutting the presintered glass solder sheet into a shape with the same size as the surface of the ceramic to be welded, and then placing the glass solder sheet between two polished zirconium oxide ceramics to form a sandwich assembly structure, wherein no pressure is used in the connection process;
(5) Connecting a joint: and (5) putting the joint assembled in the step (4) into a muffle furnace in an air atmosphere, quickly heating to the welding temperature, keeping the temperature for a long enough time to ensure that the glass solder and the ceramic crystal grains are uniformly mixed, and cooling the joint to the room temperature along with the furnace after the temperature is kept.
4. The method for glass-solder-infiltrated connection of zirconia ceramics according to claim 3, wherein: in the step (1), the grinding and polishing method comprises the following steps: sequentially sanding with 400#, 800#, and 1200# sandpaper, and sequentially polishing with diamond polishing pastes with particle sizes of 2.5 μm, 1.5 μm, and 0.5 μm.
5. The method for glass-solder-infiltrated connection of zirconia ceramics according to claim 3, wherein: in the step (2), the process of preparing the glass solder powder by the melting-water quenching method comprises the following steps: putting the weighed oxide raw material powder into a polytetrafluoroethylene ball milling tank, and taking alcohol as a ball milling medium and ZrO 2 Performing ball milling on the grinding balls, wherein the ball milling rotation speed is 400-500 r/min, and the ball milling time is 2-5h; drying the ball-milled materials, and pouring platinum into the dried materialsPlacing the gold crucible into a muffle furnace with an air atmosphere, heating to 1500-1600 ℃, preserving heat for 1-3h, and pouring the obtained glass melt into deionized water to obtain glass fragments; putting the glass fragments into an agate ball milling tank, carrying out ball milling by taking agate as a milling ball, wherein the ball milling rotation speed is 400-500 r/min, the ball milling time is 2-5h, drying after ball milling is finished, and sieving by a 200-mesh sieve to obtain the glass solder powder for later use.
6. The method for glass-solder-infiltrated connection of zirconia ceramics according to claim 3, wherein: in the step (3), polyvinyl alcohol with the weight of 1-5% of the weight of the glass solder powder is added; the pressing thickness of the sheet glass solder is 0.1-0.3mm, the pressure during pressing is 20-40MPa, and the pressure maintaining time is 1-5min.
7. The method of glass-solder-infiltrated connection of zirconia ceramics according to claim 3, wherein: in the step (3), the pre-sintering process comprises the following steps: heating to 750-850 deg.C at a rate of 5-10 deg.C/min, maintaining for 30-60min, and cooling to room temperature.
8. The method for glass-solder-infiltrated connection of zirconia ceramics according to claim 3, wherein: in the step (3), the prepared glass solder has a thermal expansion coefficient of 8-10 multiplied by 10 -6 The optimal wetting angle of the solder on the surface of the zirconia ceramic is less than 10℃.
9. The method for glass solder penetration bonding of zirconia ceramics according to claim 3, wherein in the step (5), the joint heating speed is 30 to 60min/min, the joint connection temperature is 1350 to 1500 ℃, and the holding time is 40 to 90min.
10. The method for glass-solder-infiltrated connection of zirconia ceramics according to claim 3, wherein: in the step (5), after the joint is cooled to the room temperature, the joint is heated to the crystallization temperature of 900-1100 ℃ again, and the temperature is kept for 1-4h, so that the crystallization of the glass phase among the ceramic grains of the parent metal of the joint connection area is promoted.
CN202111071504.9A 2021-09-14 2021-09-14 Method for connecting zirconia ceramics by glass solder infiltration Active CN113666766B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111071504.9A CN113666766B (en) 2021-09-14 2021-09-14 Method for connecting zirconia ceramics by glass solder infiltration

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111071504.9A CN113666766B (en) 2021-09-14 2021-09-14 Method for connecting zirconia ceramics by glass solder infiltration

Publications (2)

Publication Number Publication Date
CN113666766A CN113666766A (en) 2021-11-19
CN113666766B true CN113666766B (en) 2022-11-22

Family

ID=78549283

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111071504.9A Active CN113666766B (en) 2021-09-14 2021-09-14 Method for connecting zirconia ceramics by glass solder infiltration

Country Status (1)

Country Link
CN (1) CN113666766B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115259670B (en) * 2022-07-26 2023-11-28 冷水江市汇鑫电子陶瓷有限公司 Glass-based solder and preparation method thereof
CN115490538B (en) * 2022-10-14 2023-08-18 长春工业大学 Preparation method of alumina/glass composite material and application of alumina/glass composite material in repairing internal cracks of alumina ceramic
CN117645493B (en) * 2023-11-30 2024-06-04 西南交通大学 Oscillation pressure auxiliary ceramic connection method

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5594975A (en) * 1979-01-16 1980-07-18 Asahi Glass Co Ltd Low expansion powder composition for bonding use
JPS6379771A (en) * 1986-09-22 1988-04-09 工業技術院長 Adhesive for oxide base ceramics and adhesion therefor
JP3079581B2 (en) * 1990-12-26 2000-08-21 日本電気硝子株式会社 Sealing glass
DE102012206266B3 (en) * 2012-04-17 2013-07-11 Schott Ag Barium- and strontium-free glassy or glass-ceramic joining material and its use

Also Published As

Publication number Publication date
CN113666766A (en) 2021-11-19

Similar Documents

Publication Publication Date Title
CN113666766B (en) Method for connecting zirconia ceramics by glass solder infiltration
CN106493443B (en) A kind of method of composite interlayer ceramic soldering or ceramic matric composite and metal
KR101960264B1 (en) Residual stress free joined SiC ceramics and the processing method of the same
CN108838504B (en) Composite intermediate layer for diffusion bonding of silicon carbide ceramic and bonding process thereof
JP5978105B2 (en) Silicon carbide ceramic joined body and method for producing silicon carbide ceramic joined body
CN113880430B (en) Glass solder for connecting transparent magnesia-alumina spinel ceramic and method for connecting transparent magnesia-alumina spinel ceramic
CN112296472B (en) Brazing method of graphite material
CN110524082B (en) Method for quickly wetting carbon fibers in ceramic matrix composite by taking Fe as active element
CN105728981B (en) Weld Si3N4The solder and its method for welding of ceramics-stainless steel
CN105149717A (en) Silicon-based ceramic surface metallization method
CN110153591A (en) A kind of amorphous composite soldering for ceramic soldering and alloy
CN106944698A (en) The SiC ceramic and the direct method for welding of SiC ceramic reinforced aluminum matrix composites ultrasonic cryogenic being modified based on thermal oxide surface
CN103232257B (en) Fast connection method of carbon/carbon composite material
CN106588064A (en) Solder and connection method of carbon / carbon composites and nickel-base superalloys
CN108555476B (en) Composite brazing filler metal for brazing quartz fiber reinforced composite ceramic and Invar alloy and preparation method and brazing method thereof
CN113070543B (en) Method for brazing carbon material and nickel-based alloy by adopting Ag-Cr composite brazing filler metal
CN115490538B (en) Preparation method of alumina/glass composite material and application of alumina/glass composite material in repairing internal cracks of alumina ceramic
CN103193499B (en) A kind of method of attachment of carbon-carbon composites
CN112872523A (en) Brazing method for welding titanium-based high-entropy alloy and silicon nitride ceramic
CN112122826A (en) Soldering paste for brazing titanium-based composite material and silicon nitride ceramic, and method and application thereof
CN109369208B (en) Brazing filler metal for silicon carbide connection and preparation method and application thereof
CN111454063A (en) Ceramic connecting piece with compact connecting layer and connecting method and application thereof
Han Joining alumina ceramics in green state using a paste of ceramic slurry
CN114195542A (en) Method for connecting silicon carbide ceramic by using microcrystalline glass solder for in-situ generation of anorthite
CN106927848A (en) A kind of Zirconium Diboride-based Ultra-high Temperature Ceramics welding point and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant