CN113121116B - Microcrystalline glass solder, preparation method thereof and method for connecting alumina ceramics - Google Patents
Microcrystalline glass solder, preparation method thereof and method for connecting alumina ceramics Download PDFInfo
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- CN113121116B CN113121116B CN202110513310.3A CN202110513310A CN113121116B CN 113121116 B CN113121116 B CN 113121116B CN 202110513310 A CN202110513310 A CN 202110513310A CN 113121116 B CN113121116 B CN 113121116B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion 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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/003—Joining 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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/10—Glass interlayers, e.g. frit or flux
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/52—Pre-treatment of the joining surfaces, e.g. cleaning, machining
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Abstract
The invention discloses a microcrystalline glass solder, which comprises the chemical compositions of 15-20 wt% of CaO and Al 2 O 3 10～25wt％、SiO 2 50～55wt％、ZnO 5～10wt％、B 2 O 3 5 to 10 weight percent; the glass thermal expansion coefficient of the microcrystalline glass solder is 5.9-6.5 multiplied by 10 at the temperature of 25-700 DEG C ‑6 V. C. In addition, a preparation method of the microcrystalline glass solder and a method for connecting the alumina ceramics are also disclosed. The microcrystalline glass solder is matched with the thermal expansion coefficient of the aluminum oxide ceramic base material and has proper connection temperature, so that the aluminum oxide ceramic is connected at low temperature, the process difficulty of aluminum oxide ceramic connection is reduced, the room temperature strength of a joint is improved, the defects of pore crack and the like are avoided, and the connection quality of the aluminum oxide ceramic is effectively improved.
Description
Technical Field
The invention relates to the technical field of alumina ceramic connection, in particular to a microcrystalline glass solder, a preparation method thereof and a method for connecting alumina ceramic.
Background
The alumina ceramic has the advantages of high mechanical strength, small dielectric loss, large insulation resistance, high hardness, wear resistance, corrosion resistance, high temperature resistance and the like, and is widely applied to various fields of aviation, military, machinery, petroleum, chemical engineering, electronics and the like. However, due to the intrinsic brittleness and difficulty in machining of ceramic materials, alumina ceramics are difficult to be prepared into components with large sizes and complex shapes, and thus the application range thereof is greatly limited. In order to construct alumina ceramic components with complex shapes and large sizes, a connection technology is required to be adopted, and simple structural components are combined into a component with a complex shape, so that the method has important significance for reducing the production cost and expanding the application range of the component.
Among various techniques for connecting ceramic materials, the use of microcrystalline glass as a connecting material is a simple and easy and inexpensive connecting method. The microcrystalline glass connecting material has excellent chemical compatibility with ceramics, and the strength of the microcrystalline glass connecting material can be improved through certain crystallization. However, the microcrystalline glass solder in the prior art generally has the problems of higher melting point and poor thermal expansion coefficient matching with alumina ceramics, so that the process difficulty of ceramic connection is increased, defects such as pore cracks and the like are caused, and the mechanical property of a joint and the connection quality of the alumina ceramics are greatly influenced. Therefore, it is necessary to prepare the microcrystalline glass solder which is suitable for connecting the alumina ceramics at low temperature and is matched with the thermal expansion coefficient of the alumina ceramics.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a microcrystalline glass solder which is matched with the thermal expansion coefficient of an alumina ceramic base material and has proper connection temperature through formula design, so that low-temperature connection of alumina ceramic is realized. The invention also aims to provide a preparation method of the microcrystalline glass solder and a method for connecting the alumina ceramics.
The purpose of the invention is realized by the following technical scheme:
the invention provides a microcrystalline glass solder, which comprises 15-20 wt% of CaO and Al 2 O 3 10～25wt％、SiO 2 50～55wt％、ZnO 5～10wt％、B 2 O 3 5 to 10 weight percent; the glass thermal expansion coefficient of the microcrystalline glass solder is 5.9-6.5 multiplied by 10 at the temperature of 25-700 DEG C -6 /℃。
The other purpose of the invention is realized by the following technical scheme:
the preparation method of the microcrystalline glass solder provided by the invention comprises the following steps:
(1) Ball milling mixing material
According to the chemical composition ratio, caCO is used 3 、Al 2 O 3 、SiO 2 、ZnO、H 3 BO 3 Weighing raw materials, and mixing by wet ball milling to obtain a mixed material;
(2) Melting and cold quenching
Drying, grinding and sieving the mixed material, then carrying out melting treatment, and immediately carrying out cold quenching treatment on the melted melt material to obtain glass frit;
(3) Ball milling into powder
Crushing the glass frit by a dry ball mill, and sieving to obtain CaO-Al 2 O 3 -SiO 2 -ZnO-B 2 O 3 And (3) microcrystalline glass solder.
Further, in the preparation method, in the step (2), the drying temperature is 80-110 ℃, and the drying time is 6-12 hours; the melting temperature is 1400-1550 ℃, and the melting time is 1-3 h. The rotating speed of the dry ball mill in the step (3) is 1000-1400 r/min, and the ball milling time is 5-60 min.
The invention provides a method for connecting alumina ceramics by adopting the microcrystalline glass solder, which comprises the following steps:
(1) Grinding and polishing the surfaces to be connected of the aluminum oxide ceramics to-be-welded pieces;
(2) Mixing the microcrystalline glass solder with a polyvinyl alcohol aqueous solution with the concentration of 9wt%, and then granulating and pressing to obtain a flaky solder blank;
(3) And adhering the solder blank between the surfaces to be connected of the aluminum oxide ceramics to be welded, applying pressure to the parts to be welded, placing the parts in a brazing furnace for welding treatment, and cooling along with the furnace to complete the connection of the aluminum oxide ceramics.
Furthermore, in the step (2) of the connection method, the dosage of the polyvinyl alcohol aqueous solution is 5-7 wt% of the microcrystalline glass solder, the pressure of the compression molding is 10-30 MPa, and the thickness of the sheet solder blank is 100-300 mu m. The pressure applied in the step (3) is 0-15 KPa; the temperature schedule of the welding treatment in the brazing furnace is as follows: heating from room temperature to 350-400 ℃ at the speed of 5-10 ℃/min, preserving heat for 30-60 min, then continuously heating to 1150-1300 ℃ at the speed of 5-15 ℃/min, preserving heat for 20-40 min, then cooling to 700-900 ℃ at the speed of 10-20 ℃/min, and preserving heat for 1-2 h.
The invention has the following beneficial effects:
(1) CaO-Al of the invention 2 O 3 -SiO 2 -ZnO-B 2 O 3 The microcrystal glass solder belongs to medium-temperature glass solder, and the glass thermal expansion coefficient between 25 and 700 ℃ is 5.9 to 6.5 multiplied by 10 -6 The temperature is matched with the thermal expansion coefficient of the connected alumina ceramic base material. CaO-Al 2 O 3 -SiO 2 Is a matrix composition of microcrystalline glass, in which SiO 2 Forming a glass network structure; al (Al) 2 O 3 The silicon-oxygen tetrahedron and the silicon-oxygen tetrahedron form a unified network; caO belongs to the external network body and is CaCO 3 The form is introduced, and the addition is to separate out the calcium-containing microcrystalline phase, thereby improving the performance of the microcrystalline glass.
(2) The microcrystalline glass solder contains a small amount of ZnO and B 2 O 3 (B 2 O 3 With H 3 BO 3 Form introduction) for the purpose ofIn the following steps: znO can reduce the melting temperature of the glass solder on one hand, and can precipitate crystalline phases such as zinc silicate and the like on the other hand, thereby being beneficial to regulating and controlling the thermal expansion coefficient of the solder; b is 2 O 3 To reduce the melting and welding temperatures.
(3) The microcrystalline glass solder can realize the connection between alumina ceramics at 1150-1300 ℃, reduces the process difficulty of the alumina ceramic connection, can ensure that the room temperature strength of the joint can reach 255-280 MPa, is improved by 19-30 percent compared with the common glass joint, and effectively improves the connection quality of the alumina ceramics because the thermal expansion coefficient of the joint is better matched with that of an alumina base material and the defects of air holes, cracks and the like do not exist.
Drawings
The invention will now be described in further detail with reference to the following examples and the accompanying drawings:
FIG. 1 is a schematic view of a solder joint for joining alumina ceramics using a microcrystalline glass solder according to an embodiment of the present invention;
FIG. 2 is a temperature profile for bonding alumina ceramics using a microcrystalline glass solder according to an embodiment of the present invention.
In the figure: alumina ceramic to-be-welded parts 1, a solder blank 2, and pressure P applied on the to-be-welded parts
Detailed Description
The first embodiment is as follows:
1. this example is a glass-ceramic solder having a chemical composition of CaO 15wt% and Al 2 O 3 15 wt％、SiO 2 55 wt％、ZnO 5wt％、B 2 O 3 10wt%; the glass thermal expansion coefficient of the microcrystalline glass solder is 6.2 multiplied by 10 at the temperature of between 25 and 700 DEG C -6 /℃。
2. The preparation method of the microcrystalline glass solder comprises the following steps:
(1) Ball milling mixing material
According to the chemical composition ratio, caCO is used 3 、Al 2 O 3 、SiO 2 、ZnO、H 3 BO 3 Weighing raw materials, putting the weighed raw materials in a polytetrafluoroethylene ball milling tank according to the mass ratio of the raw materials to grinding balls to deionized water = 1: 2: 1, and taking 300r as a basisCarrying out ball milling and mixing for 5 hours at the min rotating speed by a wet method to obtain a mixed material;
(2) Melting and cold quenching
Drying the mixed material at 100 ℃ for 10h, grinding, sieving by a 200-mesh sieve, melting at 1450 ℃ for 1h, and then pouring the molten material into distilled water for cold quenching treatment to obtain glass frit;
(3) Ball milling into powder
Pulverizing the glass frit by a dry ball mill at the rotating speed of 1200r/min for 30min, and sieving by a 250-mesh sieve to obtain CaO-Al 2 O 3 -SiO 2 -ZnO-B 2 O 3 And (3) microcrystalline glass solder.
3. The method for connecting the alumina ceramics by adopting the microcrystalline glass solder comprises the following steps:
(1) Step-by-step grinding and polishing treatment is carried out on the surfaces to be connected of the aluminum oxide ceramic parts to be welded 1 by using 500 # water-grinding abrasive paper, 800 # water-grinding abrasive paper, 1200 # water-grinding abrasive paper and 1600 # water-grinding abrasive paper;
(2) Mixing the microcrystalline glass solder with 9wt% polyvinyl alcohol aqueous solution (the dosage of the polyvinyl alcohol aqueous solution is 6wt% of the microcrystalline glass solder), granulating, and performing compression molding under the pressure of 15MPa to obtain a sheet-shaped solder blank 2 with the thickness of 150 mu m;
(3) As shown in fig. 1, the above-mentioned solder green body 2 is adhered between the surfaces to be connected of the alumina ceramic pieces to be welded 1 by 502 glue, a pressure P of 10KPa is applied to the pieces to be welded, and the pieces are placed in a brazing furnace to perform the following welding process (see fig. 2): heating from room temperature to 400 deg.C at a rate of 5 deg.C/min, maintaining the temperature for 30min, then continuing heating to 1250 deg.C at a rate of 10 deg.C/min, maintaining the temperature for 30min, cooling to 750 deg.C at a rate of 10 deg.C/min, and maintaining the temperature for 1h; and then cooling along with the furnace to finish the connection of the alumina ceramics.
The room temperature strength of the alumina joint connected by the microcrystalline glass prepared by the embodiment reaches 263MPa, which is improved by 22.3% compared with the common glass joint.
Example two:
the difference between the present embodiment and the first embodiment is:
the chemical composition of the microcrystalline glass solder is 10wt% of CaO and Al 2 O 3 20 wt％、SiO 2 55 wt％、ZnO 10wt％、B 2 O 3 5 wt%; the glass thermal expansion coefficient of the microcrystalline glass solder is 6.5 multiplied by 10 at the temperature of between 25 and 700 DEG C -6 /℃。
The room temperature strength of the alumina joint connected with the microcrystalline glass prepared by the embodiment reaches 280MPa, and is improved by 30 percent compared with the common glass joint.
Example three:
the difference between the present embodiment and the first embodiment is:
in the method for connecting the alumina ceramics by using the microcrystalline glass solder in the embodiment, the welding treatment system of the step (3) in the brazing furnace is as follows: heating from room temperature to 350 deg.C at a speed of 10 deg.C/min, maintaining for 60min, heating to 1200 deg.C at a speed of 5 deg.C/min, maintaining for 40min, cooling to 860 deg.C at a speed of 20 deg.C/min, and maintaining for 1h.
The room temperature strength of the alumina joint connected with the microcrystalline glass prepared by the embodiment reaches 274MPa, and is improved by 27.5 percent compared with the common glass joint.
Claims (5)
1. A preparation method of a microcrystalline glass solder is characterized by comprising the following steps: the chemical composition of the microcrystalline glass solder is CaO 15-20 wt percent and Al 2 O 3 10～25 wt%、SiO 2 50～55 wt%、ZnO 5～10 wt%、B 2 O 3 5 to 10wt percent; the preparation method comprises the following steps:
(1) Ball milling mixing material
According to the chemical composition ratio, caCO is used 3 、Al 2 O 3 、SiO 2 、ZnO、H 3 BO 3 Weighing raw materials, and mixing by wet ball milling to obtain a mixed material;
(2) Melting and cold quenching
Drying the mixed material at 80-110 ℃ for 6-12 h, grinding, sieving by a 200-mesh sieve, then carrying out melting treatment at 1400-1550 ℃ for 1-3 h, and then carrying out cold quenching treatment on the melted melt material to obtain glass frit;
(3) Ball milling into powder
The glass frit is driedThe ball mill is pulverized at the rotating speed of 1000-1400 r/min for 5-60 min, and CaO-Al is obtained after sieving 2 O 3 -SiO 2 -ZnO-B 2 O 3 Microcrystalline glass solder, caO-Al 2 O 3 -SiO 2 Is a matrix composition of microcrystalline glass, in which SiO 2 Formed for a glass network structure, al 2 O 3 The CaO belongs to the external body of the network and is CaCO 3 Introducing the calcium-containing microcrystalline phase in a form to precipitate calcium-containing microcrystalline phase; the glass thermal expansion coefficient of the microcrystalline glass solder is 5.9-6.5 multiplied by 10 at the temperature of 25-700 DEG C -6 The connection between the alumina ceramics is realized at 1150-1300 ℃, and the room temperature strength of the joint reaches 255-280 MPa.
2. The method for connecting the microcrystalline glass solder with the alumina ceramic by adopting the preparation method of claim 1 is characterized by comprising the following steps:
(1) Grinding and polishing the surfaces to be connected of the aluminum oxide ceramic parts to be welded;
(2) Mixing the microcrystalline glass solder with a polyvinyl alcohol aqueous solution with the concentration of 9wt%, granulating, and performing compression molding to obtain a sheet solder blank;
(3) And adhering the solder blank body between the surfaces to be connected of the aluminum oxide ceramics to be welded, applying pressure to the parts to be welded, placing the parts in a brazing furnace for welding treatment, and cooling along with the furnace to complete the connection of the aluminum oxide ceramics.
3. The method of joining alumina ceramics according to claim 2, wherein: the dosage of the polyvinyl alcohol water solution in the step (2) is 5-7 wt percent of the microcrystalline glass solder, the pressure of the compression molding is 10-30 MPa, and the thickness of the sheet solder blank is 100-300 mu m.
4. The method of joining alumina ceramics according to claim 2, wherein: the pressure applied in the step (3) is 0-15 k Pa.
5. The method of joining alumina ceramics according to claim 2, wherein: the temperature schedule of the welding treatment in the brazing furnace in the step (3) is as follows: heating from room temperature to 350-400 ℃ at the speed of 5-10 ℃/min, preserving heat for 30-60 min, then continuously heating to 1150-1300 ℃ at the speed of 5-15 ℃/min, preserving heat for 20-40 min, then cooling to 700-900 ℃ at the speed of 10-20 ℃/min, and preserving heat for 1-2 h.
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| CN113732565B (en) * | 2021-09-23 | 2023-03-28 | 广东省科学院新材料研究所 | Solder, preparation method and application thereof, welding method and ceramic component |
| CN113880430B (en) * | 2021-10-29 | 2023-11-28 | 长春工业大学 | Glass solder for connecting transparent magnesia-alumina spinel ceramic and method for connecting transparent magnesia-alumina spinel ceramic |
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| CN114315401B (en) * | 2021-11-15 | 2022-09-27 | 长春工业大学 | Transient liquid phase connection method of alumina ceramics |
| CN115784719B (en) * | 2022-11-29 | 2023-11-28 | 云南雷迅科技有限公司 | Preparation method of composite mirror blank of ceramic-based reflector |
| CN116514566B (en) * | 2023-03-23 | 2024-06-21 | 江西博鑫环保科技股份有限公司 | High-temperature inorganic adhesive special for full ceramic membrane element combination and combination process method |
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