CN109604859B - Preparation method of solder paste for ceramic packaging, ceramic and packaging method thereof - Google Patents

Preparation method of solder paste for ceramic packaging, ceramic and packaging method thereof Download PDF

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CN109604859B
CN109604859B CN201811449229.8A CN201811449229A CN109604859B CN 109604859 B CN109604859 B CN 109604859B CN 201811449229 A CN201811449229 A CN 201811449229A CN 109604859 B CN109604859 B CN 109604859B
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powder
solder
ceramic
solder paste
packaging
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CN109604859A (en
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陈占军
田修营
罗飞
钟洪彬
文瑾
彭秧锡
郭军
陈志国
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Hunan University of Humanities Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material

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Abstract

The invention discloses a preparation method of solder paste for ceramic packaging, ceramic and a packaging method thereof, wherein the preparation method of the solder paste for ceramic packaging comprises the following steps: preparing solder into solder powder; mixing a binder, a solvent and a thixotropic agent to obtain a binder solution; the solder powder is mixed with the binder solution to prepare solder slurry. According to the preparation method of the solder paste for ceramic packaging, the thixotropic agent is added to enable the solder paste to have thixotropy, the consistency of the solder paste is reduced under the action of shearing force such as stirring or blade coating and the like, coating is facilitated, the viscosity of the solder paste is increased when the action of the shearing force is avoided, and solidification of the solder paste at a fixed position is facilitated. The thixotropic agent has the function of reducing or inhibiting the surface tension of the solder paste, so that the coating does not have the phenomenon of unevenness in the drying process, thereby ensuring that the solder paste can be uniformly attached to the end face of the metalized ceramic, improving the contact surface with a metal piece during packaging, enhancing the binding force and improving the welding reliability.

Description

Preparation method of solder paste for ceramic packaging, ceramic and packaging method thereof
Technical Field
The invention relates to the field of electronic ceramics, in particular to a preparation method of solder paste for ceramic packaging. In addition, the invention also relates to a ceramic comprising the preparation method of the solder paste for ceramic packaging and a packaging method thereof.
Background
The current ceramic packaging process generally uses a special stainless steel or graphite welding mold, and the metal piece, the solder sheet and the ceramic substrate are stacked and then placed in an inert atmosphere furnace for welding. The process method has the advantages of low production speed, low efficiency and complex assembly, and most of the solder used in the welding process is silver-copper solder sheets, which are thicker and have large use amount, thereby causing the waste of raw materials. In the prior art, solder powder is prepared into paste and is printed on a ceramic metalized surface, but the formed surface layer is uneven, so that the contact surface is reduced when the ceramic metalized surface is packaged with a metal piece, the packaging bonding strength is affected, and the welding reliability is reduced.
Disclosure of Invention
The invention provides a preparation method of solder paste for ceramic packaging, ceramic and a packaging method thereof, and aims to solve the technical problems that welding contact surface is easy to reduce when the ceramic packaging of the existing welding combination is packaged, so that the bonding strength is weakened and the welding reliability is reduced.
The technical scheme adopted by the invention is as follows:
a method for preparing solder paste for ceramic packaging comprises making solder into solder powder; mixing a binder, a solvent and a thixotropic agent to obtain a binder solution; the solder powder is mixed with the binder solution to prepare solder slurry.
Further, the thixotropic agent is one or two of sphingomyelin, phosphatidylserine, phosphatidylglycerol, soybean lecithin, diphosphatidylglycerol, phosphatidylinositol or cephalin.
Further, the binder adopts ethyl cellulose or nitrocellulose; the solvent is one or more of terpineol, diethylene glycol ether acetate, tributyl citrate or tributyl phthalate; the solder adopts metal powder, and the particle size of the metal powder is 100 nm-50 μm.
Further, the metal powder is at least two of silver powder, zinc powder, copper powder, manganese powder, chromium powder, iron powder, cobalt powder, titanium powder, nickel powder, molybdenum powder or tin powder, or the metal powder is alloy powder formed by at least two of silver powder, zinc powder, copper powder, manganese powder, chromium powder, iron powder, cobalt powder, titanium powder, nickel powder, molybdenum powder or tin powder; the mass ratio of the thixotropic agent to the binder is 1: 70-90; 60g to 80g of the binder is dissolved in 1500ml to 2500ml of the solvent.
Further, the particle size of the metal powder is 100nm to 5 μm or 10 μm to 50 μm.
Further, the mass ratio of the binder solution to the solder powder is 2-3: 10; the viscosity of the solder paste is 100 pas to 300 pas.
According to another aspect of the invention, a ceramic packaging method is also provided, which comprises the preparation method of the solder paste for ceramic, wherein the solder paste is silk-screen printed on the end face of the metalized ceramic, and is dried to form a solder layer; and (3) putting the metal piece and the metalized ceramic with the solder layer on a frame, and welding to realize the packaging of the ceramic end face and the metal piece and obtain the packaged ceramic.
Further, the metallized ceramic adopts one of a metallized ceramic round tube, a metallized ceramic square tube or a metallized ceramic block; the drying temperature is 90-110 ℃, and the drying time is 10-120 min; the thickness of the solder layer is 2 μm to 60 μm.
Further, the welding temperature is 600-900 ℃; the welding time is 20 min-60 min.
According to another aspect of the invention, the ceramic is prepared by adopting the ceramic packaging method.
The invention has the following beneficial effects:
the preparation method of the solder paste for ceramic packaging is simple and easy to operate. The thixotropic agent is added to enable the solder paste to have thixotropy, the consistency of the solder paste is reduced under the action of shearing force such as stirring or blade coating, coating is facilitated, the viscosity of the solder paste is increased when the solder paste is not subjected to the action of the shearing force, and solidification of the solder paste at a fixed position is facilitated. The thixotropic agent has the function of reducing or inhibiting the surface tension of the solder paste, so that the coating does not have the phenomenon of unevenness in the drying process, thereby ensuring that the solder paste can be uniformly attached to the end face of the metalized ceramic, avoiding the welding defects of insufficient solder, air holes and the like, improving the contact surface with a metal piece during packaging, enhancing the binding force and improving the packaging reliability.
According to the preparation method of the solder paste for ceramic packaging, the thixotropic agent can inhibit the oxidation of the solder powder, so that the usable particle size range of the solder powder is widened, the raw material supply is enlarged, and the popularization and the use are easy. Moreover, the thixotropic agent has a solidifying effect on the solder paste, and can reduce the settling velocity of the solder powder, so that the phenomenon that the coating is uneven in the drying process can be avoided even if the difference of the particle sizes of the solder powder is large.
The ceramic packaging method of the invention prints solder paste on the end face of the metallized ceramic, dries, and then carries out shelving and welding to obtain the ceramic. The preparation process is simple, the assembly is easy, the efficiency is high, the solder paste is effectively saved, and the production cost is reduced. The thixotropic agent is contained in the solder paste, so that the oxidation of the solder powder can be inhibited, and meanwhile, the thixotropic agent reacts with the adhesive to directly generate gas such as water, carbon dioxide and the like during the welding treatment, so that cracked carbon is not generated. Therefore, the solder paste is printed on the end face of the metallized ceramic, and can be directly packaged after being dried, organic matters do not need to be decomposed at high temperature in the hydrogen atmosphere, the working procedures are reduced, the cost is reduced, and the potential safety hazard brought by using hydrogen is also reduced.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view of a solder layer of preferred embodiment 1 of the present invention; and
fig. 2 is a schematic view of a solder layer of comparative example 1 of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
FIG. 1 is a schematic view of a solder layer of preferred embodiment 1 of the present invention; fig. 2 is a schematic view of a solder layer of a comparative example of the present invention.
As shown in fig. 1 and 2, the method for preparing solder paste for ceramic package of the present embodiment prepares solder into solder powder; mixing a binder, a solvent and a thixotropic agent to obtain a binder solution; the solder powder is mixed with the binder solution to prepare solder slurry. The preparation method of the solder paste for ceramic packaging is simple and easy to operate. The thixotropic agent is added to enable the solder paste to have thixotropy, the consistency of the solder paste is reduced under the action of shearing force such as stirring or blade coating, coating is facilitated, the viscosity of the solder paste is increased when the solder paste is not subjected to the action of the shearing force, and solidification of the solder paste at a fixed position is facilitated. The thixotropic agent has the function of reducing or inhibiting the surface tension of the solder paste, so that the coating does not have the phenomenon of unevenness in the drying process, thereby ensuring that the solder paste can be uniformly attached to the end face of the metalized ceramic, avoiding the welding defects of insufficient solder, air holes and the like, improving the contact surface with a metal piece during packaging, enhancing the binding force and improving the packaging reliability.
According to the preparation method of the solder paste for ceramic packaging, the thixotropic agent can inhibit the oxidation of the solder powder, so that the usable particle size range of the solder powder is widened, the raw material supply is enlarged, and the popularization and the use are easy. Moreover, the thixotropic agent has a solidifying effect on the solder paste, and can reduce the settling velocity of the solder powder, so that the phenomenon that the coating is uneven in the drying process can be avoided even if the difference of the particle sizes of the solder powder is large.
In this embodiment, the thixotropic agent is one or two of sphingomyelin, phosphatidylserine, phosphatidylglycerol, soybean lecithin, diphosphatidylglycerol, phosphatidylinositol, and cephalin. The thixotropic agent contains unsaturated fatty acid, can inhibit solder powder from being oxidized, and can directly react with the adhesive to generate gas such as water and carbon dioxide without generating cracked carbon when being treated at high temperature in an inert atmosphere such as nitrogen or a vacuum furnace. Due to the addition of the thixotropic agent, the usable particle size range of the solder powder is widened, the easily oxidized nano-scale solder powder can be used, the solder powder is more easily and uniformly mixed in the subsequent welding process of the solder powder, a solder layer beneficial to packaging is formed, the welding temperature is lower, and more energy is saved.
In this example, ethyl cellulose or nitrocellulose is used as the binder. The solvent is one or more of terpineol, diethylene glycol ether acetate, tributyl citrate or tributyl phthalate. The solder adopts metal powder, and the particle size of the metal powder is 100 nm-50 μm. The binder is ethyl cellulose or nitrocellulose, can chemically react with the thixotropic agent at high temperature to generate gas such as water, carbon dioxide and the like, and does not generate cracked carbon. The adhesive, the solvent and the thixotropic agent are mixed, and the adhesive can be dispersed in the solvent and then mixed with the thixotropic agent to be uniformly mixed; the three can be mixed together, the mixing time is long, the mixing mode is diversified, and the application range is wide. The solvent is one or more of oleyl alcohol, diethylene glycol ether acetate, tributyl citrate or tributyl phthalate. The solvent which is easy to volatilize and decompose is adopted, so that the solder powder can be coated on the end face of the metalized ceramic in a state of easy coating, and is easy to remove, and functional substances are remained. The amount of solvent used is generally designed according to the desired viscosity of the solder, etc. Preferably, ethyl cellulose is used as the binder, and terpineol is used as the solvent. The ethyl cellulose can improve the binding force between the solder layer and the end face of the metalized ceramic and/or between the solder particles and the solder particles, and the ethyl cellulose-terpineol system can further optimize the performance of the solder.
In this embodiment, the metal powder is at least two of silver powder, zinc powder, copper powder, manganese powder, chromium powder, iron powder, cobalt powder, titanium powder, nickel powder, molybdenum powder, and tin powder, or the metal powder is alloy powder formed by at least two of silver powder, zinc powder, copper powder, manganese powder, chromium powder, iron powder, cobalt powder, titanium powder, nickel powder, molybdenum powder, and tin powder. The mass ratio of the thixotropic agent to the binder is 1: 70-90. 60g to 80g of the binder is dispersed in 1500ml to 2500ml of the solvent. The addition of the thixotropic agent can inhibit the metal powder from being oxidized, so that the usable particle size range of the metal powder is widened, and the easily oxidized nano-scale metal powder can be used, so that the solder powder is easier to uniformly mix in the subsequent welding process, the flatness of a subsequent solder layer is increased, the contact area is increased, and the sealing property is enhanced. The mass ratio of the thixotropic agent to the binder is 1: 70-90, when the content of the thixotropic agent is low, the thixotropic effect is small in the drying process of the coating, the thixotropic agent cannot fully react with ethyl cellulose or nitrocellulose in the subsequent packaging process, the reaction is incomplete, and cracked carbon is generated, so that the sealing is not facilitated; when the thixotropic agent content is high; when the content of the thixotropic agent is higher, the ethyl cellulose or the nitrocellulose is also a polymer, so that cracked carbon can be generated during high-temperature sealing, and the sealing is not facilitated. The 60g to 80g of ethyl cellulose or nitrocellulose is dispersed in 1500ml to 2500ml of solvent, and is uniformly dispersed, so that the subsequent full reaction with soybean lecithin is facilitated.
In this example, the particle size of the metal powder is 100nm to 5 μm or 10 μm to 50 μm. Preferably, copper powder and silver powder are used as the metal powder. The mass ratio of the silver powder to the copper powder is 8: 5-3: 1. The copper powder is elemental copper powder. The silver powder is simple substance silver powder.
In this embodiment, the mass ratio of the binder solution to the solder powder is 2-3: 10. The viscosity of the solder paste is 100 pas to 300 pas. The mass ratio of the adhesive to the solder powder is 2-3: 10, the adhesive is used for preparing solder paste with the viscosity of 100 Pa.s-300 Pa.s, the solder paste is used for screen printing of 180-120 meshes, subsequent printing and drying are facilitated, and a solder layer with the thickness of 2-60 mu m is formed.
According to another aspect of the invention, a ceramic packaging method is also provided, which comprises the preparation method of the solder paste for ceramic packaging, wherein the solder paste is silk-screened on the end face of the metalized ceramic, and dried to form a solder layer; and (3) putting the metal piece and the metalized ceramic with the solder layer on a frame, and welding to realize the packaging of the ceramic end face and the metal piece and obtain the packaged ceramic. The ceramic packaging method of the invention prints solder paste on the end face of the metallized ceramic, dries, and then carries out shelving and welding to obtain the ceramic. The preparation process is simple, the assembly is easy, the efficiency is high, the solder paste is effectively saved, and the production cost is reduced. The thixotropic agent is contained in the solder paste, so that the oxidation of the solder powder can be inhibited, and meanwhile, the thixotropic agent reacts with the adhesive to directly generate gas such as water, carbon dioxide and the like during the welding treatment, so that cracked carbon is not generated. Therefore, the solder paste is printed on the end face of the metallized ceramic, and can be directly packaged after being dried, organic matters do not need to be decomposed at high temperature in the hydrogen atmosphere, the working procedures are reduced, the cost is reduced, and the potential safety hazard brought by using hydrogen is also reduced. The end face of the ceramic is firstly compounded by molybdenum-manganese alloy and ceramic, and then nickel plating is carried out on the molybdenum-manganese alloy to obtain the metallized ceramic.
In this embodiment, the metallized ceramic is one of a circular tube of metallized ceramic, a square tube of metallized ceramic, or a block of metallized ceramic. When the metallized ceramic is a metallized ceramic round tube, the metal piece, the metallized ceramic round tube with the solder layer and the metal piece are sequentially mounted and welded, so that the ceramic end face and the metal piece are packaged, and the packaged ceramic is obtained. I.e. forming a discharge vessel. When the metallized ceramic is a metallized ceramic block, one end face and the metal piece can be mounted and packaged, and the two end faces and the metal piece can also be mounted and packaged. The metallized ceramic is a square tube of metallized ceramic, which can be packaged by one end face and a metal piece, or by two end faces and the metal piece. Therefore, according to the requirements of products, the metal piece and the metalized ceramic end face with the solder layer are packaged in various modes, and the application range of the products is expanded.
In the embodiment, the drying temperature is 90-110 ℃, and the drying time is 10-120 min. The thickness of the solder layer is 2 μm to 60 μm. The drying temperature is 90-110 ℃, and the drying time is 10-120 min, so that the solder layer is more uniform, the ethyl cellulose or the nitrocellulose is better volatilized, and a more perfect solder layer is formed. In the prior art, the silver-copper solder sheet is controlled by the process, so that a very thin solder sheet cannot be used, the silver-copper solder sheet with the thickness of more than 80 microns is used in the actual production, the waste is large, the thickness of the solder layer is 2-60 microns, the use amount of the solder is effectively saved, the cost is saved, and the packaging sealing performance is high.
And silk screen printing the prepared solder paste on the end face of the metalized ceramic to be packaged by using a 180-120 mesh silk screen, and drying to form a solder layer. The screen printing can be adopted to more uniformly coat the solder paste on the end face of the metalized ceramic, and the thickness of the solder layer can be easily controlled.
In the embodiment, the welding temperature is 600 ℃ to 900 ℃; the welding time is 20 min-60 min. The concrete steps are as follows: placing a metal piece and the metalized ceramics coated with the solder layer in a vacuum furnace or an inert atmosphere furnace after the metal piece and the metalized ceramics coated with the solder layer are sequentially stacked one on another, or placing the metal piece and the metalized ceramics coated with the solder layer in the vacuum furnace or the inert atmosphere furnace after the metal piece and the metalized ceramics coated with the solder layer are mounted, wherein the welding temperature is 600-900 ℃; the welding time is 20 min-60 min. Under the protection of vacuum or inert atmosphere, metal components in the solder layer form metal alloy, and high-activity metal elements can react with the metallized ceramic and the metal piece during sintering welding, so that bonding force is formed between the solder layer and the surface of the metallized ceramic and between the solder layer and the metal piece, the bonding force is strong, and the metal alloy is not easy to fall off.
According to another aspect of the invention, the ceramic is prepared by adopting the ceramic packaging method.
Examples
Example 1
The preparation method of the solder paste for ceramic packaging comprises the following steps:
mixing 72g of 500nm silver powder copper powder and 28g of 1 micron copper powder to prepare solder powder;
dispersing 65g of ethyl cellulose in 1800ml of terpineol, adding 0.8g of soybean lecithin, and uniformly mixing to obtain a binder;
100g of solder powder and 30g of a binder were mixed to prepare solder slurry having a viscosity of 240 pas.
The ceramic packaging method comprises the following steps:
screen printing solder paste on the end face of the metalized ceramic circular tube by using a 140-mesh screen, and drying at 110 ℃ for 50min after printing to form a solder layer with the thickness of 30 microns; the method comprises the following steps of (1) putting a metal piece and a metalized ceramic circular tube covered with a solder layer on a rack after the metal piece is sequentially stacked one by one, and putting the rack in a vacuum furnace or an inert atmosphere furnace, wherein the welding temperature is 750 ℃; and (3) the welding time is 50min, and after cooling, the ceramic end face and the metal piece are packaged to obtain the packaged ceramic.
Example 2
The preparation method of the solder paste for ceramic packaging comprises the following steps:
67g of 35 μm silver powder and 23g of 200nm copper powder were mixed to prepare solder powder;
dispersing 75g of nitrocellulose in 2400ml of polyisobutylene, adding 1.2g of cephalin, and uniformly mixing to obtain a binder;
100g of solder powder and 25g of a binder were mixed to prepare solder slurry having a viscosity of 157 pas.
The ceramic packaging method comprises the following steps:
silk-screen printing solder paste on the end face of the metalized ceramic block by using a 180-mesh silk screen, and drying at 100 ℃ for 90min after printing to form a solder layer with the thickness of 10 mu m; putting the metal piece and the metalized ceramic block covered with the solder layer into a frame, and placing the frame in a vacuum furnace or an inert atmosphere furnace, wherein the welding temperature is 850 ℃; and the welding time is 40min, and after cooling, the ceramic end face and the metal piece are packaged to obtain the packaged ceramic.
Example 3
The preparation method of the solder paste for ceramic packaging comprises the following steps:
mixing 72g of 600nm silver powder and 28g of 200nm nickel powder to prepare solder powder;
uniformly mixing 76g of ethyl cellulose, 2000ml of tributyl citrate and 1g of sphingomyelin to obtain a binder;
100g of solder powder and 28g of a binder were mixed to prepare solder paste having a viscosity of 200 pas.
The ceramic packaging method comprises the following steps:
silk-screen printing solder paste on the end face of the metalized ceramic square tube by using a 150-mesh silk screen, and drying at 95 ℃ for 30min after printing to form a solder layer with the thickness of 50 microns; the method comprises the following steps of (1) putting a metal piece and a metalized ceramic square tube covered with a solder layer on a rack after the metal piece is sequentially stacked one by one, and putting the rack in a vacuum furnace or an inert atmosphere furnace, wherein the welding temperature is 650 ℃; and (3) the welding time is 50min, and after cooling, the ceramic end face and the metal piece are packaged to obtain the packaged ceramic.
Example 4
The preparation method of the solder paste for ceramic packaging comprises the following steps:
65g of 5-micron copper powder and 35g of 200nm titanium powder are mixed to prepare solder powder;
uniformly mixing 80g of ethyl cellulose, 2200ml of terpineol and 1g of soybean lecithin to obtain a binder;
100g of solder powder and 28g of a binder were mixed to prepare solder slurry having a viscosity of 196 pas.
The ceramic packaging method comprises the following steps:
screen printing solder paste on the end face of the metalized ceramic circular tube by using a 160-mesh screen, and drying at 105 ℃ for 100min after printing to form a solder layer with the thickness of 10 microns; the method comprises the following steps of (1) putting a metal piece and a metalized ceramic circular tube covered with a solder layer on a rack after the metal piece is sequentially stacked one by one, and putting the rack in a vacuum furnace or an inert atmosphere furnace, wherein the welding temperature is 890 ℃; and (3) the welding time is 30min, and after cooling, the ceramic end face and the metal piece are packaged to obtain the packaged ceramic.
Comparative example 1
The preparation method of the solder paste for ceramic packaging comprises the following steps:
mixing 72g of 1 μm silver powder and 28g of 1 μm copper powder to prepare solder powder;
dispersing 65g of ethyl cellulose in 1800ml of terpineol to obtain a binder;
100g of solder powder and 30g of a binder were mixed to prepare solder paste, and the viscosity of the solder paste was 280 pas.
The ceramic packaging method comprises the following steps:
screen printing solder paste on a circular tube with a metalized ceramic end face by using a 140-mesh screen, and drying at 110 ℃ for 80min after printing to form a solder layer with the thickness of 60 mu m; the method comprises the following steps of (1) putting a metal piece and a metalized ceramic circular tube covered with a solder layer on a rack after the metal piece is sequentially stacked one by one, and putting the rack in a vacuum furnace or an inert atmosphere furnace, wherein the welding temperature is 750 ℃; and (3) the welding time is 30min, and after cooling, the ceramic end face and the metal piece are packaged to obtain the packaged ceramic.
Examples 1-4 and comparative example 1 were subjected to tensile strength testing: on a tensile testing machine, a clamp is fixed on a hook head of the tensile testing machine, the clamp and the kovar rod are kept in good alignment, the central lines of ceramics in the embodiment and the comparative example are coincided with the action line of force, and the length of the clamp for clamping the kovar rod is required to be more than or equal to 15mm during installation. When the sealed sample is broken, the tensile test data is recorded, and the tensile strength value is obtained by dividing the tensile force by the stress area. 10 data were measured for each set of samples and averaged. The test results are shown in table 1.
TABLE 1 tensile Strength test results (Unit: MPa)
Figure BDA0001886297420000071
As shown in Table 1, the tensile strength test results show that the tensile strength of the ceramics of examples 1-4 is obviously higher than that of the ceramics of comparative example 1, which indicates that the ceramics added with the thixotropic agent have good tensile strength and strong installation and sealing performance.
The solder pastes of example 1 and comparative example 1 were screen-printed on the end faces of the metallized ceramics, and after drying treatment, a solder layer was formed, and the solder layers were compared, and the results are shown in fig. 1 and fig. 2.
Fig. 1 shows a solder layer to which no thixotropic agent is added in the comparative example, and the solder layer has grooves on its end faces after drying. After the solder layer in example 1 was dried, the end face was smooth and intact, and no recess was formed. The thixotropy can reduce the action of the surface tension of the slurry, so that the phenomenon of 'grooves' does not occur in the drying process of the coating, and the solder layer can be uniformly attached to the end face of the metallized ceramic, thereby improving the contact surface with a metal piece during packaging, enhancing the binding force and improving the sealing property of the packaging.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (4)

1. A ceramic packaging method is characterized in that,
silk-screen printing solder paste on the end face of the metallized ceramic, and drying at 90-110 ℃ for 10-120 min to form a solder layer with the thickness of 2-60 mu m;
putting the metal piece and the metalized ceramic with the solder layer on a frame, and welding at the temperature of 600-900 ℃ for 20-60 min to realize the packaging of the ceramic end face and the metal piece and obtain the packaged ceramic;
the solder paste contains a thixotropic agent to inhibit the oxidation of solder powder, and simultaneously reacts with a binder to directly generate water and carbon dioxide gas without generating cracked carbon during welding treatment, and the solder paste is printed on the end face of the metalized ceramic, can be directly packaged after being dried and does not need to decompose organic matters at high temperature in a hydrogen atmosphere;
the preparation method of the solder paste comprises the following steps:
preparing solder into solder powder, wherein the solder adopts metal powder, the particle size of the metal powder is 100 nm-5 μm or 10 μm-50 μm, and the particle sizes of the solder powder have difference;
mixing an adhesive, a solvent and a thixotropic agent, wherein the mass ratio of the thixotropic agent to the adhesive is 1: 70-90, dissolving 60-80 g of the adhesive in 1500-2500 ml of the solvent to obtain an adhesive solution, wherein the thixotropic agent is one or more of sphingomyelin, phosphatidylserine, phosphatidylglycerol, soybean lecithin, diphosphatidylglycerol, phosphatidylinositol or cephalin, the adhesive is ethyl cellulose or nitrocellulose, and the solvent is one or more of terpineol, diethylene glycol ether acetate, tributyl citrate or tributyl phthalate;
mixing the solder powder and the binder solution to prepare solder slurry, wherein the mass ratio of the binder solution to the solder powder is 2-3: 10, and the viscosity of the solder slurry is 100-300 Pa-s;
the thixotropic agent has the function of reducing or inhibiting the surface tension of the solder paste, so that the coating does not have the phenomenon of unevenness in the drying process, thereby ensuring that the solder paste can be uniformly attached to the end face of the metalized ceramic, avoiding the defects of insufficient soldering and air hole welding, improving the contact surface with a metal piece during packaging, enhancing the bonding force and improving the packaging reliability.
2. The ceramic packaging method of claim 1,
the metal powder is at least two of silver powder, zinc powder, copper powder, manganese powder, chromium powder, iron powder, cobalt powder, titanium powder, nickel powder, molybdenum powder or tin powder, or
The metal powder is alloy powder formed by at least two of silver powder, zinc powder, copper powder, manganese powder, chromium powder, iron powder, cobalt powder, titanium powder, nickel powder, molybdenum powder or tin powder.
3. The ceramic packaging method of claim 1,
the metallized ceramic is one of a metallized ceramic round tube, a metallized ceramic square tube or a metallized ceramic block.
4. A ceramic prepared by the ceramic packaging method of any one of claims 1 to 3.
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CN110563484A (en) * 2019-08-26 2019-12-13 泰州市光明电子材料有限公司 Ceramic surface metallization process
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