CN115036056B - High-weldability thick-film conductor paste - Google Patents
High-weldability thick-film conductor paste Download PDFInfo
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- CN115036056B CN115036056B CN202210958455.9A CN202210958455A CN115036056B CN 115036056 B CN115036056 B CN 115036056B CN 202210958455 A CN202210958455 A CN 202210958455A CN 115036056 B CN115036056 B CN 115036056B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention discloses a high-weldability thick film conductor paste, which is a paste with certain fluidity prepared by mixing noble metal powder, glass powder, pre-treated zirconium silicate and magnesium silicate mixed powder with an organic carrier, wherein the pre-treated zirconium silicate and magnesium silicate mixed powder is prepared by uniformly mixing zirconium silicate and magnesium silicate according to a certain proportion, and then cleaning with alcohol and roasting. The invention improves the weldability of the thick film conductor paste by adding the pretreated zirconium silicate and magnesium silicate mixed powder as an additive into the conductor paste, ensures the use requirement of the thick film conductor paste in a thick film circuit, and can meet the application requirement of a thick film circuit product in various environmental conditions.
Description
Technical Field
The invention belongs to the technical field of conductor paste, and particularly relates to thick-film conductor paste with high weldability, which can be widely applied to ceramic substrates such as aluminum oxide and beryllium oxide and thick-film circuit products adopting a thick-film printing process, and the products can be applied to various environmental conditions such as long-time reflow soldering environment.
Background
The electronic paste is a basic material for manufacturing thick film elements, is a paste formed by uniformly mixing solid powder and an organic solvent through three-roll rolling, and is widely applied to thick film products in the modern microelectronic industry. In the modern microelectronic industry thick film circuit products, people have higher and higher requirements on electronic components, the thick film circuit products are widely applied, and particularly, in the fields with various severe environmental requirements, higher requirements are provided for the high-temperature aging tensile force of thick film conductor paste products.
Generally, the main components of the electronic paste include a functional phase, an inorganic binder, an organic binder, other solvents, and additives. Generally, a functional phase in the electronic paste plays a role in electrical conduction, and generally has a good electrical conductivity, and metal powder or noble metal powder is used as the functional phase, and the commonly used noble metal powder includes gold powder, silver powder, platinum powder, palladium powder, alloy powder and the like. The inorganic binder functions to fix the electronic paste to the substrate, and is generally formed of oxide powder and glass powder, but this component has a low specific gravity in the electronic paste, and some or none of them.
In the field of the existing electronic paste, the conductor paste has the characteristics of high conductivity, stable performance, high bonding strength with a substrate and the like, and is widely applied to the production of electronic components such as integrated circuits, multi-chip assemblies, membrane switches and the like. Inorganic matters in the existing conductor paste mainly take conventional oxides and glass powder as main materials, the binding force with a substrate is ensured by adding the inorganic matters and the glass powder, the binding force with the substrate is ensured, generally, the content of the glass powder and the inorganic matters is increased, so that the weldability of the conductor paste is greatly reduced, and in the using process, poor welding is caused, so that components are out of order, especially, the components are subjected to a long-time high-temperature aging environment, the deterioration speed of the welding part of the conductor paste is greatly accelerated due to the influence of the high-temperature environment, pads can fall off, a large number of products are out of order, and the application range of the conductor paste is greatly limited. Therefore, a conductive paste with high solderability is urgently needed to meet the use requirement under the condition of extreme high-temperature environment.
Disclosure of Invention
The invention aims to solve the problems that microcracks and welding pads fall off and finally the product fails due to the influence of an internal structure and a thermal expansion coefficient at the joint part of conductor slurry and soldering tin under the long-time high-temperature aging environment condition in the conventional conductor slurry used for thick film circuit products, and provides the conductor slurry which meets the thick film printing process and has high weldability when applied to the thick film circuit products.
Aiming at the purposes, the conductor paste adopted by the invention comprises the following components in percentage by weight: 70 to 85 percent of noble metal powder, 0.5 to 5 percent of glass powder, 2.5 to 3.5 percent of additive and 10 to 25 percent of organic carrier.
The noble metal powder is any one or a mixture of more of silver powder, palladium powder and platinum powder or alloy powder of more of the silver powder, the granularity of the silver powder is 0.5 to 2.5 mu m, and the specific surface area of the palladium powder is 3 to 25m2(g) the specific surface area of the platinum powder is 3-25 m2The granularity of the alloy powder is 0.1-5 mu m.
The glass powder is a permanent product obtained after sintering electronic pasteThe binding phase material can be glass powder of lead-silicon-boron-aluminum, bismuth-silicon-boron-aluminum, lead-bismuth-silicon-boron and the like. Preferably, the bismuth-silicon-boron-aluminum glass powder adopted by the invention comprises the following components in percentage by weight: bi2O3 55%～85%、B2O3 2%～10%、SiO2 5%～20%、Al2O31 to 10 percent of BaO and 1 to 5 percent of BaO. The preparation method comprises the following steps: uniformly mixing various oxides according to weight percentage, putting the mixture into a ceramic crucible, putting the ceramic crucible into a smelting furnace for smelting at the smelting temperature of 1100-1400 ℃ for 0.5-4 h, pouring the obtained molten glass into deionized water, performing water quenching to obtain a glass body, crushing the glass body into glass slag, and ball-milling the glass slag into particles with the particle size D50 of 1.0-2.5 mu m.
The additive is pretreated zirconium silicate and magnesium silicate mixed powder, and the pretreated zirconium silicate and magnesium silicate mixed powder with the granularity D50 of 1.0-2.0 mu m is mixed with absolute ethyl alcohol according to the weight ratio of 1:1-1.5, wherein the weight ratio of zirconium silicate to magnesium silicate is 2-5:1, the mixture is subjected to ultrasonic treatment at the temperature of 30-50 ℃ for 60-120 min under the condition that the power is 0.5-1 kW, is sieved by using a 250-400-mesh screen, is calcined at the temperature of 600-700 ℃ for 6-8 h, and is sieved by using a 325-400-mesh screen, so that the pretreated zirconium silicate and magnesium silicate mixed powder is obtained.
The organic carrier is a mixture of polymer resin and a solvent, and comprises the following components in percentage by weight: 5-20% of high polymer resin and 80-95% of solvent, wherein the high polymer resin is one or more of ethyl cellulose, nitrocellulose, polyurethane resin, acrylic resin and soybean lecithin, and the solvent is one or more of terpineol, ethyl acetate, butyl cellosolve and butyl carbitol acetate.
Compared with the prior art, the invention has the following beneficial effects:
1. the conductor paste adopts pretreated zirconium silicate and magnesium silicate powder as additives, so that the weldability of the thick-film conductor paste and the welding characteristic after long-time high-temperature work after welding are improved;
2. the preparation process of the conductor paste is simple, the pollution is little, and the process adaptability is strong; the obtained conductor paste has the characteristic of high reliability on the premise of not causing other performance degradation.
Drawings
Fig. 1 is a graph of a printing screen made by conducting paste performance testing, where location 1 is a tensile test pattern and location 2 is a solderability test pattern.
Detailed Description
The invention is described in detail below with reference to the drawings and specific examples, which do not limit the scope of the invention. The scope of the present invention is defined only by the appended claims, and any omissions, substitutions, and changes in the form of the embodiments disclosed herein that may be made by those skilled in the art are intended to be included within the scope of the present invention.
The conductor paste comprises the following components in percentage by weight: 70 to 85 percent of noble metal powder, 0.5 to 5 percent of glass powder, 2.5 to 3.5 percent of additive and 10 to 25 percent of organic carrier. Wherein the noble metal powder can be any one or a mixture of more of silver powder, palladium powder and platinum powder or alloy powder of more, the granularity of the silver powder is 0.5-2.5 mu m, and the specific surface area of the palladium powder is 3-25 m2The specific surface area of the platinum powder is 3 to 25m2The grain size of the alloy powder is 0.1-5 mu m. The glass powder can be glass powder of systems such as lead-silicon-boron-aluminum, bismuth-silicon-boron-aluminum, lead-bismuth-silicon-boron and the like, wherein the bismuth-silicon-boron-aluminum glass powder comprises the following components in percentage by weight: bi2O3 55%～85%、B2O3 2%～10%、SiO2 5%～20%、Al2O31% -10% of BaO and 1% -5% of BaO, and the preparation method comprises the following steps: uniformly mixing various oxides according to weight percentage, putting the mixture into a ceramic crucible, putting the ceramic crucible into a smelting furnace for smelting at the smelting temperature of 1100-1400 ℃ for 0.5-4 h, pouring the obtained molten glass into deionized water, performing water quenching to obtain a glass body, crushing the glass body into glass slag, and ball-milling the glass slag into particles with the particle size D50 of 1.0-2.5 mu m. The additive is pretreated zirconium silicate and magnesium silicate mixed powder, and the preparation method comprises the following steps: mixing the zirconium silicate and magnesium silicate mixed powder with the granularity D50 of 1.0 to 2.0 mu m and absolute ethyl alcohol according to the weight ratio of 1:1 to 1.5, wherein the weight ratio of the zirconium silicate to the magnesium silicate is 2 to 5:1, and the work in practice is carried outThe mixture is processed by ultrasonic treatment for 60-120 min at 30-50 ℃ under the condition that the yield is 0.5-1 kW, sieving by using a 250-400 mesh sieve, calcining for 6-8 h at 600-700 ℃, and sieving by using a 325-400 mesh sieve to obtain the pretreated zirconium silicate and magnesium silicate mixed powder. The organic carrier is a mixture of polymer resin and a solvent, and comprises the following components in percentage by weight: 5-20% of high polymer resin and 80-95% of solvent, wherein the high polymer resin is any one or more of ethyl cellulose, nitrocellulose, polyurethane resin, acrylic resin and soybean lecithin, and the solvent is any one or more of terpineol, ethyl acetate, ethylene glycol butyl ether and butyl carbitol acetate.
1. Preparation of the additive
Mixing zirconium silicate and magnesium silicate mixed powder with the particle size D50 of 1.0-2.0 mu m with absolute ethyl alcohol according to a weight ratio of 1.2, wherein the weight ratio of the zirconium silicate to the magnesium silicate is 2:1, 3:1 and 5:1 respectively, performing ultrasonic treatment at 40 ℃ for 80min under the condition of 0.8kW of power, sieving by using a 250-mesh sieve, calcining for 7h at 650 ℃, and then sieving by using a 400-mesh sieve to obtain the pretreated zirconium silicate and magnesium silicate mixed powder. The obtained pre-treated zirconium silicate and magnesium silicate mixed powder is sequentially marked as an additive-1, an additive-2 and an additive-3 according to the weight ratio of 2:1, 3:1 and 5:1 of zirconium silicate to magnesium silicate.
Simultaneously, respectively pretreating zirconium silicate powder with single granularity D50 of 1.0-2.0 mu m and magnesium silicate powder with single granularity D50 of 1.0-2.0 mu m according to the method to respectively obtain an additive-4 and an additive-5, and simultaneously sequentially using a mixture of zirconium silicate powder with single untreated granularity D50 of 1.0-2.0 mu m, magnesium silicate powder with single untreated granularity D50 of 1.0-2.0 mu m and magnesium silicate powder with untreated granularity D50 of 1.0-2.0 mu m and weight ratio of 3:1 as an additive-6, an additive-7 and an additive-8.
2. Preparation of glass powder
According to the weight percentage, bi is added2O3 76%、B2O3 5%、SiO2 12%、Al2O34 percent and BaO 3 percent are fully and evenly mixed, the obtained mixture is placed in a smelting furnace for smelting, and the smelting temperature is highThe temperature is 1250 ℃ and the time is 2.5h; and then carrying out water quenching on the obtained molten glass to obtain a vitreous body, crushing the vitreous body into glass slag, carrying out ball milling on the glass slag for 32 hours, and sieving the glass slag with a 400-mesh sieve to obtain glass powder with the granularity of 1.2-1.8 mu m.
3. Preparation of organic vehicle
According to the weight percentage, 82.5 percent of terpineol is heated to 60 ℃ in a beaker, 15 percent of acrylic resin and 2.5 percent of soybean lecithin are added, and the organic carrier is obtained after full stirring and complete dissolution.
4. Preparation of conductor paste
According to the weight percentage in the table 1, silver powder with the granularity D50 of 1.0-2 mu m and the specific surface area of 15-25 m2Palladium powder in a ratio of 15-25 m2The platinum powder, the additive, the glass powder with the granularity D50 of 1.0-2.5 mu m and the organic carrier are uniformly mixed by a stirring dispersion machine, and then are rolled into paste with certain fluidity by a three-roll mill, and the conductor paste with the fineness less than or equal to 8 mu m of the embodiment 1-4 and the comparative example 1-6 are respectively prepared.
TABLE 1 conductor paste formulation
Printing the conductor slurry on an alumina ceramic substrate (25.4 mm long × 25.4mm wide × 1mm thick) by a screen printing process according to the screen printing plate pattern shown in fig. 1, drying at 150 ℃ for 10min, sintering in a belt sintering furnace at 850 + -5 ℃, keeping the peak value at the temperature for 10min, preparing a test sample, and performing the following performance tests:
and (3) sintering surface appearance: the surface state of the sintered film of the obtained sample is observed by magnifying by 20 times through a microscope;
square resistance: performing a sheet resistance test according to a sheet resistance test method of 105 electronic paste in an electronic paste performance test method for an SJ/T11512-2015 integrated circuit;
initial adhesion test: welding a lead plane with the diameter of phi 0.8mm on a sample wafer with the diameter of 2mm multiplied by 2mm, and performing initial tension test by using a tension machine after the lead is bent by 90 degrees;
and (3) aging adhesion testing: welding a lead plane with the diameter of 0.8mm on a sample wafer with the diameter of 2mm multiplied by 2mm, putting the sample wafer into a drying oven with the temperature of 150 +/-5 ℃ for 48 hours, taking out the sample wafer, putting the sample wafer at room temperature for 30 minutes, bending the lead at 90 degrees, and then testing the tensile force by using a tensile machine;
and (3) testing the weldability: placing psi 4 × 2.85mm tin particles on a 10mm × 10mm sample wafer, placing on a 260 deg.C hot plate for 10 s, taking out, cooling, and measuring the diameter of molten tin particles;
surface roughness test the test was performed using a contact surface roughness tester, position 2 in figure 1.
The results of the various tests described above are shown in table 2 and compared to a commercially available 9912A thick film conductor paste (provided by ESL corporation, usa) and a commercially available 964G thick film conductor paste (provided by He Lishi, germany).
TABLE 2 comparison of different conductor paste test data
As can be seen from table 2, the thick film conductor paste prepared in embodiments 1 to 4 of the present invention has a lower square resistance value compared to commercial thick film conductor paste products, and after long-term high temperature aging, the aging tensile force is greater, and the product reliability is high. Comparing examples 1-4 with comparative example 1, it is demonstrated that the solderability of the thick film conductor paste can be significantly improved after the pre-treated zirconium silicate and magnesium silicate mixed powder is added into the thick film conductor paste; comparing examples 1-4 with comparative example 2, comparative example 5 and comparative example 6, the addition of the pre-treated zirconium silicate and magnesium silicate mixed powder into the thick film conductor paste can significantly improve the weldability and aging tension of the thick film conductor paste, while the addition of the untreated zirconium silicate powder and magnesium silicate powder does not significantly affect the weldability or cause the reduction of the weldability, and the sintered film has uneven surface, more bubbles, large roughness and obviously reduced aging tension; comparing examples 1-4 with comparative example 3 and comparative example 4, the solderability was better after the pre-treated zirconium silicate and magnesium silicate mixed powder was added to the thick film conductor paste, while the pre-treated zirconium silicate powder or pre-treated magnesium silicate powder added alone had no significant effect on the solderability and the aged tensile force was significantly reduced.
Claims (6)
1. The high-weldability thick-film conductor paste is characterized in that the weight percentage of the conductor paste is as follows: 70 to 85 percent of noble metal powder, 0.5 to 5 percent of glass powder, 2.5 to 3.5 percent of additive and 10 to 25 percent of organic carrier;
the additive is pretreated zirconium silicate and magnesium silicate mixed powder, the zirconium silicate and magnesium silicate mixed powder with the granularity D50 of 1.0-2.0 mu m is mixed with absolute ethyl alcohol according to the weight ratio of 1:1-1.5, wherein the weight ratio of zirconium silicate to magnesium silicate is 2-5:1, after ultrasonic treatment is carried out for 60-120 min at the temperature of 30-50 ℃ under the condition that the power is 0.5-1 kW, a 250-400-mesh screen is used for sieving, then calcination is carried out for 6-8 h at the temperature of 600-700 ℃, and then the pretreated zirconium silicate and magnesium silicate mixed powder is obtained by sieving through a 325-400-mesh screen.
2. The thick film conductor paste according to claim 1, wherein said noble metal powder is a mixture or alloys of any one or more of silver powder, palladium powder and platinum powder, wherein the particle size of the silver powder is 0.5-2.5 μm, and the specific surface area of the palladium powder is 3-25 m2(g) the specific surface area of the platinum powder is 3-25 m2The granularity of the alloy powder is 0.1-5 mu m.
3. The thick-film conductor paste of claim 1, wherein said glass powder is any one of lead-silicon-boron-aluminum, bismuth-silicon-boron-aluminum, and lead-bismuth-silicon-boron glass powder.
4. The thick film conductor paste of claim 3 wherein said bismuth silicon boron aluminum based glass powder comprises, by weight: bi2O3 55%～85%、B2O3 2%～10%、SiO2 5%～20%、Al2O31 to 10 percent of BaO, 1 to 5 percent of BaO, and the granularity D50 of 1.0 to 2.5 mu m.
5. The paste according to claim 4, wherein the glass powder is prepared by mixing oxides uniformly according to weight percentage, placing the mixture in a ceramic crucible, putting the ceramic crucible into a smelting furnace for smelting at 1100-1400 ℃ for 0.5-4 h, pouring the obtained glass melt into deionized water, quenching the deionized water to obtain a glass body, crushing the glass body into glass slag, and ball-milling the glass slag into particles with a particle size D50 of 1.0-2.5 μm.
6. The highly solderable thick film conductor paste of claim 1 wherein the organic vehicle comprises, in weight percent: 5-20% of high polymer resin and 80-95% of solvent, wherein the high polymer resin is one or more of ethyl cellulose, nitrocellulose, polyurethane resin, acrylic resin and soybean lecithin, and the solvent is one or more of terpineol, ethyl acetate, butyl cellosolve and butyl carbitol acetate.
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