CN108962422B - Conductive silver paste for LTCC ceramic substrate and preparation method thereof - Google Patents
Conductive silver paste for LTCC ceramic substrate and preparation method thereof Download PDFInfo
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- CN108962422B CN108962422B CN201811002728.2A CN201811002728A CN108962422B CN 108962422 B CN108962422 B CN 108962422B CN 201811002728 A CN201811002728 A CN 201811002728A CN 108962422 B CN108962422 B CN 108962422B
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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
Abstract
The conductive silver paste for the LTCC ceramic substrate is composed of, by mass, 82% -86% of silver powder, 3% -4% of high polymer resin, 0.2% -1.1% of glass powder and 10% -15% of solvent. The high polymer resin is composed of ethyl cellulose, carboxymethyl cellulose and polyaspartic acid. The conductive silver paste prepared by the preparation method has good conductivity, strong adhesive force and flat and compact appearance. The silver layer has strong bonding force with the ceramic interface, and the inside of the device does not crack and delaminate.
Description
Technical Field
The invention relates to the technical field of conductive paste, in particular to conductive silver paste suitable for an LTCC (Low temperature Co-fired ceramic) substrate and a preparation method thereof.
Background
The demand for high performance, high density, high reliability electronic systems for applications such as communications, automotive, medical, military, aerospace, etc., is and will continue to present new challenges to electronic packaging. LTCC (Low Temperature Co-fired Ceramic) technology, an advanced passive integration and hybrid circuit packaging technology, can package three passive components (including resistors, capacitors and inductors) and various passive components (such as filters, transformers and the like) in a multilayer wiring substrate, and is integrated with active devices (such as power MOS, transistors, IC circuit modules and the like) into a complete circuit system. The low-temperature co-fired ceramic technology is a remarkable integrated assembly technology developed in recent years, and has become the first choice for integration and modularization of electronic components in the future because the technology can meet the requirements of electronic products. Unlike HTCC, LTCC technology sinters at "low temperatures" below 900 degrees, ensuring that traditional thick film conductor pastes (e.g., silver, gold, and alloys) with high conductivity and low melting point are successfully applied to LTCC processes. As a design basis of devices with high performance and low energy consumption, the research and development of the LTCC technology and related materials have great application value in the fields of military, civil and the like.
At present, the markets of low-temperature co-fired conductive paste at home and abroad are mainly monopolized by international well-known enterprises such as Ferro, Dupont and the like, and key breakthroughs are not always made in the field at home, and one of the main reasons is that the core formula and key preparation process technology of base materials such as silver powder, glass powder, organic carriers and the like required by the low-temperature co-fired conductive paste cannot be mastered by the domestic enterprises. The cost of LTCC devices developed and produced in China is high, more importantly, key core technologies and products are restricted by people, and the upgrading development of electronic paste technologies and industries in China is seriously hindered.
In order to reduce the sintering temperature of the LTCC technology, LTCC ceramics are usually realized by doping low-melting point oxide or low-melting point glass, and the complex system makes the traditional silver paste difficult to match with it, even unable to meet the basic use requirement. In the co-firing process of the traditional conductive silver paste and the LTCC ceramic substrate, due to differences of affinities of the ceramic and the silver powder and between the silver powder and the LTCC ceramic substrate, the silver powder is excessively diffused to the ceramic substrate to cause reduction of insulation resistance, the risk of electric breakdown of a circuit exists, and a silver electrode layer is easy to generate more cavities after being sintered; and the bonding force between the silver layer and the ceramic interface is insufficient, so that the serious result of cracking and layering in the device can be caused. In addition, since the diffusion coefficients of metal and ceramic are different, the difference in diffusion rate causes unevenness on both sides of the interface, resulting in a decrease in the flatness of the substrate.
Therefore, in order to promote the application of the low-temperature co-fired ceramic technology, the development of conductive silver paste more suitable for the low-temperature co-fired ceramic substrate is urgently needed in the field.
Disclosure of Invention
The invention is provided especially in view of the problems of the existing conductive silver paste. The invention provides the conductive silver paste with good co-firing matching property of the LTCC ceramic substrate, the silver layer is flat and compact after the conductive silver paste is sintered, the bonding force between the silver layer and a ceramic interface is strong, cracking and layering do not occur in a device, and the conductive silver paste has good soldering resistance.
In order to solve the technical problem, in one aspect, the invention provides a conductive silver paste for an LTCC ceramic substrate, which comprises the following components in percentage by mass: 82 to 86 percent of silver powder, 3 to 4 percent of polymer resin, 0.2 to 1.1 percent of glass powder and 10 to 15 percent of solvent; wherein: the high polymer resin is composed of ethyl cellulose, carboxymethyl cellulose and polyaspartic acid.
In the present invention, the weight ratio of ethylcellulose, carboxymethylcellulose and polyaspartic acid is preferably 1:0.1 to 0.5:0.05 to 0.1. More preferably, the weight ratio of the ethyl cellulose, the carboxymethyl cellulose and the polyaspartic acid is 1: 0.3-0.4: 0.06-0.08.
Preferably, the glass powder consists of 30-40% of bismuth oxide, 10-20% of copper oxide, 15-25% of silicon oxide, 15-20% of barium carbonate and 15-20% of aluminum oxide.
In another aspect, the present invention further provides a method for preparing the conductive silver paste for the LTCC ceramic substrate, which comprises the following steps:
(1) mixing the polymer resin and the solvent according to a certain proportion, and fully dissolving to obtain the organic carrier.
(2) And uniformly mixing the organic carrier with the silver powder and the glass powder to obtain the premix.
(3) Fully grinding the premix to obtain silver electrode slurry; and filtering, detecting and supplementing a solvent to the silver electrode slurry to obtain the conductive silver slurry.
The beneficial technical effects of the invention are as follows: the prepared conductive silver paste has good matching performance with an LTCC ceramic substrate in co-firing, a silver layer is flat and compact after the conductive silver paste is sintered, the bonding force between the silver layer and a ceramic interface is strong, cracking and layering do not occur in a device, and the device has good soldering resistance; meanwhile, the phenomenon that silver powder is excessively diffused to the porcelain body is not found in detection, and the risk of electric breakdown of a circuit is eliminated. The conductive silver paste provided by the invention does not contain lead (Pb) and cadmium (Cd), and meets the RoHS requirement.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments of the present invention are described in detail below with reference to tables. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The inventor of the invention discovers through years of research that in the process of co-firing ceramic and metal, the infiltration affinity between the ceramic and silver powder and the infiltration affinity between the silver powder and the silver powder have a crucial influence on a sintered silver layer, and if the infiltration affinity between the ceramic and the silver powder is greater than the affinity between the silver powder and the silver powder, the silver powder is excessively diffused to a ceramic body, so that on one hand, the insulation resistance is reduced, the risk of electric breakdown of a circuit exists, and on the other hand, a silver electrode layer is easy to generate more cavities after sintering. If the silver powder is incompatible with the ceramic, the bonding force between the electrode layer and the ceramic interface is reduced easily, and the serious consequence of cracking and layering in the device is caused. According to the invention, the conductive silver paste and the LTCC ceramic material are well matched through the following technical scheme.
The invention provides a conductive silver paste for an LTCC ceramic substrate, which comprises the following components in percentage by mass: consists of 82 to 86 percent of silver powder, 3 to 4 percent of macromolecular resin, 0.2 to 1.1 percent of glass powder and 10 to 15 percent of solvent.
The conductive silver paste provided by the invention is particularly suitable for CBS (CaO-B)2O3-SiO2) The LTCC substrate material, related substrate material, Ferro corporation, is disclosed in patent documents such as US5258335, and materials such as FerroA6M developed therefrom are also used in the frequency range of 10GHz to 100 GHz.
The silver powder is a basic functional material of the ceramic electronic paste, and among numerous conductive metals, the silver powder has excellent conductive and heat-conducting properties and is lower in price than noble metals such as gold and platinum handles, so that the silver powder is widely used for a functional box of the conductive paste, can provide high-quality physical and mechanical properties for the paste, and mainly determines the electrical property of the paste. The silver powder serving as the main component of the silver-containing electronic paste has direct influence on the performance of the paste on the particle size, morphology, dispersibility and the like.
In the present invention, the shape of the silver powder particles may be one or more of spherical, spheroidal, plate-like, triangular, rod-like, ribbon-like, and dendritic. Preferably, the silver powder is a plate-like silver powder. The particle size of the flake powder is not particularly limited, but preferably the average particle size (50% D) measured by a dynamic light scattering method is 2 to 8 μm. The silver paste prepared from the silver powder with the particle size within the range is beneficial to uniformly dispersing the silver powder in an organic carrier, so that a conductive electrode, a conductive grid and the like with good guiding performance uniformity are formed after sintering, and meanwhile, the sintering matching performance and the adhesion of the silver paste are improved.
In the present invention, the polymer resin is preferably contained in an amount of 3 to 3.5% by mass, or 3.5 to 3.8% by mass, or 3.8 to 4% by mass. The preferable polymer resin comprises ethyl cellulose, carboxymethyl cellulose and polyaspartic acid, and the weight ratio of the ethyl cellulose to the carboxymethyl cellulose to the polyaspartic acid is 1: 0.1-0.5: 0.05-0.1. More preferably, the weight ratio of the ethyl cellulose to the carboxymethyl cellulose to the polyaspartic acid is 1:0.3 to 0.4:0.06 to 0.08. In the structural composition of the conductive silver paste, the organic carrier is a structural framework of the conductive paste and is a carrier of the conductive phase silver powder, and the organic carrier has the functions of providing basic rheological property and adhesive force of the paste for the conductive silver paste and basic mechanical property of the paste, so that the paste has certain film forming property, durability and bending resistance. The high molecular resin is dissolved in the solvent to form the organic carrier, so that the silver powder and the glass powder are uniformly dispersed, the silver electrode slurry can be well adhered to the ceramic substrate, and after sintering, the organic carrier of various high molecular resins can be gradually volatilized and decomposed to be completely decomposed along with the temperature within the decomposition temperature range, so that the influence of sintering holes and cracks on the performances such as density, adhesive force and the like caused by weightlessness at concentrated temperature is prevented.
The glass powder is used as an adhesive in the silver electrode paste, so that the sintered silver electrode paste is firmly attached to the substrate, and the silver layer and the substrate are combined more tightly; during sintering, the glass powder is melted to have good wettability, the surface of the sintered silver electrode does not need to overflow from a glass phase, and the sintered silver electrode has enough adhesion with a substrate. The detection shows that the glass powder provided by the invention is used for conductive silver paste, has good stability, can form a good infiltration effect with silver powder and an LTCC ceramic substrate, and is particularly suitable for development of the conductive silver paste of the LTCC ceramic substrate.
In the invention, the glass powder comprises 30-40% of bismuth oxide (Bi) by mass percent2O3) 10 to 20 percent of copper oxide (CuO) and 15 to 25 percent of silicon oxide (SiO)2) 15% -20% of barium carbonate (BaCO)3) And 15% -20% of alumina (Al)2O3) And (4) forming. The glass powder can inhibit the shrinkage degree of the conductive silver paste, delay the sintering time of the silver paste and improve the sintering temperature. The glass powder enables the sintering of the silver paste to be well matched with the sintering process of the LTCC ceramic substrate, avoids the defects of mismatching of shrinkage ratio, warping and the like, and improves the adhesive force of the conductive silver paste to the ceramic and the adhesive force of the conductive silver paste to the ceramicAnd (5) compactness.
In the present invention, in order to ensure good function of the glass powder in the conductive silver paste, the preparation method is preferably as follows:
(1) weighing glass powder raw materials according to a proportion, and fully and uniformly mixing the raw materials to prepare a mixed material;
(2) placing the mixed material in a crucible, heating the mixed material in a resistance furnace at 1200-1350 ℃, and preserving heat for 20-35 min to obtain molten glass liquid;
(3) pouring molten glass liquid into deionized water for rapid quenching;
(4) and (3) putting the glass particles into a ball milling tank, ball milling for 12 hours, then sieving by a 300-mesh sieve, and drying to obtain the glass powder.
In the present invention, the solvent is preferably contained in an amount of 10% to 12% by mass, or 11% to 13% by mass, or 12% to 15% by mass. The solvent of the present invention is selected from one or two of alcohols and ethers. The alcohols include one or two of terpineol and butyl carbitol acetate, and the ethers include one or more of diethylene glycol butyl ether, diethylene glycol ethyl ether and diethylene glycol butyl ether acetate. Preferably, the solvent provided by the invention consists of terpineol and butyl carbitol acetate, and the volume ratio is preferably 1: 5-10. The solvent can fully dissolve the high polymer resin, so that the silver powder is fully dispersed in the high polymer resin, the viscosity and the stability of the internal electrode silver paste can be adjusted by the solvent, the drying speed of the internal electrode silver paste can also be adjusted, the drying speed of the internal electrode silver paste is moderate, the surface state of the dielectric layer can be changed, and the electrode silver paste and the dielectric layer have good wetting performance.
For convenience of printing, the viscosity of the conductive silver paste is preferably 50 Pa.s-300 Pa.s. In the present invention, the viscosity is measured at 25 ℃ using a Broodfield viscometer #52/1.5rpm, unless otherwise stated.
The invention also discloses a preparation method of the conductive silver paste for the LTCC ceramic substrate, which comprises the following steps:
(1) mixing the polymer resin and the solvent according to a certain proportion, and fully dissolving to obtain the organic carrier. According to the formula, a certain proportion of high molecular resin and a solvent are dissolved for 1 to 2 hours at a certain temperature of between 80 and 85 ℃ to form a uniform and transparent fluid with a certain viscosity, which is an organic carrier.
In the present invention, the preparation of the organic vehicle can be prepared by a method conventional in the art, and for example, may include the following steps: drying the polymer resin: placing the high molecular resin in an oven, keeping the constant temperature of 60-65 ℃ for 8-9 hours to fully dry the high molecular resin; mixing the polymer resin and the solvent according to a proportion, and fully dissolving to obtain a mixture: and (3) putting the container containing the solvent into a constant-temperature water bath box, selecting the temperature to be 80 ℃, adding the weighed polymer resin into the solvent, and simultaneously stirring for 2.5 hours at a constant speed by using an electric stirrer until the polymer is completely dissolved in the solvent. In the process, the solvent can be properly supplemented according to the volatilization condition of the used solvent, so that the proportion of the high molecular resin and the solvent is ensured, and the organic carrier is obtained; and filtering, standing, cooling and detecting the performance of the mixture.
(2) And uniformly mixing the organic carrier with the silver powder and the glass powder to obtain the premix. And (3) putting the organic carrier, the silver powder and the glass powder into a solid mixer for mixing, and pre-stirring by using an electric stirrer to obtain a premix.
(3) And fully grinding the premix to obtain the silver electrode slurry. The grinding is preferably repeated several times, for example 3, 4, 5, 6 or 7 more times, using a three-roll mill until a certain fineness (fineness. ltoreq.10 μm) is reached. In addition, the method also comprises the steps of filtering, detecting and supplementing the solvent for the silver electrode slurry. And removing impurities, silver sheets and other impurities from the conductive silver paste through a stainless steel filter screen. And then, detecting the viscosity and the inorganic solid content of the silver electrode slurry, and supplementing the volatile organic solvent in the grinding process according to the detection result to obtain the conductive silver slurry.
The preparation method of the silver electrode paste is simple to operate, and the prepared silver electrode paste is reasonable in proportion and easy to industrially produce in batches.
The invention is further described below by means of specific examples, which do not limit the scope of the patent protection of the invention in any way. In the present invention, various reagents used in examples are commercially available, for example, silver powder from Gui Ming platinum, Ethyl cellulose (N100) from Pianlong, carboxymethyl cellulose from North chemical, and polyaspartic acid from Texas chemical.
In the present invention, the general preparation method of the glass frit comprises:
(1) weighing glass powder raw materials according to a proportion, and fully and uniformly mixing the raw materials to prepare a mixed material;
(2) placing the mixed material in a crucible, heating the mixed material in a resistance furnace at 1250 ℃, and preserving heat for 20-35 min to obtain molten glass liquid;
(3) pouring molten glass liquid into deionized water for rapid quenching;
(4) and (3) putting the glass particles into a ball milling tank, ball milling for 12 hours, then sieving with a 300-mesh sieve, and drying to obtain the glass powder.
In the present invention, the general preparation method of the organic vehicle:
(1) placing the high molecular resin in an oven, keeping the constant temperature of 60-65 ℃ for 8-9 hours to fully dry the high molecular resin;
(2) mixing the polymer resin and the solvent according to a ratio, stirring in a constant-temperature water bath at 80 ℃ and fully dissolving to obtain a mixture, completely dissolving the polymer in the solvent, and cooling to obtain the organic carrier.
In the invention, the general preparation method of the conductive silver paste for the LTCC ceramic substrate comprises the following steps:
(1) mixing high molecular resin and a solvent according to a certain proportion, and fully dissolving to obtain an organic carrier;
(2) uniformly mixing an organic carrier with silver powder and glass powder to obtain a premix;
(3) and fully grinding the premix to obtain silver paste, and filtering, detecting and supplementing a solvent to obtain the conductive silver paste.
Table 1 shows the mass percentage composition of each example and the comparative example, in the examples, the solvent is the mixed solvent of terpineol and butyl carbitol acetate (volume ratio is 1: 5), and table 1 also shows the particle size of the silver powder used for the conductive silver paste prepared by each example. The silver content of the commercial conductive silver paste is 84% in the comparative example, and the silver content is unknown.
TABLE 1
| Composition in percentage by mass | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Silver powder (%) | 84 | 86 | 82 | 84 | 85 | 84 | 84 | 84 |
| Polymer resin (%) | 3 | 3.9 | 3 | 3 | 3.5 | 3 | 3 | / |
| Glass powder (%) | 0.7 | 0.2 | 1 | 0.7 | 0.4 | 0.7 | 0.7 | / |
| Solvent (%) | 12.3 | 9.9 | 14 | 12.3 | 11.1 | 12.3 | 12.3 | / |
| Average particle diameter of silver powder (. mu.m) | 4 | 3 | 2 | 4 | 3 | 4 | 3 | / |
The mass ratios of the components of the polymer resins in the examples and comparative examples are shown in Table 2. Wherein, the comparative example is the commercial conductive silver paste
TABLE 2
| Mass ratio of | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Ethyl cellulose | 1 | 1 | 1 | 1 | 1 | 1 | 1 | / |
| Carboxymethyl cellulose | 0.3 | 0.3 | 0.4 | 0.5 | 0.15 | 0.3 | 0 | / |
| Polyaspartic acid | 0.07 | 0.08 | 0.06 | 0.1 | 0.07 | 0 | 0.07 | / |
Table 3 shows the compositions of the glass frits of the examples and comparative examples.
TABLE 3
| Mass per hundred groupsBecome into | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Bi2O3（%） | 30 | 40 | 30 | 30 | 30 | 30 | 50 | / |
| CuO（%） | 20 | 10 | 20 | 20 | 10 | 20 | 20 | / |
| SiO2（%） | 15 | 20 | 15 | 15 | 25 | 15 | 15 | / |
| BaCO3（%） | 15 | 15 | 20 | 15 | 20 | 15 | 10 | / |
| Al2O3（%） | 20 | 15 | 15 | 20 | 15 | 20 | 5 | / |
Conductive pastes C1, C2, C3, C4, C5, CD1, CD2, and CD3 were prepared according to the foregoing preparation methods and the amounts in tables 1 to 3.
Test example
The conductive silver pastes C1, C2, C3, C4, C5, CD1, CD2 and CD3 in examples 1 to 5 and comparative examples 1 to 3 were printed on a ceramic substrate (Ferro A6M) using a 250 mesh stainless steel wire mesh, respectively, and then sintered under conditions including: sintering in the atmosphere of a tunnel furnace, wherein the peak temperature is 850 +/-5 ℃, and the peak time is 10 min. Thereafter, the respective samples were observed or tested for adhesion, conductivity, and density. At the same time, ± 1 μm at the interface of the coating and the substrate was sampled for EDS analysis of the components (with the interface being 0 point, "+" indicating the direction of the conductive silver layer and "-" indicating the direction of the substrate). The test results are shown in table 4.
TABLE 4
Wherein, the solder resistance test is carried out according to the solder resistance measurement in the noble metal slurry test method for the GB/T17473.7-2008 microelectronic technology, and the immersion time is 10 s.
In conclusion, the conductive silver paste for the LTCC ceramic substrate has good co-firing matching performance with the LTCC ceramic substrate, the silver layer has strong bonding force with a ceramic interface, and the silver layer is smooth and compact after sintering, keeps good conductivity and has good soldering resistance. With the popularization of the LTCC technology, the conductive silver paste and the preparation method thereof have great market value.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (5)
1. The utility model provides a conductive silver thick liquid for LTCC ceramic substrate which characterized in that: calculated by mass percent, comprises the following components: 82 to 86 percent of silver powder, 3 to 4 percent of polymer resin, 0.2 to 1.1 percent of glass powder and 10 to 15 percent of solvent; the polymer resin is composed of ethyl cellulose, carboxymethyl cellulose and polyaspartic acid, the weight ratio of the ethyl cellulose to the carboxymethyl cellulose to the polyaspartic acid is 1: 0.1-0.5: 0.05-0.1, and the silver powder is flake silver powder with the average particle size of 2-8 mu m.
2. The conductive silver paste for the LTCC ceramic substrate according to claim 1, wherein the weight ratio of the ethyl cellulose to the carboxymethyl cellulose to the polyaspartic acid is 1: 0.3-0.4: 0.06-0.08.
3. The conductive silver paste for the LTCC ceramic substrate according to claim 1, wherein the glass frit consists of 30-40% of bismuth oxide, 10-20% of copper oxide, 15-25% of silicon oxide, 15-20% of barium carbonate and 15-20% of aluminum oxide by mass percentage.
4. The conductive silver paste for the LTCC ceramic substrate according to claim 1, wherein the solvent is selected from one or two of alcohols and ethers, wherein the alcohols comprise one or two of terpineol and butyl carbitol acetate, and the ethers comprise one or more of diethylene glycol butyl ether, diethylene glycol ethyl ether and diethylene glycol butyl ether acetate.
5. A method for preparing the conductive silver paste for the LTCC ceramic substrate according to any one of claims 1 to 4, wherein the method comprises the following steps:
(1) mixing high molecular resin and a solvent according to a certain proportion, and fully dissolving to obtain an organic carrier;
(2) uniformly mixing an organic carrier with silver powder and glass powder to obtain a premix;
(3) and fully grinding the premix to obtain silver electrode slurry, and filtering, detecting and supplementing a solvent to the silver electrode slurry to obtain the conductive silver paste.
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