CN114155992A - High-adhesion conductive silver paste for ceramic matrix composite and preparation method thereof - Google Patents
High-adhesion conductive silver paste for ceramic matrix composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-adhesion conductive silver paste for a ceramic matrix composite material and a preparation method thereof, and relates to the field of conductive paste. The functional phase is prepared by mixing the flake silver powder and the spherical silver powder, and meanwhile, the phosphate binder is added into the organic solvent, so that the adhesive force of the silver film is improved. The invention can overcome the problems of low matching degree of the existing conductive silver paste and the ceramic matrix composite material and poor adhesive force of a silver film formed by sintering.
Description
Technical Field
The invention relates to the field of conductive paste, in particular to high-adhesion conductive silver paste for a ceramic matrix composite and a preparation method thereof.
Background
The conductive silver paste is a key functional material required by electronic components, integrated circuits and solar cell industries, and has huge market demand and technical progress potential. The conductive silver paste can be solidified on a substrate such as ceramics to form a conductive network through the processes of screen printing, leveling, drying, sintering and the like, and can be made into thick film integrated circuits, resistors, resistor networks, capacitors, multilayer ceramic capacitors (MLCC), conductor ink, solar cell electrodes, LED cold light sources, Organic Light Emitting Displays (OLED), printed and high-resolution conductors, thin film switches/flexible circuits, conductive adhesives, sensitive components and other electronic components. The electronic paste has the characteristics of high quality, high benefit, advanced technology, wide application and the like, plays an important role in the fields of information and electronics, and is widely applied to the fields of aviation, aerospace, electronic computers, measurement and control systems, communication equipment, medical equipment, automobile industry, sensors, high-temperature integrated circuits, civil electronic products and the like.
The Frequency Selective Surface (FSS) is a single-screen or multi-screen periodic array structure composed of a large number of resonance units and is composed of periodically arranged metal patch units or periodically arranged aperture units on a metal screen. FSS can adjust the passband of the electromagnetic wave, let the antenna house realize the square wave and pass through, threaten the stealthy function of ripples to effectively realize anti-interference and the stealthy function of electromagnetism. The FSS wave-transmitting material is an artificial electromagnetic material containing an FSS structure, can improve or change the electromagnetic performance of an antenna, is the centralized embodiment and successful practice of structure-function integration pursued by the wave-transmitting material for a long time, is a new focus of wave-transmitting material research in recent years, is expected to bring great change to the field of wave-transmitting materials, and has wide application prospect in the field of multifunctional wave-transmitting and stealth wave-transmitting components.
The ceramic matrix composite has the advantages of low density, small linear thermal expansion coefficient, low thermal conductivity coefficient, high mechanical strength, high temperature resistance, thermal shock resistance, corrosion resistance, good dielectric property and the like, and is one of ideal selection materials for aerospace high-temperature wave-transmitting components. With the development of the technology, high-speed flight, accurate striking and stealth penetration have become the basic requirements of a new generation of flight weapons. The increasingly rapid cruising speed brings a harsh pneumatic environment, so that the use temperature of the antenna housing can reach over 600 ℃, and the application requirements of the ceramic-based wave-transmitting material are increasingly increased. The ceramic-based FSS wave-transparent material is mainly provided for the requirement of high-temperature (above 600 ℃) resistant high-performance antenna systems.
The periodic pattern can be prepared on the surface of the ceramic matrix composite material by screen printing of conductive silver paste, and then the frequency selective surface is prepared by drying and sintering. However, the ceramic matrix composite is a composite material with a porous structure, and the surface of the ceramic matrix composite is provided with some powder, so that the adhesive force of a silver film formed by sintering conductive silver paste is poor, and the ceramic matrix composite cannot cope with the severe use environment of the ceramic radome. Therefore, it is urgently needed to provide a high-adhesion conductive silver paste for ceramic matrix composite materials to solve the above problems.
Disclosure of Invention
In order to solve the problems that the matching degree of the existing conductive silver paste and a ceramic matrix composite material is low and the adhesive force of a silver film formed by sintering is poor, the invention provides the high-adhesive-force conductive silver paste for the ceramic matrix composite material and the preparation method thereof.
The technical scheme provided by the invention is as follows:
a high-adhesion conductive silver paste for a ceramic matrix composite comprises the following components in parts by mass:
60-80 parts of silver powder, which comprises spherical silver powder and flake silver powder in a mass ratio of (20-60) to (40-80);
5-10 parts of glass powder;
10-30 parts of organic solvent containing inorganic phosphoric acid binder;
2-5 parts of a thickening agent;
2-5 parts of a surfactant.
Further, the particle diameter of the spherical silver powder is 100-300nm (nanometer silver powder), and the plate diameter of the flaky silver powder is 3-8 μm (micrometer silver powder).
Furthermore, the glass powder comprises silicon oxide and two or three of zinc oxide, aluminum oxide and barium oxide, wherein the mass ratio of zinc oxide to aluminum oxide to barium oxide to silicon oxide is (0-30): (0-50): (0-40): (30-70).
Furthermore, the organic solvent also comprises terpineol and one or two of tributyl citrate and epoxy resin, and the mass ratio of the terpineol, the tributyl citrate, the epoxy resin and the inorganic phosphoric acid binder is (30-60): (0-5): (0-30): (30-40).
Further, ethyl cellulose is used as the thickener.
Further, the surfactant is one or two of toluene and ethanol.
A preparation method of high-adhesion conductive silver paste for a ceramic matrix composite material comprises the following steps:
1) weighing 60-80 parts by mass of spherical silver powder and flake silver powder in a mass ratio of (20-60) - (40-80), mixing, ball-milling, adding the ball-milled silver powder into acetone, sealing, performing ultrasonic treatment, and stopping ultrasonic treatment until the silver powder is uniformly dispersed;
2) weighing glass powder raw material components, uniformly mixing and grinding, smelting the ground powder, sintering and melting according to the melting point of the glass powder raw material components, performing water quenching on molten glass liquid to obtain glass slag, and performing ball milling, drying and dispersing to obtain 5-10 parts by mass of glass powder;
3) weighing 10-30 parts by mass of an organic solvent raw material containing an inorganic phosphoric acid binder, 2-5 parts by mass of a thickening agent and 2-5 parts by mass of a surfactant, and heating and stirring to obtain a uniformly mixed organic carrier;
4) adding the acetone dissolved with the silver powder prepared in the step 1) into the organic carrier, uniformly mixing, then adding the glass powder, continuously heating and stirring to obtain uniform slurry, and removing the acetone through reduced pressure distillation to obtain viscous slurry;
5) and carrying out step stirring on the viscous slurry at a low speed to a high speed, continuously repeating the step stirring procedure for a plurality of times to uniformly disperse the slurry, removing bubbles in the slurry, and repeatedly grinding until the particle size is less than 10 mu m to obtain the high-adhesion conductive silver paste for the ceramic matrix composite.
Further, the particle diameter of the spherical silver powder is 100-300nm, and the plate diameter of the flaky silver powder is 3-8 μm; the rotating speed of the ball mill adopted in the step 1) is 200-300r/min, and the ball milling time is 2-4 h.
Further, the mass ratio of the acetone to the silver powder is (8-10): 1.
Further, whether the silver powder is uniformly dispersed in the acetone is observed every 30min-1h during ultrasonic treatment.
Furthermore, the glass powder comprises silicon oxide and two or three of zinc oxide, aluminum oxide and barium oxide, wherein the mass ratio of zinc oxide to aluminum oxide to barium oxide to silicon oxide is (0-30) to (0-50) to (0-40) to (30-70); the method for sintering and melting the glass powder according to the melting points of the raw material components comprises the following steps: selecting a sintering procedure according to the melting points of oxides in the raw material components of the glass powder, preserving heat for 30min-1h at the melting point of each oxide component, and preserving heat for 4-6h at the highest melting point temperature; the stepwise stirring procedure was repeated 3-4 times continuously.
Furthermore, the organic solvent also comprises terpineol and one or two of tributyl citrate and epoxy resin, and the mass ratio of the terpineol, the tributyl citrate, the epoxy resin and the inorganic phosphoric acid binder is (30-60): (0-5): (0-30): (30-40).
Further, the temperature in step 3) is 60-75 ℃.
Further, the temperature of the heating and stirring in the step 4) is 80-90 ℃, and the stirring lasts for 1-2 hours.
Further, the step stirring is performed at 100r/min for 5min, at 200r/min for 10min, at 500r/min for 10min, at 1000r/min for 20min, but the number of steps is limited, and the stirring speed and time of each step are not limited, and the step stirring is adjusted according to actual conditions so as to ensure continuous transition from low-speed stirring to high-speed stirring.
The invention achieves the following beneficial effects: (1) according to the invention, the inorganic phosphate binder is added into the organic solvent, and the binder and the silicon dioxide on the surface of the ceramic matrix composite form hydrogen bonds, so that the adhesive force of the silver film is enhanced. (2) The silver paste is mixed by the planetary gravity stirrer and the three-roller grinding machine, so that the uniform mixing of the paste is facilitated, and the silver powder particles in the silver paste are prevented from agglomerating. (3) The prepared silver paste has good adhesive force on the surface of the ceramic matrix composite material, and can be applied to the preparation of the frequency selection surface of the ceramic matrix composite material. (4) If the spherical silver powder is used alone, the particles are separated from each other during sintering, resulting in failure to form a conductive network and poor conductivity. If the flaky silver powder is used independently, the silver powder is easy to agglomerate in the mixing process, so that the silver paste is uneven.
Drawings
FIG. 1 is a flow chart of the preparation of the high adhesion conductive silver paste for ceramic matrix composites of the present invention.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below.
The invention provides a preparation method of high-adhesion conductive silver paste for a ceramic matrix composite, which comprises the following steps of:
1) functional phase dispersion: weighing 60-80 parts by mass of spherical silver powder and flake silver powder in a mass ratio of (20-60): (40-80), mixing and placing the spherical silver powder and the flake silver powder in a ball mill, mixing at the rotating speed of 300r/min, ball milling for 2-4h, adding the mixed silver powder into a beaker containing acetone in a mass ratio of (8-10):1, sealing the beaker with a preservative film, placing the beaker in an ultrasonic cleaner for ultrasonic treatment, and observing whether the silver powder is uniformly dispersed in the acetone every 30min-1h until the silver powder is uniformly dispersed, and stopping the ultrasonic treatment.
2) Preparing glass powder: firstly, weighing the using amount of oxides according to the proportion of (0-30) to (0-50) to (0-40) to (30-70) of zinc oxide, aluminum oxide, barium oxide and silicon oxide, then uniformly mixing the oxides, grinding the mixture in a mortar, smelting the ground powder in a smelting furnace, selecting a sintering procedure according to the melting point of the oxides, preserving heat for 30min to 1h at the melting point of each oxide component, preserving heat for 4 to 6h at the highest melting point temperature, and quickly pouring molten glass liquid into cold water for cooling. Pouring the water-quenched glass slag into a ball milling tank, performing ball milling for more than 24 hours, and drying and dispersing the ball-milled glass powder to obtain the required 5-10 parts by mass of glass powder.
3) Preparing an organic carrier: adding terpineol into a round-bottom flask, carrying out water bath at 60-75 ℃, adding 2-5 parts by mass of thickening agent ethyl cellulose under mechanical stirring, adding tributyl citrate, epoxy resin, inorganic phosphoric acid binder and 2-5 parts by mass of surfactant according to a proportion after the ethyl cellulose is completely dissolved, and continuing heating and stirring. Wherein the proportion of the terpineol, the tributyl citrate, the epoxy resin and the inorganic phosphoric acid adhesive is (30-60): (0-5): 0-30): 30-40, and the total is 10-30 parts.
4) Three-phase mixing: after the organic carrier is uniformly mixed, slowly adding acetone dissolved with silver powder into a round-bottom flask, uniformly mixing, then adding glass powder, increasing the mechanical stirring speed, raising the temperature of a water bath to 80-90 ℃, and continuing for 1-2 hours to obtain uniform slurry; therefore, the slurry also contains a large amount of acetone, and the acetone is subsequently removed by distillation under reduced pressure to obtain a viscous slurry.
5) Stirring the slurry: adding the viscous slurry obtained in the step 4 into a material cup of a planetary gravity stirrer, accelerating to 200r/min for 10min, accelerating to 500r/min for 10min, accelerating to 1000r/min for 20min at 100r/min, and continuously repeating the procedures for 3-4 times, so that the slurry is dispersed more uniformly and bubbles in the slurry can be removed; and pouring the prepared silver paste into a three-roll grinder, repeatedly grinding until the whole particle size is less than 10 mu m, and obtaining the conductive silver paste with uniform particle size dispersion and good relative leveling property.
The following examples adopt the above specific implementation method to prepare the high-adhesion conductive silver paste for the ceramic matrix composite, the specific implementation parameters are shown in the tables in each example, and the text description of the steps is not repeated.
Example 1
The conductive silver paste is prepared according to the following mass ratio:
80 parts of silver powder, 5 parts of glass powder, 10 parts of organic solvent, 2 parts of thickening agent and 3 parts of surfactant. Wherein the silver powder is a mixture of spherical silver powder and flake silver powder, and the ratio is 20: 80; the glass powder consists of zinc oxide, aluminum oxide and silicon oxide in a ratio of 20:20: 70; the organic solvent is terpineol, tributyl citrate and an inorganic phosphate binder in a ratio of 60:2: 38; the thickening agent is ethyl cellulose, and the surfactant is toluene.
The conductive silver paste is prepared according to the steps of the specific implementation method, and specific condition parameters are shown in the following table 1.
Table 1 condition parameters in the preparation of example 1
Comparative example 1 is given herein, and a comparative silver paste was prepared using prior art terpineol instead of the inorganic phosphate binder in the formulation and spherical silver powder instead of the mixed silver powder.
Silver films were prepared on the silica composite reinforced with quartz fibers by screen printing and sintering at 800 c using two silver pastes prepared in example 1 and comparative example 1, respectively. The adhesion of the silver film is respectively tested by a cross-cut method according to the GB/T9286-1998 test standard, and the following results are obtained: the adhesive force of the slurry added with the inorganic phosphate adhesive can reach level 1, the sheet resistance of the silver film is 5m omega/□, while the adhesive force of the slurry prepared by adopting the prior art is only level 3, and the sheet resistance is 10m omega/□.
Example 2
The conductive silver paste is prepared according to the following mass ratio:
75 parts of silver powder, 8 parts of glass powder, 13 parts of organic solvent, 3 parts of thickening agent and 2 parts of surfactant. Wherein the silver powder is a mixture of spherical silver powder and flake silver powder in a ratio of 50: 50; the glass powder consists of zinc oxide, aluminum oxide, barium oxide and silicon oxide in a ratio of 20:50:10: 50; the organic solvent is terpineol, tributyl citrate, epoxy resin and an inorganic phosphoric acid binder in a ratio of 50:5:15: 30; the thickening agent is ethyl cellulose, and the surfactant is ethanol.
The conductive silver paste is prepared according to the steps of the specific implementation method, and specific condition parameters are shown in the following table 2.
Table 2 condition parameters in the preparation of example 2
Comparative example 2 is given herein, and a comparative silver paste was prepared using prior art terpineol instead of the inorganic phosphate binder in the formulation and spherical silver powder instead of the mixed silver powder.
Silver films were prepared on the silica composite reinforced with quartz fibers by screen printing and sintering at 800 c using two silver pastes prepared in example 2 and comparative example 2, respectively. The adhesion of the silver film is respectively tested by a cross-cut method according to the GB/T9286-1998 test standard, and the following results are obtained: the adhesive force of the slurry added with the inorganic phosphate adhesive can reach 0 grade, the sheet resistance of the silver film is 7m omega/□, while the adhesive force of the slurry prepared by adopting the prior art is only 2 grade, and the sheet resistance is 12m omega/□, obviously, the invention can enhance the adhesive force of the silver film and improve the conductivity of the silver film.
Example 3
The conductive silver paste is prepared according to the following mass ratio:
60 parts of silver powder, 10 parts of glass powder, 30 parts of organic solvent, 5 parts of thickening agent and 5 parts of surfactant. Wherein the silver powder is a mixture of spherical silver powder and flake silver powder in a ratio of 60: 40; the glass powder consists of zinc oxide, barium oxide and silicon oxide in a ratio of 30:40: 30; the organic solvent is terpineol, epoxy resin and inorganic phosphate binder, and the proportion is 30:30: 40; the thickening agent is ethyl cellulose, and the surfactant is toluene.
The conductive silver paste was prepared according to the steps of the above specific implementation method, and the specific condition parameters are shown in table 3 below.
Table 3 condition parameters in the preparation of example 3
| Parameter item | Parameter(s) |
| Silver powder component | 60 parts by mass of spherical silver powder and flake silver powder in a mass ratio of 60:40 |
| Glass powder component | 10 parts by mass of zinc oxide, barium oxide and silicon oxide in a mass ratio of 30:40:30 |
| Organic solvent component | 30 parts by mass of terpineol, epoxy resin and inorganic phosphate binder in a mass ratio of 30:30:40 |
| Thickener component | 5 parts by mass of ethyl cellulose |
| Surfactant component | 5 parts by mass of toluene |
| Step 1) ball milling parameters | 300r/min，2h |
| Step 1) mass ratio of acetone to silver powder | 10:1 |
| Step 1) ultrasonic observation of the interval time | 1h |
| Step 2) sintering parameters | Keeping the temperature at the melting point of each oxide component for 1h and keeping the temperature at the highest melting point for 6h |
| Step 2) ball milling time | 36h |
| Step 3) Water bath parameters | 75℃ |
| Step 4) Water bath parameters | 90℃，1h |
| Step 5) step stirring parameters | 100r/min for 5min, 300r/min for 10min, 1000r/min for 20min |
| Step 5) repeat number of step stirring | 4 times (twice) |
Comparative example 3 is given herein, and comparative silver paste was prepared using prior art terpineol instead of the inorganic phosphate binder in the formulation and flake silver powder instead of the mixed silver powder.
Silver films were prepared on the silica composite reinforced with quartz fibers by screen printing and sintering at 800 c using two silver pastes prepared in example 3 and comparative example 3, respectively. The adhesion of the silver film is respectively tested by a cross-cut method according to the GB/T9286-1998 test standard, and the following results are obtained: the adhesive force of the slurry added with the inorganic phosphate adhesive can reach 0 grade, the sheet resistance of the silver film is 20m omega/□, while part of silver powder in the slurry prepared by the prior art is agglomerated, the adhesive force is only 3 grades, and the sheet resistance is 23m omega/□.
Although the present invention has been described with reference to the above embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The high-adhesion conductive silver paste for the ceramic matrix composite is characterized by comprising the following components in parts by mass:
60-80 parts of silver powder, which comprises spherical silver powder and flake silver powder in a mass ratio of (20-60) to (40-80);
5-10 parts of glass powder;
10-30 parts of organic solvent containing inorganic phosphoric acid binder;
2-5 parts of a thickening agent;
2-5 parts of a surfactant.
2. The high-adhesion conductive silver paste for ceramic matrix composites according to claim 1, wherein the particle size of the spherical silver powder is 100-300nm, and the plate size of the plate-shaped silver powder is 3-8 μm.
3. The high-adhesion conductive silver paste for the ceramic matrix composite material as claimed in claim 1, wherein the glass powder comprises silicon oxide and two or three of zinc oxide, aluminum oxide and barium oxide, and the mass ratio of zinc oxide, aluminum oxide, barium oxide and silicon oxide is (0-30): 0-50): 0-40): 30-70); the organic solvent also comprises terpineol, and also comprises one or two of tributyl citrate and epoxy resin, wherein the mass ratio of the terpineol to the tributyl citrate to the epoxy resin to the inorganic phosphoric acid adhesive is (30-60) to (0-5) to (0-30) to (30-40); the thickening agent adopts ethyl cellulose; the surfactant is one or two of toluene and ethanol.
4. A preparation method of high-adhesion conductive silver paste for a ceramic matrix composite is characterized by comprising the following steps:
1) weighing 60-80 parts by mass of spherical silver powder and flake silver powder in a mass ratio of (20-60) - (40-80), mixing, ball-milling, adding the ball-milled silver powder into acetone, sealing, performing ultrasonic treatment, and stopping ultrasonic treatment until the silver powder is uniformly dispersed;
2) weighing glass powder raw material components, uniformly mixing and grinding, smelting the ground powder, sintering and melting according to the melting point of the glass powder raw material components, performing water quenching on molten glass liquid to obtain glass slag, and performing ball milling, drying and dispersing to obtain 5-10 parts by mass of glass powder;
3) weighing 10-30 parts by mass of an organic solvent raw material containing an inorganic phosphoric acid binder, 2-5 parts by mass of a thickening agent and 2-5 parts by mass of a surfactant, and heating and stirring to obtain a uniformly mixed organic carrier;
4) adding the acetone dissolved with the silver powder prepared in the step 1) into the organic carrier, uniformly mixing, then adding the glass powder, continuously heating and stirring to obtain uniform slurry, and removing the acetone through reduced pressure distillation to obtain viscous slurry;
5) and carrying out step stirring on the viscous slurry at a low speed to a high speed, continuously repeating the step stirring procedure for a plurality of times to uniformly disperse the slurry, removing bubbles in the slurry, and repeatedly grinding until the particle size is less than 10 mu m to obtain the high-adhesion conductive silver paste for the ceramic matrix composite.
5. The method according to claim 4, wherein the spherical silver powder has a particle diameter of 100-300nm and the flake silver powder has a flake diameter of 3-8 μm; the rotating speed of the ball mill adopted in the step 1) is 200-300r/min, and the ball milling time is 2-4 h.
6. The method according to claim 4, wherein the mass ratio of the acetone to the silver powder is (8-10): 1.
7. The method of claim 4, wherein the glass powder is composed of silicon oxide, and two or three of zinc oxide, aluminum oxide and barium oxide, wherein the mass ratio of zinc oxide, aluminum oxide, barium oxide and silicon oxide is (0-30): 0-50): 0-40): 30-70); the method for sintering and melting the glass powder according to the melting points of the raw material components comprises the following steps: selecting a sintering procedure according to the melting points of oxides in the raw material components of the glass powder, preserving heat for 30min-1h at the melting point of each oxide component, and preserving heat for 4-6h at the highest melting point temperature; the stepwise stirring procedure was repeated 3-4 times continuously.
8. The method as in claim 4, wherein the organic solvent further comprises terpineol, and further comprises one or two of tributyl citrate and epoxy resin, and the mass ratio of the terpineol, the tributyl citrate, the epoxy resin and the inorganic phosphoric acid binder is (30-60): 0-5): 0-30: (30-40).
9. The method of claim 4, wherein the temperature in step 3) is 60-75 ℃; in the step 4), the temperature for raising the temperature and stirring is 80-90 ℃, and the stirring lasts for 1-2 hours.
10. The method of claim 4, wherein the step agitation is at 100r/min for 5min, at 200r/min for 10min, at 500r/min for 10min, and at 1000r/min for 20 min.
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| CN115594404A (en) * | 2022-10-12 | 2023-01-13 | 合肥卓华智能科技有限公司（Cn） | Preparation and use method of fluidity-controllable glass slurry |
| CN115938641A (en) * | 2022-12-13 | 2023-04-07 | 航天特种材料及工艺技术研究所 | High-temperature conductive slurry used at temperature of more than 1000 ℃ and preparation method thereof |
| CN116994795A (en) * | 2023-08-22 | 2023-11-03 | 昆明理工大学 | Silver paste for medium-temperature sintered ceramic filter and preparation method thereof |
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