CN110880376A - Thick film dielectric paste with high thermal expansion coefficient for stainless steel base material and preparation method thereof - Google Patents
Thick film dielectric paste with high thermal expansion coefficient for stainless steel base material and preparation method thereof Download PDFInfo
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
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- H—ELECTRICITY
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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Abstract
The invention relates to a thick film dielectric paste with high thermal expansion coefficient for stainless steel base material and a preparation method thereof, wherein the thick film dielectric paste is characterized in that: comprises 70-80 wt% of lead-free microcrystalline glass powder and 20-30 wt% of organic bonding phase; the lead-free microcrystalline glass powder is BaO-CaO-Al2O3‑SiO2‑B2O3‑SrO‑Sm2O3‑ZrO2Is microcrystalline glass powder, which comprises 10-20 wt% of BaO, 10-15 wt% of CaO, and 5-10 wt% of Al2O320 to 30 percent of SiO25% -20% of B2O35 to 10 percent of SrO and 5 to 10 percent of Sm2O31 to 6 percent of ZrO2(ii) a The organic bonding phase comprises 70-85 wt% of organic solvent and 2-10 wt% of high-temperature-resistant organic solventThe adhesive comprises a molecular thickener, 0.5-5% of a dispersant, 0.5-5% of a flatting agent, 0.5-5% of a thixotropic agent and 0.5-5% of a surfactant. The thick film dielectric paste with high thermal expansion coefficient based on the stainless steel substrate has the characteristics of high uniformity, high stability, high solid content and the like.
Description
Technical Field
The invention relates to the field of thick film electronic paste, in particular to a thick film dielectric paste with high thermal expansion coefficient for a stainless steel substrate and a preparation method thereof.
Background
The high-power thick film circuit element and the thick film electric heating element have the characteristics of high power density, high mechanical strength, thermal shock resistance, vibration resistance and the like, and provide corresponding mechanical and thermal performance requirements for the substrate; the stainless steel substrate has the characteristics of good mechanical property, high mechanical strength, good impact resistance and the like, so that the stainless steel substrate is widely applied to the preparation of high-power thick film circuit elements and high-power thick film electric heating elements. At present, medium pastes for thick film circuit elements and thick film electrothermal elements based on 1Cr17 type stainless steel substrate are mature and commercialized, but the thermal expansion coefficient of the existing medium pastes is low (about 7-8 × 10)-6/° c), much lower than the coefficient of thermal expansion of a 1Cr17 type stainless steel substrate (10.6 × 10)-6/° c); the direct result caused by the mismatch of the thermal expansion coefficients is that the substrate and the dielectric layer expand with heat and contract with cold asynchronously, so that great thermal stress is generated between the dielectric layer and the substrate, the substrate deforms seriously due to the overlarge thermal stress, and the dielectric layer cracks and even peels off from the surface of the substrate.
When the existing thick film dielectric paste is applied to an ultrathin (the thickness is less than 0.8 mm) stainless steel substrate, the defects that the stainless steel substrate is deformed and seriously warped or deformed due to the mismatching of the thermal expansion coefficients of the dielectric paste and the stainless steel substrate, a conductor layer and a resistor layer cannot be continuously printed and the like exist, and the application range and the reliability of a thick film circuit element and a thick film electric heating element are reduced; meanwhile, when the existing thick film dielectric paste is applied to a thicker (the thickness is higher than 3.0 mm) stainless steel base material, microcracks and defects formed in an insulating dielectric layer in the cooling process due to the fact that the thermal expansion coefficients of the dielectric paste and the stainless steel base material are not matched exist, the microcracks and the defects provide channels for movement of electrons, and therefore the dielectric layer is low in breakdown voltage, small in insulation resistance, easy to break down in the using process, even short-circuit and the like.
Therefore, further improvements are needed.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides the thick film dielectric paste with high thermal expansion coefficient for the stainless steel substrate and the preparation method thereof.
The purpose of the invention is realized as follows:
a thick film dielectric paste with high thermal expansion coefficient for stainless steel base material is characterized in that: comprises 70-80 wt% of lead-free microcrystalline glass powder and 20-30 wt% of organic bonding phase;
the lead-free microcrystalline glass powder is BaO-CaO-Al2O3-SiO2-B2O3-SrO-Sm2O3-ZrO2Is microcrystalline glass powder, which comprises 10-20 wt% of BaO, 10-15 wt% of CaO, and 5-10 wt% of Al2O320 to 30 percent of SiO25% -20% of B2O35 to 10 percent of SrO and 5 to 10 percent of Sm2O31 to 6 percent of ZrO2；
The organic bonding phase comprises, by weight, 70-85% of an organic solvent, 2-10% of a polymer thickener, 0.5-5% of a dispersant, 0.5-5% of a leveling agent, 0.5-5% of a thixotropic agent and 0.5-5% of a surfactant.
The lead-free microcrystalline glass powder has an average particle size of 2-5 μm, a softening point of 650-780 ℃, and a thermal expansion coefficient of 8.5-10.5 x 10~6/℃。
The organic solvent is one or a mixture of more than two of terpineol, butyl carbitol acetate, diethylene glycol monomethyl ether, diethylene glycol dibutyl ether, ethylene glycol ethyl ether acetate, tributyl citrate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate, dioctyl phthalate, tributyl phosphate and 1, 4-butyrolactone.
The macromolecular thickener is one or a mixture of more than two of ethyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, nitrocellulose, polyvinyl butyral, polymethyl methacrylate, polyethyl methacrylate, polybutyl methacrylate and modified rosin resin.
The dispersant is one or a mixture of more than two of triamines citrate, polymethacrylic acid amine and 1, 4-dihydroxy sulfonic acid amine.
The flatting agent is one or a mixture of more than two of polydimethylsiloxane, polyether polyester modified organic siloxane, alkyl modified organic siloxane and acrylate flatting agents.
The thixotropic agent is one or a mixture of more than two of polyamide wax, polyethylene wax, hydrogenated castor oil, thixotropic alkyd resin, organic bentonite and fumed silica.
The surfactant is one or a mixture of more than two of lecithin, span-85, tween-60 and tween-80.
The thick film dielectric paste has the viscosity range of 110 +/-10 Pa-s and the fineness of less than 10 mu m.
The preparation method of the thick film dielectric paste with high thermal expansion coefficient for the stainless steel substrate is characterized by comprising the following steps: comprises the following steps
Step 1, preparing the lead-free glass-ceramic powder: mixing BaO, CaO and Al2O3、SiO2、B2O3、SrO、Sm2O3And ZrO2After being uniformly mixed in a three-dimensional mixer, the mixture is smelted in a high-temperature smelting furnace to obtain molten glass; then water quenching the molten glass, rolling the molten glass by a roller press, and finally grinding the glass balls by taking distilled water as a medium to obtain the lead-free glass ceramic powder;
step 2, preparing the organic bonding phase: dissolving an organic solvent, a high-molecular thickening agent, a dispersing agent, a flatting agent, a thixotropic agent and a surfactant in an oil bath at the temperature of 80 ℃ to obtain an organic bonding phase, and removing impurities through a filter screen;
step 3, preparing the thick film dielectric paste: and stirring and dispersing the lead-free microcrystalline glass powder and the organic bonding phase in a container, and then repeatedly grinding in a three-roll grinder to obtain the thick film dielectric paste.
In the step 1, the smelting temperature is 1400-1600 ℃, and the heat preservation time is 2-4 hours; the grinding time of the glass slag is 4-6 hours.
The invention has the following beneficial effects:
1. by adding BaO-CaO-Al2O3-SiO2-B2O3-SrO-Sm2O3-ZrO2The types and contents of oxides in the microcrystalline glass powder are adjusted, the melting temperature, the clarifying temperature, the thermal expansion coefficient, the vitrification temperature, the softening temperature, the crystallization temperature and the like of the lead-free microcrystalline glass powder are adjusted, the compactness and the insulativity of an insulating medium layer formed by compounding the lead-free microcrystalline glass powder and an organic bonding phase are greatly improved, and finally the thermal expansion coefficient of thick film medium slurry is very close to the thermal expansion coefficient of a stainless steel substrate (the difference is 1 multiplied by 10)-6V DEG C), thereby being widely applicable to ultrathin (the thickness is less than or equal to 0.8 mm) stainless steel base materials and thickened (the thickness is more than or equal to 3.0 mm) stainless steel base materials, the dielectric layer not only has good combination performance with the stainless steel base materials, but also has very high insulating property, good weather resistance, high temperature and high humidity resistance, cold and heat shock resistance and the like, and can adapt to the severe requirements of the working environment of high-power thick-film circuit elements and thick-film electric heating elements;
2. by adding BaO-CaO-Al2O3-SiO2-B2O3-SrO-Sm2O3-ZrO2The melting temperature, clarification temperature, high-temperature viscosity and fluidity of the microcrystalline glass powder are adjusted, the interface wettability and high-temperature adhesion of thick film dielectric paste and a stainless steel substrate are improved, and the performances such as sintering compactness, co-firing matching and the like are improved; by optimizing the polymer thickener and the auxiliary agent used by the organic carrier, the organic carrier has strong adhesive force after being dried at low temperature, and is convenient for repeated printing and drying of the dielectric layer; meanwhile, resin with lower temperature, more thorough and rapid gel discharge is selected as a macromolecular thickener, so that the defects of air bubbles, pinholes and the like caused by residual organic carriers are avoided, and the thick film mediumThe slurry can be repeatedly printed and dried on a stainless steel substrate and then sintered and formed into an insulating medium layer at a high temperature at one time, so that the sintering cost of the thick film medium layer can be greatly saved, the sintering efficiency is improved, and the process complexity is greatly reduced; in addition, the thick film dielectric layer prepared by the method has the advantages of strong adhesive force, high breakdown voltage, high insulation resistance, small leakage current, capability of being matched with resistance slurry and conductor slurry for a thick film circuit of a stainless steel substrate and the like, and the preparation process is simple to operate, easy to control and beneficial to realizing large-scale industrial production;
3. the thermal expansion performance of the insulating substrate after the thick film dielectric paste is sintered is matched with that of the thick film conductor paste and the resistance paste, the matching between different interfaces of the dielectric layer and the conductor layer, the dielectric layer and the resistance layer, the conductor layer and the resistance layer and the like is good, meanwhile, the consistency of each interface in the aspects of sintering densification rate, sintering shrinkage rate, thermal expansion rate and the like is good, and the defects of delaminating, warping, cracking and the like caused by mismatching between interface layers do not exist.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the specific embodiments.
Example 1
The thick film dielectric paste for the stainless steel substrate with the high thermal expansion coefficient comprises 75 wt% of lead-free microcrystalline glass powder and 25 wt% of organic bonding phase;
the lead-free microcrystalline glass powder is BaO-CaO-Al2O3-SiO2-B2O3-SrO-Sm2O3-ZrO2The glass-ceramic powder comprises, by weight, 20% of BaO, 14% of CaO and 10% of Al2O330% SiO28% of B2O35 percent of SrO and 10 percent of Sm2O33% of ZrO2(ii) a Alkaline earth metal oxides BaO and SrO and rare earth oxide Sm are added into lead-free microcrystalline glass powder2O3The thermal expansion coefficient of the lead-free glass ceramic powder can be improved, and the insulating property of the lead-free glass ceramic powder is not reduced;
the organic bonding phase comprises, by weight, 70-85% of an organic solvent, 2-10% of a polymer thickener, 0.5-5% of a dispersant, 0.5-5% of a leveling agent, 0.5-5% of a thixotropic agent and 0.5-5% of a surfactant.
Furthermore, the lead-free microcrystalline glass powder has an average particle size of 2-5 μm, a softening point of 750 ℃, and a thermal expansion coefficient of 9 x 10~6/℃。
Further, the organic solvent comprises 36% by weight of terpineol, 35% by weight of butyl carbitol and 17% by weight of tributyl citrate; the macromolecular thickener comprises 3 percent of nitrocellulose and 3 percent of polymethyl methacrylate by weight percentage; the dispersant comprises 2 weight percent of polymethacrylic acid amine; the leveling agent comprises 1% of polydimethylsiloxane by weight; the thixotropic agent comprises 2% by weight of a polyamide wax; the surfactant comprises 1% by weight of lecithin.
Furthermore, the thick film dielectric paste has a viscosity range of 110 +/-10 Pa-s and a fineness of less than 10 μm.
The preparation method of the thick film dielectric paste with high thermal expansion coefficient for the stainless steel substrate comprises the following steps
Step 1, preparing lead-free glass-ceramic powder: mixing BaO, CaO and Al2O3、SiO2、B2O3、SrO、Sm2O3And ZrO2After being uniformly mixed in a three-dimensional mixer, the mixture is smelted in a high-temperature smelting furnace to obtain molten glass; then water quenching the molten glass, rolling the molten glass by a roller press, and finally grinding the glass balls by taking distilled water as a medium to obtain lead-free glass ceramic powder;
step 2, preparing an organic bonding phase: dissolving an organic solvent, a high-molecular thickening agent, a dispersing agent, a flatting agent, a thixotropic agent and a surfactant in an oil bath at 80 ℃ to obtain an organic bonding phase, and removing impurities through a 200-mesh nylon filter screen;
step 3, preparing thick film dielectric paste: and stirring and dispersing the lead-free microcrystalline glass powder and the organic bonding phase in a container, and then repeatedly grinding the mixture in a three-roll grinder to obtain thick film dielectric paste.
Further, in the step 1, the smelting temperature is 1500 ℃, and the heat preservation time is 3 hours; the grinding time of the glass slag is 4-6 hours.
Further, printing the thick film dielectric paste on a 1Cr17 type stainless steel substrate with the thickness of 0.5mm by using a silk screen to form a film, and drying for 10min at 150 ℃; drying the thick film dielectric paste again by screen printing at 150 ℃ for 10min, and repeating the process for 4 times; and finally, in a tunnel furnace, binder removal is carried out for 1h at 450 ℃, the peak temperature is 850 ℃ for primary sintering for 40min, the thickness of the dielectric layer after sintering and forming is 130 mu M, the breakdown voltage (AC) is more than 2000V, the insulation resistance (500V) is more than 500M omega, and the leakage current (250V) is less than 0.5 mA.
Example 2
This embodiment differs from the first embodiment in that: the thick film dielectric paste for the stainless steel substrate with the high thermal expansion coefficient comprises 78 wt% of lead-free microcrystalline glass powder and 22 wt% of organic bonding phase;
the lead-free microcrystalline glass powder is BaO-CaO-Al2O3-SiO2-B2O3-SrO-Sm2O3-ZrO2The glass-ceramic powder comprises 18 wt% of BaO, 10 wt% of CaO and 5 wt% of Al2O325% SiO218% of B2O310 percent of SrO and 10 percent of Sm2O34% of ZrO2。
Further, the lead-free glass-ceramic powder had a softening point of 770 ℃ and a coefficient of thermal expansion of 9.2X 10~6/℃。
Further, the organic solvent comprises 36% by weight of butyl carbitol, 35% by weight of butyl carbitol acetate and 17% by weight of tributyl citrate; the macromolecular thickening agent comprises 3 percent of nitrocellulose and 3 percent of polybutylmethacrylate by weight percentage; the dispersant comprises 2 weight percent of polymethacrylic acid amine; the leveling agent comprises 2 weight percent of alkyl modified organic siloxane; the thixotropic agent comprises 1 percent by weight of polyethylene wax; the surfactant comprises 1% of span-85 by weight.
The above-mentioned stainless steel substrate thick film dielectric paste with high thermal expansion coefficient was prepared in the same manner as in the first example.
Further, in the preparation step 1, the melting temperature is 1400 ℃, and the heat preservation time is 4 hours.
Further, printing the thick film dielectric paste on a 1Cr17 type stainless steel substrate with the thickness of 0.8mm by using a silk screen to form a film, and drying for 10min at 150 ℃; again screen-printing the medium slurry, drying at 150 ℃ for 10min, repeating the above steps for 4 times; and finally, in a tunnel furnace, binder removal is carried out for 1h at 450 ℃, the peak temperature is 850 ℃ for primary sintering for 40min, the thickness of the dielectric layer after sintering and forming is 130 mu M, the breakdown voltage (AC) is more than 2000V, the insulation resistance (500V) is more than 500M omega, and the leakage current (250V) is less than 0.5 mA.
Example 3
This embodiment differs from the first embodiment in that: the thick film dielectric paste for the stainless steel substrate with the high thermal expansion coefficient comprises 75 wt% of lead-free microcrystalline glass powder and 25 wt% of organic bonding phase;
the lead-free microcrystalline glass powder is BaO-CaO-Al2O3-SiO2-B2O3-SrO-Sm2O3-ZrO2The glass-ceramic powder comprises 15 wt% of BaO, 15 wt% of CaO and 10 wt% of Al2O320% SiO220% of B2O310 percent of SrO and 5 percent of Sm2O35% of ZrO2。
Furthermore, the lead-free microcrystalline glass powder has a softening point of 775 ℃ and a thermal expansion coefficient of 9.6 x 10~6/℃。
Further, the organic solvent comprises 36% by weight of butyl carbitol, 35% by weight of butyl carbitol acetate and 17% by weight of tributyl citrate; the macromolecular thickening agent comprises 3 percent of ethyl cellulose and 3 percent of polybutylmethacrylate by weight percentage; the dispersant comprises 2 weight percent of polymethacrylic acid amine; the leveling agent comprises polyether polyester modified organic siloxane with the weight percentage of 2 percent; the thixotropic agent comprises 1% by weight of hydrogenated castor oil; the surfactant comprises 1% of span-85 by weight.
The above-mentioned stainless steel substrate thick film dielectric paste with high thermal expansion coefficient was prepared in the same manner as in the first example.
Further, in the preparation step 1, the melting temperature is 1400 ℃, and the heat preservation time is 4 hours.
Further, printing the thick film dielectric paste on a 1Cr17 type stainless steel substrate with the thickness of 3.0mm by using a silk screen to form a film, and drying for 10min at 150 ℃; again screen-printing the medium slurry, drying at 150 ℃ for 10min, repeating the above steps for 4 times; and finally, in a tunnel furnace, binder removal is carried out for 1h at 450 ℃, the peak temperature is 850 ℃ for primary sintering for 40min, the thickness of the dielectric layer after sintering and forming is 130 mu M, the breakdown voltage (AC) is more than 2000V, the insulation resistance (500V) is more than 500M omega, and the leakage current (250V) is less than 0.5 mA.
Example 4
This embodiment differs from the first embodiment in that: the thick film dielectric paste for the stainless steel substrate with the high thermal expansion coefficient comprises 80 wt% of lead-free microcrystalline glass powder and 20 wt% of organic bonding phase;
the lead-free microcrystalline glass powder is BaO-CaO-Al2O3-SiO2-B2O3-SrO-Sm2O3-ZrO2The glass-ceramic powder comprises, by weight, 20% of BaO, 15% of CaO and 10% of Al2O330% SiO28% of B2O35 percent of SrO and 10 percent of Sm2O32% of ZrO2。
Further, the lead-free glass-ceramic powder had a softening point of 765 ℃ and a thermal expansion coefficient of 9.8X 10~6/℃。
Further, the organic solvent comprises 36% by weight of terpineol, 35% by weight of butyl carbitol and 17% by weight of tributyl citrate; the macromolecular thickening agent comprises 3 percent of ethyl cellulose and 3 percent of polybutylmethacrylate by weight percentage; the dispersant comprises 2% by weight of triammonium citrate; the thixotropic agent comprises 1 percent by weight of polyethylene wax; the leveling agent comprises 2 weight percent of alkyl modified organic siloxane; the surfactant comprises 1% of tween-80 by weight.
The above-mentioned stainless steel substrate thick film dielectric paste with high thermal expansion coefficient was prepared in the same manner as in the first example.
Further, in the preparation step 1, the smelting temperature is 1600 ℃, and the heat preservation time is 2 hours.
Further, printing the thick film dielectric paste on a 1Cr17 type stainless steel substrate with the thickness of 5.0mm by using a silk screen to form a film, and drying for 10min at 150 ℃; again screen-printing the medium slurry, drying at 150 ℃ for 10min, repeating the above steps for 4 times; and finally, in a tunnel furnace, binder removal is carried out for 1h at 450 ℃, the peak temperature is 850 ℃ for primary sintering for 40min, the thickness of the dielectric layer after sintering and forming is 130 mu M, the breakdown voltage (AC) is more than 2000V, the insulation resistance (500V) is more than 500M omega, and the leakage current (250V) is less than 0.5 mA.
Example 5
This embodiment differs from the first embodiment in that: the thick film dielectric paste for the stainless steel substrate with the high thermal expansion coefficient comprises 80 wt% of lead-free microcrystalline glass powder and 20 wt% of organic bonding phase;
the lead-free microcrystalline glass powder is BaO-CaO-Al2O3-SiO2-B2O3-SrO-Sm2O3-ZrO2The glass-ceramic powder comprises, by weight, 16% of BaO, 10% of CaO and 7% of Al2O325% SiO218% of B2O310 percent of SrO and 10 percent of Sm2O34% of ZrO2。
Furthermore, the lead-free microcrystalline glass powder has a softening point of 770 ℃ and a coefficient of thermal expansion of 9.5X 10~6/℃。
Further, the organic solvent comprises 36 percent by weight of terpineol, 35 percent by weight of butyl carbitol acetate and 17 percent by weight of tributyl citrate; the macromolecular thickener comprises 3 weight percent of ethyl cellulose and 3 weight percent of nitrocellulose; the dispersant comprises 2 weight percent of polymethacrylic acid amine; the leveling agent comprises polyether polyester modified organic siloxane with the weight percentage of 2 percent; the thixotropic agent comprises 1% by weight of a polyamide wax and the surfactant comprises 1% by weight of lecithin.
The above-described method for preparing a thick film dielectric paste based on a stainless steel substrate of type 1Cr17 was the same as in the first example.
Further, in the preparation step 1, the smelting temperature is 1500 ℃, and the heat preservation time is 3 hours.
Further, printing the thick film dielectric paste on a 1Cr17 type stainless steel substrate with the thickness of 5.0mm by using a silk screen to form a film, and drying for 10min at 150 ℃; again screen-printing the medium slurry, drying at 150 ℃ for 10min, repeating the above steps for 4 times; and finally, in a tunnel furnace, binder removal is carried out for 1h at 450 ℃, the peak temperature is 850 ℃ for primary sintering for 40min, the thickness of the dielectric layer after sintering and forming is 130 mu M, the breakdown voltage (AC) is more than 2000V, the insulation resistance (500V) is more than 500M omega, and the leakage current (250V) is less than 0.5 mA.
Example 6
This embodiment differs from the first embodiment in that: the thick film dielectric paste for the stainless steel substrate with the high thermal expansion coefficient comprises 80 wt% of lead-free microcrystalline glass powder and 20 wt% of organic bonding phase;
the lead-free microcrystalline glass powder is BaO-CaO-Al2O3-SiO2-B2O3-SrO-Sm2O3-ZrO2The glass-ceramic powder comprises 10 wt% of BaO, 15 wt% of CaO and 10 wt% of Al2O330% SiO215% of B2O39 percent of SrO and 5 percent of Sm2O36% of ZrO2。
Further, the lead-free glass-ceramic powder had a softening point of 780 ℃ and a thermal expansion coefficient of 10X 10~6/℃。
Further, the organic solvent comprises 36% by weight of terpineol, 40% by weight of butyl carbitol acetate and 10% by weight of dioctyl phthalate; the macromolecular thickener comprises 4 percent of ethyl cellulose and 3 percent of modified rosin resin by weight percentage; the dispersant comprises 2% by weight of triammonium citrate; the leveling agent comprises 2 percent by weight of acrylate leveling agent; the thixotropic agent comprises 1 percent by weight of polyethylene wax; the surfactant comprises 2% by weight of tween-60.
The above-mentioned stainless steel substrate thick film dielectric paste with high thermal expansion coefficient was prepared in the same manner as in the first example.
Further, in the preparation step 1, the melting temperature is 1400 ℃, and the heat preservation time is 4 hours.
Further, printing the thick film dielectric paste on a 1Cr17 type stainless steel substrate with the thickness of 5.0mm by using a silk screen to form a film, and drying for 10min at 150 ℃; again screen-printing the medium slurry, drying at 150 ℃ for 10min, repeating the above steps for 4 times; and finally, in a tunnel furnace, binder removal is carried out for 1h at 450 ℃, the peak temperature is 850 ℃ for primary sintering for 40min, the thickness of the dielectric layer after sintering and forming is 130 mu M, the breakdown voltage (AC) is more than 2000V, the insulation resistance (500V) is more than 500M omega, and the leakage current (250V) is less than 0.5 mA.
The foregoing is a preferred embodiment of the present invention, and the basic principles, principal features and advantages of the invention are shown and described. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the embodiments and descriptions described above are only illustrative of the technical solutions of the present invention, and that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, and these changes and modifications fall within the scope of the claimed invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A thick film dielectric paste with high thermal expansion coefficient for stainless steel base material is characterized in that: comprises 70-80 wt% of lead-free microcrystalline glass powder and 20-30 wt% of organic bonding phase;
the lead-free microcrystalline glass powder is BaO-CaO-Al2O3-SiO2-B2O3-SrO-Sm2O3-ZrO2Is microcrystalline glass powder, which comprises 10-20 wt% of BaO, 10-15 wt% of CaO, and 5-10 wt% of Al2O320 to 30 percent of SiO25% -20% of B2O35 to 10 percent of SrO and 5 to 10 percent of Sm2O31 to 6 percent of ZrO2；
The organic bonding phase comprises, by weight, 70-85% of an organic solvent, 2-10% of a polymer thickener, 0.5-5% of a dispersant, 0.5-5% of a leveling agent, 0.5-5% of a thixotropic agent and 0.5-5% of a surfactant.
2. The thick film dielectric paste for stainless steel substrate with high thermal expansion coefficient according to claim 1, wherein: the lead-free microcrystalline glass powder has an average particle size of 2-5 μm, a softening point of 650-780 ℃, and a thermal expansion coefficient of 8.5-10.5 x 10~6/℃。
3. The thick film dielectric paste for stainless steel substrate with high thermal expansion coefficient according to claim 1, wherein: the organic solvent is one or a mixture of more than two of terpineol, butyl carbitol acetate, diethylene glycol monomethyl ether, diethylene glycol dibutyl ether, ethylene glycol ethyl ether acetate, tributyl citrate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate, dioctyl phthalate, tributyl phosphate and 1, 4-butyrolactone.
4. The thick film dielectric paste for stainless steel substrate with high thermal expansion coefficient according to claim 1, wherein: the macromolecular thickener is one or a mixture of more than two of ethyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, nitrocellulose, polyvinyl butyral, polymethyl methacrylate, polyethyl methacrylate, polybutyl methacrylate and modified rosin resin.
5. The thick film dielectric paste for stainless steel substrate with high thermal expansion coefficient according to claim 1, wherein: the dispersant is one or a mixture of more than two of triamines citrate, polymethacrylic acid amine and 1, 4-dihydroxy sulfonic acid amine; the flatting agent is one or a mixture of more than two of polydimethylsiloxane, polyether polyester modified organic siloxane, alkyl modified organic siloxane and acrylate flatting agents.
6. The thick film dielectric paste for stainless steel substrate with high thermal expansion coefficient according to claim 1, wherein: the thixotropic agent is one or a mixture of more than two of polyamide wax, polyethylene wax, hydrogenated castor oil, thixotropic alkyd resin, organic bentonite and fumed silica.
7. The thick film dielectric paste for stainless steel substrate with high thermal expansion coefficient according to claim 1, wherein: the surfactant is one or a mixture of more than two of lecithin, span-85, tween-60 and tween-80.
8. The thick film dielectric paste for stainless steel substrate with high thermal expansion coefficient according to claim 1, wherein: the thick film dielectric paste has the viscosity range of 110 +/-10 Pa-s and the fineness of less than 10 mu m.
9. The method for preparing a thick film dielectric paste with high thermal expansion coefficient for stainless steel substrate according to claim 1, wherein: comprises the following steps
Step 1, preparing the lead-free glass-ceramic powder: mixing BaO, CaO and Al2O3、SiO2、B2O3、SrO、Sm2O3And ZrO2After being uniformly mixed in a three-dimensional mixer, the mixture is smelted in a high-temperature smelting furnace to obtain molten glass; then water quenching the molten glass, rolling the molten glass by a roller press, and finally grinding the glass balls by taking distilled water as a medium to obtain the lead-free glass ceramic powder;
step 2, preparing the organic bonding phase: dissolving an organic solvent, a high-molecular thickening agent, a dispersing agent, a flatting agent, a thixotropic agent and a surfactant in an oil bath at the temperature of 80 ℃ to obtain an organic bonding phase, and removing impurities through a filter screen;
step 3, preparing the thick film dielectric paste: and stirring and dispersing the lead-free microcrystalline glass powder and the organic bonding phase in a container, and then repeatedly grinding in a three-roll grinder to obtain the thick film dielectric paste.
10. The method for preparing a thick film dielectric paste with high thermal expansion coefficient for stainless steel substrate according to claim 1, wherein: in the step 1, the smelting temperature is 1400-1600 ℃, and the heat preservation time is 2-4 hours; the grinding time of the glass slag is 4-6 hours.
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