CN113362985A - Nano rare earth thick film electronic paste and preparation method thereof - Google Patents
Nano rare earth thick film electronic paste and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a nanometer rare earth thick film electronic paste and a preparation method thereof, belonging to the technical field of electronic materials, wherein the electronic paste comprises the following raw materials: dispersing a carrier, a binder, rare earth oxide, ruthenium dioxide and silver powder; the preparation method of the electronic paste comprises the following steps: firstly, weighing raw materials in parts by weight; and secondly, mixing the binder, the dispersing carrier, the rare earth oxide, ruthenium dioxide and the silver powder, placing the mixture into a grinding machine for grinding, and sieving the ground mixture through a 800-mesh sieve to obtain the nano rare earth thick film electronic paste. The modified microcrystalline cellulose is prepared by taking the modified microcrystalline cellulose as a raw material and adding the polydopamine-coated graphene oxide to prepare an additive, wherein the additive is a conductive and biodegradable compound. On one hand, the oxidation resistance of the thick film is improved; on the other hand, the mechanical property is improved, and in addition, the friction resistance of the material can be improved to a certain extent by the cellulose nanocrystal.
Description
Technical Field
The invention belongs to the technical field of electronic materials, and particularly relates to nano rare earth thick film electronic paste and a preparation method thereof.
Background
The thick film electronic paste can be subdivided into dielectric paste, resistance paste, electrode paste and the like according to different use functions; according to different components of the functional phase, the thick-film electronic paste can be divided into ceramic paste, precious metal paste and base metal paste; the slurry can be divided into screen printing slurry and casting slurry according to different use processes of the slurry.
The thick film integrated circuit is a circuit unit which can meet certain functional requirements by manufacturing resistors, capacitors, wires and the like on a substrate through processes of screen printing, tape casting, drying, sintering and the like. Thick film electronic pastes are primarily referred to as paste-like material systems for printing and casting. As a core material of thick film heating technology, thick film electronic paste plays an important role in thick film heating technology. After the electronic paste is sintered, oxygen or sulfur-containing gas in the environment is easily adsorbed, so that metal components in the thick film are subjected to oxidation reaction to generate oxides, sulfides and the like, and the oxides, the sulfides and the like are attached to the surface of the thick film in a floccule form, so that the surface roughness of a sample is increased, the diffuse reflectance is reduced, the metal luster is lost, and the conductivity is greatly reduced.
Disclosure of Invention
The invention aims to provide nano rare earth thick film electronic paste and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
the nanometer rare earth thick film electronic paste comprises the following raw materials in parts by weight:
10-20 parts of a dispersing carrier, 10-20 parts of a binder, 1-5 parts of rare earth oxide, 2-5 parts of ruthenium dioxide and 70-80 parts of silver powder;
the dispersion carrier is prepared by the following steps:
mixing diethylene glycol monomethyl ether, tributyl phosphate and ethyl cellulose at 70 ℃, then adding an additive, polyamide wax and 1, 4-butyrolactone, and uniformly stirring to obtain a dispersion carrier, wherein the mass ratio of the diethylene glycol monomethyl ether, the tributyl phosphate, the ethyl cellulose, the additive, the polyamide wax and the 1, 4-butyrolactone is 42: 20: 10-15: 5: 1.5: 1.
further, the additive is prepared by the following steps:
step S11, mixing graphene oxide, dopamine hydrochloride and Tris-HCl buffer solution, then performing ultrasonic dispersion for 10min at the temperature of 0 ℃, then performing stirring reaction for 24h at the temperature of 60 ℃, performing suction filtration under reduced pressure after the reaction is finished, and washing a filter cake with deionized water until a washing solution is colorless to obtain a solid a;
step S12, mixing modified microcrystalline cellulose and deionized water to prepare a suspension, adding an aqueous solution of sodium bromide and tetramethylpiperidine oxynitride while stirring, adjusting the pH value to 10 by using 0.5mol/L sodium hydroxide, adding a sodium hypochlorite solution, stirring and reacting for 4 hours at the temperature of 20 ℃, adding absolute ethyl alcohol after the reaction is finished, performing centrifugal treatment to remove a supernatant, and washing by using distilled water until a washing solution is neutral to obtain a solid b;
and step S13, mixing the solid a, the solid b and deionized water, and stirring for 3 hours to obtain the additive.
Further, in step S11, the concentration of the Tris-HCl buffer solution is 10mmol/L, the pH value is 8.5, and the dosage ratio of the graphene oxide, the dopamine hydrochloride and the Tris-HCl buffer solution is 2 mg: 1 mg: 4 mL; in step S12, the aqueous solution of tetramethylpiperidine nitroxide is tetramethylpiperidine nitroxide and deionized water in an amount of 3 mg: 8mL of the mixture is mixed; the mass fraction of the sodium hypochlorite solution is 15 percent; the dosage ratio of the modified microcrystalline cellulose to the deionized water to the aqueous solution of sodium bromide, tetramethylpiperidine oxynitride to the sodium hypochlorite solution is 0.5 g: 50mL of: 0.16 g: 50mL of: 2.48 g; the using ratio of the solid a to the solid b to the deionized water in the step S13 is 1 g: 2 g: 100 mL.
Further, the modified microcrystalline cellulose is prepared by the steps of:
step S21, mixing chlorinated trimellitic anhydride, pyridine and tetrahydrofuran, then adding microcrystalline cellulose, stirring and reacting for 11-12 h at 20 ℃, and after the reaction is finished, concentrating the obtained reaction liquid under reduced pressure to remove the solvent to obtain an intermediate 1;
and step S22, mixing the intermediate 1 with glacial acetic acid, adding ethylenediamine at 0 ℃, stirring at room temperature for 50-60 min after the ethylenediamine is added, heating to 120 ℃ for reaction for 5-8 h, cooling to room temperature after the reaction is finished, mixing with 10 times of volume of deionized water, carrying out vacuum filtration, washing a filter cake with the deionized water, and carrying out vacuum drying at 40 ℃ to constant weight after the washing is finished to obtain the modified microcrystalline cellulose.
Further, the usage ratio of the chlorinated trimellitic anhydride, pyridine, tetrahydrofuran and microcrystalline cellulose in step S21 was 12 g: 4.5 g: 300 mL: 5g of the total weight of the mixture; in the step S22, the dosage ratio of the intermediate 1, the glacial acetic acid and the ethylenediamine is 12 g: 300 mL: 3g of the total weight.
Further, the binder is prepared by the steps of:
calcium oxide, bismuth trioxide, silicon dioxide, zinc oxide, silver oxide and aluminum oxide in a mass ratio of 4: 4: 2: 3: 1: 1, mixing and grinding, then smelting at 1100 ℃ for 2h, and sieving through a 1000-mesh sieve after water quenching to obtain the binder.
Further, the particle size value of the silver powder is 200nm to 800 nm.
Further, the rare earth oxide is one or two of lanthanum oxide and yttrium oxide which are mixed according to any proportion.
A preparation method of nano rare earth thick film electronic paste comprises the following steps:
firstly, weighing raw materials in parts by weight;
and secondly, mixing the binder, the dispersing carrier, the rare earth oxide, ruthenium dioxide and the silver powder, placing the mixture into a grinding machine for grinding, and sieving the ground mixture through a 800-mesh sieve to obtain the nano rare earth thick film electronic paste.
The invention has the beneficial effects that:
in the process of preparing the nano rare earth thick film electronic paste, modified microcrystalline cellulose is prepared, an imide structure is introduced into the structure of the microcrystalline cellulose, the high and low temperature resistance is excellent, then the modified microcrystalline cellulose is used as a raw material, carboxyl is firstly introduced through oxidation to prepare a solid b, and then the polydopamine-coated graphene oxide is added to prepare an additive, wherein the additive is a conductive and biodegradable compound. The dopamine can be polymerized in an alkaline condition to form polydopamine, and the polydopamine is physically coated on the surface of the graphene oxide and reduced, so that the conductivity of the material is improved. Meanwhile, the surface of the poly-dopamine-coated graphene oxide contains a large number of catechol structures, so that on one hand, the introduction of phenolic hydroxyl groups delays the oxidation of the thick film, and the oxidation resistance of the thick film is improved; on the other hand, the material can generate strong interface interaction with matrix carboxylated cellulose nanocrystals, so that the mechanical property is improved, and in addition, the friction resistance of the material can be improved to a certain extent by the cellulose nanocrystals.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing modified microcrystalline cellulose:
step S21, mixing chlorinated trimellitic anhydride, pyridine and tetrahydrofuran, then adding microcrystalline cellulose, stirring and reacting for 11 hours at 20 ℃, and after the reaction is finished, concentrating the obtained reaction liquid under reduced pressure to remove the solvent to obtain an intermediate 1;
and step S22, mixing the intermediate 1 with glacial acetic acid, adding ethylenediamine at 0 ℃, stirring for 50min at room temperature after the addition is finished, heating to 120 ℃ for reaction for 5h, cooling to room temperature after the reaction is finished, mixing with 10 times of volume of deionized water, carrying out vacuum filtration, washing a filter cake with the deionized water, and carrying out vacuum drying at 40 ℃ to constant weight after the washing is finished to obtain the modified microcrystalline cellulose.
Wherein the dosage ratio of the chlorinated trimellitic anhydride to the pyridine to the tetrahydrofuran to the microcrystalline cellulose in the step S21 is 12 g: 4.5 g: 300 mL: 5g of the total weight of the mixture; in the step S22, the dosage ratio of the intermediate 1, the glacial acetic acid and the ethylenediamine is 12 g: 300 mL: 3g of the total weight.
Example 2
Preparing modified microcrystalline cellulose:
step S21, mixing chlorinated trimellitic anhydride, pyridine and tetrahydrofuran, then adding microcrystalline cellulose, stirring and reacting for 12 hours at 20 ℃, and after the reaction is finished, concentrating the obtained reaction liquid under reduced pressure to remove the solvent to obtain an intermediate 1;
and step S22, mixing the intermediate 1 with glacial acetic acid, adding ethylenediamine at 0 ℃, stirring for 60min at room temperature after the addition is finished, heating to 120 ℃ for reaction for 8h, cooling to room temperature after the reaction is finished, mixing with 10 times of volume of deionized water, carrying out vacuum filtration, washing a filter cake with the deionized water, and carrying out vacuum drying at 40 ℃ to constant weight after the washing is finished to obtain the modified microcrystalline cellulose.
Wherein the dosage ratio of the chlorinated trimellitic anhydride to the pyridine to the tetrahydrofuran to the microcrystalline cellulose in the step S21 is 12 g: 4.5 g: 300 mL: 5g of the total weight of the mixture; in the step S22, the dosage ratio of the intermediate 1, the glacial acetic acid and the ethylenediamine is 12 g: 300 mL: 3g of the total weight.
Example 3
Preparing an additive:
step S11, mixing graphene oxide, dopamine hydrochloride and Tris-HCl buffer solution, then performing ultrasonic dispersion for 10min at the temperature of 0 ℃, then performing stirring reaction for 24h at the temperature of 60 ℃, performing suction filtration under reduced pressure after the reaction is finished, and washing a filter cake with deionized water until a washing solution is colorless to obtain a solid a;
step S12, mixing modified microcrystalline cellulose and deionized water to prepare a suspension, adding an aqueous solution of sodium bromide and tetramethylpiperidine oxynitride while stirring, adjusting the pH value to 10 by using 0.5mol/L sodium hydroxide, adding a sodium hypochlorite solution, stirring and reacting for 4 hours at the temperature of 20 ℃, adding absolute ethyl alcohol after the reaction is finished, performing centrifugal treatment to remove a supernatant, and washing by using distilled water until a washing solution is neutral to obtain a solid b;
and step S13, mixing the solid a, the solid b and deionized water, and stirring for 3 hours to obtain the additive.
Wherein, in the step S11, the concentration of the Tris-HCl buffer solution is 10mmol/L, the pH value is 8.5, and the dosage ratio of the graphene oxide, the dopamine hydrochloride and the Tris-HCl buffer solution is 2 mg: 1 mg: 4 mL; in step S12, the aqueous solution of tetramethylpiperidine nitroxide is tetramethylpiperidine nitroxide and deionized water in an amount of 3 mg: 8mL of the mixture is mixed; the mass fraction of the sodium hypochlorite solution is 15 percent; the dosage ratio of the modified microcrystalline cellulose to the deionized water to the aqueous solution of sodium bromide, tetramethylpiperidine oxynitride to the sodium hypochlorite solution is 0.5 g: 50mL of: 0.16 g: 50mL of: 2.48 g; the using ratio of the solid a to the solid b to the deionized water in the step S13 is 1 g: 2 g: 100 mL; modified microcrystalline cellulose as obtained in example 2.
Example 4
Preparing a dispersion carrier:
mixing diethylene glycol monomethyl ether, tributyl phosphate and ethyl cellulose at 70 ℃, then adding an additive, polyamide wax and 1, 4-butyrolactone, and uniformly stirring to obtain a dispersion carrier, wherein the mass ratio of the diethylene glycol monomethyl ether, the tributyl phosphate, the ethyl cellulose, the additive, the polyamide wax and the 1, 4-butyrolactone is 42: 20: 10: 5: 1.5: 1, additive was prepared as in example 3.
Example 5
Preparing a dispersion carrier:
mixing diethylene glycol monomethyl ether, tributyl phosphate and ethyl cellulose at 70 ℃, then adding an additive, polyamide wax and 1, 4-butyrolactone, and uniformly stirring to obtain a dispersion carrier, wherein the mass ratio of the diethylene glycol monomethyl ether, the tributyl phosphate, the ethyl cellulose, the additive, the polyamide wax and the 1, 4-butyrolactone is 42: 20: 15: 5: 1.5: 1, additive was prepared as in example 3.
Example 6
A preparation method of nano rare earth thick film electronic paste comprises the following steps:
firstly, weighing the following raw materials in parts by weight: 10 parts of a dispersion carrier, 10 parts of a binding material, 1 part of rare earth oxide, 2 parts of ruthenium dioxide and 70 parts of silver powder;
and secondly, mixing the binder, the dispersing carrier, the rare earth oxide, ruthenium dioxide and the silver powder, placing the mixture into a grinding machine for grinding, and sieving the ground mixture through a 800-mesh sieve to obtain the nano rare earth thick film electronic paste.
Wherein the binder is prepared by the following steps:
calcium oxide, bismuth trioxide, silicon dioxide, zinc oxide, silver oxide and aluminum oxide in a mass ratio of 4: 4: 2: 3: 1: 1, mixing and grinding, then smelting at 1100 ℃ for 2h, and sieving through a 1000-mesh sieve after water quenching to obtain the binder.
Wherein, the rare earth oxide is lanthanum oxide; the dispersion vehicle was prepared as in example 5.
Example 7
A preparation method of nano rare earth thick film electronic paste comprises the following steps:
firstly, weighing the following raw materials in parts by weight: 15 parts of a dispersion carrier, 15 parts of a binding material, 4 parts of rare earth oxide, 4 parts of ruthenium dioxide and 75 parts of silver powder;
and secondly, mixing the binder, the dispersing carrier, the rare earth oxide, ruthenium dioxide and the silver powder, placing the mixture into a grinding machine for grinding, and sieving the ground mixture through a 800-mesh sieve to obtain the nano rare earth thick film electronic paste.
Wherein the binder is prepared by the following steps:
calcium oxide, bismuth trioxide, silicon dioxide, zinc oxide, silver oxide and aluminum oxide in a mass ratio of 4: 4: 2: 3: 1: 1, mixing and grinding, then smelting at 1100 ℃ for 2h, and sieving through a 1000-mesh sieve after water quenching to obtain the binder.
Wherein, the rare earth oxide is the mixture of lanthanum oxide and yttrium oxide by mass; the dispersion vehicle was prepared as in example 5.
Example 8
A preparation method of nano rare earth thick film electronic paste comprises the following steps:
firstly, weighing the following raw materials in parts by weight: 20 parts of a dispersion carrier, 20 parts of a binder, 5 parts of rare earth oxide, 5 parts of ruthenium dioxide and 80 parts of silver powder;
and secondly, mixing the binder, the dispersing carrier, the rare earth oxide, ruthenium dioxide and the silver powder, placing the mixture into a grinding machine for grinding, and sieving the ground mixture through a 800-mesh sieve to obtain the nano rare earth thick film electronic paste.
Wherein the binder is prepared by the following steps:
calcium oxide, bismuth trioxide, silicon dioxide, zinc oxide, silver oxide and aluminum oxide in a mass ratio of 4: 4: 2: 3: 1: 1, mixing and grinding, then smelting at 1100 ℃ for 2h, and sieving through a 1000-mesh sieve after water quenching to obtain the binder.
Wherein the rare earth oxide is yttrium oxide; the dispersion vehicle was prepared as in example 5.
Comparative example 1
The modified microcrystalline cellulose in example 3 was changed to unmodified microcrystalline cellulose, and the remaining raw materials and preparation process were kept unchanged.
Comparative example 2
The additive in the dispersion vehicle of example 5 was changed to the sample prepared in comparative example 1, and the remaining raw materials and preparation process were maintained.
Comparative example 3
The additives of example 5 were removed and the remaining raw materials and preparation process remained the same.
Comparative example 4
The dispersion carrier of example 7 was replaced with the sample prepared in comparative example 2, and the remaining raw materials and preparation process were maintained.
Comparative example 5
The dispersion carrier of example 7 was replaced with the sample prepared in comparative example 3, and the remaining raw materials and preparation process were maintained.
The slurries prepared in examples 6 to 8 and comparative examples 4 to 5 were tested at a sintering temperature of 750 c, where; removing bubbles from the sample, preparing a square thick film sample with the thickness of 18mm multiplied by 18mm by a manual screen printing process, placing for 30min, drying in an infrared oven for 30min, and then placing the thick film sample in a box-type resistance furnace with the heating rate of 5 ℃/min; and (4) carrying out a high-temperature sintering experiment, keeping the temperature for 10min, and then cooling to room temperature along with the furnace to obtain a thick film sample. Testing the square resistance of the thick film sample at different sintering temperatures by using a four-probe tester;
and (3) carrying out a rapid oxidation experiment by using 1% hydrogen sulfide gas, and analyzing and observing the change of the photoelectrochemical property of the thick film sample before and after vulcanization.
The test results are shown in table 1 below:
TABLE 1
| Item | Practice ofExample 6 | Example 7 | Example 8 | Comparative example 4 | Comparative example 5 |
| Square resistance (m omega/□) | 8 | 8 | 8 | 20 | 30 |
| Standing for 15min | Does not change color | Does not change color | Does not change color | Does not change color | Does not change color |
| After standing for 10h | Darkening of color | Darkening of color | Darkening of color | Blackening | Blackening |
From the above table 1, it can be seen that the electronic paste prepared by the invention has lower sheet resistance and good antioxidant effect.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. The nanometer rare earth thick film electronic paste comprises the following raw materials in parts by weight: 10-20 parts of a dispersing carrier, 10-20 parts of a binder, 1-5 parts of rare earth oxide, 2-5 parts of ruthenium dioxide and 70-80 parts of silver powder; characterized in that the dispersion carrier is prepared by the following steps:
mixing diethylene glycol monomethyl ether, tributyl phosphate and ethyl cellulose at 70 ℃, then adding the additive, the polyamide wax and the 1, 4-butyrolactone, and uniformly stirring to obtain the dispersion carrier.
2. The nano rare earth thick film electronic paste as claimed in claim 1, wherein the mass ratio of diethylene glycol monomethyl ether, tributyl phosphate, ethyl cellulose, additive, polyamide wax and 1, 4-butyrolactone is 42: 20: 10-15: 5: 1.5: 1.
3. the nano rare earth thick film electronic paste of claim 1, wherein the additive is prepared by the steps of:
step S11, mixing graphene oxide, dopamine hydrochloride and Tris-HCl buffer solution, then performing ultrasonic dispersion for 10min at the temperature of 0 ℃, then performing stirring reaction for 24h at the temperature of 60 ℃, and performing post-treatment to obtain a solid a;
step S12, mixing the modified microcrystalline cellulose and deionized water to prepare a suspension, adding an aqueous solution of sodium bromide and tetramethylpiperidine oxynitride while stirring, adjusting the pH value to 10 by using 0.5mol/L sodium hydroxide, adding a sodium hypochlorite solution, stirring and reacting for 4 hours at the temperature of 20 ℃, and performing aftertreatment to obtain a solid b;
and step S13, mixing the solid a, the solid b and deionized water, and stirring for 3 hours to obtain the additive.
4. The nano rare earth thick film electronic paste as claimed in claim 3, wherein the modified microcrystalline cellulose is prepared by the steps of:
step S21, mixing chlorinated trimellitic anhydride, pyridine and tetrahydrofuran, then adding microcrystalline cellulose, and stirring to react for 11-12 h at 20 ℃ to obtain an intermediate 1;
and step S22, mixing the intermediate 1 with glacial acetic acid, adding ethylenediamine at 0 ℃, stirring at room temperature for 50-60 min after the ethylenediamine is added, and then heating to 120 ℃ to react for 5-8 h to obtain the modified microcrystalline cellulose.
5. The nano rare earth thick film electronic paste as claimed in claim 1, wherein the binder is prepared by the steps of:
calcium oxide, bismuth trioxide, silicon dioxide, zinc oxide, silver oxide and aluminum oxide in a mass ratio of 4: 4: 2: 3: 1: 1, mixing and grinding, then smelting at 1100 ℃ for 2h, and sieving through a 1000-mesh sieve after water quenching to obtain the binder.
6. The nano rare earth thick film electronic paste as claimed in claim 1, wherein the silver powder has a particle size value of 200nm to 800 nm.
7. The nano rare earth thick film electronic paste as claimed in claim 1, wherein the rare earth oxide is one or two of lanthanum oxide or yttrium oxide mixed in any proportion.
8. The method for preparing nano rare earth thick film electronic paste according to claim 1, comprising the steps of:
firstly, weighing raw materials in parts by weight;
and secondly, mixing the binder, the dispersing carrier, the rare earth oxide, ruthenium dioxide and the silver powder, placing the mixture into a grinding machine for grinding, and sieving the ground mixture through a 800-mesh sieve to obtain the nano rare earth thick film electronic paste.
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Application publication date: 20210907 |