CN114918424A - Method and device for efficiently preparing low-temperature nano silver paste from silver formate - Google Patents
Method and device for efficiently preparing low-temperature nano silver paste from silver formate Download PDFInfo
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Abstract
The invention provides a method and a device for efficiently preparing low-temperature nano silver paste by using silver formate, wherein the silver formate is used as a precursor to prepare the nano silver paste, so that the silver content in the reaction can be greatly increased, the reaction efficiency is improved, and the problem of low silver content in the preparation of nano silver is solved; the prepared nano silver paste can be sintered at a low temperature of 100-200 ℃, so that the application range of the silver paste is expanded; the reaction does not need washing, so that the washing process is omitted, and the discharge of waste liquid is reduced; meanwhile, the alkylamine and the diluting solvent with low boiling point can be recovered, and the reaction is efficient, clean and environment-friendly.
Description
Technical Field
The invention relates to the technical field of nano silver, and mainly relates to a method and a device for efficiently preparing low-temperature nano silver paste by using silver formate.
Background
In recent years, with the rapid development of electronic equipment technology, higher requirements are put on equipment of various electronic devices. Silver powder and electronic paste thereof are noble metal powder which is most widely applied and used in the electronic industry, and are key functional materials for producing various electronic devices. The dispersion of the silver powder in the slurry used in practice is particularly important, and particularly when the granularity of the silver reaches the nanometer level, the nano silver can show better and higher adaptability to electronic devices due to the quantum size effect, small size effect and surface effect of the silver.
Generally, the preparation of nano silver adopts a chemical reduction method, which is to wrap silver ions with a dispersant in a solvent system or an aqueous solution and reduce the silver ions into a nano silver simple substance wrapped with the dispersant by using a reducing agent. However, the method has an obvious problem that organic high molecular polymers or organic macromolecules are used as dispersing agents, such as polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), sodium hexadecyl sulfonate (CTAB) and the like, the organic high molecular polymers or the organic macromolecules have high melting points and poor solubility, and are difficult to completely remove in the subsequent cleaning step, once residues occur, the nucleation process of the nano silver is directly influenced, the uniformity of silver product particles is poor, the problem of carbon residue during actual use and sintering of the nano silver is caused, and the conductivity of the silver product is reduced.
Patent No. cn20141005876.x, a method for surface modification of silver nanoparticles by using mercaptan, a mercapto-containing silane coupling agent, a cationic surfactant, a corrosion inhibitor and a diluting solvent as raw materials, so that the silver nanoparticles are not easy to agglomerate, can be compounded and dissolved with other materials, and broadens the application field. However, the method is simple and easy to implement and has no pollution, but the production and the post-treatment are separated, so that the nano silver product with uniform dispersion cannot be directly prepared, and meanwhile, the types of the raw materials required to be added are quite various, so that the method is not suitable for large-scale actual production.
Patent CNCN201510614853.9, a low-temperature nano silver paste and a preparation process thereof, discloses a preparation method, 1) preparing blank reversed-phase microemulsion and making a pseudo-ternary phase diagram; 2) preparing reverse microemulsion containing nano silver particles; 3) centrifugal separation: carrying out centrifugal separation for 2-4 times on the reverse microemulsion containing the nano-silver particles, and separating out an oil-phase organic matter and a water-phase solution to obtain nano-silver particles adsorbed by the compound surfactant; 4) mixing the nano silver particles adsorbed by the compound surfactant obtained in the step 3) with an organic carrier, and adjusting the viscosity to obtain the low-temperature nano silver paste. Although the method can control the particle size of the nano silver, the method has a large amount of surfactants and complicated post-treatment, has high requirements on production equipment, and has more than three impurity types to be separated.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a method and a device for efficiently preparing low-temperature nano silver paste by using silver formate, in particular to a method and a device for preparing nano silver paste by complexing the silver formate with a mixture of alkylamine and a diluting solvent, performing self-decomposition after heating to prepare a large amount of nano silver paste, sintering at a low temperature of 100-200 ℃, and effectively recovering and reacting the alkylamine and the diluting solvent with low boiling points.
The object of the present invention is achieved by the following technical means. A method for efficiently preparing low-temperature nano silver paste by silver formate comprises the following steps:
(1) preparing silver formate from silver nitrate and formate at a certain temperature, and performing centrifugal vacuum drying to obtain anhydrous silver formate;
(2) adding alkylamine and a diluting solvent into anhydrous silver formate, and carrying out stirring and complexing reaction at a certain temperature to obtain a complex;
(3) heating and stirring the complex at a certain temperature to decompose the complex, and then further heating the complex in a fractionating tower in vacuum to volatilize and recover and treat a diluting solvent, low-boiling alkylamine and water to finally obtain a nano-silver mixture with the particle size of 5-50 nm;
(4) and adding a silver paste auxiliary agent into the nano silver mixture to prepare the nano silver paste, wherein the silver paste can be sintered at 100-200 ℃.
Further, in the step (1), the formate is one or a mixture of several of compounds containing formate, such as potassium formate, sodium formate, calcium formate, and the like.
Further, the reaction temperature and the vacuum drying temperature in the step (1) are-5 to 50 ℃.
Further, the water content of the anhydrous silver formate in the step (1) is less than 1%.
Further, in the step (2), the alkylamine mixture is at least one of ethylenediamine, n-propylamine, di-n-propylamine, cyclopropylamine, n-butylamine, tert-butylamine, n-hexylamine, isohexylamine, n-octylamine, cyclooctylamine, isooctylamine, dodecylamine, tetradecylamine, n-hexadecylamine, oleylamine, and the like, wherein the number of carbons of the alkylamine mixture is less than 18, and the alkylamine mixture is a mixture of two or more of polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), and sodium hexadecylsulfonate (CTAB), wherein the alkylamine mixture having a boiling point of 100 ℃ or less is a low-boiling point alkylamine, and the rest is a high-boiling point alkylamine, and the alkylamine mixture at least comprises one low-boiling point alkylamine and one high-boiling point alkylamine.
Further, in the step (2), the diluting solvent is one or a mixture of several of alkanes, alkenes, aldehydes, esters, aromatic hydrocarbons, halogenated hydrocarbons and the like, and the diluting solvent can be replaced by low-boiling point alkylamine.
Further, the complexing temperature in the step (2) is-5-50 ℃.
Further, the heating temperature and the vacuum heating temperature in the step (3) are 50-100 ℃.
Further, the content of the nano-silver in the nano-silver mixture in the step (3) is 50-95%.
Further, the silver paste auxiliary agent in the step (4) is one or a mixture of several of phenolic resin, epoxy resin, polyester resin, cellulose, nitrocellulose, alkyl alcohols, alkanes, hydroxyaldehydes, organic silicon compounds, fluorine compounds, esters, ketones, glass powder and the like.
Further, the content of nano silver in the silver paste in the step (4) is 40-90%.
The invention also discloses a device for efficiently preparing the low-temperature nano silver paste by using the silver formate, which comprises a centrifugal drier, a heating stirrer and a fractionating tower, wherein the centrifugal drier is provided with an inlet A and an inlet B, the inlet A is used for inputting silver nitrate, and the inlet B is used for inputting formate; an outlet of the centrifugal dryer is connected with an inlet C of the heating stirrer through a pipeline, an outlet A of the heating stirrer is connected with the fractionating tower, an outlet B, an outlet C, an outlet D and an outlet E are arranged on the fractionating tower, wherein the outlet B is used for outputting low-boiling alkylamine, the outlet C is used for outputting a diluting solvent, the outlet D is used for outputting a nano-silver mixture, and the outlet E is used for outputting water vapor; the outlet B and the outlet C are communicated with the inlet C of the heating stirrer through a circulating pipeline.
Furthermore, the heating stirrer comprises a shell, a reaction cavity and a heater are arranged in the shell, a stirring motor is arranged at the top of the shell, the stirring motor is connected with a stirring paddle and extends to the bottom of the reaction cavity, and the heater is arranged below the reaction cavity; an inlet C is arranged above the reaction cavity, and an outlet A is arranged on the side surface of the reaction cavity close to the bottom.
The invention takes the silver formate as the precursor to prepare the low-temperature nano silver paste, and has the following advantages:
1. the reaction can recover alkylamine and diluting auxiliary agent, and can avoid washing nano silver, thereby greatly reducing reaction waste liquid, reducing post-treatment process, and having environment-friendly and clean reaction;
2. the silver formate can effectively improve the silver content in the reaction and greatly improve the reaction efficiency.
3. The prepared nano silver paste can be sintered at a low temperature of 100-200 ℃, the application range of the silver paste can be greatly changed by changing the sintering temperature, and the industrial prospect is expanded.
4. The reaction process does not need high temperature and high pressure conditions, reduces the reaction energy consumption, and does not need special production equipment.
Drawings
Fig. 1 is an SEM image of the silver paste prepared in example 1;
fig. 2 is an SEM image of the silver paste prepared in example 2;
fig. 3 is an SEM image of the silver paste prepared in example 3;
fig. 4 is an SEM image of the silver paste prepared in example 4;
fig. 5 is an SEM image of a silver paste prepared in a comparative example;
FIG. 6 is a schematic flow chart;
FIG. 7 is a schematic view of the apparatus of the present invention.
Description of reference numerals: an inlet A1, an inlet B2, a centrifugal dryer 3, an inlet C4, a stirring paddle 5, a heater 6, a stirring motor 7, a reaction chamber 8, a shell 9, a fractionating tower 10, an outlet A11, an outlet B12, an outlet C13, an outlet D14 and an outlet E15.
Detailed Description
The invention will be described in detail below with reference to the following figures and examples:
the invention provides a method and a device for efficiently preparing low-temperature nano silver paste by silver formate, the prepared nano silver paste has controllable particle size and stable batch, can be sintered at a low temperature of 100-200 ℃, does not need washing, and solves the problems of low content of reaction silver, harsh reaction conditions, uneven particle size after reaction, agglomeration and caking during silver separation, more post-treatment flows and the like; meanwhile, the alkylamine with low boiling point and the diluting solvent can be recovered after the reaction, and the reaction is efficient, clean and environment-friendly.
AgNO 3 +HCOO-R→AgOOCH+R-NO 3
AgOOCH+R-NH 2 →R-NH 2 ·AgOOCH
The invention provides a method for efficiently preparing low-temperature nano silver paste from silver formate, which comprises the following steps as shown in figure 6:
(1) preparing silver formate from silver nitrate and formate at a certain temperature, and performing centrifugal vacuum drying to obtain anhydrous silver formate; the reaction temperature and the vacuum drying temperature are-5-50 ℃, and the water content of the anhydrous silver formate is less than 1%.
(2) Adding alkylamine and a diluting solvent into anhydrous silver formate, and carrying out stirring complexation reaction at a complexation temperature of-5-50 ℃ to obtain a complex;
(3) heating and stirring the complex at a certain temperature to decompose the complex, and then further heating the complex in a fractionating tower in vacuum to volatilize the diluting solvent, the low-boiling point alkylamine and the water, and recovering and treating the volatile solvent, so as to obtain a nano-silver mixture with the particle size of 5-50 nm; wherein the heating temperature and the vacuum heating temperature are 50-100 ℃, and the nano silver content in the nano silver mixture is 50-95%.
(4) And adding a silver paste auxiliary agent into the nano-silver mixture to prepare the nano-silver paste, wherein the silver paste can be sintered at 100-200 ℃, and the content of the nano-silver in the silver paste is 40-90%.
As shown in fig. 7, the invention also provides a device for efficiently preparing low-temperature nano silver paste from silver formate, which comprises a centrifugal dryer 3, a heating stirrer and a fractionating tower 10, wherein the centrifugal dryer 3 is provided with an inlet a1 and an inlet B2, the inlet a1 is used for inputting silver nitrate, and the inlet B2 is used for inputting formate; an outlet of the centrifugal dryer 3 is connected with an inlet C4 of the heating stirrer through a pipeline, an outlet A11 of the heating stirrer is connected with a fractionating tower 10, the fractionating tower 10 is provided with an outlet B12, an outlet C13, an outlet D14 and an outlet E15, wherein the outlet B12 is used for outputting low-boiling point alkylamine, the outlet C13 is used for outputting a diluting solvent, the outlet D14 is used for outputting a nano-silver mixture, and the outlet E15 is used for outputting water vapor; the outlet B12 and the outlet C13 are in communication with the inlet C4 of the heating agitator via a recycle line.
The heating stirrer comprises a shell 9, a reaction cavity 8 and a heater 6 are arranged in the shell 9, a stirring motor 7 is arranged at the top of the shell 9, the stirring motor 7 is connected with a stirring paddle 5 and extends to the bottom of the reaction cavity 8, and the heater 6 is arranged below the reaction cavity 8; an inlet C4 is arranged above the reaction chamber 8, and an outlet A11 is arranged on the side surface of the reaction chamber 8 close to the bottom.
Example 1
1. Silver nitrate and potassium formate react in 100g of water solvent at 5 ℃ according to the formula, and the temperature is kept for centrifugation and vacuum drying to prepare the anhydrous silver formate.
2. According to the formula, alkylamine (diluting solvent) is added into anhydrous silver formate, and complexation is carried out for 3h at 5 ℃ and 300RPM, so as to obtain the complex.
3. And (3) decomposing the complex obtained in the step (2) at 60 ℃ and 300RPM, further heating at 100 ℃ in vacuum after no bubbles appear, and volatilizing, recovering and treating the alkylamine (diluting auxiliary agent) with low boiling point and water to obtain the nano-silver mixture.
4. And (4) adding the nano silver mixture obtained in the step (3) into epoxy resin, a solvent, an additive and the like to prepare nano silver paste, and sintering at 150 ℃ for 20min to obtain silver sheets.
5. Performance test
The performance tests of the nano silver paste and the sintered silver sheet mainly comprise SEM, laser particle size analyzer, yield and the like, and the data results are shown in Table 1.
Example 2
1. Same procedure as in example 12 Performance test
Example 3
1. The procedure was the same as in example 1.
2. Performance test
Example 4
1. The procedure was the same as in example 1.
2. Performance testing
Comparative example
Weighing 85 g of silver nitrate to prepare 1L of solution, adding 85 g of complexing agent citric acid to prepare a raw material solution, putting the solution and 2.55 g of PVP prepared solution into a nano reaction kettle with the vacuum degree of 0.2-0.3 kp, simultaneously dropwise adding 50% hydrazine hydrate solution in a constant flow manner into the nano reaction kettle, carrying out high shear dispersion and ultrasonic emulsification reaction for 2-3 hours, ageing to separate nano particles from water, and removing supernatant. After aging, the mixture is washed 2 times with pure water and 2 times with absolute alcohol in a filter, and oleic acid is added as a passivating agent (the amount of the oleic acid is 5 percent of the volume of the absolute alcohol). And then carrying out low-temperature vacuum drying in a filter, controlling the temperature at 40 ℃, and adding a silver paste auxiliary agent to prepare the nano silver paste.
TABLE 1
As can be seen from table 1 above, the silver pastes of examples 1 to 4 all have a particle size (nm) of about 20nm, a silver yield of more than 97%, a lower sintering temperature, a higher hardness, and a low resistance; the comparative example had a low silver yield, many impurities, and non-uniform silver particles throughout the particle size.
From the SEM pictures (as shown in FIGS. 1-5), it can be seen that the silver particles of examples 1-4 have uniform particle size, regular spherical shape and no agglomeration; the comparative example has more large-particle impurities, the whole particle size is different, and the blocky accumulation is also obvious.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (10)
1. A method for efficiently preparing low-temperature nano silver paste by silver formate is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing silver formate from silver nitrate and formate at a certain temperature, and performing centrifugal vacuum drying to obtain anhydrous silver formate;
(2) adding the alkylamine mixture and the diluting solvent into anhydrous silver formate, and carrying out stirring and complexing reaction at a certain temperature to obtain a complex;
(3) heating and stirring the complex at a certain temperature to decompose the complex, and then further heating the complex in a fractionating tower in vacuum to volatilize the diluting solvent, the alkylamine with low boiling point and the water, and recovering and treating the volatilized mixture to obtain a nano silver mixture with the silver particle size of 5-50 nm;
(4) and adding a silver paste auxiliary agent into the nano silver mixture to prepare nano silver paste, wherein the silver paste can be sintered at 100-200 ℃.
2. The method for efficiently preparing the low-temperature nano silver paste by using the silver formate according to claim 1, which is characterized by comprising the following steps of: in the step (1), the formate is one or a mixture of several of compounds containing formate, including potassium formate, sodium formate and calcium formate.
3. The method for efficiently preparing the low-temperature nano silver paste by using the silver formate according to claim 1 or 2, which is characterized by comprising the following steps of: in the step (1), the reaction temperature and the vacuum drying temperature are-5-50 ℃, and the water content of the anhydrous silver formate is less than 1%.
4. The method for efficiently preparing low-temperature nano silver paste from silver formate according to claim 1, characterized by comprising the following steps: in the step (2), the alkylamine mixture is a mixture of two or more of alkylamine, polyvinylpyrrolidone, polyvinyl alcohol and sodium hexadecyl sulfonate with carbon number less than 18, the alkylamine with carbon number less than 18 comprises ethylenediamine, n-propylamine, di-n-propylamine, cyclopropylamine, n-butylamine, tert-butylamine, n-hexylamine, isohexylamine, n-octylamine, cyclooctylamine, isooctylamine, dodecylamine, tetradecylamine, n-hexadecylamine and oleylamine, wherein the alkylamine mixture with boiling point less than or equal to 100 ℃ is low-boiling alkylamine, and the rest is high-boiling alkylamine, and the alkylamine mixture at least comprises one low-boiling alkylamine and one high-boiling alkylamine.
5. The method for efficiently preparing the low-temperature nano silver paste by using the silver formate according to claim 1 or 4, which is characterized by comprising the following steps of: in the step (2), the diluting solvent is one or a mixture of more of alkanes, alkenes, aldehydes, esters, aromatics and halogenated hydrocarbons.
6. The method for efficiently preparing the low-temperature nano silver paste by using the silver formate according to claim 1, which is characterized by comprising the following steps of: in the step (2), the complexing temperature is-5 to 50 ℃.
7. The method for efficiently preparing the low-temperature nano silver paste by using the silver formate according to claim 1, which is characterized by comprising the following steps of: in the step (3), the heating temperature and the vacuum heating temperature are 50-100 ℃, and the nano silver content in the nano silver mixture is 50-95%.
8. The method for efficiently preparing low-temperature nano silver paste from silver formate according to claim 1, characterized by comprising the following steps: in the step (4), the silver paste additive is one or a mixture of phenolic resin, epoxy resin, polyester resin, cellulose, nitrocellulose, alkyl alcohols, alkanes, hydroxyaldehydes, organic silicon compounds, fluorine compounds, esters, ketones and glass powder, and the content of nano silver in the silver paste is 40-90%.
9. The device for efficiently preparing the low-temperature nano silver paste by using the silver formate as claimed in claim 1 is characterized in that: the device comprises a centrifugal dryer (3), a heating stirrer and a fractionating tower (10), wherein the centrifugal dryer (3) is provided with an inlet A (1) and an inlet B (2), the inlet A (1) is used for inputting silver nitrate, and the inlet B (2) is used for inputting formate; an outlet of the centrifugal dryer (3) is connected with an inlet C (4) of the heating stirrer through a pipeline, an outlet A (11) of the heating stirrer is connected with a fractionating tower (10), an outlet B (12), an outlet C (13), an outlet D (14) and an outlet E (15) are arranged on the fractionating tower (10), wherein the outlet B (12) is used for outputting low-boiling alkylamine, the outlet C (13) is used for outputting a diluting solvent, the outlet D (14) is used for outputting a nano-silver mixture, and the outlet E (15) is used for outputting water vapor; the outlet B (12) and the outlet C (13) are connected to the inlet C (4) of the heating agitator via a circulation line.
10. The apparatus for efficiently preparing low-temperature nano silver paste from silver formate according to claim 9, wherein the apparatus comprises: the heating stirrer comprises a shell (9), a reaction cavity (8) and a heater (6) are arranged in the shell (9), a stirring motor (7) is arranged at the top of the shell (9), the stirring motor (7) is connected with a stirring paddle (5) and extends to the bottom of the reaction cavity (8), and the heater (6) is arranged below the reaction cavity (8); an inlet C (4) is arranged above the reaction cavity (8), and an outlet A (11) is arranged on the side surface of the reaction cavity (8) close to the bottom.
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| CN104540622A (en) * | 2012-08-07 | 2015-04-22 | 株式会社大赛璐 | Method for producing silver nano-particles and silver nano-particles |
| CN104540904A (en) * | 2012-08-07 | 2015-04-22 | 田中贵金属工业株式会社 | Silver particle ink, silver particle sintered body and method for manufacturing silver particle ink |
| CN105238135A (en) * | 2012-08-07 | 2016-01-13 | 田中贵金属工业株式会社 | Nano fine silver particle ink and fine silver particle sintered body |
| CN103059492A (en) * | 2012-12-31 | 2013-04-24 | 武汉理工大学 | Preparation method for silver (Ag)/polymethyl methacrylate (PMMA) nanocomposite material with high Ag content |
| JPWO2017094166A1 (en) * | 2015-12-03 | 2018-09-20 | ハリマ化成株式会社 | Method for producing conductive paste |
| CN217412454U (en) * | 2022-05-18 | 2022-09-13 | 浙江海钛新材料科技股份有限公司 | Device of high-efficient preparation low temperature nanometer silver thick liquid of silver formate |
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