CN113275584A - Micro-nano silver powder and preparation method and application thereof - Google Patents
Micro-nano silver powder and preparation method and application thereof Download PDFInfo
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- CN113275584A CN113275584A CN202110549513.8A CN202110549513A CN113275584A CN 113275584 A CN113275584 A CN 113275584A CN 202110549513 A CN202110549513 A CN 202110549513A CN 113275584 A CN113275584 A CN 113275584A
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- micro
- silver powder
- nano silver
- preparation
- prepared
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- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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Abstract
The invention provides micro-nano silver powder and a preparation method and application thereof, wherein the preparation method of the micro-nano silver powder comprises the following steps: dissolving a peptoid compound in a solvent, adding a silver salt and a reducing agent, reacting, and filtering to obtain micro-nano silver powder; the peptoid compound is a beta-hydroxybutyryl-amino acid compound. According to the preparation method of the micro-nano silver powder, the peptoid compounds are used as the dispersing agents, so that the micro-nano silver powder can be prepared, the appearance, the granularity and the structure of the micro-nano silver powder can be adjusted by adopting the peptoid compounds with different chemical structures, and the structure and the appearance of the micro-nano silver powder can be controlled. The micro-nano silver powder prepared by the method has good dispersibility, smaller specific surface area and resistivity than those of a commercially available sample, and good performance.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to micro-nano silver powder and a preparation method and application thereof.
Background
The nano and micron metal silver powder material is widely applied in the fields of electronic ceramics, solar photovoltaic power generation, sterilization, disinfection, electronic flexible printing and the like. The morphology and structure of the micro-nano silver powder prepared by the existing method cannot be well controlled, and the structure and morphology of the silver powder are directly related to the quality and performance of the prepared silver powder. Therefore, a preparation method capable of better controlling the structure and morphology of the micro-nano silver powder is needed.
Disclosure of Invention
In view of the above, the invention provides micro-nano silver powder and a preparation method thereof, so as to solve or partially solve the technical problems in the prior art.
In a first aspect, the invention provides a preparation method of micro-nano silver powder, which comprises the following steps:
dissolving a peptoid compound in a solvent, adding a silver salt and a reducing agent, reacting, and filtering to obtain micro-nano silver powder;
wherein the peptoid compound is a beta-hydroxybutyryl-amino acid compound, and the structural formula of the beta-hydroxybutyryl-amino acid is as follows:
Preferably, in the method for preparing the micro-nano silver powder, the silver salt comprises at least one of silver nitrate, silver sulfate and silver halide.
Preferably, in the preparation method of the micro-nano silver powder, the solvent comprises one of water, methanol, ethanol, glycol, glycerol and acetone.
Preferably, in the preparation method of the micro-nano silver powder, the reducing agent comprises at least one of glucose, formaldehyde, formic acid, ethylene glycol, sodium borohydride and ascorbic acid.
Preferably, the preparation method of the micro-nano silver powder comprises the steps of dissolving a peptoid compound in a solvent, adding a silver salt and a reducing agent, reacting, and filtering to obtain the micro-nano silver powder, wherein the reaction temperature is 80-220 ℃, and the reaction time is 180-720 min.
Preferably, in the preparation method of the micro-nano silver powder, the mass-to-volume ratio of the peptoid compound, the silver salt, the reducing agent and the solvent is (0.5-10) g: (0.5-15) g: (0.5-18) g: (30-80) ml.
In a second aspect, the invention also provides micro-nano silver powder prepared by the preparation method.
In a third aspect, the invention also provides application of the micro-nano silver powder in preparation of conductive silver paste, electronic ceramics, sterilization disinfectors and solar photovoltaic power generation devices.
Compared with the prior art, the micro-nano silver powder and the preparation method and application thereof have the following beneficial effects:
(1) according to the preparation method of the micro-nano silver powder, the peptoid compounds are used as the dispersing agents, so that the micro-nano silver powder can be prepared, the appearance, the granularity and the structure of the micro-nano silver powder can be adjusted by adopting the peptoid compounds with different chemical structures, and the structure and the appearance of the micro-nano silver powder can be controlled.
(2) The micro-nano silver powder prepared by the method has good dispersibility, smaller specific surface area and resistivity than those of a commercially available sample, and good performance; the conductive silver paste prepared from the micro-nano silver powder has better performance than the conductive silver paste prepared from the existing silver powder.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is a surface topography of the micro-nano silver powder prepared in embodiment 1 of the invention;
FIG. 2 is a surface topography of the micro-nano silver powder prepared in embodiment 2 of the invention;
FIG. 3 is a surface topography of the micro-nano silver powder prepared in embodiment 3 of the invention;
FIG. 4 is a surface topography of the micro-nano silver powder prepared in embodiment 4 of the invention;
FIG. 5 is a surface topography of the micro-nano silver powder prepared in embodiment 5 of the invention;
fig. 6 is a surface topography of the micro-nano silver powder prepared in embodiment 6 of the invention.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with 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 obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The embodiment of the application provides a preparation method of micro-nano silver powder, which comprises the following steps:
dissolving a peptoid compound in a solvent, adding a silver salt and a reducing agent, reacting, and filtering to obtain micro-nano silver powder;
wherein, the peptoid compound is a beta-hydroxybutyryl-amino acid compound, and the structural formula of the beta-hydroxybutyryl-amino acid is as follows:
It should be noted that, in the embodiment of the present application, the peptoid compound is used as a dispersant to implement preparation of the micro-nano silver powder, and specifically, the peptoid compound is a β -hydroxybutyryl-amino acid compound, and a structural formula of the peptoid compound is as follows:
the shape, granularity and structure of the micro-nano silver powder can be adjusted by adopting different (R) n groups, so that the structure and shape of the micro-nano silver powder can be controlled.
Specifically, in some embodiments, the α -amino acid can be alanine, arginine, aspartic acid, cysteine, glutamine, glutamic acid, histidine, isoleucine, glycine, asparagine, leucine, lysine, methionine, phenylalanine, proline, serine, threonine, tryptophan, tyrosine, valine, or the like, corresponding (R)nPolypeptide chain formed by the alpha-amino acid through polycondensation.
In particular, in some embodiments, the β -hydroxybutyryl-amino acid compound may be in particular:
the specific structure of the beta-hydroxybutyryl-amino acid compound and the synthesis method thereof all adopt the prior art, and the application does not improve the structure.
In some embodiments, the silver salt is a soluble or low-soluble silver salt, specifically, the silver salt comprises at least one of silver nitrate, silver sulfate, and silver halide.
In some embodiments, the solvent is water or an organic alcohol or ketone with a molecular weight of less than 300, and the specific solvent may be one of methanol, ethanol, ethylene glycol, glycerol and acetone.
In some embodiments, the reducing agent comprises at least one of glucose, formaldehyde, formic acid, ethylene glycol, sodium borohydride, and ascorbic acid.
In some embodiments, the peptoid compound is dissolved in a solvent, silver salt and a reducing agent are added, after reaction, the micro-nano silver powder is obtained by filtering, wherein the reaction temperature is 80-220 ℃, and the reaction time is 180-720 min.
In some embodiments, the peptoid compound is dissolved in a solvent, silver salt and a reducing agent are added, after reaction, filtration is carried out, then the filtrate is cleaned by ethanol and deionized water, organic matters and impurity salts on the surface of the filtrate are removed, and the micro-nano silver powder is obtained
In some embodiments, the mass to volume ratio of the peptoid compound, the silver salt, the reducing agent, and the solvent is (0.5-10) g: (0.5-15) g: (0.5-18) g: (30-80) ml.
Based on the same inventive concept, the invention also provides micro-nano silver powder prepared by the preparation method.
Based on the same invention concept, the invention also provides application of the prepared micro-nano silver powder in preparation of conductive silver paste, electronic ceramics, sterilization disinfectors and solar photovoltaic power generation devices.
The following further describes a preparation method of the micro-nano silver powder according to the present application with specific examples.
Example 1
The embodiment of the application provides a preparation method of micro-nano silver powder, which comprises the following steps:
adding 1.8g of silver nitrate and 1.6g of peptoid compound into 60mL of ethanol, adding 2g of reducing agent ascorbic acid, and stirring for 30min to uniformly mix the solution to obtain a mixed solution; and (3) placing the prepared mixed solution in a crystallization kettle, heating to 120 ℃, keeping the temperature for 720 minutes at a constant temperature, filtering, and cleaning with ethanol and deionized water to obtain the micro-nano silver powder.
Wherein, the peptoid compound is beta-hydroxybutyryl-lysine pseudo dipeptide, and the structural formula is as follows:
s1, adding 0.01mol of tert-butyl dimethyl silyl ether beta-hydroxybutyric acid, 0.01mol of lysine ethyl ester hydrochloride and 0.001mol of 4-dimethylamino pyridine into 50ml of dichloromethane, stirring, then adding 0.024mol of triethylamine, and stirring to react for 20min to obtain a reaction solution;
s2, dissolving 0.015mol of N, N' -dicyclohexylcarbodiimide in 20mL of dichloromethane, then dripping the reaction solution into the dichloromethane, stirring the solution at room temperature for 3 hours after dripping is finished, carrying out suction filtration, washing the filtrate with 50mL of water twice, washing the filtrate with 20mL of 0.1M dilute hydrochloric acid twice, washing the filtrate with 20mL of saturated sodium bicarbonate aqueous solution once, washing the filtrate with 20mL of saturated sodium chloride aqueous solution once, drying the dichloromethane phase and then concentrating;
s3, dissolving the condensed concentrated solution with 50mL of tetrahydrofuran, adding 1 equivalent of tetrabutyl ammonium fluoride, stirring for 1h at room temperature, then adding water for quenching reaction, evaporating the tetrahydrofuran under reduced pressure, extracting the water phase with 30mL of dichloromethane for 3 times respectively, combining organic phases, washing with 30mL of saturated sodium chloride once, concentrating, adding 1 equivalent of 1M sodium hydroxide aqueous solution into the concentrated solution, keeping the pH value at 7-8, stirring for 1h, washing the reaction solution with 20mL of dichloromethane for three times, concentrating the water phase, recrystallizing with ethanol/acetone to obtain 1.5g of white solid, namely beta-hydroxybutyryl-lysine pseudo-dipeptide sodium salt, obtaining the yield of 62.5%, adding an equivalent of hydrogen chloride ethanol solution into the beta-hydroxybutyryl-lysine pseudo-dipeptide sodium salt, filtering and concentrating to obtain the beta-hydroxybutyryl-lysine pseudo dipeptide, as a white solid. Nuclear magnetic data for β -hydroxybutyryl-lysine pseudodipeptide: 1HNMR (400MHz, D)2O)δ4.02(m，1H)，3.62(m，1H)，3.02(m，2H)，2.27(m，2H)，1.61(m，2H)，1.30(m，2H)，1.25(m，2H)，1.13(m，3H)。
Example 2
The embodiment of the application provides a preparation method of micro-nano silver powder, which comprises the following steps:
adding 2.4g of silver nitrate and 2.8g of peptoid compound into 60mL of ethanol water solution, adding 2.8g of reducing agent glucose, and stirring for 50min to uniformly mix the solution to obtain a mixed solution; and (3) placing the prepared mixed solution in a crystallization kettle, heating to 160 ℃, keeping the temperature for 480 minutes at a constant temperature, filtering, and cleaning with ethanol and deionized water to obtain the micro-nano silver powder, wherein the volume ratio of the ethanol to the water in the ethanol aqueous solution is 1: 1.
Wherein, the peptoid compound is beta-hydroxybutyryl-glutamic acid pseudo dipeptide, and the structural formula is as follows:
example 3
The embodiment of the application provides a preparation method of micro-nano silver powder, which comprises the following steps:
adding 0.6g of silver sulfate and 1.8g of peptoid compound into 60mL of acetone aqueous solution, adding 1.2g of reducing agent ascorbic acid, and stirring for 100min to uniformly mix the solution to obtain a mixed solution; and (3) placing the prepared mixed solution in a crystallization kettle, heating to 200 ℃, keeping the temperature for 600 minutes at a constant temperature, filtering, and cleaning with ethanol and deionized water to obtain the micro-nano silver powder, wherein the volume ratio of acetone to water in the acetone aqueous solution is 1: 1.
Wherein, the peptoid compound is beta-hydroxybutyryl-glycine-methionine pseudo tripeptide, and the structural formula is as follows:
specifically, the preparation method of the β -hydroxybutyryl-glycine-methionine pseudo-tripeptide can be referred to in example 1The preparation method of beta-hydroxybutyryl-lysine pseudo dipeptide is specifically characterized by preparing tert-butyl dimethyl silyl ether beta-hydroxybutyric acid, glycine ethyl ester hydrochloride and methionine ethyl ester hydrochloride. The prepared beta-hydroxybutyryl-glycine-methionine pseudo-tripeptide nuclear magnetic spectrum data are as follows:1H NMR(400MHz，D2O)δ4.21(m，1H)，4.07(m，1H)，3.84(m，2H)，2.35(m，4H)，2.00(m，1H)，1.98(s，3H)，1.80(m，1H)，1.13(d，3H)。
example 4
The embodiment of the application provides a preparation method of micro-nano silver powder, which comprises the following steps:
adding 0.6g of silver chlorate and 1.8g of peptoid compound into 60mL of acetone aqueous solution, adding 2.0g of reducing agent formaldehyde solution, and stirring for 100min to uniformly mix the solution to obtain a mixed solution; and (3) placing the prepared mixed solution in a crystallization kettle, heating to 180 ℃, keeping the temperature for 600 minutes at a constant temperature, filtering, and cleaning with ethanol and deionized water to obtain the micro-nano silver powder, wherein the volume ratio of acetone to water in the acetone aqueous solution is 1: 1.
Wherein, the peptoid compound is beta-hydroxybutyryl-glycine-isoleucine pseudo tripeptide, and the structural formula is as follows:
example 5
The embodiment of the application provides a preparation method of micro-nano silver powder, which comprises the following steps:
adding 2.6g of silver nitrate and 1.8g of peptoid compound into 60mL of glycerol aqueous solution, adding 2.0g of reducing agent sodium borohydride, and stirring for 100min to uniformly mix the solution to obtain a mixed solution; and (3) placing the prepared mixed solution in a crystallization kettle, heating to 160 ℃, keeping the temperature for 480 minutes at a constant temperature, filtering, and cleaning with ethanol and deionized water to obtain the micro-nano silver powder, wherein the volume ratio of glycerol to water in the glycerol aqueous solution is 1: 1.
Wherein, the peptoid compound is beta-hydroxybutyryl-glycyl-alanyl-methionine pseudo tetrapeptide, and the structural formula is as follows:
example 6
The embodiment of the application provides a preparation method of micro-nano silver powder, which comprises the following steps:
adding 1.6g of silver nitrate and 0.8g of peptoid compound into 60mL of ethylene glycol aqueous solution, adding 2.4g of reducing agent formic acid, and stirring for 100min to uniformly mix the solution to obtain mixed solution; and (3) placing the prepared mixed solution in a crystallization kettle, heating to 150 ℃, keeping the temperature for 660 minutes, filtering, and cleaning with ethanol and deionized water to obtain the micro-nano silver powder, wherein the volume ratio of the ethylene glycol to the water in the ethylene glycol aqueous solution is 1: 1.
Wherein, the peptoid compound is beta-hydroxybutyryl-leucyl-valyl-glutamic acid pseudotetrapeptide, and the structural formula is as follows:
the results of testing the surface morphology of the micro-nano silver powder prepared in the above embodiments 1 to 6 are shown in fig. 1 to 6, respectively.
As can be seen from fig. 1 to 6, the micro-nano silver powder prepared in different embodiments is uniform in distribution and good in dispersibility, and the micro-nano silver powder prepared in different embodiments has different particle sizes and surface forms. Specifically, as can be seen from fig. 1, the micro-nano silver powder prepared in example 1 is granular, and the average particle size is 58-100 nm. As can be seen from FIG. 2, the micro-nano silver powder prepared in example 2 is flaky, and the average particle size is 2-5 μm. As can be seen from FIG. 3, the micro-nano silver powder prepared in example 3 is flaky, and the average particle size is 2-20 μm. As can be seen from FIG. 4, the micro-nano silver powder prepared in example 3 is granular, and the average particle size is between 0.3 and 0.7 μm. As can be seen from FIG. 5, the micro-nano silver powder prepared in example 5 is granular, and the average particle size is between 0.3 and 0.5 μm. As can be seen from FIG. 6, the micro-nano silver powder prepared in example 6 is granular, and the average particle size is between 90 nm and 220 nm.
The specific surface areas and the resistivities of the micro-nano silver powder prepared in the above examples 1 to 6 and the micro-nano silver powder sold in the market are tested, and the results are shown in the following table 1. Wherein, the specific surface area adopts a BET specific surface area test method, and the resistivity test method comprises the following steps: an ST2742B type automatic powder resistivity tester manufactured by Suzhou crystal lattice electronics Limited is adopted, and the listed data are resistivity data of a sample to be tested under 28-30 MPa.
TABLE 1 specific surface area and resistivity data for different samples
As can be seen from the above table 1, the specific surface area of the micro-nano silver powder prepared by the method is smaller than that of a commercially available sample with the same morphology, and the resistivity of the micro-nano silver powder is obviously smaller than that of the commercially available sample with the same morphology.
The micro-nano silver powder prepared in the embodiment 2 and a commercially available sample with the same shape as the embodiment 2 are further used for preparing the photovoltaic heterojunction conductive silver paste. The preparation method comprises the following steps: and (3) uniformly mixing the organic system, adding the micro-nano silver powder or the commercially available sample prepared in the embodiment 2, uniformly mixing the micro-nano silver powder or the commercially available sample through a planetary gravity mixer, and finally mixing the micro-nano silver powder or the commercially available sample through a three-roll machine to obtain the photovoltaic heterojunction conductive silver paste. Wherein the organic system comprises: the adhesive comprises an adhesive phase, a solvent and an auxiliary agent, wherein the adhesive phase comprises a mixture of bisphenol A epoxy resin and bisphenol F epoxy resin, the solvent is a DBE dibasic acid ester mixture, and the auxiliary agent comprises a mixture of a defoaming agent, a thixotropic agent, a lubricant and a curing agent.
The conductive silver paste prepared by the method has the viscosity of 28-30 ten thousand cps tested by a Bohler flying viscometer.
156 × 156 heterojunction battery pieces are selected, the micro-nano silver powder in the embodiment 2 and the conductive silver paste prepared by the method according to the embodiment 2 are used for preparing the battery pieces through the processes of screen printing, curing, light injection and the like, the open circuit voltage Uoc, the short circuit current Isc, the filling factor FF, the conversion efficiency Eta and the resistance value Rser are tested, and the results are shown in the following table 2.
Table 2-properties of the cell sheets prepared from different conductive silver pastes
| Battery piece | Uoc(V) | Isc(A) | FF(％) | Eta(％) | Rser(Ohm) |
| Battery piece 1 | 0.7494 | 9.3435 | 84.02 | 24.023 | 0.0025 |
| Battery piece 2 | 0.7494 | 9.3459 | 83.24 | 23.676 | 0.0033 |
In table 2, the cell piece 1 is a cell piece prepared from the low-temperature conductive silver paste prepared from the micro-nano silver powder in the above example 2, and the cell piece 1 is a cell piece prepared from the low-temperature conductive silver paste prepared from a commercially available sample with the same shape and appearance as those in the example 2. It can be seen from table 2 that the battery piece 1 has better performance, and thus, the conductive silver paste prepared from the micro-nano silver powder prepared in the application has better performance than the conductive silver paste prepared from silver powder on the market at home.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A preparation method of micro-nano silver powder is characterized by comprising the following steps:
dissolving a peptoid compound in a solvent, adding a silver salt and a reducing agent, reacting, and filtering to obtain micro-nano silver powder; wherein the peptoid compound is a beta-hydroxybutyryl-amino acid compound, and the structural formula of the beta-hydroxybutyryl-amino acid is as follows:
2. The method for preparing micro-nano silver powder according to claim 1, wherein the silver salt comprises at least one of silver nitrate, silver sulfate and silver halide.
3. The method for preparing micro-nano silver powder according to claim 1, wherein the solvent comprises one of water, methanol, ethanol, ethylene glycol, glycerol and acetone.
4. The method for preparing micro-nano silver powder according to claim 1, wherein the reducing agent comprises at least one of glucose, formaldehyde, formic acid, ethylene glycol, sodium borohydride and ascorbic acid.
5. The method for preparing micro-nano silver powder according to claim 1, wherein the micro-nano silver powder is obtained by dissolving a peptoid compound in a solvent, adding a silver salt and a reducing agent, reacting, and filtering, wherein the reaction temperature is 80-220 ℃ and the reaction time is 180-720 min.
6. The method for preparing micro-nano silver powder according to claim 1, wherein the mass-to-volume ratio of the peptoid compound, the silver salt, the reducing agent and the solvent is (0.5-10) g, (0.5-15) g, (0.5-18) g, (30-80) ml.
7. The micro-nano silver powder is characterized by being prepared by the preparation method according to any one of claims 1 to 6.
8. The application of the micro-nano silver powder of claim 7 in preparing conductive silver paste, electronic ceramics, bactericidal disinfectant and solar photovoltaic power generation devices.
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