CN113275584B - Micro-nano silver powder and preparation method and application thereof - Google Patents

Micro-nano silver powder and preparation method and application thereof Download PDF

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CN113275584B
CN113275584B CN202110549513.8A CN202110549513A CN113275584B CN 113275584 B CN113275584 B CN 113275584B CN 202110549513 A CN202110549513 A CN 202110549513A CN 113275584 B CN113275584 B CN 113275584B
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刘成
孙光辉
张建强
曾俊良
牛亮峰
梁玮
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Jiyuan Xinghan New Materials Technology Co.,Ltd.
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Abstract

The application 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 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 compound is used as the dispersing agent, so that the preparation of the micro-nano silver powder can be realized, and the morphology, granularity and structure of the micro-nano silver powder can be adjusted by adopting the peptoid compounds with different chemical structures, so that the structure and morphology of the micro-nano silver powder can be controlled. The micro-nano silver powder prepared by the application has good dispersibility, and has specific surface area and resistivity smaller than those of commercial samples, and good performance.

Description

Micro-nano silver powder and preparation method and application thereof
Technical Field
The application relates to the technical field of nano materials, in particular to micro-nano silver powder and a preparation method and application thereof.
Background
The nanometer and micrometer metal silver powder material is widely applied to the fields of electronic ceramics, solar photovoltaic power generation, sterilization, disinfection, electronic flexible printing and the like. The shape and structure of the micro-nano silver powder prepared by the current method can not be well controlled, and the structure and shape 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 application provides micro-nano silver powder and a preparation method thereof, which aim to solve or partially solve the technical problems in the prior art.
In a first aspect, the application provides a preparation method of micro-nano silver powder, which comprises the following steps:
dissolving a peptoid compound in a solvent, adding 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:
(R) n is an alpha-amino acid substituent or is formed by polycondensation of alpha-amino acidsIs a polypeptide chain of (a).
Preferably, in the preparation method of 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, ethylene 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, in the preparation method of the micro-nano silver powder, the peptoid compound is dissolved in a solvent, then silver salt and a reducing agent are added, after the 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.
Preferably, in the preparation method of the micro-nano silver powder, the mass 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 application also provides micro-nano silver powder, which is prepared by adopting the preparation method.
In a third aspect, the application also provides application of the micro-nano silver powder in preparing conductive silver paste, electronic ceramics, sterilization disinfector 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 compound is used as the dispersing agent, so that the preparation of the micro-nano silver powder can be realized, and the morphology, granularity and structure of the micro-nano silver powder can be adjusted by adopting the peptoid compounds with different chemical structures, so that the structure and morphology of the micro-nano silver powder can be controlled.
(2) The micro-nano silver powder prepared by the method has good dispersibility, the specific surface area and the resistivity are smaller than those of commercial samples, and the micro-nano silver powder has 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 application 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 evident that the drawings in the following description are only some embodiments of the present application and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
FIG. 1 is a surface morphology graph of micro-nano silver powder prepared in example 1 of the present application;
FIG. 2 is a surface morphology graph of the micro-nano silver powder prepared in example 2 of the present application;
FIG. 3 is a surface morphology graph of the micro-nano silver powder prepared in example 3 of the present application;
FIG. 4 is a surface morphology graph of the micro-nano silver powder prepared in example 4 of the present application;
FIG. 5 is a surface morphology graph of the micro-nano silver powder prepared in example 5 of the present application;
FIG. 6 is a surface morphology graph of the micro-nano silver powder prepared in example 6 of the present application.
Detailed Description
The following description of the embodiments of the present application will be made in detail and with reference to the embodiments of the present application, but it should be apparent that the described embodiments are only some embodiments of the present application, and not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present application without making any inventive effort, are intended to fall within the scope of the present application.
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 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:
(R) n is an alpha-amino acid substituent or a polypeptide chain formed by polycondensation of alpha-amino acids.
It should be noted that, the peptoid compound in the embodiment of the application can be used as a dispersant to prepare micro-nano silver powder, and specifically, the peptoid compound is a beta-hydroxybutyryl-amino acid compound, and the structural formula is as follows:the morphology, granularity and structure of the micro-nano silver powder can be adjusted by adopting different (R) n groups, so that the structure and morphology of the micro-nano silver powder can be controlled.
Specifically, in some embodiments, the α -amino acid may be alanine, arginine, aspartic acid, cysteine, glutamine, glutamic acid, histidine, isoleucine, glycine, asparagine, leucine, lysine, methionine, phenylalanine, proline, serine, threonine, tryptophan, tyrosine, valine, and the like, corresponding (R) n Is a polypeptide chain obtained by polycondensation of the above alpha-amino acids.
Specifically, in some embodiments, the β -hydroxybutyryl-amino acid compound may be specifically:
and 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 includes at least one of silver nitrate, silver sulfate, and silver halide.
In some embodiments, the solvent is water or an organic alcohol or ketone having a molecular weight below 300, and the particular solvent may be one of methanol, ethanol, ethylene glycol, glycerol, and acetone.
In some embodiments, the reducing agent includes 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, then silver salt and a reducing agent are added, and after the reaction, the micro-nano silver powder is obtained by filtration, 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, then silver salt and a reducing agent are added, after the reaction, the mixture is filtered, and then the filtered material is washed by ethanol and deionized water to remove organic matters and impurity salts on the surface of the filtered material, thus obtaining the micro-nano silver powder
In some embodiments, the mass to volume ratio of peptoid compound, silver salt, reducing agent, and solvent is (0.5-10) g: (0.5-15) g: (0.5-18) g: (30-80 ml).
Based on the same inventive concept, the application also provides micro-nano silver powder, which is prepared by adopting the preparation method.
Based on the same inventive concept, the application also provides application of the prepared micro-nano silver powder in preparing conductive silver paste, electronic ceramics, sterilization disinfector and solar photovoltaic power generation device.
The method for preparing the micro-nano silver powder of the present application is further described in the following 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, stirring for 30min, and uniformly mixing the solutions to obtain a mixed solution; and (3) placing the prepared mixed solution into a crystallization kettle, heating to 120 ℃, keeping the temperature for 720 minutes, filtering, and cleaning with ethanol and deionized water to obtain the micro-nano silver powder.
Wherein, the peptide-like compound is beta-hydroxybutyryl-lysine pseudo dipeptide, and the structural formula is:
specifically, the preparation method of the beta-hydroxybutyryl-lysine pseudo dipeptide comprises the following steps:
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-dimethylaminopyridine into 50ml of dichloromethane, stirring, then adding 0.024mol of triethylamine, and stirring and reacting for 20min to obtain a reaction solution;
s2, dissolving 0.015mol of N, N' -dicyclohexylcarbodiimide in 20mL of dichloromethane, then dripping the reaction solution, stirring for 3 hours at room temperature after dripping, carrying out suction filtration, respectively washing the filtrate twice with 50mL of water and 20mL of 0.1M dilute hydrochloric acid twice, washing once with 20mL of saturated sodium bicarbonate water solution and 20mL of saturated sodium chloride water solution, drying a dichloromethane phase, and concentrating;
s3, dissolving the condensed concentrated solution with 50mL of tetrahydrofuran, adding 1 equivalent of tetrabutylammonium fluoride, stirring at room temperature for 1h, then adding water for quenching reaction, evaporating tetrahydrofuran under reduced pressure, extracting water phases with 30mL of dichloromethane for 3 times, merging organic phases, washing once with 30mL of saturated sodium chloride, concentrating, adding 1 equivalent of 1M aqueous sodium hydroxide 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 phases, recrystallizing with ethanol/acetone to obtain 1.5g of white solid, namely beta-hydroxybutyryl-lysine pseudo dipeptide sodium salt, wherein the yield is 62.5%, adding an equivalent of hydrogen chloride ethanol solution into the beta-hydroxybutyryl-lysine pseudo dipeptide sodium salt, filtering, concentrating, and obtaining the beta-hydroxybutyryl-lysine pseudo dipeptide as white solid. The nuclear magnetic data of the beta-hydroxybutyryl-lysine pseudo dipeptide are: 1HNMR (400 MHz, D) 2 O)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 solutions to obtain a mixed solution; and (3) placing the prepared mixed solution into a crystallization kettle, heating to 160 ℃, keeping the temperature for 480 minutes, filtering, and cleaning with ethanol and deionized water to obtain the micro-nano silver powder, wherein the volume ratio of ethanol to water in the ethanol water solution is 1:1.
Wherein, the peptide-like compound is beta-hydroxybutyryl-glutamic acid pseudo dipeptide, and the structural formula is:
specifically, the preparation method of the beta-hydroxybutyryl-glutamic acid pseudo-dipeptide can be referred to as the preparation method of the beta-hydroxybutyryl-lysine pseudo-dipeptide in example 1, and specifically, the beta-hydroxybutyryl-glutamic acid pseudo-dipeptide is prepared from tert-butyldimethylsilyl ether beta-hydroxybutyrate and ethyl glutamate hydrochloride. The prepared beta-hydroxybutyryl-glutamic acid pseudo dipeptide nuclear magnetic hydrogen spectrum data are as follows: 1 H NMR(400MHz，D 2 O)δ4.23(m，1H)，4.15(m，1H)，2.49(m，2H)，2.25(m，2H)，2.09(m，1H)，1.92(m，1H)，1.26(d，3H)。
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, stirring for 100min, and uniformly mixing the solutions to obtain a mixed solution; and (3) placing the prepared mixed solution into a crystallization kettle, heating to 200 ℃, keeping the temperature for 600 minutes at 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 peptide-like compound is beta-hydroxybutyryl-glycine-methionine pseudo tripeptide, and the structural formula is as follows:specifically, the preparation method of the beta-hydroxybutyryl-glycine-methionine pseudo-tripeptide can be referred to as the preparation method of the beta-hydroxybutyryl-lysine pseudo-dipeptide in example 1, and specifically, the beta-hydroxybutyryl-tert-butyldimethylsilyl ether beta-hydroxybutyrate, glycine ethyl ester hydrochloride and methionine ethyl ester hydrochloride are prepared. The prepared beta-hydroxybutyryl-glycine-methionine pseudo tripeptide nuclear magnetic hydrogen spectrum data are as follows: 1 H NMR(400MHz，D 2 O)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, stirring for 100min, and uniformly mixing the solutions to obtain mixed solution; and (3) placing the prepared mixed solution into a crystallization kettle, heating to 180 ℃, keeping the temperature for 600 minutes at 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 peptide-like compound is beta-hydroxybutyryl-glycine-isoleucine pseudo tripeptide, and the structural formula is as follows:
specifically, the preparation method of the beta-hydroxybutyryl-glycine-isoleucine pseudo-tripeptide can be referred to as the preparation method of the beta-hydroxybutyryl-lysine pseudo-dipeptide in example 1, and specifically, the beta-hydroxybutyryl-tert-butyldimethylsilyl ether beta-hydroxybutyrate, glycine ethyl ester hydrochloride and isoleucine ethyl ester hydrochloride are prepared. The prepared beta-hydroxybutyryl-glycine-isoleucine pseudo-tripeptide nuclear magnetic hydrogen spectrum data are as follows: 1 H NMR(400MHz，D 2 O)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 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 water solution, adding 2.0g of reducing agent sodium borohydride, stirring for 100min, and uniformly mixing the solutions to obtain a mixed solution; and (3) placing the prepared mixed solution into a crystallization kettle, heating to 160 ℃, keeping the temperature for 480 minutes, 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 peptide-like compound is beta-hydroxybutyryl-glycyl-alanyl-methionine pseudo-tetrapeptide, and the structural formula is as follows:
specifically, the method for preparing the pseudo-tetrapeptide of beta-hydroxybutyryl-glycyl-alanyl-methionine can be referred to as the method for preparing the pseudo-dipeptide of beta-hydroxybutyryl-lysine in example 1, specifically, the method comprises the steps of preparing tert-butyl dimethyl silyl ether beta-hydroxybutyric acid, glycine ethyl ester hydrochloride, alanine ethyl ester hydrochloride and methionine ethyl ester hydrochloride. The prepared beta-hydroxybutyryl-glycyl-alanyl-methionine pseudo-tetrapeptide nuclear magnetic hydrogen spectrum data are as follows: 1 H NMR(400MHz，D 2 O)δ4.31(m，1H)，4.22(m，1H)，4.12(m，1H)，3.84(m，2H)，2.57(m，2H)，2.37(m，2H)，2.05(s，3H)，1.95(m，2H)，1.32(d，3H)。
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 glycol water solution, adding 2.4g of reducing agent formic acid, stirring for 100min, and uniformly mixing the solutions to obtain a mixed solution; and (3) placing the prepared mixed solution into 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 glycol to the water in the glycol aqueous solution is 1:1.
Wherein the peptide-like compound is beta-hydroxybutyryl-leucyl-valyl-glutamic acid pseudo-tetrapeptide, and the structural formula is as follows:
specifically, the preparation method of the beta-hydroxybutyryl-leucyl-valyl-glutamic acid pseudotetrapeptide can be referred to as the preparation method of the beta-hydroxybutyryl-lysine pseudodipeptide in example 1, and specifically, the beta-hydroxybutyryl-tert-butyldimethylsilyl ether beta-hydroxybutyrate, leucine ethyl ester hydrochloride, valine ethyl ester hydrochloride and glutamic acid ethyl ester hydrochloride are prepared. The prepared beta-hydroxybutyryl-leucyl-valyl-glutamic acid pseudo-tetrapeptide nuclear magnetic hydrogen spectrum data are as follows: 1 H NMR(400MHz，D 2 O)δ4.25(m，2H)，4.06(m，1H)，3.94(m，1H)，2.51(m，2H)，2.35(m，2H)，2.11(m，2H)，1.98(m，1H)，1.52(m，3H)，1.11(d，3H)，0.76(m，12H)。
the results of testing the surface morphology of the micro-nano silver powder prepared in the above examples 1 to 6 are shown in fig. 1 to 6, respectively.
From fig. 1 to 6, it can be seen that the micro-nano silver powder prepared in different embodiments has uniform distribution and good dispersibility, and the micro-nano silver powder prepared in different embodiments has different particle sizes and surface morphologies. 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 between 58 and 100 nm. As can be seen from FIG. 2, the micro-nano silver powder prepared in example 2 is in the shape of a sheet, and the average particle size is between 2 and 5 μm. As can be seen from FIG. 3, the micro-nano silver powder prepared in example 3 is in the shape of a sheet, and the average particle size is between 2 and 20 μm. As can be seen from FIG. 4, the micro-nano silver powder prepared in example 3 is in the form of particles with an average particle size of 0.3-0.7 μm. As can be seen from FIG. 5, the micro-nano silver powder prepared in example 5 is in the form of particles with an average particle size of 0.3-0.5 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 and 220 nm.
The specific surface areas and the specific resistivities of the micro-nano silver powder and the commercially available micro-nano silver powder prepared in examples 1 to 6 were measured, and the results are shown in table 1 below. Wherein, the specific surface area adopts BET specific surface area test method, and the resistivity test method is: an ST 2742B-type automatic powder resistivity tester manufactured by Suzhou lattice electronics Inc. is adopted, and the listed data are resistivity data of the 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 the commercial sample with the same shape, and the resistivity is obviously smaller than that of the commercial sample with the same shape.
The micro-nano silver powder prepared in the embodiment 2 and a commercial sample with the same shape as the embodiment 2 are further used for preparing the photovoltaic heterojunction conductive silver paste. The specific preparation method comprises the following steps: and (3) uniformly mixing the organic systems, adding the micro-nano silver powder or the commercial sample prepared in the embodiment 2, uniformly mixing by a planetary gravity mixer, and finally mixing by a three-roller 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 viscosity of the prepared conductive silver paste is tested to be 28-30 ten thousand cps by using a Bohler flywheel viscometer.
The heterojunction battery cells of 156 x 156 were selected, and the battery cells were prepared by using the micro-nano silver powder in example 2 and the conductive silver paste prepared by the method with the commercial sample of example 2 through procedures of screen printing, curing, light injection and the like, and the open circuit voltage Uoc, the short circuit current Isc, the filling factor FF, the conversion efficiency Eta and the resistance Rser were tested, and the results are shown in the following table 2.
TABLE 2 Performance of the battery plates 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 battery piece 1 is a battery piece prepared by using the low-temperature conductive silver paste prepared by using the micro-nano silver powder in the above example 2, and the battery piece 1 is a battery piece prepared by using the low-temperature conductive silver paste prepared by using the commercial sample with the same morphology as the example 2. From table 2, it can be seen that the battery piece 1 has better performance, and thus, the performance of the conductive silver paste prepared from the micro-nano silver powder prepared by the method is better than that of the conductive silver paste prepared from silver powder on the market in China.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the application.

Claims (3)

1. The preparation method of the micro-nano silver powder is characterized by comprising the following steps of:
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 solutions to obtain a mixed solution; placing the prepared mixed solution into a crystallization kettle, heating to 160 ℃, keeping the temperature for 480 minutes, filtering, and cleaning with ethanol and deionized water to obtain micro-nano silver powder, wherein the volume ratio of ethanol to water in an ethanol water solution is 1:1;
wherein, the peptide-like compound is beta-hydroxybutyryl-glutamic acid pseudo dipeptide, and the structural formula is:
2. the micro-nano silver powder is characterized by being prepared by the preparation method according to claim 1.
3. The application of the micro-nano silver powder in preparing conductive silver paste, electronic ceramics, sterilization disinfectants and solar photovoltaic power generation devices according to claim 2.
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