CN102463351A - Methods for preparing silver nano-particles and conductive nano-film of silver nano-particles - Google Patents
Methods for preparing silver nano-particles and conductive nano-film of silver nano-particles Download PDFInfo
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- CN102463351A CN102463351A CN2010105328739A CN201010532873A CN102463351A CN 102463351 A CN102463351 A CN 102463351A CN 2010105328739 A CN2010105328739 A CN 2010105328739A CN 201010532873 A CN201010532873 A CN 201010532873A CN 102463351 A CN102463351 A CN 102463351A
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Abstract
The invention discloses methods for preparing silver nano-particles and a conductive film of the silver nano-particles. The method for preparing the silver nano-particles comprises the following steps of: 1) dripping an aqueous solution of sodium salt or potassium salt of ethylenediaminetetracetic acid into an aqueous solution of soluble silver salt until the solution is changed from turbidity to clarity, and stopping dripping to obtain a silver salt solution of an ethylenediaminetetracetic acid chelate ; and 2) dripping an aqueous solution of a reducing agent into the silver salt solution of the ethylenediaminetetracetic acid chelate under stirring condition, continuing reacting after the dripping is finished until the color of the solution is not changed, and thus obtaining the silver nano-particles. The method for preparing the conductive film comprises the following steps of: dispersing the silver nano-particles prepared by the method into water, coating a dispersion liquid on a substrate, and drying to obtain a silver nano-film; and soaking the silver nano-film in a strong electrolyte solution and treating for at least 3 seconds, taking out, and drying to obtain a film consisting of clinkery silver nano-particles. The silver nano-film has excellent electrical conductivity.
Description
Technical field
The present invention relates to a kind of method for preparing silver nano-grain and electrical-conductive nanometer film thereof.
Background technology
Silver nano-grain is a kind of broad-spectrum metal nano material.Especially its nano thin-film all has important application in fields such as flexible circuit, flexible electrode, SERS, reflectance coating, thin film transistor (TFT), Organic Light Emitting Diodes.A main method of preparation silver nano-grain is a wet chemistry method at present; Its basic ideas are in the aqueous solution that contains little molecule or big molecular organic stabilizing agent, to obtain silver nano-grain with reducing agent reduction silver ion; Utilize organic stabilizer to be adsorbed in silver nano-grain surface and suppress it and reunite and growth, thereby obtain silver nano-grain.The organic molecule that the nano thin-film that the silver nano-grain of method for preparing is formed floor height insulation because of the silver nano-grain surface coverage causes film resistor very high.Obtain the silver-colored nano thin-film of the high conductivity of suitable electronics application, must the organic molecule on silver nano-grain surface be removed.Method commonly used is a high temperature sintering, under hundreds of degrees centigrade temperature, organic molecule is decomposed because the fusing point of silver nano-grain is more much lower than body silver, be about about 200 ℃, so during high temperature sintering nano-Ag particles also by clinkering.The silver-colored nano thin-film electrical conductivity of utilizing sintering to obtain is very high; But the high temperature limit that sintering is required the application of this kind method on polymer base substrate; Because the used polymer base of flexible circuit and electrode substrate is the polymer of poor heat resistance normally, like polyphenyl dioctyl phthalate glycol ester.Except heat treatment, the researcher has also proposed methods such as laser ablation, microwave treatment, plasma treatment, high voltage sintering.Used high temperature of above method and special installation have limited its range of application, and the popularization that is unfavorable for these methods is with practical.People such as Wakuda utilize organic solvent flush away such as ethanol to be adsorbed on the lauryl amine on silver nano-grain surface, caused silver nano-grain clinkering at normal temperatures, but resulting film resistor are very high.It is the silver nano-grain of stabilizing agent that people such as Magdassi utilize PDDA to handle with the polyacrylic acid; Utilization gathers positive electrolyte and the effect that gathers between the cloudy electrolyte has caused silver nano-grain clinkering at normal temperatures, has obtained the silver-colored nano thin-film of high conduction.More than the method for two kinds of normal temperature clinkering silver nano-grains used organic solvent, organic stabilizer and specific polymers, improved cost and be unfavorable for environmental protection.
Summary of the invention
The present invention is directed to the deficiency of prior art, proposed a kind of method for preparing silver nano-grain.In the preparation process, need not to add organic stabilizer, resulting silver nano-grain is handled through electrolyte solution commonly used and is got final product clinkering, obtains the silver-colored nano thin-film of high conduction.
The method for preparing silver nano-grain provided by the present invention comprises the steps:
1) aqueous solution with disodium edta or sylvite splashes in the silver soluble saline solution, becomes clarification until solution by muddiness, stops to drip, and obtains the silver salt solution of ethylenediamine tetra-acetic acid chelating; The pH value of aqueous solution of said disodium edta or sylvite is 6-8;
2) under stirring, the reducing agent aqueous solution is splashed in the silver salt solution of said ethylenediamine tetra-acetic acid chelating, dropwise the continued reaction, no longer change until solution colour, promptly obtain silver nano-grain.
Wherein, soluble silver salt described in the step 1) can be selected from following at least a: silver nitrate, silver acetate, silver fluoride and silver perchlorate; The mass concentration of soluble silver salt can be 0.001～10% in the said silver soluble saline solution, is preferably 0.01～1%; The concentration of disodium edta or sylvite can be 0.5～1.5M in the aqueous solution of said disodium edta or sylvite.
The aqueous solution of disodium edta described in the step 1) or sylvite can be prepared according to following two kinds of methods:
1) NaOH or KOH solution are joined in the ethylenediamine tetra-acetic acid, the limit edged stirs, and till ethylenediamine tetra-acetic acid dissolves fully, adds water again and is settled to desired concn, obtains the edetate aqueous solution of pH value for 6-8; The concentration of said NaOH or KOH solution is 5～15M;
2) disodium edta or sylvite is soluble in water, again its pH value is adjusted to pH=6～8, promptly obtain the aqueous solution of said disodium edta or sylvite; Said disodium edta is specially disodium EDTA or tetrasodium salt of EDTA; Said ethylene diamine tetraacetic acid sylvite is specially EDTA Dipotassium salt or ethylenediamine tetra-acetic acid four sylvite.
Step 2) reducing agent described in can be catechol and/or hydroquinones; Described in the consumption of said reducing agent and the step 1) in the silver soluble saline solution mol ratio of soluble silver salt can be 0.1: 1～10: 1, preferred 1: 1.
Step 2) reaction temperature of reaction is 10-95 ℃ described in; Step 2) rate of addition that described in the reducing agent aqueous solution is splashed in the silver salt solution of said ethylenediamine tetra-acetic acid chelating is 0.1-0.5mL/min, and the rotating speed of said stirring is 500-1500rpm.
The present invention also provides a kind of method (being the method for silver nano-grain normal temperature clinkering) for preparing silver-colored nano conductive film.
The present invention also provides a kind of method for preparing silver-colored nano conductive film, comprises the steps:
A) prepare silver nano-grain according to method provided by the invention;
B) silver nano-grain with the step a) preparation is scattered in the water, obtains the silver nano-grain aqueous dispersions; Said dispersion liquid is coated in the substrate, drying obtains silver-colored nano thin-film again;
C) said silver-colored nano thin-film is dipped in the strong electrolyte solution handled at least 3 seconds, take out, drying, promptly obtained the conductive film of forming by the silver nano-grain of clinkering.
Wherein, substrate described in the step b) does not have specific (special) requirements, can be any substrate, comprises polymer, glass, pottery, metal etc.Strong electrolyte described in the step c) is meant in the aqueous solution electrolyte of ionization fully; Like various solubility salts, acid etc., its concentration is greater than 10
-4M.
The present invention compared with prior art has following advantage:
1, the gained silver nano-grain gets final product clinkering through general strong electrolyte solution-treated, and need not needs heat treatment just can make the silver nano-grain clinkering like conventional method, and is energy-conservation quick again.
2, the method for preparing the conductive silver nano thin-film provided by the invention can be carried out at normal temperatures, is particularly useful on the bad polymeric substrates of heat resistance, preparing conducting film.
Description of drawings
Fig. 1 is the stereoscan photograph of the silver nano-grain film handled without electrolyte solution among the embodiment 3.
Fig. 2 is the stereoscan photograph of the silver nano-grain film that the process electrolyte solution is handled among the embodiment 3.
Fig. 3 is the photo of the conductive silver nano thin-film that in the PET substrate, prepares among the embodiment 3.
The specific embodiment
Below in conjunction with specific embodiment the present invention is described further, but the present invention is not limited to following examples.
Experimental technique described in the following embodiment like no specified otherwise, is conventional method; Said reagent and material like no specified otherwise, all can obtain from commercial sources." wt% " among the following embodiment refers to " quality percentage composition ".
Embodiment 1, preparation silver nano-grain and silver-colored nano thin-film
The edetate solution (pH=7.0, EDTA are dissolved in the 10M NaOH solution, add water again and are settled to 1M) of 1M is dropwise joined the AgNO of 70g 0.1wt% (0.0004mol)
3In the aqueous solution, become clarification by muddiness, consume edetate solution 0.61mL altogether until solution.0.0454g (0.0004mol) catechol is dissolved in and obtains catechol solution in the 20g water.The AgNO that catechol solution is dropwise added the EDTA chelating for preparing
3In the middle of the solution, impose stirring simultaneously, speed is 600rpm, and reaction temperature is 25 ℃.Dropwised in 1 hour, and continued reaction and stopped reaction in 1 hour, solution becomes grey black.Products therefrom centrifugation, with water washing, three times repeatedly.The gained silver nano-grain is scattered in the 30mL water again, is coated on the substrate of glass, 60 ℃ of dry silver-colored nano thin-films, surveying its side resistance is 35k Ω/mouth.Gained silver nano thin-film is soaked in the CaCl of 0.1M
210s in the aqueous solution takes out with the water flushing, and nitrogen dries up, and promptly obtains the good silver-colored nano thin-film of electric conductivity, and surveying its side's resistance is 1.02 Ω/.
Embodiment 2, preparation silver nano-grain and silver-colored nano thin-film
The edetate solution (pH=7.0, EDTA are dissolved in the 10M NaOH solution, add water again and are settled to 1M) of 1M is dropwise joined the AgNO of 70g 0.2wt% (0.0008mol)
3In the aqueous solution, become clarification by muddiness, consume edetate solution 1.34mL altogether until solution.0.0908g (0.0008mol) catechol is dissolved in and obtains catechol solution in the 20g water.With the slow AgNO that splashes into the EDTA chelating for preparing of catechol solution
3In the middle of the solution, impose stirring simultaneously, speed is 800rpm, and reaction temperature is 40 ℃.Dropwised in 1 hour, and continued reaction and stopped reaction in 1 hour, solution becomes grey black.Products therefrom centrifugation, with water washing, three times repeatedly.The gained silver nano-grain is scattered in the 30mL water again, is coated on the ceramic bases, 60 ℃ of dryings obtain silver-colored nano thin-film, survey its side's resistance and are 15.47k Ω/mouth.Gained silver nano thin-film is soaked in the MgCl of 0.1M
215s in the aqueous solution takes out and washes with water.Nitrogen dries up, and promptly obtains the good silver-colored nano thin-film of electric conductivity, and surveying its side's resistance is 0.57 Ω/.
Embodiment 3, preparation silver nano-grain and silver-colored nano thin-film
The edetate solution (tetrasodium ethylenediamine tetraacetate is soluble in water, regulates its pH value to 7.0 again) of 1.5M is dropwise joined the AgNO of 70g 0.4wt% (0.0016mol)
3In the aqueous solution, become clarification by muddiness, consume edetate solution 1.83mL altogether until solution.0.1816g (0.0016mol) catechol is dissolved in and obtains catechol solution in the 40g water.The AgNO that catechol solution is dropwise added the EDTA chelating for preparing
3In the middle of the solution, impose stirring simultaneously, speed is 900rpm, and reaction temperature is 80 ℃.1.5 hour dropwise, continue reaction and stopped reaction in one hour, solution becomes grey black.Products therefrom centrifugation, with water washing, three times repeatedly.The gained silver nano-grain is scattered in the 30mL water again, is coated in PET (polyester) substrate, 65 ℃ of dry silver-colored nano thin-films, its electromicroscopic photograph is seen Fig. 1, surveying its side resistance is 9.42k Ω/.Gained silver nano thin-film is soaked in 5s in the NaCl aqueous solution of 0.2M, takes out with the water flushing, nitrogen dries up, and promptly obtains the good silver-colored nano thin-film of electric conductivity, and surveying its side resistance is 0.47k Ω/.The electromicroscopic photograph of the silver-colored nano thin-film after the electrolyte treatment is seen Fig. 2, can know that by Fig. 2 silver nano-grain is clinkering.
Embodiment 4, preparation silver nano-grain and silver-colored nano thin-film
The edetate solution (pH=6.5, tetrasodium ethylenediamine tetraacetate is soluble in water, regulates its pH value to 6.5 again) of 0.5M is dropwise joined the CH of 70g 0.05wt% (0.0002mol)
3In the COOAg aqueous solution, become clarification by muddiness until solution.Consume edetate solution 0.70mL altogether.0.0277g (0.0002mol) hydroquinones is dissolved in and obtains catechol solution in the 30g water.With the slow CH that splashes into the EDTA chelating for preparing of hydroquinones solution
3In the middle of the COOAg solution, impose stirring simultaneously, speed is 1000rpm, and reaction temperature is 25 ℃.Dropwised in one hour, and continued reaction and stopped reaction in one hour, solution becomes grey black.Products therefrom centrifugation, with water washing, three times repeatedly.The gained silver nano-grain is scattered in the 30mL water again, be coated at the bottom of the silicon wafer-based on, 60 ℃ of dry silver-colored nano thin-films, surveying its side resistance is 50k Ω/.Gained silver nano thin-film is soaked in 10
-3The CaCl of M
220s in the middle of the aqueous solution takes out with the water flushing, and nitrogen dries up, and promptly obtains the good silver-colored nano thin-film of electric conductivity, and surveying its side's resistance is 15.45 Ω/mouths.
Embodiment 5, preparation silver nano-grain and silver-colored nano thin-film
The edetate solution (pH=7.5, EDTA are dissolved in the 10M KOH solution, add water again and are settled to 1M) of 1M is dropwise joined the AgClO of 60g 0.8wt% (0.0023mol)
4In the aqueous solution, become clarification by muddiness until solution.Consume edetate solution 5.05mL altogether.0.3632g (0.0032mol) catechol is dissolved in and obtains catechol solution in the 20g water.With the slow AgClO that splashes into the EDTA chelating for preparing of catechol solution
4In the middle of the solution, impose stirring simultaneously, speed is 800rpm, and reaction temperature is 60 ℃.Dropwised in one hour, and continued reaction and stopped reaction in 1 hour, solution becomes grey black.Products therefrom centrifugation, with water washing, three times repeatedly.The gained silver nano-grain is scattered in the 30mL water again, is coated in PTFE (polytetrafluoroethylene (PTFE)) substrate, 60 ℃ of dry silver-colored nano thin-films, surveying its side resistance is 6k Ω/.Gained silver nano thin-film is soaked in 40s in the HCl aqueous solution of 0.1M, takes out with the water flushing, nitrogen dries up, and promptly obtains the good silver-colored nano thin-film of electric conductivity, and surveying that its side hinders is 0.45 Ω/.
Embodiment 6, preparation silver nano-grain and silver-colored nano thin-film
The edetate solution (pH=7.0, EDTA are dissolved in the 10M NaOH solution, add water again and are settled to 1M) of 1M is dropwise joined the AgNO of 70g 0.1wt% (0.0004mol)
3In the aqueous solution, become clarification by muddiness, consume edetate solution altogether until solution.0.0454g (0.0004mol) catechol is dissolved in and obtains catechol solution in the 20g water.Hydroquinones solution is slow for to splash into the AgNO of the EDTA chelating for preparing
3In the middle of the solution, impose stirring simultaneously, speed is 600rpm, and reaction temperature is 20 ℃.Dropwised in 1 hour, and continued reaction and stopped reaction in 1 hour, solution becomes grey black.Products therefrom centrifugation, with water washing, three times repeatedly.The gained silver nano-grain is scattered in the 30mL water again, is coated in PP (polypropylene) substrate, 60 ℃ of dry silver-colored nano thin-films, surveying its side resistance is 37k Ω/.Gained silver nano thin-film is soaked in the MgSO of 0.1M
420s in the middle of the aqueous solution takes out and washes with water.Nitrogen dries up, and promptly obtains the good silver-colored nano thin-film of electric conductivity, and surveying its side's resistance is 0.95 Ω/.
Claims (10)
1. a method for preparing silver nano-grain comprises the steps:
1) aqueous solution with disodium edta or sylvite splashes in the silver soluble saline solution, becomes clarification until solution by muddiness, stops to drip, and obtains the silver salt solution of ethylenediamine tetra-acetic acid chelating; The pH value of aqueous solution of said disodium edta or sylvite is 6-8;
2) under stirring, the reducing agent aqueous solution is splashed in the silver salt solution of said ethylenediamine tetra-acetic acid chelating, dropwise the continued reaction, no longer change until solution colour, promptly obtain silver nano-grain.
2. method according to claim 1 is characterized in that: soluble silver salt described in the step 1) is selected from following at least a: silver nitrate, silver acetate, silver fluoride and silver perchlorate; The mass concentration of soluble silver salt is 0.001～10% in the said silver soluble saline solution, is preferably 0.01～1%.
3. method according to claim 1 and 2 is characterized in that: the concentration of disodium edta or sylvite is 0.5～1.5M in the aqueous solution of disodium edta described in the step 1) or sylvite.
4. according to arbitrary described method among the claim 1-3, it is characterized in that: the compound method of the aqueous solution of disodium edta described in the step 1) or sylvite be following a) or b):
A) NaOH or KOH solution are joined in the ethylenediamine tetra-acetic acid, the limit edged stirs, and till ethylenediamine tetra-acetic acid dissolves fully, adds water again and is settled to desired concn, obtains the edetate aqueous solution of pH value for 6-8; The concentration of said NaOH or KOH solution is 5～15M;
B) disodium edta or sylvite is soluble in water, again its pH value is adjusted to pH=6～8, promptly obtain the aqueous solution of said disodium edta or sylvite; Said disodium edta is disodium EDTA or tetrasodium salt of EDTA; Said ethylene diamine tetraacetic acid sylvite is EDTA Dipotassium salt or ethylenediamine tetra-acetic acid four sylvite.
5. method according to claim 4 is characterized in that: the concentration of said a) middle NaOH or KOH solution is 5～15M; Said b) disodium edta described in is disodium EDTA or tetrasodium salt of EDTA; Said ethylene diamine tetraacetic acid sylvite is EDTA Dipotassium salt or ethylenediamine tetra-acetic acid four sylvite.
6. according to each described method among the claim 1-5, it is characterized in that: step 2) described in reducing agent be catechol and/or hydroquinones; Described in the consumption of said reducing agent and the step 1) in the silver soluble saline solution mol ratio of soluble silver salt be 0.1: 1～10: 1, preferred 1: 1.
7. according to each described method among the claim 1-6, it is characterized in that: step 2) described in the reaction reaction temperature be 10-95 ℃; Step 2) rate of addition that described in the reducing agent aqueous solution is splashed in the silver salt solution of said ethylenediamine tetra-acetic acid chelating is 0.1-0.5mL/min, and the rotating speed of said stirring is 500-1500rpm.
8. a method for preparing the conductive silver nano thin-film comprises the steps:
A) prepare silver nano-grain according to arbitrary described method among the claim 1-7;
B) silver nano-grain with the step a) preparation is scattered in the water, obtains the silver nano-grain aqueous dispersions; Said dispersion liquid is coated in the substrate, drying obtains silver-colored nano thin-film again;
C) said silver-colored nano thin-film is dipped in the strong electrolyte solution handled at least 3 seconds, take out, drying, obtain the conductive silver nano thin-film.
9. method according to claim 8 is characterized in that: substrate described in the step b) comprises polymer, glass, pottery or metal.
10. it is characterized in that according to Claim 8 or 9 described methods: strong electrolyte described in the step c) is meant in the aqueous solution electrolyte of ionization fully; The concentration of strong electrolyte is greater than 10 in the said strong electrolyte solution
-4M.
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| CN102828176A (en) * | 2012-07-31 | 2012-12-19 | 东南大学 | Preparation method for uniform gold nanoparticle film |
| CN102990083A (en) * | 2012-12-25 | 2013-03-27 | 中国科学院合肥物质科学研究院 | Preparation method of silver nanometer particle film |
| CN103600082A (en) * | 2013-11-26 | 2014-02-26 | 清华大学 | Silver nanoparticle layer and preparation method and application thereof |
| CN109128211A (en) * | 2018-08-16 | 2019-01-04 | 山东大学 | The method of micro-nano silver particle is prepared in water solution system |
| CN109487250A (en) * | 2017-09-13 | 2019-03-19 | 北京化工大学 | A method of preparing electroplate composite material |
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| CN114029505A (en) * | 2021-10-27 | 2022-02-11 | 南京大学 | Method for preparing metal monoatomic compound by laser ablation |
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