CN112828300A - Nano silver, preparation method and application - Google Patents
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- CN112828300A CN112828300A CN202011589085.3A CN202011589085A CN112828300A CN 112828300 A CN112828300 A CN 112828300A CN 202011589085 A CN202011589085 A CN 202011589085A CN 112828300 A CN112828300 A CN 112828300A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 35
- 239000012528 membrane Substances 0.000 claims abstract description 23
- 239000000919 ceramic Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 239000004332 silver Substances 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 12
- -1 silver ions Chemical class 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 230000009467 reduction Effects 0.000 claims abstract description 4
- 238000004108 freeze drying Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 238000000034 method Methods 0.000 claims description 17
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 14
- 239000008103 glucose Substances 0.000 claims description 14
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 229930003268 Vitamin C Natural products 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229940083025 silver preparation Drugs 0.000 claims description 2
- 235000019154 vitamin C Nutrition 0.000 claims description 2
- 239000011718 vitamin C Substances 0.000 claims description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims 3
- 238000005119 centrifugation Methods 0.000 claims 1
- 239000011148 porous material Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims 1
- 238000006722 reduction reaction Methods 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 39
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 24
- 229910001961 silver nitrate Inorganic materials 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 6
- 239000000976 ink Substances 0.000 description 5
- 238000007639 printing Methods 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000007641 inkjet printing Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XQSBLCWFZRTIEO-UHFFFAOYSA-N hexadecan-1-amine;hydrobromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[NH3+] XQSBLCWFZRTIEO-UHFFFAOYSA-N 0.000 description 1
- 238000011086 high cleaning Methods 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- 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
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses nano-silver and a preparation method and application thereof, and the preparation method comprises the following steps: s1, preparing a water reaction system containing silver ions; preparing a dispersant solution system; preparing a solution containing a reducing agent, mixing the solution containing the dispersing agent and a water reaction system containing silver ions, adjusting the pH value, and dropping the reducing agent at a controlled reaction temperature under the condition of ultrasonic stirring to prepare nano silver particles by reduction; and S2, washing the prepared nano silver particles by using ceramic membrane equipment, and washing and separating the prepared nano silver particles by centrifugal separation, and then freeze-drying. The nano silver particles prepared by the reduction reaction pass through membrane holes on the ceramic membrane after being washed by the ceramic membrane, so that the nano silver particles have better dispersibility and uniformity, and meanwhile, residual organic impurities on the surface of the nano silver are effectively removed by further centrifugal separation, and the prepared nano silver has high purity.
Description
Technical Field
The invention relates to the field of nano-silver preparation, in particular to nano-silver, a preparation method and application thereof, which are used for ink-jet printing conductive inks of different solvent systems.
Background
The circuit is printed in a printing mode, so that a new idea and a problem solution are provided for preparing the conductive pattern, the printing mode has the advantages of high material utilization rate, simple manufacturing process and low cost, and higher wiring density and precision can be achieved during circuit printing, so that the technologies such as ink jet printing and the like have very wide application prospects and can be applied to the fields of printing radio frequency electronic tags, solar cells, transparent conductive films and the like. The patterns obtained by printing are finer and more advantageous in terms of environmental factors and cost factors.
The particle conductive ink commonly used in the prior art requires that the particle size of nanoparticles is controlled within 100nm, and good dispersibility is required, otherwise, a nozzle is easily blocked, so that polymers such as polyvinylpyrrolidone, hexadecylammonium bromide, polyvinyl alcohol and the like are frequently used in the preparation process of the silver-based conductive ink to maintain the dispersibility of the nano silver, and the polymers are wrapped on the surface of the nano silver to influence the conductivity of a printed conductive layer, increase the resistivity, and extremely difficult to treat the surface of the nano silver to a satisfactory effect.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the preparation and cleaning method of the nano silver, the nano silver prepared by the method and the cleaning process have high cleaning efficiency, less residual quantity of organic impurities, good dispersibility and stability, good electrical property after sintering at 300 ℃, cost saving, simple process and convenient operation, and can be dispersed in various solvent systems.
A preparation method of nano silver comprises the following steps:
s1, preparing a water reaction system containing silver ions; preparing a dispersant solution system; preparing a solution containing a reducing agent, mixing the solution containing the dispersing agent and a water reaction system containing silver ions, adjusting the pH value, and dropping the reducing agent at a controlled reaction temperature under the condition of ultrasonic stirring to prepare nano silver particles by reduction;
and S2, washing the prepared nano silver particles by using ceramic membrane equipment, and washing and separating the prepared nano silver particles by centrifugal separation, and then freeze-drying.
Further, in step S1, the dispersibility of the silver nanoparticles is improved by irradiating with ultrasonic waves and adjusting the stirring rate.
The silver ion-containing aqueous solution contains silver nitrate or other aqueous solutions containing silver ions, and the concentration of the silver ions is 0.5-5 mol/L, and further 1-2 mol/L. And dropwise adding a solution system containing a dispersing agent into the silver nitrate or other aqueous solution containing silver ions.
In step S1, the dispersant in the dispersant-containing solution system is one or more of polyvinylpyrrolidone, cetyltrimethylammonium bromide, cetyltrimethylammonium chloride, polyethylene glycol, polyvinyl alcohol, and sodium dodecyl sulfate. Preferably, the aqueous solution of polyvinylpyrrolidone is used, and the amount of the dispersant is 1 to 10 times, more preferably 2 to 5 times, the amount of silver contained in the aqueous solution.
The reducing agent in the solution system containing the reducing agent is one or more of hydrazine hydrate, glucose, hydrogen peroxide, vitamin C and formaldehyde, and preferably glucose. Glucose is preferred.
The amount of reducing agent to be added may be in excess relative to the aqueous system containing silver ions. Further, 1.1-1.3 times.
The pH is adjusted by ammonia or sodium hydroxide.
Slowly dropping ammonia water or sodium hydroxide solution with the molar weight of 1-5 times that of silver ions into the mixed solution containing the silver ions and the dispersing agent under the conditions of ultrasound and stirring, and preferably selecting sodium hydroxide. Keeping ultrasonic and stirring, controlling the reaction temperature, and slowly dropping a reducing agent to prepare the nano-silver particles.
The reaction temperature is controlled to be 20-70 ℃. Further, 30-50 ℃.
Further, the nano-silver particle dispersion liquid obtained by reduction is washed by ceramic membrane equipment to prepare nano-silver particles, and the aperture of the ceramic membrane is 50-200 nm. Preferably 50nm, to prevent small-particle nano silver from leaking out through the ceramic membrane, and using hydrochloric acid and potassium dichromate as indicators to stop cleaning when no precipitate is generated in the filtrate.
Furthermore, the nano silver washed by the ceramic membrane is cleaned and separated by a centrifugal separation method, and the centrifugal rate is 4000-10000 r/min. And further, drying at 4000-5000 rpm by using a freeze dryer, and storing at low temperature.
The nano silver prepared by the preparation method of nano silver has an average particle size of 10-100 nm.
The conductive ink is prepared by mixing 10-40% of nano silver and 60-90% of a solvent, wherein the solvent is water or an organic solvent.
Compared with the prior art, the invention has the beneficial effects that:
1. the nano silver particles prepared by the reduction reaction pass through membrane holes on the ceramic membrane after being washed by the ceramic membrane, so that the nano silver particles have better dispersibility and uniformity, and meanwhile, residual organic impurities on the surface of the nano silver are effectively removed by further centrifugal separation, and the prepared nano silver has high purity.
2. The preparation method of the nano silver simplifies the process steps, has simple process, convenient operation, low energy consumption and cost saving.
3. The prepared nano silver has small organic residue on the surface and excellent conductivity.
4. The prepared nano silver is stored as a solid phase, and is convenient for subsequent use.
5. The nano silver can be redispersed in various solvents and has good dispersibility.
6. The prepared nano silver particles have the average particle size of 10-100 nm and low melting temperature, and can be suitable for low-temperature sintering and used for manufacturing conductive ink.
Drawings
FIG. 1 is a transmission electron microscope picture of nano-silver prepared in example 1;
FIG. 2 is a TG plot after example 1 and comparative example 1 washes, a. thermogravimetric analysis after comparative example 1 wash, b. thermogravimetric analysis after example 1 wash;
FIG. 3 is a differential thermal scanning analysis of the nano-silver particles obtained in example 1, wherein the melting range of the nano-silver is 125-220 ℃;
fig. 4 is a transmission electron microscope picture of the nano silver particles obtained in comparative example 4 and example 1, respectively.
As can be seen from FIG. 1, the nano silver prepared by the method of the invention has no agglomeration and good dispersibility;
as can be seen from FIG. 2, through the analysis of the thermal gravimetric test, the nano-silver prepared by the method of the invention has less residual organic impurities and smaller mass change after heating;
as can be seen from fig. 3, the melting point of the nano silver prepared by the method of the present invention is low, which indicates that the particle size is small and the distribution is uniform;
as can be seen from fig. 4, the ceramic membrane washing and then the centrifugal separation have better dispersibility than the direct centrifugal separation.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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.
Example 1
Dissolving 3g of silver nitrate in 50ml of deionized water to prepare 0.35mol/L solution, then adding 3.13g of PVP (K30), namely polyvinylpyrrolidone, fully shaking up to dissolve, then preparing 8ml of 0.1g/ml NaOH solution, dropwise adding the NaOH solution into the silver nitrate solution under the ultrasonic condition, after 5min dropwise addition, after half an hour, placing the solution in a water bath at 40 ℃ for constant temperature, and simultaneously adopting ultrasonic treatment; under the condition of ultrasonic stirring, 12ml of glucose aqueous solution prepared by 8g of glucose is dropwise added into the constant-temperature solution, the dropwise addition is completed within 5min, and the reaction is stopped after 15 min.
The prepared nano silver particle dispersion liquid is prepared by washing nano silver particles by adopting ceramic membrane equipment, the aperture of a ceramic membrane tube is selected to be 50nm, and deionized water is added for repeated cleaning for multiple times. And (3) centrifugally cleaning the nano silver cleaned by the ceramic membrane for multiple times by adopting a centrifugal separation method under the condition of 5000 r/min.
Comparative example 1
Dissolving 3g of silver nitrate in 50ml of deionized water to prepare 0.35mol/L solution, then adding 3.13g of PVP (K30), fully shaking up to dissolve, then preparing 8ml of NaOH solution with 0.1g/ml, dropwise adding the NaOH solution into the silver nitrate solution under the ultrasonic condition, finishing dropwise adding for 5min, and after half an hour, placing the solution in a water bath with the temperature of 40 ℃ for constant temperature, and simultaneously carrying out ultrasonic treatment; under the condition of ultrasonic stirring, 12ml of glucose aqueous solution prepared by 8g of glucose is dropwise added into the constant-temperature solution, the dropwise addition is completed within 5min, and the reaction is stopped after 15 min.
The prepared nano silver particle dispersion liquid adopts ceramic membrane equipment to wash prepared nano silver particles, the aperture of a ceramic membrane tube is selected to be 50nm, deionized water is added for repeated washing for many times, hydrochloric acid and potassium dichromate are used as indicators, and the washing is stopped until no precipitate is generated in filtrate.
Comparative example 2
Dissolving 3g of silver nitrate in 50ml of deionized water to prepare 0.35mol/L solution, then adding 3.13g of PVP (K30), fully shaking up to dissolve, then preparing 8ml of NaOH solution with 0.1g/ml, dropwise adding the NaOH solution into the silver nitrate solution under the ultrasonic condition, finishing dropwise adding for 5min, and after half an hour, placing the solution in a water bath with the temperature of 40 ℃ for constant temperature, and simultaneously carrying out ultrasonic treatment; under the condition of ultrasonic stirring, 12ml of glucose aqueous solution prepared by 8g of glucose is dropwise added into the constant-temperature solution, the dropwise addition is completed within 5min, and the reaction is stopped after 15 min.
The prepared nano silver particle dispersion liquid adopts nano silver particles prepared by washing with ceramic membrane equipment, the aperture of a ceramic membrane tube is selected to be 100nm, deionized water is added for repeated washing for many times, hydrochloric acid and potassium dichromate are used as indicators, and the washing is stopped until no precipitate is generated in the filtrate.
Comparative example 3
Dissolving 3g of silver nitrate in 50ml of deionized water to prepare 0.35mol/L solution, then adding 3.13g of PVP (K30), fully shaking up to dissolve, then preparing 8ml of NaOH solution with 0.1g/ml, dropwise adding the NaOH solution into the silver nitrate solution under the ultrasonic condition, finishing dropwise adding for 5min, and after half an hour, placing the solution in a water bath with the temperature of 40 ℃ for constant temperature, and simultaneously carrying out ultrasonic treatment; under the condition of ultrasonic stirring, 12ml of glucose aqueous solution prepared by 8g of glucose is dropwise added into the constant-temperature solution, the dropwise addition is completed within 5min, and the reaction is stopped after 15 min.
The prepared nano silver particle dispersion liquid is centrifugally cleaned for a plurality of times by adopting a centrifugal separation method under the condition of 5000 revolutions per minute.
Comparative example 4
Dissolving 3g of silver nitrate in 50ml of deionized water to prepare 0.35mol/L solution, then adding 3.13g of PVP (K30), fully shaking up to dissolve, then preparing 8ml of NaOH solution with 0.1g/ml, dropwise adding the NaOH solution into the silver nitrate solution under the ultrasonic condition, finishing dropwise adding for 5min, and after half an hour, placing the solution in a water bath with the temperature of 40 ℃ for constant temperature, and simultaneously carrying out ultrasonic treatment; under the condition of ultrasonic stirring, 12ml of glucose aqueous solution prepared by 8g of glucose is dropwise added into the constant-temperature solution, the dropwise addition is completed within 5min, and the reaction is stopped after 15 min.
The prepared nano silver particle dispersion liquid is centrifugally cleaned for a plurality of times by adopting a centrifugal separation method under the condition of 11000 r/min.
TABLE 1 ceramic membrane separation cleaning Effect
TABLE 2 cleaning Effect of different samples
Claims (10)
1. A preparation method of nano-silver is characterized by comprising the following steps:
s1, preparing a water reaction system containing silver ions; preparing a dispersant solution system; preparing a solution containing a reducing agent, mixing the solution containing the dispersing agent and a water reaction system containing silver ions, adjusting the pH value, and dropping the reducing agent at a controlled reaction temperature under the condition of ultrasonic stirring to prepare nano silver particles by reduction;
and S2, washing the prepared nano silver particles by using ceramic membrane equipment, and washing and separating the prepared nano silver particles by centrifugal separation, and then freeze-drying.
2. The method for preparing nano silver according to claim 1, wherein in the step S1, the dispersibility of the nano silver powder is improved by irradiating with ultrasonic waves and adjusting the stirring rate.
3. The method for preparing nano silver according to claim 1 or 2, wherein in step S1, the dispersant is one or more selected from polyvinylpyrrolidone, cetyltrimethylammonium bromide, cetyltrimethylammonium chloride, polyethylene glycol, polyvinyl alcohol, and sodium dodecylsulfonate.
4. The method of claim 3, wherein the pH is adjusted by ammonia or NaOH in step S1.
5. The method for preparing nano-silver according to claim 4, wherein in step S1, the reducing agent is one or more of hydrazine hydrate, glucose, hydrogen peroxide, vitamin C and formaldehyde.
6. The method of claim 5, wherein in step S2, the pore diameter of the ceramic membrane is 50-200 nm.
7. The method of claim 6, wherein in step S2, the centrifugation rate is 4000-10000 rpm.
8. The method of preparing nano silver according to claim 7, wherein the washed nano silver particles are dried by a freeze dryer in step S2.
9. The nano-silver prepared by the nano-silver preparation method according to claims 1 to 8, wherein the nano-silver has an average particle size of 10 to 100 nm.
10. The conductive ink is characterized in that 10-40% of nano silver and 60-90% of solvent are mixed to prepare the conductive ink according to the nano silver prepared by the method of any one of claims 1-8, and the solvent is water or an organic solvent.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113458410A (en) * | 2021-06-30 | 2021-10-01 | 东北大学 | With H2O2Method for synthesizing nano silver with various micro-morphologies as reducing agent |
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| CN114101697A (en) * | 2021-10-22 | 2022-03-01 | 北京航空航天大学 | Method for preparing Ag NPs particles with specified particle size |
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