CN114570937B - Synthesis method of superfine monodisperse nano Ag - Google Patents
Synthesis method of superfine monodisperse nano Ag Download PDFInfo
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- 238000001308 synthesis method Methods 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000002245 particle Substances 0.000 claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 150000001412 amines Chemical class 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 20
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 16
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical group [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 12
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 11
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 11
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 11
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000005642 Oleic acid Substances 0.000 claims description 11
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 11
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 10
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 9
- 230000002194 synthesizing effect Effects 0.000 claims description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- 239000000654 additive Substances 0.000 claims description 8
- 230000000996 additive effect Effects 0.000 claims description 8
- 150000004668 long chain fatty acids Chemical class 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical class [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 239000012046 mixed solvent Substances 0.000 claims description 6
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940071536 silver acetate Drugs 0.000 claims description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 2
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 claims description 2
- 229910000367 silver sulfate Inorganic materials 0.000 claims description 2
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 2
- WYPBVHPKMJYUEO-NBTZWHCOSA-M sodium;(9z,12z)-octadeca-9,12-dienoate Chemical compound [Na+].CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O WYPBVHPKMJYUEO-NBTZWHCOSA-M 0.000 claims description 2
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 229910017053 inorganic salt Inorganic materials 0.000 abstract description 3
- 238000013341 scale-up Methods 0.000 abstract description 3
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract 2
- 239000000376 reactant Substances 0.000 abstract 2
- 238000004627 transmission electron microscopy Methods 0.000 description 21
- 239000000047 product Substances 0.000 description 15
- 239000002244 precipitate Substances 0.000 description 11
- 230000005540 biological transmission Effects 0.000 description 10
- 238000001000 micrograph Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 238000003917 TEM image Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- RVRHBLSINNOLPI-UHFFFAOYSA-N Lythridin Natural products COc1ccc(cc1OC)C2CC(CC3CCCCN23)OC(=O)CC(O)c4ccc(O)cc4 RVRHBLSINNOLPI-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- -1 benzyl alcohol, olefin Chemical class 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- LTNZEXKYNRNOGT-UHFFFAOYSA-N dequalinium chloride Chemical compound [Cl-].[Cl-].C1=CC=C2[N+](CCCCCCCCCC[N+]3=C4C=CC=CC4=C(N)C=C3C)=C(C)C=C(N)C2=C1 LTNZEXKYNRNOGT-UHFFFAOYSA-N 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
Classifications
-
- 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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses a synthesis method of superfine monodisperse nano Ag, and belongs to the technical field of inorganic material preparation processes. The preparation method takes metal inorganic salt as a raw material, and the metal inorganic salt reacts for 20 to 60 minutes in a long-chain amine solvent at 160 to 200 ℃, and the ultra-fine monodisperse nano Ag with the particle diameter smaller than 5nm and controllable composition, structure, morphology and size is formed by controlling the mole ratio of reactants, the concentration of the reactants and experimental parameters of reaction temperature. The method has the advantages of low cost and easy acquisition of raw materials, less reaction time consumption, simple operation, good process repeatability, stable product quality and safe and reliable operation, and is suitable for industrial scale-up production.
Description
Technical Field
The invention relates to a synthesis method of superfine monodisperse nano Ag, and belongs to the technical field of inorganic material preparation processes.
Background
The nano Ag material has large specific surface area and strong chemical reaction activity, and has potential application prospect in the fields of catalysis, antibiosis, sensing and the like. Because of the special physical and chemical properties of high electric conductivity, high heat conduction and the like, the method has wide application in the fields of microelectronics, optoelectronics, electronic appliances, superconducting materials, electron radiation protection, flexible display screens and the like. At present, although nano Ag with different sizes and morphologies is synthesized by various methods, reports of Ag nano crystals with particle sizes smaller than 10nm and good dispersibility are less, and nano Ag with particle sizes smaller than 5nm is not available so far. Mainly because 1, the size of nano Ag with the grain diameter smaller than 5nm is difficult to regulate and control; 2, the small-size nano Ag has high specific surface area, so that the surface Ag atoms are extremely easy to oxidize or agglomerate. How to stabilize nano Ag and realize good dispersibility in different systems has great significance. The superfine monodisperse nano Ag not only improves the utilization efficiency of Ag powder and reduces the manufacturing cost of products, but also shows excellent performance in practice, so that the size of the nano Ag is controllable and is not easy to agglomerate. Recently, some research groups prove that the ultra-fine monodisperse nano Ag can be used as a catalyst for oxidizing methane, benzyl alcohol, olefin, low-temperature oxidizing CO, catalyzing and hydrogenating nitrobenzene and the like through experiments; the superfine monodisperse nano Ag as an important conductive component of the electronic paste creates a wide market development space for development of electronic and electric elements and new energy industries. This shows that the superfine monodisperse nanometer Ag has good prospect as a novel catalyst and conductive Ag slurry. Therefore, the structure and property research of the superfine monodisperse nano Ag is widely focused on material specialists at home and abroad.
The production of ultra-fine monodisperse nano Ag is currently mainly a physical method and a chemical reduction method. The physical method is mainly divided into high-energy ball milling and air inflation, an air flow jet atomization method and a plasma jet atomization method. The methods have the advantages of high cost, complex operation procedures, long time consumption, high energy consumption and difficult scale-up industrial production. In recent years, some research institutions have attempted to synthesize nano Ag having 5-7nm by chemical reduction (patent application of the invention, CN 102350344 a, 2012). However, the method needs extremely high temperature, and the TEM picture in the patent shows that the middle of the quasi-spherical 5-7nm mAg nanocrystalline is further distributed with fine Ag nanocrystalline in the middle of the distance of 2.4-3nm, and the size is not uniform. Controlling the size of the particle size and the uniformity of the particle size distribution is extremely important in the process of synthesizing and using the material; the size and uniformity of the particle size affects the overall performance of the process and performance. Therefore, in order to realize the industrial application of the nano Ag with smaller size and more uniformity in the fields of catalysis, conductive slurry and the like, the research of a preparation method which is simple and convenient in process, stable in product quality, less in time consumption, economical and easy for mass production is a challenge in the field of chemical technology.
Disclosure of Invention
The invention aims to provide a synthesis method of superfine monodisperse nano Ag, which adopts cheap and easily available raw materials, and can be synthesized in a large amount by a simple way so as to fill the blank of simple preparation of the superfine monodisperse nano Ag. The method is easy to amplify, convenient to regulate and control, excellent in product performance and strong in regulatability, can be used as a standard substance, and has wide market prospect in the fields of catalysis, conductive slurry and the like.
The aim of the invention is realized by the following technical scheme:
the invention relates to a method for synthesizing superfine monodisperse nano Ag, which comprises the following steps:
s1, adding a long-chain fatty acid sodium additive into a long-chain amine solvent, and then adding silver metal salt;
s2, the reaction temperature is 160-200 ℃ and the reaction time is 20-60 minutes;
and S3, washing the obtained product with ethanol, and drying to directly obtain the superfine monodisperse nano Ag.
In step S1, the silver metal salt is present in an amount of 0.002 to 0.2 g/ml of solvent.
As one embodiment of the present invention, the long-chain amine solvent is one or a mixture of several of oleylamine, octadecylamine, hexadecylamine and decamine.
As one embodiment of the present invention, the long chain fatty acid sodium additive includes sodium oleate, sodium linoleate, sodium stearate.
As an embodiment of the present invention, the silver metal salt is silver nitrate, silver sulfate, silver acetate or silver chloride.
As an embodiment of the present invention, in step S1, the molar ratio of the long-chain amine solvent and the long-chain fatty acid sodium additive is 1 to 15:1.
in step S3, the temperature of the drying is 40 to 80 ℃ and the time is 20 to 40 minutes as an embodiment of the present invention.
In step S1, octadecene is further added to the solvent as an embodiment of the present invention.
As one embodiment of the invention, the molar ratio of long chain amine to octadecene is 0.5-10:1
In step S1, oleic acid is also added to the solvent as an embodiment of the present invention.
As one embodiment of the invention, the molar ratio of oleic acid to long-chain fatty acid sodium additive is 0.1-10:1.
Compared with the prior art, the invention has the following advantages and outstanding effects:
1) The invention adopts inorganic salt as raw material and long-chain amine such as oleylamine, octadecylamine, hexadecylamine or tetramine as solvent, and adopts simple wet chemical method to prepare the superfine monodisperse nano Ag; the product has smaller size, average diameter of 4-5nm, good dispersibility and good crystallization.
2) Compared with other methods for preparing the superfine monodisperse nano Ag, the method has the most important advantages of low cost, capability of amplifying industrial production, low cost and easy acquisition of raw materials, quite simple process, easy amplification of production, quite excellent oil solubility of products, capability of directly dispersing the prepared superfine monodisperse nano Ag in slurry and quite simple process.
3) The invention adds the strong alkaline sodium oleate solution into the long-chain amine solvent, so that the reaction liquid becomes into an emulsion shape to protect the monodisperse nano Ag, the nano Ag does not undergo agglomeration reaction, and the grain size of the nano Ag is accurately controlled at 4-5nm.
In a word, the invention provides a simple and easy method for synthesizing the superfine monodisperse nano Ag, which is very suitable for industrial large-scale production and has very broad application prospect.
Drawings
Other features, objects and advantages of the present invention will become more apparent upon reading of the detailed description of non-limiting embodiments, given with reference to the accompanying drawings in which:
FIG. 1 is a powder X-ray diffraction pattern of ultra-fine monodisperse nano Ag of example 1;
FIG. 2 is a transmission electron microscope image of ultra-fine monodisperse nano Ag of example 1; wherein a is a transmission electron microscopy image at low magnification of 100nm and b is a transmission electron microscopy image at high magnification of 5 nm;
FIG. 3 is a transmission electron microscope image of ultra-fine monodisperse nano Ag of example 2; wherein a is a transmission electron microscopy image at low magnification of 100nm and b is a transmission electron microscopy image at high magnification of 5 nm;
FIG. 4 is a transmission electron microscope image of the ultra-fine monodisperse nano Ag of example 3; wherein a is a transmission electron microscopy image at low magnification of 100nm and b is a transmission electron microscopy image at high magnification of 5 nm;
FIG. 5 is a transmission electron microscope image of ultra-fine monodisperse nano Ag of example 4; wherein a is a transmission electron microscopy image at low magnification of 100nm and b is a transmission electron microscopy image at high magnification of 5 nm;
FIG. 6 is a transmission electron microscope image of ultra-fine monodisperse nano Ag of example 5; wherein a is a transmission electron microscopy image at low magnification of 100nm and b is a transmission electron microscopy image at high magnification of 5 nm;
FIG. 7 is a transmission electron microscope image of the ultra-fine monodisperse nano Ag of example 6; wherein a is a transmission electron microscopy image at low magnification of 100nm and b is a transmission electron microscopy image at high magnification of 5 nm;
FIG. 8 is a transmission electron microscope image of ultra-fine monodisperse nano Ag of comparative example 1; wherein a is a transmission electron microscopy image at low magnification of 100nm and b is a transmission electron microscopy image at high magnification of 10 nm;
FIG. 9 is a transmission electron microscope image of ultra-fine monodisperse nano Ag of comparative example 2; where a is a transmission electron micrograph at low magnification 100nm and b is a transmission electron micrograph at high magnification 10 nm.
Detailed Description
The present invention will be described in detail with reference to examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that several modifications and improvements can be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
Example 1
Heating 10ml of oleylamine, 2ml of sodium oleate and 9ml of octadecene to 160 ℃, adding silver nitrate with the mass of 0.68g into the mixture, reacting for 30 minutes, pouring out the mixed solvent of the oleylamine, the sodium oleate and the like, washing the obtained precipitate with ethanol, and drying at 40 ℃ for 30 minutes to obtain the superfine monodisperse nano Ag. The resulting products were characterized by XRD and transmission electron microscopy. The powder X-ray diffraction pattern is shown in figure 1. The transmission electron microscope photograph is shown in figure 2, wherein the synthesized sample is mostly ultra-fine monodisperse nano Ag powder.
Example 2
Heating 10ml of oleylamine, 1ml of oleic acid, 1ml of sodium oleate and 10ml of octadecene to 200 ℃, adding 1.36g of silver nitrate into the mixture, reacting for 20 minutes, pouring out the oleylamine and the like, washing the obtained precipitate with ethanol, and drying at 40 ℃ for 20 minutes to obtain the superfine monodisperse nano Ag. The obtained products are characterized by XRD and a transmission electron microscope, as shown in figure 3, wherein the synthesized samples are mostly ultrafine monodisperse nano Ag powder.
Example 3
Heating 10ml of octadecylamine, 5ml of sodium oleate and 10ml of octadecene to 180 ℃, adding silver nitrate with the mass of 2.72g into the mixture to react for 50 minutes, pouring out the mixed solvent of the octadecylamine and the sodium oleate, washing the obtained precipitate with ethanol, and drying at 40 ℃ for 40 minutes to obtain the superfine monodisperse nano Ag. The resulting products were characterized by XRD and transmission electron microscopy. As shown in fig. 4, most of the synthesized samples were ultra-fine monodisperse nano Ag powder.
Example 4
20ml of oleylamine and 10ml of sodium oleate are heated to 190 ℃, 5.64g of silver nitrate is added into the mixture to react for 60 minutes, the obtained precipitate is washed by ethanol after the mixed solvent of the oleylamine and the sodium oleate is poured out, and the precipitate is dried for 20 minutes at 40 ℃ to obtain the superfine monodisperse nano Ag. The resulting products were characterized by XRD and transmission electron microscopy. As shown in FIG. 5, the synthesized sample is mostly ultra-fine monodisperse nano Ag powder.
Example 5
Heating 10ml of oleylamine, 2ml of oleic acid and 2ml of sodium oleate to 190 ℃, adding 1.04g of silver nitrate into the mixture to react for 40 minutes, pouring out the mixed solvent of the oleylamine and the oleic acid, washing the obtained precipitate with ethanol, and drying the precipitate at 40 ℃ for 50 minutes to obtain the superfine monodisperse nano Ag. The resulting products were characterized by XRD and transmission electron microscopy. As shown in FIG. 6, most of the synthesized samples were ultra-fine monodisperse nano Ag powder.
Example 6
Heating 10ml of octadecylamine, 2ml of sodium oleate and 5ml of octadecene to 190 ℃, adding silver nitrate with the mass of 2.76g into the mixture, reacting for 30 minutes, pouring out the octadecylamine, washing the obtained precipitate with ethanol, and drying at 40 ℃ for 60 minutes to obtain the superfine monodisperse nano Ag. The resulting products were characterized by XRD and transmission electron microscopy. As shown in FIG. 7, most of the synthesized samples were ultra-fine monodisperse nano Ag powder.
Comparative example 1
Heating 10ml of oleylamine, 2ml of oleic acid and 10ml of octadecene to 200 ℃, adding 1.36g of silver nitrate into the mixture, reacting for 20 minutes, pouring out the oleylamine and the like, washing the obtained precipitate with ethanol, and drying at 40 ℃ for 20 minutes to obtain the superfine monodisperse nano Ag. The resulting products were characterized by XRD and transmission electron microscopy. As shown in FIG. 8, the silver nanoparticles in the TEM image of the synthesized sample have a size of 2-10 nm, and have the phenomena of uneven particle distribution and particle agglomeration, wherein about 30% of the nano Ag particles have a size exceeding 8nm.
Comparative example 2
20ml of oleylamine and 10ml of oleic acid are heated to 190 ℃, silver nitrate with the mass of 5.64g is added into the oleylamine and the oleic acid to react for 60 minutes, the obtained precipitate is washed by ethanol after the mixed solvent of the oleylamine and the oleic acid is poured out, and the precipitate is dried at 40 ℃ for 20 minutes, so that the superfine monodisperse nano Ag can be obtained. The resulting products were characterized by XRD and transmission electron microscopy. As shown in FIG. 9, the silver nanoparticles in the TEM image of the synthesized sample have the size of 2-10 nm, and have the phenomena of uneven particle distribution and particle agglomeration, and the Ag nanoparticles exceeding 8nm account for a larger proportion.
In conclusion, the method provided by the invention forms the superfine monodisperse nano Ag with good crystallization, controllable composition, structure, morphology and size and particle size smaller than 5nm. The method has the advantages of low cost and easy acquisition of raw materials, less reaction time consumption, simple operation, good process repeatability, stable product quality and safe and reliable operation, and is suitable for industrial scale-up production.
The foregoing describes specific embodiments of the present invention. It is to be understood that the invention is not limited to the particular embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the claims without affecting the spirit of the invention.
Claims (8)
1. The synthesis method of the superfine monodisperse nano Ag particles is characterized by comprising the following steps of:
s1, adding a long-chain fatty acid sodium additive into a long-chain amine solvent, and then adding silver metal salt; the long-chain amine solvent adopts one or more mixed solvents of oleylamine, octadecylamine, hexadecylamine and tetramine; the long-chain fatty acid sodium additive is sodium oleate, sodium linoleate or sodium stearate;
s2, the reaction temperature is 160-200 ° C, the reaction time is 20-60 minutes;
and S3, washing the obtained product with ethanol, and drying to directly obtain the superfine monodisperse nano Ag particles.
2. The method for synthesizing ultrafine monodisperse nano Ag particles according to claim 1, wherein in the step S1, the mass concentration of the silver metal salt is 0.002-0.2 g/ml of solvent.
3. The method for synthesizing the ultra-fine monodisperse nano-Ag particles according to claim 1, wherein the silver metal salt is silver nitrate, silver sulfate, silver acetate or silver chloride.
4. The method for synthesizing ultrafine monodisperse nano-Ag particles according to claim 1, wherein in step S1, the molar ratio of the long-chain amine solvent to the long-chain fatty acid sodium additive is 1-15:1.
5. According to claim 1The synthesis method of the superfine monodisperse nano Ag particles is characterized in that in the step S3, the drying temperature is 40-80 DEG ° And C, the time is 20-40 minutes.
6. The method for synthesizing ultrafine monodisperse nano Ag particles according to claim 1, wherein in the step S1, octadecene is further added into the solvent, and the molar ratio of the long-chain amine to the octadecene is 0.5-10:1.
7. The method for synthesizing ultrafine monodisperse nano-Ag particles according to claim 1, wherein oleic acid is further added to the solvent in step S1.
8. The method for synthesizing ultrafine monodisperse nano-Ag particles according to claim 7, wherein the molar ratio of oleic acid to long-chain fatty acid sodium additive is 0.1 to 10:1.
Priority Applications (1)
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