CN116060631A - Method for simply preparing silver-copper bimetallic nano-particles - Google Patents
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- NEIHULKJZQTQKJ-UHFFFAOYSA-N [Cu].[Ag] Chemical compound [Cu].[Ag] NEIHULKJZQTQKJ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 36
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 150000001879 copper Chemical class 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 15
- 238000006722 reduction reaction Methods 0.000 claims abstract description 15
- 239000010949 copper Substances 0.000 claims abstract description 14
- 229910052802 copper Inorganic materials 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 10
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052709 silver Inorganic materials 0.000 claims abstract description 4
- 239000004332 silver Substances 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 11
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- 235000006708 antioxidants Nutrition 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 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 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 4
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 claims description 4
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 4
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 4
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 4
- 229940071536 silver acetate Drugs 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 3
- QJAOYSPHSNGHNC-UHFFFAOYSA-N octadecane-1-thiol Chemical compound CCCCCCCCCCCCCCCCCCS QJAOYSPHSNGHNC-UHFFFAOYSA-N 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
- 108010010803 Gelatin Proteins 0.000 claims description 2
- 229920000159 gelatin Polymers 0.000 claims description 2
- 239000008273 gelatin Substances 0.000 claims description 2
- 235000019322 gelatine Nutrition 0.000 claims description 2
- 235000011852 gelatine desserts Nutrition 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 13
- 239000002245 particle Substances 0.000 abstract description 12
- 238000002360 preparation method Methods 0.000 abstract description 11
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 13
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 239000002216 antistatic agent Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 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
- B22F1/0545—Dispersions or suspensions of 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
Abstract
The invention discloses a preparation method of silver-copper bimetallic nanoparticles, and belongs to the field of nano material preparation. The method comprises the steps of adding soluble copper salt and silver salt into a solvent according to the mol ratio of the soluble silver salt to the soluble copper salt of 1 (2-4), and marking the generated solution as A solution; adding a reducing agent, a dispersing agent and an antioxidant into another solvent, and marking as a solution B; continuously stirring the solution A in a water bath constant temperature magnetic stirrer, heating to a certain temperature, and then dropwise adding the solution B; the reduction reaction of silver and copper is continued, and the mixed solution becomes dark color; heating the suspension in the same water bath constant temperature magnetic stirrer under the condition of continuous stirring, and obtaining a final suspension after reaction; and filtering and cleaning the suspension, and centrifugally drying to obtain the silver-copper bimetallic nano particles. The nano silver copper particles prepared by the method are smaller, the yield is higher, the reducing agent, the dispersing agent and the antioxidant are fewer, and the cost for preparing the nano silver copper is strictly controlled.
Description
Technical Field
The invention relates to a method for simply preparing silver-copper bimetallic nano-particles, and belongs to the technical field of nano-material preparation.
Background
As an emerging functional material, the nano silver copper has unique physical and chemical properties, and can be applied to optical materials, catalyst materials, antibacterial materials, biosensor materials, coatings, battery electrode materials, antistatic materials, low-temperature superconducting materials and the like; therefore, there is increasing attention; the performance and application of nano silver copper mainly depend on the particle size, morphology and stability of the nano silver copper. Thus, the precisely controllable preparation of nano silver copper is one of the hot spots of the current nano material research.
Currently, the methods for preparing the nano silver copper powder include a substitution reaction method, a melting atomization method and a liquid phase reduction method. Liquid phase reduction methods include chemical reduction methods and co-precipitation methods; the literature shows that the most common method for preparing bimetallic nanoparticles is still a chemical reduction method, and the soluble salts of silver and copper are reduced in a solution system mainly by virtue of the action of a reducing agent. In order to control particle size and particle-to-particle dispersibility, a certain amount of polymeric dispersants such as Sodium Dodecyl Sulfate (SDS), polyvinylpyrrolidone (PVP), etc. are usually added to the whole reduction system. In the process of synthesizing nano silver copper, silver copper nano particles tend to be easily oxidized, which is also one of factors limiting the mass production of silver copper bimetallic nano materials.
Thus, the invention mainly focuses on developing a simple method for preparing silver-copper bimetallic nanomaterials. The method used in the invention is a chemical reduction method, and can reduce silver-copper bimetallic nano particles in one step. The equipment is very simple, and the prepared silver-copper bimetallic nano-particles have smaller particle size, more uniform particles, higher yield and lower cost.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a simple method for preparing silver-copper bimetallic nanoparticles; preparing a nano silver-copper material by a chemical reduction method; the method has the advantages of low cost of raw materials, simple technological operation, safe experimental process and short preparation period, and the prepared nano silver-copper particles are relatively stable.
A method for simply preparing silver-copper bimetallic nano-particles comprises the following specific steps:
(1) The soluble copper salt and the silver salt are added into the solvent according to the mol ratio of the soluble silver salt to the soluble copper salt of 1 (2-4), and ultrasonic vibration treatment (complete dissolution of the salt, generally preferred 40 min) is carried out on the solvent containing the soluble copper salt and the silver salt by using an ultrasonic oscillator, and the resultant solution is marked as A solution.
(2) The reducing agent, dispersant and antioxidant are added to another solvent, and subjected to ultrasonic treatment (complete dissolution of each raw material, generally preferably 60 to 80 minutes) using an ultrasonic oscillator, labeled as solution B.
(3) Continuously stirring the solution A in a water bath constant temperature magnetic stirrer, heating to a certain temperature, and then dropwise adding the solution B; the reduction of silver copper proceeds and the mixed solution turns dark.
(4) And (3) heating the suspension obtained in the step (3) in the same water bath constant temperature magnetic stirrer for a certain time under the condition of continuous stirring, and reacting to obtain the final suspension.
(5) And (3) centrifugally drying the suspension obtained in the step (4) under a certain condition to finally obtain the silver-copper bimetallic nano particles.
Preferably, the soluble copper salt in step (1) of the present invention is one or more of copper sulfate pentahydrate and copper nitrate trihydrate; the soluble silver salt is one or more of silver nitrate and silver acetate, and the molar ratio of the soluble silver salt to the soluble copper salt is 1 (2-4).
Preferably, the solvent in the step (1) of the present invention is selected from one of glycol, ammonium hydroxide and ethylene glycol.
Preferably, in the step (2) of the invention, the reducing agent is one of sodium dihydrogen phosphate, ascorbic acid, hydrazine hydrate and formaldehyde, and the molar ratio of the reducing agent to the soluble silver salt is 1:1-3:1.
Preferably, in the step (2) of the present invention, the dispersing agent is one of Sodium Dodecyl Sulfate (SDS), polyvinylpyrrolidone (PVP), cetyltrimethylammonium bromide (CTAB) and gelatin, and the molar ratio of the dispersing agent to the soluble silver salt is 0.2:1-0.4:1.
Preferably, in the step (2) of the invention, the antioxidant is isopropanol or octadecanethiol, and the molar ratio of the antioxidant to the soluble silver salt is 0.1:1-0.3:1.
Preferably, in the step (3) of the present invention, the stirring speed is 400 to 800rpm; the heating temperature is 60-80 ℃ and the heating time is 50-90 min.
Preferably, the heating temperature in the step (4) is 60-80 ℃ and the heating time is 1-3 h.
Preferably, certain conditions in step (5) of the present invention are: the precipitation cleaning mode is that water and absolute ethyl alcohol are alternately cleaned for three times in equal quantity; the drying time is 16-24 h.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, by adding different reducing agents, dispersing agents and antioxidants and adopting a one-step reduction method, the nano silver-copper particles are prepared, and the preparation method has the advantages of simple process operation, short preparation period and the like.
(2) According to the invention, the reducing agent, the dispersing agent and the antioxidant are bonded on the surface of the silver copper to form the coating layer, so that the contact between air and the silver copper is prevented, the oxidation of the silver copper is effectively avoided, and the nano silver copper bimetallic particles can be prepared in the air.
(3) The silver-copper bimetallic nanoparticle material prepared by the invention can be applied to optical materials, catalyst materials, antibacterial materials, biosensor materials, coatings, battery electrode materials, antistatic materials, low-temperature superconducting materials and the like.
Drawings
FIG. 1 is an X-ray diffraction pattern of example 1 for preparing silver-copper bimetallic nanoparticles.
Fig. 2 is an X-ray diffraction pattern of example 2 for preparing silver-copper bimetallic nanoparticles.
Fig. 3 is a transmission electron microscope image of the silver-copper bimetallic nanoparticle prepared in example 1.
Fig. 4 is a transmission electron microscope image of the silver-copper bimetallic nanoparticle prepared in example 2.
Fig. 5 is an X-ray diffraction pattern of example 3 for preparing silver-copper bimetallic nanoparticles.
Fig. 6 is an X-ray diffraction pattern of example 4 for preparing silver-copper bimetallic nanoparticles.
Detailed Description
The present invention is a method for preparing silver-copper bimetallic nanoparticles, which is further described below with reference to the specific embodiments, but the scope of the present invention is not limited to the above.
The drugs used in the examples of the present invention were all commercially available analytically pure products and were not further purified.
Example 1
The preparation method of the silver-copper bimetallic nano-particle comprises the following specific steps:
1mmol of soluble copper salt (copper sulfate pentahydrate) and 2mmol of soluble silver salt (silver nitrate) are added into 60mL of ethylene glycol solvent, ultrasonic oscillation treatment is carried out on the solvent containing the soluble copper salt and the silver salt for 40min by using an ultrasonic oscillator, and the generated solution is marked as A solution;
1mmol of sodium dihydrogen phosphate, 0.2mmol of SDS and 0.1mmol of isopropanol are added into 30mL of ethylene glycol solvent, and ultrasonic treatment is carried out for 70min by using an ultrasonic oscillator to mark as solution B;
continuously stirring the solution A in a water bath constant temperature magnetic stirrer at a speed of 400rpm, heating to 60 ℃, and then dropwise adding the solution B; the reduction reaction of silver and copper is continued, and the mixed solution becomes dark color; obtaining a final suspension after reacting for 1 h; and (3) alternately cleaning the obtained suspension with water and absolute ethyl alcohol for three times in equal quantity, and drying for 16-24 hours to finally obtain the silver-copper bimetallic nano particles.
Example 2
The preparation method of the silver-copper bimetallic nano-particle comprises the following specific steps:
1mmol of a soluble copper salt (copper nitrate trihydrate) and 2mmol of a soluble silver salt (silver acetate) were added to 60mL of an ethylene glycol solvent, and the solvent containing the soluble copper salt and the silver salt was subjected to ultrasonic vibration treatment using an ultrasonic vibrator for 40 minutes, and the resultant solution was labeled as solution A.
1mmol of sodium dihydrogen phosphate, 0.2mmol of PVP and 0.1mmol of isopropanol were added to 30mL of ethylene glycol solvent, and the mixture was sonicated using a sonicator for 70min to obtain a solution B.
Continuously stirring the solution A in a water bath constant temperature magnetic stirrer at a speed of 400rpm, heating to 60 ℃, and then dropwise adding the solution B; the reduction of silver copper proceeds and the mixed solution turns dark. Obtaining a final suspension after reacting for 1 h; and (3) alternately cleaning the obtained suspension with water and absolute ethyl alcohol for three times in equal quantity, and drying for 16-24 hours to finally obtain the silver-copper bimetallic nano particles.
The XRD patterns of the silver-copper bimetallic nanoparticles of examples 1 and 2 are shown in FIGS. 1 and 2, and it is known from the patterns that the diffraction angles of Cu are 43.3 DEG, 50.4 DEG and 74.1 DEG, which correspond to the (111), (200) and (220) crystal planes of PDF#04-0836 standard cards, respectively; diffraction angles of Ag are 38.1 degrees, 44.3 degrees, 64.4 degrees, 77.4 degrees and 81.6 degrees, and correspond to (111), (200), (220), (311) and (222) crystal faces of PDF#04-0783 standard cards respectively. The prepared substance is nano silver copper particles.
TEM images of the silver-copper bimetallic nanoparticles prepared in examples 1 and 2 are shown in FIG. 3 and FIG. 4, and it is clear from the figures that the use of different dispersants has a large influence on the morphology and dispersibility of the silver-copper nanoparticles. SDS belongs to a sulfate dispersant, forms a micelle at a certain concentration, forms an adsorption film on the surface of the nano particle to wrap the nano particle, and disperses the nano particle through space repulsive force; PVP has high molecular water solubility, strong film forming property and dispersibility, and can prevent small particles from mutually aggregating to form a precipitate; the nanometer particles prepared by PVP have better dispersivity, the PVP is only 0.2mmol, and the cost is lower.
Example 3
The preparation method of the silver-copper bimetallic nano-particle comprises the following specific steps:
(1) 1mmol of soluble copper salt (copper sulfate pentahydrate) and 3mmol of soluble silver salt (silver acetate) were added to 60mL of ammonium hydroxide solvent, and the solvent containing the soluble copper salt and silver salt was subjected to ultrasonic vibration treatment using an ultrasonic vibrator for 40 minutes, and the resultant solution was labeled as solution A.
(2) 2mmol of ascorbic acid, 0.3mmol of cetyltrimethylammonium bromide and 0.2mmol of isopropyl alcohol were added to 30mL of ethylene glycol solvent, and sonicated using a sonicator for 70min to mark as solution B.
(3) Continuously stirring the solution A in a water bath constant temperature magnetic stirrer at a speed of 600rpm, heating to 70 ℃, and then dropwise adding the solution B; the reduction of silver copper proceeds and the mixed solution turns dark. Obtaining a final suspension after 2h of reaction; and (3) alternately cleaning the obtained suspension with water and absolute ethyl alcohol for three times in equal quantity, and drying for 16 hours to finally obtain the silver-copper bimetallic nano particles.
The silver-copper bimetallic nanoparticle prepared in this example is shown in fig. 5, and XRD analysis results show that the prepared substance is silver-copper bimetallic nanoparticle and has high crystallinity.
Example 4
The preparation method of the silver-copper bimetallic nano-particle comprises the following specific steps:
(1) 1mmol of a soluble copper salt (copper nitrate trihydrate) and 4mmol of a soluble silver salt (silver nitrate) were added to 60mL of a glycol solvent, and the solvent containing the soluble copper salt and the silver salt was subjected to ultrasonic vibration treatment using an ultrasonic vibrator for 40 minutes, and the resultant solution was labeled as solution A.
(2) 3mmol of formaldehyde, 0.4mmol of sodium dodecyl sulfate and 0.3mmol of stearyl mercaptan are added to 30mL of ethylene glycol solvent, and the mixture is subjected to ultrasonic treatment by using an ultrasonic oscillator for 70min to obtain a solution B.
(3) The solution A was stirred continuously in a water bath thermostatted magnetic stirrer at 800rpm, heated to 80℃and then the solution B was added dropwise. The reduction of silver copper proceeds and the mixed solution turns dark. After 3h of reaction, the final suspension was obtained. And (3) alternately cleaning the obtained suspension with water and absolute ethyl alcohol for three times in equal quantity, and drying for 24 hours to finally obtain the silver-copper bimetallic nano particles.
The silver-copper bimetallic nanoparticle prepared in this example is shown in fig. 6, and XRD analysis results show that the prepared substance is silver-copper bimetallic nanoparticle and has high crystallinity.
Claims (9)
1. The method for simply preparing the silver-copper bimetallic nano-particles is characterized by comprising the following steps of:
(1) Adding soluble copper salt and silver salt into a solvent according to the mol ratio of the soluble silver salt to the soluble copper salt of 1 (2-4), and carrying out ultrasonic vibration treatment on the solvent containing the soluble copper salt and the silver salt by using an ultrasonic oscillator, wherein the generated solution is marked as A solution;
(2) Adding a reducing agent, a dispersing agent and an antioxidant into a solvent, performing ultrasonic treatment by using an ultrasonic oscillator, and marking as a solution B;
(3) Continuously stirring the solution A in a water bath constant temperature magnetic stirrer, heating to a certain temperature, and then dropwise adding the solution B; the reduction reaction of silver and copper is continued, and the mixed solution becomes dark color;
(4) Heating the suspension obtained in the step (3) in the same water bath constant temperature magnetic stirrer under the condition of continuous stirring, and reacting to obtain a final suspension;
(5) And (3) filtering and cleaning the suspension obtained in the step (4), and then centrifugally drying to finally obtain the silver-copper bimetallic nano particles.
2. The method for simply preparing silver-copper bimetallic nanoparticles according to claim 1, wherein: the soluble copper salt in the step (1) is one or more of copper sulfate pentahydrate and copper nitrate trihydrate; the soluble silver salt is one or more of silver nitrate and silver acetate.
3. The method for simply preparing silver-copper bimetallic nanoparticles according to claim 1 or 2, characterized in that: the solvent in the step (1) is selected from one of glycol, ammonium hydroxide and ethylene glycol.
4. A method for simply preparing silver-copper bimetallic nanoparticles according to claim 1, characterized in that: in the step (2), the reducing agent is one of sodium dihydrogen phosphate, ascorbic acid, hydrazine hydrate and formaldehyde, and the molar ratio of the reducing agent to the soluble silver salt is 1:1-3:1.
5. A method for simply preparing silver-copper bimetallic nanoparticles according to claim 1, characterized in that: the dispersing agent in the step (2) is one of sodium dodecyl sulfate, polyvinylpyrrolidone, cetyltrimethylammonium bromide and gelatin, and the molar ratio of the dispersing agent to the soluble silver salt is 0.2:1-0.4:1.
6. A method for simply preparing silver-copper bimetallic nanoparticles according to claim 1, characterized in that: the antioxidant in the step (2) is isopropanol or octadecanethiol, and the molar ratio of the antioxidant to the soluble silver salt is 0.1:1-0.3:1.
7. A method for simply preparing silver-copper bimetallic nanoparticles according to claim 1, characterized in that: the stirring speed in the step (3) is 400-800 rpm; the heating temperature is 60-80 ℃ and the heating time is 50-90 min.
8. A method for simply preparing silver-copper bimetallic nanoparticles according to claim 1, characterized in that: the heating temperature in the step (4) is 60-80 ℃ and the heating time is 1-3 h.
9. A method for simply preparing silver-copper bimetallic nanoparticles according to claim 1, characterized in that: in the step (5): the precipitation cleaning mode is that water and absolute ethyl alcohol are alternately cleaned for three times in equal quantity; the drying time is 16-24 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310205443.3A CN116060631A (en) | 2023-03-06 | 2023-03-06 | Method for simply preparing silver-copper bimetallic nano-particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116371421A (en) * | 2023-05-31 | 2023-07-04 | 中国农业科学院农业环境与可持续发展研究所 | Supported catalyst and preparation method and application thereof |
| CN116371421B (en) * | 2023-05-31 | 2023-08-01 | 中国农业科学院农业环境与可持续发展研究所 | Supported catalyst and preparation method and application thereof |
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