CN111922358B - Method for synthesizing nano silver with controllable morphology by reduction at normal temperature - Google Patents
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Abstract
The invention provides a method for synthesizing nano silver with controllable morphology by reduction at normal temperature, which takes silver nitrate solution as a precursor, polyvinylpyrrolidone (PVP) as a protective agent and sodium borohydride solution as a reducing agent, and synthesizes cubic and lamellar nano silver by adding different etchants and controlling different reaction conditions at normal temperature; meanwhile, the prepared cubic nano silver is used as a precursor, a sodium citrate solution is used as an etching agent, and a sodium borohydride solution is used as a reducing agent to prepare the rod-shaped nano silver. The invention provides a method for synthesizing nano silver with controllable morphology at normal temperature, which can generate nano silver with high dispersibility and controllable morphology under normal temperature by using a reducing agent.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a method for synthesizing nano silver with controllable morphology by reduction at normal temperature.
Background
The nano silver is a metal silver simple substance with the particle size of nano level, the particle size is about 25 nanometers, and the nano silver has strong inhibition and killing effects on dozens of pathogenic microorganisms such as escherichia coli, gonococcus, trachoma chlamydia and the like. At present, the gradual miniaturization and the complicating of nano devices put higher demands on the diversification of the morphology of nano materials. The properties of metallic nanomaterials are largely dependent on the shape, size, composition, crystallinity and structure of the particles, and therefore multi-morphology controlled synthesis studies of metallic nanomaterials are important for nanomaterial preparation. Nano silver is an emerging functional material, and can be divided into one-dimensional, two-dimensional and three-dimensional nano silver particles according to the dimension of the particles. The one-dimensional nano silver mainly comprises nano rods, nano wires, nano tubes, nano chains and the like, is focused on the aspects of nano device design and application due to the unique quantum transmission effect, and has important application in nano photoelectric devices and biological optics.
There are many methods for preparing nano silver, among which the chemical reduction method has simple preparation process and low energy consumption, and is favored by most scientific researchers. There are many kinds of reducing agents for preparing nano silver, such as sodium borohydride, ethylene glycol, hydrazine hydrate, ascorbic acid, etc., but most researchers for synthesizing nano silver with different morphologies use ethylene glycol as a reducing agent, and the preparation of nano silver by using ethylene glycol requires that ethylene glycol reacts with silver precursor in an oil bath at about 140 ℃ and consumes more energy. And it is difficult to prepare nano silver particles with different morphologies at normal temperature by using the same reducing agent.
Disclosure of Invention
Aiming at the problems of high requirement on the conditions of the reducing agent used for preparing the nano silver in different forms, poor dispersibility of the generated nano silver and the like, the invention provides a method for synthesizing the nano silver with controllable morphology at normal temperature, the used reducing agent can generate the nano silver with high dispersibility and controllable morphology under the normal temperature condition, and the method can effectively improve the synthesis rate and quality of the nano silver and greatly reduce the required experimental conditions.
In order to achieve the above purpose, the invention adopts the following technical scheme: the method takes silver nitrate solution as a precursor, polyvinylpyrrolidone (PVP) as a protective agent and sodium borohydride solution as a reducing agent, and synthesizes the nano silver with controllable morphology by adding different etchants and controlling different reaction conditions at room temperature;
s1, preparing cubic nano silver: taking 0.1-0.5 mol/L silver nitrate solution as a precursor, 0.001-0.0035 mol/L polyvinylpyrrolidone (PVP) as a protective agent, and 0.025-0.125 mol/L sodium borohydride solution as a reducing agent; sodium chloride solution with the concentration of 0.01-0.1 mol/L is used as an etchant;
mixing silver nitrate solution and polyvinylpyrrolidone (PVP) solution to obtain solution A, and mixing sodium borohydride solution and sodium chloride solution to obtain solution B; firstly, stirring the solution A at a rotating speed of 100-1000 r/min, dropwise adding the solution B after 10-20 min, continuously stirring at the same stirring speed for 30-60 min after the dropwise adding, and washing and drying a separated product after the reaction is finished to obtain the cubic nano silver;
s2, preparing the flaky nano silver: taking 0.1-0.5 mol/L silver nitrate solution as a precursor, 0.001-0.0035 mol/L polyvinylpyrrolidone (PVP) as a protective agent, and 0.025-0.125 mol/L sodium borohydride solution as a reducing agent; sodium hydrosulfide solution with the concentration of 0.00035-0.001 mol/L and sodium chloride solution with the concentration of 0.01-0.1 mol/L are used as etching agents;
adding sodium borohydride solution into a reaction vessel, standing the added sodium borohydride solution for 2-10 min, continuously adding sodium chloride solution, standing for 2-5 min, adding polyvinylpyrrolidone (PVP) solution, standing and aging for 2-10 min, adding silver nitrate solution, reacting for 1-4 h, separating the product after the reaction is finished, washing, and drying to obtain the flaky nano silver.
Further, in the solution A in the step S1, the volume ratio of the silver nitrate solution to the polyvinylpyrrolidone (PVP) solution is 0.5-3:1; the volume ratio of the sodium borohydride solution to the sodium chloride solution in the solution B is 0.5-3:1, and the concentration ratio of the silver nitrate solution to the sodium borohydride solution is 1-5:1.
Further, in the step S2, when the concentration of the sodium chloride is 0.1mol/L, the obtained flaky nano silver is in a mixed morphology of triangle and hexagon, and when the concentration of the sodium chloride is 0.025mol/L, the obtained flaky nano silver is in a quadrilateral shape.
Further, the volume ratio of the silver nitrate solution, the polyvinylpyrrolidone (PVP) solution and the sodium borohydride solution in the step S2 is 1-4:1:1, and the volume ratio of the sodium bisulfide solution, the sodium chloride solution and the silver nitrate solution is 0.1-0.35:1:1.
Further, the cubic nano silver prepared in the step S1 is used as a precursor, sodium citrate solution with the concentration of 0.001-0.01 mol/L is used as an etching agent, and sodium borohydride solution with the concentration of 0.025-0.1 mol/L is used as a reducing agent to prepare the rod-shaped nano silver.
Further, the specific method for preparing the rod-shaped nano silver comprises the following steps: preparing a cubic nano silver solution with the concentration of 0.010-0.020 mol/L, placing the cubic nano silver solution into a reaction container, then adding a sodium citrate solution and a sodium borohydride solution to react for 30-60 min, and washing and drying a separated product to obtain the rod-shaped nano silver; wherein the volume ratio of the sodium citrate solution to the sodium borohydride is 10-40:1, and the volume ratio of the cubic nano silver solution to the sodium borohydride solution is 8-20: 1.
further, after the reaction is finished, the required nano silver can be obtained by centrifuging at the speed of 6000-10000 r/min for 10-15 min.
The silver nitrate solution, the polyvinylpyrrolidone solution, the sodium borohydride solution, the sodium chloride solution, the sodium hydrosulfide solution and the sodium citrate solution are prepared by taking water as a solvent.
Compared with the prior art, the invention has the advantages that:
1. the three nano silver particles with different morphologies are prepared from the same precursor, a reducing agent and a protective agent, and the experimental conditions are simpler;
2. the nano silver particles prepared by the invention have higher dispersivity and stability, and can be stored for a longer time at room temperature.
Drawings
FIG. 1 is a graph of the morphology of cubic nanosilver prepared in example 1 of the present invention;
FIG. 2 is a graph of the morphology of the rod-shaped nano silver prepared in example 1 of the present invention;
FIG. 3 is a morphology graph of the platy nano-silver prepared in example 2 of the present invention;
fig. 4a and 4b are morphology diagrams of the flake nano silver prepared in example 4 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
The method for synthesizing the nano silver with controllable morphology by reduction at normal temperature comprises the following steps:
s1, preparation method of cubic nano silver
Mixing 5ml of silver nitrate solution with the concentration of 0.1mol/L and 10ml of PVP solution with the concentration of 0.001mol/L, placing in a 100ml beaker, stirring for 10min under the magnetic stirring of 100r/min, dropwise adding the mixed solution (mixing 5ml of sodium borohydride solution with the concentration of 0.025mol/L and 10ml of sodium chloride solution with the concentration of 0.01 mol/L), keeping the stirring speed at the same stirring speed for 30min after the dropwise addition is completed, centrifuging for 15min at the speed of 6000r/min after the reaction is completed, pouring out supernatant, adding deionized water into the precipitate, continuing centrifuging, and repeating for three times. And washing and drying the separated product to obtain the cubic nano silver, wherein the morphology of the prepared cubic nano silver is shown in figure 1.
S2, preparation method of rod-shaped nano silver
Preparing a precursor solution with the concentration of 0.010mol/L and a sodium borohydride solution with the concentration of 0.025mol/L as a reducing agent and a sodium citrate solution with the concentration of 0.001mol/L as an etching agent by taking the prepared cubic nano silver as a precursor, placing 20ml of the precursor solution in a 100ml beaker, directly adding 40ml of the sodium citrate solution and 1ml of the sodium borohydride solution into the beaker, and reacting for 30min; after the reaction is completed, centrifuging at 6000r/min for 15min, pouring out the supernatant, adding deionized water into the precipitate, continuing centrifuging, and repeating for three times. And after the reaction is finished, separating a product, washing and drying to obtain the rod-shaped nano silver, wherein the morphology of the rod-shaped nano silver is shown in figure 2.
S3, preparation method of flaky nano silver
Sequentially adding 10ml of sodium borohydride solution with the concentration of 0.025mol/L, adding 1ml of sodium bisulfide solution with the concentration of 0.00035mol/L, standing for 2min, adding 10ml of sodium chloride solution with the concentration of 0.01mol/L, standing for 2min, adding 10ml of PVP solution with the concentration of 0.001mol/L, standing for 2min, aging, adding 10ml of silver nitrate solution with the concentration of 0.1mol/L, reacting for 1h, centrifuging at 6000r/min for 15min after the reaction is finished, pouring out supernatant, adding deionized water into the precipitate, continuing centrifuging, and repeating for three times.
Example 2
The method for synthesizing the nano silver with controllable morphology by reduction at normal temperature comprises the following steps:
s1, preparation method of cubic nano silver
10ml of silver nitrate solution with the concentration of 0.2mol/L and 10ml of PVP solution with the concentration of 0.0018mol/L are mixed, placed in a 100ml beaker, stirred for 15min under magnetic stirring of 500r/min, then the mixed solution (10 ml of sodium borohydride solution with the concentration of 0.05mol/L and 10ml of sodium chloride solution with the concentration of 0.02mol/L are mixed) is added dropwise, and after the dropwise addition is completed, the stirring reaction is continued for 45min at the same stirring speed. After the reaction is completed, centrifuging for 12min at 8000r/min, pouring out the supernatant, adding deionized water into the precipitate, continuing centrifuging, and repeating for three times.
S2, preparation method of rod-shaped nano silver
Preparing a precursor solution with the concentration of 0.012mol/L by taking the prepared cubic nano silver as a precursor, taking a sodium borohydride solution with the concentration of 0.05mol/L as a reducing agent and a sodium citrate solution with the concentration of 0.002mol/L as an etching agent, placing 16ml of the precursor solution into a 100ml beaker, directly adding 30ml of the sodium citrate solution and 1ml of the sodium borohydride solution into the beaker, reacting for 45min, centrifuging for 12min at 8000r/min after the reaction is finished, pouring out supernatant, adding deionized water into precipitate, continuing centrifuging, and repeating for three times.
S3, preparation method of flaky nano silver
Adding 5ml of sodium borohydride solution with the concentration of 0.05mol/L, adding 2ml of sodium bisulfide solution with the concentration of 0.0005mol/L, standing for 4min, adding 10ml of sodium chloride solution with the concentration of 0.025mol/L, standing for 3min, adding 5ml of PVP solution with the concentration of 0.0018mol/L, standing for 4min, adding 10ml of silver nitrate solution with the concentration of 0.2mol/L, and reacting for 2h. After the reaction is completed, centrifuging for 12min at 8000r/min, pouring out the supernatant, adding deionized water into the precipitate, continuing centrifuging, and repeating for three times. And after the reaction is finished, separating the product, washing and drying to obtain the flaky nano silver, wherein the appearance of the prepared flaky nano silver is quadrilateral, as shown in figure 3.
Example 3
The method for synthesizing the nano silver with controllable morphology by reduction at normal temperature comprises the following steps:
s1, preparation method of cubic nano silver
10ml of silver nitrate solution with the concentration of 0.3mol/L and 5ml of PVP solution with the concentration of 0.0026mol/L are mixed, placed in a 100ml beaker, stirred for 18min under magnetic stirring of 1000r/min, then the mixed solution (10 ml of mixed solution of sodium borohydride solution with the concentration of 0.075mol/L and sodium chloride solution with the concentration of 0.05 mol/L) is added dropwise, and after the dropwise addition is completed, the stirring reaction is continued for 50min at the same stirring speed. After the reaction is completed, centrifuging for 10min at 10000r/min, pouring out supernatant, adding deionized water into the precipitate, continuing centrifuging, and repeating for three times.
S2, preparation method of rod-shaped nano silver
Preparing a precursor solution with the concentration of 0.015mol/L by taking the prepared cubic nano silver as a precursor, taking a sodium borohydride solution with the concentration of 0.075mol/L as a reducing agent, taking a sodium citrate solution with the concentration of 0.005mol/L as an etching agent, placing 12ml of the precursor solution in a 100ml beaker, directly adding 20ml of the sodium citrate solution and 1ml of the sodium borohydride solution into the beaker, and reacting for 50min. After the reaction is completed, centrifuging for 10min at 10000r/min, pouring out supernatant, adding deionized water into the precipitate, continuing centrifuging, and repeating for three times.
S3, preparation method of flaky nano silver
Adding 5ml of sodium borohydride solution with the concentration of 0.075mol/L, adding 4.5ml of sodium hydrosulfide solution with the concentration of 0.0008mol/L, standing for 8min, adding 15ml of NaCl solution with the concentration of 0.05mol/L, standing for 4min, adding 5ml of PVP solution with the concentration of 0.0026mol/L, standing for 8min, aging, adding 15ml of silver nitrate solution with the concentration of 0.3mol/L, and reacting for 3h. After the reaction is completed, centrifuging for 10min at 10000r/min, pouring out supernatant, adding deionized water into the precipitate, continuing centrifuging, and repeating for three times.
Example 4
S1, preparation method of cubic nano silver
15ml of silver nitrate solution with the concentration of 0.5mol/L and 5ml of PVP solution with the concentration of 0.0035mol/L are mixed, placed in a 100ml beaker, stirred for 20min under magnetic stirring of 1000r/min, then the mixed solution (the mixed solution of 15ml of sodium borohydride solution with the concentration of 0.125mol/L and 5ml of sodium chloride solution with the concentration of 0.1 mol/L) is added dropwise, and after the dropwise addition is completed, the stirring reaction is continued for 60min at the same stirring speed. After the reaction is completed, centrifuging for 10min at 10000r/min, pouring out supernatant, adding deionized water into the precipitate, continuing centrifuging, and repeating for three times.
S2, preparation method of rod-shaped nano silver
Preparing a precursor solution with the concentration of 0.020mol/L by taking the prepared cubic nano silver as a precursor, taking a sodium borohydride solution with the concentration of 0.1mol/L as a reducing agent, taking a sodium citrate solution with the concentration of 0.01mol/L as an etching agent, placing 8ml of the precursor solution into a 100ml beaker, directly adding 10ml of the sodium citrate solution and 1ml of the sodium borohydride solution into the beaker, and standing for reaction for 60min. After the reaction is completed, centrifuging for 10min at 10000r/min, pouring out supernatant, adding deionized water into the precipitate, continuing centrifuging, and repeating for three times.
S3, preparation method of flaky nano silver
Adding 5ml of sodium borohydride solution with the concentration of 0.125mol/L, adding 7ml of sodium bisulfide solution with the concentration of 0.001mol/L, standing for 10min, adding 20ml of NaCl solution with the concentration of 0.1mol/L, standing for 5min, adding 5ml of PVP solution with the concentration of 0.0035mol/L, standing for 10min, aging, adding 20ml of silver nitrate solution with the concentration of 0.5mol/L, and reacting for 4h. After the reaction is completed, centrifuging for 10min at 10000r/min, pouring out supernatant, adding deionized water into the precipitate, continuing centrifuging, and repeating for three times. And after the reaction is finished, separating the product, washing and drying to obtain the flaky nano silver, wherein the appearance of the flaky nano silver is triangular and hexagonal, as shown in fig. 4, wherein the 4a graph is a triangular nano silver sheet, and the 4b graph is a hexagonal nano silver sheet.
The technical scheme of the invention is explained in the technical scheme, the protection scope of the invention cannot be limited by the technical scheme, and any changes and modifications to the technical scheme according to the technical substance of the invention belong to the protection scope of the technical scheme of the invention.
Claims (5)
1. A method for synthesizing nano silver with controllable morphology by reduction at normal temperature is characterized in that: according to the method, silver nitrate solution is used as a precursor, polyvinylpyrrolidone (PVP) is used as a protective agent, sodium borohydride solution is used as a reducing agent, and at normal temperature, different etchants are added and different reaction conditions are controlled to synthesize the nano silver with controllable morphology;
s1, preparing cubic nano silver: taking 0.1-0.5 mol/L silver nitrate solution as a precursor, 0.001-0.0035 mol/L polyvinylpyrrolidone as a protective agent, and 0.025-0.125 mol/L sodium borohydride solution as a reducing agent; sodium chloride solution with the concentration of 0.01-0.1 mol/L is used as an etchant;
mixing a silver nitrate solution and a polyvinylpyrrolidone solution to obtain a solution A, and mixing a sodium borohydride solution and a sodium chloride solution to obtain a solution B; firstly, stirring the solution A at a rotating speed of 100-1000 r/min, dropwise adding the solution B after 10-20 min, continuously stirring at the same stirring speed for 30-60 min after the dropwise adding, and washing and drying a separated product after the reaction is finished to obtain the cubic nano silver;
the cubic nano silver prepared in the step S1 is used as a precursor, sodium citrate solution with the concentration of 0.001-0.01 mol/L is used as an etching agent, and sodium borohydride solution with the concentration of 0.025-0.1 mol/L is used as a reducing agent to prepare rod-shaped nano silver; the specific method comprises the following steps: preparing a cubic nano silver solution with the concentration of 0.010-0.020 mol/L, placing the cubic nano silver solution into a reaction container, then adding a sodium citrate solution and a sodium borohydride solution to react for 30-60 min, and washing and drying a separated product to obtain the rod-shaped nano silver; wherein the volume ratio of the sodium citrate solution to the sodium borohydride is 10-40:1, and the volume ratio of the cubic nano silver solution to the sodium borohydride solution is 8-20: 1, a step of;
s2, preparing the flaky nano silver: taking 0.1-0.5 mol/L silver nitrate solution as a precursor, 0.001-0.0035 mol/L polyvinylpyrrolidone as a protective agent, and 0.025-0.125 mol/L sodium borohydride solution as a reducing agent; sodium hydrosulfide solution with the concentration of 0.00035-0.001 mol/L and sodium chloride solution with the concentration of 0.01-0.1 mol/L are used as etching agents;
adding sodium borohydride solution into a reaction vessel, standing the added sodium borohydride solution for 2-10 min, continuously adding sodium chloride solution, standing for 2-5 min, adding polyvinylpyrrolidone solution, standing for 2-10 min, adding silver nitrate solution, reacting for 1-4 h, separating the product after the reaction is finished, washing, and drying to obtain the flaky nano silver.
2. The method for synthesizing the nano silver with controllable morphology by reduction at normal temperature according to claim 1, which is characterized in that: the volume ratio of the silver nitrate solution to the polyvinylpyrrolidone solution in the solution A in the step S1 is 0.5-3:1; the volume ratio of the sodium borohydride solution to the sodium chloride solution in the solution B is 0.5-3:1, and the concentration ratio of the silver nitrate solution to the sodium borohydride solution is 1-5:1.
3. The method for synthesizing the nano silver with controllable morphology by reduction at normal temperature according to claim 1, which is characterized in that: in the step S2, when the concentration of the sodium chloride is 0.1mol/L, the obtained flaky nano silver with a mixed morphology of triangle and hexagon, and when the concentration of the sodium chloride is 0.025mol/L, the obtained flaky nano silver with a quadrilateral shape.
4. The method for synthesizing the nano silver with controllable morphology by reduction at normal temperature according to claim 1, which is characterized in that: the volume ratio of the silver nitrate solution, the polyvinylpyrrolidone solution and the sodium borohydride solution in the step S2 is 1-4:1:1, and the volume ratio of the sodium bisulfide solution, the sodium chloride solution and the silver nitrate solution is 0.1-0.35:1:1.
5. The method for synthesizing the nano silver with controllable morphology by reduction at normal temperature according to any one of claims 1 to 4, which is characterized in that: after the reaction is finished, the required nano silver can be obtained by centrifugation at the speed of 6000-10000 r/min for 10-15 min.
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