CN107812957B - Method for preparing fluorescent silver nanoparticles based on silver mirror reaction - Google Patents
Method for preparing fluorescent silver nanoparticles based on silver mirror reaction Download PDFInfo
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- CN107812957B CN107812957B CN201711012907.XA CN201711012907A CN107812957B CN 107812957 B CN107812957 B CN 107812957B CN 201711012907 A CN201711012907 A CN 201711012907A CN 107812957 B CN107812957 B CN 107812957B
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- 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
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
Abstract
The invention discloses a method for preparing fluorescent material based on silver mirror reactionA method of polishing silver nanoparticles. The method comprises the following steps: the preparation concentration is 5-25 mmol L‑1The silver ammonia solution of (a); putting bovine serum albumin solution into a beaker, adding silver ammonia solution, putting the beaker in a water bath, and standing for reaction; transferring the reacted test solution into a dialysis bag with the molecular weight cutoff of 2000, and dialyzing for 36-48 h; and (3) carrying out centrifugal separation on the dialyzed test solution, and centrifuging for 10-20 min at the rotating speed of 10000-12000 rpm to obtain the silver nanoparticle dispersion solution. According to the method, bovine serum albumin is used as a template and a reducing agent, silver ammonia is reduced in situ to prepare the silver nanoparticles based on the principle of silver mirror reaction, the reaction condition is mild, the equipment is simple, the operation is convenient and fast, no additional reducing agent is needed, the method has the advantages of being green and fast, and the prepared silver nanoparticles show fluorescence.
Description
Technical Field
The invention relates to a method for preparing fluorescent silver nanoparticles based on silver mirror reaction, and belongs to the technical field of preparation of nano materials.
Background
Silver nanoparticles are widely studied for use in the fields of chemistry, materials, environment, medicine, life sciences, etc. due to their excellent electronic, optical, catalytic, antibacterial, etc. properties. The silver nanoparticles with fluorescence characteristics have good photobleaching resistance and biocompatibility, so that the silver nanoparticles can be widely used for metal ion and biomolecule detection and imaging research. Therefore, the preparation of the silver nanoparticles with fluorescence characteristics has important significance.
Compared with the traditional physical and chemical synthesis methods, the biological template method avoids the use of complex and expensive instruments and equipment and high-energy-consumption high-temperature and high-pressure conditions, and has the advantages of environmental friendliness, low consumption and simple operation. Bovine serum albumin, as a cheap protein, is widely used in the preparation of precious metal and metal oxide nano-materials, and therefore, methods for preparing silver nano-materials based on bovine serum are widely studied, in these preparation methods, an additional reducing agent is usually introduced to assist synthesis, and although some green reducing agents are used to realize green synthesis, the search for a simple green method to prepare silver nano-particles is still a problem to be solved. At present, although there are reports of methods for preparing silver nanoparticles by using silver ammonia solution as a silver element source, there is no report of synthesizing fluorescent silver nanoparticles in one step without adding a reducing agent.
Disclosure of Invention
The invention aims to provide a method for preparing fluorescent silver nanoparticles based on silver mirror reaction, which is simple and environment-friendly.
The principle of the invention is as follows: bovine serum albumin is used as a biological template, and meanwhile, the reducibility of the bovine serum albumin is utilized, and the silver-ammonia solution is reduced in situ based on the silver mirror reaction principle under the condition of not adding a reducing agent, so that the silver nanoparticles are prepared by a one-step method.
The invention provides a method for preparing fluorescent silver nanoparticles based on silver mirror reaction, which comprises the following steps:
1) putting silver nitrate into a clean beaker, adding distilled water to completely dissolve the silver nitrate, dropwise adding concentrated ammonia water until brown yellow precipitate is generated, continuously dropwise adding concentrated ammonia water until the precipitate is completely dissolved, fixing the volume, and preparing 5-25 mmol L-1The silver ammonia solution of (a);
2) taking bovine serum albumin solution into a beaker, adding the silver ammonia solution obtained in the step 1), and placing the mixture in a position of 30-60%oC, standing and reacting for 90-120 min in a water bath;
the mass ratio of silver to bovine serum albumin in the silver ammonia solution is 5.39-53.95: 1000;
3) transferring the test solution obtained in the step 2) into a dialysis bag with the molecular weight cutoff of 2000, and dialyzing for 36-48 h;
4) and (3) carrying out centrifugal separation on the dialyzed sample solution in the step 3), and centrifuging for 10-20 min at the rotating speed of 10000-15000 rpm to obtain the silver nanoparticle dispersion solution.
And in the step 4), after centrifugal separation, the supernatant fluid obtains silver nanoparticle dispersion liquid with the particle size range of 3.6-11.7 nm and the average particle size of 5nm, and the precipitate obtained by the centrifugal separation is re-dispersed to obtain silver nanoparticle dispersion liquid with the particle size range of 18.2-58.8 nm and the average particle size of 24 nm.
The silver nanoparticles with fluorescence characteristics are prepared by taking bovine serum albumin as a template and a reducing agent and reducing silver ammonia in situ by utilizing a silver mirror reaction principle. After dialysis and centrifugal separation, two kinds of silver nanoparticles with the particle size ranges of 3.6-11.7 nm and 18.2-58.8 nm are obtained.
The invention has the beneficial effects that:
according to the method, bovine serum albumin is used as a template and a reducing agent, silver ammonia is reduced in situ to obtain silver nanoparticles based on a silver mirror reaction principle, the method avoids the use of high temperature and high pressure and an additional reducing agent, equipment is simple, operation is convenient and fast, synthesis is green, the obtained silver nanoparticles show good fluorescence characteristics, and the silver nanoparticles have the potential of metal ion and small molecule analysis and detection.
Drawings
FIG. 1 shows the results of example 1, wherein the bovine serum albumin solution and the silver ammonia solution were mixed at 30, 40, 50, 60oC, standing and reacting for 90min in a water bath to obtain a fluorescence spectrum of a product under 390 nm excitation;
FIG. 2 is a graph showing the results of example 2, wherein bovine serum albumin solution and silver ammonia solution of different concentrations were mixed at 50oC, standing and reacting for 90min in a water bath to obtain a fluorescence spectrum of a product under 390 nm excitation;
FIG. 3 is a graph showing the results of example 3 in which a bovine serum albumin solution and a silver ammonia solution were mixed at 50oC, standing and reacting for 120min in a water bath to obtain a fluorescence spectrum of a product under 390 nm excitation;
FIG. 4 is a graph showing the results of example 4, in which a bovine serum albumin solution and a silver ammonia solution were mixed at 50oC, standing and reacting for 90min under a water bath to obtain a nano-particle size representation diagram of a supernatant (a) and a precipitate redispersion (b) after centrifugation of the silver nano-particles;
FIG. 5 is a graph showing the results of example 4, in which a bovine serum albumin solution and a silver ammonia solution were mixed at 50oC, standing and reacting for 90min under a water bath to obtain a TEM image of the silver nanoparticles; a and b represent the cases of different magnifications respectively;
FIG. 6 shows the mixture of bovine serum albumin solution and silver ammonia solution at 50 in example 4oAnd C, standing and reacting for 90min under a water bath to obtain a high-resolution transmission electron microscope HRTEM image (a) and a selected area electron diffraction SAED image (b) of the silver nanoparticles.
FIG. 7 is a graph showing the results of example 4, in which a bovine serum albumin solution and a silver ammonia solution were mixed at 50oStanding and reacting for 90min under water bath C to obtain X-ray photoelectron spectroscopy XPS full of silver nanoparticlesSpectrum (a) and silver spectrum (b).
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
Example 1:
(1) adding 0.06375g of silver nitrate into a clean beaker, adding a small amount of distilled water to completely dissolve the silver nitrate, dropwise adding concentrated ammonia water until a brown yellow precipitate is generated, continuously dropwise adding concentrated ammonia water until the precipitate is completely dissolved, keeping the volume to 25mL, and preparing 15 mmol L-1The silver ammonia solution of (1).
(2) Weighing 2.5 g bovine serum albumin in a beaker, adding water to dissolve the bovine serum albumin, and then putting the bovine serum albumin in a 50 mL volumetric flask to obtain the bovine serum albumin with the concentration of 50 mg mL-1Taking 5mL of the bovine serum albumin solution, putting the solution into four beakers, respectively adding 5mL of the silver ammonia solution obtained in the step 1), and respectively placing the silver ammonia solution in 30, 40, 50 and 60 partsoAnd C, standing and reacting for 90min in a water bath. The reaction gives a pale yellow solution, of which 30, 40oThe product at C was visibly turbid, 60oThe product was slightly cloudy at C.
(3) The above test solution was transferred to a dialysis bag with a cut-off molecular weight of 2000 and dialyzed for 36 hours. The dialyzed solution was taken and measured for its fluorescence spectrum under excitation at 390 nm on a molecular fluorescence photometer.
FIG. 1 shows the results of the measurement of the above-mentioned 30, 40, 50, 60 by using a molecular fluorescence spectrometer (F-7000, Hitachi, Japan)oMeasuring the fluorescence spectrum of the sample after the C reaction under the excitation of 390 nm to obtain that the sample has a fluorescence peak at 490 nm and 50oC reaction product strength is greatest.
(4) And (4) carrying out centrifugal separation on the dialyzed sample solution in the step (3), and centrifuging at the rotating speed of 15000 rpm for 10 min to obtain the silver nanoparticle dispersion solution.
Example 2:
(1) respectively taking 0.02125, 0.06375 and 0.10625 g of silver nitrate, adding a small amount of distilled water into a clean beaker to completely dissolve the silver nitrate, dropwise adding concentrated ammonia water until brown yellow precipitate is generated, continuously dropwise adding concentrated ammonia water until the precipitate is completely dissolved, keeping the constant volume to 25mL, and preparing 5, 15 and 25 mmol L of silver nitrate-1Silver ammonia ofAnd (3) solution.
(2) Weighing 2.5 g bovine serum albumin in a beaker, adding water to dissolve the bovine serum albumin, and then putting the bovine serum albumin in a 50 mL volumetric flask to obtain the bovine serum albumin with the concentration of 50 mg mL-1Taking 5mL of the bovine serum albumin solution, adding 5mL of the silver ammonia solution with different concentrations in the step (1), and placing the mixture in a 50-inch flaskoAnd C, standing and reacting for 90min in a water bath.
(3) Transferring the test solution into a dialysis bag with molecular weight cutoff of 2000, and dialyzing for 48 h. The dialyzed solution was taken and measured for its fluorescence spectrum under excitation at 390 nm on a molecular fluorescence photometer.
FIG. 2 shows the results of the measurement of 5, 15 and 25 mmol L of the above-mentioned compound using a molecular fluorescence spectrometer (F-7000, Hitachi, Japan)-1The maximum emission wavelengths of the fluorescence spectra of the silver nanoparticles prepared from the silver ammonia solution are 456, 475 and 490 nm respectively.
(4) And (4) carrying out centrifugal separation on the dialyzed test solution in the step (3), and centrifuging for 20min at the rotating speed of 10000 rpm to obtain the silver nanoparticle dispersion liquid.
Example 3:
(1) adding 0.06375g of silver nitrate into a clean beaker, adding a small amount of distilled water to completely dissolve the silver nitrate, dropwise adding concentrated ammonia water until a brown yellow precipitate is generated, continuously dropwise adding concentrated ammonia water until the precipitate is completely dissolved, and preparing 15 mmol L of solution with constant volume of 25mL-1The silver ammonia solution of (1).
(2) Weighing 5.0 g bovine serum albumin in a beaker, adding water to dissolve the bovine serum albumin, and then placing the bovine serum albumin in a 50 mL volumetric flask to obtain the bovine serum albumin with the concentration of 100 mg mL-1Taking 5mL of the bovine serum albumin solution, adding 5mL of the silver ammonia solution with different concentrations in the step (1), and placing the mixture in a 50-inch flaskoAnd C, standing and reacting for 120min in a water bath.
(3) Transferring the test solution into a dialysis bag with molecular weight cutoff of 2000, and dialyzing for 48 h. The dialyzed solution was taken and measured for its fluorescence spectrum under excitation at 390 nm on a molecular fluorescence photometer.
FIG. 3 is a fluorescence spectrum of silver nanoparticles prepared by the above reaction for 120min using a molecular fluorescence spectrophotometer (F-7000, Hitachi, Japan), with a maximum emission wavelength of 475 nm.
(4) And (4) carrying out centrifugal separation on the dialyzed sample solution in the step (3), and centrifuging at the rotating speed of 12000 rpm for 20min to obtain the silver nanoparticle dispersion solution.
Example 4:
(1) adding 0.06375g of silver nitrate into a clean beaker, adding a small amount of distilled water to completely dissolve the silver nitrate, dropwise adding concentrated ammonia water until a brown yellow precipitate is generated, continuously dropwise adding concentrated ammonia water until the precipitate is completely dissolved, keeping the volume to 25mL, and preparing 15 mmol L-1The silver ammonia solution of (1).
(2) Weighing 2.5 g bovine serum albumin in a beaker, adding water to dissolve the bovine serum albumin, and then putting the bovine serum albumin in a 50 mL volumetric flask to obtain the bovine serum albumin with the concentration of 50 mg mL-1Taking 5mL of the bovine serum albumin solution, adding 5mL of the silver ammonia solution obtained in the step (1), and placing the mixture in a 50-inch flaskoAnd C, standing and reacting for 90min in a water bath.
(3) Transferring the test solution into a dialysis bag with molecular weight cutoff of 2000, and dialyzing for 48 h.
(4) And (4) centrifuging the dialyzed sample solution in the step (3) for 15 min at the rotating speed of 15000 rpm, obtaining a light yellow solution from a supernatant, separating and re-dispersing precipitates obtained by centrifugation, and respectively measuring the nano-particle sizes of the precipitates.
FIG. 4 shows the results of a Malvern nanosizer (Nano-ZS 90, Malvern) test on the centrifuged supernatant and pellet redispersion solutions. The result shows that (a) the particle size range of the silver nanoparticles in the supernatant is 3.6-11.7 nm, the average particle size is 5nm, and (b) the particle size range of the silver nanoparticles precipitated after dispersion is 18.2-58.8 nm, and the average particle size is 24 nm.
Fig. 5 shows the results of characterization of the silver nanoparticles using a transmission electron microscope (Tecnai-G20, FEI, usa). It can be clearly seen that the silver nanoparticles are spherical and that there are two size distributions.
FIG. 6 shows the results of high resolution and selective electron diffraction characterization of the silver nanoparticles using a transmission electron microscope (Tecnai-G20, FEI, USA). The crystal lattice and diffraction spots of the silver nanoparticles can be obviously seen, and the silver nanoparticles are proved to have good crystallinity.
FIG. 7 shows the characterization of the silver nanoparticles by X-ray photoelectron spectroscopy (K-Alpha, Sammer fly., USA), which indicates that the material is composed of C1 s, O1 s, N1 s, Ag 3d, etc., wherein the peaks at 374.3 and 368.3 eV in the Ag 3d spectrum correspond to Ag 3d respectively3/2And Ag 3d5/2。
Claims (3)
1. A method for preparing fluorescent silver nanoparticles based on silver mirror reaction is characterized by comprising the following steps: the method comprises the following steps:
1) putting silver nitrate into a clean beaker, adding distilled water to completely dissolve the silver nitrate, dropwise adding concentrated ammonia water until brown yellow precipitate is generated, continuously dropwise adding concentrated ammonia water until the precipitate is completely dissolved, fixing the volume, and preparing 5-25 mmol L-1The silver ammonia solution of (a);
2) putting bovine serum albumin solution into a beaker, adding the silver ammonia solution obtained in the step 1), putting the beaker in a water bath at 50 ℃, and standing for reaction for 90-120 min;
taking bovine serum albumin as a template and a reducing agent, taking the bovine serum albumin as a biological grade, and mixing the silver and the bovine serum albumin in the mixed silver ammonia solution according to the mass ratio of 5.39-53.95: 1000;
3) transferring the test solution obtained in the step 2) into a dialysis bag with the molecular weight cutoff of 2000, and dialyzing for 36-48 h;
4) and (3) carrying out centrifugal separation on the dialyzed sample solution in the step 3), and centrifuging for 10-20 min at the rotating speed of 10000-15000 rpm to obtain the silver nanoparticles.
2. The method for preparing fluorescent silver nanoparticles based on the silver mirror reaction according to claim 1, wherein: the concentration of the bovine serum albumin solution is 50-100 mg mL-1。
3. The method for preparing fluorescent silver nanoparticles based on the silver mirror reaction according to claim 1, wherein: and 4) centrifugally separating, collecting supernatant to obtain silver nanoparticle dispersion liquid with the particle size of 3.6-11.7 nm, and carrying out precipitation separation and redispersion after centrifugation to obtain silver nanoparticle dispersion liquid with the particle size of 18.2-58.8 nm.
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