CN113118453B - Silver nano particle, preparation method thereof and photoinduction device - Google Patents
Silver nano particle, preparation method thereof and photoinduction device Download PDFInfo
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- CN113118453B CN113118453B CN201911398463.7A CN201911398463A CN113118453B CN 113118453 B CN113118453 B CN 113118453B CN 201911398463 A CN201911398463 A CN 201911398463A CN 113118453 B CN113118453 B CN 113118453B
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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
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- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a silver nanoparticle, a preparation method thereof and a photoinduction device, wherein the method comprises the following steps: preparing a silver nanoparticle precursor solution; carrying out first light induction reaction treatment on the silver nanoparticle precursor solution to obtain a first mixed solution; adding an N-vinylamide compound to the first mixed solution to obtain a second mixed solution; and carrying out second light-induced reaction treatment on the second mixed solution to obtain the silver nanoparticles. The method adopts the light-induced silver nanoparticle precursor to prepare the silver nanoparticles, is simple and easy to operate, does not introduce impurities difficult to remove, and can regulate and control the morphology and the size of the nanoparticles; silver nanoparticles having a uniform size and a desired size and a specific morphology, which have good plasmon resonance scattering characteristics, can be obtained.
Description
Technical Field
The invention relates to the technical field of preparation of nano materials, in particular to silver nanoparticles, a preparation method thereof and a photoinduction device.
Background
The application of metal particles under the nanometer scale in the aspects of optics, electronics, magnetics, catalysis and the like and the great difference of bulk phase materials of the metal particles cause great interest of researchers. Noble metal nanoparticles, particularly gold and silver nanoparticles, are receiving increasing attention because of their unique spectral response in the visible and near infrared bands.
Surface plasmon resonance is then due to the interaction between the incident electromagnetic field and the free valence electrons of the nanostructured surface of the material: under the action of the incident electromagnetic field, the free electrons on the surface of the nanostructure are forced to form collective oscillation, and when the oscillation frequency is consistent with the frequency of the incident light, the resonance, namely the surface plasma resonance, is achieved. In recent years, the development of the nano-discipline has been driven by the research of scientists on the surface plasmon resonance properties and has extended several new applications, such as: surface plasmon enhanced spectroscopy, chemical and biochemical sensing, and photothermal therapy of cancer and tumors. The surface plasmon resonance properties of metallic nanoparticles are strongly dependent on their size and morphology. Therefore, it is important to regulate the influence of the size and morphology of the nanoparticles on their surface plasmon resonance properties.
The prior preparation method of the polygonal noble metal nano-particles mainly comprises a plasma mediated method and a ligand-assisted chemical reduction method. However, the inventors studied: although the ligand-assisted chemical reduction method is easy to operate, the polygonal noble metal nanoparticles prepared by the method show seriously uneven size distribution and have great shape difference; in addition, this method usually requires the addition of polymers for catalysis and induction, but in some applications these polymers are difficult to remove. Although the polygonal noble metal nanoparticles prepared by the plasma mediated method have good polygonal shapes, the preparation process of the method is complex and the preparation cost is high.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide silver nanoparticles, a preparation method thereof and a photoinduction device, and aims to solve the problems of complex preparation process, high preparation cost and easy introduction of difficult impurities in the existing preparation method of noble metal nanoparticles.
The technical scheme of the invention is as follows:
a method for preparing silver nanoparticles, comprising the steps of:
preparing a silver nanoparticle precursor solution;
carrying out first light induction reaction treatment on the silver nanoparticle precursor solution to obtain a first mixed solution;
adding an N-vinylamide compound to the first mixed solution to obtain a second mixed solution;
and carrying out second light-induced reaction treatment on the second mixed solution to obtain the silver nanoparticles.
A photoinduction device for preparing silver nanoparticles, wherein the photoinduction device is suitable for implementing the preparation method of silver nanoparticles. Thus, the light induction device may have all the features and advantages of the method described above. The light induction device comprises:
a tubular reactor;
the temperature controller is sleeved on the outer side of the tubular reactor, a liquid inlet is formed in the lower part of the temperature controller, and a liquid outlet is formed in the upper part of the temperature controller;
the short-wavelength light source array is arranged on the side wall of one side of the temperature controller in a surrounding manner;
the long wavelength light source array is arranged on the side wall on the other side of the temperature controller in a surrounding manner;
wherein the light emission wavelength of the light source of the short wavelength light source array is smaller than the light emission wavelength of the light source of the long wavelength light source array.
A silver nanoparticle, wherein the silver nanoparticle has a decahedral structure, and the silver nanoparticle is prepared by the method as described above. Thus, the silver nanoparticles may have all the features and advantages of the previously described method.
Has the advantages that: the method for preparing the silver nanoparticles by photo-inducing the silver nanoparticle precursor is simple and easy to operate, no impurities which are difficult to remove are introduced in the preparation process, and the shape and the size of the nanoparticles are easy to regulate and control; silver nanoparticles having a uniform size and a desired size and a specific morphology, which have good plasmon resonance scattering characteristics, can be obtained.
Drawings
Fig. 1 is a flow chart of a method for preparing silver nanoparticles according to an embodiment of the present invention.
Fig. 2 is a schematic diagram of a process for forming silver nanoparticles according to an embodiment of the present invention.
Fig. 3 is a schematic structural diagram of a light induction device according to an embodiment of the present invention.
FIG. 4 is a cross-sectional view of a light-inducing apparatus according to an embodiment of the present invention.
FIG. 5 is an SEM image of silver nanoparticles in example 1 of the present invention.
Fig. 6 is a comparison graph of fluorescence spectra of the spherical nanoparticle precursor obtained in step (1) and the prepared decahedral silver nanoparticles in example 1 of the present invention.
Detailed Description
The present invention provides a silver nanoparticle, a method for preparing the same, and a photoinduction apparatus, and the present invention will be described in further detail below in order to make the objects, technical solutions, and effects of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, an embodiment of the present invention provides a method for preparing silver nanoparticles, including the steps of:
s100, preparing a silver nanoparticle precursor solution;
s200, carrying out first light-induced reaction treatment on the silver nanoparticle precursor solution to obtain a first mixed solution;
s300, adding an N-vinylamide compound into the first mixed solution to obtain a second mixed solution;
s400, carrying out second light-induced reaction treatment on the second mixed solution to obtain the silver nanoparticles.
In the embodiment, the silver nanoparticles are prepared by photo-inducing the silver nanoparticle precursor, the method is simple and easy to operate, impurities which are difficult to remove are not introduced in the preparation process, and the shape and the size of the nanoparticles are easy to regulate and control; silver nanoparticles having a uniform size and a desired size and a specific morphology, which have good plasmon resonance scattering characteristics, can be obtained.
In one embodiment, step S100 specifically includes: mixing a silver source, an organic acid salt and distilled water to obtain a third mixed solution;
performing a first reaction treatment on the third mixed solution under an alkaline condition to obtain a fourth mixed solution;
and carrying out second reaction treatment on the fourth mixed solution under an acidic condition to obtain the silver nanoparticle precursor solution.
Further, in one embodiment, the pH of the third mixed solution under the alkaline condition is 9 to 11;
optionally, the pH of the fourth mixed solution under the acidic condition is 4 to 6.
Specifically, a certain amount of silver source and organic acid salt are mixed by using distilled water as a solvent to obtain a third mixed solution; performing a first reaction treatment for 5 to 30min by adjusting the pH of the third mixed solution to 9 to 11 (e.g., pH = 10) with a base to obtain a fourth mixed solution; then, the pH of the fourth mixed solution is adjusted to 4 to 6 (e.g., pH = 5) with an acid to perform a second reaction treatment (e.g., ultrasonic reaction) for 20 to 60min, to obtain a silver nanoparticle precursor solution. The alkaline pH value is selected as the initial condition, the nucleation can be rapidly carried out, and the growth speed is too fast when the pH value is more than 11, so that the spherical control can not be realized; and when the nanoparticle nucleation stage is finished, adjusting the pH value of the solution to a relatively low condition for particle growth, wherein the pH value is less than 4, and the solution forms an acid solution with a certain concentration due to the existence of acid radicals in the solution, so that small-size silver particles are dissolved. The step control of the fast nucleation and the slow growth is beneficial to obtaining the silver nano particle precursor solution which is relatively uniform and has a certain appearance (such as a sphere).
Further in one embodiment, the base may comprise NaOH, KOH, na 2 CO 3 、K 2 CO 3 、NaHCO 3 、KHCO 3 And NH 3 ·H 2 At least one of O;
optionally, the acid may include at least one of hydrochloric acid, citric acid, phosphoric acid, malic acid, acetic acid, formic acid, and oxalic acid;
optionally, the silver source may include AgNO 3 、CH 3 At least one of COOAg, agCl, agBr and AgI;
optionally, the organic acid salt may include at least one of sodium citrate, potassium citrate, sodium oxalate, potassium oxalate, sodium succinate, potassium succinate, sodium tartrate, potassium tartrate.
Referring to fig. 2, steps S200 and S400 will be described.
Step S200 specifically includes: the silver nanoparticle precursor (e.g., spherical silver nanoparticle precursor, which is used as a seed for preparing silver nanoparticles) solution obtained in step S100 is added to a light induction device, and first light induction reaction treatment is performed for 5 to 10min, i.e., the silver nanoparticle precursor forms a primary structure (e.g., quintuple twin structure) to obtain a first mixed solution.
Then, step S300 is performed: and adding the N-vinyl amide compound into the first mixed solution, and uniformly stirring to obtain a second mixed solution.
In one embodiment, the N-vinylamide compound may include at least one of N-vinylformamide, N-vinylcaprolactam, and N-vinylpyrrolidone. The N-vinyl amide compound is used as an inhibitor in the reaction process, and the action principle is as follows: the N-vinylamide compound acts on a specific crystal face (111) of the silver nanoparticle precursor, and the silver nanoparticle with a specific morphology is prepared by regulating and controlling the light-induced reaction condition and the ratio of the N-vinylamide compound to the silver source.
In one embodiment, the mass ratio of the silver source, the organic acid salt, the distilled water, and the N-vinylamide compound is (0.1 to 2): (0.01-0.05): (1-100): (0.0001-0.0002). When the amount of the organic acid salt is less than the proportion range, the silver nanoparticles obtained by synthesis are quickly precipitated due to insufficient stabilization of the organic acid salt in the solution; when the organic acid salt is larger than the ratio range, the silver nanoparticles obtained may be aggregated and precipitated in a short time due to an excessively high salt concentration in the organic acid salt solution.
Step S400 specifically includes: and carrying out second light induction reaction treatment on the second mixed solution for 5-10 min, namely, growing the primary structure according to a certain direction (such as a layered twin structure) to form a medium-level structure (such as a three-dimensional five-pointed star structure), and continuing to grow to obtain the silver nanoparticles (with a specific morphology, such as a decahedral structure).
In one embodiment, the light source that performs the first light-induced reaction process emits light at a wavelength that is less than the light source that performs the second light-induced reaction process; and/or
Performing the first light-induced reaction treatment by adopting a light source with the light-emitting wavelength of 350-500nm and the power of 5-50W; and/or
And the second light-induced reaction treatment is carried out by adopting a light source with the light-emitting wavelength of 500-700nm and the power of 5-50W.
In one embodiment, the light sources for performing the first and second light-induced reaction processes are each independently selected from: one of a laser light source, a halogen light source, an LED light source, and a xenon light source.
In one embodiment, after the second light-induced reaction treatment is performed and before the nanoparticles are obtained, the method further includes step S500:
carrying out heating reaction treatment on the second mixed solution subjected to the second light-induced reaction treatment;
wherein the temperature of the heating reaction treatment is 40-100 ℃ (rapid temperature rise), and the reaction time is 0.1-2h. The silver nanoparticles are grown to a desired size by controlling the temperature or time of the heating reaction, and silver nanoparticles having a desired size and a specific morphology (e.g., decahedron) are obtained.
The embodiment of the invention also provides a photoinduction device for preparing the silver nanoparticles, and the photoinduction device is suitable for implementing the preparation method of the silver nanoparticles. Thus, the light induction device may have all the features and advantages of the method described above. The light induction device comprises:
a tubular reactor;
the temperature controller is sleeved on the outer side of the tubular reactor, a liquid inlet is formed in the lower part of the temperature controller, and a liquid outlet is formed in the upper part of the temperature controller;
the short-wavelength light source array is arranged on the side wall of one side of the temperature controller in a surrounding manner;
the long wavelength light source array is arranged on the side wall on the other side of the temperature controller in a surrounding manner;
wherein the light emission wavelength of the light source of the short wavelength light source array is smaller than the light emission wavelength of the light source of the long wavelength light source array.
Referring to fig. 3 and 4, the light induction device for light induction includes a tubular reactor 1; the temperature controller 2 is sleeved on the outer side of the tubular reactor 1, a liquid inlet 4 is arranged at the lower part of the temperature controller 2, and a liquid outlet 5 is arranged at the upper part of the temperature controller; a light source array 3 disposed around a sidewall of the thermostat, the light source array 3 being composed of a short wavelength light source array 31 and a long wavelength light source array 32: wherein, the short wavelength light source array 31 is arranged on the side wall of one side of the temperature controller in a surrounding manner; an array of long wavelength light sources 32 is disposed around the other side wall of the thermostat. The light induction device is characterized in that: (1) The efficiency of light irradiation is improved in the form of side irradiation; (2) The main body is a jacket layer structure, the inner layer is a tubular reactor and can be used for placing reaction liquid, the outer layer is a liquid bath temperature controller and can be used for controlling the temperature of a reaction system, and simultaneously, the heat effect generated by light source luminescence and the heat released in the form of heat radiation in the light energy absorbed by reactants can also be removed.
In one embodiment, the short wavelength light source and the long wavelength light source may be independently selected from one of a laser light source, a halogen lamp light source, an LED lamp light source, and a xenon lamp light source;
optionally, the light emitted by the short-wavelength light source has the light-emitting wavelength of 350-500nm and the power of 5-50W; the light emitted from the long wavelength light source has an emission wavelength of 500 to 700nm and a power of 5 to 50W.
The embodiment of the invention also provides a silver nanoparticle, wherein the silver nanoparticle has a decahedral structure; the silver nanoparticles are prepared by the method as described in any one of the above. Thus, the silver nanoparticles may have all the features and advantages of the previously described method. The silver nanoparticles of the embodiment have uniform and controllable size and good plasma resonance scattering property.
The preparation process of the present invention is described in detail below by way of specific examples.
Example 1
(1) 0.1g of silver nitrate and 0.01g of sodium tartrate were added to 5g of distilled water to be sufficiently dissolved and mixed, and then the solution was adjusted to 10 pH with potassium hydroxide to react for 10min. Then adjusting the pH value to 5 by using hydrochloric acid, and carrying out ultrasonic reaction for 30min to obtain a spherical silver nanoparticle precursor solution.
(2) Adding the silver nanoparticle precursor solution obtained in the step (1) into a light induction device, firstly inducing the silver nanoparticle precursor solution to form a quintuple twin structure by using monochromatic argon ion laser with the power of 8W and the wavelength of 374nm, then adding 0.0001g N-vinyl pyrrolidone into the silver nanoparticle precursor solution, uniformly stirring, then inducing the layered twin structure to grow by using monochromatic argon ion laser with the wavelength of 8W and the wavelength of 514nm, and after the light induction is finished, introducing a hot water bath to quickly heat the reaction system to 60 ℃ and keeping the temperature for 20min to obtain the silver nanoparticles. The morphology of the silver nanoparticles was measured by a Scanning Electron Microscope (SEM), and the measurement result is shown in fig. 5, which indicates that the obtained silver nanoparticles have a decahedral structure and a particle size of 80-100 nm. As shown in fig. 6, a comparison graph of fluorescence spectra of the spherical silver nanoparticle precursor obtained in step (1) and the decahedral silver nanoparticle finally prepared shows that the finally prepared silver nanoparticle has good plasmon resonance scattering characteristics, as can be seen from fig. 6.
Example 2
(1) After 2g of silver chloride and 0.05g of potassium oxalate were added to 90g of distilled water and sufficiently dissolved and mixed, the solution was adjusted to pH 10 with potassium hydroxide and reacted for 8min. And then adjusting the pH value to 5 by using hydrochloric acid, and carrying out ultrasonic reaction for 20min to obtain a spherical silver nanoparticle precursor solution.
(2) Adding the silver nanoparticle precursor solution obtained in the step (1) into a light induction device, firstly inducing the silver nanoparticle precursor solution to form a quintuple twin crystal structure by using LED light with the power of 40W and the wavelength of 370nm, then adding 0.0002g N-vinylformamide into the light induction device, uniformly stirring, then inducing the layered twin crystal structure to grow by using LED light with the wavelength of 510nm of 40W, and after the light induction is finished, introducing a hot water bath to quickly heat the reaction system to 80 ℃ and keeping the temperature for 30min to obtain silver nanoparticles which have a decahedral structure and the particle size of 150-180 nm and have good plasma resonance scattering characteristics.
Example 3
(1) After 1g of silver bromide and 0.03g of sodium succinate were added to 50g of distilled water and sufficiently dissolved and mixed, the solution was adjusted to a pH of about 10 with potassium hydroxide and reacted for 25min. Then adjusting the pH value to about 5 by using hydrochloric acid, and carrying out ultrasonic reaction for 40min to obtain a spherical silver nanoparticle precursor solution.
(2) Adding the silver nanoparticle precursor solution obtained in the step (1) into a light induction device, inducing the silver nanoparticle precursor solution to form a quintuple twin crystal structure by using a xenon lamp light source with the power of 20W and the wavelength of 381nm, then adding 0.0015g N-vinyl caprolactam into the silver nanoparticle precursor solution, uniformly stirring the mixture, inducing the layered twin crystal structure to grow by using a xenon lamp light source with the wavelength of 20W and the wavelength of 541nm, raising the temperature of a water bath to 70 ℃ after the light induction is finished, and keeping the temperature for 25min to obtain silver nanoparticles, wherein the silver nanoparticles have a decahedral structure, the particle size is 120-130 nm, and the silver nanoparticles have good plasma resonance scattering characteristics.
In summary, the present invention provides a silver nanoparticle, a method for preparing the same, and a photoinduction device. The method for preparing the silver nanoparticles by photoinduction of the spherical silver nanoparticles and the precursor is simple and easy to operate, impurities which are difficult to remove are not introduced in the preparation process, and the morphology and the size of the nanoparticles are easy to regulate and control; silver nanoparticles having a uniform size and a desired size, which have good plasmon resonance scattering characteristics, can be prepared.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (8)
1. A method for preparing silver nanoparticles, comprising the steps of:
preparing a silver nanoparticle precursor solution;
carrying out first light induction reaction treatment on the silver nanoparticle precursor solution to obtain a first mixed solution;
adding an N-vinylamide compound to the first mixed solution to obtain a second mixed solution;
carrying out second light-induced reaction treatment on the second mixed solution to obtain the silver nanoparticles;
the preparation method of the silver nanoparticle precursor solution comprises the following steps:
mixing a silver source, an organic acid salt and distilled water to obtain a third mixed solution;
performing a first reaction treatment on the third mixed solution under an alkaline condition to obtain a fourth mixed solution;
performing second reaction treatment on the fourth mixed solution under an acidic condition to obtain the silver nanoparticle precursor solution;
the pH value of the third mixed solution under the alkaline condition is 9-11; the pH value of the fourth mixed solution under the acidic condition is 4-6.
2. The method of claim 1, wherein the silver source comprises AgNO 3 、CH 3 At least one of COOAg, agCl, agBr and AgI.
3. The production method according to claim 1, wherein the mass ratio among the silver source, the organic acid salt, the distilled water, and the N-vinylamide compound is (0.1-2): (0.01-0.05): (1-100): (0.0001-0.0002).
4. The production method according to claim 1, wherein an emission wavelength of a light source subjected to the first light-induced reaction treatment is smaller than an emission wavelength of a light source subjected to the second light-induced reaction treatment; and/or
The first light-induced reaction treatment is carried out by adopting a light source with the light-emitting wavelength of 350-500nm and the power of 5-50W; and/or
And the second light-induced reaction treatment is carried out by adopting a light source with the light-emitting wavelength of 500-700nm and the power of 5-50W.
5. The method according to claim 1, wherein the light sources for performing the first light-induced reaction treatment and the second light-induced reaction treatment are each independently selected from: one of a laser light source, a halogen light source, an LED light source, and a xenon light source.
6. The method according to claim 1, wherein after the second light-induced reaction treatment and before obtaining the nanoparticles, the method further comprises:
carrying out heating reaction treatment on the second mixed solution subjected to the second light-induced reaction treatment;
wherein the temperature of the heating reaction treatment is 40-100 ℃, and the reaction time is 0.1-2h.
7. The method according to claim 1, wherein the organic acid salt comprises at least one of sodium citrate, potassium citrate, sodium oxalate, potassium oxalate, sodium succinate, potassium succinate, sodium tartrate, and potassium tartrate.
8. The method according to claim 1, wherein the N-vinylamide-based compound comprises at least one of N-vinylformamide, N-vinylcaprolactam, and N-vinylpyrrolidone.
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| US8425653B2 (en) * | 2009-03-20 | 2013-04-23 | Northwestern University | Plasmon mediated photoinduced synthesis of silver triangular bipyramids |
| CN102248177B (en) * | 2011-07-29 | 2012-12-12 | 上海龙翔新材料科技有限公司 | Laser-induced method for preparing spherical silver powder |
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| CN102581299A (en) * | 2012-02-21 | 2012-07-18 | 金淞电器(九江)有限公司 | Photochemical preparation method of noble metal nanoparticles |
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