CN115570144A - Preparation method of silver nanosheet with controllable thickness - Google Patents
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Abstract
The invention discloses a preparation method of a silver nanosheet with controllable thickness, which comprises the following steps: uniformly mixing trisodium citrate, polyvinylpyrrolidone, copper chloride and water to obtain a first mixed solution, mixing the first mixed solution and the silver nanosheet seed crystal sol to obtain a second mixed solution, heating the second mixed solution to 40-100 ℃, dropwise adding a silver nitrate aqueous solution and an ascorbic acid aqueous solution into the second mixed solution at 40-100 ℃ under the stirring condition, keeping the temperature unchanged after the silver nitrate aqueous solution and the ascorbic acid aqueous solution are completely dropwise added, reacting for 20-30 min under the stirring condition to obtain a silver nanosheet sol, centrifuging the silver nanosheet sol, washing and centrifuging to obtain a precipitate, and obtaining the silver nanosheet with controllable thickness. According to the invention, the copper ions and the halogen ions are utilized to regulate the transverse growth and the longitudinal growth of the silver nanosheets, so that a series of silver nanosheets with different thicknesses and different shapes can be obtained, the preparation method is simple, and the reaction conditions are mild.
Description
Technical Field
The invention belongs to the technical field of silver nanosheet preparation, and particularly relates to a preparation method of a silver nanosheet with controllable thickness.
Background
The Local Surface Plasmon Resonance (LSPR) is a phenomenon in which free electrons on the Surface of a metal nanomaterial are driven by an incident electromagnetic field to oscillate collectively, and absorb and scatter light in a specific wavelength range. The silver nanocrystal has unique optical properties, and the surface plasmon resonance effect of the silver nanocrystal mainly occurs in a visible light region and an infrared light region. Due to the strong surface plasmon resonance effect, the silver nano material has important application in the field of surface enhancement such as surface enhanced Raman spectroscopy and surface enhanced fluorescence spectroscopy, and is a good enhancement substrate. The two-dimensional structure silver nano-meter can present a plurality of resonance modes. By regulating the size and thickness of the nanosheets, the resonance wavelength of the nanosheets can be regulated and controlled from a visible light region to a near-infrared light region, so that the silver nanosheets have wide application prospects in the field of detection and imaging related to surface enhancement. Although various methods such as a photochemical growth method, a thermal reduction method, a template method and the like have been developed to prepare the silver nanosheet at present, the preparation method capable of accurately regulating the morphology of the nanosheet and controlling the thickness of the nanosheet is still deficient.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of silver nanosheets with controllable thickness, and the preparation method utilizes halogen ions and Cu 2+ The growth of the silver nanosheets is controlled together, the size (side length) of the obtained silver nanosheets can be regulated and controlled within the range of 60nm to 200nm, and the thickness of the nanosheets can be regulated and controlled within the range of 10nm to 200 nm.
The purpose of the invention is realized by the following technical scheme.
A preparation method of silver nanosheets with controllable thickness comprises the following steps:
1) Uniformly mixing trisodium citrate, polyvinylpyrrolidone (PVP), copper chloride and water to obtain a first mixed solution, wherein the concentration of the trisodium citrate in the first mixed solution is 0.1-50 mM, the concentration of the copper chloride in the first mixed solution is 0.1-10 mM, and the concentration of the polyvinylpyrrolidone in the first mixed solution is 0.1-5 wt%;
in the step 1), the concentration of trisodium citrate in the first mixed solution is 2.0 to 5mM, the concentration of copper chloride in the first mixed solution is 0.5 to 2.0mM, and the concentration of polyvinylpyrrolidone in the first mixed solution is 0.5 to 1.0wt%.
2) Mixing the first mixed solution and the silver nanosheet seed crystal sol to obtain a second mixed solution, heating the second mixed solution to 40-100 ℃, dropwise adding a silver nitrate aqueous solution with a silver nitrate concentration of 1-50 mM and an ascorbic acid aqueous solution with an ascorbic acid concentration of 1-50 mM to the second mixed solution at 40-100 ℃ under the condition of stirring, keeping the temperature unchanged after the silver nitrate aqueous solution and the ascorbic acid aqueous solution are completely dropwise added, and reacting for 20-30 min under the condition of stirring to obtain the silver nanosheet sol, wherein the ratio of the first mixed solution to the silver nanosheet seed crystal sol is (4-20): 1, the ratio of the silver nitrate aqueous solution to the ascorbic acid aqueous solution is 1: (1-10);
in the step 2), the concentration of silver nitrate in the silver nitrate aqueous solution is 5-10 mM, and the concentration of ascorbic acid in the ascorbic acid aqueous solution is 5-10 mM.
In the step 2), the dropping speeds of the silver nitrate aqueous solution and the ascorbic acid aqueous solution are respectively 20-40 mL/h.
In the step 2), the method for preparing the silver nanosheet seed sol comprises: mixing 40-50 parts by volume of water, 3-5 parts by volume of trisodium citrate aqueous solution and 1-2 parts by volume of PVP aqueous solution, adding 1-2 parts by volume of sodium borohydride aqueous solution under stirring, stirring for 40-60 min, dropwise adding 0.3-0.5 part by volume of hydrogen peroxide aqueous solution, continuing stirring for 2-5 h, and standing for 24-48 h to obtain the silver nanosheet seed crystal sol, wherein the concentration of trisodium citrate in the trisodium citrate aqueous solution is 25-50 mM, the concentration of PVP in the PVP aqueous solution is 0.5-0.1 wt%, the concentration of sodium borohydride in the sodium borohydride aqueous solution is 100-120 mM, and the concentration of the hydrogen peroxide aqueous solution is 20-30 wt%.
3) And centrifuging the silver nanosheet sol, washing and centrifuging the obtained precipitate to obtain the silver nanosheet with controllable thickness.
In the step 3), deionized water and/or ethanol are used for washing.
In the step 3), the speed of the centrifugation is 3000-5000 rpm.
According to the invention, the copper ions and the halogen ions are utilized to regulate the transverse growth and the longitudinal growth of the silver nanosheets, so that a series of silver nanosheets with different thicknesses and different appearances can be obtained. In the growth process of the silver nanosheets, the halogen ions are selectively adsorbed on the side crystal faces of the silver nanosheets by adding, so that the lateral growth of the silver nanosheets is inhibited. Meanwhile, copper ions are easy to deposit under-potential on (111) crystal faces of the upper surface and the lower surface of the silver nanosheet, so that the deposition and growth speed of silver on the (111) crystal faces of the upper surface and the lower surface is accelerated, the silver nanosheet is promoted to grow along the longitudinal direction, and the silver nanosheet with the increased thickness is obtained. The preparation method is simple, mild in reaction condition, free of complex equipment, low in cost, good in repeatability and easy to realize large-scale industrial production. The silver nanosheet prepared by the preparation method has adjustable surface plasma resonance wavelength and excellent photo-thermal conversion performance.
Drawings
FIG. 1 is an SEM of a dispersion obtained in example 1;
FIG. 2 is an SEM of the dispersion obtained in example 2;
FIG. 3 is an SEM of a dispersion obtained in example 3;
FIG. 4 is an SEM of the dispersion obtained in example 4.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
Deionized water was used as water in the following examples.
The purchase sources of the drugs involved in the following examples are as follows: the chemicals involved in the present invention were purchased from the national drug group, and the purity of the chemical was of analytical grade (AR).
Example 1
A preparation method of silver nanosheets with controllable thickness comprises the following steps:
1) Uniformly mixing trisodium citrate, polyvinylpyrrolidone (PVP), copper chloride and water to obtain a first mixed solution, wherein the concentration of the trisodium citrate in the first mixed solution is 5.0mM, the concentration of the copper chloride in the first mixed solution is 1.5mM, and the concentration of the polyvinylpyrrolidone in the first mixed solution is 0.6wt%;
2) Mixing the first mixed solution and the silver nanosheet seed crystal sol to obtain a second mixed solution, heating the second mixed solution to 80 ℃ in a water bath (keeping the stirring condition in the heating process), simultaneously dropwise adding a silver nitrate aqueous solution with a silver nitrate concentration of 5mM and an ascorbic acid aqueous solution with an ascorbic acid concentration of 5mM to the second mixed solution at the speed of 300rpm under the stirring condition, keeping the temperature unchanged after the silver nitrate aqueous solution and the ascorbic acid aqueous solution are completely dropwise added, and reacting for 20min under the stirring condition to obtain the silver nanosheet sol, wherein the ratio of the first mixed solution to the silver nanosheet seed crystal sol is 5:1, the ratio of the silver nitrate aqueous solution to the ascorbic acid aqueous solution is 1:5, the dropping speed of the silver nitrate aqueous solution is 30mL/h, and the dropping speed of the ascorbic acid aqueous solution is 30mL/h;
the method for preparing the silver nanosheet seed sol comprises the following steps: mixing 40 parts by volume of water, 3 parts by volume of trisodium citrate aqueous solution and 1 part by volume of PVP aqueous solution, adding 1 part by volume of sodium borohydride aqueous solution under stirring, stirring for 1h, dropwise adding 0.3 part by volume of hydrogen peroxide aqueous solution, continuously stirring for 5h, and standing for 24h to obtain the silver nanosheet seed crystal sol, wherein the concentration of trisodium citrate in the trisodium citrate aqueous solution is 0.025mol/L, the concentration of PVP in the PVP aqueous solution is 0.5 wt%, the concentration of sodium borohydride in the sodium borohydride aqueous solution is 0.1mol/L, and the concentration of the hydrogen peroxide aqueous solution is 30wt%.
3) And centrifuging the silver nanosheet sol at 5000rpm for 10min, washing the precipitate obtained by centrifuging with deionized water, and obtaining the silver nanosheet with controllable thickness.
The silver nanosheet seed crystals in the silver nanosheet seed crystal sol adopted in the step 2) are triangular silver nanosheets, and the average size is about 130 nm. In the step 2) of the invention, silver nitrate aqueous solution and ascorbic acid aqueous solution silver salt are dripped to reduce, and the silver nanosheet seed crystal grows to obtain the silver nanosheet product with increased thickness.
Dispersing the precipitate obtained by centrifuging in the step 3) in deionized water to obtain a dispersion liquid, wherein the SEM of the dispersion liquid is shown in figure 1, after the dispersion liquid grows, the triangular silver nanosheets become hexagonal silver nanosheets, the average side length of the silver nanosheets is 106nm, and the average thickness of the silver nanosheets is 28nm.
Example 2
A preparation method of silver nanosheets with controllable thickness comprises the following steps:
1) Uniformly mixing trisodium citrate, polyvinylpyrrolidone (PVP), copper chloride and water to obtain a first mixed solution, wherein the concentration of the trisodium citrate in the first mixed solution is 5.0mM, the concentration of the copper chloride in the first mixed solution is 1.5mM, and the concentration of the polyvinylpyrrolidone in the first mixed solution is 0.6wt%;
2) Mixing the first mixed solution and the silver nanosheet seed crystal sol to obtain a second mixed solution, heating the second mixed solution to 80 ℃ in a water bath, keeping the stirring condition in the heating process, simultaneously dropwise adding a silver nitrate aqueous solution with the concentration of 5mM and an ascorbic acid aqueous solution with the concentration of 5mM to the second mixed solution with the speed of 300rpm under the stirring condition, keeping the temperature unchanged after the silver nitrate aqueous solution and the ascorbic acid aqueous solution are completely dropwise added, and reacting for 20min under the stirring condition to obtain the silver nanosheet sol, wherein the ratio of the first mixed solution to the silver nanosheet seed crystal sol is 5:1, the ratio of the silver nitrate aqueous solution to the ascorbic acid aqueous solution is 1:5, the dropping speed of the silver nitrate aqueous solution is 30mL/h, and the dropping speed of the ascorbic acid aqueous solution is 30mL/h;
the method for preparing the silver nanosheet seed sol comprises the following steps: mixing 40 parts by volume of water, 3 parts by volume of trisodium citrate aqueous solution and 1 part by volume of PVP aqueous solution, adding 1 part by volume of sodium borohydride aqueous solution under stirring, stirring for 1h, dropwise adding 0.3 part by volume of hydrogen peroxide aqueous solution, continuously stirring for 5h, and standing for 24h to obtain the silver nanosheet seed sol, wherein the concentration of trisodium citrate in the trisodium citrate aqueous solution is 0.025mol/L, the concentration of PVP in the PVP aqueous solution is 0.5 wt%, the concentration of sodium borohydride in the sodium borohydride aqueous solution is 0.1mol/L, and the concentration of the hydrogen peroxide aqueous solution is 30wt%.
3) And centrifuging the silver nanosheet sol at 4500rpm for 10min, washing the precipitate obtained by centrifuging with deionized water, and obtaining the silver nanosheet with controllable thickness.
Dispersing the precipitate obtained by centrifuging in the step 3) in deionized water to obtain a dispersion liquid, wherein an SEM of the dispersion liquid is shown in figure 2, the average side length of the silver nanosheet is 118nm, and the average thickness of the silver nanosheet is 63nm. During this growth process, the side lengths of the silver nanoplates remain substantially constant, while the thickness of the nanoplates continues to increase.
Example 3
A preparation method of silver nanosheets with controllable thickness comprises the following steps:
1) Uniformly mixing trisodium citrate, polyvinylpyrrolidone (PVP), copper chloride and water to obtain a first mixed solution, wherein the concentration of the trisodium citrate in the first mixed solution is 5mM, the concentration of the copper chloride in the first mixed solution is 1.5mM, and the concentration of the polyvinylpyrrolidone in the first mixed solution is 0.6wt%;
2) Mixing the first mixed solution and the silver nanosheet seed crystal sol to obtain a second mixed solution, heating the second mixed solution to 80 ℃ in a water bath (keeping the stirring condition in the heating process), simultaneously dropwise adding a silver nitrate aqueous solution with a silver nitrate concentration of 5mM and an ascorbic acid aqueous solution with an ascorbic acid concentration of 5mM to the second mixed solution at the speed of 300rpm under the stirring condition, keeping the temperature unchanged after the silver nitrate aqueous solution and the ascorbic acid aqueous solution are completely dropwise added, and reacting for 20min under the stirring condition to obtain the silver nanosheet sol, wherein the ratio of the first mixed solution to the silver nanosheet seed crystal sol is 5:1, the ratio of the silver nitrate aqueous solution to the ascorbic acid aqueous solution is 1:5, the dropping speed of the silver nitrate aqueous solution is 30mL/h, and the dropping speed of the ascorbic acid aqueous solution is 30mL/h;
the method for preparing the silver nanosheet seed sol comprises the following steps: mixing 40 parts by volume of water, 3 parts by volume of trisodium citrate aqueous solution and 1 part by volume of PVP aqueous solution, adding 1 part by volume of sodium borohydride aqueous solution under stirring, stirring for 1h, dropwise adding 0.3 part by volume of hydrogen peroxide aqueous solution, continuously stirring for 5h, and standing for 24h to obtain the silver nanosheet seed sol, wherein the concentration of trisodium citrate in the trisodium citrate aqueous solution is 0.025mol/L, the concentration of PVP in the PVP aqueous solution is 0.5 wt%, the concentration of sodium borohydride in the sodium borohydride aqueous solution is 0.1mol/L, and the concentration of the hydrogen peroxide aqueous solution is 30wt%.
3) And centrifuging the silver nanosheet sol at 3500rpm for 10min, washing the precipitate obtained by centrifuging with deionized water, and obtaining the silver nanosheet with controllable thickness.
Dispersing the precipitate obtained by centrifuging in the step 3) in deionized water to obtain a dispersion liquid, wherein the SEM of the dispersion liquid is shown in figure 3, after continuous growth, the silver nanosheet is converted into silver nanoparticles with extremely thick thickness, and the silver nanoparticles consist of top-removed triangular plates and top-removed hexagonal plates, the thickness of the nanoparticles reaches about 110nm and is almost equal to the side length.
Example 4
A preparation method of silver nanosheets with controllable thickness comprises the following steps:
1) Uniformly mixing trisodium citrate, polyvinylpyrrolidone (PVP), copper chloride and water to obtain a first mixed solution, wherein the concentration of the trisodium citrate in the first mixed solution is 5mM, the concentration of the copper chloride in the first mixed solution is 0.5mM, and the concentration of the polyvinylpyrrolidone in the first mixed solution is 0.6wt%;
2) Mixing the first mixed solution and the silver nanosheet seed crystal sol to obtain a second mixed solution, heating the second mixed solution to 80 ℃ in a water bath (keeping the stirring condition in the heating process), simultaneously dropwise adding a silver nitrate aqueous solution with a silver nitrate concentration of 5mM and an ascorbic acid aqueous solution with an ascorbic acid concentration of 5mM to the second mixed solution at the speed of 300rpm under the stirring condition, keeping the temperature unchanged after the silver nitrate aqueous solution and the ascorbic acid aqueous solution are completely dropwise added, and reacting for 20min under the stirring condition to obtain the silver nanosheet sol, wherein the ratio of the first mixed solution to the silver nanosheet seed crystal sol is 5:1, the ratio of the silver nitrate aqueous solution to the ascorbic acid aqueous solution is 1:5, the dropping speed of the silver nitrate aqueous solution is 30mL/h, and the dropping speed of the ascorbic acid aqueous solution is 30mL/h;
the method for preparing the silver nanosheet seed sol comprises the following steps: mixing 40 parts by volume of water, 3 parts by volume of trisodium citrate aqueous solution and 1 part by volume of PVP aqueous solution, adding 1 part by volume of sodium borohydride aqueous solution under stirring, stirring for 1h, dropwise adding 0.3 part by volume of hydrogen peroxide aqueous solution, continuously stirring for 5h, and standing for 24h to obtain the silver nanosheet seed sol, wherein the concentration of trisodium citrate in the trisodium citrate aqueous solution is 0.025mol/L, the concentration of PVP in the PVP aqueous solution is 0.5 wt%, the concentration of sodium borohydride in the sodium borohydride aqueous solution is 0.1mol/L, and the concentration of the hydrogen peroxide aqueous solution is 30wt%.
3) And centrifuging the silver nanosheet sol at 5000rpm for 10min, washing the precipitate obtained by centrifuging with deionized water, and obtaining the silver nanosheet with controllable thickness.
Dispersing the precipitate obtained by centrifuging in the step 3) in deionized water to obtain a dispersion liquid, wherein an SEM of the dispersion liquid is shown in figure 4, the average side length of the silver nanosheet is 217nm, and the thickness of the nanosheet is about 25nm. Under the condition of lower-concentration copper chloride, the side length and the thickness of the nanosheet can be increased simultaneously through the growth of the nanosheet.
The invention being thus described by way of example, it should be understood that any simple alterations, modifications or other equivalent alterations as would be within the skill of the art without the exercise of inventive faculty, are within the scope of the invention.
Claims (7)
1. A preparation method of silver nanosheets with controllable thickness is characterized by comprising the following steps:
1) Uniformly mixing trisodium citrate, polyvinylpyrrolidone, copper chloride and water to obtain a first mixed solution, wherein the concentration of the trisodium citrate in the first mixed solution is 0.1-50 mM, the concentration of the copper chloride in the first mixed solution is 0.1-10 mM, and the concentration of the polyvinylpyrrolidone in the first mixed solution is 0.1-5 wt%;
2) Mixing the first mixed solution and the silver nanosheet seed crystal sol to obtain a second mixed solution, heating the second mixed solution to 40-100 ℃, dropwise adding a silver nitrate aqueous solution with a silver nitrate concentration of 1-50 mM and an ascorbic acid aqueous solution with an ascorbic acid concentration of 1-50 mM to the second mixed solution at 40-100 ℃ under the condition of stirring, keeping the temperature unchanged after the silver nitrate aqueous solution and the ascorbic acid aqueous solution are completely dropwise added, and reacting for 20-30 min under the condition of stirring to obtain the silver nanosheet sol, wherein the ratio of the first mixed solution to the silver nanosheet seed crystal sol is (4-20): 1, the ratio of the silver nitrate aqueous solution to the ascorbic acid aqueous solution is 1: (1-10);
3) And centrifuging the silver nanosheet sol, washing and centrifuging the obtained precipitate to obtain the silver nanosheet with controllable thickness.
2. The preparation method according to claim 1, wherein in the step 1), the concentration of trisodium citrate in the first mixed solution is 2.0 to 5mM, the concentration of copper chloride in the first mixed solution is 0.5 to 2.0mM, and the concentration of polyvinylpyrrolidone in the first mixed solution is 0.5 to 1.0wt%.
3. The method according to claim 1, wherein in the step 2), the concentration of silver nitrate in the aqueous silver nitrate solution is 5 to 10mM, and the concentration of ascorbic acid in the aqueous ascorbic acid solution is 5 to 10mM.
4. The preparation method according to claim 1, wherein in the step 2), the dropping rates of the aqueous silver nitrate solution and the aqueous ascorbic acid solution are 20 to 40mL/h, respectively.
5. The production method according to claim 1, wherein in the step 2), the method of producing the silver nanoplate seed sol comprises: mixing 40-50 parts by volume of water, 3-5 parts by volume of trisodium citrate aqueous solution and 1-2 parts by volume of PVP aqueous solution, adding 1-2 parts by volume of sodium borohydride aqueous solution under the stirring condition, stirring for 40-60 min, dropwise adding 0.3-0.5 part by volume of hydrogen peroxide aqueous solution, continuing stirring for 2-5 h, and standing for 24-48 h to obtain the silver nanosheet seed crystal sol, wherein the concentration of trisodium citrate in the trisodium citrate aqueous solution is 25-50 mM, the concentration of PVP in the PVP aqueous solution is 0.5-0.1 wt%, the concentration of sodium borohydride in the sodium borohydride aqueous solution is 100-120 mM, and the concentration of the hydrogen peroxide aqueous solution is 20-30 wt%.
6. The method according to claim 1, wherein in the step 3), deionized water and/or ethanol are used for washing.
7. The method according to claim 1, wherein the speed of the centrifugation in the step 3) is 3000 to 5000rpm.
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