CN109290588B - Preparation method of monodisperse triangular nano silver - Google Patents
Preparation method of monodisperse triangular nano silver Download PDFInfo
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- CN109290588B CN109290588B CN201811336210.2A CN201811336210A CN109290588B CN 109290588 B CN109290588 B CN 109290588B CN 201811336210 A CN201811336210 A CN 201811336210A CN 109290588 B CN109290588 B CN 109290588B
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Abstract
The invention provides a preparation method of monodisperse triangular nano silver, which comprises the following steps: (1) preparing mixed solution of n-amyl alcohol, PVP and NaOH by dripping saturated solution of sodium hydroxide/amyl alcohol, (2) adding 0.6-1.2 wt% AgNO into the mixed solution under stirring3Putting the aqueous solution into a thermostat with the temperature of 60-95 ℃ for heat treatment; (3) and centrifuging the heat-treated reaction solution to obtain the triangular nano silver sheet. The triangular nano silver sheet in the range of 35-90 nm can be prepared by respectively adjusting the addition of NaOH/amyl alcohol saturated solution and PVP. The method has the advantages of low cost, simple operation, no need of complex equipment, mass production and the like, and has wide application prospect in the aspects of solar cells, optical sensors, Surface Enhanced Raman Scattering (SERS), catalysis, biological detection and the like due to the improvement of stability and monodispersity.
Description
Technical Field
The invention relates to a preparation method of a monodisperse triangular nano silver sheet.
Background
Noble metal nanoparticles have a wide range of applications due to their unique optical, electrical and chemical properties. The triangular nano silver serving as a typical noble metal nanoparticle has wide application in the aspects of solar cells, optical sensors, Surface Enhanced Raman Scattering (SERS), catalysis and biological detection. The reported methods for synthesizing triangular nano-silver include light-induced transformation, thermodynamic transformation, template induction method, seed crystal method, etc. In the reported preparation methods, only the photoinduction method and the seed crystal method can realize the high-purity monodisperse triangular nano silver sheet with continuously adjustable size, but the photoinduction method requires continuous irradiation of light with specific frequency in the preparation process, and the size of the obtained product is regulated and controlled by changing the frequency of the irradiated light. The method has high requirements on equipment, high operation difficulty and low yield, and is not suitable for industrial mass production. The seed crystal method firstly needs to prepare seed crystals, the process is complicated, too many various reagents need to be added, the seed crystals are not easy to remove in the later period, and the prepared triangular nano-silver product has generally larger size and also lower yield. Therefore, how to simply and cheaply prepare the triangular nano silver with large yield, high purity, good monodispersity and strong biocompatibility is not only the requirement of the application of the triangular nano silver, but also the problem which needs to be solved urgently by the current preparation technology.
CN1935422A discloses a method for preparing monodisperse triangular nano silver flakes, which comprises adding silver nitrate ethanol solution into a water/PVP/pentanol system, and then carrying out heat treatment and centrifugation to obtain the triangular nano silver flakes. The method has high yield and simple operation, and the obtained triangular nano silver has high purity and is highly dependent on the quality of PVP. It was found in the experiment that when the pH of the PVP used was below 3.6, the experiment could not be repeated. Therefore, it is necessary to adjust the pH of the initial reaction solution to ensure the success rate of the experiment.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a preparation method of a triangular nano silver sheet with simple process, low cost, high purity and adjustable size.
The technical scheme is as follows: the invention provides a novel preparation method for regulating and controlling the size of a triangular nano silver sheet on the basis of a water/PVP/pentanol system originally reported by the subject group, namely triangular nano silver with different sizes is obtained by regulating the pH value in an initial reaction system. The higher the pH value in the initial reaction system, the smaller the obtained triangular nano silver scale. Because H in the reaction system increases with the initial pH of the reaction base solution+The ion concentration is continuously reduced, the reaction is driven to be carried out towards the reduction direction, thus the nucleation rate of the silver is improved, and more silver crystal nuclei can be formed in a short time. On the other hand, if the nucleation rate is too fast, more silver ions will be consumed, and the subsequent growth process will result in a shortage of silver ions, and the crystal nucleus cannot grow. The silver core and silver ions reach a dynamic equilibrium in the reaction. Therefore, the triangular nano silver with different scales can be generated due to different pH values in the initial reaction system. If the pH of the PVP used is low, H in the system after a certain period of reaction+The reduction reaction is stopped when the concentration is higher and higher, and the triangular nano silver cannot be obtained.
The pH values of different batches of PVP are generally distributed between 3 and 5, and in order to improve the repetition rate of experiments, the pH value in a reaction system needs to be adjusted. Ethanol is caused byThe method has weak acidity, and the practical experiment also finds that the time for synthesizing the triangular nano-silver by the reaction system added with the ethanol is prolonged, and the success rate is low. Therefore, it is necessary to remove ethanol from the reaction system disclosed in the CN1935422A patent and simultaneously introduce OH–Ions. According to the reaction equation:
2NaOH+2AgNO3＝2NaNO3+Ag2O↓+H2O
AgNO3the reaction with NaOH produces a white precipitate, so that AgNO must be added dropwise3Before the aqueous solution, a saturated solution of NaOH/pentanol was added. The pH value in the system is controlled to be 5-6.5 and is not more than 7 after adjustment. In addition, AgNO used in the present invention3The occupied mass ratio is higher, and therefore the yield is higher. The invention not only provides a new idea and a new method for regulating and controlling the synthesis of the nano-silver, but also ensures the success rate of the experiment.
The preparation method of the monodisperse triangular nano silver sheet comprises the following steps:
(1) and (2) preparing a mixed solution of n-amyl alcohol, PVP and NaOH by dropwise adding a saturated solution of sodium hydroxide/amyl alcohol, wherein the saturated solution of sodium hydroxide/amyl alcohol accounts for 0.1-1% by mass, the PVP accounts for 1-20% by mass, and the n-amyl alcohol accounts for 79-98.9% by mass. The addition amount of NaOH/amyl alcohol saturated solution or/and the addition amount of PVP in the system are adjusted to obtain triangular nano silver sheets with any average side length within the range of 35-90 nm;
(2) AgNO with 0.6-1.2 wt% is prepared3Adding AgNO3 aqueous solution into the mixed solution under stirring, continuously stirring, and placing into a constant temperature box at 60-95 ℃ for heat treatment. Wherein AgNO3Aqueous solution in Total Mixed solution (step 1 Mixed solution + AgNO)3Aqueous solution) is 1-8 percent;
(3) and centrifuging the heat-treated reaction solution to obtain the high-purity triangular nano silver sheet.
In the step (1), the triangular nano silver sheet with any average side length within the range of 35-90 m can be obtained by adjusting the addition amount of the NaOH/pentanol saturated solution or/and the addition amount of PVP in the system. More specifically: controlling the pH value in the system of the step (1) to be 5-7; under the condition that the dosage of other components is not changed, the purpose of adjusting the side length of a product can be realized by adjusting the adding amount (namely adjusting the pH value) of the NaOH/pentanol saturated solution in the system, namely obtaining the triangular nano silver sheet with any average side length within the range of 35-90 nm.
The stirring time in the step (2) is 5-60 minutes, and the heat treatment time is 27-40 hours.
The product can be dispersed in different solvents for standby according to different requirements.
FIG. 1 shows transmission electron micrographs and scanning electron micrographs of different-scale triangular nano-silver synthesized by adding different amounts of saturated NaOH/pentanol solution, wherein (a)35 + -4 nm, (b)55 + -5 nm, (c)65 + -6 nm, (d)70 + -7 nm, (e)80 + -9 nm, and (f)90 + -11 nm. As seen in the figure, the obtained nano silver has a triangular shape, and the triangular shape features become more and more obvious as the size of the triangle increases. FIG. 2 shows extinction spectrum curves of triangular nano-silver with different sizes, and curves a-g are extinction spectrum curves with average side lengths of 35 + -4 nm,45 + -5 nm,55 + -5 nm,65 + -6 nm,70 + -7 nm,80 + -9 nm and 90 + -11 nm, respectively. From the figure, the half-peak widths of the extinction spectrum curves are narrow, and gradually widen as the scale of the triangular nanoparticles increases.
Organic bases also make the pH of the solution high, so we tried to adjust the pH in the reaction system with organic bases:
(1) ammonia water is introduced to prepare silver ammonia solution (silver nitrate content is 0.6 wt%), and experimental results show that Ag is caused by Ag+Ions and NH3·H2And performing O complexation to obtain triangular nano silver.
(2) Dimethylformamide (DMF) is proved to have reducibility in the presence of PVP, DMF is added into a water/PVP/pentanol system in an experiment, an extinction spectrum of triangular nano silver synthesized after the addition of the DMF is shown in figure 3(a), a scanning electron microscope image is shown in figure 4(a), and the synthesized nano silver particles have a good triangular shape but the size is basically distributed between 30 and 300nm according to the display result.
(3) In the experiment, formamide is tried to be added, fig. 3(d) shows an extinction spectrum of the triangular nano-silver synthesized after formamide is added, fig. 4(d) shows a scanning electron microscope image of the triangular nano-silver synthesized after formamide is added, and the result shows that the synthesized nano-silver particles have a good triangular shape, but the size distribution of the nano-particles is wider compared with DMF.
(4) In the experiment, ethanol in the reaction system disclosed in the patent CN1935422A was removed, and only the addition amount of PVP was adjusted without adding saturated solution of NaOH/pentanol. The experimental result shows that the triangular nano silver can be synthesized, and the average size of the triangular nano silver obtained by synthesis is larger. FIGS. 3(b) and (c) show the removal of ethanol from the reaction system, with an n-pentanol addition of 60ml, PVP additions of 0.9 and 1.0g, AgNO respectively3The extinction spectrum curve of the triangular nano silver obtained by the reaction with the addition amount of the aqueous solution (0.6 wt%) of 3.9ml shows that the distribution of the in-plane dipole resonance peak is wide. FIGS. 4(b) and (c) show the SEM images of the reaction system with ethanol removed and PVP added in the amount of 0.9g and 1.0g, respectively, and show that the synthesized silver nanoparticles have good triangular shapes but wide size distribution, which also corresponds to the results shown by the extinction spectrum curve.
(5) The triangular nano silver is prepared by a seed-mediated method, namely, firstly, utilizing a water/PVP/pentanol system to react to obtain seed crystals, then dispersing the seed crystals into a silver nitrate aqueous solution, injecting the silver nitrate/seed crystal aqueous solution into a PVP pentanol mixed solution under a stirring state to form an n-pentanol/PVP/water ternary solution system with the seed crystals, continuing stirring for 30 minutes, and then placing the n-pentanol/PVP/water ternary solution system into a 95 ℃ constant temperature box for heat treatment. Fig. 5(a) is a scanning electron microscope image of the prepared triangular nano-silver plate, and fig. 5(B) is an extinction spectrum curve of the triangular nano-silver, wherein a is an extinction spectrum curve of the seed crystal; curve b is the triangular nanosilver extinction spectrum curve. The scanning electron microscope picture and the extinction spectrum curve result show that the nano particles are equally distributed widely in size.
Has the advantages that: compared with the prior art, the invention has the following remarkable characteristics:
(1) the experiment repetition rate is high, and because different batches of PVP have different pH values, in order to ensure the experiment repetition rate, the pH value of the original water/PVP/pentanol system needs to be adjusted, so that OH is introduced into the solution–Ions.
(2) Triangular nano silver sheets with average side length from 35nm to 90nm can be prepared by simply changing the content of PVP and saturated solution of NaOH/amyl alcohol according to practical requirements.
(3) Can be mass-produced.
(4) Simple process, low requirement on equipment and low cost.
Drawings
FIG. 1 is a transmission electron micrograph and a scanning electron micrograph of six representative mean side length triangular silver nanoplates made, wherein (a) 35. + -.4 nm; (b)55 +/-5 nm; (c)65 +/-6 nm; (d)70 +/-7 nm; (e)80 +/-9 nm; (f)90 +/-11 nm.
FIG. 2 is an extinction spectrum of an ethanol solution of seven representative triangular silver nanoplates with average side lengths; wherein the curves a-g point to the average side length of 35 +/-4 nm respectively; 45 +/-5 nm; 55 +/-5 nm; 65 +/-6 nm; 70 +/-7 nm; 80 +/-9 nm; 90. + -.11 nm samples.
FIG. 3 is a scanning electron microscope image of a triangular nanosilver plate prepared by removing ethanol, adding an organic base, wherein (a) 3ml of DMF is added; (b)0.9g PVP without NaOH/pentanol saturated solution; (c)1.0g PVP without NaOH/pentanol saturated solution; (d) 3ml of formamide are added.
FIG. 4 is an extinction spectrum of a triangular nanosilver plate prepared by removing ethanol and adding an organic base, wherein (a) 3ml of DMF is added; (b)0.9g PVP without NaOH/pentanol saturated solution; (c)1.0g PVP without NaOH/pentanol saturated solution; (d) 3ml of formamide are added;
FIG. 5 is a scanning electron micrograph (A) and an extinction spectrum graph (B) of a triangular silver nanoplate prepared by a seed-mediated method, wherein a is an extinction spectrum curve of a seed crystal; curve b triangle nanometer silver extinction spectrum curve.
Detailed Description
The technical solution of the present invention is described in detail below, but the scope of the present invention is not limited to the embodiments.
Example 1: the preparation method of the triangular nano silver sheet with the average side length of 35 +/-4 nm (shown in figure 1a) comprises the following steps:
(1) adding 60mL of n-amyl alcohol into a triangular flask with a plug, and adding the n-amyl alcohol into the flask under the stirring state1.8gPVP(Mw＝30000g.mol–1) Then, 500. mu.L of a saturated solution of NaOH/n-pentanol was added dropwise thereto, followed by stirring.
(2) To the Erlenmeyer flask was added 3.9mL of 1.2wt% AgNO while stirring3Continuously stirring the aqueous solution for 30 minutes to form an n-amyl alcohol/PVP/water ternary solution system, and then putting the system into a constant temperature box at 95 ℃ for heat treatment for 40 hours;
(3) and centrifuging the heat-treated reaction solution to obtain the triangular nano silver sheet.
Example 2: the preparation method of the triangular nano silver sheet with the average side length of 55 +/-5 nm (figure 1b) comprises the following steps:
(1) 60mL of n-pentanol was added to a Erlenmeyer flask with a stopper, and 1.8g of PVP (Mw 30000 g.mol.) was added with stirring–1) Then, 350. mu.L of a saturated solution of NaOH/n-pentanol was added dropwise thereto, followed by stirring.
(2) To the Erlenmeyer flask was added 3.9mL of 1.2wt% AgNO while stirring3Continuously stirring the aqueous solution for 30 minutes to form an n-amyl alcohol/PVP/water ternary solution system, and then putting the system into a constant temperature box at 95 ℃ for heat treatment for 37 hours;
(3) and centrifuging the heat-treated reaction solution to obtain the triangular nano silver sheet.
Example 3: the preparation method of the triangular nano silver sheet with the average side length of 70 +/-7 nm (shown in figure 1d) comprises the following steps:
(1) 60mL of n-pentanol was added to a Erlenmeyer flask with a stopper, and 1.8g of PVP (Mw 30000 g.mol.) was added with stirring–1) Then, 175. mu.L of a saturated solution of NaOH/n-pentanol was added dropwise thereto, followed by stirring.
(2) While stirring, 3.9mL of 0.6 wt% AgNO was added to the Erlenmeyer flask3Continuously stirring the aqueous solution for 30 minutes to form an n-amyl alcohol/PVP/water ternary solution system, and then putting the system into a constant temperature box at 95 ℃ for heat treatment for 32 hours;
(3) and centrifuging the heat-treated reaction solution to obtain the triangular nano silver sheet.
Example 4: the preparation method of the triangular nano silver sheet with the average side length of 80 +/-9 nm (shown in figure 1e) comprises the following steps:
(1) 60mL of n-pentanol was added to a Erlenmeyer flask with a stopper, and 1.8g of PVP (Mw) was added with stirring＝30000g.mol–1) Then, 100. mu.L of a saturated solution of NaOH/n-pentanol was added dropwise thereto, followed by stirring.
(2) To the Erlenmeyer flask was added 3.9mL of 1.2wt% AgNO while stirring3Continuously stirring the aqueous solution for 30 minutes to form an n-amyl alcohol/PVP/water ternary solution system, and then putting the system into a constant temperature box at 95 ℃ for heat treatment for 29 hours;
(3) and centrifuging the heat-treated reaction solution to obtain the triangular nano silver sheet.
Fitting shows that the addition of the saturated solution of NaOH/amyl alcohol has a linear relation with the scale of the triangular nano silver, and the fitting formula is as follows: and y is 23.140.115 x, wherein x is the addition amount (mu L) of saturated solution of NaOH/pentanol, y is the average size (nm) of the triangular nano silver, and the fitting degree is 0.984. PVP with different pH values is selected, the fitting formula may have differences, the pH value of the PVP used for the fitting is 3.64, and the use amount of the PVP is 1.8 g.
Claims (3)
1. A preparation method of monodisperse triangular nano silver is characterized by comprising the following steps:
(1) preparing a mixed solution of n-amyl alcohol, PVP and NaOH by dropwise adding a sodium hydroxide/amyl alcohol saturated solution, wherein the sodium hydroxide/amyl alcohol saturated solution accounts for 0.1-1% by mass, the PVP accounts for 1-20% by mass, and the n-amyl alcohol accounts for 79-98.9% by mass; the pH value in the system is controlled to be 5-7;
(2) AgNO with 0.6-1.2 wt% is prepared3Aqueous solution, adding AgNO to the mixed solution under stirring3Continuously stirring the aqueous solution, and then putting the aqueous solution into a constant temperature box at 60-95 ℃ for heat treatment; wherein AgNO3The mass ratio of the water solution is 1-8% of the total mixed solution;
(3) and centrifuging the heat-treated reaction solution to obtain the high-purity triangular nano silver sheet.
2. The method for preparing monodisperse triangular nano silver according to claim 1, wherein the method comprises the following steps: the addition of NaOH/pentanol saturated solution or/and PVP in the adjusting system in the step (1) can obtain the triangular nano silver sheet with any average side length within the range of 35-90 nm.
3. The method for preparing monodisperse triangular nano silver according to claim 1, wherein the method comprises the following steps: the heat treatment time in the step (2) is 27-40 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2007149387A2 (en) * | 2006-06-19 | 2007-12-27 | Northwestern University | Ph-controlled photosynthesis of silver nanoprisms |
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| CN1935422A (en) * | 2006-09-30 | 2007-03-28 | 南京大学 | Method for preparing single dispersion triangular nano silver slice |
| WO2010108158A2 (en) * | 2009-03-20 | 2010-09-23 | Northwestern University | Plasmon mediated, photoinduced synthesis of triangular bipyramids |
| CN102085574A (en) * | 2009-12-04 | 2011-06-08 | 深圳先进技术研究院 | Water-dispersible silver nanometer particles and preparation method thereof |
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