CN113878127B - Method for assisted synthesis of superfine nano silver wire by taking Grignard reagent as auxiliary agent - Google Patents
Method for assisted synthesis of superfine nano silver wire by taking Grignard reagent as auxiliary agent Download PDFInfo
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Abstract
The invention discloses a method for synthesizing superfine nano silver wires with the aid of Grignard reagent as an auxiliary agent, which comprises the following steps: PVP and Grignard reagent are dissolved in the same polyalcohol in sequence to prepare a solution; dissolving silver nitrate in a polyol solution; fully mixing the two solutions under the stirring condition to obtain a mixed solution; transferring the mixed solution into a round-bottom flask, heating to a specific temperature and preserving heat to obtain a nano silver wire stock solution; and (3) carrying out centrifugal washing and purification treatment on the nano silver wire stock solution to obtain the superfine nano silver wire with the average diameter of 10-25 nm and the average length of 10-25 mu m. The invention has simple process, mild condition, environment protection, high efficiency and easy realization of mass production. The synthesized nano silver wire has small wire diameter, large length-diameter ratio and high uniformity, and has extremely wide application prospect in flexible transparent conductive films.
Description
Technical Field
The invention relates to the technical field of one-dimensional nanomaterial preparation, in particular to a rapid synthesis method of an ultrafine nano silver wire for a flexible transparent conductive film, and particularly relates to a method for synthesizing the ultrafine nano silver wire with the assistance of a Grignard reagent as an auxiliary agent.
Background
With the upgrading and transformation of the electronic industry and the rapid development of the flexible transparent conductive electrode material industry technology, wearable electronic equipment, flexible solar cells, flexible supercapacitors, flexible liquid crystal displays, stretchable organic Light Emitting Diodes (LEDs), touch sensors and the like are applied in a dispute. However, it is increasingly difficult to satisfy the technical requirements of various flexible transparent electronic products by using Indium Tin Oxide (ITO) which is widely used at present, and how to develop an alternative flexible transparent conductive material of ITO is a technical problem which needs to be solved at present.
The main characteristics of conventional ITO are the combination of its "optical transparency" and "electrical conduction", which is one of the main materials for the preparation of rigid electronic products. However, indium is used as rare metal, the price is high, and the ITO layer is fragile and lacks flexibility, so that glass is required to be added as a protective layer in the use process, the difficulty and the cost of production are increased, and the development of electronic products to flexibility is hindered, so that the substitution technology of various ITO (indium tin oxide) such as metal nanowires, graphene, conductive polymers, carbon nanotubes, metal grids and the like is promoted.
Silver is well known to have excellent conductivity, and in contrast, nano silver wire technology is now mature. The conductive film made of the nano silver wire has smaller bending radius than that made of the metal grid technology, and the resistance change rate of the nano silver wire is smaller during bending, so that the nano silver wire has more advantages when being applied to a flexible display screen. Meanwhile, the nanomaterial has excellent light transmittance and flexure resistance due to the small-size effect of the nanomaterial. In addition, the preparation of the nano silver wire does not need harsh conditions such as vacuum, high temperature and the like, so that the cost can be greatly reduced, the mass production is realized, the nano silver wire becomes one of ITO (indium tin oxide) alternative materials with realistic application prospect, and is also one of key materials for manufacturing flexible electronic devices.
Among the preparation methods of nano silver wires, the most widely studied and most mature is the polyol reduction method. The method generally uses one or more inorganic auxiliary agents to assist in preparing silver nanowires, such as KBr, naCl or CuCl 2 NaCl and KBr, KCl and FeCl 3 Etc. But the diameter of the nano silver wire prepared by adopting the inorganic auxiliary agent is basically more than 20nm, and the length-diameter ratio is less than 1000. For example, silva et al (ACS nano 2016,10 (8), 7892-7900) injecting sodium bromide and silver nitrate glycol solution into polyvinylpyrrolidone glycol solution to obtain silver bromide seed crystal, and finally obtaining nano silver wire with diameter of 20nm and length of less than 20 μm. Miao et al (Chemical Engineering Journal 2018,345,260-270) synthesized nano-silver wires with diameters approaching 20nm by NaCl and KBr mediated polyol reduction. It is well known that the wire length and wire diameter of the nano silver wire are critical to the photoelectric performance of the transparent conductive film made of the nano silver wire. The transparent conductive film made of the nano silver wire with ultra-small wire diameter, ultra-high length-diameter ratio, fewer particles and good uniformity has lower sheet resistance, lower haze and higher light transmittance.
Therefore, how to provide a preparation method of ultrafine nano silver wires with small wire diameter, large length-diameter ratio, easy mass production in workshops and low cost is a problem to be solved at present.
Disclosure of Invention
Aiming at the defects of complex process, complicated process, large wire diameter, small length-diameter ratio and the like of the traditional nano silver wire synthesis process, the invention provides the synthesis method of the superfine nano silver wire, which does not need to be protected by introducing inert gas, does not need to be additionally added with seed crystal, has simple process, mild condition, is environment-friendly and efficient, and is easy to realize batch production.
In order to achieve the aim, the invention provides a method for synthesizing superfine nano silver wires with the assistance of a Grignard reagent as an auxiliary agent, which adopts the following technical scheme:
the method for synthesizing the superfine nano silver wire in one step comprises the following steps:
(1) PVP and a Grignard reagent are dissolved in the same polyalcohol in sequence to prepare a solution a for standby;
(2) Dissolving silver nitrate in polyalcohol to prepare a solution b for standby;
(3) Fully stirring and mixing the solutions prepared in the steps (1) and (2) to obtain a mixed solution c;
(4) Transferring the mixed solution obtained in the step (3) into a round-bottom flask, heating to a specific temperature, and preserving heat for a certain time at the temperature to obtain a nano silver wire stock solution;
(5) And (3) performing centrifugal washing and purification treatment on the nano silver wire stock solution obtained in the step (4) for multiple times by using deionized water and absolute ethyl alcohol, so as to obtain the superfine nano silver wire.
The polyol is selected from one of ethylene glycol, propylene glycol or glycerol.
The molar ratio of PVP and a Grignard reagent in the solution a is 1:0.001-1:0.050, the molar volume concentration of PVP is 0.007-0.040 mol/L, and the molar volume concentration of the Grignard reagent is 0.00004-0.00035 mol/L.
The molar volume concentration of the silver nitrate in the solution b is 0.05-0.50 mol/L.
The volume ratio of the solution a to the solution b is 2:1-10:1.
The polyvinylpyrrolidone (PVP) has a Mw of 40000 ～ 1300000.
The Grignard reagent is halogenated hydrocarbon magnesium halide, and the general formula is X-R-MgX, wherein X-R is halogenated hydrocarbon, and X is one of halogen chlorine and bromine.
The stirring speed of the fully stirring and mixing is 1-20r/s, and the stirring time is 1-120 min.
The volume of the mixed solution c accounts for 50% of the total volume of the round-bottomed flask.
The temperature rising rate is 1-20 ℃/min.
The heat preservation temperature is 120-180 ℃, and the heat preservation time is 20-240 min.
The mechanism of the invention comprises:
unlike the traditional synthesis of silver nanowire with inorganic halide as assistant, the assistant adopted in the invention is an organic Grignard reagent, and the addition of the assistant is more favorable for forming fine crystal nucleus in the reaction process, and the specific reaction principle is shown as follows:
X 2 -R 1 -MgX 1 +R 2 -OH→X 2 -R 1 H+Mg(OR 2 )X 1 (1)
Mg(OR 2 )X 1 +AgNO 3 →Mg(OR 2 ) + +NO 3 - +AgX 1 ↓ (2)
wherein R is 1 、R 2 Are all organic hydrocarbon radicals, X 1 、X 2 Are all halogen.
As can be seen from equations (1) and (2), the Grignard reagent releases halogen X preferentially without heating during the initial period of the reaction 1 And generating halogenated hydrocarbon, X 1 With Ag in solution + Binding to AgX 1 . The reaction formula (3) shows that the halohydrocarbon can further slowly release halogen X in the subsequent heating reaction process 2 And with Ag + Binding to AgX 2 . Compared with the traditional inorganic halogen ion, the slow silver halide forming mode is more favorable for nucleation of fine silver crystal nucleus, and provides necessary conditions for subsequent growth and final formation of superfine nano silver wire. The SEM and EDS results corresponding to the examples and comparative examples also demonstrate this conclusionAs discussed, with conventional inorganic halogen ions, silver halide particles of larger average size tend to form during the reaction; in contrast, with the organic grignard reagent according to the present invention, silver halide particles having a finer overall size tend to be formed in the reaction solution, and silver nanowires having a finer wire diameter are further formed using the silver halide particles as seed crystals.
The beneficial effects of the invention are as follows:
(1) The method does not need to be protected by introducing inert gas, does not need to additionally add seed crystal, has simple process, mild condition, environment protection and high efficiency, and is easy to realize batch production;
(2) The superfine nano silver wire prepared by the invention has the average diameter of 10-25 nm and the average length of 10-25 mu m.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a process flow diagram of the present invention.
Fig. 2 is a Transmission Electron Microscope (TEM) image of the silver nanowires prepared in example 1 of the present invention.
Fig. 3 is a Scanning Electron Microscope (SEM) image of the silver nanowires prepared in example 1 of the present invention.
Fig. 4 is a Scanning Electron Microscope (SEM) and energy spectrum (EDS) of silver halide particles prepared in example 2 of the present invention.
Fig. 5 is a Scanning Electron Microscope (SEM) image of the silver nanowires prepared in example 2 of the present invention.
Fig. 6 is a Scanning Electron Microscope (SEM) image of the silver nanowires prepared in example 2 of the present invention.
Fig. 7 is a Scanning Electron Microscope (SEM) and energy spectrum (EDS) diagram of the silver halide particles prepared in comparative example 1 of the present invention.
Fig. 8 is a Scanning Electron Microscope (SEM) image of the silver nanowires prepared in comparative example 1 of the present invention.
Fig. 9 is a Scanning Electron Microscope (SEM) image of the silver nanowires prepared in comparative example 1 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The method for synthesizing the superfine nano silver wire in one step comprises the following steps:
(1) PVP and a Grignard reagent are dissolved in the same polyalcohol in sequence to prepare a solution a for standby;
(2) Dissolving silver nitrate in polyalcohol to prepare a solution b for standby;
(3) Fully stirring and mixing the solutions prepared in the steps (1) and (2) to obtain a mixed solution c;
(4) Transferring the mixed solution obtained in the step (3) into a round-bottom flask, heating to a specific temperature, and preserving heat for a certain time at the temperature to obtain a nano silver wire stock solution;
(5) And (3) performing centrifugal washing and purification treatment on the nano silver wire stock solution obtained in the step (4) for multiple times by using deionized water and absolute ethyl alcohol, so as to obtain the superfine nano silver wire.
The polyol is selected from one of ethylene glycol, propylene glycol or glycerol.
The molar ratio of PVP and a Grignard reagent in the solution a is 1:0.001-1:0.050, the molar volume concentration of PVP is 0.007-0.040 mol/L, and the molar volume concentration of the Grignard reagent is 0.00004-0.00035 mol/L.
The molar volume concentration of the silver nitrate in the solution b is 0.05-0.50 mol/L.
The volume ratio of the solution a to the solution b is 2:1-10:1.
The polyvinylpyrrolidone (PVP) has a Mw of 40000 ～ 1300000.
The Grignard reagent has a general formula of X-R-MgX, wherein X-R is halogenated hydrocarbon, and X is one of halogen chlorine and bromine.
The stirring speed of the stirring and mixing is 1-20r/s, and the stirring time is 10-120 min.
The volume of the mixed solution c accounts for 50% of the total volume of the round-bottomed flask.
The heat preservation temperature is 120-180 ℃, and the heating rate is 1-20 ℃/min; the heat preservation time is 20-240 min.
The invention is further illustrated by the following examples.
Example 1
(1) 0.172g PVP (molecular weight Mw=40000) and 3.2 mu L of 5-chloro-2-thienyl magnesium bromide are dissolved in 40mL of propylene glycol to prepare a solution a for later use;
(2) Dissolving 0.17g of silver nitrate in 20mL of propylene glycol to prepare a solution b for later use;
(3) Pouring the solution b into the solution a, and fully mixing for 120min at the stirring speed of 1r/s to obtain a mixed solution c;
(4) Transferring the mixed solution c into a 150mL round-bottom flask, raising the temperature to 120 ℃ at a heating rate of 1 ℃/min, and preserving the temperature at 120 ℃ for 240min;
(5) And (3) carrying out centrifugal washing and purification treatment on the prepared nano silver wire stock solution for a plurality of times by using deionized water and absolute ethyl alcohol, thus obtaining the superfine nano silver wire with the average diameter of 10nm, the average length of 10 mu m and uniform length and fewer nano particles. Transmission electron microscopy and scanning electron microscopy of silver nanowires prepared from this example are shown in figures 2 and 3.
Example 2
(1) 0.15g PVP (molecular weight Mw=1300000) and 140 mu L (2-bromothiophene-3-yl) magnesium chloride are dissolved in 200mL of ethylene glycol to prepare a solution a for later use;
(2) 1.7g of silver nitrate is dissolved in 20mL of glycol to prepare a solution b for standby;
(3) Pouring the solution b into the solution a, and fully mixing for 10min at a stirring speed of 20r/s to obtain a mixed solution c;
(4) The mixed solution c was transferred into a 500mL round bottom flask, raised to 180℃at a heating rate of 20℃per minute, and incubated at 180℃for 20min. In the heating process, when the temperature is raised to 70 ℃, part of samples are timely removed, and Scanning Electron Microscope (SEM) and energy spectrum (EDS) analysis is carried out, wherein the specific result is shown in figure 4;
(5) And (3) carrying out centrifugal washing and purification treatment on the prepared nano silver wire stock solution for a plurality of times by using deionized water and absolute ethyl alcohol, thus obtaining the superfine nano silver wire with the average diameter of 25nm, the average length of 25 mu m and uniform length and fewer nano particles. Scanning electron microscopy images of silver nanowires prepared from this example are shown in figures 5 and 6.
Comparative example 1
(1) Dissolving 1.0g PVP (molecular weight Mw=1300000), 0.004g sodium bromide and 0.0024g sodium chloride in 130mL ethylene glycol to prepare a solution a for later use;
(2) 1.4g of silver nitrate is dissolved in 20mL of glycol to prepare a solution b for standby;
(3) Pouring the solution b into the solution a, and fully mixing for 10min at a stirring speed of 20r/s to obtain a mixed solution c;
(4) Transferring the mixed solution c into a 300mL round-bottom flask, raising the temperature to 180 ℃ at a heating rate of 20 ℃/min, and preserving the temperature at 180 ℃ for 20min; in the heating process, when the temperature is raised to 70 ℃, part of samples are timely removed, and Scanning Electron Microscope (SEM) and energy spectrum (EDS) analysis is carried out, wherein the specific result is shown in figure 7;
(5) And (3) carrying out centrifugal washing and purification treatment on the prepared nano silver wire stock solution for multiple times by using deionized water and absolute ethyl alcohol to obtain the nano silver wire with the average diameter of 50nm, the average length of 3 mu m, higher particle content and more short rods. Scanning electron microscopy images of silver nanowires prepared from this comparative example are shown in figures 8 and 9.
As can be seen from the above figures, the nano silver wires prepared by the method can obtain finer average diameter and longer average length, and have better overall uniformity, and the products prepared by the method are not compared with products prepared by the method, and have higher impurity particle content and more short rod-shaped nano silver wires.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. The method for synthesizing the superfine nano silver wire with the assistance of the Grignard reagent is characterized by comprising the following steps of:
step 1, PVP and Grignard reagent are dissolved in the same polyalcohol in sequence to prepare a solution a for standby;
step 2, silver nitrate is dissolved in polyalcohol to prepare a solution b for standby;
step 3, fully stirring and mixing the solutions prepared in the step 1 and the step 2 to obtain a mixed solution c;
step 4, transferring the mixed solution obtained in the step 3 into a round-bottom flask, heating to 120-180 ℃, and preserving heat for a certain time at the temperature to obtain a nano silver wire stock solution;
step 5, centrifugally washing and purifying the nano silver wire stock solution obtained in the step 4 to obtain the superfine nano silver wire;
the Grignard reagent is halogenated hydrocarbon magnesium halide, and the general formula of the Grignard reagent is X-R-MgX, wherein X-R is halogenated hydrocarbon, and X is one of chlorine and bromine.
2. The method according to claim 1, wherein the molar ratio of PVP to grignard reagent in the solution a is 1:0.001-1:0.050, the molar volume concentration of PVP is 0.007-0.040 mol/L, and the molar volume concentration of grignard reagent is 0.00004-0.00035 mol/L.
3. The method according to claim 1, wherein the molar volume concentration of silver nitrate in the solution b is 0.05-0.50 mol/L.
4. The method according to claim 1, wherein the volume ratio of the solution a to the solution b is 2:1 to 10:1.
5. The method of claim 1, wherein the PVP has a Mw of 40000 ～ 1300000.
6. The method according to any one of claims 1 to 5, wherein the polyol is selected from one of ethylene glycol, propylene glycol or glycerol.
7. The method according to any one of claims 1 to 5, wherein the stirring speed of the stirring and mixing is 1 to 20r/s and the stirring time is 1 to 120min.
8. The method according to any one of claims 1 to 5, wherein in step 4, the rate of temperature increase is 1 to 20 ℃/min; the heat preservation time is 20-240 min.
9. The method according to any one of claims 1 to 5, characterized in that in step 5 the centrifugal washing is in particular a multiple centrifugal washing with deionized water and absolute ethanol.
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