CN112008092A - Method for controlling silver-prepared nanowires by using microwave, ultrasonic and ultraviolet combined technology - Google Patents
Method for controlling silver-prepared nanowires by using microwave, ultrasonic and ultraviolet combined technology Download PDFInfo
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- CN112008092A CN112008092A CN202010891047.7A CN202010891047A CN112008092A CN 112008092 A CN112008092 A CN 112008092A CN 202010891047 A CN202010891047 A CN 202010891047A CN 112008092 A CN112008092 A CN 112008092A
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Abstract
The invention discloses a method for controlling silver nanowire preparation by using a microwave ultrasonic ultraviolet combined technology, which combines the advantages of a microwave synthesis method, an ultrasonic chemical method and an ultraviolet ray irradiation method, utilizes microwave energy to uniformly and quickly heat a reaction system, and is matched with ultrasonic cavitation to accelerate the reaction rate and improve the reaction efficiency in order to solve the problems of impure phase, uneven wire diameter, large energy loss and the like of a silver nanowire preparation in the prior art. The invention utilizes the high-energy environment provided by the synergistic effect of microwave, ultrasound and ultraviolet to replace the conventional hydrothermal heating method in the market, not only saves the reaction time, but also reduces the preparation cost of the silver nanowire, has the advantages of high synthesis efficiency and high uniform utilization rate of the product, and finally provides solid theoretical basis and practical experience for the high-efficiency synthesis and general application of the silver nanowire.
Description
[ technical field ]: the invention relates to the field of silver nanowire material preparation, in particular to a method for preparing silver nanowires controllably by utilizing a microwave ultrasonic ultraviolet combined technology.
[ background Art ] A method of: silver (Ag) is an important metal element, and its conductivity is first in all the elements. Compared with the common silver material, the silver nanowire has better electrical conductivity, thermal conductivity and stability, is widely applied to the fields of optical equipment, catalysts, field emission display, polarizing devices, photonic crystals, biochemical sensors and the like, and has huge market application value and development potential.
At present, the common methods for preparing the silver nanowire material comprise an AAO template method, a hydrothermal method, a polyol method, an electrochemical method and the like; however, the traditional preparation method has the problems of complex and harsh reaction conditions, high preparation cost, low yield and the like. Particularly, certain technical bottlenecks still exist in the aspect of efficiently and controllably synthesizing the silver nanowire material with regular appearance and uniform size.
Based on the consideration, the invention utilizes the microwave ultrasonic ultraviolet combined technology, combines the advantages of a microwave synthesis method, an ultrasonic chemical method and an ultraviolet ray irradiation method, utilizes microwave energy to uniformly and quickly heat a reaction system, accelerates the reaction rate by matching with the ultrasonic cavitation, and adopts the ionic liquid to guide growth so as to improve the reaction efficiency and simply, effectively and low-cost realize the large-scale preparation of the silver nanowires. The reaction system can accurately control the length and the diameter of the silver nanowire by adjusting key experimental parameters such as the frequency, the power and the like of microwave, ultrasound and ultraviolet, synthesize the silver nanowire material with regular appearance and uniform size, and finally provide solid theoretical basis and practical experience for the efficient synthesis and the general application of the material.
[ summary of the invention ]: the invention provides a new idea for preparing silver nanowires, adopts a microwave ultrasonic ultraviolet combined technical route, combines the advantages of a microwave synthesis method, an ultrasonic chemical method and an ultraviolet ray irradiation method, and has the advantages of simplicity, high efficiency, lower cost, controllable product and the like compared with the existing preparation method. The method is characterized in that: the reaction system is uniformly and quickly heated by microwave energy, the reaction rate is accelerated by matching with the ultrasonic cavitation, the oriented growth of the ionic liquid is facilitated, and the synthesis reaction efficiency is improved. Solves the technical problems of large energy consumption under reaction conditions and impure preparation phases. The prepared silver nanowire is expected to remarkably improve the application value of the silver nanowire in the fields of optical equipment, catalysts, field emission display, polarizing devices, photonic crystals, biochemical sensors and the like.
[ technical solution of the present invention ]: the invention relates to a method for controlling silver-prepared nanowires by using a microwave ultrasonic ultraviolet combined technology, which adopts the technical scheme that:
at room temperature, 20-100 mL of analytically pure ethylene glycol containing 1.00-20.00 g of polyvinylpyrrolidone and 1.00-20.00 g of hydrazine hydrate and 15-45 mL of iron chloride aqueous solution with the concentration of 0.1-10.0 mmol/L are added into a 50-200 mL three-neck quartz flask, then the three-neck quartz flask is transferred into an XH-300UP computer microwave ultrasonic ultraviolet light combined catalytic synthesizer, and 0.1500g of trihexyltetradecyl phosphine chloride ([ P6,6,6,14 ] is added][Cl]) Ionic liquids (a)
Wherein X-＝Cl-) The method comprises the following steps of (1) inducing the directional growth of a material, dropwise adding a silver nitrate solution into a three-opening quartz flask at a speed of 1-5 mL/min through an additional constant-pressure dropping funnel under the magnetic stirring at a rotating speed of 200-800 rpm, wherein the concentration of the silver nitrate solution is 10-400 mmol/L; after the dropwise adding is finished, carrying out reflux reaction at a constant temperature of 10-100 ℃ for 30-240 min under the synchronous action of microwave, ultrasound and ultraviolet, stopping heating when the reaction temperature exceeds a set temperature, and continuing heating when the reaction temperature is lower than the set temperature; the preparation conditions of the microwave, the ultrasonic and the ultraviolet of the synthesizer are set as follows: the microwave frequency is 2450MHz, and the microwave power is 1-1000W; the ultrasonic power is 0-1500W, and the ultrasonic frequency is 24-26 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 0.100 multiplied by 105 muW/cm2～1.999×105μW/cm2(ii) a Cooling the reaction product to room temperature, centrifuging at the rotating speed of 4000-10000 rpm for 1-10 min, washing the obtained solid product with deionized water and ethanol for 3 times, and finally drying at 50-100 ℃ for 8-12 h to obtain pure silver nanowire powder which is identical to a card number JCPDS No.04-0783, has a space point group of Fm-3m (225), has a diameter of 10-120 nm and a length of 10-150 mu m;
advantages and achievements of the present invention: the invention discloses a method for controlling silver-prepared nanowires by utilizing a microwave ultrasonic ultraviolet combined technology, which has the following advantages and beneficial effects: 1. the technical problem of low preparation speed is solved; 2. by adjusting key experimental parameters such as microwave, ultrasonic and ultraviolet frequencies, power, reaction time, reaction temperature and the like, the prepared silver nanowire can grow along a specific direction, the length and the diameter can be controlled, and the energy utilization rate is high; 3. the prepared silver nanowire is expected to remarkably improve the application value of the silver nanowire in the fields of optical equipment, catalysts, field emission display, polarizing devices, photonic crystals, biochemical sensors and the like.
Drawings
FIG. 1A roadmap for nanomaterial synthesis
The specific implementation mode is as follows:
example 1: preparation of silver nanowire sample 1 controllable by microwave ultrasonic ultraviolet coupling technology
The invention discloses a method for controlling silver-prepared nanowires by utilizing a microwave ultrasonic ultraviolet combined technology; the method is characterized in that: 100mL of analytical grade ethylene glycol containing 1.00g of polyvinylpyrrolidone, 1.00g of hydrazine hydrate and 45mL of a 5mmol/L aqueous solution of ferric chloride were put into a 100mL three-necked quartz flask at room temperature, and then the three-necked quartz flask was transferred to a computer microwave ultrasonic ultraviolet light combined catalytic synthesizer of XH-300UP, to which 0.1500g of trihexyltetradecylphosphine chloride ([ P6,6,6,14 ] was added][Cl]) Under the magnetic stirring of 500rpm, dropwise adding a silver nitrate solution into the three-mouth quartz flask at the speed of 3mL/min by an additional constant-pressure dropping funnel, wherein the concentration of silver nitrate is 200 mmol/L; after the dropwise addition is finished, carrying out reflux reaction at a constant temperature of 50 ℃ for 200min under the synchronous action of microwave, ultrasound and ultraviolet, stopping heating when the temperature exceeds a set temperature, and continuing heating when the temperature is lower than the set temperature; the preparation conditions of the microwave, the ultrasonic and the ultraviolet of the synthesizer are set as follows: microwave frequency 2450MHz and microwave power 500W; the ultrasonic power is 1000W, and the ultrasonic frequency is 24 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 0.100 multiplied by 105 muW/cm2～1.999×105μW/cm2(ii) a Cooling the reaction product to room temperature, centrifuging at 6000rpm for 5min, washing the obtained solid product with deionized water and ethanol for 3 timesAnd finally drying at 80 ℃ for 10h to obtain the pure silver nanowire powder which is inosculated with the card number JCPDS No.04-0783, has a space point group of Fm-3m (225), has a diameter of 40nm and a length of 100 mu m.
Example 2: preparation of silver nanowire sample 2 controllable by microwave ultrasonic ultraviolet coupling technology
The invention discloses a method for controlling silver-prepared nanowires by utilizing a microwave ultrasonic ultraviolet combined technology; the method is characterized in that: 80mL of analytical grade ethylene glycol containing 2.00g of polyvinylpyrrolidone, 2.00g of hydrazine hydrate and 40mL of an aqueous solution of iron chloride having a concentration of 10.0mmol/L were put into a 200mL three-necked quartz flask at room temperature, and then the three-necked quartz flask was transferred to a computer microwave ultrasonic ultraviolet light combined catalytic synthesizer model XH-300UP, and 0.1500g of trihexyltetradecylphosphine chloride ([ P6,6,6,14 ] was further added][Cl]) Under the magnetic stirring of the rotation speed of 800rpm, dropwise adding a silver nitrate solution into the three-mouth quartz flask at the speed of 5mL/min through an additional constant-pressure dropping funnel, wherein the concentration of the silver nitrate solution is 300 mmol/L; after the dropwise addition is finished, carrying out reflux reaction at a constant temperature of 90 ℃ for 200min under the synchronous action of microwave, ultrasound and ultraviolet, stopping heating when the reaction temperature exceeds a set temperature, and continuing heating when the reaction temperature is lower than the set temperature; the preparation conditions of the microwave, the ultrasonic and the ultraviolet of the synthesizer are set as follows: microwave frequency 2450MHz and microwave power 800W; the ultrasonic power is 1500W, and the ultrasonic frequency is 26 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 0.100 multiplied by 105 muW/cm2～1.999×105μW/cm2(ii) a And cooling the reaction product to room temperature, centrifuging at 10000rpm for 10min, washing the obtained solid product with deionized water and ethanol for 3 times, and drying at 100 ℃ for 12h to obtain pure silver nanowire powder which is identical to the card number JCPDS No.04-0783, has a space point group of Fm-3m (225), has a diameter of 55nm and a length of 120 mu m.
Comparative example 1 of example 1:
publication No. CN 101310899B (publication No. 2010.12.08) provides a preparation method: (1) 50ml of 0.01mol/l AgNO are added in a 100w ultrasonic water bath3And 50ml of 0.02mol/l PVPThe glycol solution is dropped into 50ml of glycol at the speed of 1 drop/second for mixing; (2) transferring the mixed solution into a 2.5GHz household microwave oven for heating, adjusting the microwave power to 100w, and carrying out microwave treatment for 5 min; (3) after the reaction is finished, cooling the obtained mixture to room temperature, and adding acetone with the volume of 400ml into the mixture to wash away the ethylene glycol and the excessive PVP; (4) performing ultrasonic treatment for 5min, and centrifuging the mixture at 10000rpm for 5 min; (5) and washing the separated solid with deionized water, performing ultrasonic treatment and centrifugal separation, repeating for 5 times to obtain solid powder, and drying in a vacuum oven for 6h to obtain the solid silver nanowire.
Only an ultrasonic water bath and a household microwave oven are selected, the extract is ethylene glycol, the microwave power is 100w, ultrasonic treatment is carried out for 5min, the speed is 10000 r/min, centrifugal separation is carried out for 5min, drying is carried out for 6h, and the silver nanowire is prepared without ultraviolet radiation catalysis.
The invention discloses a method for controlling silver-prepared nanowires by utilizing a microwave ultrasonic ultraviolet combined technology; the method is characterized in that: 100mL of analytical grade ethylene glycol containing 1.00g of polyvinylpyrrolidone, 1.00g of hydrazine hydrate and 45mL of a 5mmol/L aqueous solution of ferric chloride were put into a 100mL three-necked quartz flask at room temperature, and then the three-necked quartz flask was transferred to a computer microwave ultrasonic ultraviolet light combined catalytic synthesizer of XH-300UP, to which 0.1500g of trihexyltetradecylphosphine chloride ([ P6,6,6,14 ] was added][Cl]) Under the magnetic stirring of 500rpm, dropwise adding a silver nitrate solution into the three-mouth quartz flask at the speed of 3mL/min by an additional constant-pressure dropping funnel, wherein the concentration of silver nitrate is 200 mmol/L; after the dropwise addition is finished, carrying out reflux reaction at a constant temperature of 50 ℃ for 200min under the synchronous action of microwave, ultrasound and ultraviolet, stopping heating when the temperature exceeds a set temperature, and continuing heating when the temperature is lower than the set temperature; the preparation conditions of the microwave, the ultrasonic and the ultraviolet of the synthesizer are set as follows: microwave frequency 2450MHz and microwave power 500W; the ultrasonic power is 1000W, and the ultrasonic frequency is 24 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 0.100 multiplied by 105 muW/cm2～1.999×105μW/cm2(ii) a After cooling the reaction product to room temperature, it was centrifuged at 6000rpm for 5miAnd n, washing the obtained solid product with deionized water and ethanol for 3 times respectively, and finally drying at 80 ℃ for 10 hours to obtain pure silver nanowire powder which is identical with the card number JCPDS No.04-0783, has a space point group of Fm-3m (225), has the diameter of 40nm and the length of 100 mu m.
Claims (1)
1. The invention relates to a method for controlling silver-prepared nanowires by using a microwave ultrasonic ultraviolet combined technology, which adopts the technical scheme that:
at room temperature, 20-100 mL of analytically pure ethylene glycol containing 1.00-20.00 g of polyvinylpyrrolidone and 1.00-20.00 g of hydrazine hydrate and 15-45 mL of iron chloride aqueous solution with the concentration of 0.1-10.0 mmol/L are added into a 50-200 mL three-neck quartz flask, then the three-neck quartz flask is transferred into an XH-300UP computer microwave ultrasonic ultraviolet light combined catalytic synthesizer, and 0.1500g of trihexyltetradecyl phosphine chloride ([ P6,6,6,14 ] is added][Cl]) Ionic liquids (a)
Wherein X-＝Cl-) The method comprises the following steps of (1) inducing the directional growth of a material, dropwise adding a silver nitrate solution into a three-opening quartz flask at a speed of 1-5 mL/min through an additional constant-pressure dropping funnel under the magnetic stirring at a rotating speed of 200-800 rpm, wherein the concentration of the silver nitrate solution is 10-400 mmol/L; after the dropwise adding is finished, carrying out reflux reaction at a constant temperature of 10-100 ℃ for 30-240 min under the synchronous action of microwave, ultrasound and ultraviolet, stopping heating when the reaction temperature exceeds a set temperature, and continuing heating when the reaction temperature is lower than the set temperature; the preparation conditions of the microwave, the ultrasonic and the ultraviolet of the synthesizer are set as follows: the microwave frequency is 2450MHz, and the microwave power is 1-1000W; the ultrasonic power is 0-1500W, and the ultrasonic frequency is 24-26 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 0.100 multiplied by 105μW/cm2～1.999×105μW/cm2(ii) a Cooling the reaction product to room temperature, centrifuging at the rotating speed of 4000-10000 rpm for 1-10 min, washing the obtained solid product with deionized water and ethanol for 3 times, and finally drying at 50-100 ℃ for 8-12 h to obtain the product which is identical to the card JCPDS No.04-0783,The space point group is pure silver nanowire powder with Fm-3m (225), the diameter of 10-120 nm and the length of 10-150 mu m.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113210623A (en) * | 2021-04-30 | 2021-08-06 | 无锡纤发新材料科技有限公司 | Preparation method for synthesizing pure silver nanowires with controllable length-diameter ratio under assistance of microwaves |
| CN115582553A (en) * | 2022-10-18 | 2023-01-10 | 德清县浙工大莫干山研究院 | Method for assisting in stimulating growth of silver nanowires through ultraviolet rays |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113210623A (en) * | 2021-04-30 | 2021-08-06 | 无锡纤发新材料科技有限公司 | Preparation method for synthesizing pure silver nanowires with controllable length-diameter ratio under assistance of microwaves |
| CN115582553A (en) * | 2022-10-18 | 2023-01-10 | 德清县浙工大莫干山研究院 | Method for assisting in stimulating growth of silver nanowires through ultraviolet rays |
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