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Large-scale preparation method of silver nano-sheets

A silver nanosheet, a large number of technologies, applied in the field of nanomaterials, can solve the problems of difficult dispersion of product agglomeration, small product concentration, complex reaction system, etc., and achieve the effect of no exhaust gas emission, simple equipment, and good dispersion

Inactive Publication Date: 2015-04-29
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The main disadvantage of the above silver nanosheet preparation technology is that the concentration of silver source solution in the reaction system is low, the output is too small, it is difficult to realize large-scale preparation, and some reaction systems are complex, the process conditions are difficult to accurately control, the requirements for equipment are high, and the product morphology Diverse, wide size distribution; some systems such as polyols and PVP require higher reduction temperature, longer reaction time, and the price of raw polyols is relatively high; The group is not easy to remove and degrade, which will pollute the environment and is not environmentally friendly; some preparation systems use sodium borohydride as a reducing agent, and the size of the prepared silver nanosheets is relatively small, and the concentration of the product in the system is relatively small; some systems use Glucose is used as a reducing agent, which has a high viscosity, which will make the product agglomerated and difficult to disperse, which is not conducive to application

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0031] A method for preparing silver nanosheets in large quantities, the steps are as follows:

[0032] (1) At a temperature of 30°C, disperse the silver nanosheet seed crystals in water to obtain a suspension with a solid content of 0.03g / L, then add 2mL of the suspension to 415mL of a 0.28mmol / L sodium citrate aqueous solution In the solution, stir and mix evenly, add 21 μL of hydrazine hydrate, and then slowly add 3 mL of silver nitrate aqueous solution with a concentration of 59 mmol / L. The injection time of the silver nitrate aqueous solution is 1 min, and the reaction is stirred at a constant temperature for 1 h to generate a product suspension;

[0033] (2) Centrifuge and wash the product suspension generated in step (1) to obtain the product. The yield is 99%, the purity is 95%, the side length of the silver nanosheet is about 95nm±8nm, and the thickness is 20±1.2nm.

Embodiment 2

[0035] A method for preparing silver nanosheets in large quantities, the steps are as follows:

[0036] (1) At a temperature of 30°C, disperse the silver nanosheet seed crystals in water to obtain a suspension with a solid content of 0.03g / L, then add 2mL of the suspension to 415mL of a 1.3mmol / L sodium citrate aqueous solution In the solution, stir and mix evenly, add 110 μL of hydrazine hydrate, and then slowly add 15 mL of silver nitrate aqueous solution with a concentration of 59 mmol / L. The injection time of the silver nitrate aqueous solution is 10 minutes, and the reaction is stirred at a constant temperature for 1 hour to generate a product suspension;

[0037] (2) Centrifuge and wash the product suspension generated in step (1) to obtain the product. The yield is 99%, the purity is 93%, the side length of the silver nanosheet is about 111±15nm, and the thickness is 19±2.2nm.

Embodiment 3

[0039] A method for preparing silver nanosheets in large quantities, the steps are as follows:

[0040](1) At a temperature of 30°C, disperse the silver nanosheet seed crystals in water to obtain a suspension with a solid content of 0.03g / L, then add 10mL of the suspension to 75mL of a sodium citrate aqueous solution with a concentration of 8.2mmol / L In the solution, stir and mix evenly, add 110 μL of hydrazine hydrate, and then slowly add 15 mL of silver nitrate aqueous solution with a concentration of 59 mmol / L. The injection time of the silver nitrate aqueous solution is 10 minutes, and the reaction is stirred at a constant temperature for 1 hour to generate a product suspension;

[0041] (2) Centrifuge and wash the product suspension generated in step (1) to obtain the product. The yield is 95%, the purity is 98%, the side length of the silver nanosheet is about 102±7nm, and the thickness is 19±2.2nm.

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Abstract

The invention relates to a large-scale preparation method of silver nano-sheets; the method comprises the steps: (1) dispersing the seed crystals of the silver nano-sheets in water to form a suspension liquid with solid content of 0.01-1.6g / L, adding citric acid or sodium citrate solution with concentration of 0.06-170g / L to the suspension liquid, stirring and mixing uniformly, adding hydrazine hydrate or ascorbic acid, slowing adding silver nitrate or silver acetate with concentration of 0.2-250g / L, performing constant-temperature stirring reaction for 30 min to 4h to generate the silver nano-sheets; and (2) obtaining the finished silver nano-sheets after filtering and washing the silver nano-sheets generated in the step (1). Not only the silver nano-sheets prepared by the method are high in yield, high in purity, uniform in appearance, good in dispersibility and good in stability, but the needed equipment is simple in structure, convenient in operation and low in cost and has no emission of waste gas; the produced waste liquid is easy to be processed and the silver nano-sheets are applicable to large-scale preparation.

Description

technical field [0001] The invention relates to a method capable of preparing silver nanosheets in large quantities, and belongs to the technical field of nanomaterials. Background technique [0002] Flake silver powder has a relatively large specific surface area, low surface energy, low oxidation degree and oxidation potential, surface contact or line contact between particles, relatively low resistance, and good conductivity. It is ideal for optical sensors, capacitors, and filters. , carbon film potentiometer, membrane switch, semiconductor chip and other electronic components as the main electrode material. Mirkin et al. used the method of light irradiation to prepare triangular silver nanosheets for the first time (Science 2001, 294 (5548), 1901). The experiment found the quadrupole plasmon resonance of nanomaterials. The strong absorption capacity of triangular silver nanosheets in the infrared region makes It has great application potential in the fields of biosensi...

Claims

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Application Information

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IPC IPC(8): B22F9/24
Inventor 陈代荣田尚玲焦秀玲陈波
Owner SHANDONG UNIV
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