CN106757373B - A kind of preparation method of the quasi- ball of nano silver polyhedron - Google Patents

A kind of preparation method of the quasi- ball of nano silver polyhedron Download PDF

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CN106757373B
CN106757373B CN201611115374.3A CN201611115374A CN106757373B CN 106757373 B CN106757373 B CN 106757373B CN 201611115374 A CN201611115374 A CN 201611115374A CN 106757373 B CN106757373 B CN 106757373B
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王海龙
苗蕾
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Guilin University of Electronic Technology
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Abstract

The invention discloses a kind of preparation methods of quasi- ball of nano silver polyhedron, this method is using silver nitrate as presoma, polyalcohol is solvent and reducing agent, polyvinylpyrrolidone is end-capping reagent and stabilizer, it the use of microwave irradiation is heat source, the uniform epitaxial growth of crystal is set to reach morphology and size control in kind of a brilliant nucleation stage using inducer nickel nitrate, it is environmentally protective, simple process, it is with short production cycle, it is at low cost, production concentration purity is high, yield is high, easy mass production, obtained nano silver polyhedron torispherical looks are single, particle diameter distribution is uniform, particle size modification scope is wide, it can regulate and control within the scope of 48.7-411.9nm, the quasi- ball of nano silver polyhedron is mainly surrounded by { 111 } crystal face, physics and chemical property are stablized, monodispersity is good, local surface plasma resonance absorption spectrum Modulatory character is strong, have Excellent optics, electrical properties, are widely used.

Description

A kind of preparation method of the quasi- ball of nano silver polyhedron
Technical field:
The present invention relates to noble silver technical field of nano material, and in particular to a kind of preparation of the quasi- ball of nano silver polyhedron Method.
Background technique:
Block silver is the best noble metal of electric conductivity, and excellent thermal conductivity, the size of nano-Ag particles is in 1-100nm range It is interior, due to nano effect (skin effect, small-size effect, quantum size effect, macro quanta tunnel effect), nano-Ag particles Chemistry, optics, electricity, magnetics, mechanics, calorifics, in terms of have many Strange properties for being different from macroscopical block silver and It is concerned.For example, silver is a kind of broad spectrum type antibacterial agent, nano-Ag particles have stronger since partial size is minimum, large specific surface area Tissue permeability and surface-active, bactericidal effect is much higher than common silver;The local surface plasma of nano-Ag particles is total Vibration (localized surface plasmon resonance, abbreviation LSPR) absorption spectrum depends on its shape and size, leads to Often as size increases, red shift occurs for LSPR absorption peak, conversely, can control its LSPR characteristic by regulating and controlling nano-scale.With Nanotechnology development, nano-Ag particles have in industries such as chemical, electronics, biological medicine, the energy, environmental protection, daily necessities It is widely applied.
From crystallography analysis, silver-colored crystalline form is face-centered cubic (fcc), although { 111 } crystal face energy (γ { 111 }) is lower than { 100 } crystal face energy (γ { 100 }), but γ { 111 } and γ { 100 } is closer to, and when kind of a crystalline substance is nucleated, { 111 } crystal face is surrounded Crystal is easy to break through γ { 100 }-γ { 111 } potential barrier under thermodynamics driving, fluctuates between the crystal that different crystal faces surround Oscillation, causes crystal of different shapes to mix.Therefore preparing nano-Ag particles kind crystalline substance nucleation using Self-absorption Correction Factor is to Guan Chong It wants, the brilliant shape for directly determining final product of kind.Silver-colored kind of the crystalline substance of the brilliant nucleation stage of kind is in the fluctuation stage, and silver-colored kind of crystalline substance is by monocrystalline at this time Crystal, (wherein monocrystalline crystal and twin crystal are enclosed three kinds of crystal mixing compositions of twin crystal and polycrystalline crystal by { 100 } crystal face At polycrystalline crystal is surrounded by { 111 } crystal face), thus the method from top to bottom reported at present, in the solution prepared by silver ion reduction The final product shape of nano-Ag particles mixes, size is uneven, even reunites, is sintered, irregular shape, can not regulate and control nano silver The shape and size of grain, seriously hinder its commercial applications.
Summary of the invention:
The purpose of the present invention is lead in view of the shortcomings of the prior art, provide a kind of preparation method of quasi- ball of nano silver polyhedron Inducer effect is crossed using microwave irradiation as heat source, one kettle way prepares the quasi- ball of nano silver polyhedron, environmentally protective, simple process, life The production period is short, at low cost, product purity is high, yield height, easy mass production, obtained nano silver polyhedron torispherical looks list One, particle diameter distribution is uniformly, particle size modification scope is wide, can regulate and control within the scope of 48.7-411.9nm, physics and chemical property Stabilization, monodispersity are good.
The present invention is achieved by the following technical programs:
A kind of preparation method of the quasi- ball of nano silver polyhedron, this method using silver nitrate as presoma, polyalcohol be solvent and Reducing agent, polyvinylpyrrolidone are end-capping reagent and stabilizer, inorganic metal salt nickel nitrate are inducer, are using microwave irradiation Heat source is selectively oxidized etching to the kind crystalline substance that different crystal faces surround in kind of a brilliant nucleation stage using inducer nickel nitrate, goes The monocrystalline and twin kind surrounded except { 100 } crystal face is brilliant, only retains the polycrystalline kind crystalline substance that { 111 } crystal face surrounds, reaches shape control;Together When inducer in crystal growth phase to regulate and control local thermodynamics/dynamics uneven, eliminate because local thermodynamics/dynamics unevenness is drawn The secondary nucleation and crystal inhomogeneous growth risen, makes the uniform epitaxial growth of crystal reach morphology and size control, this method includes Following steps:
(1) polyalcohol reagent is removed water in 105-110 DEG C of continuous drying 1h or more, by 0.02-0.05M AgNO3、2.5- 7.5mM Ni(NO3)2·6H2O and 0.09-0.14M polyvinylpyrrolidone sequentially adds in the polyol solvent of water removal, sealing 0.5-1h is quickly stirred afterwards, is slowly stirred 5-10min, is dissolved it sufficiently and without concentration gradient;Wherein polyvinylpyrrolidone Concentration is calculated with monomer, the weight average molecular weight Mw=30000 of polyvinylpyrrolidone, and 58000,130000;
(2) solution that step (1) obtains is open or on container install condensation reflux unit additional, it is 2450MHz with frequency Micro-wave oven prepares that pattern is single, the uniform nano silver of particle size is more in 140-165 DEG C of irradiation 3-15min of 300-1000W power The quasi- ball of face body;After the reaction was completed, to room temperature, reaction solution is added deionized water and dilutes 2-5 times for room temperature or use water-bath quenching, 10-20min is stirred, is centrifugated after ultrasonic 5-10min, upper liquid is removed, bottom micelle successively uses deionized water and anhydrous second Alcohol washs 2-3 times;Product after washing, which is scattered in solvent, is made the quasi- ball dispersion liquid of nano silver polyhedron, solvent and polynary alcohol Product is than being (0.5-0.8): 1;Or powder-tight preservation is made in 105 DEG C of product dry 2h or more after washing.
Step (1) the polyalcohol reagent is selected from one or more of ethylene glycol, glycerine, polyethylene glycol.
Step (1) polyvinylpyrrolidone is PVPK30, PVPK29-32, PVPK88-96 of different polymerization degree, weight Average molecular weight is respectively 30000,58000,130000.
Step (2), the centrifuge speeds are 3000-8000rpm, and the solvent is selected from deionized water or anhydrous second One of alcohol, isopropanol, n-butanol.
Since polyalcohol hygroscopicity is very strong, when reaction solution capacity is big or needs long-time microwave heating, step (2) preferably exists It installs additional and is condensed back on container, prevent polyol solvent volatilization in reaction process excessive, meanwhile, the polyalcohol of volatilization is aggregated micro- On wave reactor, due to the strong hygroscopicity of polyalcohol, easily corrode microwave reactor wall.
Inducer is brilliant in kind of brilliant nucleation stage selective oxidation etching removal monocrystalline and twin kind, to only retain { 111 } The polycrystalline kind that crystal face surrounds is brilliant, reaches kind of brilliant pattern by the selective oxidation etching of inducer and controls, while inducer exists The growth phase of crystal can be sustained thermodynamics/Dynamical localization unevenness, caused by eliminating because of local thermodynamics/dynamics unevenness Secondary nucleation and crystal inhomogeneous growth, make crystal growth phase can with continuous uniform epitaxial growth, thus reach pattern and Size Control.
The quasi- ball particle size range of the nano silver polyhedron that the present invention obtains is 48.7-411.9nm, and product pattern is single, partial size It is evenly distributed, particle size modification scope is wide, physics and chemical property are stable, monodispersity is good, local surface plasma is total Absorption spectrum Modulatory character of shaking is strong.
Particularly, the nano-Ag particles of this discovery preparation are high-concentration nanoparticles, the quasi- ball dispersion liquid of nano silver polyhedron The concentration of middle nano-Ag particles is up to 1.0 × 1013NPS/mL.Nano-Ag particles micellar concentration, is estimated by constant mass: N (AgNPs) /=0.12 × 1021×m/D3(products collection efficiency calculates by 50% and (has micelle in mainly multiple centrifugal process to damage Lose), Conservative estimation products collection efficiency, actual product yield should be 90% or more);Wherein m is precursor quality, unit g, D For nano colloidal particles diameter, unit nm;Such as nano colloidal particles diameter D=50nm, forerunner weight m=0.51g, then N=4.9 ×1014(micelle density XRD standard card provides ρ=10.5g/cm to NPs (a)3);If being dispersed in 50ml dispersion liquid, NC= 1.0×1013NPs/ml。
Beneficial effects of the present invention are as follows:
One kettle way of the present invention prepares the quasi- ball of nano silver polyhedron, environmentally protective, simple process, it is with short production cycle, at low cost, Production concentration is high, and yield is high, easy mass production, and obtained nano silver polyhedron torispherical looks are single, with high purity, particle diameter distribution Uniformly, particle size modification scope is wide, can regulate and control within the scope of 48.7-411.9nm, the quasi- ball of nano silver polyhedron mainly by { 111 } crystal face surrounds, and physics and chemical property are stable, monodispersity is good, local surface plasma resonance absorption spectrum is adjustable Control property is strong, has excellent optics, electrical properties, is widely used, there is huge commercial promise.
Detailed description of the invention:
Fig. 1 is scanning electron microscope (SEM) figure of the product 1-6 product A-F of 1-6 of the embodiment of the present invention;
Fig. 2 is scanning electron microscope (SEM) figure of 7-13 product G of the embodiment of the present invention-M;
Fig. 3 is scanning electron microscope (SEM) figure for the experimental product that comparative example 2 and 3 of the present invention obtains;
Wherein, A is 2 experimental product of comparative example, and B is the experimental product of comparative example 3;
Fig. 4 is X-ray diffraction (XRD) map of 1-13 product of embodiment of the present invention A-M;
Fig. 5 is ultraviolet-visible-near infrared light optical absorption spectra (Uv-vis-NIR of 1-13 product of embodiment of the present invention A-M Absorption spectra) figure;
Fig. 6 is transmission electron microscope-power spectrum (TEM-EDS) figure of product of the present invention.
Specific embodiment:
It is to further explanation of the invention, rather than limiting the invention below.
Embodiment 1: the preparation quasi- ball of 48.7nm nano silver polyhedron
Ethylene glycol reagent is removed water using preceding in 105-110 DEG C of continuous drying 1h or more, by 0.03M AgNO3、5mM Ni (NO3)2·6H2The polyvinylpyrrolidone of O and 0.14M, Mw=30000 sequentially add in the 100mL ethylene glycol solvent of water removal, Preservative film sealing is vigorously stirred 0.5-1h, is slowly stirred 5-10min, sufficiently dissolves.Preservative film is removed, container is open, will be above-mentioned Solution is 2450MHz micro-wave oven in 140-165 DEG C of microwave irradiation 3min of 300-1000W power with frequency, is stopped after 2-3min again Microwave irradiation 1min, after the reaction was completed, room temperature is cooled to room temperature, and deionized water is added and dilutes 2-5 times, stirs 10- After 20min, ultrasonic 5-10min 3000-8000rpm be centrifugated, remove upper liquid, bottom micelle use according to this deionized water and Ethanol washing 3 times;Micelle after washing is scattered in anhydrous ethanol solvent and the quasi- ball dispersion liquid guarantor of suspension nano silver polyhedron is made It deposits, product A is made, the quasi- bulb diameter of nano silver polyhedron is 48.7 ± 2.5nm, and scanning electron microscope (SEM) figure is referring to Fig. 1 Middle A, referring to fig. 4, ultraviolet-visible-near infrared light optical absorption spectra figure is referring to A in Fig. 5, the present invention for X-ray diffraction (XRD) figure Transmission electron microscope-power spectrum (TEM-EDS) of product is referring to Fig. 6.
Embodiment 2: the preparation quasi- ball of 65.8nm nano silver polyhedron
Reference implementation example 1, the difference is that: polyvinylpyrrolidone is reduced to 0.09M, and microwave irradiation time is 4min, can be made product B, and the quasi- bulb diameter of nano silver polyhedron is 65.8 ± 3.7nm, scanning electron microscope (SEM) figure, ginseng See B in Fig. 1, product shape rule, size uniformity, shape and size are controllable.X-ray diffraction (XRD) figure is referring to fig. 4, purple Outside-visible-near-infrared optical absorption spectra figure is referring to B in Fig. 5, transmission electron microscope-power spectrum (TEM- of product of the present invention EDS) referring to Fig. 6.
Comparative example 2:
Reference implementation example 2, the difference is that: when being added without inducer nickel nitrate, microwave irradiation 4min, product obtained Shape is random, size is uneven, even aggregation of particles, can not regulate and control shape and size (its scanning electron microscope (SEM) figure ginseng See A in Fig. 3).
Embodiment 3: the preparation quasi- ball of 75.8nm nano silver polyhedron
Reference implementation example 1, the difference is that: product C, nano silver multi-panel can be made in microwave irradiation time 4-5min The quasi- bulb diameter of body is 75.8 ± 4.2nm, and scanning electron microscope (SEM) figure is referring to C in Fig. 1, X-ray diffraction (XRD) figure ginseng See Fig. 4, ultraviolet-visible-near infrared light optical absorption spectra figure is referring to C in Fig. 5, transmission electron microscope-energy of product of the present invention (TEM-EDS) is composed referring to Fig. 6.
Comparative example 3:
Reference implementation example 3, the difference is that when being added without inducer nickel nitrate, microwave irradiation 4-5min, production obtained Object shape mixes, size is uneven, can not regulate and control shape and size (its scanning electron microscope (SEM) figure is referring to B in Fig. 3).
Embodiment 4: the preparation quasi- ball of 81.7nm nano silver polyhedron
Reference implementation example 1, the difference is that: stop 2-3min after microwave irradiation 3min and irradiate 2min again, stops 2- 1min is irradiated after 3min again, product D can be made, the quasi- bulb diameter of nano silver polyhedron is 81.7 ± 2.9nm, scanning electron microscopy Mirror (SEM) figure is referring to D in Fig. 1, and X-ray diffraction (XRD) figure referring to fig. 4, join by ultraviolet-visible-near infrared light optical absorption spectra figure See D in Fig. 5, transmission electron microscope-power spectrum (TEM-EDS) of product of the present invention is referring to Fig. 6.
Embodiment 5: the preparation quasi- ball of 92.0nm nano silver polyhedron
Reference implementation example 4, the difference is that: stop 2-3min after microwave irradiation 3min and irradiate 2min again, stops 2- 2min is irradiated after 3min again, product E can be made, the quasi- bulb diameter of nano silver polyhedron is 92.0 ± 6.6nm, scanning electron microscopy Mirror (SEM) figure is referring to E in Fig. 1, and X-ray diffraction (XRD) figure referring to fig. 4, join by ultraviolet-visible-near infrared light optical absorption spectra figure See E in Fig. 5, transmission electron microscope-power spectrum (TEM-EDS) of product of the present invention is referring to Fig. 6.
Embodiment 6: the preparation quasi- ball of 100.7nm nano silver polyhedron
Reference implementation example 3, the difference is that: AgNO3Increase to 0.045M, Ni (NO3)2·6H2O increases to 7.5mM, Polyvinylpyrrolidone is 0.13M, and product F can be made, and the quasi- bulb diameter of nano silver polyhedron is 100.7 ± 6.7nm, scanning electricity Sub- microscope (SEM) figure referring to F in Fig. 1, X-ray diffraction (XRD) figure referring to fig. 4, ultraviolet-visible-near infrared light light absorption light Spectrogram is referring to F in Fig. 5, and transmission electron microscope-power spectrum (TEM-EDS) of product of the present invention is referring to Fig. 6.
Embodiment 7: the preparation quasi- ball of 111.5nm nano silver polyhedron
Reference implementation example 4, the difference is that: stop 2- after polyvinylpyrrolidone Mw=58000 microwave irradiation 3min 3min irradiates 2min again, irradiates 3min again after stopping 2-3min, and product G can be made, and the quasi- bulb diameter of nano silver polyhedron is 111.5 ± 5.4nm, scanning electron microscope (SEM) figure referring to fig. 2 in A, X-ray diffraction (XRD) figure referring to fig. 4, ultraviolet-visible- Near infrared light optical absorption spectra figure is referring to G in Fig. 5, and transmission electron microscope-power spectrum (TEM-EDS) of product of the present invention is referring to figure 6。
Embodiment 8: the preparation quasi- ball of 121.2nm nano silver polyhedron
Reference implementation example 3, the difference is that: product H, the quasi- ball of nano silver polyhedron can be made in microwave irradiation 5-6min Diameter be 121.2 ± 4.0nm, scanning electron microscope (SEM) figure referring to fig. 2 in B, X-ray diffraction (XRD) figure is referring to figure 4, ultraviolet-visible-near infrared light optical absorption spectra figure is referring to H in Fig. 5, transmission electron microscope-power spectrum of product of the present invention (TEM-EDS) referring to Fig. 6.
Embodiment 9: the preparation quasi- ball of 155.5nm nano silver polyhedron
Reference implementation example 3, the difference is that: AgNO3For 0.015M, polyvinylpyrrolidone 0.09M, microwave irradiation 8-9min, can be made product I, and the quasi- bulb diameter of nano silver polyhedron is 155.5 ± 4.1nm, scanning electron microscope (SEM) figure Middle C referring to fig. 2, X-ray diffraction (XRD) figure referring to fig. 4, ultraviolet-visible-near infrared light optical absorption spectra figure referring to I in Fig. 5, Transmission electron microscope-power spectrum (TEM-EDS) of product of the present invention is referring to Fig. 6.
Embodiment 10: the preparation quasi- ball of 184.0 ± 7.8nm nano silver polyhedron
Reference implementation example 3, the difference is that: polyvinylpyrrolidone 0.09M, Mw=58000, microwave irradiation 7- 8min, can be made product J, and the quasi- bulb diameter of nano silver polyhedron is 184.0 ± 7.8nm, scanning electron microscope (SEM) figure ginseng See D in Fig. 2, referring to fig. 4, ultraviolet-visible-near infrared light optical absorption spectra figure is referring to J in Fig. 5, originally for X-ray diffraction (XRD) figure Transmission electron microscope-power spectrum (TEM-EDS) of invention product is referring to Fig. 6.
Embodiment 11: the preparation quasi- ball of 206.8nm nano silver polyhedron
Reference implementation example 10, the difference is that: Ni (NO3)2·6H2O is 2.5mM, polyvinylpyrrolidone 0.09M, Mw=1300000, can be made product K, and the quasi- bulb diameter of nano silver polyhedron is 206.8 ± 8.8nm, scanning electron microscope (SEM) figure referring to fig. 2 in E, X-ray diffraction (XRD) figure referring to fig. 4, ultraviolet-visible-near infrared light optical absorption spectra figure referring to K in Fig. 5, transmission electron microscope-power spectrum (TEM-EDS) of product of the present invention is referring to Fig. 6.
Embodiment 12: the preparation quasi- ball of 330.8nm nano silver polyhedron
Reference implementation example 7, the difference is that: AgNO3Increase to 0.045M, Ni (NO3)2·6H2O increases to 7.5mM, Polyvinylpyrrolidone is 0.09M, Mw=1300000, can be made L, the quasi- bulb diameter of nano silver polyhedron is 330.8 ± 18.5nm, scanning electron microscope (SEM) figure referring to fig. 2 in F, X-ray diffraction (XRD) figure referring to fig. 4, ultraviolet-visible- Near infrared light optical absorption spectra figure is referring to L in Fig. 5, and transmission electron microscope-power spectrum (TEM-EDS) of product of the present invention is referring to figure 6。
Embodiment 13: the preparation quasi- ball of 411.9nm nano silver polyhedron
Reference implementation example 6, the difference is that: polyvinylpyrrolidone Mw=58000, microwave irradiation 12-15min, it can Product M is made, the quasi- bulb diameter of nano silver polyhedron is 411.9 ± 12.9nm, and scanning electron microscope (SEM) figure is referring to fig. 2 Middle G, referring to fig. 4, ultraviolet-visible-near infrared light optical absorption spectra figure is referring to M in Fig. 5, the present invention for X-ray diffraction (XRD) figure Transmission electron microscope-power spectrum (TEM-EDS) of product is referring to Fig. 6.
Scanning electron microscope (SEM) Fig. 1, Fig. 2 and Fig. 3 of the said goods, uses FESEM, S-4800, Hitachi Japan table Sign, the XRD (see Fig. 4) of above-mentioned sample use GAXRD, and PANalytical X ' pert Pro MPD powder diffractometer characterization (makes With 40KV, 40mA, Cu-Ka radiation), ultraviolet-visible-near infrared light optical absorption spectra (Uv-vis- NIR absorption spectra) figure (see Fig. 5) tested using Lambda 750, and the TEM-EDS of Fig. 6 uses Thermo power spectrum Instrument sign.
Fig. 1 and Fig. 2 shows the nano silver polyhedron torispherical looks of this method preparation single (product purity is high), particle diameter distribution Uniformly, morphology and size regulation precisely, when Fig. 3 show the effect of no inducer, the product shape of preparation irregularly or shape mix, Size is uneven, and shape and size can not regulate and control, and illustrates that inducer plays an important role to the regulation of shape and size in the present invention. The product XRD that in Fig. 4 prepared by this method shows that the quasi- ball of silver nanoparticle polyhedron is made of silver completely, face-centered cubic (fcc) crystal form, not Introduce other impurities.The TEM-EDS of Fig. 6 further proves that inducer concentrations product morphology in 2.5-7.5mM is controllable, while not Introduce impurity.Fig. 5 obtains the optical characteristics of product with change in size, as colloid size increases, local surface of micelle etc. from There is red shift in daughter resonance absorbing peak, and multipole formant occurs.The quasi- ball size of nano silver polyhedron of this method preparation Can control accurate, have excellent optics, electrical properties, application field is extensive, and industrialization prospect is wide.

Claims (3)

1. a kind of preparation method of the quasi- ball of nano silver polyhedron, which is characterized in that this method is using silver nitrate as presoma, polyalcohol For solvent and reducing agent, polyvinylpyrrolidone be end-capping reagent and stabilizer, inorganic metal salt nickel nitrate are inducer, and use is micro- It is heat source that amplitude, which is shone, is selectively oxidized in kind of a brilliant nucleation stage to the kind crystalline substance that different crystal faces surround using inducer nickel nitrate Etching reaches shape control, while inducer regulates and controls local thermodynamics/dynamics unevenness in crystal growth phase, eliminates because of local Secondary nucleation and crystal inhomogeneous growth caused by thermodynamics/dynamics is uneven, make the uniform epitaxial growth of crystal reach pattern and Size Control, the quasi- ball of nano silver polyhedron are surrounded by { 111 } crystal face, and partial size regulates and controls within the scope of 48.7-411.9nm, shape list One, particle diameter distribution is uniform, method includes the following steps:
(1) polyol solvent is removed water in 105-110 DEG C of continuous drying 1h or more, by 0.02-0.05MAgNO3、2.5-7.5mM Ni(NO3)2·6H2O and 0.09-0.14M polyvinylpyrrolidone sequentially adds in the polyol solvent of water removal, after sealing quickly 0.5-1h is stirred, 5-10min is slowly stirred, dissolves it sufficiently and without concentration gradient;Wherein polyvinylpyrrolidoneconcentration concentration with Monomer calculates, the weight average molecular weight Mw=30000 of polyvinylpyrrolidone or 58000 or 130000;
(2) by solution that step (1) obtains is open or container on install condensation reflux unit additional, be 2450MHz micro-wave oven with frequency In 140-165 DEG C of irradiation 3-15min of 300-1000W power, prepare that pattern is single, the uniform nano silver polyhedron of particle size is quasi- Ball;After the reaction was completed, room temperature or use water-bath quenching are to room temperature, and reaction solution is added deionized water and dilutes 2-5 times, stirring It is centrifugated after 10-20min, ultrasonic 5-10min, centrifuge speeds 3000-8000rpm, removes upper liquid, bottom micelle Successively washed 2-3 times with deionized water and dehydrated alcohol;Product after washing, which is scattered in solvent, is made nano silver polyhedron standard Ball dispersion liquid, solvent and polyalcohol volume ratio are (0.5-0.8): 1, the solvent is selected from deionized water or dehydrated alcohol, isopropyl One of alcohol, n-butanol;Or powder-tight preservation is made in 105 DEG C of product dry 2h or more after washing.
2. the preparation method of the quasi- ball of nano silver polyhedron according to claim 1, which is characterized in that step (1) is described polynary Alcoholic solvent is selected from one or more of ethylene glycol, glycerine, polyethylene glycol.
3. the preparation method of the quasi- ball of nano silver polyhedron according to claim 1, which is characterized in that the quasi- ball of nano silver polyhedron The concentration of nano-Ag particles is up to 1.0 × 10 in dispersion liquid13NPS/mL。
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CN102784926A (en) * 2012-07-16 2012-11-21 太原理工大学 Method for preparing spherical nano-silver particles
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