CN106541149B - A kind of accurate-size controls the preparation method of extra small nano-Ag particles - Google Patents
A kind of accurate-size controls the preparation method of extra small nano-Ag particles Download PDFInfo
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Abstract
The invention discloses the preparation methods that a kind of accurate-size controls extra small nano-Ag particles, this method is using silver nitrate as presoma, polyalcohol be solvent it is simultaneous be reducing agent, under stabilizer polyvinylpyrrolidone and the effect of inducer nickel nitrate, it the use of microwave irradiation is heat source, by controlling reactant concentration, ratio, microwave irradiation time and temperature, quickly, it is precisely controlled the continuous growth course of colloid size, reach being precisely controlled for ultra-small grain size size, it is with short production cycle, simple process, equipment is simple, it is low in cost, easy mass production, obtained nano-Ag particles particle size range is 1.91-30.5nm, minimum diameter only 1.91nm, reach nano-scale dimension to the excessive size of atom level, close to nanometer dimension limit, product purity is high, particle diameter distribution is uniform, coefficient of variation 4.7-17.3, stablize Property and monodispersity are strong, provide condition for the theoretical research and application and development of the chemically and physically characteristic of extra small nano particle.
Description
Technical field:
The present invention relates to noble silver technical field of nano material, and in particular to a kind of extra small nano silver of accurate-size control
The preparation method of particle.
Background technique:
It is silver atoms by restoring silver salt in the liquid phase silver ion reduction, silver atoms supersaturated solution is formed, from lower
Upper deposition growing nano-Ag particles.The process is roughly divided into three phases: silver ion reduction is silver atoms, silver atoms are gathered into
Core-kind crystalline substance and crystal growth.Wherein the silver atoms aggregation nucleation-kind brilliant stage directly determines the pattern and crystalline epitaxial of final product
Growth pattern controls pattern most important.The thermodynamics potential barrier that silver atoms assemble the brilliant stage nucleation of nucleation-kind is very big, anti-
It answers the initial stage, silver atoms assemble the brilliant very high silver atomic concentration of needs of nucleation-kind, and assemble nucleation-kind crystalline substance compared to silver atoms
Stage, nucleus formed after the silver atomic concentration that needs of crystal growth phase far below the former, because such brilliant once forming micelle
I.e. quick epitaxial growth, the very fast increase of crystallite dimension.The nano-Ag particles partial size prepared at present is usually in 20nm or more, nano silver
Grain diameter is rarely reported less than 10nm, and the pattern of nano-Ag particles mixes, and product purity is low, particle size uniformity is poor.
Summary of the invention:
The object of the present invention is to provide the preparation method that a kind of accurate-size controls extra small nano-Ag particles, production cycles
Short, simple process, simple, low in cost, the easy mass production of equipment, obtained nano-Ag particles minimum diameter only 1.91nm,
Reach nano-scale dimension to the excessive size of atom level, close to nanometer dimension limit, product cut size is evenly distributed, stability and single point
It is strong to dissipate property, provides condition for the theoretical research and application and development of the chemically and physically characteristic of extra small nano particle, solves existing
There are nano-Ag particles in technology to be difficult to prepare super-small, particle diameter distribution unevenness, be unable to control crystal continuous growth and be difficult to essence
The technical problem of quasi- control partial size small size.
The present invention is achieved by the following technical programs:
A kind of accurate-size controls the preparation method of extra small nano-Ag particles, and this method is polynary using silver nitrate as presoma
Alcohol be solvent it is simultaneous be reducing agent, under the action of stabilizer polyvinylpyrrolidone and inducer nickel nitrate, use microwave irradiation
For heat source, by control reactant concentration, ratio, microwave irradiation time and temperature, quickly, it is precisely controlled colloid size and continuously gives birth to
Long process reaches being precisely controlled for ultra-small grain size size, method includes the following steps:
(1) polyalcohol reagent is removed water in 105-120 DEG C of continuous drying 2h or more, by 0.01-0.04M AgNO3、2.5-
10.0mM Ni(NO3)2·6H2O and 0.09-0.15M 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 for obtaining step (1) is open, is 2450MHz micro-wave oven in 300-700W low-power 110- with frequency
150 DEG C of irradiation 2-8min, prepare the nanoscale ultra-small grain size Argent grain of different-grain diameter；After the reaction was completed, ice-water bath is used at once
Quenching, stopped reaction, reaction solution are added deionized water and dilute 2-3 times, stir 5-10min, are centrifugated after ultrasonic 5min, remove
Upper liquid, bottom micelle are successively washed 2-3 times with deionized water and dehydrated alcohol；Washed product be scattered in deionized water or
In organic solvent, stored protected from light obtains target product.
The extra small nano-Ag particles particle size range that the present invention obtains is 1.91-30.5nm, and purity is high, particle diameter distribution are uniform,
It can be precisely controlled particle size in the coefficient of variation (CV=standard deviation/average value × 100%) 4.7-17.3, product 2-10nm, directly
Diameter is lower than the nano-Ag particles coating of 5nm, under the conditions of room temperature is protected from light, can stablize holding nanotopography 7 weeks or more, standard is big
70 DEG C are resistant under air pressure.
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 8000-15000rpm, and the organic solvent is selected from dehydrated alcohol, isopropyl
One of alcohol, n-butanol.
Step (2) the washed product is scattered in deionized water or organic solvent, is preferably scattered in added with steady
Determine in deionized water or the organic solvent of agent (such as sodium citrate).
The stored protected from light is preferably stored at 4-10 DEG C, helps to extend keeping life.
Step (2) uses ice-water bath quenching, and stopped reaction prevents waste heat from causing growth of colloidal particles uneven, improves the grain of product
Diameter homogeneity.
When microwave irradiation 300-700W low-power, inducer plays sustained release local thermodynamics/dynamics unevenness, avoids secondary
Nucleation and local growth are uneven, and crystal is made to be in the continuous uniform epitaxial growth stage.It is micro- by controlling after having regulated and controled response parameter
Wave irradiation time is precisely controlled nano-Ag particles size.
Beneficial effects of the present invention are as follows:
With short production cycle, simple process, simple, low in cost, the easy mass production of equipment of the invention, obtained nano silver
Particle size range is 1.91-30.5nm, and minimum diameter only 1.91nm reaches nano-scale dimension to the excessive size of atom level, connects
Nearly nanometer dimension limit, product purity is high, particle diameter distribution is uniform, the coefficient of variation (CV=standard deviation/average value × 100%) 4.7-
17.3, stability and monodispersity are strong, and particle size can be precisely controlled in product 2-10nm, and diameter is lower than the nano silver of 5nm
Grain coating can be stablized holding nanotopography 7 weeks or more, it is super that normal atmosphere pressure, which is resistant to 70 DEG C, under the conditions of room temperature is protected from light
The theoretical research and application and development of the chemically and physically characteristic of small nano particle provide condition.
Detailed description of the invention:
Fig. 1 is transmission electron microscope (TEM) figure of the product a-i of 1-9 of the embodiment of the present invention；
Fig. 2 is partial size (diameter) distribution statistics figure of the product a-i of 1-9 of the embodiment of the present invention；
Fig. 3 is the coefficient of variation of the product a-i of 1-9 of the embodiment of the present invention with the variation diagram of its partial size；
Fig. 4 is uv-visible absorption spectroscopy (the Uv-vis absorption of the product a-i of 1-9 of the embodiment of the present invention
Spectra) figure；
Fig. 5 is transmission electron microscope (TEM) figure of products therefrom in comparative example of the present invention,
Fig. 6 is 1-3 product of embodiment of the present invention storage front and back transmission electron microscope (TEM) comparative diagram；Wherein a-1, a-2
1 product of embodiment storage front and back transmission electron microscope comparative diagram is respectively referred to, before b-1, b-2 respectively refer to the storage of 2 product of embodiment
Transmission electron microscope comparative diagram afterwards, c-1, c-2 respectively refer to 3 product of embodiment storage front and back transmission electron microscope comparative diagram.
Specific embodiment:
It is to further explanation of the invention, rather than limiting the invention below.
Embodiment 1: the preparation extra small nano-Ag particles of 1.91nm
Ethylene glycol reagent is removed water using preceding in 105-120 DEG C of continuous drying 2h or more drying, by 0.03M silver nitrate AgNO3、
2.5-5mM nickel nitrate Ni (NO3)2·6H2O and 0.14M polyvinylpyrrolidone (K30) sequentially adds the ethylene glycol of 50mL water removal
In solvent, after preservative film sealing, it is vigorously stirred 0.5-1h, 5-10min is slowly stirred and waits for after completely dissolution, removing preservative film, hold
Device is open, is at once 2450MHz micro-wave oven microwave spoke at 110-150 DEG C of low-power (300-700W) with frequency by above-mentioned solution
According to 2.5min.It is heated to after the default stage at once using ice-water bath quenching, terminating waste heat makes crystal continued growth, prevents crystal grain
Diameter is uneven.Reaction solution is added deionized water and dilutes 2-3 times, stirs 5-10min, 8000-15000rpm centrifugation point after ultrasonic 5min
From removal upper liquid, bottom micelle uses deionized water and dehydrated alcohol to wash 3 times according to this, is scattered in dehydrated alcohol and is protected from light guarantor
It deposits, product a is made, extra small nano-Ag particles diameter is 1.91 ± 0.29nm (referring to a in Fig. 1), and particle diameter distribution is uniformly (referring to figure
2), the coefficient of variation is 15.2 (referring to Fig. 3), and the local plasmon resonance body absorption spectrum under super-small is sent out with size increase
Raw " red shift " (referring to Fig. 4 is seen).Nano-Ag particles coating under the conditions of room temperature is protected from light, can stablize keep nanotopography 7 weeks with
Upper (referring to Fig. 6), normal atmosphere pressure are resistant to 70 DEG C, for the chemically and physically characteristic of extra small nano particle theoretical research and answer
Condition is provided with exploitation.
Embodiment 2: the preparation extra small nano-Ag particles of 2.7nm
Product b, extra small nano-Ag particles can be made the difference is that microwave irradiation time is 3min in reference implementation example 1
Diameter is 2.7 ± 0.47nm (see b in Fig. 1).Uniformly (referring to fig. 2), the coefficient of variation is 17.3 (referring to Fig. 3) to particle diameter distribution, is received
Rice Argent grain coating can stablize holding nanotopography 7 weeks or more (referring to Fig. 6), standard atmospheric pressure under the conditions of room temperature is protected from light
Under be resistant to 70 DEG C, provide condition for the theoretical research and application and development of the chemically and physically characteristic of extra small nano particle.
Embodiment 3: the preparation extra small nano-Ag particles of 3.83nm
Product c, extra small nano silver can be made the difference is that microwave irradiation time is 3.5min in reference implementation example 1
Grain diameter is 3.83 ± 0.65nm (see c in Fig. 1).Particle diameter distribution is uniformly (referring to fig. 2).The coefficient of variation is 17.0 (referring to Fig. 3),
Nano-Ag particles coating can be stablized holding nanotopography 7 weeks or more (referring to Fig. 6) under the conditions of room temperature is protected from light.Normal atmosphere
Pressure is resistant to 70 DEG C, provides condition for the theoretical research and application and development of the chemically and physically characteristic of extra small nano particle.
Embodiment 4: the preparation extra small nano-Ag particles of 4.65nm
Product d, extra small nano-Ag particles can be made the difference is that microwave irradiation time is 4min in reference implementation example 1
Diameter is 4.65 ± 0.65nm (see d in Fig. 1).Uniformly (referring to fig. 2), the coefficient of variation is 13.9 (referring to Fig. 3), mark to particle diameter distribution
It is resistant to 70 DEG C under quasi- atmospheric pressure, provides item for the theoretical research and application and development of the chemically and physically characteristic of extra small nano particle
Part.
Comparative example:
Reference implementation example 4, the difference is that be added without nickel nitrate, products therefrom shape mixes, size it is uneven (product
Transmission electron microscope figure is referring to Fig. 5), shape can not regulate and control, size can not control accurate；Known to Fig. 5 is compareed with Fig. 1 d: induction
Agent plays an important role in accurate-size control of the invention.When microwave irradiation 300-700W low-power, inducer plays sustained release
Local thermodynamics/dynamics is uneven, avoids secondary nucleation and local from growing uneven, crystal is made to be in continuous uniform epitaxial growth rank
Section.
Embodiment 5: the preparation extra small nano-Ag particles of 10.5nm
Reference implementation example 1, the difference is that: nickel nitrate 5.0-7.5mM, microwave irradiation time 5min can be made
Product e, extra small nano-Ag particles diameter are 10.5 ± 0.49nm (see e in Fig. 1).Particle diameter distribution is uniform (referring to fig. 2), variation lines
Number is 4.9 (referring to Fig. 3), and normal atmosphere pressure is resistant to 70 DEG C, and the theory for the chemically and physically characteristic of extra small nano particle is ground
Study carefully and provides condition with application and development.
Embodiment 6: the preparation quasi- ball of 13.1nm nano silver polyhedron
Reference implementation example 5, the difference is that: product f can be made in microwave irradiation time 5.5min, and nano-Ag particles are straight
Diameter is 13.1 ± 1.35nm (see f in Fig. 1).Uniformly (referring to fig. 2), the coefficient of variation is 10.3 (referring to Fig. 3), standard to particle diameter distribution
It is resistant to 70 DEG C under atmospheric pressure, provides item for the theoretical research and application and development of the chemically and physically characteristic of extra small nano particle
Part.
Embodiment 7: preparation 21.8nm nano-Ag particles
Reference implementation example 5, the difference is that: nickel nitrate 5.0-10.0mM, microwave irradiation time 6min can be made
Product g, nano-Ag particles diameter are 21.8 ± 1.34nm (see g in Fig. 1).Uniformly (referring to fig. 2), the coefficient of variation is particle diameter distribution
6.2 (referring to Fig. 3), normal atmosphere pressure be resistant to 70 DEG C, be extra small nano particle chemically and physically characteristic theoretical research and
Application and development provides condition.
Embodiment 8: the preparation quasi- ball of 25.6nm nano silver polyhedron
The difference is that microwave irradiation time is 6.5min product h can be made, nano-Ag particles are straight in reference implementation example 7
Diameter is 25.6 ± 1.46nm (see h in Fig. 1).Uniformly (referring to fig. 2), the coefficient of variation is 5.7 (referring to Fig. 3), standard to particle diameter distribution
It is resistant to 70 DEG C under atmospheric pressure, provides item for the theoretical research and application and development of the chemically and physically characteristic of extra small nano particle
Part.
Embodiment 9: the preparation quasi- ball of 30.5nm nano silver polyhedron
Product i, nano-Ag particles diameter can be made the difference is that microwave irradiation time is 7min in reference implementation example 7
For 30.5 ± 2.33nm (see i in Fig. 1).Uniformly (referring to fig. 2), the coefficient of variation is 7.6 (referring to Fig. 3) to particle diameter distribution, and standard is big
It is resistant to 70 DEG C under air pressure, provides condition for the theoretical research and application and development of the chemically and physically characteristic of extra small nano particle.
It should be pointed out that the bigger stability of particle size analysis and temperature tolerance are stronger, embodiment 4-13 according to thermodynamic principles
Product stability and temperature tolerance can be more preferable than embodiment 1-3.
When microwave irradiation 300-700W low-power, inducer plays sustained release local thermodynamics/dynamics unevenness, avoids secondary
Nucleation and local growth are uneven, and crystal is made to be in the continuous uniform epitaxial growth stage.After having regulated and controled response parameter, pass through control
Microwave irradiation time regulates and controls product size, this is also turned out under inducer slow releasing function, and crystal is in continuous growth phase, therefore can
To be precisely controlled nano-Ag particles size.
Claims (4)
1. the preparation method that a kind of accurate-size controls extra small nano-Ag particles, which is characterized in that the nano-Ag particles partial size
Range is 1.91-30.5nm, method includes the following steps:
(1) polyalcohol reagent is removed water in 105-120 DEG C of continuous drying 2h or more, by 0.01-0.04M AgNO3、2.5-10.0mM
Ni(NO3)2·6H2O and 0.09-0.15M 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, weight average molecular weight Mw=30000,58000 or 130000 of polyvinylpyrrolidone；
(2) solution for obtaining step (1) is open, is 2450MHz micro-wave oven at 110-150 DEG C of 300-700W low-power with frequency
2-8min is irradiated, the nanoscale ultra-small grain size Argent grain of different-grain diameter is prepared；After the reaction was completed, using ice-water bath quenching, stop
Reaction, reaction solution are added deionized water and dilute 2-3 times, stir 5-10min, are centrifugated after ultrasonic 5min, centrifuge speeds
For 8000-15000rpm, upper liquid is removed, bottom micelle is successively washed 2-3 times with deionized water and dehydrated alcohol；It is washed
Product is scattered in the deionized water or organic solvent added with sodium citrate stabilizer, and stored protected from light obtains target product；It is described
Organic solvent is selected from one of dehydrated alcohol, isopropanol, n-butanol.
2. accurate-size controls the preparation method of extra small nano-Ag particles according to claim 1, which is characterized in that step
(1) the polyalcohol reagent is selected from one or more of ethylene glycol, glycerine, polyethylene glycol.
3. the preparation method that accurate-size according to claim 1 or claim 2 controls extra small nano-Ag particles, which is characterized in that institute
Stored protected from light is stated to store at 4-10 DEG C.
4. a kind of preparation for controlling extra small nano-Ag particles using accurate-size described in any claim in claim 1-3
The extra small nano-Ag particles that method obtains, which is characterized in that the nano-Ag particles particle size range is 1.91-30.5nm, partial size
It is evenly distributed, coefficient of variation 4.7-17.3.
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| CN107570912B (en) * | 2017-08-30 | 2020-04-14 | 桂林电子科技大学 | Preparation method of nano-silver soldering paste with high wettability |
| CN107777718B (en) * | 2017-09-05 | 2019-11-22 | 航天特种材料及工艺技术研究所 | A kind of Y2O3Nano-powder and preparation method thereof |
| CN109267232B (en) * | 2018-12-04 | 2024-02-06 | 江苏和茧丝绸科技有限公司 | Antibacterial silk quilt coated with nano silver in layering mode and preparation method thereof |
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| CN102264494A (en) * | 2008-12-26 | 2011-11-30 | 同和电子科技有限公司 | Silver microparticle powder, method for producing said powder, silver paste using said powder, and method for using said paste |
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Application publication date: 20170329 Assignee: Guangxi Ouliwen Information Technology Co.,Ltd. Assignor: GUILIN University OF ELECTRONIC TECHNOLOGY Contract record no.: X2022450000388 Denomination of invention: A Preparation Method of Ultrasmall Silver Nanoparticles with Precise Size Control Granted publication date: 20190419 License type: Common License Record date: 20221226 |