CN106541149A - 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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- CN106541149A CN106541149A CN201611115392.1A CN201611115392A CN106541149A CN 106541149 A CN106541149 A CN 106541149A CN 201611115392 A CN201611115392 A CN 201611115392A CN 106541149 A CN106541149 A CN 106541149A
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Abstract
The invention discloses a kind of accurate-size controls the preparation method of extra small nano-Ag particles，The method is with silver nitrate as presoma，Polyalcohol is solvent and is reducing agent，Under stabilizer polyvinylpyrrolidone and the effect of derivant nickel nitrate，The use of microwave irradiation is thermal 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 with low cost、Easily mass production，The nano-Ag particles particle size range for obtaining is 1.91 30.5nm，Minimum diameter only 1.91nm，Nano-scale dimension is reached to the excessive size of atom level，Close nanometer dimension limit，Product purity is high、Even particle size distribution，The coefficient of variation 4.7 17.3，Stability and monodispersity are strong，Theoretical research and application and development for the chemically and physically characteristic of extra small nano particle provides condition.
Description
Technical field：
The present invention relates to noble silver technical field of nano material, and in particular to a kind of accurate-size controls extra small Nano Silver
The preparation method of particle.
Background technology：
Be silver atoms by silver salt being reduced in the liquid phase silver ion reduction, form silver atoms supersaturated solution, 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 of crystalline substance and crystal growth.Wherein silver atoms aggregation nucleation-kind of brilliant stage directly determines the pattern and crystalline epitaxial of final product
Growth pattern, controls to pattern most important.The thermodynamics potential barrier of silver atoms aggregation nucleation-kind of brilliant stage nucleation is very big, anti-
Answer the starting stage, silver atoms aggregation nucleation-kind brilliant needs very high silver atomic concentration, and compare silver atoms aggregation nucleation-kind brilliant
Stage, nucleus formed after the silver atomic concentration that needs of crystal growth phase far below the former, therefore plant brilliant once shaping micelle
I.e. quick epitaxial growth, the very fast increase of crystallite dimension.The nano-Ag particles particle diameter for preparing at present is generally in more than 20nm, 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.
The content of the invention：
It is an object of the invention to provide a kind of accurate-size controls the preparation method of extra small nano-Ag particles, production cycle
Short, simple process, equipment are simple, with low cost, easy mass production, the nano-Ag particles minimum diameter only 1.91nm for obtaining,
Nano-scale dimension being reached to the excessive size of atom level, being close to nanometer dimension limit, product cut size is evenly distributed, stability and single point
Scattered property is strong, and the theoretical research and application and development for the chemically and physically characteristic of extra small nano particle provides condition, solves existing
In having technology, nano-Ag particles are difficult to prepare uneven super-small, particle diameter distribution, uncontrollable crystal continuous growth and are difficult to essence
It is accurate to control the undersized technical barrier of particle diameter.
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 the method is with silver nitrate as presoma, polynary
Alcohol is solvent and is reducing agent, in the presence of stabilizer polyvinylpyrrolidone and derivant nickel nitrate, using microwave irradiation
It is for thermal source, by controlling reactant concentration, ratio, microwave irradiation time and temperature, quick, be precisely controlled colloid size and continuously give birth to
Long process, reaches being precisely controlled for ultra-small grain size size, and the method is comprised the following steps：
(1) by polyalcohol reagent in 105-120 DEG C of continuous drying more than 2h eliminating water, by 0.01-0.04M AgNO3、2.5-
10.0mM Ni(NO3)2·6H2O and 0.09-0.15M polyvinylpyrrolidones are sequentially added in the polyol solvent of eliminating water, sealing
0.5-1h is quickly stirred afterwards, 5-10min is slowly stirred so as to fully dissolved and without concentration gradient；Wherein polyvinylpyrrolidone
Concentration is calculated with monomer, weight average molecular weight Mw=30000 of polyvinylpyrrolidone, and 58000,130000；
(2) solution for obtaining step (1) is open, is 2450MHz micro-wave ovens 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 completion of reaction, at once using ice-water bath
Quenching, stopped reaction, reactant liquor add deionized water to dilute 2-3 times, stir 5-10min, and centrifugation after ultrasonic 5min is removed
Upper liquid, bottom micelle deionized water and absolute ethanol washing 2-3 time successively；Scrubbed 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 is obtained is 1.91-30.5nm, and purity is high, even particle size distribution,
The coefficient of variation (CV=standard deviations/mean value × 100%) 4.7-17.3, can be precisely controlled particle size, directly in product 2-10nm
Footpath can stably keep nanotopography more than 7 weeks less than the nano-Ag particles coating of 5nm under the conditions of normal temperature lucifuge, and 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 PVPK30, PVPK29-32, PVPK88-96 for 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 absolute ethyl alcohol, isopropyl
One kind in alcohol, n-butanol.
Step (2) the scrubbed product is scattered in deionized water or organic solvent, is preferably scattered in added with steady
Determine in the deionized water or organic solvent of agent (such as sodium citrate).
The stored protected from light is preferably stored at 4-10 DEG C, contributes to extending keeping life.
Step (2) is prevented waste heat from causing growth of colloidal particles uneven, is improved the grain of product using ice-water bath quenching, stopped reaction
Footpath homogeneity.
During microwave irradiation 300-700W low-power, it is uneven that derivant plays sustained release local thermodynamics/dynamics, it is to avoid secondary
Nucleation and local growth are uneven, make crystal be in the continuous uniform epitaxial growth stage.It is after having regulated and controled response parameter, micro- by controlling
Ripple exposure time is precisely controlled nano-Ag particles size.
Beneficial effects of the present invention are as follows：
With short production cycle, simple process of the invention, equipment are simple, with low cost, easy mass production, the Nano Silver for obtaining
Particle size range is 1.91-30.5nm, 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, even particle size distribution, the coefficient of variation (CV=standard deviations/mean value × 100%) 4.7-
17.3, stability and monodispersity are strong, and particle size, Nano Silver of the diameter less than 5nm can be precisely controlled in product 2-10nm
Grain coating can stably keep nanotopography more than 7 weeks under the conditions of normal temperature lucifuge, and normal atmosphere pressure is resistant to 70 DEG C, is super
The theoretical research and application and development of the chemically and physically characteristic of little nano particle provides condition.
Description of the drawings：
Fig. 1 is transmission electron microscope (TEM) figure of the product a-i of embodiment of the present invention 1-9；
Fig. 2 is particle diameter (diameter) the distribution statisticses figure of the product a-i of embodiment of the present invention 1-9；
Fig. 3 is the variation diagram of the coefficient of variation with its particle diameter of the product a-i of embodiment of the present invention 1-9；
Fig. 4 is uv-visible absorption spectroscopy (the Uv-vis absorption of the product a-i of embodiment of the present invention 1-9
Spectra) figure；
Fig. 5 is transmission electron microscope (TEM) figure of products therefrom in comparative example of the present invention,
Fig. 6 is transmission electron microscope (TEM) compares figure before and after the storage of embodiment of the present invention 1-3 product；Wherein a-1, a-2
Before referring to that transmission electron microscope compares figure before and after the storage of 1 product of embodiment, b-1, b-2 refer to the storage of 2 product of embodiment respectively respectively
Transmission electron microscope compares figure afterwards, c-1, c-2 refer to transmission electron microscope compares figure before and after the storage of 3 product of embodiment respectively.
Specific embodiment：
The following is and the present invention is further illustrated, rather than limitation of the present invention.
Embodiment 1：Prepare the extra small nano-Ag particles of 1.91nm
Ethylene glycol reagent is dried eliminating water in 105-120 DEG C of continuous drying more than 2h using front, by 0.03M silver nitrate AgNO3、
2.5-5mM nitric acid nickel (NO3)2·6H2O and 0.14M polyvinylpyrrolidones (K30) sequentially add the ethylene glycol of 50mL eliminating waters
In solvent, after preservative film sealing, 0.5-1h is stirred vigorously, 5-10min is slowly stirred after fully dissolving, removes preservative film, held
Device is open, at once by the above-mentioned solution frequency microwave spoke that is 2450MHz micro-wave ovens at 110-150 DEG C of low-power (300-700W)
According to 2.5min.Use ice-water bath quenching after being heated to the default stage at once, terminating waste heat makes crystal continued growth, prevents crystal grain
Footpath is uneven.Reactant liquor adds deionized water to dilute 2-3 times, stirs 5-10min, 8000-15000rpm centrifugations point after ultrasonic 5min
From, upper liquid is removed, bottom micelle uses deionized water and absolute ethanol washing 3 times according to this, is scattered in absolute ethyl alcohol lucifuge guarantor
Deposit, be obtained product a, a diameter of 1.91 ± 0.29nm (referring to a in Fig. 1) of extra small nano-Ag particles, even particle size distribution is (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 with size increase
Raw " red shift " (referring to Fig. 4 is seen).Nano-Ag particles coating under the conditions of normal temperature lucifuge, can stably keep nanotopography 7 weeks with
It is upper that (referring to Fig. 6), normal atmosphere pressure is resistant to 70 DEG C, be the chemically and physically characteristic of extra small nano particle theoretical research and should
With exploitation there is provided condition.
Embodiment 2：Prepare the extra small nano-Ag particles of 2.7nm
Reference implementation example 1, difference are that microwave irradiation time is 3min, and product b, extra small nano-Ag particles can be obtained
A diameter of 2.7 ± 0.47nm (see b in Fig. 1).Even particle size distribution (referring to Fig. 2), the coefficient of variation are 17.3 (referring to Fig. 3), are received
Rice Argent grain coating can stably keep nanotopography more than 7 weeks (referring to Fig. 6), standard atmospheric pressure under the conditions of normal temperature lucifuge
Under be resistant to 70 DEG C, the theoretical research and application and development for the chemically and physically characteristic of extra small nano particle provides condition.
Embodiment 3：Prepare the extra small nano-Ag particles of 3.83nm
Reference implementation example 1, difference are that microwave irradiation time is 3.5min, and product c, extra small Nano Silver can be obtained
A diameter of 3.83 ± the 0.65nm of grain (see c in Fig. 1).Even particle size distribution (referring to Fig. 2).The coefficient of variation is 17.0 (referring to Fig. 3),
Nano-Ag particles coating can stably keep nanotopography more than 7 weeks under the conditions of normal temperature lucifuge (referring to Fig. 6).Normal atmosphere
Pressure is resistant to 70 DEG C, and the theoretical research and application and development for the chemically and physically characteristic of extra small nano particle provides condition.
Embodiment 4：Prepare the extra small nano-Ag particles of 4.65nm
Reference implementation example 1, difference are that microwave irradiation time is 4min, and product d, extra small nano-Ag particles can be obtained
A diameter of 4.65 ± 0.65nm (see d in Fig. 1).Even particle size distribution (referring to Fig. 2), the coefficient of variation are 13.9 (referring to Fig. 3), are marked
70 DEG C are resistant under quasi- atmospheric pressure, the theoretical research and application and development for the chemically and physically characteristic of extra small nano particle provides bar
Part.
Comparative example：
Reference implementation example 4, difference are to be added without nickel nitrate, products therefrom shape mixes, size it is uneven (product
Transmission electron microscope figure is referring to Fig. 5), shape cannot regulate and control, size cannot control accurate；Fig. 5 is compareed with Fig. 1 d and is understood：Induction
Agent plays an important role in the accurate-size control of the present invention.During microwave irradiation 300-700W low-power, derivant plays sustained release
Local thermodynamics/dynamics is uneven, it is to avoid secondary nucleation and local growth are uneven, make crystal be in continuous uniform epitaxial growth rank
Section.
Embodiment 5：Prepare the extra small nano-Ag particles of 10.5nm
Reference implementation example 1, difference is：Nickel nitrate is 5.0-7.5mM, and microwave irradiation time is 5min, can be obtained
Product e, a diameter of 10.5 ± 0.49nm of extra small nano-Ag particles (see e in Fig. 1).Even particle size distribution (referring to Fig. 2), variation lines
Number is 4.9 (referring to Fig. 3), and normal atmosphere pressure is resistant to 70 DEG C, is that the theory of the chemically and physically characteristic of extra small nano particle is ground
Study carefully condition is provided with application and development.
Embodiment 6：Prepare the quasi- ball of 13.1nm Nano Silver polyhedrons
Reference implementation example 5, difference is：Microwave irradiation time 5.5min, can be obtained product f, and nano-Ag particles are straight
Footpath is 13.1 ± 1.35nm (see f in Fig. 1).Even particle size distribution (referring to Fig. 2), the coefficient of variation be 10.3 (referring to Fig. 3), standard
70 DEG C are resistant under atmospheric pressure, the theoretical research and application and development for the chemically and physically characteristic of extra small nano particle provides bar
Part.
Embodiment 7：Prepare 21.8nm nano-Ag particles
Reference implementation example 5, difference is：Nickel nitrate is 5.0-10.0mM, and microwave irradiation time is 6min, can be obtained
Product g, a diameter of 21.8 ± 1.34nm of nano-Ag particles (see g in Fig. 1).Even particle size distribution (referring to Fig. 2), the coefficient of variation is
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：Prepare the quasi- ball of 25.6nm Nano Silver polyhedrons
Reference implementation example 7, difference are that microwave irradiation time is 6.5min, and product h can be obtained, and nano-Ag particles are straight
Footpath is 25.6 ± 1.46nm (see h in Fig. 1).Even particle size distribution (referring to Fig. 2), the coefficient of variation be 5.7 (referring to Fig. 3), standard
70 DEG C are resistant under atmospheric pressure, the theoretical research and application and development for the chemically and physically characteristic of extra small nano particle provides bar
Part.
Embodiment 9：Prepare the quasi- ball of 30.5nm Nano Silver polyhedrons
Reference implementation example 7, difference are that microwave irradiation time is 7min, and product i, nano-Ag particles diameter can be obtained
For 30.5 ± 2.33nm (see i in Fig. 1).Even particle size distribution (referring to Fig. 2), the coefficient of variation are 7.6 (referring to Fig. 3), and standard is big
70 DEG C are resistant under air pressure, the theoretical research and application and development for the chemically and physically characteristic of extra small nano particle provides condition.
It should be pointed out that according to thermodynamic principles, the bigger stability of particle size analysis and temperature tolerance are stronger, embodiment 4-13
Product stability and temperature tolerance can be more preferable than embodiment 1-3.
During microwave irradiation 300-700W low-power, it is uneven that derivant plays sustained release local thermodynamics/dynamics, it is to avoid secondary
Nucleation and local growth are uneven, make crystal be in the continuous uniform epitaxial growth stage.After response parameter has been regulated and controled, by control
Microwave irradiation time regulates and controls product size, and this is also demonstrated that under derivant slow releasing function, and crystal is in continuous growth phase, therefore can
To be precisely controlled nano-Ag particles size.
Claims (7)
1. a kind of accurate-size controls the preparation method of extra small nano-Ag particles, it is characterised in that the method is with silver nitrate as front
Body is driven, polyalcohol is solvent and is reducing agent, in the presence of stabilizer polyvinylpyrrolidone and derivant nickel nitrate, used
Microwave irradiation is thermal source, by controlling reactant concentration, ratio, microwave irradiation time and temperature, quickly, is precisely controlled micelle chi
Very little continuous growth course, reaches being precisely controlled for ultra-small grain size size, and the method is comprised the following steps：
(1) by polyalcohol reagent in 105-120 DEG C of continuous drying more than 2h eliminating water, by 0.01-0.04M AgNO3、2.5-10.0mM
Ni(NO3)2·6H2O and 0.09-0.15M polyvinylpyrrolidones are sequentially added in the polyol solvent of eliminating water, quick after sealing
Stirring 0.5-1h, is slowly stirred 5-10min so as to fully dissolve and without concentration gradient；Wherein polyvinylpyrrolidoneconcentration concentration with
Monomer is calculated, weight average molecular weight Mw=30000 of polyvinylpyrrolidone, and 58000,130000；
(2) solution for obtaining step (1) is open, is 2450MHz micro-wave ovens in 300-700W low-power 110-150 DEG C with frequency
Irradiation 2-8min, prepares the nanoscale ultra-small grain size Argent grain of different-grain diameter；After the completion of reaction, using ice-water bath quenching, stop
Reaction, reactant liquor add deionized water to dilute 2-3 times, stir 5-10min, and centrifugation after ultrasonic 5min removes upper liquid, bottom
Layer micelle deionized water and absolute ethanol washing 2-3 time successively；Scrubbed product is scattered in deionized water or organic solvent
In, stored protected from light obtains target product.
2. accurate-size controls the preparation method of extra small nano-Ag particles according to claim 1, it is characterised in that step
(1) the polyalcohol reagent is selected from one or more of ethylene glycol, glycerine, polyethylene glycol.
3. accurate-size according to claim 1 or claim 2 controls the preparation method of extra small nano-Ag particles, it is characterised in that step
Suddenly (2), the centrifuge speeds are 8000-15000rpm, and the organic solvent is selected from absolute ethyl alcohol, isopropanol, n-butanol
In one kind.
4. accurate-size controls the preparation method of extra small nano-Ag particles according to claim 3, it is characterised in that step
(2) the scrubbed product is scattered in deionized water or organic solvent, for be scattered in added with stabilizer deionized water or
In organic solvent.
5. accurate-size controls the preparation method of extra small nano-Ag particles according to claim 4, it is characterised in that described steady
Agent is determined for sodium citrate.
6. accurate-size according to claim 1 or claim 2 controls the preparation method of extra small nano-Ag particles, it is characterised in that institute
State stored protected from light to store at 4-10 DEG C.
7. the accurate-size in a kind of utilization claim 1-6 described in any claim controls the preparation of extra small nano-Ag particles
The extra small nano-Ag particles that method is obtained, it is characterised in that the nano-Ag particles particle size range be 1.91-30.5nm, particle diameter
It is evenly distributed, coefficient of variation 4.7-17.3.
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| CN109267232A (en) * | 2018-12-04 | 2019-01-25 | 江苏和茧丝绸科技有限公司 | A kind of layered coated have the anti bacteria natural silk of nano silver by and preparation method thereof |
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| CN106541149B (en) | 2019-04-19 |
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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 |