CN106735300A - A kind of synthetic method of ultra-thin silver nanoparticle plate - Google Patents
A kind of synthetic method of ultra-thin silver nanoparticle plate Download PDFInfo
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Abstract
The present invention is the synthetic method of ultra-thin silver nanoparticle plate, and the method includes：The seed-solution of crystal seed type highly consistentization is prepared by adding a large amount of and excessive hydrogen peroxide and strong reductant in the mixed solution to silver nitrate and surfactant；Using seed-solution, by controlling the amount of reducing agent and silver nitrate in course of reaction, it is controllable to obtain pattern, size, and monodispersed the first silver nanoparticle plate；Second silver nanoparticle plate with random " gap " and " focus " is obtained by the continuous growth of many wheels；By introducing halide ion/hydrogen peroxide etching defect, take turns continuous growth more and obtain the smooth superelevation draw ratio in edge, super large and the third ultra-thin silver nanoparticle plate；And by wrapping up the nano-plates of above-mentioned three kinds of unique structures, obtain the ultra-thin silver nanoparticle plate of core shell structure.The present invention creatively proposes a kind of preparation method of the nano-plates structure with random " gap " and " focus "；Solve the problem of silver nanoparticle plate material stability difference.
Description
Technical field
The present invention relates to nanophotonics, phasmon, infrared optics, nano material, printed electronic and thin-film device
Field, the synthesis of more particularly to ultra-thin silver nanoparticle plate and size, morphological control method.
Background technology
Silver nanoparticle plate is a kind of special two-dimension nano materials, with unique physics, chemical property.Especially in optics side
Face, with surface phasmon (SPs) effect.In illumination, the electronics of silver nanoparticle plate surface free vibration is mutual with incident light
Effect, forms resonance, produces the local electromagnetic wave transmitted along surface.Its property has close ties with scantling.
Width has local surface etc. at several nanometers to the small size silver nanoparticle plate between tens nanometer in visible light wave range
From plasmon resonance effect (LSPR), local optical intensity density can be caused significantly to strengthen by light field local around particle.In size and
In the case of pattern is in monodispersed, the resonance absorbing peak of silver nanoparticle plate solution is unimodal, and peak value is with the increase of nanometer board size
Red shift, causes macroscopical sample to have a series of different colors such as Huang, orange, plum, purple, indigo plant.Importantly, sample single dispersing degree
Better, the halfwidth of resonance absorbing peak is narrower.On this basis, the small size nano-plates of high yield can be assembled to form the thin of macroscopic view
Membrane module, by the size for adjusting nano-plates, you can realize the accuracy controlling of local light distribution.Except thin-film device, small chi
Very little silver nanoparticle plate is also widely used for printed electronic field, makes electrically conductive ink.There are some researches show leading for, same size
Line, sample 4 orders of magnitude smaller than the sample resistance that silver nanoparticle ball is constituted being made up of silver nanoparticle plate, can effectively reduce the electricity of wire
Resistance.This be because metal particle size is smaller, its atom it is more living more, be more suitable as electrically conductive ink, and silver nanoparticle plate is two dimension
Anisotropic nano material, size in a thickness direction is only several nanometers, much smaller than the nano particle of other various patterns.
Therefore, silver nanoparticle plate easily forms welding effect each other, and then forms block materials, therefore conductance is significantly higher than it
The wire that his pattern nano particle is formed.And with the lifting of nano-plates yield, the thickness of nano-plates is thinner, nanometer in ink
Grain morphological regions homogenization, the wire and the resistance of electronic device for being printed can also be reduced further, and performance can also be significantly improved.
In sum, high yield, the ultra-thin single dispersing silver nanoparticle plate of small size are prepared, is metal nano material and device arts
One research focus, can solve the bottleneck problem of above-mentioned various application fields.
The synthetic method of existing small size silver nanoparticle plate has：Photo-reduction, electrochemical process, supercritical ultrasonics technology etc., this
A little method cycles are long, low yield is, it is necessary to pass through purification to improve yield.Seeded growth method is by by the generation of crystal seed by contrast
Separated with growth course, the condition of requirement according to different times kinetics control reaction, from pattern, size can be obtained
Controllable silver nanoparticle plate sample.But sample prepared by existing crystal seed method, mostly there is very a high proportion of spherical in final product
Particle, it is impossible to realize monodispersed silver nanoparticle plate.Its Main Bottleneck is that the crystal seed of initial reaction stage generation cannot be screened fully,
The crystal seed type for being generated is various, and including single crystal seed and twin crystal seed etc., different types of crystal seed is obtained by continuous growth
Granule-morphology is different, so as to directly affects the raising of yield.Therefore, it is badly in need of introducing more efficient Filtering system, realizes brilliant
Highly consistentization of type.Highly consistentization of crystal seed can also cause that the controllability of continuous growth work strengthens simultaneously, can improve
Solution concentration, acquisition yield is high, concentration high crystalline is good, size adjustable silver nanoparticle plate.
Size in hundreds of nanometers to the large-sized nano-plates between some tens of pm, its surface plasmon resonance (SPR)
Peak can red shift to mid and far infrared, even terahertz wave band is formed in infrared and terahertz wave band new opplication.Therefore, develop
Go out large-sized silver nanoparticle plate, can fill up these wave bands can use the blank of surface plasmons metal nano plate material.Meanwhile,
Size is a kind of important sub-wavelength fiber waveguide transmission medium in large-sized silver nanoparticle plate of hundreds of nanometers to some tens of pm.By
There is surface phasmon effect in silver nanoparticle plate, light local can be propagated in sub-wavelength spatial, the pattern hot spot of formation is remote
Less than traditional Medium Wave Guide, optical diffraction limit is broken through, drastically increase the integrated level of photonic device, be to realize the next generation
The key raw material of ultralarge scale integration photon chip system.The large scale silver nano material of mono-crystalline structures is inherently a kind of
High-quality two-dimensional waveguide, can transmit subwavelength information on two dimensional surface.Meanwhile, if introduced on large scale silver nanoparticle plate
Special sub-wavelength structure, forms " focus ", in also subwavelength information being scattered into space, also can further strengthen light and thing
Interaction between matter, this will be people in the case of diffraction limit is broken through, probe under meso-scale between light and material
The physics law of interaction provides new technical method.Therefore, the silver nanoparticle plate of large scale smooth surface, and surface is repaiied
Decorations, produce the large scale silver nanoparticle plate of focus, have important application prospect in field of nanometer technology.
At this stage, this large area and large-sized silver nanoparticle film are prepared mainly by traditional coating technique, then are passed through
The operations such as photoetching, etching are shaped.This method complex process, high cost, and the silver nanoparticle film produced is
Amorphous, substantially, loss is very big, and prepared device performance is low for scattering effect when electronics and photon are transmitted wherein, it is impossible to full
The application requirement on full border.Therefore researchers propose the Yin Na more than a few micrometers magnitude with the monocrystalline and size of chemical synthesis
Rice plate, instead of silver nanoparticle film prepared by film deposition techniques, as the raw material for preparing metal waveguide device.But existingization
The silver nanoparticle plate of method synthesis, typically more than 100 nanometers, thinner large-sized silver nanoparticle plate there is no method to pass through to change to thickness
Method is prepared, and cannot also meet existing requirement on devices.Theoretical research shows, only when the thickness of silver nanoparticle plate is reduced to
During 20 ran, its loss can just be significantly reduced, and meet the requirement of actual nanometer waveguide device.Therefore for solve etc. from
The loss problem of excimer waveguide device, improves device performance, and large scale, ultra-thin silver nanoparticle plate can be prepared in the urgent need to inventing
Chemical synthesis process.
The content of the invention
Technical problem：Weak point the invention aims to overcome prior art, it is proposed that a kind of ultra-thin silver is received
The synthetic method of rice plate, by introducing the competition mechanism of strong reductant/strong oxidizer, realizes the highly consistentization sieve of crystal seed type
Choosing, and by the strict control size of continuous growth, pattern, realize the small size silver nanoparticle plate of 100% yield, with " gap " and
The large scale silver nanoparticle plate of " focus ", ultra-thin, super large draw ratio (1000:1) large scale silver nanoparticle plate and various single dispersings
Core shell structure silver nanoparticle plate.Above product has in fields such as printed electronic, thin-film device and nanometer waveguides widely should
Use prospect.
Technical scheme：The synthetic method of ultra-thin silver nanoparticle plate of the invention is comprised the following steps：
Step one：Seeded growth and screening
Silver nitrate and surfactant are mixed, is stirred 1-3 minutes, be configured to mixed solution a, the wherein concentration of silver ion
It is 0.1-100mmol/L；To excessive hydrogen peroxide solution is added in mixed solution a, it is sufficiently stirred for, wherein hydrogen peroxide is in reactant
Concentration in system is 0.5-1000mmol/L, is more than 5 times of silver nitrate concentration；After stirring, excessive strong reduction is added
Agent；Now, the galactic longitude in solution go through repeatedly, the growth-etching process of many wheels, along with solution colour after：It is transparent, black, light
A series of yellow, black, yellow, black changes, finally give the twin seed-solution of crystal seed type highly consistentization；
Step 2：It is prepared by the controllable single dispersing silver nanoparticle plate of size
The seed-solution that step one is obtained is taken, 10-1000 times of deionized water dilution is added, and is added thereto to reducing agent
And surfactant, obtain mixed solution b；To silver nitrate solution is added in mixed solution b, for the growth of silver nanoparticle plate, its
Concentration of the middle silver ion in reaction system is 0.01-100mmol/L；With the increase of silver nitrate concentration in reaction system, silver
Nano-plates are gradually grown up, mixed solution after：A series of color changes such as Huang, orange, plum, purple, indigo plant, ultimately generate 100% product
The first silver nanoparticle plate solution of rate, size is accurate adjustable at 10-2000 nanometers；
Step 3：It is prepared by the continuous growth of wheel more than the silver nanoparticle plate with random " gap " and " focus "
A small amount of the first silver nanoparticle plate solution obtained by step 2 is taken, addition deionized water is diluted to silver-colored elemental concentration and is
0.001-100mmol/L；A small amount of hydrogen peroxide solution is added thereto to, is sufficiently stirred for 3-5 minutes, carry out pre-etching, strict control
The concentration of hydrogen peroxide is 0.001-100mmol/L in system, makes nano-plates edge roughening while being unlikely to broken or decomposing；In advance
Etching terminates to be added thereto to surfactant and reducing agent successively again, is uniformly mixing to obtain mixed solution c；To mixed solution c
Middle addition silver nitrate solution, silver nitrate can generate hydrogen ion while reduction, and control often takes turns silver ion in reaction system
Concentration etches the coarse site in edge for 0.01-100mmol/L, the repair process phase of this etching process and the hydrogen atom of reduction
Mutually competition, it is ensured that edge is unlikely to broken or decomposes while forming cracking；Fully after reaction, deionized water is added to be diluted to silver
Elemental concentration is 0.001-100mmol/L；The 5-6 that repeats the above steps takes turns, and solution colour gradually bleaches, and the distinguishable silver of naked eyes occurs
White particles are suspended in solution, form second silver nanoparticle plate of the edge cracking with many random " gaps " and " focus "
Solution, when wheel number increases to the 8 wheel above, the size of nano-plates reaches 3-10 microns, and increases with wheel number, and size keeps dynamic
Stabilization, second yield of silver nanoparticle plate can be improved by continuing increase wheel number；
Step 4：The preparation of the smooth superelevation draw ratio in edge, super large and ultra-thin silver nanoparticle plate
A small amount of the first silver nanoparticle plate solution obtained by step 2 is taken, addition deionized water is diluted to silver-colored elemental concentration and is
0.01-100mmol/L；Hydrogen peroxide solution and alkali halide are added thereto to, the concentration of hydrogen peroxide in precise control system
It is 0.001-100mmol/L, the concentration of alkali halide is 0.001-100mmol/L, to the nanometer in whole course of reaction
Plate shape looks are screened in real time, and the nano-plates for making edge coarse are decomposed rapidly, and only retaining the good nano-plates of crystal orientation is used for continuous life
It is long；Surfactant and reducing agent are added thereto to again, are stirred 1-3 minutes, obtain mixed solution d；Added in mixed solution d
Silver nitrate solution, concentration of the silver ion in reaction system is 0.01-100mmol/L；Fully after reaction, 10-100 times is added
Deionized water dilutes；Within the 2-3 that repeats the above steps wheels, the silver nanoparticle plate growth limit can be broken through, obtain diameter on 20 microns of left sides
The right side, and thickness is less than 20 nanometers, draw ratio is up to 1000：The smooth superelevation draw ratio in 1 edge, super large and ultra-thin the third are received
Rice plate solution；
Step 5：It is prepared by core shell structure silver nanoparticle plate
Using the silver nanoparticle plate solution obtained by step 2 or step 3 or step 4 preparation process for raw material prepares nucleocapsid
Nano-plates heterojunction structure, specific method is as follows：
Tetraethyl orthosilicate TEOS is dissolved in ethanol, the precursor solution that volume fraction is 0.1%-10%, note is configured to
Make solution A；The appropriate silver nanoparticle plate solution centrifugal as obtained in step 2 or step 3 or step 4 is taken, is diluted and is added quality point
Number is the hydrogen peroxide solution of 10%-30%, is configured to solution B；By 1：The ratio of (0.01-10) mixes solution A, B, persistently stirs
Mix more than 5 hours；By the way that the unreacted excessive medicine of removal is centrifuged, obtains uniform, the ultra-thin silver of monodispersed core-shell structural and receive
Rice plate.
The surfactant includes：Polyvinylpyrrolidone PVP, trisodium citrate, mercaptan, polymethylacrylic acid, benzene
Formic acid or sodium lactate；Concentration of the surfactant in reaction system be 0.01-1000mmol/L, in reaction system silver nitrate with
The mol ratio of surfactant is 1:(0.1-10).
Described strong reductant includes：Ascorbic acid AA, formaldehyde, hydrazine hydrate or sodium borohydride；In reaction system by force also
The concentration of former agent is 0.5-1000mmol/L, is more than 5 times of silver nitrate concentration.
Described reducing agent includes：Ascorbic acid, formaldehyde, hydrazine hydrate or polyalcohol；Reducing agent is dense in reaction system
It is 0.01-100mmol/L to spend.
Described surfactant includes：Polyvinylpyrrolidone, trisodium citrate, mercaptan, polymethylacrylic acid, grape
Sodium saccharate or lauryl sodium sulfate SDS；Concentration of the surfactant in reaction system is 0.01-100mmol/L.
Described surfactant includes：Polymethylacrylic acid, sodium gluconate, trisodium citrate, mercaptan or polyethylene
Pyrrolidones；Concentration of the surfactant in reaction system is 0.001-100mmol/L.
Described reducing agent includes：Ascorbic acid, formaldehyde, hydrazine hydrate or polyalcohol；Reducing agent is dense in reaction system
It is 0.001-100mmol/L to spend.
The alkali halide is：Sodium chloride, potassium chloride, sodium bromide, KBr, sodium iodide or KI；Wherein, alkali
Concentration of the metal halide in reaction system is 0.001-100mmol/L.
Described surfactant includes：Polymethylacrylic acid, sodium gluconate, trisodium citrate, mercaptan or polyethylene
Pyrrolidones；Concentration of the surfactant in reaction system is 0.001-100mmol/L.
Described reducing agent includes：Ascorbic acid, formaldehyde, hydrazine hydrate or polyalcohol；Reducing agent is dense in reaction system
It is 0.001-100mmol/L to spend.
In four the step of the inventive method, hydrogen peroxide solution and alkali halide are provided and made with superpower oxide etch
Oxonium ion/halide ion etching agent, is screened in real time to the nano-plates pattern in whole course of reaction, makes edge thick
Rough nano-plates are decomposed rapidly, and only retaining the good nano-plates of crystal orientation is used for continuous growth.But need hydrogen peroxide in precise control system
Concentration is 0.001-100mmol/L, and the concentration of alkali halide is nanometer 0.001-100mmol/L good to ensure radial direction
Plate is not broken off.Simultaneously as silver nitrate can generate hydrogen ion while reduction, as wheel number increases, hydrogen ion is gradually
Accumulation, oxide etch effect is more and more obvious, therefore to expect super large, ultra-thin silver nanoparticle plate, it is necessary to reduce reaction as far as possible
Wheel number, suppresses hydrionic accumulation.
Beneficial effect：The present invention has the following advantages that compared with prior art：
1. the present invention proposes a kind of new crystal seed preparation method, and compared with previously reported method, this method exists
Screening crystal seed method aspect has significant advanced.By introducing strong reductant machine is competed with the oxidation/reduction of strong oxidizer
System, screens crystal seed type, has etched away isotropism crystal seed, realizes the preparation of the plane twin crystal seed of highly consistentization, from
Source inhibits the generation of non-nano plate particle, is the breakthrough to existing nano-plates preparation method.Based on crystalline substance proposed by the present invention
Preparation method is planted, magnanimity, high concentration, single dispersing silver nanoparticle plate (the first of 100% yield under normal temperature, water base environment is realized
Silver nanoparticle plate) preparation.
2. single dispersing silver nanoparticle plate solution proposed by the present invention, absworption peak is unimodal in visible-range, and halfwidth is most
Low is only 80 nanometers, is 1/3rd of prior art.In the same volume aqueous solution, yield is 100 times of prior art.And close
Into method it is simple to operate, success rate is high, pollution-free, sample size can accuracy controlling, preparation process without complex device, be capable of achieving
The quick production of high-volume, is particularly suitable for industrialization.
3. present invention firstly provides a kind of brand-new system with the hardened structure of the random silver nanoparticle in " gap " and " focus "
Preparation Method (second nano-plates), report is had no before this structure." gap " and " focus " size of these random distributions
Minimum is only several nanometers, is distributed Relatively centralized, it is easy to encourage " gap pattern " so that local electric field intensity is obtained on hundred
Thousand times of enhancing.Meanwhile, silver nanoparticle plate of this macro-size more than 5 microns has obvious two dimensional conductive pattern, can use
In the remote sensing Raman detection and high-definition remote sensing imaging technique of heterodoxy excitation/output.
4. the present invention realizes a kind of superelevation draw ratio, large scale, ultra-thin, monocrystal silver nano-plates preparations the (the 3rd first
Plant nano-plates).In 20 microns, below 20 nanometers, draw ratio is about 1000 to thickness to this ultra-thin silver nanoparticle board size:1,
It is 5-10 times of existing report.Its surface etc. from exciton unit resonance (SPR) peak can red shift to mid and far infrared, even THz wave
Section, having filled up these wave bands can use the blank of surface plasmons nano-plates material.Can also be by electron beam lithography system
For into high-quality two-dimensional waveguide device, the device exploitation in the fields such as optic communication, quantum optices is applied to.
Brief description of the drawings
Fig. 1 is SEM (SEM) figure of single dispersing silver nanoparticle plate in embodiment 1.
Fig. 2 is the scanning electron microscope diagram of the silver nanoparticle plate with random " gap " and " focus " in embodiment 2, wherein
Interior illustration is transmission electron microscope (TEM) image in edge " gap " and " focus " place region.
Fig. 3 is the SEM of edge smooth superelevation draw ratio, super large and ultra-thin silver nanoparticle plate in embodiment 3
Figure.
Specific embodiment
The present invention is further illustrated below by specific embodiment and comparative example：
Embodiment 1
Step one：Seeded growth and screening
10mL deionized waters are taken, silver nitrate solution and 200 μ L that 100 μ L concentration are 0.5mol/L is added thereto to successively dense
The polyvinylpyrrolidonesolution solution for 3mol/L is spent, is stirred 3 minutes, be configured to mixed solution a；To adding 500 in mixed solution a
μ L concentration is the hydrogen peroxide solution of 1mol/L, is sufficiently stirred for；The hydration that 500 μ L concentration are 1mol/L is added after stirring
Hydrazine solution；Now, the galactic longitude in solution go through repeatedly, the growth-etching process of many wheels, along with solution colour after：Transparent,
A series of black, yellowish, black, yellow, black changes, finally give the twin seed-solution of crystal seed type highly consistentization；
Step 2：It is prepared by the controllable single dispersing silver nanoparticle plate of size
1L deionized waters are taken, the seed-solution obtained in 5mL steps one is added thereto to successively, 5mL concentration is 1mol/L
Polyvinylpyrrolidonesolution solution and 6mL concentration for 1mol/L ascorbic acid solution, obtain mixed solution b；After being sufficiently stirred for,
It is the silver nitrate solution of 0.1mol/L to 100mL concentration is added in mixed solution b；As reaction is carried out, silver nanoparticle plate is gradually long
Greatly, mixed solution after：A series of color changes such as Huang, orange, plum, purple, indigo plant, ultimately generate the first silver of 100% yield
Nano-plates solution.
The scanning electron microscope diagram of obtained the first silver nanoparticle plate is shown in Fig. 1, as shown in Figure 1, silver prepared by embodiment 1
Nano-plates are evenly distributed, without other patterns, a diameter of 400 ran, pattern, size uniformity.
Embodiment 2
Step one：Seeded growth and screening
5mL deionized waters are taken, silver nitrate solution and 60 μ L concentration that 60 μ L concentration are 1mol/L are added thereto to successively is
The sodium dodecyl sulfate solution of 2mol/L, stirs 1 minute, is configured to mixed solution a；To being added in mixed solution a, 300 μ L are dense
The hydrogen peroxide solution for 1mol/L is spent, is sufficiently stirred for；The sodium borohydride that 500 μ L concentration are 1mol/L is added after stirring
Solution；Now, the galactic longitude in solution go through repeatedly, the growth-etching process of many wheels, along with solution colour after：Transparent, black,
A series of yellowish, black, yellow, black changes, finally give the twin seed-solution of crystal seed type highly consistentization；
Step 2：It is prepared by the controllable single dispersing silver nanoparticle plate of size
60mL deionized waters are taken, the seed-solution obtained in 400 μ L steps one is added thereto to successively, 50 μ L concentration are
The sodium dodecyl sulfate solution of 1mol/L and 100 μ L concentration are the citric acid solution of 1mol/L, obtain mixed solution b；Fully
It is the silver nitrate solution of 0.5mol/L to 1.5mL concentration is added in mixed solution b after stirring；As reaction is carried out, silver nanoparticle plate
Gradually grow up, mixed solution after：A series of color changes such as Huang, orange, plum, purple, indigo plant, ultimately generate the of 100% yield
A kind of silver nanoparticle plate solution.
Step 3：It is prepared by the continuous growth of wheel more than the silver nanoparticle plate with random " gap " and " focus "
60mL deionized waters are taken, the silver nanoparticle plate solution that 200 μ L steps 5 are obtained is added thereto to；It is added thereto to 50 μ L
Concentration is the hydrogen peroxide solution of 0.5mol/L, is sufficiently stirred for 5 minutes, carries out pre-etching；Pre-etching terminates to add thereto successively again
It is the citric acid solution of 1mol/L to enter sodium dodecyl sulfate solution and 100 μ L concentration that 50 μ L concentration are 1mol/L, and stirring is equal
It is even to obtain mixed solution c；It is the silver nitrate solution of 0.5mol/L to 1.5mL concentration is added in mixed solution c；Fully reaction
Afterwards, 10mL solution is taken, plus deionized water is diluted to volume for 60ml；Above-mentioned steps 8 are taken turns in repeat step three, and solution colour is gradually
Bleach, the distinguishable silvery white little particle of naked eyes occur and be suspended in solution, form edge cracking with many random " gaps " and
The second silver nanoparticle plate solution of " focus ".
The scanning electron microscope diagram of obtained second silver nanoparticle plate is shown in Fig. 2, as shown in Figure 2, silver prepared by embodiment 2
Nano-plates are with many random " gaps " and " focus ", a diameter of 7 microns.
Embodiment 3
Step one：Seeded growth and screening
8mL deionized waters are taken, silver nitrate solution and 100 μ L concentration that 60 μ L concentration are 1mol/L are added thereto to successively is
The polymethyl acid solution of 1mol/L, stirs 2 minutes, is configured to mixed solution a；To adding 100 μ L concentration in mixed solution a
It is the hydrogen peroxide solution of 2mol/L, is sufficiently stirred for；The citric acid for adding 100 μ L concentration to be 3mol/L after stirring is molten
Liquid；Now, the galactic longitude in solution go through repeatedly, the growth-etching process of many wheels, along with solution colour after：It is transparent, black, light
A series of yellow, black, yellow, black changes, finally give the twin seed-solution of crystal seed type highly consistentization；
Step 2：It is prepared by the controllable single dispersing silver nanoparticle plate of size
80mL deionized waters are taken, the seed-solution obtained in 400 μ L steps one is added thereto to successively, 50 μ L concentration are
The polymethyl acid solution of 1mol/L and 100 μ L concentration are the formalin of 1mol/L, obtain mixed solution b；It is sufficiently stirred for
Afterwards, it is added thereto to the silver nitrate solution that 2mL concentration is 0.6mol/L；As reaction is carried out, silver nanoparticle plate is gradually grown up, mixing
Solution after：A series of color changes such as Huang, orange, plum, purple, indigo plant, the first silver nanoparticle plate for ultimately generating 100% yield is molten
Liquid.
Step 3：The preparation of the smooth superelevation draw ratio in edge, super large and ultra-thin silver nanoparticle plate
80mL deionized waters are taken, the silver nanoparticle plate solution that 100 μ L steps 5 are obtained is sequentially added thereto, 100 μ L concentration are
The potassium bromide solution of 0.01mol/L and 500 μ L concentration are the hydrogen peroxide solution of 0.2mol/L；Being added thereto to 50 μ L concentration again is
The polymethyl acid solution of 1mol/L and 100 μ L concentration are the formalin of 1mol/L, are stirred 3 minutes, obtain mixed solution
d；It is the silver nitrate solution of 0.6mol/L to 2mL concentration is added in mixed solution d；Fully after reaction, take 10mL solution, plus go from
Sub- water is diluted to volume for 80ml；Within above-mentioned steps 2 are taken turns in repeat step three, the silver nanoparticle plate growth limit can be broken through, obtained
Diameter is in 20 microns, and thickness is less than 20 nanometers, and draw ratio is up to 1000：The smooth superelevation draw ratio in 1 edge, super large and
The third ultra-thin nano-plates solution.
The scanning electron microscope diagram of obtained the third silver nanoparticle plate is shown in Fig. 3, from the figure 3, it may be seen that silver prepared by embodiment 3
Nano-plates flush edge, size is big, and in 20 microns, below 20 nanometers, draw ratio is about 1000 to thickness to diameter:1.
In addition, those skilled in the art can also make other changes in spirit of the invention, these are according to present invention essence certainly
The change that god is made, should all be included in scope of the present invention.
Claims (10)
1. a kind of synthetic method of ultra-thin silver nanoparticle plate, it is characterised in that the synthetic method is comprised the following steps：
Step one：Seeded growth and screening
Silver nitrate and surfactant are mixed, is stirred 1-3 minutes, be configured to mixed solution a, the concentration of wherein silver ion is
0.1-100mmol/L；To excessive hydrogen peroxide solution is added in mixed solution a, it is sufficiently stirred for, wherein hydrogen peroxide is in reaction system
In concentration be 0.5-1000mmol/L, be more than 5 times of silver nitrate concentration；After stirring, excessive strong reductant is added；
Now, the galactic longitude in solution go through repeatedly, the growth-etching process of many wheels, along with solution colour after：Transparent, black, yellowish,
A series of black, yellow, black changes, finally give the twin seed-solution of crystal seed type highly consistentization；
Step 2：It is prepared by the controllable single dispersing silver nanoparticle plate of size
The seed-solution that step one is obtained is taken, 10-1000 times of deionized water dilution is added, and is added thereto to reducing agent and table
Face activating agent, obtains mixed solution b；To silver nitrate solution is added in mixed solution b, for the growth of silver nanoparticle plate, wherein silver
Concentration of the ion in reaction system is 0.01-100mmol/L；With the increase of silver nitrate concentration in reaction system, silver nanoparticle
Plate is gradually grown up, mixed solution after：A series of color changes such as Huang, orange, plum, purple, indigo plant, ultimately generate 100% yield
The first silver nanoparticle plate solution, size is accurate adjustable at 10-2000 nanometers；
Step 3：It is prepared by the continuous growth of wheel more than the silver nanoparticle plate with random " gap " and " focus "
A small amount of the first silver nanoparticle plate solution obtained by step 2 is taken, addition deionized water is diluted to silver-colored elemental concentration and is
0.001-100mmol/L；A small amount of hydrogen peroxide solution is added thereto to, is sufficiently stirred for 3-5 minutes, carry out pre-etching, strict control
The concentration of hydrogen peroxide is 0.001-100mmol/L in system, makes nano-plates edge roughening while being unlikely to broken or decomposing；In advance
Etching terminates to be added thereto to surfactant and reducing agent successively again, is uniformly mixing to obtain mixed solution c；To mixed solution c
Middle addition silver nitrate solution, silver nitrate can generate hydrogen ion while reduction, and control often takes turns silver ion in reaction system
Concentration etches the coarse site in edge for 0.01-100mmol/L, the repair process phase of this etching process and the hydrogen atom of reduction
Mutually competition, it is ensured that edge is unlikely to broken or decomposes while forming cracking；Fully after reaction, deionized water is added to be diluted to silver
Elemental concentration is 0.001-100mmol/L；The 5-6 that repeats the above steps takes turns, and solution colour gradually bleaches, and the distinguishable silver of naked eyes occurs
White particles are suspended in solution, form second silver nanoparticle plate of the edge cracking with many random " gaps " and " focus "
Solution, when wheel number increases to the 8 wheel above, the size of nano-plates reaches 3-10 microns, and increases with wheel number, and size keeps dynamic
Stabilization, second yield of silver nanoparticle plate can be improved by continuing increase wheel number；
Step 4：The preparation of the smooth superelevation draw ratio in edge, super large and ultra-thin silver nanoparticle plate
A small amount of the first silver nanoparticle plate solution obtained by step 2 is taken, addition deionized water is diluted to silver-colored elemental concentration and is
0.01-100mmol/L；Hydrogen peroxide solution and alkali halide are added thereto to, the concentration of hydrogen peroxide in precise control system
It is 0.001-100mmol/L, the concentration of alkali halide is 0.001-100mmol/L, to the nanometer in whole course of reaction
Plate shape looks are screened in real time, and the nano-plates for making edge coarse are decomposed rapidly, and only retaining the good nano-plates of crystal orientation is used for continuous life
It is long；Surfactant and reducing agent are added thereto to again, are stirred 1-3 minutes, obtain mixed solution d；Added in mixed solution d
Silver nitrate solution, concentration of the silver ion in reaction system is 0.01-100mmol/L；Fully after reaction, 10-100 times is added
Deionized water dilutes；Within the 2-3 that repeats the above steps wheels, the silver nanoparticle plate growth limit can be broken through, obtain diameter on 20 microns of left sides
The right side, and thickness is less than 20 nanometers, draw ratio is up to 1000：The smooth superelevation draw ratio in 1 edge, super large and ultra-thin the third are received
Rice plate solution；
Step 5：It is prepared by core shell structure silver nanoparticle plate
Using the silver nanoparticle plate solution obtained by step 2 or step 3 or step 4 preparation process for raw material prepares core-shell nano
Plate heterojunction structure, specific method is as follows：
Tetraethyl orthosilicate TEOS is dissolved in ethanol, the precursor solution that volume fraction is 0.1%-10% is configured to, is denoted as molten
Liquid A；The appropriate silver nanoparticle plate solution centrifugal as obtained in step 2 or step 3 or step 4 is taken, is diluted and add the mass fraction to be
The hydrogen peroxide solution of 10%-30%, is configured to solution B；By 1：The ratio of (0.01-10) mixes solution A, B, persistently stirs 5
More than hour；By the way that the unreacted excessive medicine of removal is centrifuged, uniform, the ultra-thin silver nanoparticle of monodispersed core-shell structural is obtained
Plate.
2. the synthetic method of ultra-thin silver nanoparticle plate as claimed in claim 1, it is characterised in that：The surfactant includes：
Polyvinylpyrrolidone PVP, trisodium citrate, mercaptan, polymethylacrylic acid, benzoic acid or sodium lactate；Surfactant is anti-
The concentration in system is answered for 0.01-1000mmol/L, silver nitrate and the mol ratio of surfactant are 1 in reaction system:(0.1-
10)。
3. the synthetic method of ultra-thin silver nanoparticle plate as claimed in claim 1, it is characterised in that：Described strong reductant includes：
Ascorbic acid AA, formaldehyde, hydrazine hydrate or sodium borohydride；The concentration of strong reductant is 0.5-1000mmol/L in reaction system,
It is more than 5 times of silver nitrate concentration.
4. the synthetic method of ultra-thin silver nanoparticle plate as claimed in claim 1, it is characterised in that：Described reducing agent includes：It is anti-
Bad hematic acid, formaldehyde, hydrazine hydrate or polyalcohol；Concentration of the reducing agent in reaction system is 0.01-100mmol/L.
5. the synthetic method of ultra-thin silver nanoparticle plate as claimed in claim 1, it is characterised in that：Described surfactant bag
Include：Polyvinylpyrrolidone, trisodium citrate, mercaptan, polymethylacrylic acid, sodium gluconate or lauryl sodium sulfate SDS；
Concentration of the surfactant in reaction system is 0.01-100mmol/L.
6. the synthetic method of ultra-thin silver nanoparticle plate as claimed in claim 1, it is characterised in that：Described surfactant bag
Include：Polymethylacrylic acid, sodium gluconate, trisodium citrate, mercaptan or polyvinylpyrrolidone；Surfactant is in reactant
Concentration in system is 0.001-100mmol/L.
7. the synthetic method of ultra-thin silver nanoparticle plate as claimed in claim 1, it is characterised in that：Described reducing agent includes：It is anti-
Bad hematic acid, formaldehyde, hydrazine hydrate or polyalcohol；Concentration of the reducing agent in reaction system is 0.001-100mmol/L.
8. the synthetic method of ultra-thin silver nanoparticle plate as claimed in claim 1, it is characterised in that：The alkali halide is：
Sodium chloride, potassium chloride, sodium bromide, KBr, sodium iodide or KI；Wherein, alkali halide is dense in reaction system
It is 0.001-100mmol/L to spend.
9. the synthetic method of ultra-thin silver nanoparticle plate as claimed in claim 1, it is characterised in that：Described surfactant bag
Include：Polymethylacrylic acid, sodium gluconate, trisodium citrate, mercaptan or polyvinylpyrrolidone；Surfactant is in reactant
Concentration in system is 0.001-100mmol/L.
10. the synthetic method of ultra-thin silver nanoparticle plate as claimed in claim 1, it is characterised in that：Described reducing agent includes：It is anti-
Bad hematic acid, formaldehyde, hydrazine hydrate or polyalcohol；Concentration of the reducing agent in reaction system is 0.001-100mmol/L.
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| CN109967760A (en) * | 2019-04-17 | 2019-07-05 | 宁波大学 | A kind of dendritic silver nanometer sheet material and its preparation method and application containing zigzag inner surface |
| CN110238385A (en) * | 2019-08-01 | 2019-09-17 | 河南金渠银通金属材料有限公司 | The preparation method of round pie chip super fine silver powder |
| CN110355380A (en) * | 2019-08-13 | 2019-10-22 | 山东建邦胶体材料有限公司 | A kind of preparation method of hexagonal flake micron crystalline substance silver powder |
| CN111590086A (en) * | 2020-06-02 | 2020-08-28 | 江西贝特利新材料有限公司 | Ultrathin flake silver powder with smooth surface and preparation method thereof |
| CN111599507A (en) * | 2020-06-02 | 2020-08-28 | 江西贝特利新材料有限公司 | Conductive silver paste based on smooth ultrathin flake silver powder and preparation method thereof |
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| CN111599507A (en) * | 2020-06-02 | 2020-08-28 | 江西贝特利新材料有限公司 | Conductive silver paste based on smooth ultrathin flake silver powder and preparation method thereof |
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