CN103817346A - Shape-controlled triangle flaky nano silver powder preparation method - Google Patents
Shape-controlled triangle flaky nano silver powder preparation method Download PDFInfo
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- CN103817346A CN103817346A CN201410087803.5A CN201410087803A CN103817346A CN 103817346 A CN103817346 A CN 103817346A CN 201410087803 A CN201410087803 A CN 201410087803A CN 103817346 A CN103817346 A CN 103817346A
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Abstract
The invention relates to a shape-controlled triangle flaky nano silver powder preparation method, which is characterized in that silver nitrate, reductant trisodium citrate, oxidizing agent hydrogen peroxide, and redox initiator sodium borohydride are sequentially added to deionized water pro rata, uniform blending is carried out, a product is prepared after hybrid reaction, the product is subjected to centrifugal cleaning, is diluted and dispersed by virtue of ethyl alcohol, and then the triangle nano flaky silver powder is prepared. Compared with the prior art, the preparation method disclosed by the invention has the advantages that auxiliary forces such as photocatalysis, catalyst and mechanical sanding are not involved, the reaction yield and the flake formation rate are high, the triangular shape is obvious, the side length and thickness are uniform, and a good shape base is provided for representation and application.
Description
Technical field
The present invention relates to the preparation method of electronic product, especially relate to the controlled triangle sheet nano-silver powder preparation method of a kind of pattern.
Background technology
In recent years, the preparation of flake nano silver powder and pattern regulation and control are popular research topics.Not only because it has the characteristic in electricity, the magnetics of common Nano Silver, also because flake nano silver has the special optical performance that its specific morphology is brought.When the side edge length of nano-sheet silver is during much larger than thickness, itself will have very high tunable surface plasma resonance effect, causes producing maximum Electromagnetic enhancement effect.The method of preparing flake nano silver comprises photochemical method, electrochemical synthesis, template and direct chemical reduction method.Wherein, photochemical method and electrochemical synthesis can only carry out microsynthesis, and the operating time is longer; Template cost high yield is low; Above method all can not put into production in enormous quantities.Directly chemical reduction method, large because it has output, purity is high, simple to operate, the feature of device simple, has the prospect that can produce in enormous quantities, is widely used.
Along with the development of electronics technology, the application of original nano-silver powder slurry in micro-nano electronic package conducting resinl slurry run into bottleneck already.
Along with scientific and technological progress, require nano-silver powder slurry to adapt to microminiaturization, the integrated and intelligentized trend of electronic product.Therefore require nano-silver powder to there is higher information storage and Electromagnetic enhancement effect.Be wherein the flake silver powder that length and Thickness Ratio are very large by the nano-silver powder pattern control in nanometer silver paste, be one and easily realize and lower-cost change direction.
In order to reach this technical requirement, need to make the triangle nano-sheet silver of high technology content, specific requirement is exactly: high rate in flakes, sheet thickness is even, side edge length homogeneous, through the retrieval of prior art is found, use the technology foreign study group of chemical preparation nano-sheet silver powder to have the research of comparative maturity, prepare the nano-sheet silver powder that productive rate is higher.Set forth and realize the regulation and control of sheet silver pattern to reach the requirement of producing advanced electronic product but the prior art is not concrete.
Application number is the preparation method that 200910273103.4 Chinese patent discloses a kind of nano-Ag particles.First prepare the mixed aqueous solution of AgNO3 and its complexing agent, add again a certain amount of surfactant, and the pH value of regulation system, stirring is dissolved added surfactant completely, under violent stirring, in above-mentioned solution, dropwise drip reducing agent again, control reaction temperature in room temperature, after reducing agent dropwises, continue to be again stirred to reaction and finish, obtain nano silver colloidal sol; The pH value of nano silver colloidal sol is adjusted to subacidity or neutrality (pH=2-7) with pH value conditioning agent, separate out solid, be isolated, after this with this solid of organic solvent washing, again separate, can obtain the nano-Ag particles of " wetting ", obtain nano-Ag particles through vacuum drying, but its course of reaction is relatively complicated and the concrete pattern of the uncontrollable nano-Ag particles preparing.
Summary of the invention
Object of the present invention is exactly to provide in order to overcome the defect that above-mentioned prior art exists that high, the in blocks rate of a kind of silver powder productive rate is high, size homogeneous, be easy to control the triangle sheet nano-silver powder preparation method of its pattern and size.
Object of the present invention can be achieved through the following technical solutions:
The triangle sheet nano-silver powder preparation method that a kind of pattern is controlled, silver nitrate, reducing agent trisodium citrate, oxidants hydrogen peroxide and reduction initator sodium borohydride are joined successively in proportion in deionized water and evenly mixed, through hybrid reaction, the product preparing is through eccentric cleaning, and disperseed by ethanol dilution, prepare triangle nano-sheet silver powder.
The concentration of described trisodium citrate is 1.50～2.25mM, the concentration of described hydrogen peroxide is 0.72～1.44mg/ml, utilize with the reducing agent trisodium citrate of a dicarboxyl structure and exist in reactant liquor with the hydrogen peroxide with oxidisability simultaneously, reach the redox balance of balance silver crystal seed.
Described sodium borohydride concentration is 1.00～2.00mM, utilizes strong reductant sodium borohydride, causes rapidly reduction reaction and obtains silver-colored nucleus.
The concentration of described silver nitrate is 0.1～0.15mM.
As preferred embodiment, hybrid reaction is under high-speed stirred, controls reaction temperature at 30-50 ℃, reaction 1-5min.
As preferred embodiment, eccentric cleaning be by the product preparing through 3 centrifugal ultrasonic cleaning of deionized water and 1 centrifugal ultrasonic cleaning of absolute ethyl alcohol, be finally dispersed in absolute ethyl alcohol.
As the embodiment being more preferably, eccentric cleaning is after reaction finishes, treat that solution is become after navy blue color no longer changes from colourless, stop heating and continue to stir until be down to room temperature, products therefrom is placed in to centrifuge tube, controlling rotating speed, to be that 10000rpm carries out centrifugal, washed with de-ionized water, 3 times repeatedly, then uses absolute ethyl alcohol eccentric cleaning ultrasonic 1 time, finally be dispersed in absolute ethyl alcohol, prepare triangle nano-sheet silver.
Compared with prior art, the present invention adopt sodium borohydride as reaction initiator rapidly by AgNO
3be reduced into a large amount of silver-colored nucleus, then under the effect of reducing agent natrium citricum, nucleus is grown up gradually.Innovation of the present invention is embodied in that in experiment, to apply reproducibility weak and have a reducing agent trisodium citrate of a dicarboxyl structure, special carboxyl structure and silver-colored nucleus <111> crystal face are combined closely, stop crystal to be grown in this direction, promote <110> and the growth of <100> direction simultaneously, <111> looks unfamiliar to grow and is prevented from, form laminated structure, <100> and <110> crystal face are grown faster than other crystal faces, finally make silver-colored Crystallization triangle sheet structure, have the following advantages:
(1) reaction condition is simple and easy, is the most basic redox reaction, does not relate to that other are as auxiliary in external force such as photocatalysis, catalyst and mechanical grinding;
(2) reaction yield and rate in blocks are higher, and triangle is obvious, and the length of side and thickness homogeneous, for characterize and application provides good pattern basis;
(3) reaction time short, simple to operate, be easy to produce in enormous quantities;
(4) be widely used: aspect optical property, can be by reconciling the length of side of triangle nano-sheet silver and the ratio of thickness, make triangle nano-sheet silver have stronger surface plasma body resonant vibration absworption peak at visible ray and near-infrared region, have no idea to accomplish for spherical nano-silver particle; Aspect catalytic performance, triangle nano-sheet silver can etch the empty structure with special appearance in silicon chip surface catalysis, and different empty structures has a great impact the anti-reflection performance of improving silicon chip surface; Aspect prepared by electrode silver plasm, triangle nano-sheet silver can be regarded two-dimensional surface structure as, and its electric property has larger difference compared with three-dimensional sphere and one dimension line body.
Accompanying drawing explanation
Fig. 1 is the absorption spectrum of the triangle nano-sheet silver for preparing of embodiment 1;
Fig. 2 is the transmission electron microscope photo of triangle nano-sheet silver.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
To anti-application container used, magnetic agitation rotor etc., all should be at 75 ℃, 150g/L NaOH, 80ml/L H
2o
2solution in clean 15min.Fully make reactor surface hydroxylating, while avoiding reacting, produce silver mirror.Reactor application deionized water after cleaning is cleaned.Preparation reaction stoste is stand-by, wherein 1. silver nitrate 0.05M, 2. trisodium citrate 75mM, 3. hydrogen peroxide 30wt%, 4. sodium borohydride 100mM, and the solvent of above solution is deionized water.Before reaction starts, the deionized water of getting 24.75ml is placed in the round-bottomed flask of 100ml, 40 ℃ of vigorous stirring 30min of constant temperature.Then add successively 50 μ l 1., 500 μ l 2., 60 μ l 3. and 250 μ l 4., control reaction temperature at 40 ℃ and vigorous stirring 3min, treat that solution is become after navy blue color no longer changes from colourless, stops heating and continues to stir until be down to room temperature.By product pack centrifuge tube into, 10000rpm rotating speed is centrifugal, washed with de-ionized water, 3 times repeatedly, then use absolute ethyl alcohol eccentric cleaning ultrasonic 1 time, be finally dispersed in absolute ethyl alcohol, be exactly triangle nano-sheet silver to be prepared.
Utilize ultraviolet specrophotometer to measure product solution, its result as shown in Figure 1, absorption spectrum shows that product solution has comparatively significantly absworption peak near 350nm, 450nm, 780nm, lot of documents was set forth, these three characteristic peaks that peak is triangle sheet Nano Silver have been verified the conclusion that contains triangle nano-sheet silver in solution aspect optics.The transmission electron microscope of Fig. 2 just clearly shows simultaneously, and the product of synthesized is the uniform triangle nano-sheet silver of particle diameter solution.
Embodiment 2
To anti-application container used, paddle etc., all should be at 80 ℃, 150g/L NaOH, 50ml/L H
2o
2solution in clean 10min.Fully make reactor surface hydroxylating, while avoiding reacting, produce silver mirror.Reactor application deionized water after cleaning is cleaned.Stoste configuration: 1. silver nitrate 0.05M, 2. trisodium citrate 75mM, 3. hydrogen peroxide 30wt%, 4. sodium borohydride 100mM, the solvent of above solution is deionized water.Before reaction starts, the deionized water of getting 24.47ml is placed in the round-bottomed flask of 100ml, 30 ℃ of vigorous stirring 30min of constant temperature.Then add successively 50 μ l 1., 750 μ l 2., 90 μ l 3. and 250 μ l 4., control reaction temperature at 30 ℃ and vigorous stirring 3min, treat that solution is become after navy blue color no longer changes from colourless, stops heating and continues to stir until be down to room temperature.By product pack centrifuge tube into, 10000rpm rotating speed is centrifugal, washed with de-ionized water, 3 times repeatedly, then use absolute ethyl alcohol eccentric cleaning ultrasonic 1 time, be finally dispersed in absolute ethyl alcohol, be exactly triangle nano-sheet silver to be prepared.
Embodiment 3
To anti-application container used, paddle etc., all should be at 82 ℃, 175g/LNaOH, 50ml/L H
2o
2solution in clean 10min.Fully make reactor surface hydroxylating, while avoiding reacting, produce silver mirror.Reactor application deionized water after cleaning is cleaned.Stoste configuration: 1. silver nitrate 0.05M, 2. trisodium citrate 75mM, 3. hydrogen peroxide 30wt%, 4. sodium borohydride 100mM, the solvent of above solution is deionized water.Before reaction starts, the deionized water of getting 23.88ml is placed in the round-bottomed flask of 100ml, 50 ℃ of vigorous stirring 30min of constant temperature.Then add successively 50 μ l 1., 500 μ l 2., 120 μ l 3. and 500 μ l 4., control reaction temperature at 50 ℃ and vigorous stirring 3min, treat that solution is become after navy blue color no longer changes from colourless, stops heating and continues to stir until be down to room temperature.By product pack centrifuge tube into, 10000rpm rotating speed is centrifugal, washed with de-ionized water, 3 times repeatedly, then use absolute ethyl alcohol eccentric cleaning ultrasonic 1 time, be finally dispersed in absolute ethyl alcohol, be exactly triangle nano-sheet silver to be prepared.
Embodiment 4
The triangle sheet nano-silver powder preparation method that a kind of pattern is controlled, silver nitrate, reducing agent trisodium citrate, oxidants hydrogen peroxide and reduction initator sodium borohydride are joined successively in proportion in deionized water and evenly mixed, wherein, the concentration of trisodium citrate is 1.50mM, the concentration of hydrogen peroxide is 0.72mg/ml, utilize with the reducing agent trisodium citrate of a dicarboxyl structure and exist in reactant liquor with the hydrogen peroxide with oxidisability simultaneously, reach the redox balance of balance silver crystal seed.Sodium borohydride concentration is 1.00mM, utilizes strong reductant sodium borohydride, causes rapidly reduction reaction and obtains silver-colored nucleus.The concentration of silver nitrate is 0.1mM.Under high-speed stirred, controlling reaction temperature is 30 ℃, hybrid reaction 5min, and the product preparing process eccentric cleaning, and disperseed by ethanol dilution, prepare triangle nano-sheet silver powder.Eccentric cleaning be wherein by the product preparing through 3 centrifugal ultrasonic cleaning of deionized water and 1 centrifugal ultrasonic cleaning of absolute ethyl alcohol, be finally dispersed in absolute ethyl alcohol.
Embodiment 5
The triangle sheet nano-silver powder preparation method that a kind of pattern is controlled, silver nitrate, reducing agent trisodium citrate, oxidants hydrogen peroxide and reduction initator sodium borohydride are joined successively in proportion in deionized water and evenly mixed, wherein, the concentration of trisodium citrate is 2.25mM, the concentration of hydrogen peroxide is 1.44mg/ml, utilize with the reducing agent trisodium citrate of a dicarboxyl structure and exist in reactant liquor with the hydrogen peroxide with oxidisability simultaneously, reach the redox balance of balance silver crystal seed.Sodium borohydride concentration is 2.00mM, utilizes strong reductant sodium borohydride, causes rapidly reduction reaction and obtains silver-colored nucleus, and the concentration of silver nitrate is 0.15mM.Under high-speed stirred, controlling reaction temperature is 50 ℃, hybrid reaction 1min, and the product preparing process eccentric cleaning, and disperseed by ethanol dilution, prepare triangle nano-sheet silver powder.Eccentric cleaning is wherein after reaction finishes, treat that solution is become after navy blue color no longer changes from colourless, stopping heating continuing to stir until be down to room temperature, products therefrom is placed in to centrifuge tube, and controlling rotating speed, to be that 10000rpm carries out centrifugal, washed with de-ionized water, 3 times repeatedly, then use absolute ethyl alcohol eccentric cleaning ultrasonic 1 time, be finally dispersed in absolute ethyl alcohol, prepare triangle nano-sheet silver.
Due to adopt sodium borohydride as reaction initiator rapidly by AgNO
3be reduced into a large amount of silver-colored nucleus, then under the effect of reducing agent natrium citricum, nucleus is grown up gradually.Innovation of the present invention is embodied in that in experiment, to apply reproducibility weak and have a reducing agent trisodium citrate of a dicarboxyl structure, special carboxyl structure and silver-colored nucleus <111> crystal face are combined closely, stop crystal to be grown in this direction, promote <110> and the growth of <100> direction simultaneously, <111> looks unfamiliar to grow and is prevented from, form laminated structure, <100> and <110> crystal face are grown faster than other crystal faces, finally make silver-colored Crystallization triangle sheet structure.
Claims (7)
1. the triangle sheet nano-silver powder preparation method that pattern is controlled, it is characterized in that, the method joins silver nitrate, reducing agent trisodium citrate, oxidants hydrogen peroxide and reduction initator sodium borohydride successively in proportion in deionized water and evenly mixes, through hybrid reaction, the product preparing is through eccentric cleaning, and disperseed by ethanol dilution, prepare triangle nano-sheet silver powder.
2. the controlled triangle sheet nano-silver powder preparation method of a kind of pattern according to claim 1, it is characterized in that, the concentration of described trisodium citrate is 1.50～2.25mM, the concentration of described hydrogen peroxide is 0.72～1.44mg/ml, utilize with the reducing agent trisodium citrate of a dicarboxyl structure and exist in reactant liquor with the hydrogen peroxide with oxidisability simultaneously, reach the redox balance of balance silver crystal seed.
3. the controlled triangle sheet nano-silver powder preparation method of a kind of pattern according to claim 1, is characterized in that, described sodium borohydride concentration is 1.00～2.00mM, utilizes strong reductant sodium borohydride, causes rapidly reduction reaction and obtains silver-colored nucleus.
4. the controlled triangle sheet nano-silver powder preparation method of a kind of pattern according to claim 1, is characterized in that, the concentration of described silver nitrate is 0.1～0.15mM.
5. the controlled triangle sheet nano-silver powder preparation method of a kind of pattern according to claim 1, is characterized in that, described hybrid reaction is under high-speed stirred, controls reaction temperature at 30-50 ℃, reaction 1-5min.
6. the controlled triangle sheet nano-silver powder preparation method of a kind of pattern according to claim 1, it is characterized in that, described eccentric cleaning be by the product preparing through 3 centrifugal ultrasonic cleaning of deionized water and 1 centrifugal ultrasonic cleaning of absolute ethyl alcohol, be finally dispersed in absolute ethyl alcohol.
7. the controlled triangle sheet nano-silver powder preparation method of a kind of pattern according to claim 6, it is characterized in that, eccentric cleaning is after reaction finishes, treat that solution is become after navy blue color no longer changes from colourless, stopping heating continuing to stir until be down to room temperature, products therefrom is placed in to centrifuge tube, controlling rotating speed, to be that 10000rpm carries out centrifugal, washed with de-ionized water, 3 times repeatedly, then use absolute ethyl alcohol eccentric cleaning ultrasonic 1 time, be finally dispersed in absolute ethyl alcohol, prepare triangle nano-sheet silver.
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| CN105224151A (en) * | 2014-06-12 | 2016-01-06 | 宸鸿科技(厦门)有限公司 | Nano-silver thread conductive laminate structure and capacitance type touch-control panel |
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| CN106563811A (en) * | 2015-10-13 | 2017-04-19 | 中国科学院大连化学物理研究所 | Method for continuously preparing urchin-like Ag-ZnO nano particles by using microchannel reactor |
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| CN109261985A (en) * | 2018-11-29 | 2019-01-25 | 韩金玲 | A kind of preparation method of triangle Pt nanocrystal |
| CN109500405A (en) * | 2019-01-17 | 2019-03-22 | 鲁东大学 | A kind of preparation method of triangle Nano silver piece |
| CN110747439A (en) * | 2019-09-11 | 2020-02-04 | 南京柔导科技有限公司 | Preparation method of micron-sized ultrathin metal sheet for conductive adhesive filler |
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| CN104551007A (en) * | 2015-01-13 | 2015-04-29 | 山东大学 | Large-scale preparation method of silver nano-sheets |
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| CN109500405B (en) * | 2019-01-17 | 2022-02-22 | 鲁东大学 | Preparation method of triangular silver nanosheet |
| CN110747439A (en) * | 2019-09-11 | 2020-02-04 | 南京柔导科技有限公司 | Preparation method of micron-sized ultrathin metal sheet for conductive adhesive filler |
| CN114042929A (en) * | 2021-10-26 | 2022-02-15 | 西安交通大学 | High-concentration silver nano-micron sheet and synthesis method thereof |
| CN115570144A (en) * | 2022-09-20 | 2023-01-06 | 天津理工大学 | Preparation method of silver nanosheet with controllable thickness |
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Application publication date: 20140528 |