CN101716684B - Highly dispersible spherical nano-silver powder and preparation method thereof - Google Patents
Highly dispersible spherical nano-silver powder and preparation method thereof Download PDFInfo
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- CN101716684B CN101716684B CN2009102139709A CN200910213970A CN101716684B CN 101716684 B CN101716684 B CN 101716684B CN 2009102139709 A CN2009102139709 A CN 2009102139709A CN 200910213970 A CN200910213970 A CN 200910213970A CN 101716684 B CN101716684 B CN 101716684B
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Abstract
The invention discloses highly dispersible spherical nano-silver powder and a preparation method thereof. The method comprises the following steps of: mixing PEG and deionized water in a molar ratio of 1 to (0.005-5), and uniformly stirring the obtained solution; then mixing AgNO3 and a glucose solid in the molar ratio of 1 to (0.005-2), then adding the mixture into solution of the PEG, dissolving the mixture, uniformly stirring the obtained solution, and reacting for 3 to 10 hours at the temperature of between 20 and 70 DEG C, wherein the molar ratio of the PEG to the AgNO3 is (400-10) to 1; and then centrifugating and filtering a reaction product, and washing the obtained product with distilled water to obtain the nano-silver particles. The preparation method is simple and easy to operate; the spherical nano-silver powder has the particle size of between 3 and 20nm, and belongs to a nanometer level; silver nano-particles have the advantages of small size, uniform distribution, good stability and strong antibacterial ability; all used solvents are non-toxic; and the spherical nano-silver powder is easy to add into other products.
Description
Technical field
The present invention relates to a kind of nano-silver powder, particularly relate to highly dispersible spherical nano-silver powder and preparation method.
Background technology
Because the peculiar property and the application prospects of Nano Silver, its preparation and application have become research emphasis.When the granularity of silver is low to moderate nanoscale, itself have quantum size effect, small-size effect and skin effect.Nano particle presents physics, the chemical property of many uniquenesses, and as high specific area, strong activity, low-temperature sintering etc., these characteristics make silver nano-grain obtain in a lot of fields using widely, has good catalytic action, antibiotic property, nonlinear optical properties, superelevation electrical conductivity.
The preparation method of Nano Silver generally must satisfy following these basic demands: surface clean of (1) gained nano silver particles and purity height; (2) can control grain shape, size and size distribution; (3) be easy to collect (separation); (4) stability and keeping quality are preferably arranged; (5) be easy to mate with downstream product.
The control of Nano Silver size and shape at present mainly based on light or chemical reducing solution method, mainly prepares the Nano Silver of controlled dimensions, narrow distribution and controllable shape, the kind and the concentration of (1) silver salt by control or following these conditions of research; (2) environment of reaction system (as pH value of solvent species, reaction temperature and reaction solution etc.); (3) factors such as kind of dispersant and reducing agent.According to above these conditions, concrete main following preparation method: liquid phase chemical reduction method (RongM Z etc., [J] .Polymer, 1999,40 (22): 6169-6178; AnderssonM etc., [J] .Langmuir, 2005,21 (24): 113811396; KimKY etc., [J] Materials Chemistryand Physics, 2004,88 (2-3:377-382; ), electrochemical reducing (Zhu J, Liu S etc., [J] .Langmuir, 2000,16 (16): 6396-6399), the photoreduction method (Yao Suwei etc., [J]. Acta PhySico-Chimica Sinica, 2003,19 (5): 464.468; Zhou Y etc., [J] .Advanced Materials, 1999,11 (10): 850-852.), molecule self-assembly method (Tessier P M etc., [J] AdvancedMaterials, 2001,13 (6): 396-400).
Chinese invention patent ZL 01118992.4 discloses a kind of preparation method of ultra-fine ball silver powder, this method may further comprise the steps: the concentration of adjusting liquor argenti nitratis ophthalmicus is 10-120g/L, regulate pH value to 1-7, take by weighing the L-ascorbic acid of the 100-200% of the theoretical consumption of the required L-ascorbic acid of reduction silver ion, control reaction temperature at 15-60 ℃, reaction time 0.5-10 minute.Just can get the ball shape silver powder of the different-grain diameter of 0.3-3.0 μ m.The size of Zhi Bei ball shape silver powder is big in this way, belongs to micron-sized, and particle diameter distributes wide, the product size poor stability, and reaction condition need be under acid condition, and cost of material is than higher.
Summary of the invention
The objective of the invention is at size Control difficulty owing to Nano Silver, the easy oxidation of Nano Silver, provide a kind of preparation method simple, easy to operate, the silver nano-grain size is little, be evenly distributed, good stability, the strong and avirulence of antibacterial ability, the nano-silver powder of polymolecularity and preparation method, its silver-colored grain diameter is 3～20nm, belongs to nanoscale.
The spherical nano-silver powder of gained of the present invention is a polymolecularity, does not have between the particle and reunites.
A kind of preparation method of highly dispersible spherical nano-silver powder is characterized in that comprising the steps:
(1) PEG and deionized water are pressed 1: (0.005～5) mixed in molar ratio stirs; The molecular weight ranges of described PEG is 400～4000;
(2) with AgNO
3With glucose solids be 1 in molar ratio: mix (0.005～2), joins then in the solution of PEG of step (1) gained, and dissolving stirs, and temperature is under 20～70 ℃ of conditions, reacts 3～10 hours; PEG and AgNO
3Mol ratio be (400-10): 1;
(3) the step reaction product is centrifugal, filter, with the distilled water washing, obtain nano-Ag particles.
Centrifugal speed is 5000～10000rmp in the step (3).
Nano Silver has quantum size effect, small-size effect, skin effect and macro quanta tunnel effect and presents the unusual performance of the aspects such as light, electricity, magnetic, thermodynamics and chemical reaction that are different from common material, is a kind of important functional material.Nano silver particles has the remarkable characteristic of nanostructured, can be widely used in a plurality of fields such as catalyst, medicine, antibiotic, composite.
The present invention compared with prior art has following characteristics:
1, the surface clean of this method gained nano silver particles and purity height can be controlled grain shape, size and size distribution, are easy to collect (separation), and stability and keeping quality are preferably arranged, and are easy to mate with downstream product.
2, technology of the present invention is simple, only need simply stir, centrifugal washing.
3, synthesis material of the present invention (as PEG series etc.) source is abundant, low price, and cost is low.
4, the used solvent of the present invention all is nontoxic, is easy to add in other products.
Description of drawings
Fig. 1 is the transmission electron microscope figure of the Nano Silver of preparation among the embodiment 1.
Fig. 2 prepares the XRD figure of gained Nano Silver for Fig. 1.
Fig. 3 is the transmission electron microscope figure of the Nano Silver of preparation among the embodiment 2.
Fig. 4 is the transmission electron microscope figure of the Nano Silver of preparation among the embodiment 3.
Fig. 5 is the transmission electron microscope figure of the Nano Silver of preparation among the embodiment 4.
The specific embodiment
Below in conjunction with specific embodiment the present invention is done description further, but specific embodiment does not constitute qualification to the scope of protection of present invention.
Embodiment 1
A kind of preparation method of highly dispersible spherical nano-silver powder comprises the steps:
(1) 400gPEG400 and 100gPEG2000 are added the mixing of 18g deionized water, stir.
(2) take by weighing 425mgAgNO
3With the 100mg glucose solids, add in the solution of step (1) gained, dissolving fully stirs.
(3) reaction temperature is 70 ℃, and the reaction time is 3h, and product is centrifugal under 5000rmp, filters, and with distilled water washing three times, obtains nano-Ag particles.
The transmission electron microscope picture that present embodiment prepares the gained Nano Silver as shown in Figure 1, as can be seen from the figure, this Nano Silver presents sphere, particle diameter is about 3～20nm, belongs to nanoscale, the spherical nano-silver powder of gained is a polymolecularity, does not have between the particle and reunites.The XRD figure of present embodiment gained Nano Silver, as shown in Figure 2, the as can be seen from Figure 2 typical crystal face [111] of Nano Silver, [200], [220] strong characteristic absorption peak, this shows that Nano Silver after separating, has stability and keeping quality preferably, because used solvent all is nontoxic, be easy to add in other products.
Embodiment 2
A kind of preparation method of highly dispersible spherical nano-silver powder comprises the steps:
(1) 600gPEG600 and 50gPEG1000 are added the mixing of 18g deionized water, stir.
(2) take by weighing 1200mgAgNO
3With the 100mg glucose solids, add in the solution of PEG, dissolving fully stirs.
(3) reaction temperature is 60 ℃, and the reaction time is 10h, and product is centrifugal under 8000rmp, filters, and with distilled water washing three times, obtains nano-Ag particles.
The transmission electron microscope picture that present embodiment prepares the gained Nano Silver as shown in Figure 3, as can be seen from the figure, this Nano Silver presents sphere, particle diameter is about 3～10nm, no agglomerated particle.The XRD figure of present embodiment gained Nano Silver is substantially with shown in Figure 2.
Embodiment 3
A kind of preparation method of highly dispersible spherical nano-silver powder comprises the steps:
(1) 400gPEG400 and 100gPEG600 are added the mixing of 90g deionized water, stir.
(2) take by weighing 2000mgAgNO
3With the 100mg glucose solids, add in the solution of step (1) gained, dissolving fully stirs.
(3) reaction temperature is 70 ℃, and the reaction time is 2h, and product is centrifugal under 7000rmp, filters, and with distilled water washing three times, obtains nano-Ag particles.
The transmission electron microscope picture that present embodiment prepares the gained Nano Silver as shown in Figure 4, as can be seen from the figure, this Nano Silver presents sphere, particle diameter is about 3～20nm, no agglomerated particle.The XRD figure of present embodiment gained Nano Silver is substantially with shown in Figure 2.
Embodiment 4
A kind of preparation method of highly dispersible spherical nano-silver powder comprises the steps:
(1) 300gPEG400 and 200gPEG4000 are added the mixing of 90g deionized water, stir.
(2) take by weighing 425mgAgNO
3With the 900mg glucose solids, add in the solution of step (1) gained, dissolving fully stirs.
(3) reaction temperature is 20 ℃, and the reaction time is 8h, and product is centrifugal under 10000rmp, filters, and with distilled water washing three times, obtains nano-Ag particles.
The transmission electron microscope picture that present embodiment prepares the gained Nano Silver as shown in Figure 5, as can be seen from the figure, this Nano Silver presents sphere, particle diameter is about 3～15nm, no agglomerated particle.The XRD figure of present embodiment gained Nano Silver is substantially with shown in Figure 2.
As mentioned above, can better implement the present invention.
Claims (3)
1. the preparation method of a highly dispersible spherical nano-silver powder is characterized in that comprising the steps:
(1) PEG and deionized water are pressed 1: (0.005～5) mixed in molar ratio stirs; The molecular weight ranges of described PEG is 400～4000;
(2) with AgNO
3With glucose solids be 1 in molar ratio: mix (0.005～2), joins then in the solution of PEG of step (1) gained, and dissolving stirs, and temperature is under 20～70 ℃ of conditions, reacts 2～10 hours; PEG and AgNO
3Mol ratio be (400-10): 1;
(3) step (2) product is centrifugal, filter, with the distilled water washing, obtain nano-Ag particles.
2. the preparation method of highly dispersible spherical nano-silver powder according to claim 1, it is characterized in that: centrifugal speed is 5000～10000rmp in the step (3).
3. highly dispersible spherical nano-silver powder is characterized in that: by the described method preparation of claim 1, the particle diameter of this spherical nano-silver powder is 3-20nm.
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Families Citing this family (15)
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| CN101999412B (en) * | 2010-11-19 | 2014-05-28 | 深圳兰度生物材料有限公司 | Nano-silver solution and preparation method thereof |
| CN102198512A (en) * | 2011-05-13 | 2011-09-28 | 同济大学 | Method for preparing nano silver dispersed by glucose reduction complexing agent |
| US9849512B2 (en) * | 2011-07-01 | 2017-12-26 | Attostat, Inc. | Method and apparatus for production of uniformly sized nanoparticles |
| CN102513544B (en) * | 2011-12-13 | 2014-04-09 | 江苏大学 | Method for preparing nanometer silver sol |
| CN102784926B (en) * | 2012-07-16 | 2015-04-01 | 太原理工大学 | Method for preparing spherical nano-silver particles |
| CN104259471A (en) * | 2014-08-29 | 2015-01-07 | 昆明贵金属研究所 | Method for preparing spherical silver nanoparticles uniform in particle size rapidly |
| CN104525964B (en) * | 2014-12-21 | 2017-02-22 | 北京工业大学 | Preparing method for regular spherical silver nanometer particles |
| CN104721227B (en) * | 2015-02-10 | 2016-10-12 | 长沙迪谷纳米生物科技有限公司 | A kind of medicinal nano silver paste and preparation method thereof |
| US9839652B2 (en) | 2015-04-01 | 2017-12-12 | Attostat, Inc. | Nanoparticle compositions and methods for treating or preventing tissue infections and diseases |
| CN104710808B (en) * | 2015-04-10 | 2017-07-25 | 民勤县家兴节能服务有限公司 | The method that municipal manhole cover is processed using waste mulching film |
| US11473202B2 (en) | 2015-04-13 | 2022-10-18 | Attostat, Inc. | Anti-corrosion nanoparticle compositions |
| EP3283580A4 (en) | 2015-04-13 | 2019-03-20 | Attostat, Inc. | Anti-corrosion nanoparticle compositions |
| US11018376B2 (en) | 2017-11-28 | 2021-05-25 | Attostat, Inc. | Nanoparticle compositions and methods for enhancing lead-acid batteries |
| US11646453B2 (en) | 2017-11-28 | 2023-05-09 | Attostat, Inc. | Nanoparticle compositions and methods for enhancing lead-acid batteries |
| US12115250B2 (en) | 2019-07-12 | 2024-10-15 | Evoq Nano, Inc. | Use of nanoparticles for treating respiratory infections associated with cystic fibrosis |
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| CN1548260A (en) * | 2003-05-12 | 2004-11-24 | 贵研铂业股份有限公司 | Surface processing method of superfine silver powder |
| CN101497135A (en) * | 2009-03-12 | 2009-08-05 | 宁波大学 | Method for preparing spherical silver nano granule |
| CN101569937A (en) * | 2009-06-05 | 2009-11-04 | 中国乐凯胶片集团公司 | Preparation method for high-dispersing silver powder used for conductive silver paste |
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