CN106077674A - A kind of silver nano-grain colloid solution with efficient sterilizing performance - Google Patents
A kind of silver nano-grain colloid solution with efficient sterilizing performance Download PDFInfo
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- CN106077674A CN106077674A CN201610443315.2A CN201610443315A CN106077674A CN 106077674 A CN106077674 A CN 106077674A CN 201610443315 A CN201610443315 A CN 201610443315A CN 106077674 A CN106077674 A CN 106077674A
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- colloid solution
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- grain colloid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/38—Silver; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/08—Solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0545—Dispersions or suspensions of nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a kind of silver nano-grain colloid solution with efficient sterilizing performance, its preparation method includes: use pulse laser that the elemental silver target being soaked in deionized water is carried out liquid laser corrode, burn-out time is 10~60 minutes, thus prepares the homodisperse silver nano-grain colloid solution with efficient sterilizing performance.The present invention not only has that size is extra small, surface is pure, is uniformly dispersed, the advantage such as good stability, pure free from admixture, and can efficient sterilizing, to human normal cell's nonhazardous.
Description
Technical field
The present invention relates to silver nano-grain preparing technical field, particularly relate to a kind of silver nanoparticle with efficient sterilizing performance
Particle colloid solution.
Background technology
The surface atom of silver nano-grain is " Jie's state " between solid and molecule, and these silver being in " Jie's state " are former
Son has active and the strongest the highest antibacterial ability, can kill the pathogenic microorganisms such as virus, antibacterial, mycoplasma, chlamydia,
Therefore silver nano-grain has the antibacterial characteristics such as potent, quick, lasting, wide spectrum, is a kind of inorganic antibacterial material received much concern.
At present, the synthetic method of silver nano-grain can be divided into chemical method and Physical two class: chemical method mainly includes also
Former dose of reducing process, electrochemical reduction method and photoreduction met hod etc., and Physical mainly includes that mechanical milling method, vacuum vapour deposition, vacuum are spattered
Penetrate and send out and plasma sputtering method etc..Physical is all directly with elemental silver as raw material, it is possible to obtain pure silver nano-grain, but
It is that Physical of the prior art has that device therefor is expensive, yield poorly, synthesize the shortcomings such as poor controllability;Chemical method has cost
The advantages such as silver nano-grain colloidal stability low, that yield is high, controllability is strong, prepared is good, but chemistry of the prior art
Method inevitably introduces impurity in building-up process, it is difficult to obtain pure silver nano-grain.
Summary of the invention
For above-mentioned weak point of the prior art, the invention provides a kind of silver nanoparticle with efficient sterilizing performance
Particle colloid solution, not only has that size is extra small, surface is pure, is uniformly dispersed, the advantage such as good stability, pure free from admixture, and
And can efficient sterilizing, to human normal cell's nonhazardous.
It is an object of the invention to be achieved through the following technical solutions:
A kind of silver nano-grain colloid solution with efficient sterilizing performance, its preparation method includes: use pulse laser
The elemental silver target being soaked in deionized water is carried out liquid laser corrode, and burn-out time is 10~60 minutes, thus prepares
The homodisperse silver nano-grain colloid solution with efficient sterilizing performance.
Preferably, the wavelength of described pulse laser is 1064nm, 532nm or 355nm.
Preferably, the energy of described pulse laser is 30~150mJ/pulse.
Preferably, the granularity of described silver nano-grain is 1~50nm.
Silver nano-grain colloid solution described in technique scheme is used for efficient sterilizing field.
Silver nano-grain colloid solution described in technique scheme is for the efficient sterilizing field relevant with human body.
Silver nano-grain colloid solution described in technique scheme is for Candida albicans, escherichia coli or golden yellow
At least one in color staphylococcus sterilizes.
As seen from the above technical solution provided by the invention, the silver with efficient sterilizing performance provided by the present invention
Nanoparticle colloid solution is to use pulse laser that the elemental silver target being soaked in deionized water is carried out liquid laser corrode
One step is made, and is not added with any surfactant and stabilizer, therefore silver nano-grain surface height pure, active, and should
Silver nano-grain colloid solution does not contains any other impurity outside moisture removal and silver.Simultaneously as silver nano-grain surface band
Have electric charge, therefore this silver nano-grain colloid solution also have be uniformly dispersed, the advantage such as good stability.In liquid laser corrode mistake
Cheng Zhong, by adjusting or several in the wavelength of pulse laser, the energy of pulse laser or burn-out time, can make to prepare
The granularity of silver nano-grain change between 1~50nm.The present invention not only has that size is extra small, surface is pure, is uniformly dispersed,
The advantage such as good stability, pure free from admixture, and can efficient sterilizing, to human normal cell's nonhazardous, therefore this silver nanoparticle
Particle colloid solution can be used for efficient sterilizing field, is particularly suited for the efficient sterilization field relevant with human body.
Accompanying drawing explanation
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, required use in embodiment being described below
Accompanying drawing be briefly described, it should be apparent that, below describe in accompanying drawing be only some embodiments of the present invention, for this
From the point of view of the those of ordinary skill in field, on the premise of not paying creative work, it is also possible to obtain other according to these accompanying drawings
Accompanying drawing.
Fig. 1 is the transmission electron microscope photo of the silver nano-grain colloid solution obtained by the embodiment of the present invention 1.
Fig. 2 is the uv-visible absorption spectroscopy figure of the silver nano-grain colloid solution obtained by the embodiment of the present invention 1.
Fig. 3 is that the silver nano-grain colloid solution obtained by the embodiment of the present invention 1 is respectively to staphylococcus aureus, large intestine
Bacillus and Candida albicans carry out the bactericidal effect figure sterilized.
Fig. 4 is the silver nano-grain colloid solution obtained by the embodiment of the present invention 1 and the silver of conventional chemical reduction synthesis
Nanoparticle colloid solution carries out the toxicity test to Human Lung fibroblast respectively, thus the cell viability obtained contrasts
Figure.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground describes, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on this
Inventive embodiment, the every other enforcement that those of ordinary skill in the art are obtained under not paying creative work premise
Example, broadly falls into protection scope of the present invention.
Below the silver nano-grain colloid solution with efficient sterilizing performance provided by the present invention is described in detail.
A kind of silver nano-grain colloid solution with efficient sterilizing performance, its preparation method includes: use pulse laser
The elemental silver target being soaked in deionized water is carried out liquid laser corrode, and burn-out time is 10~60 minutes, thus prepares
The homodisperse silver nano-grain colloid solution with efficient sterilizing performance.
Wherein, the wavelength of pulse laser is 1064nm, 532nm or 355nm, and the energy of pulse laser is 30~150mJ/
pulse.By adjusting or several in the wavelength of pulse laser, the energy of pulse laser or burn-out time, system can be made
The granularity of the silver nano-grain obtained changes between 1~50nm.
Specifically, the silver nano-grain colloid solution with efficient sterilizing performance provided by the present invention is to use liquid phase to swash
Light corrode one step is made, and is not added with any surfactant and stabilizer, therefore silver nano-grain surface height pure, active,
And without any other impurity outside moisture removal and silver in described silver nano-grain colloid solution.Simultaneously as silver nanoparticle
Grain surface with electric charge, the most described silver nano-grain colloid solution also have be uniformly dispersed, the advantage such as good stability.In liquid phase
During laser ablation, by adjusting or several in the wavelength of pulse laser, the energy of pulse laser or burn-out time,
The granularity that can make the silver nano-grain prepared changes between 1~50nm.Additionally, the present invention not only has, size is extra small, table
Face is pure, be uniformly dispersed, the advantage such as good stability, pure free from admixture, and can efficient sterilizing, nontoxic to human normal cell
Evil, therefore this silver nano-grain colloid solution can be used for efficient sterilizing field, is particularly suited for the efficient sterilizing relevant with human body
Sterilization field, such as: this silver nano-grain colloid solution may be used for Candida albicans, escherichia coli or Staphylococcus aureus
At least one in bacterium sterilizes.
In order to more clearly from show technical scheme provided by the present invention and produced technique effect, below with tool
The silver nano-grain colloid solution with efficient sterilizing performance provided by the present invention is described in detail by body embodiment.
Embodiment 1
A kind of silver nano-grain colloid solution with efficient sterilizing performance, its preparation method is: employing wavelength is
532nm, energy be the pulse laser of 100mJ/pulse the elemental silver target being soaked in deionized water is carried out liquid laser melt
Erosion, a diameter of 1mm of focal beam spot, burn-out time is 30 minutes, thus prepares the homodisperse silver with efficient sterilizing performance
Nanoparticle colloid solution.
Specifically, detecting the silver nano-grain colloid solution obtained by the embodiment of the present invention 1, its result is as follows:
(1) the silver nano-grain colloid solution obtained by the embodiment of the present invention 1 is yellowish-brown, pure free from admixture, and pH value is
6.0, colloidal stability is 1 week at normal temperatures, and silver nano-grain content is 25 μ g/mL, and the granularity of silver nano-grain is 1~2nm.
The minimum inhibitory concentration of this silver nano-grain colloid solution is 1 μ g/mL, it is proposed that concentration is 5 μ g/mL.
(2) use transmission electron microscope that the silver nano-grain colloid solution obtained by the embodiment of the present invention 1 is seen
Examine shooting, thus obtain transmission electron microscope photo as shown in Figure 1.As seen from Figure 1: this silver nano-grain colloid is molten
In liquid, the even size distribution of silver nano-grain;Carry out granularmetric analysis further to understand: at this silver nano-grain colloid solution
In, the distribution of sizes of silver nano-grain is 1~2nm, and this super-small, surface silver nano-grain clean, finely dispersed are
Cannot be obtained by existing chemical reduction method.
(3) the silver nano-grain colloid solution obtained by the embodiment of the present invention 1 is carried out extinction experiment, thus obtain such as figure
Uv-visible absorption spectroscopy figure shown in 2.As seen from Figure 2: this silver nano-grain colloid solution occurs at 397nm
The plasma resonance of typical silver nano-grain (surface plasma resonance, SPR) optical absorption peak.
(4) the silver nano-grain colloid solution obtained by the embodiment of the present invention 1 is diluted to silver nano-grain content respectively
Be 1.0 μ g/mL, three kinds of silver nano-grain colloid solution of 5.0 μ g/mL and 10.0 μ g/mL, and use these three silver nano-grain
Colloid solution carries out sterilization experiment respectively to staphylococcus aureus, escherichia coli and Candida albicans, thus obtains such as Fig. 3 institute
The bactericidal effect figure shown.Wherein, Fig. 3 a is the staphylococcus aureus training being separately added into these three silver nano-grain colloid solution
Nutrient solution light absorption value at 600nm and the graph of a relation of incubation time;Fig. 3 b is molten for being separately added into these three silver nano-grain colloid
The E. coli broth of liquid light absorption value at 600nm and the graph of a relation of incubation time;Fig. 3 c is for being separately added into these three silver
The Candida albicans bacteria culture fluid of nanoparticle colloid solution light absorption value at 600nm and the graph of a relation of incubation time;Fig. 3 d is
It is separately added into the staphylococcus aureus culture fluid of the these three silver nano-grain colloid solution bacterial population after cultivating four hours
Mesh cartogram;Fig. 3 e is that the E. coli broth being separately added into these three silver nano-grain colloid solution is after cultivating four hours
Number of bacteria cartogram;Fig. 3 f is that the Candida albicans bacteria culture fluid being separately added into these three silver nano-grain colloid solution is in training
Number of bacteria cartogram after supporting four hours.By Fig. 3 a, 3b and 3c it can be seen that along with the prolongation of incubation time, three kinds of antibacterials
The light absorption value of culture fluid all gradually decreases, this show silver nano-grain colloid solution obtained by the embodiment of the present invention 1 to this three
That plants antibacterial all has killing effect;And under identical incubation time, the concentration of this silver nano-grain colloid solution is the highest, kills
Bacterium efficiency is the highest.By Fig. 3 d, 3e and 3f it can be seen that when silver nano-grain content is 5.0 μ g/mL, the embodiment of the present invention 1 institute
Staphylococcus aureus, Candida albicans, colibacillary sterilizing rate are respectively by the silver nano-grain colloid solution prepared
96%, 92%, 100%, this shows that the silver nano-grain colloid solution obtained by the embodiment of the present invention 1 also has when very low concentrations
There is extremely strong sterilizing ability.
(5) using the silver nano-grain colloid solution obtained by the embodiment of the present invention 1 as sample A, and by traditional chemical also
Sample A, as sample B, is then diluted to silver nano-grain content and is respectively by the silver nano-grain colloid solution of former method synthesis
Four kinds of colloid solution of 2.5 μ g/mL, 5.0 μ g/mL, 10.0 μ g/mL and 20.0 μ g/mL, are also diluted to silver nanoparticle by sample B
Grain content is respectively four kinds of colloid solution of 2.5 μ g/mL, 5.0 μ g/mL, 10.0 μ g/mL and 20.0 μ g/mL.It is respectively adopted sample
Four kinds of colloid solution after A dilution and four kinds of colloid solution after sample B dilution carry out the toxicity to Human Lung fibroblast
Experiment, thus obtain cell viability comparison diagram as shown in Figure 4.As seen from Figure 4: sample B is to Human Lung fibroblast
There is certain toxicity, and the biggest toxicity of silver nano-grain concentration is the strongest;And sample A is to Human Lung fibroblast not only
There is no toxic action, have the effect promoting its vigor on the contrary, and along with the increase of silver nano-grain concentration, cell viability first by
Cumulative big after be gradually reduced;When the silver nano-grain concentration of sample A is 10 μ g/mL, cell viability reaches maximum (i.e.
130%);Therefore compared with the silver nano-grain colloid solution of conventional chemical reduction synthesis, the silver nanoparticle obtained by the present invention
Particle colloid solution, to human normal cell's nonhazardous, is very suitable for the fields such as the sterilizing relevant to human body.
As fully visible, the embodiment of the present invention not only have that size is extra small, surface is pure, be uniformly dispersed, good stability, pure
The advantages such as free from admixture, and can efficient sterilizing, to human normal cell's nonhazardous.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, the change that can readily occur in or replacement,
All should contain within protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be as the criterion.
Claims (7)
1. a silver nano-grain colloid solution with efficient sterilizing performance, it is characterised in that its preparation method includes: use
Pulse laser carries out liquid laser corrode to the elemental silver target being soaked in deionized water, and burn-out time is 10~60 minutes,
Thus prepare the homodisperse silver nano-grain colloid solution with efficient sterilizing performance.
Silver nano-grain colloid solution the most according to claim 1, it is characterised in that the wavelength of described pulse laser is
1064nm, 532nm or 355nm.
Silver nano-grain colloid solution the most according to claim 1 and 2, it is characterised in that the energy of described pulse laser
Amount is 30~150mJ/pulse.
Silver nano-grain colloid solution the most according to claim 1 and 2, it is characterised in that described silver nano-grain
Granularity is 1~50nm.
5. the silver nano-grain colloid solution according to any one of the claims 1 to 4 is used for efficient sterilizing field.
6. the silver nano-grain colloid solution according to any one of the claims 1 to 4 is used for efficiently kill relevant with human body
Bacterium field.
7. the silver nano-grain colloid solution according to any one of the claims 1 to 4 is for Candida albicans, large intestine bar
At least one in bacterium or staphylococcus aureus sterilizes.
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Cited By (2)
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CN107185530A (en) * | 2017-04-24 | 2017-09-22 | 天津大学 | The method of silver nano-grain of the Laser synthesizing rich in crystal defect |
CN114632481A (en) * | 2022-03-04 | 2022-06-17 | 安徽大学 | Method for preparing uniformly dispersed metal nanoparticle colloid |
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