CN105817642B - A kind of Au/Ag core-shell nano materials with Efficient antibacterial performance and preparation method thereof - Google Patents
A kind of Au/Ag core-shell nano materials with Efficient antibacterial performance and preparation method thereof Download PDFInfo
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- CN105817642B CN105817642B CN201610244061.1A CN201610244061A CN105817642B CN 105817642 B CN105817642 B CN 105817642B CN 201610244061 A CN201610244061 A CN 201610244061A CN 105817642 B CN105817642 B CN 105817642B
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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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
- B22F1/17—Metallic particles coated with metal
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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 Au/Ag core-shell nano materials with Efficient antibacterial performance and preparation method thereof, belong to technical field of nano material.This method utilizes nano silver in situ synthesis, prepare using gold nano grain as core, silver nano-grain is the Au/Ag core-shell nano materials of shell, by the way that to Surface-modification of Nanoparticles dodecyl sodium sulfate, the Au/Ag core-shell nano materials with high bacteriostasis property are prepared.Compared with simple gold, silver nano particle, the present invention has the following advantages：1) a small amount of concentration is only needed, you can strong bactericidal effect is produced to Gram-negative bacteria and gram-positive bacteria, there is broad-spectrum sterilization；2) by modifying dodecyl sodium sulfate, the biocidal property of nano material can be effectively improved, reduces its toxicity；3) good dispersion, chemical property are stablized, can be preserved for a long time.The nano material has boundless application prospect.
Description
Technical field
The present invention relates to a kind of Au/Ag core-shell nano materials with Efficient antibacterial performance and preparation method thereof, belong to and receive
Rice field of material technology.
Background technology
Silver nano-grain is the noble metal nanometer material being most widely used at present, due to higher surface-active,
Surface catalysis performance and conductance hot property etc. so that silver nano-grain is easily absorbing in antimicrobial surface, utilizes silver ion pair
The destruction of protein, DNA etc., so as to effectively kill the pathogenic microorganisms such as bacterium, fungi, mycoplasma, efficiently and are not easy
Produce drug resistance.Due to the antibacterial activity of its wide spectrum, nano silver is used widely in daily life and medical and health.
But at present studies have found that nano silver have to mammal certain toxicity, nano silver absorbed by alimentary canal after directly
Into the organ such as blood and liver, and accumulated in its hetero-organization and organ, after reaching a certain amount of, liver poison can be produced to human body
The toxic reaction such as property, renal toxicity, neurotoxicity.Therefore, how to obtain green, nontoxic, efficient silver system bacteriostatic agent becomes mesh
The hot issue of preceding research.
The content of the invention
The present invention be directed to defect existing in the prior art, there is provided a kind of Au/Ag nucleocapsids with Efficient antibacterial performance are received
Rice material and preparation method thereof, which can be incorporated into one on the whole by two kinds of different metal materials, have concurrently core with
While two kinds of material advantages of shell, the Nomenclature Composition and Structure of Complexes of core and shell can be controlled as needed unprecedented to obtain
Physics and chemical property.In addition, by the way that in core-shell nano material surface modification activities material, nano material can not only be effectively improved
Biocidal property, while the biocompatibility of nano material can be improved, substantially reduce the toxicity of nano material.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of Au/Ag core-shell nano materials with Efficient antibacterial performance, which is to be prepared via a method which to obtain：
1) after gold nano grain solution is mixed with polyvinylpyrrolidonesolution solution, ascorbic acid solution, silver nitrate solution
Reaction, is prepared Au/Ag core shell nanoparticles solution；
2) by Au/Ag core shell nanoparticles solution prepared by step 1) and dodecyl sodium sulfate hybrid reaction, SDS is obtained
The Au/Ag core-shell nano antibacterial materials of functionalization.
The particle diameter of gold nano grain is 5~15nm in the step 1) of technical solution of the present invention；In the solution of gold nano grain
Nanogold molar concentration is 5-20nmol/L.
The content of PVP is 0.2~1% in the step 1) of technical solution of the present invention；The content of ascorbic acid for 100~
400mmol/L；The content of silver nitrate is 0.1~0.4mmol/L；Gold nano grain solution and polyvinylpyrrolidonesolution solution, resist
Bad hematic acid solution, the volume ratio of silver nitrate solution are 5~10：2~6：1~3：0.5~2.5.
2~4h of room temperature lucifuge concussion reaction after mixing in the step 1) of technical solution of the present invention.
The volume matter of Au/Ag core shell nanoparticles solution and dodecyl sodium sulfate in the step 2) of technical solution of the present invention
It is 100~500 μ L to measure ratio：1~5mg.
A kind of Au/Ag core-shell nano material preparation methods with Efficient antibacterial performance, this method comprise the following steps：
1) after gold nano grain solution is mixed with polyvinylpyrrolidonesolution solution, ascorbic acid solution, silver nitrate solution
Reaction, is prepared Au/Ag core shell nanoparticles solution；
2) by Au/Ag core shell nanoparticles solution prepared by step 1) and dodecyl sodium sulfate hybrid reaction, SDS is obtained
The Au/Ag core-shell nano antibacterial materials of functionalization.
The particle diameter of gold nano grain is 5~15nm in the step 1) of technical solution of the present invention；In the solution of gold nano grain
Nanogold molar concentration is 5-20nmol/L.
The content of PVP is 0.2~1% in the step 1) of technical solution of the present invention；The content of ascorbic acid for 100~
400mmol/L；The content of silver nitrate is 0.1~0.4mmol/L；Gold nano grain solution and polyvinylpyrrolidonesolution solution, resist
The volume ratio 5~10 of bad hematic acid solution, silver nitrate solution：2~6：1~3：0.5~2.5.
Mixed liquor room temperature lucifuge concussion reaction 2-4h in the step 1) of technical solution of the present invention.
The volume matter of Au/Ag core shell nanoparticles solution and dodecyl sodium sulfate in the step 2) of technical solution of the present invention
It is 100~500 μ L to measure ratio：1~5mg.
Beneficial effects of the present invention：
(1) strong kill can be produced to Gram-negative bacteria and gram-positive bacteria by only needing the nano material of a small amount of concentration
Bacterium effect, has broad-spectrum sterilization.
(2) by Surface-modification of Nanoparticles anion surfactant SDS, effectively increasing the antibacterial of nano material
Property, substantially reduce its toxicity；
(3) good dispersion, chemical property are stablized, effectively prevent the oxidation and reunion of nano silver, can preserve for a long time.
(4) reaction condition is gentle, reagent is environmentally protective, easy to operate, easily controllable.
Brief description of the drawings
Fig. 1 is the TEM photos for the Au/Ag nano particles that embodiment 1 is prepared.
Fig. 2 is the cytotoxicity test result figure of embodiment 1~3 and comparative example 1~4.
Embodiment
With reference to embodiment, the present invention will be further described, but protection scope of the present invention not limited to this：
The particle diameter of gold nano grain is 8~12nm in the embodiment of the present invention.
Embodiment 1
(1) preparation of Au/Ag core shell nanoparticles
PVP solution by 250 μ L concentration for 5nmol/L gold nano grains solution and 100 μ L 0.2%, 50 μ L 0.1mol/
The ascorbic acid solution of L, after mixing, adds the AgNO of 35 μ L 0.1mmol/L3Solution, at room temperature lucifuge concussion reaction
2h, is prepared Au/Ag core shell nanoparticles solution；
(2) Au/Ag core shell nanoparticles surface modification SDS
500 μ L of Au/Ag core shell nanoparticles solution prepared by step (1) are taken to add 1mg thereto in 1mL centrifuge tubes
Dodecyl sodium sulfate, reacts at room temperature 1h, and the Au/Ag core shell nanoparticles of SDS functionalization are prepared.
Embodiment 2
(1) preparation of Au/Ag core shell nanoparticles
PVP solution by 350 μ L concentration for 10nmol/L gold nano grains solution and 200 μ L 0.5%, 100 μ L
The ascorbic acid solution of 0.2mol/L, after mixing, adds the AgNO of 70 μ L 0.2mmol/L3Solution, at room temperature lucifuge
Concussion reaction 2h, is prepared Au/Ag core shell nanoparticles solution；
(2) Au/Ag core shell nanoparticles surface modification SDS
300 μ L of Au/Ag core shell nanoparticles solution prepared by step (1) are taken to add 3mg thereto in 1mL centrifuge tubes
Dodecyl sodium sulfate, reacts at room temperature 1h, and the Au/Ag core shell nanoparticles of SDS functionalization are prepared.
Embodiment 3
(1) preparation of Au/Ag core shell nanoparticles
PVP solution by 500 μ L concentration for 20nmol/L gold nano grains solution and 300 μ L 1%, 150 μ L 0.4mol/
The ascorbic acid solution of L, after mixing, adds the AgNO of 125 μ L 0.4mmol/L3Solution, lucifuge concussion is anti-at room temperature
2h is answered, Au/Ag core shell nanoparticles solution is prepared；
(2) Au/Ag core shell nanoparticles surface modification SDS
100 μ L of Au/Ag core shell nanoparticles solution prepared by step (1) are taken to add 5mg thereto in 1mL centrifuge tubes
Dodecyl sodium sulfate, reacts at room temperature 1h, and the Au/Ag core shell nanoparticles of SDS functionalization are prepared.
Comparative example 1
The synthesis of Au nano particles：A clean conical flask A is taken to sequentially add the gold chloride of 79mL ultra-pure waters and 1mL 1%
Solution.Separately a conical flask B is taken to sequentially add 15.8mL ultra-pure waters, the citric acid three sodium solution of 4mL 1%, the list of 0.1mL 1%
Peaceful acid solution, the K of 0.1mL 25mmol/L2CO3.A, B solution are positioned over 60 DEG C of heating water bath 30min, it is then that B liquid is rapid
It is added in A liquid, and quickly stirs, 60 DEG C is continued to heat 30min, after solution colour becomes claret, stop heating, cold
But to room temperature.
Comparative example 2
The synthesis of Ag nano particles：Take a clean conical flask to be placed in ice bath, sequentially add 20mL ultra-pure waters, 5mL1%
Polyvinylpyrrolidone and 0.6mL 0.01mol/L sodium borohydride aqueous solutions.Then, filled respectively with the needle tubing of two 50mL
The aqueous povidone solution of 5mL 1% and the silver nitrate aqueous solution of 5mL 0.1%, two are fixed on miniflow syringe pump by all means
Both sides, two kinds of solution are added in the conical flask in ice bath at the same time with the speed of 30mL/h, are added while stirring until anti-
It should terminate, solution becomes buff from colourless, and reactant is placed in 80 DEG C of reaction 2h removes unreacted sodium borohydride, last molten
Liquid is changed into glassy yellow.
Comparative example 3
(1) preparation of Au/Ag core shell nanoparticles
PVP solution by 250 μ L concentration for 20nmol/L gold nano grains solution and 300 μ L 1%, 150 μ L 0.4mol/
The ascorbic acid solution of L, after mixing, adds the AgNO of 125 μ L 0.4mmol/L3Solution, lucifuge concussion is anti-at room temperature
2h is answered, Au/Ag core shell nanoparticles solution is prepared, centrifugation removes supernatant, obtains Au/Ag core shell nanoparticles.
Comparative example 4
(1) preparation of Au/Ag core shell nanoparticles
PVP solution by 500 μ L concentration for 20nmol/L gold nano grains solution and 300 μ L 1%, 150 μ L 0.4mol/
The ascorbic acid solution of L, after mixing, adds the AgNO of 125 μ L 0.4mmol/L3Solution, lucifuge concussion is anti-at room temperature
2h is answered, Au/Ag core shell nanoparticles solution is prepared；
(2) Au/Ag core shell nanoparticles surface modification SH-PEG
100 μ L of Au/Ag core shell nanoparticles solution prepared by step (1) are taken to add 5mg thereto in 1mL centrifuge tubes
Sulfydryl-polyethylene glycol (SH-PEG, molecular weight 1000), reacts at room temperature 1h, and the Au/Ag nucleocapsids that SH-PEG functionalization is prepared are received
Rice grain.
Blank group
Using physiological saline as blank group.
Performance detection：
Structure and performance test are carried out to the Au/Ag core-shell nanos material of preparation, it is specific as follows：
(1) transmission electron microscope (TEM) is tested
The TEM photos for the Au/Ag nano particles that embodiment 1 is prepared are as shown in Figure 1.It can be seen from the figure that Au/Ag
Nano particle shows obvious double-deck core shell structure, and it is gold nano core that it is internal, and particle diameter is in 10nm or so, one layer of outside parcel
For silver-colored shell, its thickness is 2-4nm.Core shell nanoparticles are evenly distributed, and form the spherical of rule, its average grain diameter is left in 15nm
It is right.
(2) bacteriostasis property is tested：
Using staphylococcus aureus and Escherichia coli as representing, measure Au/Ag core-shell nano materials are to Gram-positive
Bacterium and the bacteriostasis property of negative bacterium, embodiment 1~3, blank group and comparative example 1~4 take same volume, are mixed respectively with bacterial solution
After closing culture 6h, by contrasting the change of bacteria colony count, the bacteriostasis property of Au/Ag nano materials is evaluated.
Before sterilization processing, the clump count of bacterium is 7.0 ± 0.15log.
After embodiment 1~3, blank group and comparative example 1~4 are mixed with bacterial solution, bacteria colony count reduced value is such as
Shown in table.
1 S. aureus colonies number reduced value of table
From table 1 it follows that the bacterium of (embodiment 1~3) staphylococcus aureus of Au/Ag core-shell nano material process
Fall several reduced value and be far longer than blank group, simple gold, silver nano particle group (comparative example 1,2), Au/Ag core shell nanoparticles groups
(comparative example 3) and Au/Ag core shell nanoparticles modification SH-PEG groups (comparative example 4), fungistatic effect is obvious.This mainly with nanometer material
The concentration ratio and nano material of Au and silver Ag are related with the synergic remove of SDS in material.
2 E. coli clones number reduced value of table
| Group | Clump count reduced value (log) |
| Embodiment 1 | 6.31±0.84 |
| Embodiment 2 | 6.73±0.95 |
| Embodiment 3 | 6.55±0.64 |
| Comparative example 1 | 1.24±1.04 |
| Comparative example 2 | 3.52±0.92 |
| Comparative example 3 | 3.21±0.85 |
| Comparative example 4 | 2.48±0.75 |
| Blank group | 0 |
From Table 2, it can be seen that the clump count of (embodiment 1~3) Escherichia coli of Au/Ag core-shell nano material process subtracts
Few value is far longer than blank group, simple gold, silver nano particle group (comparative example 1,2), Au/Ag core shell nanoparticles group (comparative examples
3) and Au/Ag core shell nanoparticles modify SH-PEG groups (comparative example 4), and fungistatic effect is obvious.
3) cytotoxicity test
Using tetramethyl azo azoles salt (MTT) colorimetric method, the cytotoxicity of measure Au/Ag core-shell nano materials.Embodiment 1
~3 and the material of comparative example 1~4 take same volume, mixed respectively with Hela cell suspending liquids, 2.5%CO2, under the conditions of 37 DEG C
24h is incubated, adds MTT dyeing liquors, continues to cultivate 4h.Cell is taken out, reject nutrient solution, add dimethyl sulfoxide (DMSO), at room temperature
Lucifuge gently vibrates 15min.With the absorption value at enzyme-linked immunosorbent assay instrument measurement solution 570nm.
Figure it is seen that embodiment 1~3 and comparative example 1 and 4 show less cytotoxicity, and comparative example 2 and 3
Show larger cytotoxicity.
By the above results as can be seen that Au/Ag core shell nanoparticles prepared by this method are a kind of efficient wide spectrums kills
Microbial inoculum, it is only necessary to a small amount of concentration, you can strong bactericidal effect is produced to Gram-negative bacteria and gram-positive bacteria.Separately
Outside, it is contemplated that the toxicity that the nanometer Ag of high concentration can be larger to mammal generation, Au/Ag nano particles prepared by this method,
Under same concentrations of nanoparticles, the content of its silver ion drops significantly well below the content of silver ion in pure nano-Ag particles
Its low bio-toxicity, is a kind of novel green, efficient silver system bacteriostatic agent, is with a wide range of applications.
Claims (4)
1. a kind of Au/Ag core-shell nano materials with Efficient antibacterial performance, it is characterized in that：The material is to make by the following method
It is standby to obtain：
1）By gold nano grain solution and polyvinylpyrrolidonesolution solution,Ascorbic acid solution, silver nitrate solution mixing after room temperature
2 ~ 4 h of lucifuge concussion reaction, is prepared Au/Ag core shell nanoparticles solution；
2）By step 1）The Au/Ag core shell nanoparticles solution of preparation and dodecyl sodium sulfate hybrid reaction, obtain SDS functions
The Au/Ag core-shell nano antibacterial materials of change；
Step 1）The content of middle PVP is 0.2 ~ 1%；The content of ascorbic acid is 100 ~ 400 mmol/L；The content of silver nitrate is
0.1~0.4 mmol/L；Gold nano grain solution and polyvinylpyrrolidonesolution solution, ascorbic acid solution, the body of silver nitrate solution
Product is than being 5 ~ 10：2~6：1~3：0.5~2.5；
Step 2）The volume mass ratio of middle Au/Ag core shell nanoparticles solution and dodecyl sodium sulfate is 100 ~ 500 μ L：1~
5mg。
2. the Au/Ag core-shell nano materials according to claim 1 with Efficient antibacterial performance, it is characterised in that：Step
1）The particle diameter of middle gold nano grain is 5 ~ 15 nm；Nanogold molar concentration is 5-20 nmol/L in the solution of gold nano grain.
3. a kind of Au/Ag core-shell nano material preparation methods with Efficient antibacterial performance, it is characterized in that：This method includes following
Step：
1）Room temperature after gold nano grain solution is mixed with polyvinylpyrrolidonesolution solution, ascorbic acid solution, silver nitrate solution
2 ~ 4 h of lucifuge concussion reaction, is prepared Au/Ag core shell nanoparticles solution；
2）By step 1）The Au/Ag core shell nanoparticles solution of preparation and dodecyl sodium sulfate hybrid reaction, obtain SDS functions
The Au/Ag core-shell nano antibacterial materials of change；
Step 1）The content of middle PVP is 0.2 ~ 1%；The content of ascorbic acid is 100 ~ 400mmol/L；The content of silver nitrate is
0.1~0.4 mmol/L；Gold nano grain solution and polyvinylpyrrolidonesolution solution, ascorbic acid solution, the body of silver nitrate solution
Product ratio 5 ~ 10：2~6：1~3：0.5~2.5；
Step 2）The volume mass ratio of middle Au/Ag core shell nanoparticles solution and dodecyl sodium sulfate is 100 ~ 500 μ L：1~
5mg。
4. the Au/Ag core-shell nano material preparation methods according to claim 3 with Efficient antibacterial performance, its feature exist
In：Step 1）The particle diameter of middle gold nano grain is 5 ~ 15 nm；Nanogold molar concentration is 5-20 in the solution of gold nano grain
nmol/L。
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| CN107347913A (en) * | 2017-06-14 | 2017-11-17 | 南阳师范学院 | The preparation method of paper substrate two dimension Au@Ag core-shell nano compound disinfectants |
| CN109387500B (en) * | 2018-09-29 | 2021-01-12 | 南京农业大学 | Method for detecting escherichia coli based on magnetic graphene oxide composite star @ gold-silver alloy nanoparticles |
| CN114082973B (en) * | 2021-10-22 | 2023-02-28 | 北京航空航天大学 | Ag shell thickness control method of Au @ Ag nano core-shell material and application thereof |
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