CN109329304A - Mesoporous graphene-supported silver nano particle composite material of one kind and its preparation method and application - Google Patents
Mesoporous graphene-supported silver nano particle composite material of one kind and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of mesoporous graphene-supported silver nano particle composite materials and its preparation method and application.The mesoporous graphene-supported silver nano particle composite material is first directly to be loaded to Nano silver grain on graphene using infusion process, obtains graphene-supported silver nano particle composite material；Again by graphene-supported silver nano particle composite material carry out high temperature sintering, and obtain composite material；By weight percentage, the load capacity of Nano silver grain is 1%~20%.Synthesis process of the present invention is easy, and reaction process is easily-controllable, and prepared mesoporous graphene-supported Nano silver grain composite nano materials show excellent catalytic antimicrobial performance.
Description
Technical field
The present invention relates to the synthesis technical fields of nano carbon composite material, and in particular to a kind of to be closed using dipping-sintering process
At the mesoporous graphene-supported silver nano particle composite material with high load amount.
Background technique
Graphene is each carbon atom with SP2The form of hydridization it is tightly packed at single layer bi-dimensional cellular shape structure carbonaceous
Material, because tool high-specific surface area, surface have stronger hydrophily, thermally conductive mechanical property outstanding and outstanding electron transmission
The advantages that energy, in recent years in fields such as water process, high performance energy memory device, sensor, composite material and Raman enhancings
It is used widely.Nano silver grain makes it in chemical reaction due to its special electronic structure and huge specific surface area
Catalysis, Surface enhanced Raman scattering, sensing, biomarker and antibacterial etc. also have important application.
Currently, as drug resistance of the germ to antibiotic enhances, so that public health problem is increasingly serious, so, it finds
Novel antibacterial material is very urgent.Nano silver grain has ground the influence that different types of bacterium includes Escherichia coli extensively
Study carefully, however, the Nano silver grain as just antibacterial agent cannot be met the requirements, since the high surface energy of Nano silver grain has height
Degree reactivity, makes Nano silver grain reunite in air or in water, so a kind of complex antimicrobials of substitution must be found
To enhance the antibacterial activity of variety classes bacterium.
Summary of the invention
The object of the present invention is to be dedicated to developing high load amount and the uniform mesoporous graphene-supported silver of particle size is received
Rice corpuscles composite material has the properties such as special construction and bigger serface using graphene, is effectively controlled metal nano
The size of particle, modifies metal nanoparticle uniformly on graphene, while room temperature of the present invention carries out reducing experiment hardly possible
Degree reacts easy to control.
To achieve the above object, The technical solution adopted by the invention is as follows: a kind of mesoporous graphene-supported Nano silver grain
Composite material is first directly to be loaded to Nano silver grain on graphene using infusion process, obtains graphene-supported silver nanoparticle
Particle composite material；Again by graphene-supported silver nano particle composite material carry out high temperature sintering, and obtain composite material；It presses
Weight percent, the load capacity of Nano silver grain are 1%~20%.
A kind of preparation method of mesoporous graphene-supported silver nano particle composite material, includes the following steps:
1) it impregnates: graphene being dissolved in the mixed solution of water and ethyl alcohol, obtain graphene solution；By silver nitrate plus water-soluble
Solution, ammonium hydroxide is added to be become clarifying to solution from muddiness, obtains silver ammino solution；Silver ammino solution is added dropwise in graphene solution,
It stirs evenly, is impregnated at room temperature to solvent and volatilized completely, obtain graphene-supported silver nano particle composite material；
2) be sintered: graphene-supported silver nano particle composite material is sprawled in porcelain boat, is put in tube furnace, is gradually warmed up
To 400~450 DEG C, 30~300min is kept, mesoporous graphene-supported silver nano particle composite material is obtained.
The preparation method of the above-mentioned mesoporous graphene-supported silver nano particle composite material of one kind, by volume, water: ethyl alcohol
=1:1.
Application of the above-mentioned mesoporous graphene-supported silver nano particle composite material in catalytic antimicrobial.Method is as follows: in
In bacteria suspension, above-mentioned mesoporous graphene-supported silver nano particle composite material is added.Further, bacteria suspension pH=7.0
Phosphate buffer solution dilution；The phosphoric acid buffer of above-mentioned mesoporous graphene-supported silver nano particle composite material pH=7.0
Solution ultrasonic disperse.
Compared with prior art, the present invention has the advantage that
1. the present invention selects graphene as carrier, first is that graphene can serve as Nano silver grain place steady in a long-term
Main, for drug transmission platform；Second is that, with Nano silver grain for antibacterial center, graphene, which is used as, to be divided during antibacterial
Powder reduces the reunion of Nano silver grain, while being modified again to graphene surface, and graphene surface is made to generate bound site
Point, increases the bigger serface effect of Nano silver grain, and biggish specific surface area enables it to the cell for being quickly adsorbed on bacterium
In film surface, the normal substance transmitting of cell membrane is hindered, or enter into the cell, make its inactivation to change in conjunction with the enzyme of part
The physiological activity of cell reaches the process for inhibiting to increase.
2. the present invention uses the mesoporous graphene-supported Nano silver grain composite wood of dipping-sintering process preparation high load amount
Material.Joined concentrated ammonia liquor in course of dissolution promotes metal nanoparticle to have good dispersibility, at the same time entire reaction
It is added without additional reducing agent, mild condition is pollution-free, can get the graphene-supported Nano silver grain composite wood of high load amount
Material.
3. there is graphene surface by sintering mesoporous, improves the contact area of nano silver, and make Yin Na in the present invention
Rice corpuscles forms twin, reduces Nano silver grain partial size, improves material antibacterial action.
4. mesoporous graphene-supported silver nano particle composite material of the invention, in chemical engineering, catalysis and biology doctor
There is boundless application prospect in the fields such as medicine.
5. the present invention, can be obtained mesoporous graphene-supported Nano silver grain composite wood by simple heat treatment
Material.
6. the present invention, metal nanoparticle modification is single step reaction, and reaction condition is controllable, and step is easy, is easy to weight
It is multiple.
7. the present invention, the partial size of the Nano silver grain of preparation is small, and in 5-10nm or so, size distribution is uniform, is in granular form.
8. the present invention is added without additional reducing agent, environment-friendly high-efficiency, disposition is conveniently.
Detailed description of the invention
Fig. 1 is the dependent transmissive electron microscope picture (TEM figure) of graphene；
Wherein, A:50nm；B:2nm.
Fig. 2 is that the correlation of graphene-supported silver nano particle composite material (load capacity 10wt%) prepared by infusion process is saturating
Penetrate electron microscope picture (TEM figure)；
Wherein, A:50nm；B:2nm.
Fig. 3 is the related X of graphene-supported silver nano particle composite material (load capacity 10wt%) prepared by infusion process
X ray diffration pattern x (XRD diagram).
Fig. 4 is that (load capacity is for the mesoporous graphene-supported silver nano particle composite material of dipping-sintering process (2h) preparation
Dependent transmissive electron microscope picture (TEM figure) 10wt%).
Wherein, A:20nm；B:2nm.
Fig. 5 is that (load capacity is for the mesoporous graphene-supported silver nano particle composite material of dipping-sintering process (2h) preparation
Associated x-ray diffraction pattern (XRD diagram) 10wt%)
Fig. 6 is that (load capacity is for the mesoporous graphene-supported silver nano particle composite material of dipping-sintering process (5h) preparation
Dependent transmissive electron microscope picture (TEM figure) 10wt%).
Wherein, A:100nm；B:5nm.
Fig. 7 is that (load capacity is for the mesoporous graphene-supported silver nano particle composite material of dipping-sintering process (5h) preparation
Associated x-ray diffraction pattern (XRD diagram) 10wt%)
Fig. 8 is graphene-supported silver nano particle composite material (load capacity 10wt%) prepared by infusion process and dipping-
The dependent antimicrobial effect picture of the mesoporous graphene-supported silver nano particle composite material of sintering process (2h and 5h) preparation.
Wherein, A: blank；B: infusion process Ag-GO antibacterial effect figure；C: dipping-sintering process (2h) Ag-GO antibacterial effect figure；
D: dipping-sintering process (5h) Ag-GO antibacterial effect figure.
Specific embodiment
Technical solution for a better understanding of the present invention, spy are described in further detail with specific embodiment, but side
Case is without being limited thereto.
The preparation of mesoporous graphene-supported silver nano particle composite material includes the following steps:
1. infusion process prepares graphene-supported silver nano particle composite material: it is soluble in water to weigh silver nitrate, and ammonium hydroxide is added
Become clarifying to solution from muddiness, obtains silver ammino solution；Graphene is dissolved in water and ethyl alcohol (volume ratio 1:1) mixed solution,
Obtain graphene solution；Silver ammino solution is added dropwise in graphene solution, after being sufficiently mixed, constant temperature is stirred to molten at 25 DEG C
Agent is volatilized completely, obtains graphene-supported silver nano particle composite material.
In this step, needed for the dosage of silver nitrate on prepared graphene according to loading in silver nano particle composite material
Silver atoms content determines.By weight percentage, the load capacity of Nano silver grain is 1%~20%.
2. sintering process prepares mesoporous graphene-supported silver nano particle composite material: step 1 being obtained graphene-supported
Silver nano particle composite material is sprawled in porcelain boat, is put in tube furnace, is gradually heated to 400~450 DEG C, keep 30~
300min obtains mesoporous graphene-supported silver nano particle composite material.
The graphene-supported silver nano particle composite material of embodiment 1
(1) infusion process prepares graphene-supported silver nano particle composite material
200mg graphene 10mL water and the dissolution of 10mL ethyl alcohol are weighed, graphene solution is obtained.
Weigh 0.035g AgNO3It is dissolved with 0.1mL water, concentrated ammonia liquor is then added thereto, until solution becomes clear from muddiness
Clearly, silver ammino solution is obtained.
Silver ammino solution is added dropwise in graphene solution, mixing shakes up, and constant temperature stirs complete to solvent at 25 DEG C
Volatilization obtains the graphene-supported silver nano particle composite material that silver load capacity is 10wt%.
(2) it detects
Fig. 1 is the dependent transmissive electron microscope picture (TEM figure) of graphene.As seen from Figure 1, it can be seen that graphene is in piece
Shape structure possesses biggish specific surface area, this facilitates the load and dispersion of Nano silver grain.
Fig. 2 is to use load capacity prepared by infusion process for the phase of the graphene-supported silver nano particle composite material of 10wt%
It closes transmission electron microscope figure (TEM figure).As seen from Figure 2, it can be seen that Nano silver grain partial size is smaller, it is well dispersed, with list
Crystalline form exists, and agglomeration does not occur.
Fig. 3 is to use load capacity prepared by infusion process for the phase of the graphene-supported silver nano particle composite material of 10wt%
Close X-ray diffractogram.As seen from Figure 3, Nano silver grain is in 38.5 ° of 111 crystal face preferential growth, and there is no changing for structure
Become.
The mesoporous graphene-supported silver nano particle composite material of embodiment 2
(1) dipping-sintering process prepares mesoporous graphene-supported silver nano particle composite material
1, infusion process prepares graphene-supported silver nano particle composite material:
With embodiment 1 (one)
2, sintering process prepares mesoporous graphene-supported silver nano particle composite material:
It weighs the graphene-supported silver nano particle composite material that 50mg step 1 obtains to sprawl in porcelain boat, is put in tubular type
In furnace, 400 DEG C are gradually heated to, is sintered 2h, it is compound to obtain the mesoporous graphene-supported Nano silver grain that silver load capacity is 10wt%
Material.
(2) it detects
Fig. 4 be the sintering 2h for using the preparation of dipping-sintering process after load capacity for the mesoporous graphene-supported silver of 10wt%
The dependent transmissive electron microscope picture (TEM figure) of nano composition.As seen from Figure 4, it can be seen that occur on graphene
Mesoporous, Nano silver grain partial size becomes smaller, is well dispersed, forming twin, and agglomeration does not occur.
Fig. 5 be the sintering 2h for using the preparation of dipping-sintering process after load capacity for the mesoporous graphene-supported silver of 10wt%
The associated x-ray diffraction pattern of nano composition.As seen from Figure 5, Nano silver grain is in 38.5 ° of 111 crystal face preferential growth,
No change has taken place for structure.
The mesoporous graphene-supported silver nano particle composite material of embodiment 3
(1) dipping-sintering process prepares mesoporous graphene-supported silver nano particle composite material
1, infusion process prepares graphene-supported silver nano particle composite material:
With embodiment 1 (one)
2, sintering process prepares mesoporous graphene-supported silver nano particle composite material:
It weighs the graphene-supported silver nano particle composite material that 50mg step 1 obtains to sprawl in porcelain boat, is put in tubular type
In furnace, 400 DEG C are gradually heated to, is sintered 5h, it is compound to obtain the mesoporous graphene-supported Nano silver grain that silver load capacity is 10wt%
Material.
(2) it detects
Fig. 6 be the sintering 5h for using the preparation of dipping-sintering process after load capacity for the mesoporous graphene-supported silver of 10wt%
The dependent transmissive electron microscope picture (TEM figure) of nano composition.As seen from Figure 6, it can be seen that graphene skeleton quilt
Serious to destroy, Nano silver grain aggregation is serious.
Fig. 7 be the sintering 5h for using the preparation of dipping-sintering process after load capacity for the mesoporous graphene-supported silver of 10wt%
The associated x-ray diffraction pattern of nano composition.As seen from Figure 7, Nano silver grain is in 38.5 ° of 111 crystal face preferential growth,
Partial size increases.
4 anti-microbial property test of embodiment
The preparation of LB culture medium: weighing sodium chloride 2.5012g, peptone 2.5015g, and yeast extract 1.2519g is added water to
250mL adjusts its pH=7.2~7.4 with NaOH solution, obtains LB liquid medium；2% fine jade is added into fluid nutrient medium
Solid medium can be obtained in rouge, and culture medium is placed in 121 DEG C of high-pressure steam sterilizing pans the 30min that sterilizes, is refrigerated spare.
With oese picking strain Escherichia coli (E.coli ATCC 15597), cross on solid medium, at 37 DEG C
It is cultivated in incubator for 24 hours, picking single bacterium is fallen in LB liquid medium, cultivates 11h in 37 DEG C of constant temperature oscillator, obtains OD value
For 1.820 bacteria suspension.
Take 5mL bacteria suspension in being centrifuged 20min on centrifuge, with the phosphate buffer solution (hereinafter referred to as " PBS ") of pH=7.0
After washing, PBS is added, obtains PBS bacteria suspension；Bacteria suspension is diluted step by step with phosphate buffer solution, keeps it final dilute
Releasing concentration is 103cfu·mL-1。
Graphene-supported silver nano particle composite material (the load of Nano silver grain of the preparation of 5mg embodiment 1 is weighed respectively
The mesoporous graphene-supported silver nano particle composite material (load capacity of Nano silver grain that amount is 10wt%), prepared by embodiment 2
For 10wt%, be sintered 2h) and the preparation of embodiment 3 mesoporous graphene-supported silver nano particle composite material (Nano silver grain
Load capacity is 10wt%, is sintered 5h) it is put in centrifuge tube, PBS ultrasonic disperse is added, 0.5mL concentration, which is then added, is
103cfu·mL-1Bacteria suspension, sufficiently shake up, take 100 μ L spread plates, plate is put in 37 DEG C of constant incubators and is cultivated
For 24 hours, bacterium colony growing state is observed, while counting and calculating sterilizing rate, as a result as shown in Figure 8.
As seen from Figure 8, it is found by antibacterial experiment, embodiment 1 is using prepared by infusion process unsintered graphene-supported
The antibiotic rate of silver nano particle composite material is 55%, and embodiment 2 and 3 is negative by the mesoporous graphene of sintering 2h, 5h preparation
The antibiotic rate of silver-carrying nano particle composite material respectively reaches 100%, 86%, obtains after adequately illustrating sintering 2h of the invention
Mesoporous graphene-supported silver nano particle composite material have excellent anti-microbial property.
Claims (6)
1. a kind of mesoporous graphene-supported silver nano particle composite material, which is characterized in that the mesoporous graphene-supported silver
Nano composition is first directly to be loaded to Nano silver grain on graphene using infusion process, and it is negative to obtain graphene
Silver-carrying nano particle composite material；Graphene-supported silver nano particle composite material is subjected to high temperature sintering again, and what is obtained answers
Condensation material；By weight percentage, the load capacity of Nano silver grain is 1%~20%.
2. the preparation method of the mesoporous graphene-supported silver nano particle composite material of one kind described in claim 1, feature exist
In including the following steps:
1) it impregnates: graphene being dissolved in the mixed solution of water and ethyl alcohol, obtain graphene solution；Silver nitrate is dissolved in water,
Ammonium hydroxide is added to be become clarifying to solution from muddiness, obtains silver ammino solution；Silver ammino solution is added dropwise in graphene solution, is stirred
Uniformly, it is impregnated at room temperature to solvent and is volatilized completely, obtain graphene-supported silver nano particle composite material；
2) be sintered: graphene-supported silver nano particle composite material is sprawled in porcelain boat, is put in tube furnace, is gradually heated to
400~450 DEG C, 30~300min is kept, mesoporous graphene-supported silver nano particle composite material is obtained.
3. the preparation method of the mesoporous graphene-supported silver nano particle composite material of one kind according to claim 2, special
Sign is, by volume, water: ethyl alcohol=1:1.
4. application of the mesoporous graphene-supported silver nano particle composite material described in claim 1 in catalytic antimicrobial.
5. application according to claim 4, which is characterized in that method is as follows: in bacteria suspension, claim 1 institute is added
The mesoporous graphene-supported silver nano particle composite material stated.
6. application according to claim 5, which is characterized in that bacteria suspension is diluted with the phosphate buffer solution of pH=7.0；Power
Benefit require 1 described in mesoporous graphene-supported silver nano particle composite material pH=7.0 phosphate buffer solution ultrasonic disperse.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114477152A (en) * | 2021-12-30 | 2022-05-13 | 杭州电子科技大学 | Silver nanoparticle/multilayer graphene composite material and preparation method thereof |
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