CN108557757B - A kind of supported porous silver oxide nanosheet composite material of nano-porous silver and preparation method thereof - Google Patents
A kind of supported porous silver oxide nanosheet composite material of nano-porous silver and preparation method thereof Download PDFInfo
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Abstract
The present invention is supported porous silver oxide nanosheet composite material of a kind of nano-porous silver and preparation method thereof.The composite material is bar, including noncrystal substrate, the nano-porous silver being covered on noncrystal substrate and the porous oxidation Nano silver piece for being supported on nanoporous silver surface；The noncrystal substrate is CuxZryAgzAlloying component, wherein x, y, z are atomic percent, 35≤x≤45,35≤y≤45,10≤z≤30, and x+y+z=100；Wherein 100~150 μm of nano-porous silver thickness, tough 20~110nm of bandwidth, 30~150nm of aperture size；Nanometer sheet 50~110nm of thickness, nanometer length of a film 150~400nm, wide 10~100nm, 5~10nm of thickness；Nano aperture in nanometer sheet is having a size of 1~3nm.The composite material occupies unique structure and performance advantage in anti-biotic material field.
Description
Technical field:
The present invention relates to nano-porous materials technical field, specifically a kind of supported porous silver oxide of nano-porous silver
Nanosheet composite material and preparation method thereof.
Background technique:
In recent years, the harmful microbes such as bacterium, fungi are propagated wantonly has seriously threatened human health.How to prepare
A kind of material with good anti-microbial property out, becomes the problem of people increasingly pay attention to.It is well known that Ag and Ag+Yin Qizhuo
Sterilization more, bacteria resistance function occupy an important position in anti-biotic material field.And nanosizing and porous, it is to improve Ag and Ag+It is anti-
The effective ways of bacterium performance.
First technology, publication number CN107338402A " a kind of nanoporous copper-silver bimetallic/bimetallic oxide and its system
Preparation Method and application " in the patent, prepares copper-silver bimetallic/bimetallic oxide nanowire composite, due to copper gold
The presence of category/copper metal oxide so that the antibacterial agent do not have specificity, and weaken to a certain extent silver metal/
The antibacterial ability of siluer metal oxide.In addition to this, copper has faint toxicity, can be to surrounding material band if a large amount of use
Potentially threaten.
First technology, publication number CN1771807B " inorganic antiseptic of zinc oxide lattice carried silver and preparation method thereof ", this is specially
In benefit, need intermediate product obtained in N2Zinc oxide can just be obtained by roasting 30~180 minutes under atmosphere in 600~1000 DEG C
Lattice carried silver antibacterial agent.The demand of hot conditions consumes a large amount of energy, and N2Antibacterial agent increasing is prepared under ambient conditions
Add experimental cost, is unfavorable for marketing.In addition to this, zinc oxide carrier is mostly graininess, and is had to size stringent
It is required that graininess sample is easy mutually to block and accumulate, antimicrobial efficiency is reduced.And it is not easy to recycle after application, increase is drawn
A possibility that sending out secondary pollution.The antibacterial agent prepared, Ag+It is only entrained in zinc oxide carrier, connection is not close, is using
It is easy to be detached from the carrier in the process.
Summary of the invention:
It is an object of the present invention to easily reunite in use for antimicrobial granular material in current techniques, use
After the deficiencies of being not easily recycled and being separated with matrix, provide a kind of supported porous silver oxide nanosheet composite material of nano-porous silver and
Preparation method.The material includes the nano-porous silver composite bar of noncrystal substrate support and the porous oxygen for being supported on its surface
Change Nano silver piece.Its method is that amorphous bar is first carried out a step to take off the nano-porous silver that alloying technology prepares noncrystal substrate support
Composite bar then aoxidizes out porous oxidation Nano silver piece in nano-porous silver surface in situ using cyclic voltammetry, by phase
The appropriate selection of parameter and combining closely to each other are closed, the composite material with the structure is prepared.Prepared by the present invention
Rodlike composite material has bigger specific surface area, and then the Fast Stripping of more conducively silver ion compared to reported at present, and
And oxidation Nano silver piece is completely embedded with metallic silver, is not readily separated.Use easily recycling later, is recycled recycling.This is compound
Material occupies unique structure and performance advantage in anti-biotic material field.
The technical scheme is that
A kind of supported porous silver oxide nanosheet composite material of nano-porous silver, the composite material are bar, including amorphous
Matrix, the nano-porous silver being covered on noncrystal substrate and the porous oxidation Nano silver piece for being supported on nanoporous silver surface；
The noncrystal substrate is CuxZryAgzAlloying component, wherein x, y, z are atomic percent, 35≤x≤45,35≤y≤45,10
≤ z≤30, and x+y+z=100；Wherein 100~150 μm of nano-porous silver thickness, tough 20~110nm of bandwidth, aperture size 30
~150nm；Nanometer sheet 50~110nm of thickness, nanometer length of a film 150~400nm, wide 10~100nm, 5~10nm of thickness；In nanometer sheet
Nano aperture having a size of 1~3nm.
The preparation method of the supported porous silver oxide nanosheet composite material of the nano-porous silver, includes the following steps:
The first step, de- alloy treatment Cu-Zr-Ag amorphous bar prepare nano-porous silver
The Cu-Zr-Ag amorphous bar that diameter is 1~2mm of Ф is placed in and carries out freely taking off alloy in corrosive liquid, obtains nanometer
Porous silver metal；Wherein, corrosive liquid is the HNO of the HF and 0.5~4M of 0.05~0.25M of concentration3The mixed solution of solution, mixing
The volume ratio of solution is HF solution: HNO3Solution=1:1；Etching time is 0.5~5h；Corrosion temperature is 25 DEG C of constant temperature；
Second step, cyclic voltammetry prepare the supported porous silver oxide nanosheet composite material of nano-porous silver
Using platinum electrode as auxiliary electrode, Ag/AgCl makees as reference electrode, nanoporous silver metal obtained in the previous step
For working electrode, three electrode test systems are combined into, carry out cyclic voltammetry preparation；Composite material obtained is placed in drying box
In in 60~100 DEG C of dry 1~2h, obtain the supported porous silver oxide nanosheet composite material of nano-porous silver；
Wherein, in cyclic voltammetry, voltage window is 0~0.6V, sweep speed 100mV s-1, scan all numbers 10~50
Week；Electrolyte is the NaOH solution that concentration is 0.5~2M；Operating temperature is 25 DEG C of constant temperature.
The application of the supported porous silver oxide nanosheet composite material of the nano-porous silver, for killing except bacterium or very
Bacterium.
The bacterium or fungi is one or both of Escherichia coli, staphylococcus aureus.
Above-mentioned supported porous silver oxide nanosheet composite material of a kind of nano-porous silver and preparation method thereof, used original
Material and facility passes through well known approach and obtains, and operating procedure used is that those skilled in the art can grasp
's.
Substantive distinguishing features of the invention are as follows:
In current techniques, silver or silver oxide powder are prepared often through colloidal sol, gel method, is easily rolled into a ball in use
It is poly-, antimicrobial efficiency is reduced, and be not easily recycled after application, is difficult to reuse；Either by infusion process silver metal or
Ag+Other antibacterial metal surfaces such as Ti piece, ZnO are loaded to, but this makes silver-colored and between silver oxide and matrix binding force weaker, makes
Easy to fall off with process, the mechanical integrity of material is destroyed, and antimicrobial efficiency reduces.And this patent passes through cyclic voltammetry,
The oxidation of nano-porous silver composite bar surface in situ generates porous oxidation Nano silver piece, so that porous oxidation Nano silver piece and matrix
Between binding force it is quite strong, be difficult to fall off in use process, and easily recycling, realize recycling.In addition to this, this patent is made
Composite material there was only silver element, purity is high, exclusive antibacterial characteristics are improved.Composite material obtained has a large amount of hole
Structure, not only increases the specific surface area of material, and has saved cost, improves economic benefit.
Compared with existing technology, beneficial effects of the present invention are as follows:
(1) present invention prepares a kind of antimicrobial composite material with multilevel structure for the first time, including noncrystal substrate, is covered on
Nano-porous silver on noncrystal substrate and the porous oxidation Nano silver piece for being supported on nanoporous silver surface.Wherein taking off alloy can
100~150 μm of thickness are prepared, the nanoporous silver metal of tough 20~110nm of bandwidth, 30~150nm of aperture size.Then benefit
50~110nm of thickness, long 150~400nm, wide 10~100nm is prepared on its surface out with cyclic voltammetry, 5~10nm's of thickness
Ultra-thin oxidation Nano silver piece.It distributed nano aperture largely having a size of 1~3nm in nanometer sheet, which has efficient
Bactericidal property.
(2) de- alloying technology and cyclic voltammetry are dexterously combined together by the present invention, only need 1.5~7h that can prepare
A kind of supported porous oxidation Nano silver piece composite bar of nano-porous silver, the preparation process is simple, short preparation period；Pass through circulation
Voltammetry aoxidizes out porous oxidation Nano silver piece in nano-porous silver composite bar surface in situ, so that porous oxidation Nano silver piece
It is completely embedded with nano-porous silver, therefore the composite material possesses good mechanical integrity and porous structure.It is recyclable to repeat
It utilizes, save the cost, economic benefit is improved.
(3) it is covered with the nano aperture having a size of 1~3nm on the ultra-thin oxidation Nano silver piece prepared by the present invention.Therefore it gathers around
There are more abundant porosity and bigger specific surface area.Be conducive to the anti-biotic material to come into full contact with bacterial solution, thus fastly
Speed is efficiently killed except bacterium.In addition to this, nano-porous silver/silver oxide prepared by the present invention does not have other element dopings, so that
Anti-microbial property is strengthened.Compared with the Cu-Zr-Ag amorphous bar without this hole configurations of same size, prepared by the present invention
Composite bar anti-microbial property improve 40.6%~50.8%.
Detailed description of the invention:
Fig. 1: the stereoscan photograph of the nano-porous silver prepared in embodiment 1.
Fig. 2: the EDS map of the supported porous oxidation Nano silver piece of the nano-porous silver prepared in embodiment 1.
Fig. 3: the stereoscan photograph of the supported porous oxidation Nano silver piece of the nano-porous silver prepared in embodiment 1.
Specific embodiment
Cu of the present inventionxZryAgzAlloying component is well known materials, wherein x, y, and z is atomic percent, 35≤x≤
45,35≤y≤45,10≤z≤30, and x+y+z=100.
Embodiment 1
The Cu for being Ф 2mm by diameter40Zr40Ag20Amorphous bar is cut into the stub that length is 10mm.Place it in corrosion
It carries out freely taking off alloy in liquid.Experiment condition is that will contain 0.1M HF and 0.67M HNO3Mixed solution as corrosive liquid, it is rotten
The volume ratio for losing liquid is HF solution: HNO3Solution=1:1, etching time 1h, 25 DEG C of corrosion temperature.It is clear with deionized water after taking-up
It washes, obtains nanoporous silver metal.Fig. 1 is the stereoscan photograph of the nano-porous silver prepared in the present embodiment, can be determined
Nano-porous silver obtained has uniform, co-continuous ligament/hole configurations three-dimensional (3D) nanoporous pattern.Nanoporous
Silver layer is 110 μm, ligament width 80nm, aperture size 50nm thick.
Using platinum electrode as auxiliary electrode, Ag/AgCl makees as reference electrode, nanoporous silver metal obtained in the previous step
Three electrode test systems are combined into for working electrode, carry out cyclic voltammetry.Wherein, in cyclic voltammetry, voltage window 0
~0.6V, sweep speed 100mV s-1, scan all number 10 weeks；Electrolyte is that concentration is 1M NaOH solution；25 DEG C of operating temperature.
It is cleaned after composite material obtained is taken out with deionized water, is placed in drying box in 60 DEG C of dry 1h, obtains nanoporous
The supported porous silver oxide nanosheet composite material of silver.Fig. 2 is the supported porous silver oxide of nano-porous silver prepared in the present embodiment
The EDS map of nanometer sheet, it was demonstrated that obtained porous nano-sheet is silver oxide.Fig. 3 is the nanoporous prepared in the present embodiment
The stereoscan photograph of the supported porous oxidation Nano silver piece of silver, it can be observed that neat fine and close on nanoporous silver metal cover
One layer of cuprous nano piece of lid, wherein nanometer sheet thickness 60nm, nanometer length of a film 200nm, wide 50nm, thick 5nm.It is more by nanometer
The transmission electron microscope photo of the supported porous oxidation Nano silver piece of hole silver is we can observe that the bore hole size in nanometer sheet is 1nm.
The supported porous silver oxide nanosheet composite material of the nano-porous silver made from the present embodiment carries out bactericidal property survey
The experimentation of examination is as follows:
It selects Escherichia coli to carry out bactericidal property test experiments, Escherichia coli is configured to 1 × 10 in the medium8~2
×108The bacteria suspension of a/ml (a is bacterium number), 121 DEG C of autoclave sterilization 20min in retort are placed in 37 DEG C of constant temperature trainings
Support cradle in shaken cultivation for 24 hours.After for 24 hours, take 8ml bacterium solution in centrifuge tube.It is when experiment that nano-porous silver obtained load is more
The Cu without this hole configurations of hole silver oxide nanosheet composite material and same size40Zr40Ag20Amorphous bar (control group) point
It is not placed in above-mentioned centrifuge tube.After centrifuge tube is shaken up, the 200 μ l of bacterium solution after culture is taken out respectively, utilizes DNM-9602 enzyme mark
Analyzer carries out absorbance test.The result shows that composite material made from the present embodiment is than same size within a certain period of time
Cu without this hole configurations40Zr40Ag20Amorphous bar (control group) germicidal efficiency is higher by 50%.The composite material is recycled
Sterilization experiment, discovery is to (each circulation 10min) after 5 circulations of congruent, different batches bacterium solution sterilization, still than identical rule
The Cu without this hole configurations of lattice40Zr40Ag20Amorphous bar (control group) germicidal efficiency is higher by 42.8%.Illustrate that this implementation is made
The supported porous silver oxide nanosheet composite material of nano-porous silver has good bactericidal property.The performance has benefited from composite material
The structural advantage of itself regulatable nanoporous silver matrix and porous oxidation Nano silver piece, while it is good also to have benefited from material
Self-supporting and mechanical integrity so that porous oxidation Nano silver piece connect during the reaction with nanoporous silver matrix it is good
It is good.
Embodiment 2
The Cu for being Ф 1.5mm by diameter35Zr35Ag30Amorphous bar is cut into the stub that length is 10mm.Place it in corruption
It carries out freely taking off alloy in erosion liquid.Experiment condition is that will contain 0.2M HF and 3.5M HNO3Mixed solution as corrosive liquid,
The volume ratio of corrosive liquid is HF solution: HNO3Solution=1:1, etching time 0.5h, 25 DEG C of corrosion temperature.Deionization is used after taking-up
Water cleaning, obtains nanoporous silver metal.Nano-porous silver obtained has uniform, co-continuous ligament/hole configurations three
Tie up (3D) nanoporous pattern.130 μm of nano-porous silver thickness, ligament width 50nm, aperture size 75nm.
Using platinum electrode as auxiliary electrode, Ag/AgCl makees as reference electrode, nanoporous silver metal obtained in the previous step
Three electrode test systems are combined into for working electrode, carry out cyclic voltammetry.Wherein, in cyclic voltammetry, voltage window 0
~0.6V, sweep speed 100mV s-1, scan all number 30 weeks；Electrolyte is that concentration is 2M NaOH solution；25 DEG C of operating temperature.
It is cleaned after composite material obtained is taken out with deionized water, is placed in drying box in 70 DEG C of dry 2h, obtains nanoporous
The supported porous silver oxide nanosheet composite material of silver.Wherein nanometer sheet thickness 70nm, nanometer length of a film 350nm, wide 30nm are thick
8.5nm.Bore hole size in nanometer sheet is 3nm.
The supported porous silver oxide nanosheet composite material of the nano-porous silver made from the present embodiment carries out bactericidal property survey
The experimentation of examination is as follows:
It selects gold-coloured staphylococci to carry out bactericidal property test experiments, gold-coloured staphylococci is configured to 1 in the medium
×108~2 × 108The bacteria suspension of a/ml (a is bacterium number), 121 DEG C of autoclave sterilization 20min in retort are placed in 37 DEG C
Shaken cultivation is for 24 hours in constant temperature incubation cradle.After for 24 hours, take 8ml bacterium solution in centrifuge tube.By nano-porous silver obtained when experiment
The Cu without this hole configurations of supported porous silver oxide nanosheet composite material and same size35Zr35Ag30(the control of amorphous bar
Group) it is respectively placed in above-mentioned centrifuge tube.After centrifuge tube is shaken up, the 200 μ l of bacterium solution after culture is taken out respectively, utilizes DNM-9602
Enzyme micro-plate reader carries out absorbance test.The result shows that composite material made from the present embodiment is than identical rule within a certain period of time
The Cu without this hole configurations of lattice35Zr35Ag30Amorphous bar (control group) germicidal efficiency is higher by 50.8%.By the composite material into
(each circulation 10min) after 5 circulations of congruent, different batches bacterium solution sterilization is still compared in the experiment of row recycling sterilizing, discovery
The Cu without this hole configurations of same size35Zr35Ag30Amorphous bar (control group) germicidal efficiency is higher by 45%.Illustrate this implementation
The made supported porous silver oxide nanosheet composite material of nano-porous silver has good bactericidal property.
Embodiment 3
The Cu for being Ф 1mm by diameter45Zr45Ag10Amorphous bar is cut into the stub that length is 10mm.Place it in corrosion
It carries out freely taking off alloy in liquid.Experiment condition is that will contain 0.15M HF and 1.5M HNO3Mixed solution as corrosive liquid, it is rotten
The volume ratio for losing liquid is HF solution: HNO3Solution=1:1, etching time 3h, 25 DEG C of corrosion temperature.It is clear with deionized water after taking-up
It washes, obtains nanoporous silver metal.Nano-porous silver obtained has uniform, co-continuous ligament/hole configurations three-dimensional
(3D) nanoporous pattern.150 μm of nano-porous silver thickness, ligament width 100nm, aperture size 110nm.
Using platinum electrode as auxiliary electrode, Ag/AgCl makees as reference electrode, nanoporous silver metal obtained in the previous step
Three electrode test systems are combined into for working electrode, carry out cyclic voltammetry.Wherein, in cyclic voltammetry, voltage window 0
~0.6V, sweep speed 100mV s-1, scan all number 40 weeks；Electrolyte is that concentration is 0.5M NaOH solution；Operating temperature 25
℃.It is cleaned after composite material obtained is taken out with deionized water, is placed in drying box in 80 DEG C of dry 1h, it is more to obtain nanometer
The supported porous silver oxide nanosheet composite material of hole silver.Wherein nanometer sheet thickness 100nm, nanometer length of a film 300nm, wide 95nm are thick
10nm.Bore hole size in nanometer sheet is 2nm.
The supported porous silver oxide nanosheet composite material of the nano-porous silver made from the present embodiment carries out bactericidal property survey
The experimentation of examination is as follows:
It selects Escherichia coli and staphylococcus aureus to carry out bactericidal property test experiments, gold-coloured staphylococci is being cultivated
1 × 10 is configured in base8~2 × 108The bacteria suspension of a/ml (a is bacterium number), 121 DEG C of autoclave sterilizations in retort
20min is placed in 37 DEG C of constant temperature incubation cradles shaken cultivation for 24 hours.After for 24 hours, take 8ml bacterium solution in centrifuge tube.It will system when experiment
Nano-porous silver supported porous silver oxide nanosheet composite material and same size without this hole configurations
Cu45Zr45Ag10Amorphous bar (control group) is respectively placed in above-mentioned centrifuge tube.After centrifuge tube is shaken up, after taking out culture respectively
200 μ l of bacterium solution, utilize DNM-9602 enzyme micro-plate reader carry out absorbance test.The result shows that this implementation within a certain period of time
Cu without this hole configurations of the composite material made from example than same size45Zr45Ag10Amorphous bar (control group) germicidal efficiency
It is higher by 40.6%.The composite material is subjected to recycling sterilizing experiment, discovery is sterilized 5 to congruent, different batches bacterium solution and followed
After ring (each circulation 10min), still than the Cu without this hole configurations of same size45Zr45Ag10Amorphous bar (control group)
Germicidal efficiency is higher by 39.5%.Illustrate that the supported porous silver oxide nanosheet composite material of the made nano-porous silver of this implementation has very
Good bactericidal property.
Comparative example 1:
In de- alloy, select 2M HF as corrosive liquid, other conditions are examined with embodiment 1, products therefrom through micro- Electronic Speculum
It surveys, not it is observed that nano-porous silver.
Comparative example 2:
In cyclic voltammetry, selecting circulating cycle number is 100 weeks, and other conditions do not generate with embodiment 1, gained sample
Nano-sheet silver oxide, and generate the spherical silver oxide of non-uniform nanometer.
Comparative example 3:
In cyclic voltammetry, select electrolyte for 1M KOH, other conditions are with embodiment 1, and gained sample surfaces are only
Generation quantity is few and the oxidation Nano silver piece of scattered distribution.
The above comparative example is to implement the case of failure, arbitrarily change preparation parameter of the present invention will lead to can not obtain it is tough
The good nano-porous silver of band/hole pattern or porous oxidation Nano silver piece etc..
When amorphous alloy bar obtained is carried out de- alloying technology, it is necessary to select HF and HNO3Mixed solution conduct
Otherwise corrosive liquid cannot get nanoporous silver metal；When cyclic voltammetry, experiment parameter need to be reasonably selected, otherwise nanometer is more
The oxidation Nano silver piece effect that hole silver surface generates is undesirable, and then has an impact to composite material anti-microbial property.
Unaccomplished matter of the present invention is well-known technique.
Claims (3)
1. a kind of supported porous silver oxide nanosheet composite material of nano-porous silver, it is characterized in that the composite material is bar, packet
Include noncrystal substrate, the nano-porous silver that is covered on noncrystal substrate and the porous oxidation silver for being supported on nanoporous silver surface are received
Rice piece；The noncrystal substrate is CuxZryAgzAlloying component, wherein x, y, z are atomic percent, 35≤x≤45,35
≤ y≤45,10≤z≤30, and+z=100 x+y；Wherein 100 ~ 150 μm of nano-porous silver thickness, tough bandwidth
20 ~ 110 nm, 30 ~ 150 nm of aperture size；50 ~ 110 nm of nanometer sheet thickness, nanometer length of a film 150 ~ 400 nm, it is wide by 10 ~ 100
Nm, 5 ~ 10 nm of thickness；Nano aperture in nanometer sheet is having a size of 1 ~ 3 nm；
The preparation method of the supported porous silver oxide nanosheet composite material of the nano-porous silver, includes the following steps:
The first step, de- alloy treatment Cu-Zr-Ag amorphous bar prepare nano-porous silver
The Cu-Zr-Ag amorphous bar that diameter is 1 ~ 2 mm of Ф is placed in and carries out freely taking off alloy in corrosive liquid, it is more to obtain nanometer
Hole silver metal；
Wherein, corrosive liquid is the HNO of the HF and 0.5 ~ 4 M of 0.05 ~ 0.25 M of concentration3The mixed solution of solution, mixed solution
Volume ratio is HF solution: HNO3Solution=1:1；Etching time is 0.5 ~ 5 h；Corrosion temperature is 25 DEG C of constant temperature；
Second step, cyclic voltammetry prepare the supported porous silver oxide nanosheet composite material of nano-porous silver
Using platinum electrode as auxiliary electrode, Ag/AgCl is as reference electrode, and nanoporous silver metal obtained in the previous step is as work
Make electrode, be combined into three electrode test systems, carries out cyclic voltammetry preparation；By composite material obtained be placed in drying box in
60 ~ 100 DEG C of 1 ~ 2 h of drying, obtain the supported porous silver oxide nanosheet composite material of nano-porous silver；
Wherein, in cyclic voltammetry, voltage window is 0 ~ 0.6V, 100 mV s of sweep speed-1, scan all number 10 ~ 50 weeks；Electricity
Solution liquid is the NaOH solution that concentration is 0.5 ~ 2 M；Operating temperature is 25 DEG C of constant temperature.
2. the application of the supported porous silver oxide nanosheet composite material of nano-porous silver as described in claim 1, it is characterized in that
Bacterium or fungi are removed for killing.
3. the application of the supported porous silver oxide nanosheet composite material of nano-porous silver as claimed in claim 2, it is characterized in that
The bacterium or fungi is one or both of Escherichia coli, staphylococcus aureus.
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