CN106135203A - A kind of Graphene parcel nano zine oxide hetero-junctions anti-biotic material and preparation method thereof - Google Patents

A kind of Graphene parcel nano zine oxide hetero-junctions anti-biotic material and preparation method thereof Download PDF

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Publication number
CN106135203A
CN106135203A CN201610487682.2A CN201610487682A CN106135203A CN 106135203 A CN106135203 A CN 106135203A CN 201610487682 A CN201610487682 A CN 201610487682A CN 106135203 A CN106135203 A CN 106135203A
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China
Prior art keywords
graphene
junctions
nano zine
zine oxide
zinc oxide
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张新娟
邱彩玉
徐梦
徐一梦
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WENZHOU BIOMEDICAL MATERIALS AND ENGINEERING RESEARCH INSTITUTE
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WENZHOU BIOMEDICAL MATERIALS AND ENGINEERING RESEARCH INSTITUTE
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Priority to CN201610487682.2A priority Critical patent/CN106135203A/en
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16—Heavy metals; Compounds thereof

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a kind of Graphene parcel nano zine oxide hetero-junctions anti-biotic material and preparation method thereof, this material is with nano zinc oxide material as matrix, is enclosed with Graphene at surface of nanometer zinc oxide.Its preparation method be Graphene is mixed according to weight ratio 0.0001～1 with the powder of nano zinc oxide material after, add in solvent, form the suspension of mixed-powder；It is then sonicated 10 seconds～30 minutes；By centrifugation and be dried, Graphene parcel nano zine oxide hetero-junctions anti-biotic material is obtained.The present invention fully combines zinc oxide, the antibacterial ability of Graphene itself, and improves its sterilization antibacterial effect by Graphene with nano zine oxide formation hetero-junctions.The anti-biotic material technique of the present invention is simple, is suitable to produce in enormous quantities.

Description

A kind of Graphene parcel nano zine oxide hetero-junctions anti-biotic material and preparation method thereof
Technical field
The present invention relates to a kind of high-performance antibiosis material and preparation method thereof, particularly relate to a kind of Graphene parcel nano oxygen Change zinc hetero-junctions anti-biotic material and preparation method thereof, belong to anti-biotic material preparation field.
Background technology
The most common anti-biotic material has natural antibacterial material, organic anti-bacterial material and inorganic antibacterial material, wherein, nothing Machine anti-biotic material have wide spectrum, efficiently, thermostability, safety, the plurality of advantages such as persistency and environmental friendliness is by widely Pay close attention to.In inorganic antibacterial material, Ag granule is widely used a kind of material, but Ag granule enters human body and is harmful to, and uses Journey should be noted that and avoids enter into human body.Zinc oxide material, because having the performances such as nontoxic, absorption and scatters ultraviolet, is the widest Concerned anti-biotic material.The antibacterial dominant mechanism of zinc oxide is based on its photocatalytic process.Zinc oxide material energy gap is big, inhales Producing the electron hole pair of high energy after receiving the high-energy photon of nature, high energy holes therein has Strong oxdiative ability, passes through Act on the oxygen in air and water form oxide group or directly act on mushroom and reach the antibacterial effect that sterilizes.Nano oxidized Zinc, owing to having higher specific surface area, therefore has more preferable anti-microbial property than regular oxidation zinc.
After grapheme material was stably prepared first in 2004, increasing research finds monatomic The grapheme material of layer has the electricity of excellence, optical property, such as high carrier mobility, high Young's modulus etc..With Time, research finds that nano level Graphene can effectively kill antibacterial, the most following potential for anti-biotic material field.
Summary of the invention
It is an object of the invention to provide a kind of good anti-bacterial effect, to prepare simple Graphene parcel nano zine oxide heterogeneous Knot anti-biotic material and preparation method thereof.
The Graphene parcel nano zine oxide hetero-junctions anti-biotic material of the present invention, this material is to be with nano zinc oxide material Matrix, is enclosed with Graphene at surface of nanometer zinc oxide.
In technique scheme, described nano zinc oxide material is that size is micro-to 1 in 10 nanometers on some direction The zinc oxide material of rice, can be the forms such as nano-particle, nano wire, nano belt, nano flower.
Described Graphene portion envelops or fully wrapped around nano zinc oxide material.
The method preparing above-mentioned Graphene parcel nano zine oxide hetero-junctions anti-biotic material, comprises the steps:
1) Graphene is mixed according to weight ratio=0.0001～1 with the powder of nano zinc oxide material；
2) above-mentioned mixed-powder is added in solvent, form the suspension of mixed-powder；
3) by step 2) suspension that obtains carries out supersound process 10 seconds～30 minutes；
4) by the solution centrifugal after above-mentioned process and be dried, the Graphene parcel antibacterial material of nano zine oxide hetero-junctions is obtained Material.
Wherein, the solvent described in step (2) is deionized water, ethanol, IPA (isopropanol), acetone, NMP (N-methylpyrrole Alkanone), the mixing of one or more in DMF (dimethylformamide).
The anti-biotic material of the present invention is on the basis of zinc oxide and Graphene automatic sterilization function performance, by Graphene and nano oxygen Changing zinc contact and can form Schottky hetero-junctions, owing to zinc oxide is natural in N-shaped conductive characteristic, Graphene is by moisture in air shadow Ringing in p-type electric-conducting characteristic, bi-material combines rear oxidation zinc surface energy band and is bent upwards, and photohole spreads to graphene layer, It is more easy to diffuse to surface, is greatly improved the anti-microbial property of end-product.The present invention fully combines zinc oxide, Graphene itself Antibacterial ability, and the nano zine oxide heterojunction material of the final Graphene parcel obtained can obtain 1+1 > 2 antibacterial effect Really.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the zinc oxide nanowire of Graphene parcel；
Fig. 2 is the staphylococcus anti-microbial property contrast of the zinc oxide nanowire with/without Graphene parcel.
Fig. 3 is the antibacterial characterization result of the Graphene parcel nano zine oxide antibacterial that embodiment 2 prepares.Wherein A For the antibacterial effect after 10mg Graphene parcel nano zine oxide antibacterial effect 2h, B is that 10mg Graphene parcel is nano oxidized Antibacterial effect after zinc antibacterial effect 5h, C is the matched group without antibacterial arranged.
Detailed description of the invention
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1:
1) according to weight ratio Graphene: Graphene and zinc oxide nanowire powder are put in container by zinc oxide=0.0001 Mixing；Zinc-oxide nano linear diameter is about 50nm；
2) add deionized water and obtain Graphene, nano zine oxide mixed-powder suspension；
3) suspension step 2 obtained carries out supersound process 30 minutes；
4) by after above-mentioned process solution centrifugal separate and 120 DEG C of drying obtain Graphene parcel nano zine oxide antibacterial Material.
5) by prepared solid graphene parcel nano zine oxide anti-biotic material, weigh 10mg, join equipped with 1mL 106In the test tube of CFU/ml Escherichia coli bacteria liquid；In test tube, add peptone water 800 μ L, then, test tube is put into air Bath shaken cultivation case is cultivated；After sample 1 cultivates 2 hours, taking out test solution 0.1mL, uniform application is at LB agar plates In, it is inverted in 37 DEG C of constant incubators and cultivates 16～24h, observe and Taking Pictures recording；After sample 2 cultivates 5 hours, take out test solution 0.1mL, uniform application, in LB agar plates, is inverted in 37 DEG C of constant incubators and cultivates 16～24h, note of observing and take pictures Record.Observing display, effect 2h has a small amount of colony growth, and substantially can kill antibacterial after 5h completely.
Embodiment 2:
1) according to weight ratio Graphene: Graphene and nano granular of zinc oxide are put in container by zinc oxide=1；Zinc oxide Nano particle diameter about 100nm；
2) add ethanol and obtain Graphene, nano zine oxide mixed-powder suspension with IPA mixed solvent；
3) suspension step 2 obtained carries out supersound process 10 seconds；
4) by Graphene, nano zine oxide centrifugation and 100 DEG C be dried to obtain Graphene parcel nano zine oxide resist Bacterium material.
5) by prepared solid graphene parcel nano zine oxide anti-biotic material, weigh 10mg, join equipped with 1mL 106In the test tube of CFU/ml staphylococcus aureus liquid；In test tube, add peptone water 800 μ L, then, test tube is put into Air bath shaken cultivation case is cultivated；After sample 1 cultivates 2 hours, taking out test solution 0.1mL, uniform application is trained at LB agar Support in ware, be inverted in 37 DEG C of constant incubators and cultivate 16～24h, observe and Taking Pictures recording；After sample 2 cultivates 5 hours, take out examination Liquid 0.1mL, uniform application, in LB agar plates, is inverted in 37 DEG C of constant incubators and cultivates 16～24h, note of observing and take pictures Record.The antibacterial characterization result of Graphene parcel nano zine oxide antibacterial sees Fig. 2 and 3.From figure 3, it can be seen that effect 2h has A small amount of colony growth, and after 5h, substantially can kill antibacterial completely.
Embodiment 3:
1) according to weight ratio Graphene: Graphene and nano zine oxide are put in container by zinc oxide=0.01；
2) add NMP and obtain Graphene, nano zine oxide mixed-powder suspension；
3) suspension step 2 obtained carries out supersound process 1 minute；
4) suspension is directly dried obtain Graphene parcel nano zine oxide anti-biotic material.
5) by prepared solid graphene parcel nano zine oxide anti-biotic material, weigh 10mg, join equipped with 1mL 106In the test tube of CFU/ml Escherichia coli bacteria liquid；In test tube, add peptone water 800 μ L, then, test tube is put into air Bath shaken cultivation case is cultivated；After sample 1 cultivates 2 hours, taking out test solution 0.1mL, uniform application is at LB agar plates In, it is inverted in 37 DEG C of constant incubators and cultivates 16～24h, observe and Taking Pictures recording；After sample 2 cultivates 5 hours, take out test solution 0.1mL, uniform application, in LB agar plates, is inverted in 37 DEG C of constant incubators and cultivates 16～24h, note of observing and take pictures Record.Effect 2h has a small amount of colony growth, and substantially can kill antibacterial after 5h completely.

Claims (5)

1. a Graphene parcel nano zine oxide hetero-junctions anti-biotic material, it is characterised in that this material is with nano zine oxide Material is matrix, is enclosed with Graphene at surface of nanometer zinc oxide.
Graphene the most according to claim 1 parcel nano zine oxide hetero-junctions anti-biotic material, it is characterised in that described Nano zinc oxide material be on some direction size at the zinc oxide material of 10 nanometers to 1 micron.
Graphene the most according to claim 1 parcel nano zine oxide hetero-junctions anti-biotic material, it is characterised in that Graphene Portion envelops or fully wrapped around nano zinc oxide material.
4. the method for preparation Graphene parcel nano zine oxide hetero-junctions anti-biotic material as described in any one of claim 1-3, It is characterized in that, comprise the steps:
1) Graphene is mixed according to weight ratio=0.0001～1 with the powder of nano zinc oxide material；
2) above-mentioned mixed-powder is added in solvent, form the suspension of mixed-powder；
3) by step 2) suspension that obtains carries out supersound process 10 seconds～30 minutes；
4) by the solution centrifugal after above-mentioned process and be dried, Graphene parcel nano zine oxide hetero-junctions anti-biotic material is obtained.
5. the preparation method of described Graphene parcel nano zine oxide hetero-junctions anti-biotic material as claimed in claim 4, its Being characterised by, described solvent is the mixing of one or more in deionized water, ethanol, IPA, acetone, NMP, DMF.
CN201610487682.2A 2016-06-23 2016-06-23 A kind of Graphene parcel nano zine oxide hetero-junctions anti-biotic material and preparation method thereof Pending CN106135203A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107163654A (en) * 2017-05-26 2017-09-15 中国石油大学(华东) The preparation method and application of Nano-Zinc composite antibacterial material
CN110449169A (en) * 2019-07-04 2019-11-15 中山大学 A kind of semi-metallic Te nano wire/graphene hydrogel composite material and its preparation method and application
CN110787066A (en) * 2019-10-24 2020-02-14 深圳永昌和科技有限公司 Dental 3D printing antibacterial material and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103361044A (en) * 2013-07-16 2013-10-23 东南大学 Preparation method of core-shell structure with zinc oxide quantum dot being enveloped by graphene oxide sheet
CN103449504A (en) * 2013-06-26 2013-12-18 中山大学 Zinc oxide nanodisk/graphene composite material and preparation method thereof
CN103734188A (en) * 2014-01-02 2014-04-23 上海大学 Preparation method and applications of zinc oxide-graphene oxide composite nanomaterial

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103449504A (en) * 2013-06-26 2013-12-18 中山大学 Zinc oxide nanodisk/graphene composite material and preparation method thereof
CN103361044A (en) * 2013-07-16 2013-10-23 东南大学 Preparation method of core-shell structure with zinc oxide quantum dot being enveloped by graphene oxide sheet
CN103734188A (en) * 2014-01-02 2014-04-23 上海大学 Preparation method and applications of zinc oxide-graphene oxide composite nanomaterial

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107163654A (en) * 2017-05-26 2017-09-15 中国石油大学(华东) The preparation method and application of Nano-Zinc composite antibacterial material
CN107163654B (en) * 2017-05-26 2019-08-16 中国石油大学(华东) The preparation method and application of Nano-Zinc composite antibacterial material
CN110449169A (en) * 2019-07-04 2019-11-15 中山大学 A kind of semi-metallic Te nano wire/graphene hydrogel composite material and its preparation method and application
CN110449169B (en) * 2019-07-04 2021-03-12 中山大学 Semi-metal material Te nanowire/graphene hydrogel composite material and preparation method and application thereof
CN110787066A (en) * 2019-10-24 2020-02-14 深圳永昌和科技有限公司 Dental 3D printing antibacterial material and preparation method thereof

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Application publication date: 20161123