CN108147458B - A kind of method that one-step method prepares vanadium oxide quantum dot - Google Patents

A kind of method that one-step method prepares vanadium oxide quantum dot Download PDF

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CN108147458B
CN108147458B CN201711309241.4A CN201711309241A CN108147458B CN 108147458 B CN108147458 B CN 108147458B CN 201711309241 A CN201711309241 A CN 201711309241A CN 108147458 B CN108147458 B CN 108147458B
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vanadium oxide
quantum dot
oxide quantum
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CN108147458A (en
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许元红
黄蕾
牛玉生
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Qingdao University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/02—Oxides
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area

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Abstract

The invention belongs to the fields of the preparation of nano material, are related to a kind of method that one-step method prepares vanadium oxide quantum dot, first weigh vanadium oxide and be dissolved in dimethyl sulphoxide solution, and stirring and dissolving obtains nattier blue clear solution；Solution is fitted into the beaker of mL in 150 again, ultrasound is greater than 1 hour under the conditions of being greater than 100W by the solution in beaker；Solution after ultrasound is stirred 24 hours with being greater than 200 revs/min at room temperature, the solution after stirring is taken after to be mixed is greater than 5 minutes into centrifuge tube with the revolving speed centrifugation greater than 10000 revs/min；The supernatant in solution after collecting centrifugation obtains vanadium oxide quantum dot solution, compared with prior art, the present invention preparation process is simple, preparation efficiency is high, and products obtained therefrom has size substep uniform, and fluorescence property is strong, stability is high, safety and environmental protection, application environment is friendly, wide market.

Description

A kind of method that one-step method prepares vanadium oxide quantum dot
Technical field:
The invention belongs to the fields of the preparation of nano material, are related to a kind of method for preparing micro nano structure with one-step method, Any surfactant is added without using ultrasound plus stirring using dimethyl sulfoxide and vanadium oxide as raw material more particularly to one kind Or the method that the method for template prepares quantum dot, while vanadium oxide quantum dot is applied to metal ion, small organic molecule The method of detection and anti-biotic material preparation field.
Background technique:
Currently, barium oxide and its derivative are because its excellent performance is attracted wide public concern and studied, they are wide It is general to apply in various industrial processes, the oxidation including sulfur dioxide, hydrocarbon, nitric oxide production reduction etc., because Barium oxide and its derivative flexible structure and physicochemical properties and other many interested materials of application field, such as High power lithium battery, environmental renovation catalysis, hydrogen storage, organic synthesis, hot fluid and sensor etc..On the other hand, the performance of material is normal It is often relied on the factors such as its aggregated structure, crystalline structure, particle size.When certain material is cut into 100 nanometers, especially 10 nanometers once when, due to quantum confined effect and edge effect, it is generally possible to obtain quanta point materials, with its bulk material phase Than in addition to the inherent feature for retaining block presoma, quantum dot will have large specific surface area, novel fluorescence property and good Water solubility, stability the advantages that, in terms of Photoelectric Detection, Application in Sensing have be widely applied potentiality.
For barium oxide, the antibacterial action of barium oxide is also paid attention to by people, is a kind of potential excellent Inhibit bacterial growth, the material for preventing biofilm formation and biological pollution from preventing and treating, it is excellent anti-that vanadium oxide quantum dot remains its Bacterium performance, be expected to applied to nano anti-biotic material to prepare current vanadium oxide nanometer sheet, nanometer rods preparation method more, it is such as molten Glue-gel method, hydro-thermal and solvent-thermal method, vapour deposition process, template etc., but the preparation of vanadium oxide quantum dot rarely has document report Road.As can successfully prepare, new application field can be opened up such as the application of vanadium oxide: metal ion and small organic molecule it is glimmering Light detection etc..In addition, the antibacterial action of barium oxide is also paid attention to by people, it is that a kind of potential excellent inhibition bacterium is raw Material that is long, preventing biofilm formation and biological pollution from preventing and treating, it is desirable to vanadium oxide quantum dot, can to retain vanadium oxide excellent Anti-microbial property, while a kind of novel nano anti-biotic material can be obtained.
Summary of the invention:
It is an object of the invention to overcome defect of the existing technology, seeks design and a kind of one-step method preparation oxidation is provided The method of vanadium quantum dot, the method stirred using ultrasonic wave added are sheared by ultrasound removing with stirring using vanadium oxide as presoma Power formed vanadium oxide quantum dot, and prepare vanadium oxide quantum dot can be used as a kind of good fluorescence probe, metal from Son has broad application prospects with small organic molecule context of detection；And the anti-microbial property of the vanadium oxide quantum dot prepared is good It is good.
To achieve the goals above, one-step method of the present invention prepares the concrete technology packet of the method for vanadium oxide quantum dot Include following steps:
S1, it weighs vanadium oxide and is dissolved in dimethyl sulphoxide solution, stirring and dissolving obtains nattier blue clear solution；
S2, the beaker that solution prepared in S1 is fitted into mL in 150 are super under the conditions of being greater than 100W by the solution in beaker Sound is greater than 1 hour；
S3, the solution after ultrasound in S2 is stirred 24 hours with being greater than 200 revs/min at room temperature, knot to be mixed Solution after taking stirring after beam is greater than 5 minutes into centrifuge tube with the revolving speed centrifugation greater than 10000 revs/min；
S4, the supernatant collected in the solution after being centrifuged in S3 obtain vanadium oxide quantum dot solution.
Compared with prior art, the present invention having the following beneficial effects: only with dimethyl sulfoxide as solvent, without adding Enter the programs such as template or high-temperature heating, be a kind of preparation method of completely new vanadium oxide quantum dot, and finds one-step method for the first time Vanadium oxide quantum dot can be made, can reliably prepare vanadium oxide quantum dot and the vanadium oxide prepared with higher compares table Area, this method preparation process is simple, and preparation efficiency is high, and products obtained therefrom has size substep uniform, and fluorescence property is strong, steady Qualitative height, safety and environmental protection, application environment is friendly, wide market.
Detailed description of the invention:
Fig. 1 is the synthesis process and application schematic diagram of vanadium oxide quantum dot of the present invention.
Fig. 2 (A) is the transmission electron microscope figure of the vanadium oxide quantum dot of preparation of the present invention；Fig. 2 (B) is this hair The particle size distribution figure of the bright high-resolution-ration transmission electric-lens figure and quantum dot being related to.
Fig. 3 is that vanadium oxide quantum dot passes through fluorescent quenching and recovery process is applied to Fe3+It is examined with the specificity of pyrophosphate Mapping.
Fig. 4 is that various concentration Fe is added in vanadium oxide quantum dot3+With change in fluorescence figure after pyrophosphate be added concentration with it is glimmering Variation relation figure between luminous intensity.
Fig. 5 is that life after quantum dot is added in vanadium oxide quantum dot Bactericidal test figure and Escherichia coli and staphylococcus aureus Long curve determination figure.
Fig. 6 is the transmission electron microscope shooting figure of the bacterial cell after the processing of vanadium oxide quantum dot.
Specific embodiment:
Below by example with reference, the invention will be further described.
Embodiment 1:
The one-step method that the present embodiment is related to prepare the concrete technology of the method for vanadium oxide quantum dot the following steps are included:
S1, the vanadium oxide of 1g is weighed in 100mL dimethyl sulfoxide, stirring and dissolving obtains nattier blue clear solution；
S2, solution prepared in S1 is fitted into the beaker of 150mL, by the solution in beaker ultrasonic 3 under the conditions of 300W Hour；
S3, the solution after ultrasound in S2 is stirred 24 hours for 250 revs/min at room temperature, is taken after to be mixed Solution after stirring is centrifuged 5 minutes into centrifuge tube with 12000 revs/min of revolving speed；
S4, the supernatant collected in the solution after being centrifuged in S3 obtain vanadium oxide quantum dot solution.
Embodiment 2:
Vanadium oxide quantum dot prepared by the present embodiment 1 is subjected to ferric ion fluorescent quenching and pyrophosphate restores real It tests, 400 μM of Ni is separately added into vanadium oxide quantum dot solution2+,Al3+,Co2+,Cu2+,Mg2+,Mn2+,K+,Zn2+, and Its fluorescence intensity is surveyed under the excitation wavelength of 360nm, resulting fluorescence intensity is almost identical with stoste, as shown in Fig. 3 (A), adds Enter 400 μM of Fe3+Obvious discovery fluorescence intensity declines to a great extent, and illustrates vanadium oxide quantum dot obtained to Fe3+Detection have pole Fe is added in order to probe into strong specificity and selectivity3+Concentration (0-540 μM) and fluorescence intensity linear relationship, will be a series of The Fe of concentration gradient3+Solution is added in the vanadium oxide quantum dot solution of 3.0mL, Fe3+Solution concentration is respectively 0,30 μM, 60 μ M、90μM、120μM、150μM、180μM、210μM、240μM、270μM、300μM、330μM、360μM、390μM、420μM、450μ M, 480 μM, 510 μM and 540 μM obtain a series of different fluorescence intensities, such as Fig. 4 (A), to obtain Fe3+To vanadium oxide amount The influence of the fluorescence intensity of son point, linear relationship such as Fig. 4 (B), according to Stern-Volmer equation: I/I0=1+ [M] KSV, enable Y =[M] KSV=(I-I0)/I0, X Fe3+Concentration, then Y=0.0287+0.0038X；Similarly, the present embodiment SO4 2–,F–,Cl–, NO3 –,PO4 3–Fluorescence has been carried out with anion such as PPi and has restored experiment, and as shown in Fig. 3 (B), only pyrophosphate anion has relatively strong Fluorescence restitution, Fig. 4 (C) is that various concentration pyrophosphate solution change in fluorescence figure is added, and Fig. 4 (D) shows its fluorescence Linear relationship between intensity (Y) and pyrophosphate concentration (X) are as follows: Y=3317.55+86.68X.
Embodiment 3:
Vanadium oxide quantum dot prepared by this example 1 is subjected to anti-microbial property test, test bacterium is Escherichia coli (gram Negative bacterium) and staphylococcus aureus (gram-positive bacteria), firstly, primarily determining vanadium oxide quantum dot by Bactericidal test Anti-microbial property, it is as shown in Fig. 5 (A) and 5 (B), two kinds of bacterium are equal in planar surface after superclean bench is respectively coated plate 200 μ L 0.01g/mL vanadium oxide quantum dots, the 200 pure dimethyl of μ L are added dropwise in filter paper in three susceptibility filter papers of even placement respectively Sulfoxide and 200 μ L distilled waters, be then only added dropwise after constant temperature incubation 10 hours at 37 degrees Celsius quantum dot filter paper have it is antibacterial Circle generates, and then further confirms vanadium oxide by the growth curve that absorbance method measures Escherichia coli and staphylococcus aureus The anti-microbial property of quantum dot, as shown in Fig. 5 (C) and 5 (D), the bacterium solution of addition vanadium oxide quantum dot extinction compared with compareing bacterium solution Degree is substantially reduced, and bacterial growth amount is decreased obviously, and is handled finally by transmission electron microscope (TEM) directly observation through quantum dot Ne ar variation afterwards, such as Fig. 6, it can be seen that treated that ne ar changes through quantum dot, permeability of cell membrane Change, part cell ruptures, content outflow, by above-mentioned experimental result it can be seen that vanadium oxide quantum dot can effectively be broken Bad bacterium cell structure inhibits bacterial growth, there is good restraining and sterilizing bacteria performance, can be used in anti-biotic material preparation.

Claims (1)

1. a kind of method that one-step method prepares vanadium oxide quantum dot, it is characterised in that the concrete technology of the method for this method include with Lower step:
S1, it weighs vanadium oxide and is dissolved in dimethyl sulphoxide solution, stirring and dissolving obtains nattier blue clear solution；
S2, solution prepared in S1 is fitted into the beaker of 150mL, by the solution in beaker, ultrasound is big under the conditions of being greater than 100W In 1 hour；
S3, the solution after ultrasound in S2 is stirred 24 hours with being greater than 200 revs/min at room temperature, after to be mixed Solution after taking stirring is greater than 5 minutes into centrifuge tube with the revolving speed centrifugation greater than 10000 revs/min；
S4, the supernatant collected in the solution after being centrifuged in S3 obtain vanadium oxide quantum dot solution；
The vanadium oxide quantum dot of above method preparation has specificity and selectivity, can specifically cause fluorescence by ferric iron It is quenched, prepared molybdenum oxide quantum dot can be applied to the quick inspection of specificity personality of ferric iron and pyrophosphate anions content It surveys, and the vanadium oxide quantum dot bacteriostasis property prepared is good, can be used as anti-biotic material.
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Citations (1)

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CN103073942A (en) * 2012-01-19 2013-05-01 中国科学院上海硅酸盐研究所 Vanadium dioxide composite powder and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN103073942A (en) * 2012-01-19 2013-05-01 中国科学院上海硅酸盐研究所 Vanadium dioxide composite powder and preparation method thereof

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* Cited by examiner, † Cited by third party
Title
2D-MoO3 nanosheets for superior gas sensors;Fangxu Ji et al.;《Nanoscale》;20160316;第8卷;第8696-8703页 *
液相剥离制备二维三氧化钼及其气敏性能的研究;纪方旭;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20170515(第5期);第20,34,37页 *

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