CN108147458A - 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 PDFInfo
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- CN108147458A CN108147458A CN201711309241.4A CN201711309241A CN108147458A CN 108147458 A CN108147458 A CN 108147458A CN 201711309241 A CN201711309241 A CN 201711309241A CN 108147458 A CN108147458 A CN 108147458A
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- C01—INORGANIC CHEMISTRY
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- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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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, and first weighing vanadium oxide is 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 more than 1 hour under the conditions of more than 100W by the solution in beaker；Solution after ultrasound with being more than 200 revs/min is stirred 24 hours at ambient temperature, is taken after to be mixed in solution to centrifuge tube after stirring, is more than 5 minutes with the rotating speed centrifugation for being more than 10000 revs/min；The supernatant collected in the solution after 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 uniform step by step, and fluorescence property is strong, stability is high, safety and environmental protection, application environment is friendly, wide market.
Description
Technical field：
The invention belongs to the fields of the preparation of nano material, are related to a kind of method that micro nano structure is prepared with one-step method,
Any surfactant is added without using ultrasound plus stirring as raw material using dimethyl sulfoxide (DMSO) and vanadium oxide 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
Detection and the method for anti-biotic material preparation field.
Background technology：
At present, because its excellent performance causes extensive concern and research, they are wide for barium oxide and its derivative
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 material, 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, have in terms of Photoelectric Detection, Application in Sensing extensively using potentiality.
For barium oxide, the antibacterial action of barium oxide is also paid attention to by people, is a kind of potential excellent
Growth is inhibited bacteria, the material for preventing biofilm formation and biological pollution from preventing, 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.Can be that the application of vanadium oxide opens up new application field such as can successfully preparing：Metal ion and small organic molecule it is glimmering
Light detection etc..It is a kind of potential excellent to inhibit bacteria life in addition, the antibacterial action of barium oxide is also paid attention to by people
Material that is long, preventing biofilm formation from being prevented with biological pollution, it is excellent can to retain vanadium oxide it is desirable to vanadium oxide quantum dot
Anti-microbial property, while a kind of novel nano anti-biotic material can be obtained.
Invention content：
It is an object of the invention to overcome defect of the existing technology, seek 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 using vanadium oxide as presoma, are sheared by ultrasound stripping with stirring
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 these goals, 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 surpass the solution in beaker under the conditions of more than 100W
Sound is more than 1 hour；
S3, the solution after ultrasound in S2 is stirred 24 hours at ambient temperature with being more than 200 revs/min, knot to be mixed
It takes after beam in the solution to centrifuge tube after stirring, is more than 5 minutes with the rotating speed centrifugation for being more 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 it has the advantages that：Only with dimethyl sulfoxide (DMSO) 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 find one-step method for the first time
With regard to vanadium oxide quantum dot can be made, the vanadium oxide that can reliably prepare vanadium oxide quantum dot and prepare has higher ratio 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.
Description of the drawings：
Fig. 1 is the building-up 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 being related to and quantum dot.
Fig. 3 is applied to Fe for vanadium oxide quantum dot by fluorescent quenching and recovery process3+It is examined with the specificity of pyrophosphate
Mapping.
Fig. 4 adds in various concentration Fe for vanadium oxide quantum dot3+With change in fluorescence figure after pyrophosphate with add in concentration with it is glimmering
Variation relation figure between luminous intensity.
Fig. 5 is vanadium oxide quantum dot Bactericidal test figure and Escherichia coli and life after staphylococcus aureus addition quantum dot
Long curve determination figure.
Fig. 6 is the transmission electron microscope shooting figure of bacterial cell after the processing of oxidized vanadium quantum dot.
Specific embodiment：
Below by example with reference, the invention will be further described.
Embodiment 1：
The concrete technology that the one-step method that the present embodiment is related to prepares the method for vanadium oxide quantum dot includes the following steps：
S1, the vanadium oxide of 1g is weighed in 100mL dimethyl sulfoxide (DMSO)s, 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 ambient temperature, is taken after to be mixed
In solution to centrifuge tube after stirring, centrifuged 5 minutes with 12000 revs/min of rotating 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 restores real with pyrophosphate
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, the fluorescence intensity of gained is almost identical with stoste, as shown in Fig. 3 (A), adds
Enter 400 μM of Fe3+Apparent to find that fluorescence intensity declines to a great extent, vanadium oxide quantum dot is to Fe made from explanation3+Detection have pole
Strong specificity and selectivity adds in Fe to probe into3+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), so as 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 equatioies：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, for Fig. 4 (C) to add in various concentration pyrophosphate solution change in fluorescence figure, Fig. 4 (D) shows its fluorescence
Linear relationship between intensity (Y) and pyrophosphate concentration (X) is：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), first, vanadium oxide quantum dot is primarily determined 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 tablet
Three susceptibility filter papers of even placement, 200 μ L 0.01g/mL vanadium oxides quantum dots, the 200 pure dimethyl of μ L are added dropwise in filter paper respectively
Sulfoxide and 200 μ L distilled waters, then 37 degrees Celsius of constant temperature incubations be only added dropwise after 10 hours quantum dot filter paper have it is antibacterial
Circle generates, and the growth curve of Escherichia coli and staphylococcus aureus is then measured by absorbance method and further confirms vanadium oxide
The anti-microbial property of quantum dot, as shown in Fig. 5 (C) and 5 (D), the bacterium solution of the 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 bacteria growth, there is good restraining and sterilizing bacteria performance, can be used in anti-biotic material preparation.
Claims (5)
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, the beaker that solution prepared in S1 is fitted into mL in 150, by the solution in beaker, ultrasound is big under the conditions of more than 100W
In 1 hour；
S3, the solution after ultrasound in S2 is stirred 24 hours at ambient temperature with being more than 200 revs/min, after to be mixed
It takes in the solution to centrifuge tube after stirring, is more than 5 minutes with the rotating speed centrifugation for being more than 10000 revs/min；
S4, the supernatant collected in the solution after being centrifuged in S3 obtain vanadium oxide quantum dot solution.
2. the method that one-step method according to claim 1 prepares vanadium oxide quantum dot, it is characterised in that prepared by this method
Vanadium oxide quantum dot has specificity and selectivity, and fluorescent quenching, prepared molybdenum oxide can be specifically caused by ferric iron
Quantum dot can be applied to the specificity Sensitive Detection of ferric iron and pyrophosphate anions content.
3. the method that one-step method according to claim 2 prepares vanadium oxide quantum dot, it is characterised in that prepared by this method
With ferric concentration there are linear relationship, linear relationship is the fluorescence intensity of vanadium oxide quantum dot：Y=0.0287+
0.0038X。
4. the method that one-step method according to claim 2 prepares vanadium oxide quantum dot, it is characterised in that prepared by this method
With the concentration of pyrophosphate anion there are linear relationship, linear relationship is the fluorescence intensity of vanadium oxide quantum dot：Y=
3317.55+86.68X。
5. the method that a kind of one-step method according to claim 1 prepares vanadium oxide quantum dot, it is characterised in that party's legal system
Standby vanadium oxide quantum dot bacteriostasis property is good, can be used as anti-biotic material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110316757A (en) * | 2019-07-24 | 2019-10-11 | 青岛大学 | A kind of vanadium oxide preparation method and applications |
Citations (1)
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
Non-Patent Citations (2)
| Title |
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| FANGXU JI ET AL.: "2D-MoO3 nanosheets for superior gas sensors", 《NANOSCALE》 * |
| 纪方旭: "液相剥离制备二维三氧化钼及其气敏性能的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110316757A (en) * | 2019-07-24 | 2019-10-11 | 青岛大学 | A kind of vanadium oxide preparation method and applications |
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