CN114392741A - Vacancy-rich silver-loaded tungsten oxide nanowire for improving visible light and near infrared light dynamic bacteriostasis and preparation and application thereof - Google Patents
Vacancy-rich silver-loaded tungsten oxide nanowire for improving visible light and near infrared light dynamic bacteriostasis and preparation and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title abstract description 11
- 229910052709 silver Inorganic materials 0.000 title abstract description 9
- 239000004332 silver Substances 0.000 title abstract description 8
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 title description 2
- 239000002070 nanowire Substances 0.000 claims abstract description 65
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 229940095731 candida albicans Drugs 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 18
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- 238000001291 vacuum drying Methods 0.000 claims description 10
- 230000007547 defect Effects 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
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- YOUIDGQAIILFBW-UHFFFAOYSA-J tetrachlorotungsten Chemical compound Cl[W](Cl)(Cl)Cl YOUIDGQAIILFBW-UHFFFAOYSA-J 0.000 claims description 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 2
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/683—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten
- B01J23/687—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten with tungsten
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- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
- A61L2/08—Radiation
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Abstract
The invention belongs to the field of photocatalytic materials, and relates to a small-size silver nanoparticle modified W with oxygen defects18O49A preparation method of the nano-wire and application thereof in photodynamic antibiosis. Discloses an influence mechanism of the construction of a one-dimensional material interface on the photodynamic inhibition of the activity of the candida albicans. Research results show that the one-dimensional structure is beneficial to the directional transmission of carriers so as to promote the material to generate active oxygen species with stronger toxicity. Further, W18O49The oxygen vacancy in the film can promote the separation of photogenerated carriers and enhance W18O49Photocatalytic activity of (1). On the other hand, the plasmon resonance (LSPR) effect of Ag nanoparticles can not only enhance W18O49Is photo-responsive, induces photo-generated carriersThe rapid separation can improve the generation amount of photoinduction OH, and is beneficial to photodynamic antibiosis.
Description
Technical Field
The invention belongs to the field of synthesis of photocatalytic nano materials, and relates to W modified by Ag nano particles18O49Nano meterPreparation and application of the thread.
Background
Bacterial infections represent a health threat to humans worldwide, and the excessive use of traditional antibiotics leads to bacterial resistance, thereby further threatening human health. Antibiotic-free strategies are therefore highly desirable. Photodynamic antibacterial therapy is a nonspecific therapeutic means which is not easy to cause bacterial drug resistance, so the design of antibacterial nano materials has been remarkably developed in recent years, and more nano materials are designed for photodynamic therapy of bacterial infection, such as TiO2,ZnO,WO3ZrO, etc., are mainly studied in an effort to improve the absorption of visible light and the antibacterial property thereof. However, the main active species of photodynamic anti-bacterial is Reactive Oxygen Species (ROS), which mainly has O2 -、H2O2OH and1O2but they exhibit different kinetics and activity levels. O is2 -And H2O2Is less toxic than OH and1O2large because the former is much less active and can be consumed by endogenous antioxidants (including enzymatic and non-enzymatic) induced by oxidative stress. In contrast, no enzyme can consume OH and1O2this makes them extremely toxic and acutely fatal.
Disclosure of Invention
The purpose of the invention is as follows: aims to solve the problems of low yield of active oxygen and low toxicity of the generated active oxygen in the prior art.
The technical scheme is as follows: w18O49As a semiconductor material with oxygen defects and visible light absorption, the material is widely applied to the fields of near-infrared shielding films, gas sensors, photocatalysis, biotherapy and the like. W18O49Has a forbidden band width of 2.33eV, W18O49Due to its appropriate valence band position (EVB ═ 3.35eV), H can be converted to2O is oxidized into OH in one step, and the specific reaction process is as follows: h2O+h+→·OH+H+(E02.38eV), the light absorption range of which is from the visible region to the near infrared region, and the photogenerated electrons under the illumination conditionFaster hole recombination and lower photocatalytic activity, and therefore direct use of W18O49As a photocatalytic material, it is difficult to efficiently utilize sunlight. Numerous methods have been used to modify W18O49And the absorption and utilization of visible light are improved, wherein the light absorption and photocatalysis performance are greatly improved based on the deposition of noble metal nano particles on the surface of the nano wire. The introduction of the noble metal nanoparticles induces the photocatalyst to generate more defects, the photocatalyst with the defects is favorable for adsorbing and activating more target molecules, and can effectively promote the separation of electrons and holes and reduce the energy barrier of interface charge transfer. The LSPR effect of the noble metal promotes the absorption of the material to visible light and near infrared light, and the generated hot electrons are injected into a semiconductor, so that the photocatalytic activity of the material is obviously improved. Meanwhile, the one-dimensional structure has abundant active sites and directional electron transmission, so that the photocatalytic performance of the semiconductor can be further improved.
In view of the above, the present invention provides a W modified with Ag nanoparticles having oxygen deficiency18O49A preparation method of the nano-wire and application thereof in photodynamic anti-candida albicans.
A preparation method of a nanoparticle modified W18O49/Ag nanowire comprises the following steps:
(1) completely dissolving 0.01-0.07g of tungsten chloride in 50-70ml of n-propanol (AR, analytical purity), transferring to a 50-100ml reaction kettle, and placing into a 100-200 ℃ oven for reaction for 12-24 h; after the reaction is finished, cooling to room temperature, pouring out the product in the kettle, cleaning the obtained sample, and putting the sample into a vacuum drying oven at 60-80 ℃ for vacuum drying for 6-12h to obtain uniform W18O49The nanowires are about 10-50 mg;
(2) dispersing the sample obtained in the step (1) in 10-20ml of ethanol (AR, analytically pure), adding 2-8ml of 1-10 ml of MAGAGNO 3 solution, stirring at normal temperature for 1-3h, and carrying out oil bath reaction for 12-24h, wherein the reaction temperature is 50-70 ℃; after the reaction is finished, cleaning the sample, putting the sample into a vacuum drying oven for vacuum drying to obtain W18O49Ag nano wire.
Has the advantages that: 1. the prepared silver nano-particles prepared by the inventionParticle modified W18O49The maximum absorption peak of the/Ag nanowire is in a visible light region and a near infrared light region. As shown in fig. 6.
2. The silver nanoparticle modified W provided by the invention18O49Ag nanowires vs. original W18O49The absorption of the nano-wire to visible light, the photocatalysis performance and the like are obviously improved. As shown in fig. 6 and 11.
3. The invention develops a simple and controllable small-size silver nanoparticle modified defect-rich W by using a solvothermal method18O49A method of nanowires. Ag nanoparticles directly deposited on W18O49The surface of the nanowire. As shown in fig. 3. The LSPR effect of Ag nanoparticles can enhance W18O49The photoresponsiveness of (2) is shown in FIG. 9. While deposition of Ag nanoparticles makes W18O49With more oxygen vacancies, Ag nanoparticles and W18O49The contact interface facilitates rapid separation and transfer of photo-generated electrons, which helps to increase the photocatalytic activity of the material, as shown in fig. 5 and 8.
4. The invention provides a W modified by simple and controllable synthesized silver nano particles18O49Ag nano wire. Small size Ag nanoparticles in W18O49Uniform growth of nano wire surface and inducing W18O49More oxygen vacancies are generated, so that the adsorption and activation of target molecules are facilitated, and meanwhile, the Ag nanoparticles have the LSPR effect, so that the absorption of visible light and near infrared light by the material can be improved, hot electrons can be generated to be injected into a semiconductor, and the transfer and transfer of photo-generated electrons are promoted. The defect-rich W modified by the controllable synthesized small-size silver nano particles18O49The Ag nanowire has excellent light absorption, more active sites and faster electron transfer, thereby remarkably improving W18O49Ag is the photocatalytic activity.
Drawings
FIG. 1 is W18O49SEM pictures of nanowires.
FIG. 2 is W18O49SEM image of/Ag nanowireAnd (3) slicing.
FIG. 3 is W18O49TEM pictures of/Ag nanowires.
FIG. 4 is W18O49Nanowire and W18O49X-ray diffraction pattern of/Ag nano-wire.
FIG. 5 is W18O49Nanowire and W18O49X-ray photoelectron energy spectrum of/Ag nano wire.
FIG. 6 is W18O49Nanowire and W18O49Solid ultraviolet-visible spectrum of/Ag nano-wire.
FIG. 7 is W18O49Nanowire and W18O49Schottky spectrum of/Ag nano wire.
FIG. 8 is W18O49Nanowire and W18O49Fluorescence spectrum of/Ag nano-wire.
FIG. 9 is W18O49Nanowire and W18O49The current-time spectrogram of the/Ag nanowire is under the same light intensity.
FIG. 10 is W18O49Nanowire and W18O49Electrochemical impedance spectrogram of/Ag nano wire.
FIG. 11 is W18O49Nanowire and W18O49TMB ultraviolet visible absorption spectrum of/Ag nano-wire.
FIG. 12 is W18O49The bacteriostatic concentration graph of the Ag nanowire.
FIG. 13 is W18O49Nanowire and W18O49Bacterial growth profile after Ag nanowire treatment.
Detailed Description
The following further illustrates the related aspects of the invention in connection with specific examples. It should be noted that these examples are only for illustrating the present invention and are not to be construed as limiting the scope of the present invention, and that various changes or modifications of the present invention can be made by those skilled in the art after reading the contents of the present invention, which also fall within the scope of the claims appended to the present application.
Examples
Weighing tungsten chloride in n-propanol (analytically pure), stirring and dissolving, transferring to a reaction kettle, putting into an oven, setting the temperature at 100 ℃ and 250 ℃, and reacting for a period of time. After the reaction is finished, cooling the reaction kettle to room temperature, pouring out a product in the kettle, using methanol (analytically pure) as a washing liquid, centrifugally washing, and drying the washed product in a vacuum drying oven to obtain W18O49A nanowire. Then weighing W18O49Ultrasonically dispersing in ethanol (analytically pure) solution to prepare 10mmol L-1AgNO of3Adding W into the ethanol solution18O49Stirring in ethanol solution at normal temperature for a period of time, carrying out oil bath reaction for 24h, washing the product with ethanol as washing liquid for 3 times, and drying in a vacuum drying oven to obtain W18O49Ag nano wire. The specific experimental data for some of the examples are as follows:
as shown in FIG. 1, is W prepared18O49SEM pictures of nanowires. Illustrating the synthesized W18O49The nano wire is slender and regular and has good dispersibility.
As shown in FIG. 2, is W18O49SEM pictures of/Ag nanowires. Visible W18O49the/Ag nanowire morphology did not change significantly and was difficult to observe by SEM due to the small silver particles deposited.
As shown in FIG. 3, is W18O49TEM pictures of/Ag nanowires. It can be seen that Ag particles are uniformly deposited on W18O49The surface of the nanowire.
As shown in FIG. 4, is W18O49Nanowire and W18O49X-ray diffraction pattern of/Ag nano-wire. Can find W18O49And W18O49The X-ray diffraction peak of Ag can be well matched with monoclinic W18O49(JCPDS No.71-2450) phaseAnd (7) corresponding.
As shown in FIG. 5, is W18O49Nanowire and W18O49X-ray photoelectron energy spectrum of/Ag nano wire. Can find W18O49W, O elements, W, are present in the material18O49W, O and Ag element exist in the/Ag composite material, and the successful deposition of Ag nanoparticles on W is proved18O49A surface. As can be seen from the figure, W18O49And W18O49W is present in all of the Ag5+And W6+Two valence states. Notably, W18O49After depositing Ag nanoparticles on the surface, W5+Signal enhancement of characteristic peaks, W6+The signal of the characteristic peak is weakened, and the peak position moves to a low field, which shows that the concentration of oxygen vacancy is increased after the Ag nano particles are deposited.
As shown in FIG. 6, is W18O49Nanowire and W18O49Solid ultraviolet-visible spectrum of/Ag nano-wire. Indicates W alone18O49Phase comparison W18O49The light absorption of Ag to visible light and near infrared light is obviously enhanced.
As shown in FIG. 7, is W18O49Nanowire and W18O49Schottky spectrum of/Ag nano wire. Description of W18O49Ag and W18O49In contrast, it has a higher concentration of photogenerated carriers.
As shown in FIG. 8, is W18O49Nanowire and W18O49Fluorescence spectrum of/Ag nano-wire. The separation capability of photoproduction electrons and holes is obviously improved after the Ag nano particles are deposited.
As shown in FIG. 9, is W18O49Nanowire and W18O49The current-time spectrogram of the/Ag nanowire is under the same light intensity. The Ag nano particles are more strong in photoresponse after being deposited.
As shown in FIG. 10, is W18O49Nanowire and W18O49Electrochemical impedance spectrogram of/Ag nano wire. Description of W18O49Ag and W18O49CompareThe electron transfer resistance is lower.
As shown in FIG. 11, is W18O49Nanowire and W18O49TMB ultraviolet visible absorption spectrum of/Ag nano-wire. W18O49Ag and W18O49Compared with the prior art, the catalyst has stronger oxidation characteristic peak, which shows that W is18O49Ag can generate active oxygen very well.
As shown in FIG. 12, is W18O49The bacteriostatic concentration graph of the Ag nanowire. Description of W18O49The antibacterial concentration of Ag is low.
As shown in FIG. 13, is W18O49Nanowire and W18O49Bacterial growth profile after Ag nanowire treatment. Description of Ag-W18O49And W18O49Compared with the prior art, the antibacterial agent has better antibacterial effect.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (3)
1. Vacancy-rich W for improving dynamic bacteriostasis of visible light and near infrared light18O49Ag nano wire, which is characterized in that: w with silver nanoparticles loaded on surface18O49The nanowires have oxygen defects.
2. The vacancy-rich W of claim 1 for improving visible and near infrared photodynamic inhibition18O49The preparation method of the Ag nanowire is characterized by comprising the following specific steps:
(1) completely dissolving 0.01-0.07g of tungsten chloride in 50-70ml of n-propanol, transferring the solution into a 50-100ml reaction kettle, and putting the reaction kettle into a 100-200 ℃ drying oven for reaction for 12-24 h; after the reaction is finished, cooling to room temperature, pouring out the product in the kettle, cleaning the obtained sample, and putting the sample into a vacuum drying oven at 60-80 ℃ for vacuum drying for 6-12h to obtain uniform W18O49The nano wire is about10-50mg;
(2) Dispersing the sample obtained in the step (1) in 10-20ml of ethanol solution, and adding 1-10mM AGNO3Stirring the solution 2-6ml at normal temperature for 1-3h, and carrying out oil bath reaction for 12-24h at the reaction temperature of 50-70 ℃; after the reaction is finished, cleaning the sample, putting the sample into a vacuum drying oven for vacuum drying to obtain W18O49Ag nano wire.
3. W according to claim 118O49The Ag nanowire is applied to photodynamic anti-Candida albicans.
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