CN110065968B - Tetragonal phase (NH) with photo-thermal characteristic4)2V3O8Preparation method and application of nanosheet - Google Patents
Tetragonal phase (NH) with photo-thermal characteristic4)2V3O8Preparation method and application of nanosheet Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 39
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 26
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 26
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 25
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 13
- 229910003206 NH4VO3 Inorganic materials 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 241000282414 Homo sapiens Species 0.000 abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000004321 preservation Methods 0.000 abstract description 3
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical group CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 17
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 17
- 239000000463 material Substances 0.000 description 13
- 239000013078 crystal Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 206010028980 Neoplasm Diseases 0.000 description 6
- 201000011510 cancer Diseases 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 5
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 4
- 238000011534 incubation Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000007626 photothermal therapy Methods 0.000 description 4
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- -1 class of anionic metal oxide Chemical class 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000002560 therapeutic procedure Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005880 cancer cell killing Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010351 charge transfer process Methods 0.000 description 1
- 238000002512 chemotherapy Methods 0.000 description 1
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- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 230000003902 lesion Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000036210 malignancy Effects 0.000 description 1
- 230000003211 malignant effect Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 238000001959 radiotherapy Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0052—Thermotherapy; Hyperthermia; Magnetic induction; Induction heating therapy
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Life Sciences & Earth Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a tetragonal phase (NH) with photo-thermal characteristics4)2V3O8The preparation method and the application of the nano-sheet are characterized in that deionized water is used as a solvent, and the ratio of the added substances is 1: (4-8) obtaining a mixed solution B by using a vanadium source and a reducing agent, reacting the mixed solution B in a normal atmospheric environment, and growing a pure tetragonal phase (NH) through three stages of heating, heat preservation and cooling4)2V3O8Nanosheets. The invention avoids high temperature and time consumption, does not need complex equipment, has simple, convenient, high-efficiency and good repeatability, does not relate to harmful reagents, is safe to human bodies and is harmless.
Description
Technical Field
The invention belongs to the technical field of preparation and application of nano photothermal materials, and particularly relates to a tetragonal phase (NH) with excellent photothermal characteristics4)2V3O8A preparation method of a nano sheet and application thereof.
Background
Today, the rapid development of human economy, health issues are the most interesting topics for human beings. Today, there are various intractable malignancies, the most serious of which is cancer. Cancer, i.e., malignant tumor, is a progressive malignant disease, gradually erodes normal cells to cause local lesions, and then spreads to the whole body, seriously threatening the human life and health. The currently common cancer clinical treatment methods include surgical treatment, chemotherapy, radiotherapy and other therapies. However, these therapies have certain limitations, are not easy to remove all cancer cells, and have the disadvantages of great side effects, high risk and undesirable effects. Therefore, photothermal therapy is the focus of research. In recent years, photothermal therapy has become a method of treating cancer, which has attracted much attention because of its low side effects and high cancer cell killing rate. The preparation and properties of the nanomaterials used in the treatment are the determining factors that determine the effect of photothermal therapy.
At present, a plurality of common photothermal materials exist. Inorganic non-metallic materials such as carbon-based nanomaterials, graphene, and the like; noble metal materials such as gold, silver, palladium, and the like; organic compounds such as polypyrrole, polyaniline, and the like. There are many reports on these materials, but they still have inevitable drawbacks. Noble metal nano materials such as Au, Pd and the like are generally expensive, and the thermal stability is poor; the preparation processes of carbon-based nano materials, graphene and the like are complex, the preparation cost is high, and the conditions are harsh; organic compound photo-thermal materials may be photo-degraded under light irradiation, and have a problem in stability. Therefore, the nano photothermal material with excellent preparation performance, stable structure, low cost and simple synthesis method is very important. Polyoxometallate Oxides (POMs) are a class of anionic metal oxide clusters consisting of d-block transition metals (W, Mo, V), which are a class of good electronic energy storage materials. They can undergo latent photo-or electron-induced charge transfer processes without changing the structure, which makes them interesting materials in electrochemistry and photochemistry. The vanadate material has good optical, electrochemical, magnetic and catalytic properties, so that the vanadate material has good application prospects in the fields of optics, lithium batteries, chemical catalysis and the like, and special nanostructures optimize the properties of the vanadate material and even obtain more novel properties, so that the nanometer vanadate material is a hotspot in the field of new material research in recent years. And (NH)4)2V3O8Because of the special two-dimensional layered structure and the good near infrared absorption characteristic, the optical near infrared absorption material has good prospect in the aspect of optics.
To prepare (NH)4)2V3O8There have been many studies on the approach of (c). Due to two valence states of vanadium (V)5+And V4+) Coexisting in the compound, and thus it is substantially difficult to make (NH)4)2V3O8Synthesized by a conventional synthetic route (low temperature, atmosphere and common precursor). NH at 2500 deg.C under vacuum according to previous report4VO3And V2O3Performing solid state reaction, and electrochemically reducing NH with platinum electrode4VO3Or reduction of V in solutions of ammonium salts without tin powder2O5Can prepare (NH)4)2V3O8The method has harsh reaction conditions and complex process; with ethanol-H in the presence of a poly (ethylene oxide) -poly (propylene oxide) -poly (ethylene oxide) triblock copolymer2Solution of O in NH4VO3Hydrothermally reducing to synthesize (NH)4)2V3O8And (3) single crystal. Adding NH to pyrrolidone4VO3Adding a certain amount of H into the obtained solution2C2O4.2H2The hydrothermal reaction of O can obtain flake (NH)4)2V3O8And (3) single crystal. However, all these reported methods are rather complicated, difficult to control, not easy to operate and time consuming. Thus, to (NH)4)2V3O8The preparation process is interesting.
Disclosure of Invention
The present invention is directed to provide a tetragonal phase (NH) with excellent photo-thermal characteristics, which overcomes the above-mentioned shortcomings of the prior art4)2V3O8The preparation method and the application of the nano-sheet can grow pure (NH)4)2V3O8Nanosheets, the greatest feature of the present invention being the provision of a simple and straightforward solution process for obtaining pure phase (NH)4)2V3O8Nanosheets. The whole reaction process is carried out in a closed environment, and the danger of toxic and harmful substances which can be contacted with a human body can not be generated in the production process. The raw material NH can be mixed by adopting a reducing agent4VO3Conversion to pure phase (NH) in hydrothermal environment4)2V3O8Nanosheets.
The invention adopts the following technical scheme:
tetragonal phase (NH) with photo-thermal characteristic4)2V3O8The preparation method of the nano-sheet takes deionized water as a solvent, and the quantity ratio of the added substances is 1: (4-8) obtaining a mixed solution B by using a vanadium source and a reducing agent, reacting the mixed solution B in a normal atmospheric environment, and growing a pure tetragonal phase (NH) through three stages of heating, heat preservation and cooling4)2V3O8Nanosheets.
Specifically, every 3mmol of vanadium source is dispersed in 15-20 ml of deionized water, the mixture is magnetically stirred and heated to completely dissolve the vanadium source to obtain a solution A, a reducing agent is added into the solution A to obtain a mixed solution B, and 12-24 mmol of reducing agent is added into every 3mmol of vanadium source.
Further, the temperature rise temperature for completely dissolving the vanadium source is 80-100 ℃.
Further, the vanadium source is NH4VO3The reducing agent is thioacetamide.
Specifically, heating the mixed solution B to 150-250 ℃, preserving heat for 15-20 min, cooling to room temperature after the reaction is finished, taking out a reaction product, adding a cleaning solvent for cleaning, removing supernate through centrifugal separation, performing solid-liquid separation to obtain a precipitate, and drying the precipitate to obtain a tetragonal phase (NH)4)2V3O8Nanosheets.
Further, the cleaning solvent comprises ethanol and deionized water.
Further, the speed of centrifugal separation is 4000-10000 r/min, and the separation treatment time is 3-10 min.
Further, the drying treatment temperature is 60-80 ℃, and the drying treatment time is 3-6 hours.
Specifically, (NH)4)2V3O8The nano sheet is two-dimensional sheet-shaped, the thickness of the nano sheet is 160-400 nanometers, and the diameter of the sheet is 2.5-5.6 micrometers.
Another technical scheme of the invention is that the invention is a tetragonal phase (NH)4)2V3O8Use of nanoplatelets in photothermal therapy.
Compared with the prior art, the invention has at least the following beneficial effects:
the method adopts a simple solution method to synthesize the transition metal vanadium compound in the two-dimensional layered material, has the advantages of simplicity, high efficiency, safety and harmlessness, and can synthesize (NH) through three stages of simple temperature rise, temperature preservation and temperature reduction4)2V3O8Under the condition that the molar ratio of the vanadium source to the TAA is 1 (4-8), pure tetragonal phase (NH) can be synthesized4)2V3O8Nanosheets and provides for higher operational accessibility and shorter reaction times.
Furthermore, deionized water is used as a solvent, so that the reaction is not influenced and is harmless to a human body.
Further, the precursor NH can be heated to 80-100 DEG C4VO3And completely dissolving.
Further, the addition of the reducing agent in the present invention was successful in preparing (NH)4)2V3O8The vanadium source is NH4VO3The reducing agent is thioacetamide and NH is adopted4VO3The purpose of the method is that the precursor is easy to dissolve in the water phase; the purpose of thioacetamide is that it is a reducing agent, which would not otherwise yield (NH)4)2V3O8The phase of (1).
Furthermore, the method has the great advantage that a hydrothermal process with high temperature and long-time consumption and complex equipment are avoided, and the heat is only preserved for 15-20 min at the temperature of 150-250 ℃.
Further, the present invention is directed to (NH) produced4)2V3O8The mixed liquid is only required to be cleaned by ethanol and deionized water after separation, and no pollution is caused to the environment.
(NH) prepared by the invention4)2V3O8The nano-sheet has good photo-thermal conversion effect and has a decisive factor in the application of photo-thermal treatment.
In conclusion, the invention avoids high temperature and time consumption, does not need complex equipment, has simple, convenient, high-efficiency and good repeatability, does not relate to harmful reagents, and is safe and harmless to human bodies.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is an XRD spectrum of example 1;
FIG. 2 is an SEM image of example 1;
FIG. 3 is an SEM image of example 1;
FIG. 4 is a temperature rise curve diagram of the nanosheets prepared in example 1 in different concentrations of octadecene solution;
FIG. 5 is an XRD spectrum of example 2;
FIG. 6 is an SEM image of example 2;
FIG. 7 is an XRD spectrum of example 3;
figure 8 is the XRD pattern of example 4.
Detailed Description
The present invention provides a tetragonal phase (NH) having excellent photothermal characteristics4)2V3O8The preparation method of the nano-sheet comprises the steps of firstly, adding NH into a 50mL conical flask4Heating VO powder, heating and stirring to dissolve the VO powder in deionized water to obtain a vanadium source solution A; continuously stirring the vanadium source solution A, keeping the temperature, adding TAA, heating to the temperature required by the reaction, keeping the temperature for 15-20 min, stopping heating after the reaction is finished, and cooling to room temperature in air to grow pure tetragonal phase (NH)4)2V3O8Nanosheets, pure tetragonal phase (NH)4)2V3O8The nano sheet is two-dimensional sheet-shaped, the thickness of the nano sheet is 160-400 nanometers, and the diameter of the sheet is 2.5-5.6 micrometers. The invention avoids high temperature and time consumption, does not need complex equipment, has simple, convenient, high-efficiency and good repeatability, does not relate to harmful reagents, is safe to human bodies and is harmless.
The invention relates to a tetragonal phase (NH) with photo-thermal characteristics4)2V3O8A process for preparing nanoplatelets comprisingThe method comprises the following steps:
s1, dispersing a vanadium source in deionized water, magnetically stirring and heating to completely dissolve the vanadium source to obtain a solution A;
wherein the vanadium source is NH4VO3Per 3mmol of NH4VO3Adding 15-20 ml of deionized water, and heating to 100 ℃;
s2, keeping the temperature and stirring continuously, and adding a reducing agent into the solution A to obtain a mixed solution B;
wherein the reducing agent is Thioacetamide (TAA) and NH is added in every 3mmol4VO3Adding 12-24 mmol of TAA and NH4VO3: the proportion of the molar ratio of TAA is 1 (4-8);
s3, continuously stirring, and preserving the temperature of the mixed solution B at a specified temperature for a period of time to complete crystal growth;
wherein the temperature is 150-250 ℃ and the time is 15-20 min;
s4, after the reaction is finished, keeping the reaction system away from a heat source and cooling to room temperature;
s5, taking out the reaction product, adding a cleaning solvent, performing centrifugal separation, discarding supernatant, and performing solid-liquid separation to obtain a precipitate;
wherein the cleaning solvent comprises ethanol and deionized water, the ethanol and the deionized water are respectively used for cleaning, and the centrifugal separation rate is 4000-10000 r/min;
s6, drying the precipitate obtained in the step S5 in a drying oven to obtain black powder, namely the target product tetragonal phase (NH)4)2V3O8Nanosheets.
The drying temperature is 60-80 ℃, and the drying time is 3-6 hours.
For pure tetragonal phase (NH)4)2V3O8The photo-thermal effect of the nano-sheets in the near-infrared region is researched, and after 808nm laser irradiation for 10min, the concentration of (NH) is 2mg/ml4)2V3O8The temperature of the octadecene solution rises by 32.24 ℃, while the temperature of pure octadecene serving as a control group only rises by 0.17 ℃ under the same condition, and the nano sheet prepared by the method is shown to have better performanceThe photothermal effect of (1).
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Firstly, injecting 15mL of deionized water into a 50mL conical flask, mixing 3mmol of ammonium metavanadate in the deionized water, and heating to 100 ℃ to dissolve to obtain a vanadium source solution A;
then, stirring was continued and incubation was carried out at 100 ℃. Subsequently, 12mmol of TAA were added to react NH4VO3: the molar ratio of TAA was 1: 4. Raising the temperature to 150 ℃, preserving the temperature for 15min to complete the growth of the nano-sheets, then stopping heating, and cooling the reaction system to room temperature;
then, after centrifugal separation at 9600r/min, washing with ethanol and deionized water for 2 times respectively, pouring out supernatant, and drying at 60 ℃ for 6 hours to obtain black powder, namely the target product.
FIG. 1 shows a single crystal (NH) grown in accordance with example 14)2V3O8The X-ray diffraction spectrum of the nanosheet, with almost no impurity peaks, indicates that the product is pure (NH)4)2V3O8。
FIG. 2 shows a single crystal (NH) grown according to example 14)2V3O8SEM morphology photograph of nanosheet, it can be seen that (NH4)2V3O8Is in the shape of quadrangle sheet and canTo see (NH)4)V3O8The sample diameter was observed to be 2.5 micron nm at the smallest and 5.6 micron at the largest in the square shape.
To understand the thickness of the nanosheets grown, a vertically aligned, lamellar scan picture was chosen. FIG. 3 shows a single crystal (NH) grown according to example 14)2V3O8SEM morphology photograph of nanosheet, it can be seen that (NH4)2V3O8The thickness of the sample measured is 160 nm at the minimum and 400 nm at the maximum. FIG. 4 shows the laser power density at 1W/cm2Laser wavelength 808nm) of different concentrations of (NH)4)2V3O8Temperature rise curve of nano sheet octadecylene solution with concentration of 2mg/ml (NH)4)2V3O8The temperature in the octadecene solution increased by 32.24 deg.C, while the same conditions for pure octadecene as a control increased only by 0.17 deg.C.
Example 2
Firstly, injecting 17mL of deionized water into a 50mL conical flask, mixing 3mmol of ammonium metavanadate in the deionized water, and heating to 100 ℃ to dissolve to obtain a vanadium source solution A;
then, stirring was continued and incubation was carried out at 100 ℃. Subsequently, 15mmol of TAA were added to react NH4VO3: the molar ratio of TAA is 1:5, the temperature is increased to 200 ℃ and kept for 16min to finish the growth of the nano-sheets, then the heating is stopped, and the reaction system is cooled to the room temperature;
and finally, centrifugally separating at 5600r/min, washing with ethanol and deionized water for 2 times respectively, pouring out supernatant, and drying at 70 ℃ for 4 hours to obtain black powder, namely the target product.
FIG. 5 shows a single crystal (NH) grown according to example 24)2V3O8X-ray diffraction spectra of the nanoplates, with almost no impurity peaks present, indicate that the product is pure (NH4)2V3O8。
FIG. 6 shows a single crystal (NH) grown in example 24)2V3O8SEM appearance photograph of the nanosheet, it can be seen that (NH)4)2V3O8Is in the shape of a rectangular sheet.
Example 3
Firstly, injecting 18mL of deionized water into a 50mL conical flask, mixing 3mmol of ammonium metavanadate in the deionized water, and heating to 100 ℃ to dissolve to obtain a vanadium source solution A;
then, stirring was continued and incubation was carried out at 100 ℃. Subsequently, 18mmol of TAA were added to react NH4VO3: the molar ratio of TAA was 1: 6. Raising the temperature to 200 ℃ and preserving the temperature for 18min to finish the growth of the nano-sheets, then stopping heating, and cooling the reaction system to room temperature;
then, after centrifugal separation at 4000r/min, washing with ethanol and deionized water for 2 times respectively, pouring out supernatant, and drying at 80 ℃ for 3 hours to obtain black powder, namely the target product.
FIG. 7 shows a single crystal (NH) grown according to example 34)2V3O8The X-ray diffraction spectrum of the nanosheet is almost free of impurity peaks, indicating that the product is pure (NH)4)2V3O8。
Example 4
Firstly, injecting 20mL of deionized water into a 50mL conical flask, mixing 3mmol of ammonium metavanadate in the deionized water, and heating to 100 ℃ to dissolve to obtain a vanadium source solution A;
then, stirring was continued and incubation was carried out at 100 ℃. Subsequently, 24mmol of TAA were added to react NH4VO3: the molar ratio of TAA was 1: 8. Raising the temperature to 250 ℃, preserving the temperature for 20min to complete the growth of the nano-sheets, then stopping heating, and cooling the reaction system to room temperature;
and finally, performing centrifugal separation at 10000r/min, washing with ethanol and deionized water for 2 times respectively, pouring out supernatant, and drying at 70 ℃ for 4 hours to obtain black powder, namely the target product.
Figure 8 is an XRD pattern of the sample obtained in example 4. The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (7)
1. Tetragonal phase (NH) with photo-thermal characteristic4)2V3O8The preparation method of the nano-sheet is characterized in that deionized water is used as a solvent, and the quantity ratio of the added substances is 1: (4-8) obtaining a mixed solution B by using a vanadium source and a reducing agent, wherein the vanadium source is NH4VO3Reacting the mixed solution B in a normal atmospheric environment, heating the mixed solution B to 150-250 ℃, preserving the temperature for 15-20 min, cooling to room temperature after the reaction is finished, taking out a reaction product, adding a cleaning solvent for cleaning, discarding supernatant through centrifugal separation, obtaining a precipitate through solid-liquid separation, and drying the precipitate to obtain a tetragonal phase (NH)4)2V3O8Nanosheets.
2. The preparation method of claim 1, wherein 3mmol of vanadium source is dispersed in 15-20 ml of deionized water, the solution A is obtained by completely dissolving the vanadium source through magnetic stirring and temperature rise, the mixed solution B is obtained by adding a reducing agent into the solution A, and 12-24 mmol of reducing agent is added into 3mmol of vanadium source.
3. The method according to claim 2, wherein the temperature of raising the temperature at which the vanadium source is completely dissolved is 80 to 100 ℃.
4. The method of claim 2, wherein the cleaning solvent comprises ethanol and deionized water.
5. The method according to claim 2, wherein the centrifugal separation rate is 4000 to 10000r/min, and the separation treatment time is 3 to 10 min.
6. The method according to claim 2, wherein the drying is carried out at a temperature of 60 to 80 ℃ for 3 to 6 hours.
7. The method according to claim 1, wherein (NH) is4)2V3O8The nano sheet is two-dimensional sheet-shaped, the thickness of the nano sheet is 160-400 nanometers, and the diameter of the sheet is 2.5-5.6 micrometers.
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