CN113912118A - Preparation method of monodisperse large-size ultrathin two-dimensional strontium niobate nanosheet - Google Patents
Preparation method of monodisperse large-size ultrathin two-dimensional strontium niobate nanosheet Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- VIUKNDFMFRTONS-UHFFFAOYSA-N distrontium;niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Sr+2].[Sr+2].[Nb+5].[Nb+5] VIUKNDFMFRTONS-UHFFFAOYSA-N 0.000 title claims abstract description 22
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 17
- 239000010955 niobium Substances 0.000 claims abstract description 17
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 11
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 238000000703 high-speed centrifugation Methods 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 238000011049 filling Methods 0.000 abstract description 7
- 239000002086 nanomaterial Substances 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 6
- 238000004146 energy storage Methods 0.000 abstract description 5
- 239000000725 suspension Substances 0.000 abstract description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 abstract description 3
- 239000005457 ice water Substances 0.000 abstract description 2
- 229910052758 niobium Inorganic materials 0.000 abstract 2
- 230000008569 process Effects 0.000 description 16
- 239000000843 powder Substances 0.000 description 10
- 239000013078 crystal Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000004108 freeze drying Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
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- 230000001699 photocatalysis Effects 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
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- 238000002524 electron diffraction data Methods 0.000 description 1
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- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
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- 238000000713 high-energy ball milling Methods 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
- 230000028161 membrane depolarization Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- BFRGSJVXBIWTCF-UHFFFAOYSA-N niobium monoxide Chemical compound [Nb]=O BFRGSJVXBIWTCF-UHFFFAOYSA-N 0.000 description 1
- 239000003605 opacifier Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- UYLYBEXRJGPQSH-UHFFFAOYSA-N sodium;oxido(dioxo)niobium Chemical compound [Na+].[O-][Nb](=O)=O UYLYBEXRJGPQSH-UHFFFAOYSA-N 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910001427 strontium ion Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention relates to a preparation method of a monodisperse large-size ultrathin two-dimensional strontium niobate nanosheet, which comprises the following steps: adding niobium pentoxide into a potassium hydroxide solution, obtaining a niobium pentoxide suspension in an ice-water bath environment, controlling the filling volume of a reaction kettle to be 30-40%, and reacting at the temperature of more than 170 ℃ and less than 200 ℃ for 12-24 hours to obtain a clear niobium-containing solution; after the solution is centrifuged at high speed to remove trace impurities, a strontium nitrate solution with the same volume as the niobium-containing solution is slowly dripped by using a syringe pump and is continuously stirred strongly for 8 to 10 hours, and then the solution reacts at the temperature of 230 ℃ and 250 ℃ for 66 to 78 hours to obtain the ultrathin two-dimensional strontium niobate nano material. The large-size ultrathin two-dimensional strontium niobate nano material prepared by the method has the thickness of below 5 nanometers, the length and width of 1-4 micrometers, simple preparation process and low cost, and simultaneously provides wide application prospects in the fields of piezoelectric catalysis, organic and inorganic composite energy storage and microwave resonance.
Description
Technical Field
The invention relates to a high-purity strontium niobate nano material, in particular to monodisperse large-size ultrathin two-dimensional Sr2Nb2O7(SNO) nanosheet preparation method.
Background
The SNO with the layered perovskite structure has ultrahigh Curie temperature (more than 1300 ℃), and the resistivity of the SNO is 2 to 3 orders of magnitude higher than that of the traditional perovskite and bismuth layered ferroelectric materials, so the SNO has very good application prospect in the fields of structural control and health monitoring sensors in aerospace, nuclear power stations and automobile industries. The band gap of SNO is 3.5eV, the state density at the conduction band is mainly from the d orbit of Nb, which determines that the Nb has certain photocatalytic activity, and the rotation of the niobium-oxygen octahedron makes the Nb have the property of spontaneous polarization. When subjected to mechanical strain, a depolarization electric field induced by polarization can promote the separation of electrons and holes, so that charge accumulation is caused, and the photocatalytic activity is improved. Therefore, the SNO has a good application prospect in the field of piezoelectric catalysis. In addition, SNO has a lower dielectric constant of about 60 compared with piezoelectric materials such as barium titanate and sodium niobate, but the higher resistivity indicates that the SNO has better breakdown-resistant property, so that in the field of organic-inorganic composite energy storage, the dielectric property of the polymer can be improved to a certain extent, and the breakdown-resistant strength of the composite material can be prevented from being rapidly attenuated.
However, the traditional synthesis technology of SNO powder is mainly based on solid state reaction, and not only needs higher sintering temperature (>1200 ℃), but also needs further high energy ball milling process, and meanwhile, solid phase synthesis is easy to cause the result of lower purity of reaction products due to uneven distribution of local elements. In addition, the piezoelectric catalysis and organic-inorganic composite energy storage material has higher requirements on the powder, namely high surface energy and large length-diameter ratio, so as to meet the requirements of high-activity catalytic reaction and effective improvement of polymer dielectric constant. At present, SNO nano powder which is successfully synthesized has small and uneven size and does not meet the requirement of large length-diameter ratio.
Disclosure of Invention
The present invention has been made to solve the above problems, and an object of the present invention is to provide a monodispersed large-sized ultra-thin two-dimensional Sr2Nb2O7The preparation method of the (SNO) nanosheet can obtain a flaky two-dimensional SNO material with micron-sized length and width and nano-sized thickness, the material can be used as a raw material for high-temperature sensors, piezoelectric catalysis and organic-inorganic composite energy storage, and the preparation method is simple in preparation process and low in cost.
Monodisperse large-size ultrathin two-dimensional Sr2Nb2O7(SNO) sodium saltThe preparation method of the rice flakes comprises the following steps:
(1) adding niobium pentoxide into a potassium hydroxide solution, performing pulse ultrasonic dispersion in an ice-water bath environment to obtain a niobium pentoxide suspension, transferring the niobium pentoxide suspension into a reaction kettle for heat treatment to obtain a clear solution;
(2) and (3) centrifuging the solution at a high speed to remove trace impurities, adding a strontium nitrate solution into the solution, stirring the solution with strong force continuously, and reacting the solution in a reaction kettle to obtain the ultrathin two-dimensional strontium niobate nano material.
Further, in the step (1), the concentration of the potassium hydroxide solution is 3.8-4.2mol L-1。
Further, in the step (1), the molar addition amount of the niobium pentoxide is 0.015-0.018 times of the molar number of the potassium hydroxide.
Further, in the step (1), the pulse ultrasonic dispersion process should be carried out at 0-10 ℃, the ultrasonic frequency is 20-25kHz, the power is 150-.
Further, in the step (1), the hydrothermal reaction kettle is made of polytetrafluoroethylene, the filling volume is 30-40%, the heat treatment temperature is 170-200 ℃, and the time is 12-24 h.
Further, in the step (2), the clarified solution is centrifuged at a high speed to remove trace impurities, wherein the centrifugation speed is 10000r/min, and the time is 10 min.
Further, the concentration of the strontium nitrate solution in the step (2) is 0.16-0.24 mol/L.
Further, in the step (2), the strontium nitrate solution is slowly dripped by using a syringe pump, the injection rate is 30-50ml/h, strong stirring is required in the dripping process, and the stirring is continuously carried out for 8-10h, so that the uniformity of the solution is ensured. Wherein the molar ratio of strontium to niobium atoms is 1: 1.
Further, in the step (2), the hydrothermal reaction kettle is made of PPL material, the filling volume is 60-80%, the reaction temperature is 230-250 ℃, and the time is 66-78 h.
Further, in the step (2), the hydrothermal reaction product needs to be soaked in hydrochloric acid for 3-5h, then is respectively centrifugally cleaned for 3-5 times by using absolute ethyl alcohol and deionized water, and finally is subjected to freeze drying treatment at the vacuum-50 ℃ for 18-24 hours to obtain the monodisperse large-size ultrathin two-dimensional strontium niobate nanosheet.
The invention provides a monodispersed large-size ultrathin two-dimensional Sr prepared by the method2Nb2O7(SNO) nanosheets, wherein the length and width of each nanosheet are 1-4 microns, and the thickness of each nanosheet is less than 5 nanometers.
The technical scheme of the invention provides the monodisperse large-size ultrathin two-dimensional Sr which has the advantages of low cost, simple process and easy industrial production2Nb2O7The preparation method of the (SNO) nanosheet, and the obtained SNO nanomaterial provides a new material for high-temperature sensors, piezoelectric catalysis and organic-inorganic composite energy storage capacitors, and promotes the development of nanomaterials and electronic industry.
Compared with the prior art, the invention has the following characteristics: the monodisperse ultrathin SNO nanosheet powder synthesized by the two-step hydrothermal method is high in purity, free of impurity phase, high in surface energy and large in length-diameter ratio, and the transverse size of the powder reaches 1-4 micrometers, the thickness of the powder is less than 5 nanometers.
Drawings
FIG. 1 is a schematic diagram of the crystal structure and XRD spectrum of SNO synthesized by hydrothermal method in example 2;
FIG. 2 is a FESEM topography of the synthetic SNO of example 2;
FIG. 3 is a TEM high resolution lattice fringe and electron diffraction pattern of the synthetic SNO of example 2;
FIG. 4 is a graph of AFM topography analysis and thickness measurement of the synthetic SNO of example 2.
Detailed Description
The present invention is described in detail below with reference to the attached drawings and specific embodiments so that aspects and advantages of the invention can be better understood. The following detailed description and examples are for illustrative purposes only.
Through multiple exploration of the synthesis process, the invention invents monodisperse large-size ultrathin two-dimensional Sr2Nb2O7(SNO) nanosheet preparation method.
The technological scheme of the present invention includes two steps, including the first step of hydrothermal reaction in strong alkali condition to obtain soluble niobate solution, and the second step of hydrothermal reaction in strontium nitrate solution.
The preparation method of the nano material comprises the following steps:
1) preparing hydrothermal kettle with 30-40% of capacity and 3.8-4.2mol L of concentration-1Adding niobium pentoxide powder into the potassium hydroxide solution, wherein the mole number of the niobium pentoxide powder is 0.15-0.18 times of that of the potassium hydroxide. Under the condition of 0-10 ℃ cold water bath, pulse ultrasound is carried out for 4-6h, the ultrasound frequency is 20-25kHz, and the power is 150-. Heat treatment is carried out for 12-24h at the temperature of 170-200 ℃;
2) and (3) centrifuging the clarified solution obtained in the first step at a high speed to remove trace impurities, wherein the centrifugation speed is 10000r/min, and the centrifugation time is 10 min. Slowly dripping a strontium nitrate solution with the concentration of 30-50ml/h by using a syringe pump, continuously stirring strongly for 8-10h, wherein the mol number of the added strontium nitrate is 60-80% of the filling volume of the hydrothermal kettle, and reacting for 66-78h at the temperature of 230 ℃ and 250 ℃.
3) And (3) soaking the obtained SNO powder in hydrochloric acid for 3-5h, respectively centrifugally cleaning with absolute ethyl alcohol and deionized water for 3-5 times, and finally carrying out freeze drying treatment at the temperature of-50 ℃ in vacuum for 18-24 hours to obtain the monodisperse large-size ultrathin two-dimensional SNO nanosheet.
The following examples are given in detail to illustrate the embodiments and specific procedures of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
This example was used to prepare a soluble niobate solution, the preparation method comprising the following steps:
1) prepared into 35ml with the concentration of 4mol L-1The potassium hydroxide solution of (a) was added to a 100ml inner liner of a polytetrafluoroethylene hydrothermal reactor.
2) 0.5g of niobium pentoxide powder is added into the potassium hydroxide solution, and pulse ultrasound is carried out for 5 hours under the condition of a cold water bath at 5 ℃, wherein the ultrasonic frequency is 25kHz, and the power is 200W.
3) Subsequently, the suspension after ultrasonic dispersion is subjected toHeat treating at 180 deg.C for 20h to obtain clear soluble niobate solution K8Nb6O19·10H2O。
Example 2
This example is for monodisperse large size ultra-thin two-dimensional Sr2Nb2O7The preparation and characterization of (SNO) nanosheet, the preparation method comprising:
1) the clarified solution obtained in example 1 was centrifuged at high speed for 10min at 10000r/min to remove trace impurities and transferred to a 100ml inner liner of a hydrothermal kettle made of PPL.
2) 35ml of 0.2mol/L strontium nitrate solution is slowly dripped into the solution, a syringe pump is used in the dripping process, the injection rate is 40ml/h, white opacification is generated in the process, therefore, the continuous strong stirring is needed in the dripping process, the stirring is continued for 10h, and the filling volume of the hydrothermal kettle is about 70 percent at the moment.
3) Sealing the white emulsion in a hydrothermal kettle, and carrying out heat treatment for 72h, wherein the temperature rise process is 3 ℃/min from room temperature to 200 ℃, and then at 1 ℃/min to 240 ℃;
4) and after the reaction is finished, soaking the obtained white precipitate in a hydrochloric acid solution for 4 hours, continuously stirring, centrifugally cleaning for 5 times by using absolute ethyl alcohol and deionized water respectively, and freeze-drying for 20 hours at the temperature of minus 50 ℃ in a freeze dryer to obtain the monodisperse large-size ultrathin two-dimensional SNO nanosheets.
FIG. 1 shows the crystal structure and XRD pattern of the synthesized SNO, which has a sandwich layered structure with Sr ion layers spaced apart, and all diffraction peaks in the pattern completely match Sr2Nb2O7The standard diffraction peak of PDF #70-0114 shows that the synthesized SNO powder contains no impurity phase and has high purity.
Fig. 2 is an FESEM image of the synthesized SNO, and it can be seen that the nanosheet has a good two-dimensional structural feature, is thin in thickness, shows a certain transparent characteristic, and has a transverse dimension of about 1-4 microns.
FIG. 3 is a TEM image of the synthesized SNO with lattice fringe spacing
Corresponding to a (002) crystal face in a crystal structure, the electronic diffraction pattern is the superposition of two sets of lattices, corresponding to a special sandwich layer crystal structure, the lattice of the diffraction pattern can be calibrated through analysis, and the crystal axis is obtained as [010 ]]And (4) direction.
Fig. 4 is an AFM image of the synthesized SNO, which corresponds to an FESEM image, and shows that the SNO has an obvious two-dimensional structural feature, and the thickness of the SNO can be obtained by measuring nanosheets tiled on a substrate to be about 4-5 nm.
Example 3
This example is for monodisperse large size ultra-thin two-dimensional Sr2Nb2O7The preparation and characterization of (SNO) nanosheet, the preparation method comprising:
1) the clarified solution obtained in example 1 was centrifuged at high speed for 10min at 10000r/min to remove trace impurities and transferred to a 100ml inner liner of a hydrothermal kettle made of PPL.
2) And slowly dropwise adding 30ml of 0.2mol/L strontium nitrate solution into the solution, wherein a syringe pump is used in the dropwise adding process, the injection rate is 30ml/h, white opacifier is generated in the process, therefore, the hydrothermal kettle is continuously stirred strongly and is continuously stirred for 8h, and the filling volume of the hydrothermal kettle is about 60 percent.
3) Sealing the white emulsion in a hydrothermal kettle, and carrying out heat treatment for 66h, wherein the temperature rise process is 3 ℃/min from room temperature to 200 ℃, and then at 1 ℃/min to 250 ℃;
4) and after the reaction is finished, soaking the obtained white precipitate in a hydrochloric acid solution for 3 hours, continuously stirring, centrifugally cleaning for 5 times by using absolute ethyl alcohol and deionized water respectively, and freeze-drying in a freeze dryer at-50 ℃ for 18 hours to obtain the monodisperse large-size ultrathin two-dimensional SNO nanosheet.
Example 4
This example is for monodisperse large size ultra-thin two-dimensional Sr2Nb2O7The preparation and characterization of (SNO) nanosheet, the preparation method comprising:
1) the clarified solution obtained in example 1 was centrifuged at high speed for 10min at 10000r/min to remove trace impurities and transferred to a 100ml inner liner of a hydrothermal kettle made of PPL.
2) 40ml of 0.2mol/L strontium nitrate solution is slowly dripped into the solution, a syringe pump is used in the dripping process, the injection speed is 50ml/h, white opacification is generated in the process, therefore, the continuous strong stirring is needed in the dripping process, the stirring is continued for 8h, and the filling volume of the hydrothermal kettle is about 80 percent at the moment.
3) Sealing the white emulsion in a hydrothermal kettle, and carrying out heat treatment for 78h, wherein the temperature rise process is 3 ℃/min from room temperature to 200 ℃, and then at 1 ℃/min to 230 ℃;
4) and after the reaction is finished, soaking the obtained white precipitate in a hydrochloric acid solution for 5 hours, continuously stirring, centrifugally cleaning for 5 times by using absolute ethyl alcohol and deionized water respectively, and freeze-drying for 24 hours at the temperature of minus 50 ℃ in a freeze dryer to obtain the monodisperse large-size ultrathin two-dimensional SNO nanosheets.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of monodisperse large-size ultrathin two-dimensional strontium niobate nano-sheets is characterized in that the chemical formula of the strontium niobate nano-sheets is Sr2Nb2O7The preparation method comprises the following steps:
(1) adding niobium pentoxide into a potassium hydroxide solution, performing ultrasonic dispersion, and performing a first-step hydrothermal reaction to obtain a clear solution;
(2) and (2) dropwise adding a strontium nitrate solution into the clear solution obtained in the step (1), continuously stirring strongly, carrying out a second-step hydrothermal reaction, and carrying out post-treatment to obtain the ultrathin two-dimensional strontium niobate nanosheet.
2. The preparation method of monodisperse large-size ultrathin two-dimensional strontium niobate nanosheets as claimed in claim 1, wherein the potassium hydroxide solution in step (1) has a concentration of 3.8-4.2mol/L and a volume of 30-40% of the hydrothermal kettle capacity, and the addition amount of niobium pentoxide is 0.015-0.018 times the mole number of potassium hydroxide.
3. The preparation method of monodisperse large-size ultrathin two-dimensional strontium niobate nanosheets as claimed in claim 1, wherein the ultrasonic frequency in step (1) is 20-25kHz, the power is 150-200W, 2s pulse ultrasonic intervals, and the ultrasonic time is 4-6 hours.
4. The method for preparing monodisperse large-size ultrathin two-dimensional strontium niobate nanosheets as recited in claim 1, wherein the first hydrothermal reaction in step (1) is at a temperature of 170-200 ℃ for 12-24 hours.
5. The method for preparing monodisperse large-size ultrathin two-dimensional strontium niobate nanosheets according to claim 1, wherein the clear solution in step (1) requires further high speed centrifugation to remove trace amounts of reaction impurities.
6. The method for preparing monodisperse large-size ultrathin two-dimensional strontium niobate nanosheets according to claim 1, wherein the concentration of the strontium nitrate solution in step (2) is 0.16-0.24 mol/L.
7. The preparation method of monodisperse large-size ultrathin two-dimensional strontium niobate nanosheets as claimed in claim 1, wherein the strontium nitrate solution in step (2) needs to be slowly added dropwise to the clear solution in step (1) under the control of an injection pump, and continuously stirred with strong force, the injection rate is 30-50ml/h, and stirring needs to be continued for 8-10h after the dropwise addition is finished.
8. The method for preparing monodisperse large-size ultrathin two-dimensional strontium niobate nanosheets as recited in claim 1, wherein the second hydrothermal reaction temperature in step (2) is 230-250 ℃ and the reaction time is 66-78 hours.
9. The preparation method of the monodisperse large-size ultrathin two-dimensional strontium niobate nanosheets as claimed in claim 1, wherein the hydrothermal reaction product in step (2) is soaked in hydrochloric acid for 3-5 hours, then respectively washed centrifugally 3-5 times with absolute ethanol and deionized water, and finally freeze-dried at-50 ℃ under vacuum for 18-24 hours to obtain the monodisperse large-size ultrathin two-dimensional strontium niobate nanosheets.
10. The method for preparing monodisperse large-size ultrathin two-dimensional strontium niobate nanosheets according to any one of claims 1 to 9, wherein the large-size ultrathin two-dimensional strontium niobate nanosheets are 1-4 microns in length and width and 5 nanometers or less in thickness.
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