CN110721689A - Porous spherical NiO/TiO2Heterostructure nano material and preparation method thereof - Google Patents
Porous spherical NiO/TiO2Heterostructure nano material and preparation method thereof Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims description 11
- TWBYWOBDOCUKOW-UHFFFAOYSA-N isonicotinic acid Chemical compound OC(=O)C1=CC=NC=C1 TWBYWOBDOCUKOW-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000002243 precursor Substances 0.000 claims abstract description 29
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 25
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001000 nickel titanium Inorganic materials 0.000 claims abstract description 14
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims abstract description 5
- 235000019441 ethanol Nutrition 0.000 claims abstract description 4
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims abstract description 4
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000012298 atmosphere Substances 0.000 claims abstract description 3
- 230000001681 protective effect Effects 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 239000011941 photocatalyst Substances 0.000 abstract description 7
- 239000004065 semiconductor Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 2
- PVNIIMVLHYAWGP-UHFFFAOYSA-N nicotinic acid Natural products OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 13
- 239000002245 particle Substances 0.000 description 6
- 238000004626 scanning electron microscopy Methods 0.000 description 5
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000003795 desorption Methods 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
- 239000011148 porous material Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
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- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
Porous spherical NiO/TiO2Dissolving nickel nitrate hexahydrate and isonicotinic acid in a mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and deionized water, transferring the mixed solution into a high-pressure reaction kettle, heating and reacting for a period of time, centrifuging, cleaning and drying to obtain a spherical nickel and isonicotinic acid coordination precursor assembled in sheets; dissolving spherical nickel, isonicotinic acid coordination precursor and isopropyl titanate in ethanol solution, transferring to a high-pressure reaction kettle, heating for reaction for a period of time, centrifugally collecting a product, cleaning, and drying to obtain uniform spherical nickel-titanium precursor; calcining the spherical nickel-titanium precursor at high temperature in a protective atmosphere to obtain the porous spherical NiO/TiO2A heterostructure nanomaterial. The porous spherical NiO/TiO of the invention2Heterostructure material ofCompared with a NiO single catalyst, the semiconductor P-N junction photocatalyst has higher photocatalytic activity, can be used as a new photocatalytic material, and has better application prospect.
Description
Technical Field
The invention relates to preparation of a novel nano material, in particular to porous spherical NiO/TiO2Heterostructure nanomaterials and methods of making the same.
Background
Photocatalysis using semiconductors as photocatalysts has shown great potential in addressing environmental and energy issues. However, the photocatalytic efficiency is still too low to meet the practical use requirements due to certain limitations, wherein NiO is used as a P-type semiconductor due to the fact that NiO is between a valence band and a conduction bandThere is a wide bandwidth, the band gap is 3.5eV, the utilization of light is low, and the generated photo-generated electron and hole pairs are susceptible to rapid recombination. Thus, the charge separation efficiency is improved, and the recombination of photo-generated electrons and hole pairs can be inhibited, so that the photocatalytic activity is improved. The construction of heterojunctions, particularly P-N heterojunctions, has proven to be an effective method to improve the efficiency of the separation of photogenerated electrons and hole carriers. The P-N junction is based on a semiconductor heterostructure with a photocatalyst capable of providing an internal electric field that can act as a barrier to minimize the recombination of electron and hole carriers, thereby facilitating charge separation. By integrating P-type and N-type semiconductors, an efficient P-N junction photocatalyst may be obtained. Especially NiO/TiO2P-N junction photocatalyst (wherein NiO as a P-type semiconductor is N-type TiO)2Effective promoters of (a) perform well in various photocatalytic reactions. In addition, interconnected mesopores existing in a layered three-dimensional porous structure of the material can improve the diffusion efficiency of reaction molecules, expose more active sites for catalytic reaction, improve the usability of the inner surface, and simultaneously, the porous structure can increase multiple scattering of light so as to improve the light capture efficiency, thereby having good photocatalytic property. However, a porous spherical NiO/TiO is designed2Heterogeneous structure photocatalysts remain a great challenge.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a porous spherical NiO/TiO2Heterostructure nanomaterials and methods of making the same.
Specifically, the invention provides porous spherical NiO/TiO2The preparation method of the heterostructure nano material comprises the following steps:
s1: dissolving nickel nitrate hexahydrate and isonicotinic acid in a mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and deionized water, transferring the mixed solution to a high-pressure reaction kettle, heating and reacting for a period of time, centrifugally collecting a product after the reaction is finished, cleaning, and drying to obtain a spherical nickel and isonicotinic acid coordination precursor assembled in sheets;
s2: dissolving spherical nickel, isonicotinic acid coordination precursor and isopropyl titanate in ethanol solution, transferring the mixed solution to a high-pressure reaction kettle, heating for reaction for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain a uniform spherical nickel-titanium precursor;
s3: calcining the spherical nickel-titanium precursor at a certain heating rate and a certain calcining temperature for a period of time in a protective atmosphere to obtain the porous spherical NiO/TiO2A heterostructure nanomaterial.
Further, in the step S1, the volume ratio of the N, N-dimethylformamide to the absolute ethyl alcohol to the deionized water is 9: 5: 1.
further, in the step S1, the heating temperature is 150 ℃, and the reaction time is 6 hours.
Further, in the step S2, the heating temperature is 150 ℃, and the reaction time is 3-6 hours.
Further, in the step S3, the heating rate is 2 ℃/min, the calcining temperature is 550-600 ℃, and the calcining time is 2-4 h.
The invention also provides the porous spherical NiO/TiO prepared by the preparation method2A heterostructure nanomaterial.
Compared with the prior art, the invention has the beneficial effects that:
the NiO/TiO with porous spheres of the invention2The preparation method of the heterostructure has simple process, obtains the spherical precursor of nickel titanium coordinated with isonicotinic acid by hydrothermal synthesis, and obtains uniform porous spherical NiO/TiO by high-temperature calcination2A heterostructure nanomaterial; the porous spherical NiO/TiO prepared by the invention2A heterostructure material belongs to a semiconductor P-N junction photocatalyst, has higher photocatalytic activity compared with a NiO single catalyst, can be used as a new photocatalytic material, and has better application prospect.
Drawings
FIG. 1 is an X-ray powder diffraction pattern (XRD) (a) of a Ni and isonicotinic acid coordinated precursor prepared by an embodiment of the present invention; scanning Electron Microscopy (SEM) of Ni and isonicotinic acid coordinated precursors (b); ni and isonicotinic acid coordinated precursor element distribution map (EDX) (c-h);
FIG. 2 is a Scanning Electron Microscope (SEM) (a) of a nickel titanium precursor prepared according to an embodiment of the invention; nickel titanium precursor primitive distribution maps (EDX) (b-f);
FIG. 3 NiO/TiO prepared by the inventive example2A heterostructure in which a is NiO/TiO2X-ray powder diffraction pattern (XRD) of the heterostructure; (b) is NiO/TiO2A heterostructure (SEM); c-f is NiO/TiO2Heterostructure element distribution diagram (EDX);
FIG. 4 NiO/TiO prepared by the inventive example2Transmission images (TEMs) of the heterostructure (a-d);
FIG. 5 NiO/TiO prepared according to the example of the invention2Nitrogen desorption and pore size analysis (BET) of the heterostructure.
The specific implementation mode is as follows:
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 only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Examples
Porous spherical NiO/TiO2The preparation method of the heterostructure nano material comprises the following steps:
the first step is as follows: synthesizing the nickel and isonicotinic acid coordination precursor.
0.0290g of nickel nitrate hexahydrate and 0.0123g of isonicotinic acid are dissolved in a mixed solution of N, N-dimethylformamide (9mL), absolute ethyl alcohol (5mL) and deionized water (1mL), the mixed solution is transferred to a polytetrafluoroethylene high-pressure reaction kettle, and the reaction is carried out for 6 hours under the condition of heating to 150 ℃. After the reaction is finished, products are collected through centrifugation, the products are washed for a plurality of times by absolute ethyl alcohol, and the products are placed in a drying box to be dried, so that the Ni and isonicotinic acid coordination precursor can be obtained. FIG. 1a shows an X-ray powder diffraction pattern (XRD) of Ni and isonicotinic acid coordinated precursor, a stronger diffraction peak shows that the product has good crystallinity, FIG. 1b shows a Scanning Electron Microscope (SEM) of Ni and isonicotinic acid coordinated precursor, the obtained morphology is porous spherical, and FIGS. 1C-h show element distribution diagrams (EDX) of Ni and isonicotinic acid coordinated precursor, and the results show that Ni, C, N and O elements are uniformly distributed in the whole spherical particles.
The second step is that: synthetic nickel titanium and isonicotinic acid coordinated porous spherical precursor
Dissolving spherical nickel, isonicotinic acid coordination precursor (15mg) and isopropyl titanate (0.2mL) in an ethanol solution, transferring the mixed solution into a polytetrafluoroethylene high-pressure reaction kettle, heating to a target reaction temperature (150 ℃) and required reaction time (3-6h), collecting a product by centrifugation, washing the product with absolute ethyl alcohol for a plurality of times, and drying in a drying box to obtain the uniform spherical nickel-titanium precursor. FIG. 2a is a Scanning Electron Microscope (SEM) of the nickel titanium precursor, from which it can be seen that the overall morphology of the product after loading titanium still maintains porous spherical shape, and FIGS. 2b-f are EDX diagrams of the nickel titanium precursor, and the results show that the Ni, Ti, C, N and O elements are uniformly distributed throughout the particle.
The third step: calcining to obtain NiO/TiO with porous spheres2Heterostructure composite material
The synthesized spherical nickel-titanium precursor is calcined at high temperature under the protection of argon atmosphere, and the porous spherical NiO/TiO can be obtained by selecting and setting a proper temperature rise rate (2 ℃/min), a proper calcination temperature (550 ℃ -600 ℃) and a proper calcination time (2-4h)2Heterostructure nanomaterials, porous spherical NiO/TiO2The size of the heterostructure is around 5-7 um. FIG. 3a shows NiO/TiO, respectively2The X-ray powder diffraction pattern (XRD) of the heterostructure shows that all diffraction peaks correspond to NiO and anatase TiO2Phase, FIG. 3b, NiO/TiO2SEM image of heterostructure, from which it can be seen that the calcined product still remains porous spherical, FIGS. 3c-f are NiO/TiO2The results of the EDX profile of the heterostructure elements show that the Ni, Ti and O elements are uniformly distributed throughout the particle. FIGS. 4a-d show NiO/TiO2Transmission images (TEM) of the heterostructure, the results of which show that the whole particle is a sheet-assembled porous sphere, whereas TiO2The NiO film is distributed on the NiO sheet in the form of small particles; FIG. 5 shows NiO/TiO2Heterogeneous natureNitrogen desorption and pore size analysis (BET) of the structure, and the results showed that the whole particle had 71.3m2Specific surface area per gram, and the particles are porous.
Claims (6)
1. Porous spherical NiO/TiO2The preparation method of the heterostructure nano material is characterized by comprising the following steps:
s1: dissolving nickel nitrate hexahydrate and isonicotinic acid in a mixed solution of N, N-dimethylformamide, absolute ethyl alcohol and deionized water, transferring the mixed solution to a high-pressure reaction kettle, heating and reacting for a period of time, centrifugally collecting a product after the reaction is finished, cleaning, and drying to obtain a spherical nickel and isonicotinic acid coordination precursor assembled in sheets;
s2: dissolving spherical nickel, isonicotinic acid coordination precursor and isopropyl titanate in ethanol solution, transferring the mixed solution to a high-pressure reaction kettle, heating for reaction for a period of time, centrifugally collecting a product after the reaction is finished, cleaning and drying to obtain a uniform spherical nickel-titanium precursor;
s3: calcining the spherical nickel-titanium precursor at a certain heating rate and a certain calcining temperature for a period of time in a protective atmosphere to obtain the porous spherical NiO/TiO2A heterostructure nanomaterial.
2. The method according to claim 1, wherein in step S1, the volume ratio of N, N-dimethylformamide to absolute ethanol to deionized water is 9: 5: 1.
3. the method according to claim 1, wherein the heating temperature is 150 ℃ and the reaction time is 6 hours in step S1.
4. The preparation method according to claim 1, wherein in the step S2, the heating temperature is 150 ℃ and the reaction time is 3-6 h.
5. The preparation method according to claim 1, wherein in the step S3, the temperature rise rate is 2 ℃/min, the calcination temperature is 550-600 ℃, and the calcination time is 2-4 h.
6. The porous spherical NiO/TiO prepared by the preparation method of any one of the preceding claims2A heterostructure nanomaterial.
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Cited By (1)
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| CN112921337A (en) * | 2021-01-21 | 2021-06-08 | 三峡大学 | Ni/NiO/TiO2Preparation method of heterojunction material and application of heterojunction material in bifunctional catalytic electrolysis of water |
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