CN111874959B - SmMoO 4 (OH)-Ni(OH) 2 Preparation method of nano-sheet - Google Patents
SmMoO 4 (OH)-Ni(OH) 2 Preparation method of nano-sheet Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 25
- 229910018661 Ni(OH) Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000758 substrate Substances 0.000 claims abstract description 34
- YZDZYSPAJSPJQJ-UHFFFAOYSA-N samarium(3+);trinitrate Chemical compound [Sm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YZDZYSPAJSPJQJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 20
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 239000006260 foam Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 239000008367 deionised water Substances 0.000 claims description 37
- 229910021641 deionized water Inorganic materials 0.000 claims description 37
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 30
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 25
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 24
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 19
- 229910052750 molybdenum Inorganic materials 0.000 claims description 19
- 239000011733 molybdenum Substances 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 19
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 18
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- -1 polyethylene Polymers 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 9
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 7
- 239000004698 Polyethylene Substances 0.000 claims description 7
- 239000004743 Polypropylene Substances 0.000 claims description 7
- 239000002585 base Substances 0.000 claims description 7
- 229920000573 polyethylene Polymers 0.000 claims description 7
- 229920001155 polypropylene Polymers 0.000 claims description 7
- 229920000428 triblock copolymer Polymers 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 5
- ARVBXAKTGHWMTM-UHFFFAOYSA-N molybdenum;pentane-2,4-dione Chemical compound [Mo].CC(=O)CC(C)=O ARVBXAKTGHWMTM-UHFFFAOYSA-N 0.000 abstract description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 238000009997 thermal pre-treatment Methods 0.000 abstract 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 9
- 150000002910 rare earth metals Chemical class 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- MGRWKWACZDFZJT-UHFFFAOYSA-N molybdenum tungsten Chemical compound [Mo].[W] MGRWKWACZDFZJT-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
-
- 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
-
- 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
-
- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
SmMoO 4 (OH)‑Ni(OH) 2 The invention relates to a preparation method of nano-sheet, which uses foam nickel as substrate, through hydro-thermal pretreatment of the substrate, then mixing with acetylacetone molybdenum solution, samarium nitrate solution and surfactant, then reacting, smMoO with uniform growth can be obtained through reasonable regulation of raw material types and technological parameters 4 (OH)‑Ni(OH) 2 A nano-sheet. The method has the advantages of simple process, energy conservation and no pollution, and the obtained nano-sheet has uniform size and potential application value in the fields of luminescent materials and photocatalysis.
Description
Technical Field
The invention relates to the technical field of nano functional materials and rare earth composite materials, in particular to SmMoO 4 (OH)-Ni(OH) 2 A preparation method of a nano-sheet.
Background
SmMoO 4 (OH) belongs to the important rare earth molybdenum (tungsten) acid salts. Because of the uniqueness of the fluorescence spectrum of the rare earth element, the molybdate or tungstate containing the rare earth has excellent luminescence property, photocatalysis property, photolysis water property, electric property, magnetic property and the like, and the rare earth resource in China is rich, so that the rare earth molybdate (tungstate) has important research and practical values. At present, the common methods for preparing rare earth molybdenum (tungsten) acid salts are a solid-phase method and a hydrothermal method, researchers also adopt a molten salt method, a sol-gel method and an electrostatic spinning technology to synthesize the rare earth tungsten acid salts, different preparation methods have important points in the process, the obtained material properties are also greatly different, and the proper preparation process is generally selected according to the specific application and production conditions of the material.
The hydrothermal method (solvothermal method) belongs to the current common method for preparing nano materialsThe method is suitable for reducing defects existing in the nano material to a large extent, and has high production efficiency. As disclosed in Chinese patent application 2014101551853, smWO is obtained by a microwave hydrothermal process 4 (OH) nanosheets, pu et al prepared EuW by hydrothermal method 2 O 6 (OH) 3 （Hydrothermal synthesis and luminescent properties of EuW 2 O 6 (OH) 3 red micro-phosphins). However, the nano material with uniform size and distribution of the material which is difficult to obtain by the prior art, so how to realize the controllable size of the rare earth molybdenum (tungsten) acid salt has important research and application values.
Disclosure of Invention
The invention aims at providing a SmMoO with reasonable design aiming at the defects and shortcomings of the prior art 4 (OH)-Ni(OH) 2 The preparation method of the nano-sheet takes foam nickel as a substrate, carries out hydrothermal pretreatment on the substrate, then carries out hydrothermal reaction after being mixed with a molybdenum acetylacetonate solution, a samarium nitrate solution and a surfactant, and can obtain SmMoO with uniform growth through reasonable regulation and control of raw material types and technological parameters 4 (OH)-Ni(OH) 2 The nano-sheets are uniform in size and distribution.
In order to achieve the above purpose, the present invention adopts the following technical scheme: it comprises the following steps:
step (1), substrate pretreatment: performing ultrasonic treatment on the nickel substrate by using dilute hydrochloric acid, washing by using deionized water or absolute ethyl alcohol to remove redundant dilute hydrochloric acid, placing the washed nickel substrate in a hydrothermal reaction kettle, adding a proper amount of deionized water, heating to 90-110 ℃ after sealing, performing low-temperature hydrothermal pretreatment, alternately washing by using deionized water and absolute ethyl alcohol for 3-5 times after the hydrothermal pretreatment is finished, and drying for later use;
step (2), raw material preparation: adding a proper amount of molybdenum acetylacetonate into isopropanol under the stirring condition, and continuing stirring for 5-10min to obtain a molybdenum acetylacetonate solution; adding samarium nitrate into deionized water under the stirring condition, and continuing stirring for 5-10min to obtain a samarium nitrate solution; adding a proper amount of surfactant into the molybdenum acetylacetonate solution, and slowly dropwise adding the samarium nitrate solution under continuous stirring to obtain a precursor solution A;
step (3), hydrothermal reaction: placing the pretreated substrate in the step (1) into a polytetrafluoroethylene lining reaction kettle, then adding a precursor solution A, adding a proper amount of weak base solution to adjust the pH of the solution to be weak base, sealing the reaction kettle for hydrothermal reaction, naturally cooling to room temperature after the reaction is finished, washing the obtained product with deionized water and absolute ethyl alcohol for a plurality of times, and drying at 50 ℃ to obtain the SmMoO4 (OH) -Ni (OH) 2 nanosheets;
in a preferred embodiment, in the step (1), the nickel substrate is a porous nickel substrate, and more preferably a porous foam nickel substrate; the ultrasonic treatment time is 15-30min; the adding volume of the deionized water is 50-70mL; the low-temperature hydrothermal pretreatment time is 4-6 h, the drying is vacuum drying, the drying temperature is 50-60 ℃, and the drying time is 15-30min.
In a preferred scheme, in the step (2), the molar mass of the molybdenum acetylacetonate is 4-6mmol, the molar mass of the samarium nitrate is 8-12 mmol, and the volume ratio of the isopropanol to deionized water to surfactant is 15-30mL:20-35mL:0.5-1.5mL, wherein the surfactant is polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer.
In the preferred scheme, in the step (3), the weak base solution is a mixed alkali solution of triethylamine and hexamethylenetetramine, the volume ratio of the triethylamine to the hexamethylenetetramine in the mixed alkali solution is 1:1, the pH value is 6.5-7.5, the hydrothermal reaction temperature is 120-140 ℃, and the hydrothermal reaction time is 6-12h.
As a further preferable scheme, in the step (1), the low-temperature hydrothermal pretreatment temperature is 90-100 ℃, more preferably 100 ℃, and the low-temperature hydrothermal pretreatment time is 4-5h, more preferably 5h.
As a further preferable scheme, in the step (2), the volume ratio of the isopropyl alcohol to deionized water to the surfactant is 25mL:30mL:1.0mL.
As a further preferable scheme, in the step (3), the pH value is 7.0, the hydrothermal reaction temperature is 130 ℃, and the hydrothermal reaction time is 12 hours.
The beneficial effects of the invention are as follows: the invention uses foam nickel as a substrate, provides enough active sites for the growth of composite nano-sheets through hydrochloric acid washing and low-temperature hydrothermal pretreatment, uses molybdenum acetylacetonate as a molybdenum source, uses samarium nitrate as a samarium source, uses isopropanol and deionized water as solvents, uses polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer as a surfactant, can provide a proper hydrothermal growth environment for the nano-sheets, and finally uses a compounded organic weak base solution-triethylamine and hexamethylenetetramine to adjust the pH value, thereby obtaining the SmMoO with uniform growth through low-temperature hydrothermal reaction 4 (OH)-Ni(OH) 2 A nano-sheet. The SmMoNi composite oxide can be prepared by calcining a hydrothermal product. The invention has simple process, energy conservation and no pollution, the thickness of the obtained nano sheet is 30-60nm, and the dimension and the distribution have potential application value in the fields of luminescent materials and photocatalysis.
Description of the drawings:
FIG. 1 is a sample of SmMoO of example 1 4 (OH)-Ni(OH) 2 Nanoplatelet SEM images.
The specific embodiment is as follows:
the following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
step (1), substrate pretreatment: and (3) carrying out ultrasonic treatment on the porous foam nickel substrate for 15min by using dilute hydrochloric acid, washing for 3 times by using deionized water or absolute ethyl alcohol to remove redundant dilute hydrochloric acid, placing the washed nickel substrate in a hydrothermal reaction kettle, adding 60mL of deionized water, heating to 100 ℃ after sealing for carrying out low-temperature hydrothermal pretreatment, carrying out heat preservation for 5h, alternately washing for 5 times by using the deionized water and absolute ethyl alcohol, and drying for later use.
Step (2), raw material preparation: under the stirring condition, adding 5 mmol of molybdenum acetylacetonate into 25mL of isopropanol, continuously stirring for 5-10min to obtain a molybdenum acetylacetonate solution, and under the stirring condition, adding 10 mmol of samarium nitrate into 30mL of deionized water, continuously stirring for 5-10min to obtain a samarium nitrate solution; 1 mL polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer is added into an acetylacetone molybdenum solution, and a samarium nitrate solution is slowly added dropwise under continuous stirring to obtain a precursor solution A.
Step (3), hydrothermal reaction: placing the pretreated substrate in the step (1) into a polytetrafluoroethylene lining reaction kettle, sequentially adding a precursor solution A, triethylamine and hexamethylenetetramine mixed alkali liquor, regulating the pH value of the solution to 7.0, sealing the reaction kettle, heating to 130 ℃, preserving heat for 12 hours for hydrothermal reaction, naturally cooling to room temperature after the reaction is finished, washing the obtained product with deionized water and absolute ethyl alcohol, and drying at 50 ℃ to obtain SmMoO 4 (OH)-Ni(OH) 2 A nano-sheet. The nanoplatelets are about 50nm in size as observed by scanning electron microscopy.
Example 2:
step (1), substrate pretreatment: and (3) carrying out ultrasonic treatment on the porous foam nickel substrate for 15min by using dilute hydrochloric acid, washing for 3 times by using deionized water or absolute ethyl alcohol to remove redundant dilute hydrochloric acid, placing the washed nickel substrate in a hydrothermal reaction kettle, adding 60mL of deionized water, heating to 90 ℃ after sealing for carrying out low-temperature hydrothermal pretreatment, carrying out heat preservation for 6h, alternately washing for times by using the deionized water and the absolute ethyl alcohol, and drying for later use.
Step (2), raw material preparation: under the stirring condition, adding 5 mmol of molybdenum acetylacetonate into 25mL of isopropanol, continuously stirring for 5-10min to obtain a molybdenum acetylacetonate solution, and under the stirring condition, adding 10 mmol of samarium nitrate into 30mL of deionized water, continuously stirring for 5-10min to obtain a samarium nitrate solution; 1 mL polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer is added into an acetylacetone molybdenum solution, and a samarium nitrate solution is slowly added dropwise under continuous stirring to obtain a precursor solution A.
Step (3), hydrothermal reaction: placing the pretreated substrate in the step (1) into a polytetrafluoroethylene lining reaction kettle, sequentially adding a precursor solution A, triethylamine and hexamethylenetetramine mixed alkali liquor, regulating the pH value of the solution to 7.0, sealing the reaction kettle, heating to 120 ℃, preserving heat for 10 hours, performing hydrothermal reaction, naturally cooling to room temperature after the reaction is finished, washing the obtained product with deionized water and absolute ethyl alcohol, and drying at 50 ℃ to obtain SmMoO 4 (OH)-Ni(OH) 2 A nano-sheet.
Example 3:
step (1), substrate pretreatment: and (3) carrying out ultrasonic treatment on the porous foam nickel substrate for 15min by using dilute hydrochloric acid, washing for 3 times by using deionized water or absolute ethyl alcohol to remove redundant dilute hydrochloric acid, placing the washed nickel substrate in a hydrothermal reaction kettle, adding 60mL of deionized water, heating to 90 ℃ after sealing for carrying out low-temperature hydrothermal pretreatment, carrying out heat preservation for 6h, alternately washing for times by using the deionized water and the absolute ethyl alcohol, and drying for later use.
Step (2), raw material preparation: adding 6mmol of molybdenum acetylacetonate into 30mL of isopropanol under stirring, continuing stirring for 5-10min to obtain a molybdenum acetylacetonate solution, adding 12mmol of samarium nitrate into 35mL of deionized water under stirring, and continuing stirring for 5-10min to obtain a samarium nitrate solution; 1.5mL polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer is added into an acetylacetone molybdenum solution, and a samarium nitrate solution is slowly added dropwise under continuous stirring to obtain a precursor solution A.
Step (3), hydrothermal reaction: placing the pretreated substrate in the step (1) into a polytetrafluoroethylene lining reaction kettle, sequentially adding a precursor solution A, triethylamine and hexamethylenetetramine mixed alkali liquor, regulating the pH of the solution to 7.5, sealing the reaction kettle, heating to 125 ℃, preserving heat for 8 hours for hydrothermal reaction, naturally cooling to room temperature after the reaction is finished, washing the obtained product with deionized water and absolute ethyl alcohol, and drying at 50 ℃ to obtain SmMoO 4 (OH)-Ni(OH) 2 A nano-sheet.
Example 4:
step (1), substrate pretreatment: and (3) carrying out ultrasonic treatment on the porous foam nickel substrate for 15min by using dilute hydrochloric acid, washing for 3 times by using deionized water or absolute ethyl alcohol to remove redundant dilute hydrochloric acid, placing the washed nickel substrate in a hydrothermal reaction kettle, adding 60mL of deionized water, heating to 110 ℃ after sealing for carrying out low-temperature hydrothermal pretreatment, carrying out heat preservation for 4h, alternately washing for times by using the deionized water and the absolute ethyl alcohol, and drying for later use.
Step (2), raw material preparation: under the stirring condition, adding 6mmol of molybdenum acetylacetonate into 25mL of isopropanol, continuously stirring for 5-10min to obtain a molybdenum acetylacetonate solution, and under the stirring condition, adding 12mmol of samarium nitrate into 30mL of deionized water, continuously stirring for 5-10min to obtain a samarium nitrate solution; 1.0mL polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer is added into an acetylacetone molybdenum solution, and a samarium nitrate solution is slowly added dropwise under continuous stirring to obtain a precursor solution A.
Step (3), hydrothermal reaction: placing the pretreated substrate in the step (1) into a polytetrafluoroethylene lining reaction kettle, sequentially adding a precursor solution A, triethylamine and hexamethylenetetramine mixed alkali liquor, regulating the pH of the solution to 7.5, sealing the reaction kettle, heating to 120 ℃, preserving heat for 12 hours for hydrothermal reaction, naturally cooling to room temperature after the reaction is finished, washing the obtained product with deionized water and absolute ethyl alcohol, and drying at 50 ℃ to obtain SmMoO 4 (OH)-Ni(OH) 2 A nano-sheet.
Although the present invention has been described with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements and changes may be made without departing from the spirit and principles of the present invention.
Claims (5)
1. SmMoO 4 (OH)-Ni(OH) 2 The preparation method of the nano-sheet is characterized by comprising the following steps:
step (1), substrate pretreatment: performing ultrasonic treatment on the nickel substrate by using dilute hydrochloric acid, washing by using deionized water or absolute ethyl alcohol to remove redundant dilute hydrochloric acid, placing the washed nickel substrate in a hydrothermal reaction kettle, adding a proper amount of deionized water, heating to 90-110 ℃ after sealing, performing low-temperature hydrothermal pretreatment, alternately washing by using deionized water and absolute ethyl alcohol for 3-5 times after the hydrothermal pretreatment is finished, and drying for later use;
the nickel substrate is a porous foam nickel substrate; the ultrasonic treatment time is 15-30min; the adding volume of the deionized water is 50-70mL; the low-temperature hydrothermal pretreatment time is 4-6 h, the drying is vacuum drying, the drying temperature is 50-60 ℃, and the drying time is 15-30min;
step (2), raw material preparation: adding a proper amount of molybdenum acetylacetonate into isopropanol under the stirring condition, and continuing stirring for 5-10min to obtain a molybdenum acetylacetonate solution; adding samarium nitrate into deionized water under the stirring condition, and continuing stirring for 5-10min to obtain a samarium nitrate solution; adding a proper amount of surfactant into the molybdenum acetylacetonate solution, and slowly dropwise adding the samarium nitrate solution under continuous stirring to obtain a precursor solution A;
the dosage of the molybdenum acetylacetonate is 4-6mmol, the dosage of the samarium nitrate is 8-12 mmol, and the volume ratio of the isopropyl alcohol to deionized water to surfactant is 15-30mL:20-35mL:0.5-1.5mL, wherein the surfactant is polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer;
step (3), hydrothermal reaction: placing the pretreated substrate in the step (1) into a polytetrafluoroethylene lining reaction kettle, then adding a precursor solution A, adding a proper amount of weak base solution to adjust the pH of the solution to be weak base, sealing the reaction kettle for hydrothermal reaction, naturally cooling to room temperature after the reaction is finished, washing the obtained product with deionized water and absolute ethyl alcohol for a plurality of times, and drying at 50 ℃ to obtain SmMoO 4 (OH)-Ni(OH) 2 A nanosheet;
the weak base solution is mixed alkali solution of triethylamine and hexamethylenetetramine, the volume ratio of the triethylamine to the hexamethylenetetramine in the mixed alkali solution is 1:1, the pH value is 6.5-7.5, the hydrothermal reaction temperature is 120-140 ℃, and the hydrothermal reaction time is 6-12h.
2. Smoo according to claim 1 4 (OH)-Ni(OH) 2 The preparation method of the nano-sheet is characterized in that in the step (1), the low-temperature hydrothermal pretreatment temperature is 90-100 ℃, and the low-temperature hydrothermal pretreatment time is 4-5h.
3. Smoo according to claim 1 4 (OH)-Ni(OH) 2 The preparation method of the nano-sheet is characterized in that in the step (2), the volume ratio of the isopropanol to deionized water to the surfactant is 25mL:30mL:1.0mL.
4. Smoo according to claim 1 4 (OH)-Ni(OH) 2 The preparation method of the nano-sheet is characterized in that in the step (3), the pH value is 7.0, the hydrothermal reaction temperature is 130 ℃, and the hydrothermal reaction time is 12 hours.
5. Smoo according to claim 1 4 (OH)-Ni(OH) 2 A method for preparing nano-sheets is characterized in that in the step (3), the SmMoO 4 (OH)-Ni(OH) 2 The thickness of the nano-sheet is 30-60nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010828364.4A CN111874959B (en) | 2020-08-18 | 2020-08-18 | SmMoO 4 (OH)-Ni(OH) 2 Preparation method of nano-sheet |
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