CN106927505B - A kind of ultra-thin magnesium molybdate nano-chip arrays and preparation method thereof - Google Patents
A kind of ultra-thin magnesium molybdate nano-chip arrays and preparation method thereof Download PDFInfo
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- CN106927505B CN106927505B CN201710216509.3A CN201710216509A CN106927505B CN 106927505 B CN106927505 B CN 106927505B CN 201710216509 A CN201710216509 A CN 201710216509A CN 106927505 B CN106927505 B CN 106927505B
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- MODMKKOKHKJFHJ-UHFFFAOYSA-N magnesium;dioxido(dioxo)molybdenum Chemical compound [Mg+2].[O-][Mo]([O-])(=O)=O MODMKKOKHKJFHJ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000003491 array Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 claims abstract description 6
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 claims abstract description 6
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 6
- 238000002604 ultrasonography Methods 0.000 claims abstract 2
- 238000001354 calcination Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001338 self-assembly Methods 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229940091250 magnesium supplement Drugs 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- -1 again Substances 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000011534 incubation Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000007789 sealing Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 239000002060 nanoflake Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Classifications
-
- 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
- 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
-
- 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
- C01P2004/50—Agglomerated particles
Abstract
A kind of ultra-thin magnesium molybdate nano-chip arrays and preparation method thereof, first, magnesium chloride hexahydrate and P123 are hybridly prepared into solution A, secondly, Sodium Molybdate Dihydrate is dissolved in and is configured to the solution B that concentration is 1-5 mM/ls in ethylene glycol, again, solution A and B are mixed, it moves in reaction kettle, sealing, incubation water heating reaction, product vacuum filters after reaction, washing, it is dry, finally, upper step products therefrom and isopropanol are hybridly prepared into suspension, ultrasound, it stands, product centrifugation, washing, it is dry, gained magnesium molybdate nanometer sheet is calcined under an argon atmosphere, obtain ultra-thin magnesium molybdate nano-chip arrays, the ultra-thin magnesium molybdate nano-chip arrays stable appearance prepared, it is regular, purity is high, crystallinity is high, large specific surface area, it is suitble to large-scale production, with at low cost, strong operability, yield is big Feature.
Description
Technical field
The invention belongs to field of inorganic nano-material preparation, in particular to a kind of ultra-thin magnesium molybdate nano-chip arrays and its system
Preparation Method.
Background technique
Ultra-thin two-dimension nano material has unique two-dimensional structure and large specific surface area, mechanical performance and electric conductivity excellent
Feature has important application in fields such as lithium ion battery, supercapacitor and photocatalysis.In recent years, due to nano-chip arrays
Excellent performance, make its photovoltaic device, light emitting diode, gas sensor and electrochemical cell in terms of answer
With more and more extensive, therefore the controlledly synthesis of the nano-chip arrays of regular appearance causes the highest attention of people.Current
In report, nano-chip arrays preparation is mainly substrate synthesis, as Chinese patent CN 104868112A disclose it is a kind of carbon-coated
Titanium dioxide nanoplate array and graphene combination electrode material and preparation method thereof.The invention is by solvent-thermal method in graphene
Synthesizing titanium-containing organic double compound nano-chip arrays in substrate obtain carbon-coated titanium dioxide further across the heat treatment of argon hydrogen and receive
Rice chip arrays and graphene combination electrode material, but this method higher cost, are unfavorable for industrialized production.
Summary of the invention
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of ultra-thin magnesium molybdate nanometer sheet battle arrays
Column and preparation method thereof, the ultra-thin magnesium molybdate nano-chip arrays stable appearance prepared, regular, with high purity, crystallinity is high, compares table
Area is big, is suitble to large-scale production, has the characteristics that at low cost, strong operability, yield are big.
In order to achieve the above object, the technical scheme adopted by the invention is as follows:
A kind of preparation method of ultra-thin magnesium molybdate nano-chip arrays, steps are as follows:
Step 1: by magnesium chloride hexahydrate and P123 according to mass ratio (10-100): 1 is hybridly prepared into solution A；
Step 2: Sodium Molybdate Dihydrate being dissolved in and is configured to the solution B that concentration is 1-5 mM/ls in ethylene glycol；
Step 3: solution A and B are mixed 10-15 minutes according to volume ratio 2:(1-5), moves in reaction kettle, seals,
Incubation water heating reacts 5-10 hours, and hydrothermal temperature is 140-180 DEG C, and product vacuum is filtered, washing, done after reaction
It is dry；
Step 4: step 3 products therefrom and isopropanol being hybridly prepared into suspension according to mass ratio for 1:(10-30), surpassed
Sound is stood, and gained magnesium molybdate nanometer sheet is calcined 1-3 hours, calcination temperature by product centrifugation, washing, drying under an argon atmosphere
It is 400-700 DEG C, obtains ultra-thin magnesium molybdate nano-chip arrays.
Step 4 ultrasonic time is 0.5-2 hours.
Step 4 time of repose is 12-48 hours.
The magnesium molybdate nano-chip arrays are formed by magnesium molybdate nanometer sheet self assembly, and nanometer sheet cross-sectional diameter is 300-
500nm, with a thickness of 10-15nm.
The present invention having the beneficial effect that compared with prior art
The present invention has synthesized ultra-thin molybdenum by hydro-thermal, solvent intercalation and pyrolysismethod using conventional molybdate, magnesium salts as raw material
Sour magnesium nano-chip arrays, do not need base material, prepared magnesium molybdate nano-chip arrays by the self assembly of magnesium molybdate nanometer sheet and
At, crystallinity height, purity is high and regular appearance, large specific surface area, the cross-sectional diameter of nanometer sheet is 300-500nm, with a thickness of
10-15nm.The preparation method strong operability, yield are big, are suitable for industrialized production, prepared magnesium molybdate nano-chip arrays tool
There is biggish specific surface area, and there is high surface energy, therefore, there is biggish application prospect in the energy and photocatalysis field.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of magnesium molybdate nanometer sheet.
Fig. 2 is the scanning electron microscope (SEM) photograph of ultra-thin magnesium molybdate nano-chip arrays.
Fig. 3 is the XRD diagram of ultra-thin magnesium molybdate nano-chip arrays.
Specific embodiment
The present invention is described in further details below with reference to embodiment.
Embodiment one
Step 1: by magnesium chloride hexahydrate and P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide) according to mass ratio
10:1 is hybridly prepared into solution A；
Step 2: Sodium Molybdate Dihydrate being dissolved in and is configured to the solution B that concentration is 3 mM/ls in ethylene glycol；
Step 3: solution A and B being mixed 10 minutes according to volume ratio 2:1, moves in reaction kettle, seals, thermostatted water
Thermal response 5 hours, hydrothermal temperature was 180 DEG C, and product vacuum is filtered, washed, is dry after reaction；
Step 4: step 3 products therefrom and isopropanol (IPA) being hybridly prepared into suspension according to mass ratio for 1:10, surpassed
Sound 1 hour, 36 hours are stood, it is small to be calcined 2 by product centrifugation, washing, drying under an argon atmosphere for gained magnesium molybdate nanometer sheet
When, calcination temperature is 600 DEG C, obtains ultra-thin magnesium molybdate nano-chip arrays.
Fig. 1 is the scanning electron microscope diagram of magnesium molybdate nanometer sheet before embodiment one is calcined, as can be seen from the figure molybdic acid
Nano flake of the magnesium nanometer sheet by thickness in 20nm or so is laminated.
Fig. 2 is the scanning electron microscope of the calcined ultra-thin magnesium molybdate nano-chip arrays of one magnesium molybdate nanometer sheet of embodiment
Figure, wherein ultra-thin magnesium molybdate nano-chip arrays are formed by the pyrolysis self assembly of magnesium molybdate nanometer sheet, cross-sectional diameter 300-
500nm, with a thickness of 10-15nm.
Fig. 3 is the XRD diagram of ultra-thin magnesium molybdate nano-chip arrays, and the object phase of ultra-thin magnesium molybdate nanometer sheet can be determined from Fig. 3
Composition.
Embodiment two
Step 1: by magnesium chloride hexahydrate and P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide) according to mass ratio
50:1 is hybridly prepared into solution A；
Step 2: Sodium Molybdate Dihydrate being dissolved in and is configured to the solution B that concentration is 5 mM/ls in ethylene glycol；
Step 3: solution A and B being mixed 15 minutes according to volume ratio 2:5, moves in reaction kettle, seals, thermostatted water
Thermal response 8 hours, hydrothermal temperature was 140 DEG C, and product vacuum is filtered, washed, is dry after reaction；
Step 4: step 3 products therefrom and isopropanol (IPA) being hybridly prepared into suspension according to mass ratio for 1:20, surpassed
Sound 0.5 hour, 48 hours are stood, it is small to be calcined 3 by product centrifugation, washing, drying under an argon atmosphere for gained magnesium molybdate nanometer sheet
When, calcination temperature is 400 DEG C, obtains ultra-thin magnesium molybdate nano-chip arrays.
Embodiment three
Step 1: by magnesium chloride hexahydrate and P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide) according to mass ratio
100:1 is hybridly prepared into solution A；
Step 2: Sodium Molybdate Dihydrate being dissolved in and is configured to the solution B that concentration is 1 mM/l in ethylene glycol；
Step 3: solution A and B being mixed 12 minutes according to volume ratio 2:3, moves in reaction kettle, seals, thermostatted water
Thermal response 10 hours, hydrothermal temperature was 160 DEG C, and product vacuum is filtered, washed, is dry after reaction；
Step 4: step 3 products therefrom and isopropanol (IPA) being hybridly prepared into suspension according to mass ratio for 1:30, surpassed
Sound 2 hours, 12 hours are stood, it is small to be calcined 1 by product centrifugation, washing, drying under an argon atmosphere for gained magnesium molybdate nanometer sheet
When, calcination temperature is 700 DEG C, obtains ultra-thin magnesium molybdate nano-chip arrays.
Claims (4)
1. a kind of preparation method of ultra-thin magnesium molybdate nano-chip arrays, which comprises the steps of:
Step 1: by magnesium chloride hexahydrate and P123 according to mass ratio (10-100): 1 is hybridly prepared into solution A；
Step 2: Sodium Molybdate Dihydrate being dissolved in and is configured to the solution B that concentration is 1-5 mM/ls in ethylene glycol；
Step 3: solution A and B being mixed 10-15 minutes according to volume ratio 2:(1-5), moves in reaction kettle, seals, constant temperature
Hydro-thermal reaction 5-10 hours, hydrothermal temperature was 140-180 DEG C, and product vacuum is filtered, washed, is dry after reaction；
Step 4: step 3 products therefrom and isopropanol are hybridly prepared into suspension according to mass ratio for 1:(10-30), ultrasound,
It stands, product centrifugation, washing, drying calcine gained magnesium molybdate nanometer sheet 1-3 hours, calcination temperature is under an argon atmosphere
400-700 DEG C, obtain ultra-thin magnesium molybdate nano-chip arrays.
2. a kind of preparation method of ultra-thin magnesium molybdate nano-chip arrays according to claim 1, which is characterized in that the step
Rapid 4 ultrasonic time is 0.5-2 hours.
3. a kind of preparation method of ultra-thin magnesium molybdate nano-chip arrays according to claim 1, which is characterized in that the step
Rapid 4 time of repose is 12-48 hours.
4. a kind of preparation method of ultra-thin magnesium molybdate nano-chip arrays according to claim 1, which is characterized in that the molybdenum
Sour magnesium nano-chip arrays are formed by magnesium molybdate nanometer sheet self assembly, and nanometer sheet cross-sectional diameter is 300-500nm, with a thickness of
10-15nm。
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| CN201710216509.3A CN106927505B (en) | 2017-04-05 | 2017-04-05 | A kind of ultra-thin magnesium molybdate nano-chip arrays and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104374810A (en) * | 2014-11-14 | 2015-02-25 | 湖北大学 | Method for preparing hydrogen sensitive element based on quadrature-phase molybdenum oxide nano-belt |
| CN104437470A (en) * | 2014-11-06 | 2015-03-25 | 上海市纳米科技与产业发展促进中心 | Homogeneous yolk-shell structure Bi2MoO6 microsphere as well as preparation method and application thereof |
-
2017
- 2017-04-05 CN CN201710216509.3A patent/CN106927505B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437470A (en) * | 2014-11-06 | 2015-03-25 | 上海市纳米科技与产业发展促进中心 | Homogeneous yolk-shell structure Bi2MoO6 microsphere as well as preparation method and application thereof |
| CN104374810A (en) * | 2014-11-14 | 2015-02-25 | 湖北大学 | Method for preparing hydrogen sensitive element based on quadrature-phase molybdenum oxide nano-belt |
Non-Patent Citations (1)
| Title |
|---|
| Facile solvothermal synthesis of hierarchical flower-like Bi2MoO6 hollow spheres as high performance visible-light driven photocatalysts;Guohui Tian，et al;《Journal of Materials Chemistry》;20101112;第21卷;第887-892页 |
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