CN105289660B - A kind of preparation method and use of magnesium ferrite/molybdenum sulfide heterojunction nano-wire - Google Patents
A kind of preparation method and use of magnesium ferrite/molybdenum sulfide heterojunction nano-wire Download PDFInfo
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- CN105289660B CN105289660B CN201510702322.5A CN201510702322A CN105289660B CN 105289660 B CN105289660 B CN 105289660B CN 201510702322 A CN201510702322 A CN 201510702322A CN 105289660 B CN105289660 B CN 105289660B
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- magnesium ferrite
- magnesium
- molybdenum sulfide
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- 239000011777 magnesium Substances 0.000 title claims abstract description 79
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 78
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 73
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000002070 nanowire Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims description 6
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 44
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006731 degradation reaction Methods 0.000 claims abstract description 10
- 230000015556 catabolic process Effects 0.000 claims abstract description 8
- 238000001523 electrospinning Methods 0.000 claims abstract description 8
- 238000010041 electrostatic spinning Methods 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 19
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 14
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 9
- 150000002823 nitrates Chemical class 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 229910052573 porcelain Inorganic materials 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000010189 synthetic method Methods 0.000 claims 5
- 229920003082 Povidone K 90 Polymers 0.000 claims 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 9
- 238000000151 deposition Methods 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- 239000004098 Tetracycline Substances 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 229960002180 tetracycline Drugs 0.000 abstract description 4
- 229930101283 tetracycline Natural products 0.000 abstract description 4
- 235000019364 tetracycline Nutrition 0.000 abstract description 4
- 150000003522 tetracyclines Chemical class 0.000 abstract description 4
- 239000011259 mixed solution Substances 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000001354 calcination Methods 0.000 description 11
- 238000002474 experimental method Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 230000005611 electricity Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 125000005909 ethyl alcohol group Chemical group 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical class [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 238000010025 steaming Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- -1 nanometer Rod Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention belongs to nano material synthesis technical field, synthesizes magnesium ferrite first with electrospinning process, then molybdenum sulfide is grown above using vapour deposition method, so as to form magnesium ferrite/molybdenum sulfide heterojunction nano-wire.MgFe prepared by the present invention2O4/MoS2Heterojunction nano-wire reaches 92% in 120min to the degradation rate of tetracycline, and the hydrogen generation efficiency in water and methanol mixed solution is 5.8 mmol/h m2。
Description
Technical field
The invention belongs to nano material synthesis technical field, and magnesium ferrite, Ran Houli are synthesized first with electrospinning process
Molybdenum sulfide is grown above with vapour deposition method, so as to form magnesium ferrite/molybdenum sulfide heterojunction nano-wire.
Background technology
Optical electro-chemistry（PEC）It is a kind of emerging environmental energy technology, solar energy can be effectively utilized dyestuff is degraded
With production hydrogen, in PEC, electrode produces photogenerated charge and hole, and has carried out oxidation-reduction reaction；Semi-conducting material has
There are wider bandgap structure and preferable physical and chemical stability, its important function in PEC, except the property of semiconductor in itself
Matter, the form of semiconductor also play a crucial role in the PEC performances of optoelectronic pole；Social now, PEC hydrogen production by water decomposition is one to be had very much
Using the technology of future, the technology can realize conversion of the solar energy to chemical energy, and free of contamination combustion process makes it
There is incomparable advantage in terms of green energy resource.
Nano science and nanometer technology are arisen at the historic moment in recent years, and one-dimensional nano structure is in physics, chemistry, the energy, bioid
In terms of, and huge progress is achieved in terms of exploitation to new function material, and electrostatic spinning is a preparation nanometer
The simple and convenient method of material, this method can be used for preparing various expected one-dimensional nano structures（Including nano wire, nanometer
Rod, nanotube and nanobelt）；Generally, the most of one-dimensional nano structures manufactured by Electrospun are assembled into little particle（Size
For from 1 nanometer to 100 nanometers）, this further makes them have higher intensity, diffusivity and plasticity.
Spinel-type ferrous acid magnesium is face-centered cubic closs packing spinel structure and n-type semiconductor, have outstanding magnetic and
Photoelectric characteristic, it is often more important that its band gap is about 1.9 electron-volts, so spinel-type ferrous acid magnesium can ring to visible ray
Should, this causes it to turn into a kind of material for being used to prepare the reaction of photocatalysis potentiality matrix, the separation in light induced electron and hole and multiple
The ideal photocatalytic activity for make it that spinel-type ferrous acid magnesium has in terms of degraded or hydrogen manufacturing is closed, in addition, molybdenum disulfide has
There is excellent electronic conductivity, and the molybdenum disulfide of narrow band gap can also extend its absorption region to light, improve the profit of light
Use efficiency；The research of magnesium ferrite and molybdenum sulfide is more at present, but its composite studies is less, and molybdenum disulfide and spinel-type
The one-dimensional composite material of magnesium ferrite is possible to be endowed the PhotoelectrochemicalProperties Properties of enhancing.
The content of the invention
Molybdenum disulfide/magnesium ferrite nano wire of the present invention（P-n heterojunction）The advantages of sufficiently make use of both materials
And the shortcomings that can overcoming its own, so as to strengthen photoelectric catalytically active, this can be attributed to the sulphur of the magnesium ferrite to be formed/bis-
Change the restructuring that molybdenum heterojunction structure effectively suppresses photogenerated charge, so as to be effectively improved the utilization rate of solar energy.
The preparation method of this heterojunction nano-wire, carried out according to the following steps:
（1）Weigh nine water ferric nitrates and magnesium nitrate hexahydrate is placed in test tube, add solvent, stir and add PVP
(K90), it is finally fully mixed to obtain to settled solution, i.e. electrostatic spinning precursor liquid.
The mol ratio of nine water ferric nitrates and magnesium nitrate hexahydrate is 3 in the experiment:1, the solvent is the water of absolute ethyl alcohol
Solution, wherein the volume ratio of 2 distilled water and absolute ethyl alcohol is 1:3, magnesium nitrate hexahydrate and PVP molal weight ratio position 1
mmol:0.26g。
（2）Precursor liquid is drawn, electrospinning is then carried out by electrostatic spinning apparatus, then collects product, and pass through Muffle furnace
Calcining, obtains magnesium ferrite.
Described to carry out electrospinning by electrostatic spinning apparatus be that electrospinning is carried out under 25 KV, and under 25 degrees Celsius, 55 humidity
Carry out；And it is that Elevated Temperature Conditions are 1 DEG C/min to 400 DEG C, 5 DEG C/min to 500 DEG C, then calcined to calcine.
（3）Magnesium ferrite, ammonium molybdate and thiocarbamide are weighed, ammonium molybdate and the well mixed rear and magnesium ferrite of thiocarbamide are respectively placed in porcelain boat
Both ends, it is put into tube furnace in N2Under protection, in order to which molybdenum sulfide preferably can be supported on magnesium ferrite under nitrogen flowing, so
After be warming up to 500 DEG C, the h of constant temperature 2, obtain MgFe2O4/MoS2。
The mass ratio of the molybdenum sulfide and magnesium ferrite is 0.02-0.3：1；Heating rate is 2 DEG C/min.
This experiment using using method of electrostatic spinning before this, be it is a kind of it is easy, effective, the new of nanofiber can be produced
Type process technology, it has, and device is simple, cost is cheap, can spin the advantages of substance classes are various, technique is controllable.
Secondly vapour deposition method is used, makes MoS2In MgFe2O4Surface homoepitaxial, so as to be to synthesize more pure MgFe2O4/
MoS2, vapour deposition method can on metal, semiconductor etc. deposited metal or semiconductive thin film.Sample high purity that the method obtains and
And can be with on-line checking and control film, and the method is substantially without 2 pollutions.
The purpose of the present invention：The first, prepared MgFe is provided2O4/MoS2The preparation method of heterojunction nano-wire, two, will
MgFe2O4/MoS2Heterojunction nano-wire is used for photoelectrochemical degradation and reacts and produce hydrogen reaction.
MgFe2O4/MoS2Heterojunction nano-wire photoelectrochemical degradation reacts and production hydrogen reaction experiment step difference is as follows：
Photoelectrochemical degradation：Carried out under CHI 852C type electrochemical workstations, add 50 mL 1mol/L's in electrolytic cell
The tetracycline aqueous solution, silver chloride electrode is added as reference electrode, platinum electrode is added and is used as to electrode, MgFe2O4/MoS2It is heterogeneous
Junction nanowire carries out photoelectrochemical degradation reaction as working electrode.
Photoelectricity liberation of hydrogen：Carried out under CHI 852C type electrochemical workstations, add 50 mL 1mol/L's in electrolytic cell
The tetracycline aqueous solution, water and methanol mixed solution（Volume ratio 5:1）, silver chloride electrode is added as reference electrode, adds platinum electricity
Pole is used as to electrode, MgFe2O4/MoS2Heterojunction nano-wire carries out photoelectrochemical degradation reaction as working electrode.
MgFe prepared by the present invention2O4/MoS2Heterojunction nano-wire reaches to the degradation rate of tetracycline in 120min
92%, and the hydrogen generation efficiency in water and methanol mixed solution is 5.8 mmol/h m2.Beneficial effect
Present invention synthesis MgFe2O4/MoS2Heterojunction nano-wire photochemical catalyst, is a kind of novel photocatalysis material, the material
Material is with good chemical stability and photoelectrochemical behaviour.
Present invention process is simple, favorable reproducibility, and raw materials are simple compounds, and cheap and easy to get, cost is low, symbol
Environment-friendly requirement is closed, the reaction time is shorter, so as to reduce energy consumption and reaction cost, is easy to produce in batches；Simultaneously because
MgFe2O4/MoS2Heterojunction nano-wire photochemical catalyst has stronger photoelectric catalysis degrading ability, very high so as to make it have
Actual application ability.
Brief description of the drawings
The x-ray photoelectron spectroscopy figure of Fig. 1 magnesium ferrites/molybdenum disulfide（XPS）.（a）Quan Pu,（b）Mo 3d,（c）S
2p,（d）Fe 2P,（e）O 1s and（f）Mg 1s.
Fig. 2 (a) magnesium ferrites;(b) magnesium ferrite/molybdenum disulfide (ω=2%);(c) magnesium ferrite/molybdenum disulfide (ω=
5%);(d) magnesium ferrite/molybdenum disulfide (ω=10%);(e) magnesium ferrite/molybdenum disulfide (ω=20%) and (f) magnesium ferrite/
Field emission scanning electron microscope (SEM) figure of molybdenum disulfide (ω=30%).
The transmission electron microscope of Fig. 3 magnesium ferrites (a, b, c) and magnesium ferrite/molybdenum disulfide (d, e)（TEM）And iron
The high resolution electron microscope (f) of sour magnesium/molybdenum disulfide.
The photoelectric catalysis degrading efficiency of Fig. 4 magnesium ferrites and magnesium ferrite/molybdenum disulfide.
The hydrogen production rate schematic diagram of Fig. 5 magnesium ferrites/molybdenum disulfide (ω=10%) and magnesium ferrite.
Embodiment
With reference to embodiment, the present invention is described in detail, so that those skilled in the art more fully understand this hair
It is bright, but the invention is not limited in following examples.
The mass ratio of the molybdenum sulfide of embodiment 1 and magnesium ferrite is 0.02
（1）Weigh 15 mmol ferric nitrates and 5 mmol magnesium nitrates are placed in 50 mL test tubes, add 2.5mL2 steaming
Distilled water and 7.5mL absolute ethyl alcohols simultaneously stir, and then add 1.3 g PVP（K90）, finally it is fully mixed must clarify it is molten
Liquid, i.e. electrostatic spinning precursor liquid.
（2）5 mL precursor liquids are drawn in glass syringe, then carry out electricity under 25 KV by electrostatic spinning apparatus
Spin, then collect product, and calcined by Muffle furnace at 500 DEG C, obtain magnesium ferrite；Electrostatic spinning experiment 25 degrees Celsius,
Elevated Temperature Conditions are 1 DEG C/min to 400 DEG C, 5 DEG C/min to 500 DEG C when carrying out, and calcining under 55 humidity.
（3）Weigh 2 mg ammonium molybdates, 19 mg thiocarbamides are well mixed, then be respectively placed in porcelain boat both ends with 100 mg magnesium ferrites,
It is put into constant-temperature tubular stove in N2Under protection, in order to which molybdenum sulfide preferably can be supported on magnesium ferrite under nitrogen flowing,
2 h are calcined at 500 DEG C, obtain MgFe2O4/MoS2, heating rate is 2 DEG C/min during calcining.
The mass ratio of the molybdenum sulfide of embodiment 2 and magnesium ferrite is 0.05
（1）Weigh 15 mmol ferric nitrates and 5 mmol magnesium nitrates are placed in 50 mL test tubes, add 2.5mL2 steaming
Distilled water and 7.5mL absolute ethyl alcohols simultaneously stir, and then add 1.3 g PVP（K90）, finally it is fully mixed must clarify it is molten
Liquid, i.e. electrostatic spinning precursor liquid.
（2）5 mL precursor liquids are drawn in glass syringe, then carry out electricity under 25 KV by electrostatic spinning apparatus
Spin, then collect product, and calcined at 500 DEG C by Muffle furnace, obtain magnesium ferrite, electrostatic spinning experiment 25 degrees Celsius,
Elevated Temperature Conditions are 1 DEG C/min to 400 DEG C, 5 DEG C/min to 500 DEG C when carrying out, and calcining under 55 humidity.
（3）Weigh 5 mg ammonium molybdates, 47.5 mg thiocarbamides are well mixed, then be respectively placed in porcelain boat two with 100 mg magnesium ferrites
End, is put into constant-temperature tubular stove in N2Under protection, in order to which molybdenum sulfide preferably can be supported on magnesium ferrite under nitrogen flowing,
2 h are calcined at 500 DEG C, obtain MgFe2O4/MoS2, heating rate is 2 DEG C/min during calcining.
The mass ratio of the molybdenum sulfide of embodiment 3 and magnesium ferrite is 0.1
（1）Weigh 15 mmol ferric nitrates and 5 mmol magnesium nitrates are placed in 50 mL test tubes, add 2.5mL2 steaming
Distilled water and 7.5mL absolute ethyl alcohols simultaneously stir, and then add 1.3 g PVP（K90）, finally it is fully mixed must clarify it is molten
Liquid, i.e. electrostatic spinning precursor liquid.
（2）5 mL precursor liquids are drawn in glass syringe, then carry out electricity under 25 KV by electrostatic spinning apparatus
Spin, then collect product, and calcined at 500 DEG C by Muffle furnace, obtain magnesium ferrite, electrostatic spinning experiment 25 degrees Celsius,
Elevated Temperature Conditions are 1 DEG C/min to 400 DEG C, 5 DEG C/min to 500 DEG C when carrying out, and calcining under 55 humidity.
（3）Weigh 10 mg ammonium molybdates, 95 mg thiocarbamides are well mixed, then be respectively placed in porcelain boat two with 100 mg magnesium ferrites
End, is put into constant-temperature tubular stove in N2Under protection, in order to which molybdenum sulfide preferably can be supported on magnesium ferrite under nitrogen flowing,
2 h are calcined at 500 DEG C, obtain MgFe2O4/MoS2.Heating rate is 2 DEG C/min during calcining.
The mass ratio of the molybdenum sulfide of embodiment 4 and magnesium ferrite is 0.2
（1）Weigh 15 mmol ferric nitrates and 5 mmol magnesium nitrates are placed in 50 mL test tubes, add 2.5mL2 steaming
Distilled water and 7.5mL absolute ethyl alcohols simultaneously stir, and then add 1.3 g PVP（K90）, finally it is fully mixed must clarify it is molten
Liquid, i.e. electrostatic spinning precursor liquid.
（2）5 mL precursor liquids are drawn in glass syringe, then carry out electricity under 25 KV by electrostatic spinning apparatus
Spin, then collect product, and calcined at 500 DEG C by Muffle furnace, obtain magnesium ferrite, electrostatic spinning experiment 25 degrees Celsius,
Elevated Temperature Conditions are 1 DEG C/min to 400 DEG C, 5 DEG C/min to 500 DEG C when carrying out, and calcining under 55 humidity.
（3）Weigh 20 mg ammonium molybdates, 190 mg thiocarbamides are well mixed, then be respectively placed in porcelain boat two with 100 mg magnesium ferrites
End, is put into constant-temperature tubular stove in N2Under protection, in order to which molybdenum sulfide preferably can be supported on magnesium ferrite under nitrogen flowing,
2 h are calcined at 500 DEG C, obtain MgFe2O4/MoS2, heating rate is 2 DEG C/min during calcining.
The mass ratio of the molybdenum sulfide of embodiment 5 and magnesium ferrite is 0.3
（1）Weigh 15 mmol ferric nitrates and 5 mmol magnesium nitrates are placed in 50 mL test tubes, add 2.5mL2 steaming
Distilled water and 7.5mL absolute ethyl alcohols simultaneously stir, and then add 1.3 g PVP（K90）, finally it is fully mixed must clarify it is molten
Liquid, i.e. electrostatic spinning precursor liquid.
（2）5 mL precursor liquids are drawn in glass syringe, then carry out electricity under 25 KV by electrostatic spinning apparatus
Spin, then collect product, and calcined at 500 DEG C by Muffle furnace, obtain magnesium ferrite, electrostatic spinning experiment 25 degrees Celsius,
Elevated Temperature Conditions are 1 DEG C/min to 400 DEG C, 5 DEG C/min to 500 DEG C when carrying out, and calcining under 55 humidity.
（3）Weigh 30 mg ammonium molybdates, 285mg thiocarbamides are well mixed, then be respectively placed in porcelain boat two with 100 mg magnesium ferrites
End, is put into constant-temperature tubular stove in N2Under protection, in order to which molybdenum sulfide preferably can be supported on magnesium ferrite under nitrogen flowing,
2 h are calcined at 500 DEG C, obtain MgFe2O4/MoS2, heating rate is 2 DEG C/min during calcining.
MgFe in the present invention2O4/MoS2The composition of heterojunction nano-wire by x-ray photoelectron spectroscopy (XPS) determine,
Occurs Mg, Fe, O, Mo and S characteristic peak in XPS；And meet MgFe2O4、MoS2Energy spectral position, so as to preliminary proof
MgFe2O4/MoS2The synthesis of heterojunction nano-wire.
And what field emission scanning electron microscope (SEM) test showed to be apparent from from figure finds out that molybdenum sulfide is combined with magnesium ferrite
Together.And the MgFe prepared by vapour deposition method2O4/MoS2Heterojunction nano-wire diameter is 50nm or so.
Then transmission electron microscope is passed through（TEM）It can further prove to be grown in MgFe with lattice fringe2O4Surface is
MoS2, this can further prove MgFe2O4/MoS2The formation of heterojunction nano-wire.
Prepared by can be seen that from the photoelectric catalysis degrading efficiency schematic diagram of magnesium ferrite and magnesium ferrite/molybdenum disulfide
The degradation efficiency of magnesium ferrite/molybdenum disulfide is higher than the magnesium ferrite of pure sample；And the degradation efficiency of magnesium ferrite/molybdenum disulfide is first
Increase and reduce again, its best sample is magnesium ferrite/molybdenum disulfide (ω=10%), i.e., the mass ratio of molybdenum sulfide and magnesium ferrite is 0.1
When；When magnesium ferrite and magnesium ferrite/molybdenum disulfide (ω=10%) are used for producing hydrogen, hydrogen generation efficiency reaches 5.8 mmol/h m2It is higher than
3.5 mmol/h m of magnesium ferrite2。
The present invention is to add different amounts of nine water ferric nitrate and magnesium nitrate hexahydrate by controlling so as to obtain simple substance magnesium ferrite,
Then the different molybdenum sulfide particle of magnesium ferrite surface deposition density, the sample prepared by it are made at different temperatures by vapour deposition method again
Product MgFe2O4/MoS2The performance of hetero-junctions has differences, and then seeks its optimal concentration ratio by probing into for its performance.
Claims (6)
- A kind of 1. synthetic method of magnesium ferrite/molybdenum sulfide heterojunction nano-wire, it is characterised in that：Weigh magnesium ferrite, ammonium molybdate and After thiocarbamide, ammonium molybdate and thiocarbamide are well mixed and magnesium ferrite is respectively placed in porcelain boat both ends, is put into tube furnace in N2Under protection, rise Temperature the h of constant temperature 2, obtains MgFe to 500 DEG C2O4/MoS2；The mass ratio of the molybdenum sulfide and magnesium ferrite is 0.02-0.3：1；Rise Warm speed is 2 DEG C/min.
- A kind of 2. synthetic method of magnesium ferrite/molybdenum sulfide heterojunction nano-wire as claimed in claim 1, it is characterised in that：Institute The mass ratio for stating molybdenum sulfide and magnesium ferrite is 0.1：1.
- 3. the synthetic method of a kind of magnesium ferrite/molybdenum sulfide heterojunction nano-wire as claimed in claim 1, it is characterised in that described The preparation method of magnesium ferrite is as follows：（1）Weigh nine water ferric nitrates and magnesium nitrate hexahydrate is placed in test tube, add solvent, stir and add PVP K90, finally It is fully mixed to obtain to settled solution, i.e. electrostatic spinning precursor liquid；（2）Precursor liquid is drawn, electrospinning is then carried out by electrostatic spinning apparatus, then collects product, and is calcined by Muffle furnace, Obtain magnesium ferrite.
- A kind of 4. synthetic method of magnesium ferrite/molybdenum sulfide heterojunction nano-wire as claimed in claim 3, it is characterised in that：Step Suddenly（1）In the mol ratio of nine water ferric nitrates and magnesium nitrate hexahydrate be 3:1, the solvent is the water of absolute ethyl alcohol and 2 distilled water Solution, wherein the volume ratio of 2 distilled water and absolute ethyl alcohol is 1:3, magnesium nitrate hexahydrate and PVP molal weight ratio are 1mmol: 0.26g。
- A kind of 5. synthetic method of magnesium ferrite/molybdenum sulfide heterojunction nano-wire as claimed in claim 3, it is characterised in that：Step Suddenly（2）In, described to carry out electrospinning by electrostatic spinning apparatus be that electrospinning is carried out under 25 KV, and under 25 degrees Celsius, 55 humidity Carry out；And it is that Elevated Temperature Conditions are 1 DEG C/min to 400 DEG C, 5 DEG C/min to 500 DEG C, then calcined to calcine.
- 6. magnesium ferrite/molybdenum sulfide heterojunction nano-wire prepared by method as claimed in claim 1 reacts for photoelectrochemical degradation With the purposes of production hydrogen reaction.
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