CN108404938A - A kind of electrocatalytic hydrogen evolution MoS2Nano flower sphere catalyst and preparation method thereof - Google Patents
A kind of electrocatalytic hydrogen evolution MoS2Nano flower sphere catalyst and preparation method thereof Download PDFInfo
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 65
- 239000001257 hydrogen Substances 0.000 title claims abstract description 65
- 239000003054 catalyst Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002057 nanoflower Substances 0.000 claims abstract description 46
- 239000002096 quantum dot Substances 0.000 claims abstract description 40
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 36
- 239000010703 silicon Substances 0.000 claims abstract description 36
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 23
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 23
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 230000033228 biological regulation Effects 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 33
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 22
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 22
- 229960005055 sodium ascorbate Drugs 0.000 claims description 22
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 235000015393 sodium molybdate Nutrition 0.000 claims description 13
- 239000011684 sodium molybdate Substances 0.000 claims description 11
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 8
- 238000000502 dialysis Methods 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 5
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- -1 CS are pressed2 Chemical compound 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 9
- 239000003929 acidic solution Substances 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 description 16
- 230000010287 polarization Effects 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000005611 electricity Effects 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 150000002171 ethylene diamines Chemical class 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 150000004780 naphthols Chemical class 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000000711 polarimetry Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 235000019187 sodium-L-ascorbate Nutrition 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/33—
-
- B01J35/51—
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
A kind of electrocatalytic hydrogen evolution MoS2Nano flower sphere catalyst and preparation method thereof, the present invention relates to electrocatalytic hydrogen evolution catalyst and preparation method thereof.The present invention is to solve existing electro-catalysis reduction catalyst for preparing hydrogen technical problems of high cost.The electrocatalytic hydrogen evolution MoS of the present invention2Nano flower sphere catalyst is the stratiform MoS adulterated with silicon quantum dot2The nano flower spheroidal material of composition.Preparation method：One, hydrothermal synthesis silicon quantum dot；Two, CS2Spherical MoS is synthesized with the regulation and control of Si quantum dots2.The electrocatalytic hydrogen evolution MoS of the present invention2Nano flower sphere catalyst is 10mA.cm in current density‑2When, overpotential 212mV, while Tafel slope only has 70mVdecade‑1, and have good stability in an acidic solution, it can be used in electrocatalytic hydrogen evolution.
Description
Technical field
The present invention relates to electrocatalytic hydrogen evolution catalyst and preparation method thereof.
Background technology
World today's energy crisis and environmental problem are increasingly severe, therefore clean reproducible energy receives great pass
Note.Generally solar energy, wind energy and a series of regenerative resource of biomass energy can be converted into the form of electricity.In order to answer
To i.e. by the exhausted energy, electric energy needs are stored by lasting, and it is numerous then to be stored in the form of Hydrogen Energy later
The solution being most concerned by people inside energy storage scheme.The acquisition of Hydrogen Energy can use most basic mode, that is, electrolysis water, electricity
Solution moisture is oxygen evolution reaction (OER) and evolving hydrogen reaction (HER).Elctro-catalyst is greatly facilitated in electro-catalysis in the demand of clean energy resource
Restore the application prospect of hydrogen manufacturing.Two can be substantially divided into according to the source of electric energy by preparing the sustainable Hydrogen Energy of cleaning by electric energy
Class, first, electro-catalysis water decomposition, is used as energy source by solar cell, wind energy, hydroelectric generation and decomposes water；Second is that photocatalysis
Water decomposition generates electron hole pair directly from sun light absorption energy.And the principal element for influencing photocatalysis and electro-catalysis is to urge
The activity of agent.
Electro-catalysis reduction hydrogen manufacturing is a kind of efficiently large-scale hydrogen production process, and the catalyst of electro-catalysis reduction hydrogen manufacturing is generally
Noble metal catalyst, such as Pt have good catalytic effect, but since it is scarce resource, expensive, limit its
Using.
Invention content
The present invention is to solve existing electro-catalysis reduction catalyst for preparing hydrogen technical problems of high cost, and provide curing
The electrocatalytic hydrogen evolution MoS of carbon and the double regulation and control synthesis of silicon quantum dot2Nano flower sphere catalyst and preparation method thereof.
The electrocatalytic hydrogen evolution MoS of the present invention2Nano flower sphere catalyst is the stratiform MoS adulterated with silicon quantum dot2It constitutes
Nano flower spheroidal material.
The electrocatalytic hydrogen evolution MoS of the present invention2The preparation method of nano flower sphere catalyst carries out according to the following steps：
One, hydrothermal synthesis silicon quantum dot：
(1) a concentration of 0.005g~0.006g/mL for pressing sodium ascorbate, water deionized water is added to by sodium ascorbate
In be uniformly mixed, be then allowed to stand, obtain sodium ascorbate solution；
(2) sodium ascorbate solution is pressed, the volume ratio of trimethyoxysilane is (1.2~1.3): 1: the ratio of (20~25)
Example, sodium ascorbate solution is added in trimethyoxysilane, deionized water is added, is configured to mixed solution；
(3) mixed solution is poured into hydrothermal reaction kettle, is heated to 200~220 DEG C, kept 12~14h, obtain silicon quantum
Solution is put, then after dialysis, the silicon quantum dot solution purified；
Two, CS2Spherical MoS is synthesized with the regulation and control of Si quantum dots2：
(1) sodium molybdate, CS are pressed2, ethylenediamine, water molar ratio be 1: (15~17): (3~4): (700~900), by molybdenum
Sour sodium, CS2, ethylenediamine be added to the water, 20~30min of ultrasonic disperse obtains mixed liquor；
(2) it is 1 in the molar ratio of silicon quantum dot and sodium molybdate: the ratio of (35~60), by the silicon quantum dot solution of purifying
It is added in mixed liquor, 20~30min of ultrasonic disperse obtains precursor liquid；
(3) precursor liquid is poured into hydrothermal reaction kettle, 20~28h is reacted under conditions of temperature is 195~210 DEG C, from
After so cooling, deposit is collected, with ethyl alcohol and deionized water washes clean, then is freeze-dried, obtains electrocatalytic hydrogen evolution MoS2It receives
Popped rice sphere catalyst.
The present invention uses flexible subserate sulphur source CS2, pass through CS2With the common regulation and control of silicon quantum dot, having synthesized has special form
Looks MoS2Nanometer bouquet, composition principle figure is as shown in Figure 1, this nanometer flower ball-shaped MoS2Large specific surface area, and surface have it is rich
Rich sheet MoS2, abundant active site is provided for electrocatalytic hydrogen evolution, the presence of silicon quantum dot expands MoS2Interlamellar spacing
From changing its phase, reduce its band gap, enhance electric conductivity, change MoS2Band structure, have good electricity
Catalytic performance is 10mAcm in current density-2When, overpotential 212mV greatly reduces overpotential, while Ta Feier
Slope only has 70mVdecade-1, and have good stability in an acidic solution, be that a kind of good electrocatalytic hydrogen evolution is urged
Agent.
Description of the drawings
Fig. 1 is the MoS of the present invention2Nanometer bouquet composition principle figure；
Fig. 2 is to test the 1 electrocatalytic hydrogen evolution MoS prepared2The photo of nano flower sphere catalyst；
Fig. 3 is to test the 1 electrocatalytic hydrogen evolution MoS prepared2The stereoscan photograph of nano flower sphere catalyst；
Fig. 4 is to test the 1 electrocatalytic hydrogen evolution MoS prepared2The powerful stereoscan photograph of nano flower sphere catalyst；
Fig. 5 is to test the 1 electrocatalytic hydrogen evolution MoS prepared2The polarization curve of nano flower sphere catalyst；
Fig. 6 is to test the 1 electrocatalytic hydrogen evolution MoS prepared2The Tafel curve of nano flower sphere catalyst；
Fig. 7 is to test the 2 electrocatalytic hydrogen evolution MoS prepared2The stereoscan photograph of nano flower sphere catalyst；
Fig. 8 is to test the 2 electrocatalytic hydrogen evolution MoS prepared2The powerful stereoscan photograph of nano flower sphere catalyst；
Fig. 9 is to test the 2 electrocatalytic hydrogen evolution MoS prepared2The polarization curve of nano flower sphere catalyst；
Figure 10 is to test the 2 electrocatalytic hydrogen evolution MoS prepared2The Tafel curve of nano flower sphere catalyst.
Specific implementation mode
Specific implementation mode one：The electrocatalytic hydrogen evolution MoS of present embodiment2Nano flower sphere catalyst is with silicon quantum dot
The stratiform MoS of doping2The nano flower ball material of composition.
Specific implementation mode two：Electrocatalytic hydrogen evolution MoS described in specific implementation mode one2The preparation of nano flower sphere catalyst
Method carries out according to the following steps：
One, hydrothermal synthesis silicon quantum dot：
(1) a concentration of 0.005g~0.006g/mL for pressing sodium ascorbate, water deionized water is added to by sodium ascorbate
In be uniformly mixed, be then allowed to stand, obtain sodium ascorbate solution；
(2) sodium ascorbate solution is pressed, the volume ratio of trimethyoxysilane is (1.2~1.3)：1：The ratio of (20~25)
Example, sodium ascorbate solution is added in trimethyoxysilane, deionized water is added, is configured to mixed solution；
(3) mixed solution is poured into hydrothermal reaction kettle, is heated to 200~220 DEG C, kept 12~14h, obtain silicon quantum
Solution is put, then after dialysis, the silicon quantum dot solution purified；
Two, CS2Spherical MoS is synthesized with the regulation and control of Si quantum dots2：
(1) sodium molybdate, CS are pressed2, ethylenediamine, water molar ratio be 1: (15~17): (3~4): (700~900), by molybdenum
Sour sodium, CS2, ethylenediamine be added to the water, 20~30min of ultrasonic disperse obtains mixed liquor；
(2) it is 1 in the molar ratio of silicon quantum dot and sodium molybdate: the ratio of (35~60), by the silicon quantum dot solution of purifying
It is added in mixed liquor, 20~30min of ultrasonic disperse obtains precursor liquid；
(3) precursor liquid is poured into hydrothermal reaction kettle, 20~28h is reacted under conditions of temperature is 195~210 DEG C, from
After so cooling, deposit is collected, with ethyl alcohol and deionized water washes clean, then is freeze-dried, obtains electrocatalytic hydrogen evolution MoS2It receives
Popped rice sphere catalyst.
Specific implementation mode three：Present embodiment and time of repose in step 1 (1) unlike specific implementation mode two
For 20~30min.It is other to be identical with embodiment two.
Present embodiment keeps reducing agent sodium ascorbate more stable by standing, and keeps the silicon quantum dot that subsequent step obtains equal
One, stablize.
Specific implementation mode four：Present embodiment is unlike specific implementation mode two or three described in step 1 (3)
Dialysis refer to that silicon quantum dot solution is added in plate bag, be immersed in deionized water, change water daily 4 times, impregnate 2 days.
It is other identical as specific implementation mode two or three.
Specific implementation mode five：In step 2 (1) unlike one of present embodiment and specific implementation mode two to four
The sodium molybdate, CS2, ethylenediamine, water molar ratio be 1: 16: 3.5: 800.One of other and specific implementation mode two to four
It is identical.
Specific implementation mode six：In step 2 (2) unlike one of present embodiment and specific implementation mode two to five
The molar ratio of the silicon quantum dot and sodium molybdate is 1: 40.It is other identical as one of specific implementation mode two to five.
Specific implementation mode seven：In step 2 (3) unlike one of present embodiment and specific implementation mode two to six
The reaction temperature is reacted for 24 hours under conditions of being 200 DEG C.It is other identical as one of specific implementation mode two to six.
With following verification experimental verification beneficial effects of the present invention：
Experiment 1：The electrocatalytic hydrogen evolution MoS of this experiment2The preparation method of nano flower sphere catalyst carries out according to the following steps：
One, hydrothermal synthesis silicon quantum dot：
(1) 0.0594g sodium ascorbates are added in 10mL deionized waters, are uniformly mixed, are then allowed to stand 20min, led to
Crossing standing keeps reducing agent sodium ascorbate more stable, obtains sodium ascorbate solution；
(2) 1.25ml sodium ascorbate solutions are added in 1mL trimethyoxysilanes, add 20ml deionizations
Water is configured to mixed solution；
(3) mixed solution is poured into hydrothermal reaction kettle, is heated to 200 DEG C, kept 12h, obtain silicon quantum dot solution；With
Deionized water dialysis, changes water 4 times daily, impregnates 2 days, is purified, the silicon quantum dot solution purified；
Two, CS2Spherical MoS is synthesized with the regulation and control of Si quantum dots2：
(1) by 1.2mmol sodium molybdates, 1.2mL CS2, 1.2mL ethylenediamines be added in 15mL deionized waters, ultrasonic disperse
20min obtains mixed liquor；
(2) solution of the silicon quantum dot purified containing 0.030mmol is added in mixed liquor, ultrasonic disperse 20min is obtained
Precursor liquid；
(3) precursor liquid is poured into hydrothermal reaction kettle, is reacted for 24 hours under conditions of temperature is 200 DEG C, after natural cooling,
Black deposit is collected, with ethyl alcohol and deionized water washes clean, then 12h is freeze-dried under conditions of -50 DEG C, obtains electricity and urge
Change liberation of hydrogen MoS2Nano flower sphere catalyst.
The electrocatalytic hydrogen evolution MoS that this experiment obtains2Nano flower sphere catalyst is the powder of black, and photo is as indicated with 2.This
Test obtained electrocatalytic hydrogen evolution MoS2The stereoscan photograph of nano flower sphere catalyst is as shown in figure 3, as can be seen from Figure 3
MoS2The inside of nanometer bouquet is by loose MoS2Nanometer sheet is constituted, and the outer surface of ball grows loose small pieces MoS2, such
Loose multi-sheet structure makes it with great specific surface area, exposes many active sites, is conducive to electrocatalytic hydrogen evolution,
MoS2The outer diameter of nanometer bouquet is 200nm~800nm.
Electrocatalytic hydrogen evolution MoS prepared by this experiment2Nano flower sphere catalyst sample is ground into fine powder, then weighs 5mg
Sample, is added 20uL naphthols, the isopropanol of 980uL, and ultrasonic 30min obtains dispersion liquid；20uL dispersant liquid drops are drawn to a diameter of
On the glass-carbon electrode of 3mm, drying, as working electrode；At room temperature with CHI660e electrochemical workstation standard three electrodes system
Electrocatalysis characteristic test is carried out, Ag/AgCl electrodes are used as reference electrode, carbon-point to electrode, are coated with the glass-carbon electrode of sample
As working electrode, it is 0~-0.6V, scanning voltage 5mV/s that electrolyte, which uses the sulfuric acid of 0.5mol/L, setting voltage range, is surveyed
Its polarization curve and catalytic stability are tried, all results of test are all demarcated with standard hydrogen electrode potential (RHE), obtained
The polarization curve arrived is as shown in figure 5, from fig. 5, it can be seen that electrocatalytic hydrogen evolution MoS prepared by this experiment2Nano flower sphere catalyst
In 10mA.cm-2Corresponding overpotential is 212mV under current density, has good electro-catalysis effect.
Electrocatalytic hydrogen evolution MoS prepared by experiment 12The Tafel curve of nano flower sphere catalyst is as shown in Figure 6.It can from Fig. 6
To find out, the electrocatalytic hydrogen evolution MoS of this experiment preparation2The Tafel slope of nano flower sphere catalyst is 70mVdecade-1。
Electrocatalytic hydrogen evolution MoS prepared by experiment 12Nano flower sphere catalyst is 0~-0.6V, sweep speed in voltage range
For 100mVs-1Under conditions of CV cycle 1000 circle after, continue polarimetry curve, performance consistent with original polarization curve
Do not weaken, illustrates that the catalyst has good stability in acid solution.
Experiment 2：The electrocatalytic hydrogen evolution MoS of this experiment2The preparation method of nano flower sphere catalyst carries out according to the following steps：
One, hydrothermal synthesis silicon quantum dot：
(1) 0.0594g sodium ascorbates are added in 10ml deionized waters, are uniformly mixed, are then allowed to stand 20min, led to
Crossing standing keeps reducing agent sodium ascorbate more stable, obtains sodium ascorbate solution；
(2) 1.25ml sodium ascorbate solutions are added in 1ml trimethyoxysilanes, add 20ml deionizations
Water is configured to mixed solution；
(3) mixed solution is poured into hydrothermal reaction kettle, is heated to 200 DEG C, kept 12h, obtain silicon quantum dot solution；With
Deionized water dialysis, changes water 4 times daily, impregnates 2 days, is purified, the silicon quantum dot solution purified；
Two, CS2Spherical MoS is synthesized with the regulation and control of Si quantum dots2：
(1) by 1.2mmol sodium molybdates, 1.2ml CS2, 1.2ml ethylenediamines be added in 15ml deionized waters, ultrasonic disperse
20min obtains mixed liquor；
(2) solution of the silicon quantum dot purified containing 0.040mmol is added in mixed liquor, ultrasonic disperse 20min is obtained
Precursor liquid；
(3) precursor liquid is poured into hydrothermal reaction kettle, reacts 26h under conditions of temperature is 210 DEG C, after natural cooling,
Black deposit is collected, with ethyl alcohol and deionized water washes clean, then 12h is freeze-dried under conditions of -50 DEG C, obtains electricity and urge
Change liberation of hydrogen MoS2Nano flower sphere catalyst.
The electrocatalytic hydrogen evolution MoS that this experiment obtains2The stereoscan photograph of nano flower sphere catalyst is as shown in Figure 7 and Figure 8,
From Fig. 7 and 8 as can be seen that prepared MoS2The inside of nanometer bouquet is by loose MoS2Nanometer sheet is constituted, and the appearance of ball is looked unfamiliar
Have loose small pieces MoS2, such loose multi-sheet structure makes it with great specific surface area, exposes many urge
Change active site, is conducive to electrocatalytic hydrogen evolution, MoS2The outer diameter of nanometer bouquet is 200~800nm.
Electrocatalytic hydrogen evolution MoS prepared by this experiment2Nano flower sphere catalyst sample is ground into fine powder, then weighs 5mg
Sample, is added 20uL naphthols, the isopropanol of 980uL, and ultrasonic 30min obtains dispersion liquid；20uL dispersant liquid drops are drawn to a diameter of
On the glass-carbon electrode of 3mm, drying, as working electrode；At room temperature with CHI660e electrochemical workstation standard three electrodes system
Electrocatalysis characteristic test is carried out, Ag/AgCl electrodes are used as reference electrode, carbon-point to electrode, are coated with the glass-carbon electrode of sample
As working electrode, it is 0~-0.6V, scanning voltage 5mV/s that electrolyte, which uses the sulfuric acid of 0.5mol/L, setting voltage range, is surveyed
Its polarization curve and catalytic stability are tried, all results of test are all demarcated with standard hydrogen electrode potential (RHE), obtained
The polarization curve arrived is as shown in figure 9, from fig. 9, it can be seen that electrocatalytic hydrogen evolution MoS prepared by this experiment2Nano flower sphere catalyst
In 10mA.cm-2Corresponding overpotential is 220mV under current density, has good electro-catalysis effect.
Electrocatalytic hydrogen evolution MoS prepared by experiment 22The Tafel curve of nano flower sphere catalyst is as shown in Figure 10.From Figure 10
As can be seen that electrocatalytic hydrogen evolution MoS prepared by this experiment2The Tafel slope of nano flower sphere catalyst is 73mVdecade-1。
Electrocatalytic hydrogen evolution MoS prepared by experiment 22Nano flower sphere catalyst stability in acid solution is good, in voltage range
For 0~-0.6V, sweep speed 100mVs-1Under conditions of after 1000 circle of CV cycles, continue polarimetry curve, and it is original
Polarization curve it is consistent, performance does not weaken.
Claims (7)
1. a kind of electrocatalytic hydrogen evolution MoS2Nano flower sphere catalyst, it is characterised in that the catalyst is the layer adulterated with silicon quantum dot
Shape MoS2The nano flower ball material of composition.
2. a kind of electrocatalytic hydrogen evolution MoS2The preparation method of nano flower sphere catalyst, it is characterised in that this method according to the following steps into
Row：
One, hydrothermal synthesis silicon quantum dot：
(1) a concentration of 0.005g~0.006g/mL for pressing sodium ascorbate, sodium ascorbate is added in water deionized water and is mixed
It closes uniformly, is then allowed to stand, obtains sodium ascorbate solution；
(2) it is (1.2~1.3) in the volume ratio of sodium ascorbate solution, trimethyoxysilane: 1: the ratio of (20~25),
Sodium ascorbate solution is added in trimethyoxysilane, deionized water is added, is configured to mixed solution；
(3) mixed solution is poured into hydrothermal reaction kettle, is heated to 200~220 DEG C, kept 12~14h, it is molten to obtain silicon quantum dot
Liquid, then after dialysis, the silicon quantum dot solution purified；
Two, CS2Spherical MoS is synthesized with the regulation and control of Si quantum dots2：
(1) sodium molybdate, CS are pressed2, ethylenediamine, water molar ratio be 1: (15~17): (3~4): (700~900), by sodium molybdate,
CS2, ethylenediamine be added to the water, 20~30min of ultrasonic disperse obtains mixed liquor；
(2) it is 1 in the molar ratio of silicon quantum dot and sodium molybdate: the silicon quantum dot solution of purifying is added the ratio of (35~60)
Into mixed liquor, 20~30min of ultrasonic disperse obtains precursor liquid；
(3) precursor liquid is poured into hydrothermal reaction kettle, 20~28h is reacted under conditions of temperature is 195~210 DEG C, it is naturally cold
But after, deposit is collected, with ethyl alcohol and deionized water washes clean, then is freeze-dried, obtains electrocatalytic hydrogen evolution MoS2Nano flower
Sphere catalyst.
3. a kind of electrocatalytic hydrogen evolution MoS according to claim 22The preparation method of nano flower sphere catalyst, it is characterised in that
Time of repose is 20~30min in step 1 (1).
4. a kind of electrocatalytic hydrogen evolution MoS according to claim 2 or 32The preparation method of nano flower sphere catalyst, feature
It is that the dialysis described in step 1 (3) refers to that silicon quantum dot solution is added in plate bag, is immersed in deionized water, often
It changes water 4 times, impregnates 2 days.
5. a kind of electrocatalytic hydrogen evolution MoS according to claim 2 or 32The preparation method of nano flower sphere catalyst, feature
It is sodium molybdate, CS described in step 2 (1)2, ethylenediamine, water molar ratio be 1: 16: 3.5: 800.
6. a kind of electrocatalytic hydrogen evolution MoS according to claim 2 or 32The preparation method of nano flower sphere catalyst, feature
It is that the molar ratio of the silicon quantum dot and sodium molybdate described in step 2 (2) is 1: 40.
7. a kind of electrocatalytic hydrogen evolution MoS according to claim 2 or 32The preparation method of nano flower sphere catalyst, feature
It is to react for 24 hours under conditions of the reaction temperature described in step 2 (3) is 200 DEG C.
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| CN112316965A (en) * | 2020-09-30 | 2021-02-05 | 江苏大学 | Preparation method and application of composite material derived by loading molybdenum disulfide nanosheet based on laccase-copper phosphate nanoflowers as substrate |
| CN112844421A (en) * | 2021-01-18 | 2021-05-28 | 厦门大学 | MoS (MoS) enhanced by utilizing plasma2Method for electrocatalytic and/or photoelectrocatalytic properties |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111298833A (en) * | 2020-03-05 | 2020-06-19 | 安徽理工大学 | MoS based on carbazole functionalization2Quantum dot, preparation method and application |
| CN111298833B (en) * | 2020-03-05 | 2023-05-05 | 安徽理工大学 | MoS based on carbazole functionalization 2 Quantum dot, preparation method and application |
| CN112316965A (en) * | 2020-09-30 | 2021-02-05 | 江苏大学 | Preparation method and application of composite material derived by loading molybdenum disulfide nanosheet based on laccase-copper phosphate nanoflowers as substrate |
| CN112316965B (en) * | 2020-09-30 | 2022-10-28 | 江苏大学 | Preparation method and application of composite material derived by loading molybdenum disulfide nanosheet based on laccase-copper phosphate nanoflowers as substrate |
| CN112844421A (en) * | 2021-01-18 | 2021-05-28 | 厦门大学 | MoS (MoS) enhanced by utilizing plasma2Method for electrocatalytic and/or photoelectrocatalytic properties |
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