CN108014820A - A kind of molybdenum disulfide elctro-catalyst with nanometer multilayer membrane structure and preparation method thereof - Google Patents
A kind of molybdenum disulfide elctro-catalyst with nanometer multilayer membrane structure and preparation method thereof Download PDFInfo
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 49
- 239000003054 catalyst Substances 0.000 title claims abstract description 38
- 239000012528 membrane Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000758 substrate Substances 0.000 claims abstract description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- 238000000137 annealing Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 claims abstract description 5
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 8
- 238000007654 immersion Methods 0.000 claims description 4
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 4
- -1 oxometallate Chemical compound 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 230000005622 photoelectricity Effects 0.000 claims 1
- 230000001953 sensory effect Effects 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 239000010410 layer Substances 0.000 description 23
- GFLJTEHFZZNCTR-UHFFFAOYSA-N 3-prop-2-enoyloxypropyl prop-2-enoate Chemical compound C=CC(=O)OCCCOC(=O)C=C GFLJTEHFZZNCTR-UHFFFAOYSA-N 0.000 description 7
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 description 7
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000012467 final product Substances 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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- B01J35/33—
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- B01J35/39—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
- B01J37/0228—Coating in several steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- 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
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- 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
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- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The present invention relates to a kind of molybdenum disulfide elctro-catalyst with nanometer multilayer membrane structure and preparation method thereof, the described method includes 1）Diallyl dimethyl ammoniumchloride is dissolved in the water solution a is made；2）Polyoxometallate is dissolved in the water solution b is made；3）Individual layer molybdenum disulfide is dissolved in stable solution c is made in N ~ methyl pyrrolidone；4）Conductive substrates are immersed in corresponding solution successively according to the order of a, b, a, c, is all washed with deionized water totally after conductive substrates are often taken out from a kind of solution, is then dried up with nitrogen, obtain the conductive substrates with multilayer film；5）By step 4）In the conductive substrates with multilayer film that prepare make annealing treatment under nitrogen protection, up to having the molybdenum disulfide elctro-catalyst of nanometer multilayer membrane structure.The problem of catalyst that the present invention is prepared using membrane method has new nanometer multilayer membrane structure, overcomes molybdenum disulfide its electro-catalysis efficiency of conductivity lower limit between layers well.
Description
Technical field
The invention belongs to new energy field, and in particular to a kind of molybdenum disulfide elctro-catalyst with nanometer multilayer membrane structure
And preparation method thereof.
Background technology
Individual layer molybdenum disulfide be widely used in excellent greasy property and catalytic field-effect transistor, sensor,
In the field such as battery electrode and optics, it is found that before individual layer molybdenum disulfide, field uses mono-layer graphite always
Alkene, nevertheless, but since graphene does not have band gap, cause the application of graphene to be restricted, with individual layer molybdenum disulfide
Discovery and preparation, overcome the above problem well, can be fine because the band gap of individual layer molybdenum disulfide has reached 1.8eV
Ground makes up the deficiency of zero band gap of single-layer graphene.
Hydrogen Energy is one of following most promising clean energy resource, and individual layer molybdenum disulfide can be used for as a kind of catalyst
Decompose hydrone and obtain hydrogen, however, the elctro-catalyst of electro-catalysis splitting water need to be provided simultaneously with conductivity height and catalytic activity point
More advantages, research show：The molybdenum disulfide of individual layer has more rich edge, so as to there is more active site, but layer with
Conductivity between layer is low to again limit further improving for its electro-catalysis efficiency, in order to improve conductivity, can use two
The molybdenum sulfide material highly conductive with metallic particles, graphene etc. is for composite, but the structure of this mixing is unfavorable for research receives
The other relation be- tween structure and properties of meter level.
To sum up, existing individual layer molybdenum disulfide during being used as catalyst still have problems, it is necessary to
Continue to study, explore, improve, for this reason, there is an urgent need for a kind of enhancing individual layer molybdenum disulfide electrocatalysis characteristic that can overcome the above problem
Catalyst and preparation method thereof.
The content of the invention
For above-mentioned deficiency of the prior art, the present invention is intended to provide a kind of curing with nanometer multilayer membrane structure
Molybdenum elctro-catalyst and preparation method thereof, compared with prior art, cost of manufacture of the invention reduces, preparation method is simple, obtains
Catalyst electro-catalysis it is efficient；And the preparation method of the present invention is low to reaction condition requirement, industrialized production is more suitable for.
An object of the present invention is to provide a kind of molybdenum disulfide elctro-catalyst with nanometer multilayer membrane structure.
The second object of the present invention is to provide a kind of preparation of the molybdenum disulfide elctro-catalyst with nanometer multilayer membrane structure
Method.
The third object of the present invention is to provide above-mentioned molybdenum disulfide elctro-catalyst and its system with nanometer multilayer membrane structure
The application of Preparation Method.
For achieving the above object, specifically, the invention discloses following technical scheme：
First, the invention discloses a kind of molybdenum disulfide elctro-catalyst with nanometer multilayer membrane structure, the catalyst
For：On conductive substrates from bottom to top successively covered with diallyl dimethyl ammoniumchloride (PDDA), oxometallate, poly- two
The circulation multilayer film of allyl dimethyl ammonium chloride (PDDA), individual layer molybdenum disulfide.
Secondly, the invention discloses a kind of preparation method of the molybdenum disulfide elctro-catalyst with nanometer multilayer membrane structure,
Described method includes following steps：
1) diallyl dimethyl ammoniumchloride is dissolved in the water and solution a is made.
2) polyoxometallate is dissolved in the water and solution b is made.
3) individual layer molybdenum disulfide is dissolved in N~methyl pyrrolidone (NMP) and stable solution c is made.
4) conductive substrates are immersed in corresponding solution successively according to the order of a, b, a, c, are often taken out from a kind of solution
All it is washed with deionized water after conductive substrates totally, is then dried up with nitrogen, obtain the conductive substrates with multilayer film.
5) conductive substrates with multilayer film prepared in step 4) are made annealing treatment under nitrogen protection, had to obtain the final product
The molybdenum disulfide elctro-catalyst of nanometer multilayer membrane structure.
In step 1), the concentration of the solution a is：10~20mg/ml.The main function of solution a is absorption molybdenum disulfide
And polyoxometallate, molybdenum disulfide and polyoxometallate is combined securely with conductive substrates.
In step 2), the polyoxometallate includes：Phosphomolybdic acid, phosphotungstic acid etc..
In step 2), the concentration of the solution b is：5~10mg/ml.The main function of solution b is inhaled in bridging step 1)
Attached molybdenum disulfide, increases conductance.
In step 3), the concentration of the solution c is：0.1~0.3mg/ml.The main function of solution c is catalytic hydrogen evolution.
In step 4), the conductive substrates include：The stannic oxide (FTO) of fluorine doped, indium-doped stannic oxide (ITO) etc..
In step 4), the time of the immersion is 10~30 minutes.
Preferably, the time of the immersion is 20 minutes
In step 4), the thickness of film that can be as needed repeats this process.Thickness ensures maximal efficiency.
In step 5), the condition of the lower annealing of nitrogen protection is：Annealing temperature is 350~450 degree, the time 1~
3h。
Preferably, the condition of the lower annealing of the nitrogen protection is：Annealing temperature is 400 degree, time 2 h.
Finally, the invention discloses a kind of above-mentioned molybdenum disulfide elctro-catalyst and its preparation with nanometer multilayer membrane structure
The application of method, the application include being used in the fields such as photoelectrocatalysis, sensing.
The method have the characteristics that：The method for employing membrane is prepared for orderly multilayer film, specifically employ a, b,
A, the order immersion substrate of c；First, so design can increase catalytic activity point, and secondly, so design can control active site
Balance between conductance.
Compared with prior art, the present invention achieves following beneficial effect：
(1) catalyst that the present invention is prepared using membrane method has new nanometer multilayer membrane structure, and the structure is significantly
Degree improves the active site of individual layer molybdenum disulfide, can overcome molybdenum disulfide well and be limited between layers because conductivity is low
The problem of having made molybdenum disulfide electro-catalysis efficiency.
(2) active site and conductance are added, while also controls the balance of the two.
(3) manufacture craft is simple and practicable, reproducible.
Brief description of the drawings
Fig. 1 is the structure diagram of catalyst prepared by the present invention (by taking phosphomolybdic acid as an example).
Fig. 2 is the test chart of the sample current density of embodiment 1 and comparative example 1.
Embodiment
It is noted that described further below is all illustrative, it is intended to provides further instruction to the application.It is unless another
Indicate, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
As background technology is introduced, existing individual layer molybdenum disulfide is still deposited during being used as catalyst
In the problem such as conductivity is low, to solve the above-mentioned problems, the present invention provides a kind of enhancing individual layer molybdenum disulfide electrocatalysis characteristic
Catalyst and preparation method thereof；With reference to specific embodiment, the present invention is described further.
Embodiment 1：
(1) PDDA is dissolved in the water and the solution a of 20 mg/ml of concentration is made；
(2) phosphomolybdic acid is dissolved in the water and the solution b of 10 mg/ml of concentration is made；
(3) individual layer molybdenum disulfide is added to the solution c that 0.214 mg/ml of concentration is prepared into NMP；
(4) conductive substrates are immersed in corresponding solution each 20 minutes successively according to the order of a, b, a, c, often from a kind of molten
It is washed with deionized water after being taken out in liquid totally, is then dried up with nitrogen.
(5) by the multilayer film prepared under nitrogen protection, when annealing 2 is small in the environment of temperature is 400 DEG C, to obtain the final product
Molybdenum disulfide elctro-catalyst with nanometer multilayer membrane structure.
Embodiment 2：
(1) PDDA is dissolved in the water and the solution a of 10 mg/ml of concentration is made.
(2) phosphomolybdic acid is dissolved in the water and the solution b of 10 mg/ml of concentration is made.
(3) individual layer molybdenum disulfide is added to the solution c that 0.1 mg/ml of concentration is prepared into NMP.
(4) conductive substrates are immersed in corresponding solution each 15 minutes successively according to the order of a, b, a, c, often from a kind of molten
It is washed with deionized water after being taken out in liquid totally, is then dried up with nitrogen.
(5) by the multilayer film prepared under nitrogen protection, when annealing 1.5 is small in the environment of temperature is 420 DEG C, i.e.,
There must be the molybdenum disulfide elctro-catalyst of nanometer multilayer membrane structure.
Embodiment 3：
(1) PDDA is dissolved in the water and the solution a of 15 mg/ml of concentration is made；
(2) phosphotungstic acid is dissolved in the water and the solution b of 5 mg/ml of concentration is made；
(3) individual layer molybdenum disulfide is added to the solution c that 0.3 mg/ml of concentration is prepared into NMP；
(4) conductive substrates are immersed in corresponding solution each 10 minutes successively according to the order of a, b, a, c, often from a kind of molten
It is washed with deionized water after being taken out in liquid totally, is then dried up with nitrogen.
(5) by the multilayer film prepared under nitrogen protection, when annealing 3 is small in the environment of temperature is 450 DEG C, to obtain the final product
Molybdenum disulfide elctro-catalyst with nanometer multilayer membrane structure.
Embodiment 4：
(1) PDDA is dissolved in the water and the solution a of 15 mg/ml of concentration is made；
(2) phosphotungstic acid is dissolved in the water and the solution b of 5 mg/ml of concentration is made；
(3) individual layer molybdenum disulfide is added to the solution c that 0.1 mg/ml of concentration is prepared into NMP；
(4) conductive substrates are immersed in corresponding solution each 30 minutes successively according to the order of a, b, a, c, often from a kind of molten
It is washed with deionized water after being taken out in liquid totally, is then dried up with nitrogen.
(5) by the multilayer film prepared under nitrogen protection, when annealing 1 is small in the environment of temperature is 350 DEG C, to obtain the final product
Molybdenum disulfide elctro-catalyst with nanometer multilayer membrane structure.
Comparative example 1：
(1) PDDA is dissolved in the water and the solution a of 10 mg/ml of concentration is made.
(2) individual layer molybdenum disulfide is added to the solution c that 0.1 mg/ml of concentration is prepared into NMP.
(3) conductive substrates are immersed in corresponding solution each 15 minutes successively according to the order of a, c, often from a kind of solution
It is washed with deionized water after taking-up totally, is then dried up with nitrogen.
(4) by the multilayer film prepared under nitrogen protection, when annealing 1.5 is small in the environment of temperature is 420 DEG C, i.e.,
There must be the molybdenum disulfide elctro-catalyst of nanometer multilayer membrane structure.
The performance of the two kinds of catalyst samples prepared to embodiment 1 with comparative example 1 is tested, and the results are shown in Figure 2, can
To find out, compared with the catalyst sample (comparative example 1) without phosphomolybdic acid, there is the catalyst sample (embodiment 1) of phosphomolybdic acid
Current density improves 50%, and the catalyst that this explanation present invention is prepared by membrane method has new nano-multilayer film knot
The active site of individual layer molybdenum disulfide is greatly improved in structure, the structure, overcomes molybdenum disulfide leading between layers well
Electric rate low the problem of limiting its electro-catalysis efficiency.
The foregoing is merely the preferred embodiment of the application, the application is not limited to, for those skilled in the art
For member, the application can have various modifications and variations.All any modifications within spirit herein and principle, made,
Equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
- A kind of 1. molybdenum disulfide elctro-catalyst with nanometer multilayer membrane structure, it is characterised in that：The catalyst is：In conduction From bottom to top successively covered with diallyl dimethyl ammoniumchloride, oxometallate, diallyl dimethyl chlorine on substrate Change ammonium, the circulation multilayer film of individual layer molybdenum disulfide.
- 2. a kind of preparation method of the molybdenum disulfide elctro-catalyst as claimed in claim 1 with nanometer multilayer membrane structure, its It is characterized in that：Described method includes following steps：1) diallyl dimethyl ammoniumchloride is dissolved in the water and solution a is made；2) polyoxometallate is dissolved in the water and solution b is made；3) individual layer molybdenum disulfide is dissolved in and stable solution c is made in N~methyl pyrrolidone；4) conductive substrates are immersed in corresponding solution successively according to the order of a, b, a, c, are often taken out from a kind of solution conductive All it is washed with deionized water after substrate totally, is then dried up with nitrogen, obtain the conductive substrates with multilayer film；5) conductive substrates with multilayer film prepared in step 4) are made annealing treatment under nitrogen protection, up to having nanometer The molybdenum disulfide elctro-catalyst of multi-layer film structure.
- 3. preparation method as claimed in claim 2, it is characterised in that：In step 2), the polyoxometallate includes：Phosphorus molybdenum Acid；Phosphotungstic acid.
- 4. preparation method as claimed in claim 2, it is characterised in that：In step 1), the concentration of the solution a is：10~ 20mg/ml。
- 5. preparation method as claimed in claim 2, it is characterised in that：In step 2), the concentration of the solution b is：5~ 10mg/ml。
- 6. preparation method as claimed in claim 2, it is characterised in that：In step 3), the concentration of the solution c is：0.1~ 0.3mg/ml。
- 7. such as claim 2-6 any one of them preparation methods, it is characterised in that：In step 4), the conductive substrates include： The stannic oxide of fluorine doped, indium-doped stannic oxide.
- 8. preparation method as claimed in claim 7, it is characterised in that：In step 4), the time of the immersion is 10~30 points Clock.
- 9. preparation method as claimed in claim 8, it is characterised in that：In step 5), the annealing temperature is 350~450 degree, 1~3h of time；Preferably, the annealing temperature is 400 degree, time 2 h.
- 10. catalyst as claimed in claim 1 and/or such as claim 2-6 any one of them preparation methods are urged in photoelectricity Change, the application in sensory field.
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| CN112525974A (en) * | 2020-11-19 | 2021-03-19 | 苏州健雄职业技术学院 | Method for measuring concentrations of dopamine and uric acid in presence of ascorbic acid |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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