CN110404577A - A kind of carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent, preparation method and application - Google Patents
A kind of carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent, preparation method and application Download PDFInfo
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- CN110404577A CN110404577A CN201910817804.3A CN201910817804A CN110404577A CN 110404577 A CN110404577 A CN 110404577A CN 201910817804 A CN201910817804 A CN 201910817804A CN 110404577 A CN110404577 A CN 110404577A
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000001257 hydrogen Substances 0.000 title claims abstract description 22
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000010802 sludge Substances 0.000 title claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 17
- 230000000694 effects Effects 0.000 title claims abstract description 17
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 25
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 claims abstract description 12
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000137 annealing Methods 0.000 claims abstract description 8
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims abstract description 7
- 235000019837 monoammonium phosphate Nutrition 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000013019 agitation Methods 0.000 claims abstract description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000004108 freeze drying Methods 0.000 claims abstract description 3
- 238000004321 preservation Methods 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 230000004087 circulation Effects 0.000 abstract description 4
- 230000007423 decrease Effects 0.000 abstract description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 15
- 239000000243 solution Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000001453 impedance spectrum Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 1
- 101710112672 Probable tape measure protein Proteins 0.000 description 1
- 101710204224 Tape measure protein Proteins 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- AMWVZPDSWLOFKA-UHFFFAOYSA-N phosphanylidynemolybdenum Chemical compound [Mo]#P AMWVZPDSWLOFKA-UHFFFAOYSA-N 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000002604 ultrasonography 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
- B01J27/24—Nitrogen compounds
-
- B01J35/33—
-
- 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
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
- C25B11/095—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds at least one of the compounds being organic
-
- 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 discloses a kind of carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent, preparation method and application, Ammonium Molybdate Tetrahydrate, ammonium dihydrogen phosphate and urea are successively dispersed in deionized water, then it is ultrasonically treated, it stirs evenly and seals, then it is heated to 70~90 DEG C in the state of at the uniform velocity magnetic agitation and keeps 1~2h, solution to be mixed removes sealing after being cooled to room temperature, freeze-drying finally obtains fluffy white presoma；White presoma obtained is placed in the nitrogen atmosphere of flowing constant-speed heating to annealing at 850~950 DEG C, MoP-NC elctro-catalyst is made in 2~2.5h of heat preservation.The present invention passes through the two-step method being simple and efficient and has synthesized unformed short grained MoP-NC, even if elctro-catalyst of the invention also shows insignificant performance decline after 1000 CV circulations of scanning.Meanwhile carbon-coated MoP can also overcome alkaline environment, realize excellent HER electro catalytic activity and stability.
Description
Technical field
The present invention relates to a kind of evolving hydrogen reaction catalyst more particularly to a kind of carbon-based phosphating sludge nano particle liberation of hydrogen electricity
Catalyst, preparation method and application.
Background technique
Social high speed development makes fossil energy gradually exhausted, therefore researchers are endeavoured to seek a kind of couple of environment friend
The good energy contains this vicious circle, and the high speed development of electrocatalytic hydrogen evolution reaction (HER) effectively mitigated this bad
State.Researcher had found that some non-precious metal catalysts had good cost performance in liberation of hydrogen direction in recent years, wherein with mistake
The phosphating sludge report crossed in metal phosphide (TMPs) is the most extensive.And the conductivity of simple phosphating sludge is not satisfactory,
Hydrogen Evolution Performance and stability in alkaline solution are also not so good as in acidic environment, therefore can be enhanced by introducing carbon-based material
Its conductivity and stability.
Summary of the invention
Technical problem to be solved by the present invention lies in: how efficiently simply to synthesize carbon-based phosphating sludge nano particle liberation of hydrogen
Elctro-catalyst, and meet its use in alkaline environment, provide a kind of carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent,
Preparation method and application.
The present invention be by the following technical programs solution above-mentioned technical problem, the present invention the following steps are included:
(1) presoma is prepared
Successively disperse according to Ammonium Molybdate Tetrahydrate, ammonium dihydrogen phosphate and the urea that molar ratio is 0.667~1:7.5:171.5
In deionized water, then it is ultrasonically treated, stirred evenly and sealed, then added in the state of at the uniform velocity magnetic agitation
Heat removes sealing to 70~90 DEG C and after keeping 1~2h, solution to be mixed to be cooled to room temperature, and freeze-drying finally obtains fluffy
White presoma；
(2) it makes annealing treatment
White presoma obtained is placed in the nitrogen atmosphere of flowing constant-speed heating to annealing at 850~950 DEG C, is kept the temperature
MoP-NC elctro-catalyst is made in 2~2.5h.
In the step (1), Ammonium Molybdate Tetrahydrate, ammonium dihydrogen phosphate and urea successively disperse in deionized water, to prepare
Solution concentration be 0.0465~0.0481g/mL.
In the step (1), the time of ultrasonic treatment is 5~10min.
In the step (2), white presoma, which is placed in quartz boat, to be made annealing treatment.Endothermic effect can be improved.
In the step (2), heating speed is 5 DEG C/min.
Carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent made from method described in a kind of.
Application of the carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent under alkaline environment.
Due to relevant report it has been confirmed that in addition to Ni base, HER of the simple transition metal phosphide in alkaline medium
Electro catalytic activity and stability are poor, therefore the present invention will realize the skill of the HER electro catalytic activity under alkaline environment
Art difficulty is very high, and final detection result is shown, HER electro catalytic activity of the present invention under alkaline environment can reach existing skill
Effect of the simple transition metal phosphide under acidic environment in art.
The present invention passes through the two-step method being simple and efficient and has synthesized unformed short grained MoP-NC, specific two-step method synthesis
Are as follows: first water bath processing is more fully mixed, is then made annealing treatment, obtained because reagent is in free state in the solution
Be it is pure to phosphating sludge compound, directly can be used for electrocatalytic hydrogen evolution, without carrying out purification process.Without repeatedly handling,
It is simple and efficient, convenient for commercialization.
It is unformed that the present invention has the advantage that the present invention has been synthesized by the two-step method being simple and efficient compared with prior art
Short grained MoP-NC, since MoP nanoparticle is by carbon coating, their localized clusters are together.This localized clusters integrally divide
Scattered small-particulate materials only need the overpotential of 131mV to provide for 10mA/cm in 1M KOH2Current density, this is better than
HER performance of the single phosphatization molybdenum material of existing report in alkaline environment.In addition, even if after scanning 1000 CV circulation,
Elctro-catalyst of the invention also shows insignificant performance decline.Meanwhile carbon-coated MoP can also overcome alkaline environment,
Realize excellent HER electro catalytic activity and stability.
Detailed description of the invention
Fig. 1 is the TEM picture of MoP-NC catalyst made from embodiment 1；
Fig. 2 is the SEM picture of MoP-NC catalyst made from embodiment 1；
Fig. 3 is liberation of hydrogen efficiency performance map of the invention；
Fig. 4 is 1000 CV cycle analysis figures that catalyst is made in embodiment 1；
Fig. 5 is the double layer capacity performance map of the obtained catalyst of the present invention；
Fig. 6 is the EIS impedance spectrum of the obtained catalyst of the present invention；
Fig. 7 is 1000 CV cycle analysis figures of the catalyst of different Ammonium Molybdate Tetrahydrate contents.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
The specific implementation process of the present embodiment is as follows:
(1) preparation of presoma: first by load weighted 0.240g Ammonium Molybdate Tetrahydrate, 0.167g ammonium dihydrogen phosphate and
2.000g urea is successively dispersed in 50mL deionized water, then carries out being ultrasonically treated for 5~10 minutes to it, and then will be above-mentioned
Mixed solution is placed on uniform stirring 10~15 minutes on magnetic stirring apparatus, then seals mixed solution, mixed solution is enabled to protect
It holds and is heated to 80 DEG C in the state of at the uniform velocity magnetic agitation and is kept for 1 hour, solution to be mixed removes sealing after being cooled to room temperature
And placed in freeze drier and be dried, finally obtain fluffy white presoma；
(2) quartz boat for filling white presoma is placed in the nitrogen atmosphere of flowing and is existed with the rate of heat addition of 5 DEG C/min
It anneals at 900 DEG C, heat preservation obtains MoP-NC catalyst in 2 hours；
(3) preparation of working electrode: catalyst made from 10mg step (2) is weighed, is dispersed in comprising 650mL deionization
Mass colour electrolyte is formed in the solution of water, 350mL isopropanol and 50uL Nafion (5wt%), then by mass colour electrolyte super
It carries out obtaining evenly dispersed ink in ultrasound 20~30 minutes in sound machine.Finally 10uL ink is drawn with micro dosimeter to be loaded into
Equipped on the glass-carbon electrode of rotating circular disk device, to its natural air drying；
(4) preparation steps of electrolyte solution: preparing 100mL 1M KOH solution, weighs 5.61g potassium hydroxide and moves to burning
In cup, 100mL deionized water is slowly poured into beaker, the above-mentioned beaker containing lye is then placed on magnetic stirring apparatus
Upper slowly stirring；
(5) LSV curve, volt-ampere stable circulation then are obtained with the conventional three electrode work stations equipped with rotating circular disk device
Property, the performance parameters such as double layer capacity and EIS impedance spectrum.
Embodiment 2
The present embodiment uses 2.000g glucose to substitute urea as carbon source.Other embodiments and embodiment 1 are identical.
Embodiment 3
The Ammonium Molybdate Tetrahydrate that the present embodiment uses is 0.16g, and other embodiments and embodiment 1 are identical.
Embodiment 4
The Ammonium Molybdate Tetrahydrate that the present embodiment uses is 0.20g, and other embodiments and embodiment 1 are identical.
Embodiment 5
The Ammonium Molybdate Tetrahydrate that the present embodiment uses is 0.28g, and other embodiments and embodiment 1 are identical.
It is as depicted in figs. 1 and 2 that TEM and SEM detection is carried out to MoP-NC catalyst made from embodiment 1.It can be seen that carbon coating
Molybdenum phosphide catalyst successful preparation, and carbon-based introducing slows down the polymerization of sample.
As shown in figure 3, wherein MoP-NC catalyst only needs 131mV that 10mA/cm can be realized in 1M KOH electrolyte2's
Current density illustrates that the catalyst has excellent HER electro catalytic activity under alkaline environment；It can be seen from Fig. 4 that MoP-NC is urged
Agent showing insignificant performance decline after 1000 CV are recycled, it was demonstrated that prepared catalyst is under alkaline environment
There is good stability；Fig. 5 is the double layer capacity performance map of prepared catalyst, and wherein the double layer capacity of MoP-NC is
10.9mF/cm2, this is far longer than other two groups of double-layer capacitance values, it was demonstrated that the nitrogen co-doped phosphating sludge of carbon has larger electricity
Chemical activity area, electrocatalysis characteristic are more preferable；Fig. 6 is the EIS impedance spectrum of prepared sample, the impedance spectrum convergence radius of MoP-NC
Much smaller than other two groups, it was demonstrated that the conductivity by the nitrogen co-doped MoP of carbon has great promotion.
As shown in fig. 7, in the embodiment 1,3,4,5, respectively Ammonium Molybdate Tetrahydrate be (0.16g, 0.20g, 0.24g,
0.28g), ammonium dihydrogen phosphate 0.167g, urea are that 2g carries out multiple groups experiment, and wherein first three groups performance is almost close, 0.28g's
One group of performance is poor, and the atomic weight through analyzing the Mo element that the Ammonium Molybdate Tetrahydrate in this group is included is to be greater than biphosphate
The atomic weight for the P element that ammonium is included, that is, metallic element are excessive.The MoP- of superperformance is prepared if necessary
NC catalyst needs the atomic weight ratio of strict control Mo and P to be less than or equal to 1.
Simultaneously as can be seen that when using glucose and urea as carbon source synthetic material respectively, urged prepared by glucose
The HER performance of agent is always weaker than catalyst prepared by urea.This is because urea in the synthesis process not only as carbon source but also
As nitrogen source, it also decomposes and generates portion gas during this period, slows down the polymerization of the MoP of N, C codope, plays excellent
Auxiliary synthesis.Catalyst prepared by urea has excellent HER electro catalytic activity in alkaline medium (1M KOH)
And stability, only need the overpotential of 131mV to realize 10mA/cm2Current density and 1000CV circulation after show
Insignificant reduced performance out.Therefore, the present invention be overcome the HER catalytic activity of transition metal phosphide under alkaline condition and
Stability provides new approach.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (8)
1. a kind of preparation method of carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent, which comprises the following steps:
(1) presoma is prepared
It is successively dispersed according to Ammonium Molybdate Tetrahydrate, ammonium dihydrogen phosphate and the urea that molar ratio is 0.667~1:7.5:171.5
In ionized water, then it is ultrasonically treated, stir evenly and is sealed, is then heated in the state of at the uniform velocity magnetic agitation
And sealing is removed after keeping 1~2h, solution to be mixed to be cooled to room temperature, freeze-drying finally obtains fluffy white by 70~90 DEG C
Color presoma；
(2) it makes annealing treatment
White presoma obtained is placed in the nitrogen atmosphere of flowing constant-speed heating to annealing at 850~950 DEG C, heat preservation 2~
MoP-NC elctro-catalyst is made in 2.5h.
2. a kind of preparation method of carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent according to claim 1, feature
Be, in the step (1), Ammonium Molybdate Tetrahydrate, ammonium dihydrogen phosphate and urea successively disperse in deionized water, preparation it is molten
Liquid concentration is 0.0465~0.0481g/mL.
3. a kind of preparation method of carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent according to claim 1, feature
It is, in the step (1), the time of ultrasonic treatment is 5~10min.
4. a kind of preparation method of carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent according to claim 1, feature
It is, in the step (2), white presoma, which is placed in quartz boat, to be made annealing treatment.
5. a kind of preparation method of carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent according to claim 1, feature
It is, in the step (2), heating speed is 5 DEG C/min.
6. a kind of use carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent made from the method as described in claim 1.
7. the carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent according to claim 6, which is characterized in that described to urge
In agent, the atomic weight ratio of Mo and P are less than or equal to 1.
8. application of the carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent under alkaline environment as claimed in claim 6.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111672527A (en) * | 2020-06-22 | 2020-09-18 | 齐鲁工业大学 | Molybdenum phosphide catalyst and preparation method thereof |
| CN112007673A (en) * | 2020-09-09 | 2020-12-01 | 安徽师范大学 | N-doped porous carbon-coated MoP nano rod material and preparation method and application thereof |
| CN112028041A (en) * | 2020-09-03 | 2020-12-04 | 中国科学院地球化学研究所 | Carbon thermal reduction preparation method of MoP, product and application |
| CN114497587A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Catalyst in proton exchange membrane fuel cell and preparation method thereof |
| CN115207299A (en) * | 2022-03-31 | 2022-10-18 | 浙江大学衢州研究院 | Molybdenum phosphide/nitrogen-doped hollow carbon sphere composite material, positive electrode material and preparation method thereof |
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