CN109647458A - The method that self-template methods synthesis has the double-metal phosphide elctro-catalyst of hollow structure - Google Patents
The method that self-template methods synthesis has the double-metal phosphide elctro-catalyst of hollow structure Download PDFInfo
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- CN109647458A CN109647458A CN201910026784.8A CN201910026784A CN109647458A CN 109647458 A CN109647458 A CN 109647458A CN 201910026784 A CN201910026784 A CN 201910026784A CN 109647458 A CN109647458 A CN 109647458A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 18
- 239000002184 metal Substances 0.000 title claims abstract description 18
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 13
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 13
- 229910003271 Ni-Fe Inorganic materials 0.000 claims abstract description 28
- 239000002091 nanocage Substances 0.000 claims abstract description 14
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 13
- 238000000137 annealing Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 20
- 229910001868 water Inorganic materials 0.000 claims description 15
- 238000005119 centrifugation Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 230000001376 precipitating effect Effects 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 125000004093 cyano group Chemical group *C#N 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- OINIXPNQKAZCRL-UHFFFAOYSA-L nickel(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Ni+2].CC([O-])=O.CC([O-])=O OINIXPNQKAZCRL-UHFFFAOYSA-L 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
- 238000011144 upstream manufacturing Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 229910000859 α-Fe Inorganic materials 0.000 claims description 5
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 238000012360 testing method Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005530 etching Methods 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000012546 transfer Methods 0.000 abstract description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 2
- 238000011160 research Methods 0.000 abstract description 2
- 229910052723 transition metal Inorganic materials 0.000 abstract description 2
- 150000003624 transition metals Chemical class 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010189 synthetic method 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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J37/04—Mixing
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses the methods that a kind of synthesis of self-template methods has the double-metal phosphide elctro-catalyst of hollow structure, belong to the synthesis technical field of new energy elctro-catalyst.Technical solution of the present invention main points are as follows: choose the elctro-catalyst best performance that etching agent one is hydrated ammonia solution 8mL, sodium hypophosphite amount is 100mg, annealing temperature is 350 DEG C, annealing time 2h condition synthesizes, by further characterizing research, the double-metal phosphide prepared under this condition has special hollow structure.Compared to most transition metal phosphide catalysis materials, the resulting Ni-Fe PBA nanocages of the preparation method have biggish specific surface area, more active sites, the advantages such as electric charge transfer of promotion.
Description
Technical field
The invention belongs to the synthesis technical fields of new energy elctro-catalyst, and in particular to during a kind of synthesis of self-template methods has
The method of the double-metal phosphide elctro-catalyst of hollow structure.
Background technique
With economic rapid development, the consumption of conventional fossil fuel (petroleum, natural gas and coal etc.) increasingly increase so that
These non-renewable resources are on the verge of exhausted and adjoint a series of problem of environmental pollution.In the new energy developed, Hydrogen Energy because
, from a wealth of sources and advantages of environment protection high with combustion heat value causes the extensive concern of all circles.Water electrolysis hydrogen production analysis oxygen is recognized
To be a kind of method for preferably preparing high-purity hydrogen, reactant is water, and product is oxygen and hydrogen, and there are no pollution to the environment
Harm, is an environmentally friendly green energy resource system.
Water electrolysis method for hydrogen manufacturing have always been considered as be renewable energy conversion and storage a kind of ideal strategy, but
It is obstructed since its slow kinetic effect discharges hydrogen and oxygen, the evolving hydrogen reaction on cathode is by the oxygen evolution reaction on anode
The slow dynamic (dynamical) serious restriction generated.Platinum (Pt) and iridium (Ir) sill are to have highest HER and OER active respectively
Material, however the scarcity and unstability of this kind of precious metal material make them be difficult to be introduced energy conversion on a large scale and deposit
In storage application.Therefore, it is dedicated to design and synthesis high activity, durable and inexpensive base metal base analysis oxygen electro-catalysis material now
Material.
A large number of studies show that different synthetic methods not only influences granular size, shape and its crystal form of Ni-Fe PBA etc.
Structural form feature also will affect its electrical properties and catalytic activity.The synthesis of hollow structure depends on template no matter
It is hard template or soft template, the removal of internal template is needed by calcining or dissolved to realize, takes a long time and be also easy to produce
Secondary pollution.Ni-Fe PBA is usually nano cubic volume morphing, and by self-template mode, changing etching reagent or etching agent makes
Dosage can obtain different hollow structures.The catalytic performance of enhancing is attributed to the specific surface area of its increase, active site quantity
Increase, the electrolyte osmosis of less obstruction, the electric charge transfer of promotion and the gas release of promotion.Therefore seek a kind of new efficient
The synthetic strategy of elctro-catalyst is vital.
Summary of the invention
The technical problem to be solved by the present invention is to provide the bimetallic phosphatizations that a kind of synthesis of self-template methods has hollow structure
The analysis oxygen elctro-catalyst of higher performance is finally made in the method for object elctro-catalyst, this method, so that oxygen precipitation efficiency is effectively improved,
Reduce energy consumption.
The present invention adopts the following technical scheme that self-template methods synthesis has the double of hollow structure to solve above-mentioned technical problem
The method of metal phosphide elctro-catalyst, it is characterised in that specific steps are as follows:
Step S1: 0.3g Nickel diacetate tetrahydrate and 0.441g citrate trisodium dihydrate are dissolved in 40mL deionized water and obtained
To solution A, 0.264g six cyano ferrite potassium is dissolved in 60mL deionized water and obtains solution B, solution B is added in solution A
And be uniformly mixed, for 24 hours in aged at room temperature by mixed solution, precipitating is collected by centrifugation, it is with water and ethanol washing and dry in 60 DEG C
It is dry to obtain Ni-Fe PBA nanocube；
Step S2: 20mL is contained into 2.5-8mL NH3·H2The ammonia spirit of O, which is added to 10mL and contains 20mg Ni-Fe PBA, to be received
In the alcohol dispersion liquid of rice cube, it is uniformly mixed, precipitating is collected by centrifugation, it is with water and ethanol washing and dry in 60 DEG C
To Ni-Fe PBA nanocages；
10mg Ni-Fe PBA nanocages and 100mg sodium hypophosphite: being placed in two different locations of quartz boat by step S3,
Middle sodium hypophosphite is placed on upstream side, is warming up to 350 DEG C of annealing 2h in a nitrogen atmosphere with the heating rate of 2 DEG C/min, cooling
The double-metal phosphide elctro-catalyst with hollow structure is obtained to room temperature.
Further preferably, 8mL NH is contained in ammonia spirit described in step S23·H2O, having for preparing under this condition are hollow
Electrochemical property test of the double-metal phosphide elctro-catalyst of structure Jing Guo standard three electrode system, in 10mA/cm2Electric current
Overpotential is 1.53V under density conditions.
Technical concept of the invention are as follows: speculate that a hydration ammonia should be by regioselectivity chemical etching in cube to cage
Cavity producer is used as in formula conversion process.5min is converted into hollow nanocages at room temperature, confirms, carves through XRD and EDX analysis
Product after erosion is still Ni-Fe PBA and the Ni/Fe atom almost the same with nanocube with cubic crystal structure
Than.Fourier transform infrared (FTIR) spectrum is carried out to track chemical composition of the product in the differential responses time and change.With erosion
The passage of time is carved from 0-5min, the pattern of material to the plate-like of collapsing and deduces chemistry again from nanocube to nanocages
The variation of bond energy.By the phosphorization of ion-exchange reactions and subsequent sodium hypophosphite, to obtain having of haveing excellent performance
The double-metal phosphide of hollow structure.
Compared with the prior art, the invention has the following beneficial effects: being prepared using self-template methods with hollow structure
Double-metal phosphide electrocatalysis material has more excellent electrocatalysis characteristic, is that one kind can be by simpler preparation process
The method for obtaining hollow structure elctro-catalyst.
Detailed description of the invention
Fig. 1 is the XRD diagram that Ni-Fe PBA elctro-catalyst is made in embodiment 3；
Fig. 2 is the SEM figure that Ni-Fe PBA elctro-catalyst is made in embodiment 3；
Fig. 3 is the SEM figure that Ni-Fe PBA elctro-catalyst is made in embodiment 3.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
Step S1: 0.3g Nickel diacetate tetrahydrate and 0.441g citrate trisodium dihydrate are dissolved in 40mL deionized water and obtained
To solution A, 0.264g six cyano ferrite potassium is dissolved in 60mL deionized water and obtains solution B, solution B is added in solution A
And be uniformly mixed, for 24 hours in aged at room temperature by mixed solution, precipitating is collected by centrifugation, it is with water and ethanol washing and dry in 60 DEG C
It is dry to obtain Ni-Fe PBA nanocube；
Step S2: 20mL is contained into 2.5mL NH3·H2The ammonia spirit of O is added to 10mL and contains PBA nanometers of 20mg Ni-Fe
It in the alcohol dispersion liquid of cube, is uniformly mixed, precipitating is collected by centrifugation, be dried to obtain with water and ethanol washing and in 60 DEG C
Ni-Fe PBA nanocages；
10mg Ni-Fe PBA nanocages and 100mg sodium hypophosphite: being placed in two different locations of quartz boat by step S3,
Middle sodium hypophosphite is placed on upstream side, is warming up to 350 DEG C of annealing 2h in a nitrogen atmosphere with the heating rate of 2 DEG C/min, cooling
The double-metal phosphide elctro-catalyst with hollow structure is obtained to room temperature.Chemical property by standard three electrode system is surveyed
Examination, in 10mA/cm2Current density condition under overpotential be 1.63V.
Embodiment 2
Step S1: 0.3g Nickel diacetate tetrahydrate and 0.441g citrate trisodium dihydrate are dissolved in 40mL deionized water and obtained
To solution A, 0.264g six cyano ferrite potassium is dissolved in 60mL deionized water and obtains solution B, solution B is added in solution A
And be uniformly mixed, for 24 hours in aged at room temperature by mixed solution, precipitating is collected by centrifugation, it is with water and ethanol washing and dry in 60 DEG C
It is dry to obtain Ni-Fe PBA nanocube；
Step S2: 20mL is contained into 5mL NH3·H2The ammonia spirit of O be added to 10mL contain PBA nanometers of 20mg Ni-Fe it is vertical
It in the alcohol dispersion liquid of cube, is uniformly mixed, precipitating is collected by centrifugation, be dried to obtain with water and ethanol washing and in 60 DEG C
Ni-Fe PBA nanocages；
10mg Ni-Fe PBA nanocages and 100mg sodium hypophosphite: being placed in two different locations of quartz boat by step S3,
Middle sodium hypophosphite is placed on upstream side, is warming up to 350 DEG C of annealing 2h in a nitrogen atmosphere with the heating rate of 2 DEG C/min, cooling
The double-metal phosphide elctro-catalyst with hollow structure is obtained to room temperature.Chemical property by standard three electrode system is surveyed
Examination, in 10mA/cm2Current density condition under overpotential be 1.59V.
Embodiment 3
Step S1: 0.3g Nickel diacetate tetrahydrate and 0.441g citrate trisodium dihydrate are dissolved in 40mL deionized water and obtained
To solution A, 0.264g six cyano ferrite potassium is dissolved in 60mL deionized water and obtains solution B, solution B is added in solution A
And be uniformly mixed, for 24 hours in aged at room temperature by mixed solution, precipitating is collected by centrifugation, it is with water and ethanol washing and dry in 60 DEG C
It is dry to obtain Ni-Fe PBA nanocube；
Step S2: 20mL is contained into 8mL NH3·H2The ammonia spirit of O be added to 10mL contain PBA nanometers of 20mg Ni-Fe it is vertical
It in the alcohol dispersion liquid of cube, is uniformly mixed, precipitating is collected by centrifugation, be dried to obtain with water and ethanol washing and in 60 DEG C
Ni-Fe PBA nanocages；
10mg Ni-Fe PBA nanocages and 100mg sodium hypophosphite: being placed in two different locations of quartz boat by step S3,
Middle sodium hypophosphite is placed on upstream side, is warming up to 350 DEG C of annealing 2h in a nitrogen atmosphere with the heating rate of 2 DEG C/min, cooling
The double-metal phosphide elctro-catalyst with hollow structure is obtained to room temperature.Chemical property by standard three electrode system is surveyed
Examination, in 10mA/cm2Current density condition under overpotential be 1.53V.
Based on above embodiments, the hydration of etching agent one ammonia solution 8mL is chosen, sodium hypophosphite amount is 100mg, annealing temperature is
350 DEG C, annealing time 2h condition synthesis elctro-catalyst best performance prepared under this condition by further characterizing research
Double-metal phosphide have special hollow structure.Compared to most transition metal phosphide catalysis materials, the preparation side
The resulting Ni-Fe PBA nanocages of method have biggish specific surface area, more active sites, the electric charge transfer etc. of promotion
Advantage.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (2)
1. the method that self-template methods synthesis has the double-metal phosphide elctro-catalyst of hollow structure, it is characterised in that specific steps
Are as follows:
Step S1: 0.3g Nickel diacetate tetrahydrate and 0.441g citrate trisodium dihydrate are dissolved in 40mL deionized water and obtained
To solution A, 0.264g six cyano ferrite potassium is dissolved in 60mL deionized water and obtains solution B, solution B is added in solution A
And be uniformly mixed, for 24 hours in aged at room temperature by mixed solution, precipitating is collected by centrifugation, it is with water and ethanol washing and dry in 60 DEG C
It is dry to obtain Ni-Fe PBA nanocube；
Step S2: 20mL is contained into 2.5-8mL NH3·H2The ammonia spirit of O, which is added to 10mL and contains 20mg Ni-Fe PBA, to be received
In the alcohol dispersion liquid of rice cube, it is uniformly mixed, precipitating is collected by centrifugation, it is with water and ethanol washing and dry in 60 DEG C
To Ni-Fe PBA nanocages；
10mg Ni-Fe PBA nanocages and 100mg sodium hypophosphite: being placed in two different locations of quartz boat by step S3,
Middle sodium hypophosphite is placed on upstream side, is warming up to 350 DEG C of annealing 2h in a nitrogen atmosphere with the heating rate of 2 DEG C/min, cooling
The double-metal phosphide elctro-catalyst with hollow structure is obtained to room temperature.
2. the side that self-template methods synthesis according to claim 1 has the double-metal phosphide elctro-catalyst of hollow structure
Method, it is characterised in that: contain 8mL NH in ammonia spirit described in step S23·H2O, what is prepared under this condition has hollow structure
Electrochemical property test of the double-metal phosphide elctro-catalyst Jing Guo standard three electrode system, in 10mA/cm2Current density
Under the conditions of overpotential be 1.53V.
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Cited By (9)
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| CN110038603A (en) * | 2019-05-27 | 2019-07-23 | 安徽理工大学 | A kind of mixed metal phosphide base hollow out nanometer box and preparation method thereof, application |
| CN110152708A (en) * | 2019-05-27 | 2019-08-23 | 安徽理工大学 | A kind of hollow open-celled structure Ferrious material phosphide and preparation method thereof, application |
| CN110157006A (en) * | 2019-06-03 | 2019-08-23 | 贵阳学院 | The preparation and application of the electrode material of the preparation and material containing double-metal phosphide of double-metal phosphide material |
| CN110227549A (en) * | 2019-06-28 | 2019-09-13 | 陕西科技大学 | A kind of hollow cube structure anode catalyst and preparation method thereof |
| CN110237860A (en) * | 2019-06-28 | 2019-09-17 | 陕西科技大学 | A kind of electrolysis water and electrolysis urea anode catalyst and preparation method thereof |
| CN110354876A (en) * | 2019-07-19 | 2019-10-22 | 南京理工大学 | A kind of hollow Ni2P/Co2P/Fe2The preparation method of the nano combined elctro-catalyst of P |
| CN110624605A (en) * | 2019-10-28 | 2019-12-31 | 陕西科技大学 | Shell-core structured anode catalyst and preparation method thereof |
| CN111715248A (en) * | 2020-06-22 | 2020-09-29 | 陕西科技大学 | Cathode catalyst for hollow nano electrolyzed water and preparation method thereof |
| CN113578365A (en) * | 2021-08-12 | 2021-11-02 | 华侨大学 | Preparation method and application of surface-modified nano-iron-manganese composite catalyst |
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