CN108358181A - A kind of the evolving hydrogen reaction elctro-catalyst and preparation method and application of phosphide - Google Patents
A kind of the evolving hydrogen reaction elctro-catalyst and preparation method and application of phosphide Download PDFInfo
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- CN108358181A CN108358181A CN201810132899.0A CN201810132899A CN108358181A CN 108358181 A CN108358181 A CN 108358181A CN 201810132899 A CN201810132899 A CN 201810132899A CN 108358181 A CN108358181 A CN 108358181A
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- 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
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- 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 the evolving hydrogen reaction elctro-catalyst and preparation method and application of a kind of phosphide, evolving hydrogen reaction elctro-catalyst ingredient formula is RuP.RuP is formed to improve the evolving hydrogen reaction chemical property of metal Ru by mixing P element in metal Ru (Ru).RuP materials have anti-(HER) catalytic performance of excellent liberation of hydrogen and long-time stability in conductivity in extensive pH solution, and compared to metal Ru, 10mAcm‑2Corresponding overpotential, Tafel slope, exchange current density are all significantly improved, it is often more important that activity and stability are better than commercialized metal oxide containing precious metals Pt/C catalyst.This method for preparing catalyst in the present invention is easy to operate, is easy to mass produce, and can be widely applied to this energy storage of electrolysis water and switch technology, has higher practical value.
Description
Technical field
The invention belongs to electrochemical catalyst field, it is related to a kind of phosphide evolving hydrogen reaction elctro-catalyst and preparation method thereof
And application, it can be used for the elctro-catalyst of electrolysis water this energy storage and switch technology.
Background technology
The world today, energy problem are the critical issues of human social development.It is used with the transition of fossil energy, the whole world
It warms, greenhouse effects, the environment such as air pollution and pollution problem become increasingly serious.In order to realize the sustainable development of the mankind,
Develop and utilize the theme that economic, new energy efficiently, clean is 21 century world energy sources science and technology.Currently, solar energy, wind energy and
The regenerative resources such as tide energy receive World Focusing, however these generations of electricity by new energy belong to uncontrollable power supply, exist it is intermittent and
The shortcomings of unstability.Develop advanced electrochemical energy storage and switch technology, such as fuel cell, metal-air battery, electricity
Xie Shui etc. is the fundamental way solved the problems, such as.
Wherein, electrochemistry hydrolytic hydrogen production is method that is a kind of effective and being concerned, but its cathode hydrogen evolution reacts (HER)
By slow dynamic (dynamical) serious limitation.Therefore, catalyst is needed to accelerate to react.But presently the most efficient catalysis
Agent is still the noble metal catalyst of platinum family.The high price of noble metal and it is rare the shortcomings of seriously limit it again and greatly develop.
So in order to improve the electrochemical efficiency of electrolysis water, the cathode hydrogen evolution catalyst of superior performance is found with as far as possible
Ground reduces cost, is the difficult point and hot issue for being electrolysed wate research.
Invention content
It is an object of the present invention to provide a kind of phosphatization ruthenium evolving hydrogen reaction elctro-catalyst and its preparation method and application,
To improve the problems such as existing best evolving hydrogen reaction elctro-catalyst (Pt/C) is expensive and stability is poor.The catalyst and Pt/C
Compare, not only have more remarkable hydrogen and be precipitated (HER) catalytic performance and long-time stability, but also with relative inexpensiveness and
The advantages that preparation method is simple.
The first aspect of the invention provides to achieve the goals above, and technical scheme is as follows：
A kind of evolving hydrogen reaction elctro-catalyst of phosphatization ruthenium, the evolving hydrogen reaction elctro-catalyst ingredient formula are RuP.
The second aspect of the invention provides a kind of preparation method of evolving hydrogen reaction elctro-catalyst.The preparation method
It is by RuCl3·3H2O is prepared by low temperature phosphor reaction.
Preferably, the preparation method, is as follows：
By RuCl3·3H2O and NaH2PO2It is individually placed to the downstream and upstream of tube furnace；
Then low-temp reaction is carried out, required evolving hydrogen reaction elctro-catalyst is obtained.
This method step is simple, is suitble to industrialization is extensive to prepare.
Preferably, NaH2PO2And RuCl3·3H2The mass ratio of O is 5-10:1.
Preferably, the RuCl3·3H2O and NaH2PO2Distance at a distance of 5-10cm and it is intermediate be located at stove middle,
The condition of the low-temp reaction process is 400-500 DEG C of processing 1-5h, and atmosphere is inert atmosphere, including but not limited to argon gas,
Nitrogen, helium.
The third aspect of the invention provides a kind of test electrolyte pH ranges of evolving hydrogen reaction elctro-catalyst, described
The electrolyte pH ranges of evolving hydrogen reaction elctro-catalyst are 0-14.
The fourth aspect of the invention provides a kind of application of evolving hydrogen reaction elctro-catalyst in electrolysis water, the electricity
It is ruthenium-oxide to solve water anode catalyst, and the electrolyte in the electrolytic water device is 1M KOH.
The fifth aspect of the invention provides：
RuP is in the 10mA cm for reducing metal Ru evolving hydrogen reaction elctro-catalysts-2The application of corresponding overpotential.
Applications of the RuP in the Tafel slope for reducing metal Ru evolving hydrogen reaction elctro-catalysts.
Applications of the RuP in the exchange current density for increasing metal Ru evolving hydrogen reaction elctro-catalysts.
Applications of the RuP in the stability for increasing metal Ru evolving hydrogen reaction elctro-catalysts.
RuP is distributed to increase the application of the valence state of Ru for reducing the electronics of metal Ru.
RuP is in the 10mA cm for the evolving hydrogen reaction elctro-catalyst Pt/C that is above standard-2The application of corresponding overpotential.
Applications of the RuP in the Tafel slope for the evolving hydrogen reaction elctro-catalyst Pt/C that is above standard.
Applications of the RuP in the exchange current density for the evolving hydrogen reaction elctro-catalyst Pt/C that is above standard.
Applications of the RuP in the stability for the evolving hydrogen reaction elctro-catalyst Pt/C that is above standard.
In conclusion by using above-mentioned technical proposal, beneficial effects of the present invention are as follows：It is prepared using a step parco-lubrizing
Obtained RuP is as new evolving hydrogen reaction elctro-catalyst.By comparing the Hydrogen evolving reaction performance of RuP and metal Ru, the introducing of P
It significantly improves its hydrogen and catalytic activity and stability is precipitated.In addition, there is the liberation of hydrogen catalyst of the present invention extremely excellent hydrogen to analyse
Go out (HER) activity and operational stability, is superior to the metal oxide containing precious metals Pt/C catalyst of business, can be used as the cathode of water electrolysis
Elctro-catalyst.The present invention relates to RuP materials, preparation method is very simple, is suitable for preparing on a large scale, be beneficial to business
Change.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is X-ray diffraction (XRD) curve graph of RuP catalyst；
Fig. 2 is the N of RuP2Absorption-desorption (BET) curve graph；
Fig. 3 is the full spectrograms of XPS of RuP；
Fig. 4 is the 3p track XPS result figures of Ru elements；
Fig. 5 is the 2p track XPS result figures of P element；
Fig. 6 is the SEM figures of RuP powders；
Fig. 7 is the TEM figures of RuP powders；
Fig. 8 is RuP, polarization curve of the Ru and Pt/C catalyst in 1M KOH solutions；
Fig. 9 is by RuP, and the Ta Feier that polarization curve of the Ru and Pt/C catalyst in 1M KOH solutions is derived is oblique
Rate figure；
Figure 10 is the exchange electricity that polarization curve of the Ru and Pt/C catalyst in 1M KOH solutions is derived by RuP
Current density figure；
Figure 11 is stability test figure of the RuP and Pt/C catalyst in 1M KOH solutions；
Figure 12 is RuP and Pt/C respectively as cathod catalyst and RuO2The complete solution water installations of anode catalyst composition are in 1M
Electrolysis water performance map in KOH solution.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
The present embodiment provides a kind of preparation methods of evolving hydrogen reaction elctro-catalyst RuP, are as follows：Weigh 0.1g's
RuCl3·3H2The NaH of O and 1g2PO2It is individually placed to the downstream and upstream of tube furnace, the two is at a distance of 7cm and intermediate is being located at stove just
It is intermediate.Then it is heated to 400 DEG C of calcining 2h under an argon atmosphere, obtain required evolving hydrogen reaction elctro-catalyst.
Embodiment 2
The present embodiment provides a kind of preparation methods of evolving hydrogen reaction elctro-catalyst RuP, are as follows：Weigh 0.1g's
RuCl3·3H2The NaH of O and 0.5g2PO2It is individually placed to the downstream and upstream of tube furnace, the two is at a distance of 7cm and centre is positioned at stove
Middle.Then it is heated to 400 DEG C of calcining 2h under an argon atmosphere, obtain evolving hydrogen reaction elctro-catalyst.The catalytic reaction
Agent compared with Example 1,10mA cm-2Corresponding overpotential becomes larger, and Tafel slope becomes larger, and exchange current density becomes smaller, and stablizes
Property be deteriorated.
Embodiment 3
The present embodiment provides a kind of preparation methods of evolving hydrogen reaction elctro-catalyst RuP, are as follows：Weigh 0.1g's
RuCl3·3H2The NaH of O and 0.5g2PO2It is individually placed to the downstream and upstream of tube furnace, the two is at a distance of 10cm and centre is positioned at stove
Sub- middle.Then it is heated to 400 DEG C of calcining 2h under an argon atmosphere, obtain evolving hydrogen reaction elctro-catalyst.The reaction is urged
Agent compared with Example 1,10mA cm-2Corresponding overpotential becomes larger, and Tafel slope becomes larger, and exchange current density becomes smaller, surely
Qualitative variation.
Embodiment 4
The present embodiment provides a kind of preparation methods of evolving hydrogen reaction elctro-catalyst RuP, are as follows：Weigh 0.1g's
RuCl3·3H2The NaH of O and 0.5g2PO2It is individually placed to the downstream and upstream of tube furnace, the two is at a distance of 7cm and centre is positioned at stove
Middle.Then it is heated to 500 DEG C of calcining 2h under an argon atmosphere, obtain evolving hydrogen reaction elctro-catalyst.The catalytic reaction
Agent compared with Example 1,10mA cm-2Corresponding overpotential becomes larger, and Tafel slope becomes larger, and exchange current density becomes smaller, and stablizes
Property be deteriorated.
Reference examples 1：According to the preparation method in embodiment 1, it is added without NaH2PO2, by the RuCl of 0.1g3·3H2O is direct
It is put into the middle part of tube furnace, then it under hydrogen argon atmospher is heated to 400 DEG C of calcining 2h, RuO can correspondingly be prepared2Analysis
Hydrogen reacts elctro-catalyst.In addition, business Pt/C catalyst is also to be used.
The evolving hydrogen reaction elctro-catalyst RuP prepared in order to further illustrate the present invention is with good performance, and invention carries out
Following application test：
1. material is characterized as below
RuP Sample crystals structure by room temperature X-ray diffraction (XRD) within the scope of 10-90 ° with interval 0.02 ° tested.
The diffraction curve of acquisition is analyzed by general structure analysis system (GSAS) and EXPGUI interfaces.Sample compares table
Area and pore-size distribution pass through BELSORP | | device is based on N under the boiling temperature of liquid nitrogen2Absorption-desorption (BET) curve comes
It obtains.
X-ray photoelectron spectroscopy test is carried out to RuP powders, analyzes its surface chemistry composition and chemical valence state.
The pattern of RuP powders can be obtained by scanning electron microscope (SEM) photograph and G2T20 testing electronic microscopes.
(HER) catalytic performance is precipitated using catalyst preparation electrode, the evaluation electrode hydrogen prepared by the present invention, process is such as
Under：
1. the preparation of catalyst pulp：RuP powders are mixed into (conductive black mass fraction with a certain amount of conductive black
85%, play a part of conductive and carrier, almost without catalytic action) be dispersed in ethyl alcohol or other organic solvents, then to
Appropriate Nafion (mass fraction 5%) solution is wherein added, (catalyst concn 1.5mg/mL, Nafion in the solution dense
Degree is 0.2mg/mL), then sonic oscillation makes to be uniformly mixed the slurry for obtaining preparing catalyst.
2. prepared by electrode：By the catalyst pulp of above-mentioned preparation, pipetted with micro syringe a certain amount of to rotating circular disk electricity
On pole (RDE), it is 0.232mg/cm to make its load capacity on RDE2, then put and dry up naturally in air.
3. the measurement of electrode activity：The electrode prepared is attached on rotating circular disk device (Pine companies) and carries out electrification
Learn test.
The process of test is as follows：
1) system of electro-chemical test be three-electrode system (glass-carbon electrode is working electrode, platinized platinum or platinum filament be to electrode,
Ag/AgCl is reference electrode), electrolyte is 1M KOH, 1M PBS, 0.5M H2SO4。
2) before test, continuously lead to 30~60min of argon gas into reactor, to ensure that electrolyte solution is satisfied by oxygen
It is 150~250mL/min with, ventilation flow rate.Oxygen is also always maintained at and is passed through during the test.
3) (HER) catalytic activity is precipitated in evaluation hydrogen, to carry out polarization curve test (LSV), and voltage scan range is 0.2~
1V, sweep speed 5mV/s, rotary speed 1600rpm.
4) catalytic stability is evaluated, galvanostatic method test (fixed 10mA cm are carried out-2It is constant) observation voltage is at any time
Variation relation investigates catalyst stability.
Characterization result is as follows：
1.XRD is characterized
Fig. 1 is the XRD spectrum of RuP tested within the scope of 10~90 ° at room temperature.It can be seen from the figure that its show it is good
The RuP phase structures of good rhombic system.Wherein 31.91 °, 44.02 ° of and, 46.02 ° of three main peaks correspond respectively to (011),
(112) and (211) crystal face.
2.BET is characterized
Fig. 2 is the N of RuP2Absorption-desorption (BET) curve, it is 4.6m that its specific surface area, which can be calculated,2g-1。
3.XPS is analyzed
In order to probe into the surface chemistry composition and chemical valence state of RuP, XPS tests have been carried out to RuP.Fig. 3 demonstrates Ru, P,
The presence of tri- elements of O.From fig. 4, it can be seen that the peaks 3p3/2 and 3p1/2 of ruthenium are respectively at 462.2 and 484.4eV combination energy, with
Metal Ru is compared, can locate to deviate to high combination, it was demonstrated that the presence of RuP.For P the peaks 2p mainly there are two big region：One
A is to combine that 131eV can be arrived 130, represents phosphide signal；One is to combine that phosphate species can be represented in 134eV or so.
From fig. 5, it can be seen that the presence of phosphide signal further demonstrates the formation of RuP.
4.SEM and TEM characterizations
Fig. 6 and Fig. 7 is respectively the SEM figure and TEM figures of RuP.It can be seen from the figure that the pattern of RuP is 10-30 nanoparticles
Molecular big micro particles.From the illustration of Fig. 7, it can be seen that it is brilliant to correspond to RuP (112) by lattice fringe 0.206nm
Face further demonstrates the formation of RuP.
5.HER electro catalytic activities characterize
Fig. 8 is the polarization curve of RuP, Ru and the Pt/C HER in 1M KOH.It can be seen from the figure that the initial mistake of RuP
Current potential and 10mA cm-2Corresponding overpotential is all significantly less than Ru and Pt/C, illustrates significantly improve HER electro-catalysis in RuP
Activity.
Fig. 9 and Figure 10 is respectively that RuP, Ru and Pt/C derive the Tafel obtained by the polarization curve of HER in its 1M KOH
Slope figure and exchange current density figure.The Tafel slopes of RuP are significantly less than metal Ru, are slightly less than Pt/C, illustrate that RuP is faster
Kinetics, better HER catalytic activity.From exchange current density figure, it can be seen that RuP exchange current densities considerably beyond
Metal Ru and Pt/C disclose the superior intrinsic catalytic activity of RuP.
6.HER electro-catalysis stability characterizes
Figure 11 is the galvanostatic method stability test of RuP and Pt/C.Pass through fixed 10mA cm-2Constant, observation voltage is at any time
Between variation relation investigate catalyst stability.It is apparent as can be seen that by 100h test, Pt/C decaying it is obvious that
And RuP is almost unchanged, illustrates its excellent stability.
7. complete solution water performance characterization
It is tested by above characterization, it can be seen that RuP has remarkable HER electro catalytic activities and stability, not only exists
Various aspects have also exceeded classical Pt/C commercial catalysts considerably beyond metal Ru.When as actual electrolysis water the moon
When pole, RuP shows better electrolysis water performance, 10mA cm again-2Corresponding operation voltage only has 1.49V, becomes electrolysis
The electrocatalyst for cathode of great some commercial potential in water installations.
Each embodiment is described by the way of progressive in this specification, the highlights of each of the examples are with other
The difference of embodiment, just to refer each other for identical similar portion between each embodiment.For device disclosed in embodiment
For, since it is corresponded to the methods disclosed in the examples, so description is fairly simple, related place is said referring to method part
It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest range caused.
Claims (9)
1. a kind of preparation method of evolving hydrogen reaction elctro-catalyst, which is characterized in that the method is by RuCl3·3H2O passes through low
Warm phosphating reaction prepares evolving hydrogen reaction elctro-catalyst, and the method is as follows：
First by RuCl3·3H2O and NaH2PO2It is individually placed to the downstream and upstream of tube furnace, the RuCl3·3H2O and described
NaH2PO2The distance between at a distance of 5-10cm and being respectively positioned on tube furnace middle
Then low-temp reaction is carried out, obtains required evolving hydrogen reaction elctro-catalyst, the condition of the low-temp reaction process is 400-500
DEG C, processing time 1-5h, atmosphere is inert atmosphere, and the inert atmosphere includes but not limited to argon gas, nitrogen, helium；
The NaH2PO2With the RuCl3·3H2The mass ratio of O is 5-10:1.
2. a kind of evolving hydrogen reaction elctro-catalyst being prepared according to claim 1, which is characterized in that the evolving hydrogen reaction electricity is urged
Agent ingredient formula is RuP.
3. a kind of test electrolyte pH ranges of evolving hydrogen reaction elctro-catalyst, which is characterized in that the evolving hydrogen reaction elctro-catalyst
Electrolyte pH ranges be 0-14.
4. a kind of evolving hydrogen reaction elctro-catalyst of phosphatization ruthenium is in the application of electrolysis water.
5. a kind of evolving hydrogen reaction elctro-catalyst according to claim 4 is in the application of electrolysis water, which is characterized in that electrolysis water
Anode catalyst is ruthenium-oxide.
6. a kind of evolving hydrogen reaction elctro-catalyst according to claim 4 is in the application of electrolysis water, which is characterized in that electrolysis water
Electrolyte in device is 1M KOH.
7. the evolving hydrogen reaction elctro-catalyst of a phosphatization ruthenium reduces the 10mA cm of metal Ru evolving hydrogen reaction elctro-catalysts-2Corresponding mistake
Current potential, Tafel slope, and increase the application of the exchange current density and stability of metal Ru evolving hydrogen reaction elctro-catalysts.
8. the electronics that the evolving hydrogen reaction elctro-catalyst of a phosphatization ruthenium reduces metal Ru is distributed to increase the application of the valence state of Ru.
The 10mA cm of evolving hydrogen reaction elctro-catalyst Pt/C 9. the evolving hydrogen reaction elctro-catalyst of a phosphatization ruthenium is above standard-2It is corresponding
The application of overpotential, Tafel slope, exchange current density and stability.
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Cited By (6)
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| CN109306499A (en) * | 2018-10-31 | 2019-02-05 | 浙江工业大学 | A kind of RuP@PNC catalyst of porous hollow and its preparation method and application |
| CN110860301A (en) * | 2019-11-26 | 2020-03-06 | 中国科学技术大学 | Ruthenium phosphide-loaded carbon micron sheet dual-functional electrocatalyst, preparation method thereof and application of dual-functional electrocatalyst in efficient electrolytic hydrogen production |
| CN112237932A (en) * | 2020-09-14 | 2021-01-19 | 青岛大学 | RuP3Modified two-dimensional CoP nanosheet hydrogen evolution electrocatalyst and preparation method and application thereof |
| CN112680741A (en) * | 2021-01-12 | 2021-04-20 | 江苏大学 | Preparation method and application of ruthenium-doped cobalt phosphide electrocatalyst |
| CN113668009A (en) * | 2021-07-15 | 2021-11-19 | 徐州天启新材料科技有限公司 | Hydrogen evolution reaction electrocatalyst of phosphide and preparation method |
| CN114293222A (en) * | 2021-11-22 | 2022-04-08 | 江西师范大学 | Synthesis method of ultrafine ruthenium diphosphide nanoparticle electrocatalyst |
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| CN110860301A (en) * | 2019-11-26 | 2020-03-06 | 中国科学技术大学 | Ruthenium phosphide-loaded carbon micron sheet dual-functional electrocatalyst, preparation method thereof and application of dual-functional electrocatalyst in efficient electrolytic hydrogen production |
| CN112237932A (en) * | 2020-09-14 | 2021-01-19 | 青岛大学 | RuP3Modified two-dimensional CoP nanosheet hydrogen evolution electrocatalyst and preparation method and application thereof |
| CN112237932B (en) * | 2020-09-14 | 2023-05-05 | 青岛大学 | RuP 3 Modified two-dimensional CoP nanosheet hydrogen evolution electrocatalyst and preparation method and application thereof |
| CN112680741A (en) * | 2021-01-12 | 2021-04-20 | 江苏大学 | Preparation method and application of ruthenium-doped cobalt phosphide electrocatalyst |
| CN113668009A (en) * | 2021-07-15 | 2021-11-19 | 徐州天启新材料科技有限公司 | Hydrogen evolution reaction electrocatalyst of phosphide and preparation method |
| CN114293222A (en) * | 2021-11-22 | 2022-04-08 | 江西师范大学 | Synthesis method of ultrafine ruthenium diphosphide nanoparticle electrocatalyst |
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