CN109908938A - A kind of preparation method of Novel electrolytic water Oxygen anodic evolution catalyst Co@NC/CNT - Google Patents
A kind of preparation method of Novel electrolytic water Oxygen anodic evolution catalyst Co@NC/CNT Download PDFInfo
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- 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
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Abstract
The invention discloses the preparation methods of Novel electrolytic water Oxygen anodic evolution catalyst Co@NC/CNT a kind of, the specific steps are as follows: (1) preparation of Co-MOF；(2) preparation of Co@PDA；(3) preparation of Co@NC/CNT.The present invention is prepared for the Co-MOF nano cubic block of morphological rules by simple coprecipitation；It then is that carbon source carries out carbon coating to it, while introducing nitrogen source with Dopamine hydrochloride (DA) under weak basic condition；Next sample is uniformly mixed to growth and the carbonisation for promoting carbon nanotube (CNT) with typical two-part method in a nitrogen atmosphere with melamine.Entire synthesis process method is simple, and product morphology is controllable.Catalyst has good electro-catalysis analysis oxygen performance, higher conductivity and cyclical stability.The catalyst is than contrast sample Co NC and business RuO2Electrolysis elutriation oxygen catalytic activity will get well, be with a wide range of applications.
Description
Technical field:
The invention belongs to electrocatalysis material preparation technical fields, are related to a kind of Novel electrolytic water Oxygen anodic evolution catalyst Co@
The preparation method of NC/CNT.
Background technique:
Economic fast development and energy shortage and problem of environmental pollution is got worse, and people need exploitation environment friend
Good reversible energy stores and energy conversion device, such as electrolysis water, zinc and air cell, fuel cell etc. have been widely studied.
Hydrogen Energy is future most promising green energy resource recognised by people, therefore height weight of the water electrolysis hydrogen production technology by countries in the world
Depending on.In electro-catalysis water splitting processes, H is generated in cathode2It is a two electron reaction processes, and obtains O in anode2Reaction be
A kind of four electronics or polyelectron process, excessive electronics transfer are intended to consume more energy, therefore the analysis oxygen of anode
Reaction (OER) is the ratedeterming step of electro-catalysis water decomposition.Therefore cheap, the efficient electro-catalysis anode production oxygen of one kind is researched and developed
Catalyst is particularly important.Under alkaline condition, Oxygen anodic evolution catalyst is with RuO2And IrO2Based on.Although traditional noble metal
Oxide catalyst OER activity is high, and overpotential and Tafel slope value are all very low, and cannot be neglected is, the system of noble metal catalyst
Standby with high costs, natural abundance is low；And in alkaline electrolyte, under the electrode potential of Gaoyang, noble metal catalyst RuO2It is easy to molten
It solves and makes the reduction of its stability, these features of noble metal catalyst limit their application.Therefore design and develop it is novel,
Inexpensively, efficient elctro-catalyst replaces conventional precious metal oxide (such as RuO2And IrO2) catalyticing anode oxygen evolution reaction is to grind at present
The emphasis studied carefully.
Following several respects factor should be considered by designing and developing OER elctro-catalyst: (1) activity is good, resourceful, at low cost
It is honest and clean, it is suitable for popularization and application；(2) large specific surface area is conducive to improve active site, increases electrode/electrolyte interface；(3) stablize
Good, the good corrosion resistance of property.
Summary of the invention:
The object of the present invention is to provide a kind of novel base metal base anode of electrolytic water oxygen-separating catalyst Co@NC/CNT's
Preparation method, the method for preparing catalyst is simple, and electro-catalysis analysis oxygen performance is better than business RuO2, as Novel electrolytic water sun
Electrode catalyst is hopeful to replace traditional precious metal oxide catalyst.The present invention provides a kind of Novel electrolytic water Oxygen anodic evolution and urges
The preparation method of agent Co@NC/CNT, the specific steps are as follows:
(1) preparation of Co-MOF.Preparation synthesis size is uniform under the conditions of relatively mild, nanometer of favorable dispersibility
Grade Co-MOF presoma.A certain amount of cobalt nitrate, sodium citrate and potassium cobalticyanide are added separately in a certain amount of ultrapure water,
Quick magnetic agitation to form transparent and homogeneous solution to being completely dispersed, and pink solid powder is obtained after ageing, and centrifugation washs, is cold
Freeze the nanoscale Co-MOF presoma of drying to obtain morphological rules size uniformity.
(2) preparation of [email protected] preparation of Co@PDA is that auto polymerization is formed under weak basic condition by Dopamine hydrochloride
Poly-dopamine, and then spontaneous it is anchored on the surface Co-MOF.Co-MOF and Dopamine hydrochloride that ratio is 2:1~2 are dispersed first
In 50~100ml Tris aqueous slkali, switch at the uniform velocity stir after ultrasonic disperse, obtain black solid powder, centrifugation, is done washing
It is dry to obtain Co PDA sample.
(3) preparation of Co@NC/CNT.Co@PDA and melamine that certain proportion is 1:2~10 are subjected to ground and mixed
After uniformly, it is fitted into corundum Noah's ark, is put into tube furnace, be passed through nitrogen, heated using typical two-part temperature program,
And after keeping the temperature a period of time, natural cooling obtains Co@NC/CNT and efficiently analyses oxygen elctro-catalyst.
Further: the specific surface area of the Co@NC/CNT catalyst is 70~80m2/g。
It is further: to be first dispersed in cabaltous nitrate hexahydrate and citrate trisodium dihydrate in the step (1) ultrapure
In water, then potassium cobalticyanide solution is added in above-mentioned solution.
Further: digestion time is 24~48 hours in the step (1).
Further: centrifugation ginseng setting number is 8000rpm in the step (1), continues 6-10 minutes.Next with ultrapure
Water and dehydrated alcohol wash 3 times respectively, and sublimation drying is 12 hours.
Further: centrifugation ginseng setting number is 10000rpm in the step (2), continues 10 minutes.Next with ultrapure
Water and dehydrated alcohol wash 3~5 times respectively, and vacuum drying temperature is 60 DEG C, are kept for 12 hours.
Further: temperature program is nitrogen 30~60 minutes logical first in the step (3), empties inner air tube, so
After be warming up to 500 DEG C keep the temperature 2 hours, heating rate be 2 DEG C/min；Add and gets off to be warming up to 600~800 DEG C of heat preservations 2 hours, heating
Rate is 2 DEG C/min.
It is further: catalyst Co NC/CNT load is applied to oxygen evolution reaction under alkaline condition on a current collector.
Electrolyte is 1 M KOH solution.
Further: it is as follows that preparing for electrode is precipitated in electrocatalytic oxidation:
(1) pretreatment of substrate: by the substrate for cutting into suitable shape impregnated first in dilute hydrochloric acid solution 15 minutes with
Surface oxide layer is removed, ultrapure water, dehydrated alcohol is next separately immersed in, is ultrasonically treated in acetone, it is dry to be finally putting into vacuum
It is dry, it is dried at 60 DEG C, it is spare.
(2) preparation of catalyst pulp: the Co@NC/CNT catalyst, conductive black (super P) and binder weighed up
PVDF is put into mortar to grind and be added organic solvent wet-milling 30 minutes after ten minutes, and viscous paste is made, spare.
(3) it analyses the preparation of oxygen electrode: the ground catalyst pulp of step (2) is coated uniformly on processing in step (1)
In good substrate, it is put into 60 DEG C of vacuum oven overnight, obtains electro-catalysis analysis oxygen electrode.
Further: the concentration of dilute hydrochloric acid is 2mol/L in the step (1), and substrate is in ultrapure water, dehydrated alcohol, acetone
Middle sonication treatment time is at least 30 minutes respectively.
Further: catalyst in the step (2): conductive black: the mass ratio of binder is 7:2:1.
Further: organic solvent is N-Methyl pyrrolidone in the step (2).
Further: the coated area of catalyst pulp on a current collector is 1*1cm in the step (3)2。
Further: the load capacity of catalyst Co@NC/CNT on a current collector is about 1mg/cm in the step (3)2。
Further: collector is selected from one or more of nickel foam, stainless (steel) wire, carbon cloth, carbon paper, electro-conductive glass.
Further: the electrochemical Characterization for the catalyst that the technical solution obtains is in Autolab electrochemical workstation
Upper progress is tested in 1 M KOH electrolyte using three-electrode system, i.e., working electrode, to electrode and reference electrode.Its
Middle working electrode is that catalyst loadings are about 1mg/cm2Foam nickel electrode, be platinum plate electrode to electrode, reference electrode is
Ag/AgCl electrode.
Further: the preparation method of the analysis oxygen electrode of comparative catalyst is identical as Co@NC/CNT.
Detailed description of the invention
Fig. 1 is the SEM figure of Co@NC/CNT catalyst prepared by the present invention.
Fig. 2 is the TEM figure of Co@NC/CNT catalyst prepared by the present invention.
Fig. 3 is the XRD of Co@NC/CNT catalyst prepared by the present invention.
Fig. 4 is that the Co@NC/CNT catalyst prepared according to the technology of the present invention sweeps the non-faraday area tested under speed in difference
Cyclic voltammetry curve.
Fig. 5 is that the contrast sample Co NC catalyst prepared according to the technology of the present invention sweeps the non-farad tested under speed in difference
The cyclic voltammetry curve in area.
Fig. 6 is the Co@NC/CNT prepared according to the technology of the present invention and contrast sample Co@NC catalyst in 1.0M KOH item
Electrochemical surface area measurement result under part.
Fig. 7 is N2 adsorption/desorption isothermal curve figure of Co@NC/CNT catalyst prepared by the present invention.Wherein rectangular mark
Note is Adsorption, circle markings Desorption.
Fig. 8 is the pore size distribution curve of Co@NC/CNT catalyst prepared by the present invention.
Fig. 9 is the linear scan curve of Co@NC/CNT catalyst and comparative experiments prepared by the present invention, is used under room temperature
Three-electrode system carries out half-cell test, sweep speed 5mV/s.
Figure 10 is the Tafel curve of Co@NC/CNT catalyst and comparative experiments prepared by the present invention.
Figure 11 is the chronoa mperometric plot of Co@NC/CNT catalyst prepared by the present invention.
Specific embodiment
This experiment inventive technique is described in further detail below with reference to the specific embodiment that this experiment is invented.This
Experimental method mentioned in inventive embodiments is general experimental method unless otherwise specified, used in the embodiment of the present invention
Drug, reagent, the material arrived can be obtained through commercial channels unless otherwise specified.The catalyst material of the technology of the present invention preparation
Expect physical characterization, the surface topography of sample is obtained by scanning electron microscope (SEM) characterization, the submicroscopic structure of material passes through
Transmission electron microscope (TEM) obtains.Material phase analysis is carried out to material by X-ray diffraction (XRD).The BET specific surface area of sample and
Pore-size distribution is completed by specific surface area and Porosimetry.According to the Co@NC/CNT catalyst modification of technical solution preparation
Nickel foam anode analysis oxygen electrode electro-chemical test carried out on Autolab work station.
Embodiment 1:
(1) preparation of Co-MOF.It is about with simple coprecipitation preparation morphological rules, size in this technical solution
The Co-MOF presoma of 900nm.It is ultrapure that 0.3g cabaltous nitrate hexahydrate and 0.53g citrate trisodium dihydrate are distributed to 40ml
Magnetic agitation about 10 minutes in water form solution one, and 0.3g potassium cobalticyanide is dissolved in 40ml ultrapure water, form solution two；It will be molten
Liquid two is slowly added into solution one, after ten minutes by mixed solution stir about, is stood 24 hours at room temperature, is obtained pink
Solid powder, centrifuge separation, revolving speed be 8000rpm continue 8 minutes, next with ultrapure water and dehydrated alcohol wash respectively 3 times,
It is freeze-dried again after being put into refrigerator freeze-drying to get the nanoscale Co-MOF presoma of morphological rules size uniformity is arrived.
(2) preparation of [email protected] 100mg Co-MOF presoma, ultrasonic disperse in 100ml Tris aqueous slkali,
25mg Dopamine hydrochloride is added afterwards, is persistently stirred 24 hours at room temperature after ultrasonic disperse, solution becomes black.Centrifuge separation produces
Object, revolving speed are that 10000rpm continues 10 minutes, and respectively with after water and ethanol washing, 60 DEG C are dried in vacuo 12 hours, be can be obtained
Co@PDA sample.
The preparation of Tris aqueous slkali is that 1.21g Trizmabase powder is distributed to 1000ml in the above-mentioned technical solutions
In ultrapure water, it is made in scheme and commonly uses Tris aqueous slkali.
(3) preparation of Co@NC/CNT.The Co@PDA sample and melamine powder that mass ratio is 1:10 are weighed, is added to
It is uniformly mixed it in agate mortar, next mixture is transferred in corundum Noah's ark, be sent into the quartz ampoule of tube furnace quasi-
Standby heat treatment, N is led into quartz ampoule2Half an hour to empty inner air tube, is next handled with typical two-part temperature program,
Diamond heating is kept the temperature 2 hours to 500 DEG C, continues to heat to 700 DEG C and keeps the temperature 2 hours, heating rate is 2 DEG C/
Min obtains Co@NC/CNT product after Temperature fall.
Embodiment 2:
Contrast sample is prepared basically according to method same as Example 1, is a difference in that and does not draw before the heat treatment
Enter melamine, dinectly bruning Co@PDA is passed through N2 half an hour first to empty inner air tube, next will during heating
Diamond heating keeps the temperature 2 hours to 700 DEG C, and heating rate is 2 DEG C/min, after Temperature fall, obtains contrast sample catalyst Co@
NC。
The present invention is described in further details it in conjunction with attached drawing after adopting the above technical scheme, mainly have the advantage that:
(1) technical solution is simple and easy, and product morphology is uniform controllable, can carry out large scale preparation.It is as shown in Figure 1
The SEM image of catalyst Co@NC/CNT, it can be seen that the size of Co@NC/CNT is about 900nm.Fig. 2 illustrates Co@NC/CNT
TEM image, the pattern of Co-MOF remains intact in figure, and has cobalt granule infiltration in surrounding carbon nanotube.Fig. 3 is Co@NC/
The XRD spectra of CNT and contrast sample, Co@NC/CNT and the XRD signal peak-to-average power of contrast sample can be marked with PDF as seen from the figure
Quasi- card is corresponding.Two kinds of catalyst 44.2 °, 51.5 ° and 75.9 ° of characteristic peak respectively correspond (111) of Co, (200) and
(220) crystal face.
(2) large specific surface area.According to Co@NC/CNT catalyst prepared by above-mentioned technical proposal, metal organic frame surface
The introducing of CNT increases the specific surface area of catalyst material.The generation for being incorporated as carbon nanotube of melamine provides carbon source.
It is as shown in Figure 4 and Figure 5 respectively the Co@NC/CNT prepared according to the technology of the present invention and contrast sample Co@NC catalyst not
With the cyclic voltammetry curve for sweeping the non-faraday area tested under speed.The Co@NC/CNT that is prepared by Fig. 6 according to the technology of the present invention and
Electrochemical surface area measurement result of contrast sample Co@NC catalyst under the conditions of 1.0 M KOH is it is found that according to skill of the present invention
The electrochemical surface area of the Co@NC/CNT of art preparation is almost 2 times of contrast sample [email protected]. 7 is Co@NC/CNT catalysis
The nitrogen adsorption desorption curve of agent.Fig. 8 is the pore size distribution curve of Co@NC/CNT catalyst.This is disclosed by Fig. 7 and Fig. 8 respectively
The specific surface area of the Co@NC/CNT catalyst of inventive technique example preparation is 75m2/ g and average pore size are 1.16nm.It uses simultaneously
Nickel foam does collector due to its unique open-celled structure, also increases the contact area of catalyst and electrolyte.To make Co@
The more active sites of NC/CNT catalyst exposure, and then improve catalytic efficiency.
(3) electro-catalysis analysis oxygen performance is good.Oxygen is analysed according to the nickel foam anode of the catalyst modification of above-mentioned technical proposal preparation
Electrode is 10mA/cm in current density2When overpotential be 302mV, be better than business noble metal catalyst RuO2(313mV), especially
Under high current density, catalytic performance is much better than business RuO2.The linear scan curve of Co@NC/CNT catalyst and comparative experiments
As shown in Figure 9.Tafel slope is the important parameter for disclosing catalytic mechanism, especially in terms of illustrating rate-determing step, by
Tafel equation (η=blogj+a) it is found that the smaller explanation of static Tafel slope (b) with current density increase, overpotential
Change smaller, shows rate-determing step in the end that multielectron transfer reacts, i.e. catalytic performance is better.Figure 10 is the present invention
The Tafel curve of prepared Co@NC/CNT catalyst and comparative experiments.It is known from figures that, prepared by the present invention
The Tafel slope of Co@NC/CNT catalysis analysis oxygen electrode is 50.34mV/dec, business RuO2The Tafel slope of electrode is
The Tafel slope that 73.75mV/dec, comparative catalyst Co@NC analyse oxygen electrode is 88.41mV/dec.The Tafel of Co@NC/CNT
Slope ratio RuO2It is all small with the Tafel slope of contrast sample Co@NC, illustrate the catalysis analysis oxygen of the Co@NC/CNT as prepared by the present invention
There is electrode more excellent electro-catalysis to analyse oxygen performance.
(4) stability is good.With the electrochemical stability of chronoamperometry assessment catalyst, pass through the electricity of control working electrode
Pressure, the current density for measuring working electrode change with time.As shown in figure 11, the Co@NC/ prepared according to above-mentioned technical proposal
After continuing working 28 hours under voltage is 1.55 V, current density becomes the nickel foam anode analysis oxygen electrode of CNT catalyst modification
It is original 80.6%.Illustrate that the Co@NC/CNT catalyst of above-mentioned technical proposal preparation has preferable electrochemical stability.
Claims (6)
1. a kind of preparation of Novel electrolytic water Oxygen anodic evolution catalyst Co@NC/CNT, it is characterised in that: material preparation method letter
Single controllable, pattern is uniform, is easy to large scale preparation.Preparation method includes following steps:
(1) preparation of Co-MOF；Potassium cobalticyanide, cobalt nitrate and sodium citrate are dispersed in ultrapure water, stood after magnetic agitation,
Pink precipitate is obtained, is centrifuged, washing obtains Co-MOF presoma after dry.
(2) preparation of Co@PDA；Step (1) Co-MOF obtained and Dopamine hydrochloride are dispersed in Tris alkali by a certain percentage
Co@PDA is centrifugally separating to obtain in solution, after stirring.
(3) preparation of Co@NC/CNT.After Co@PDA obtained by step (2) and melamine are sufficiently mixed, pass through in a nitrogen atmosphere
Typical two-part temperature program calcining is crossed, Co@NC/CNT catalyst is obtained.
2. a kind of Novel electrolytic water Oxygen anodic evolution catalyst Co@NC/CNT according to claim 1, it is characterised in that: institute
Stating the ratio of potassium cobalticyanide, cobalt nitrate and sodium citrate in step (1) is about 3:3:5.And the size of gained Co-MOF is about
It is 70~80m for 900nm and BET specific surface area2/g。
3. a kind of Novel electrolytic water Oxygen anodic evolution catalyst Co@NC/CNT according to claim 1, it is characterised in that: institute
Stating the ratio of Co-MOF and Dopamine hydrochloride in step (2) is about 4:1, and Dopamine hydrochloride can autohemagglutination under weak basic condition
Conjunction forms poly-dopamine (PDA).The spontaneous surface Co-MOF that is anchored on thin layer PDA forms carbon protective shell.
4. a kind of Novel electrolytic water Oxygen anodic evolution catalyst Co@NC/CNT according to claim 1, it is characterised in that: only
The ordered structure that would generally destroy MOF and porous pattern are calcined by presoma of MOF, Co PDA is being undergone in the step (3)
During calcining, carbon protects the presence of shell, it is made to maintain good pattern.
5. a kind of Novel electrolytic water Oxygen anodic evolution catalyst Co@NC/CNT according to claim 1, it is characterised in that: institute
Stating two-part holding temperature in step (3) is respectively 500 DEG C and 600~800 DEG C, and soaking time is respectively 2~4 hours.
6. a kind of Novel electrolytic water Oxygen anodic evolution catalyst Co@NC/CNT according to claim 1, it is characterised in that: institute
Stating the ratio of Co@PDA and melamine in step (3) is 1:10.Melamine has been catalyzed melamine as carbon source, the presence of Co
Amine grows up to carbon nanotube in a heated condition.
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