CN106111997B - A kind of preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material - Google Patents
A kind of preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material Download PDFInfo
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- CN106111997B CN106111997B CN201610481717.1A CN201610481717A CN106111997B CN 106111997 B CN106111997 B CN 106111997B CN 201610481717 A CN201610481717 A CN 201610481717A CN 106111997 B CN106111997 B CN 106111997B
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Abstract
The invention provides a kind of preparation method of porous nickel alloy electrolysis cathode for hydrogen evolution composite, is mainly used in electrolysis liberation of hydrogen technical field.The present invention uses powdered reaction synthetic method, by Ni, Fe, Mo, C, LaNi5Five kinds of powder prepare by a certain percentage, wherein Fe, Mo, C, LaNi5Powder accounts for 22.5 ~ 52wt% of total content altogether, and the powder prepared is well mixed, and adds 0.5 ~ 4% stearic acid, and green compact are obtained by pressure forming after drying, and carries out vacuum-sintering to green compact using the principle that solid phase spreads partially, you can obtain Ni Fe Mo C/LaNi5Porous electrolysis cathode material for hydrogen evolution.Porous electrolysis liberation of hydrogen composite cathode material produced by the present invention has the advantages that specific surface area is big, overpotential of hydrogen evolution is low, catalytic is good, excellent corrosion resistance, stable work in work, preparation technology are simple and environmentally-friendly, the exploitation important in inhibiting to hydrogen energy source.
Description
Technical field
The present invention relates to a kind of technology of preparing of porous nickel alloy material, and liberation of hydrogen composite cathode is electrolysed more particularly to one kind
The preparation method of material.
Background technology
Secondary energy sources of the hydrogen energy source as high effect cleaning, it is considered as one of following most potential new energy.Hydrogen energy source
Large-scale use will make the mankind enter green epoch of sustainable development, and hydrogen gas production largely, cheap be exploitation and
Utilize the important prerequisite of Hydrogen Energy.Hydrogen preparation method common at present has water electrolysis hydrogen production, biological hydrogen production, photocatalysis hydrogen production and change
The methods of stone fuel hydrogen manufacturing.In numerous hydrogen production process, the advantage of water electrolysis hydrogen production technology is the most notable：Hydrogen feedstock cost
It is low, resource is wide, equipment cost is low, hydrogen purity is high and in the absence of carbon emission problem.But current water electrolysis hydrogen production technology
Because hydrogen-precipitating electrode overpotential is high and stability is poor, cause energy consumption larger, should so as to limit the large-scale promotion of the technology
With.Therefore, the catalytic activity for hydrogen evolution and electro-catalysis stability for improving electrode have a very big significance.
Transition metal Ni electronic configuration is [Ar] 3d84s2, there is not paired 3d electronics, reacted in Electrocatalytic Activity for Hydrogen Evolution Reaction
In, it can be matched with hydrogen atom 1s tracks, form the Ni-H adsorption bonds of moderate strength, have excellent catalytic activity of hydrogen evolution and valency concurrently
Lattice advantage, thus it is acknowledged as the preferable alternate material of noble metal.In order to improve the catalytic activity of cathode hydrogen evolution electrode, Ni-based electricity
The development of pole mainly has three directions：Porous electrode, alloy electrode and combination electrode.Porous electrode is by improving the true of itself
Surface area so that catalytic active center increases, and the apparent catalytic activity of electrode is improved, so as to substantially increase electrolytic efficiency.
Alloy electrode includes Ni- metals and Ni- non-metal alloys.Theoretical, the d track underfills according to Engel-Brewer " volcano "
Or the metal (such as Fe, Co, Ni) on the transition system left side being partly full of with paired but the uncomfortable compound key in simple metal d electricity
When metal (such as W, Mo, Cr, La, Ha, Zr) on the right of the transition system of son is melt into alloy, evolving hydrogen reaction can be produced clearly
Electro-catalysis synergy.Such as patent CN102719846, by controlling electro-deposition current potential and electrolyte on three-dimensional nickel screen matrix
The electrochemical deposition Ni-Mo alloy layers of middle Ni and Mo concentration, anode etching is then carried out in ammonia solution and prepares Ni bases three
Tie up netted graded alloy cathode material for hydrogen evolution.Alloy electrode material specific surface area prepared by the technology is high, and overpotential of hydrogen evolution is small
In 100mV, catalytic performance is good, but used electrochemical deposition has the environmental protection such as preparation technology complexity and waste water and waste liquid and asked
Topic.Show that by increasing surface area and forming two methods of alloy the intrinsic catalytic activity of electrode can be effectively improved, improve electricity
Efficiency is solved, reduces energy consumption.But porous electrode and alloy electrode still have degeneration-resistant CURRENT OXIDATION ability, liberation of hydrogen it is unstable,
The problems such as coating easily peels off and service life is short.And power failure phenomenon unavoidably occurs in actual industrial operating process, it is more
Pore electrod and alloy electrode are easily corroded oxidation in power-off gap, substantially reduce catalytic activity for hydrogen evolution；And powered off in long-time
In the case of, catalyst component meeting solution modeling, hydrogen evolution activity is easy to lose and cause energy consumption increase even electrolysis to be interrupted.It is multiple
Composite electrode is embedded in the second phase solid particle (such as oxide, carbide and hydrogen storage material) in parent metal, forms composite alloy
Reach high catalytic performance.Hydrogen storing alloy powder LaNi5Particle is due to the ability with very strong absorption hydrogen so that power-off when
Wait, the hydrogen slow release of absorption comes out, prevents electrode surface to be oxidized, that is, serve protective effect.Such as patent CN
102899681 using Ni as matrix by composite electrodeposition by LaNi5It is embedded into Al particle capsules in coating and obtains Ni/ (LaNi5+Al)
Precursor, porous nickel combination electrode is obtained after then the aluminium in coating is dissolved using alkali solution technique, the electrode has excellent analysis
Hydrogen electrocatalysis characteristic and excellent stability.
The Ni-Fe-Mo-C/LaNi that the present invention is prepared using powdered reaction synthetic method5Porous electrode, there is higher ratio table
Good, the good stability of area, relatively low overpotential of hydrogen evolution, the corrosion resistance of relative good, anti-power-off short-circuit capacity, machinery
The advantages that intensity is high, preparation technology is simple and environmentally-friendly, the exploitation to hydrogen energy source have great significance with application.
The content of the invention
The present invention is for existing hydrogen-precipitating electrode catalytic activity is not high, corrosion resistance is bad, anti-power-off short-circuit capacity is poor, liberation of hydrogen
Unstable, the shortcomings of preparation technology is complicated, provides a kind of preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material.
The present invention provides a kind of preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material, its specific preparation method
Comprise the following steps：
(1) powder is prepared：By Ni, Fe, Mo, C, LaNi5Five kinds of powder prepare by a certain percentage, wherein Fe, Mo, C, LaNi5
Powder accounts for 22.5~52wt% of total content altogether；
(2) powder mixes：The powder prepared is well mixed, adds stearic acid, dries 5~14h；
(3) pressure forming：Dried powder is subjected to isostatic cool pressing, obtains green compact；
(4) green sintering：Green compact are placed in vacuum drying oven, keep 10~15 DEG C/min programming rate to be risen to from room temperature
100~130 DEG C, it is incubated 20~40min；Again 250~300 DEG C are warming up to 10~15 DEG C/min programming rate, insulation 20~
40min；Then 350~380 DEG C are warming up to 3~10 DEG C/min programming rate and are incubated 20~40min at such a temperature；Again
490~550 DEG C are warming up to 10~15 DEG C/min programming rate and are incubated 30~50min at such a temperature；Then with 3~10
DEG C/min programming rate is warming up to 590~640 DEG C and is incubated 50~80min at such a temperature；Again with 10~15 DEG C/min's
Programming rate is warming up to 800~1000 DEG C and is incubated 30~50min at such a temperature；Cool to room temperature with the furnace, that is, obtain being sent out
Bright porous electrolysis cathode material for hydrogen evolution.
Preferably, the powder diameter of Ni powder described in step (1) is 3~5 μm, and percentage is 48~77.5wt%..
Preferably, the powder diameter of Fe powder described in step (1) is 3~5 μm, and percentage is 20~30wt%.
Preferably, the powder diameter of Mo powder described in step (1) is 3~5 μm, and percentage is 1~10wt%.
Preferably, the percentage of C powder described in step (1) is 1~10wt%.
Preferably, LaNi described in step (1)5The powder diameter of alloyed powder is 10~80 μm, LaNi5The percentage of powder is
0.5~2wt%.
Preferably, step (2) stearic addition is the 0.5~4% of powder total mass fraction.
Preferably, the pressure of powder compacting is 50MPa~250MPa in step (3), and the dwell time is 2~3min.
Preferably, the vacuum in step (4) in vacuum drying oven is 1 × 10-2Pa~1 × 10-3Pa。
Preferably, C powder used is carbon black in step (1), LaNi5Powder is AB5Type hydrogen storage alloy.
The advantages of present invention uses above-mentioned technical proposal is：
(1) internal void enriches, and specific surface area is big.The present invention utilizes diffusion generation partially between element powders in sintering process
A large amount of holes, material internal duct is crisscross, interpenetrates, and porosity is 30%~60%, and aperture is 1~10 μm, micron
The loose structure of level is easy to gas transport, is advantageous to the progress of evolving hydrogen reaction.
(2) overpotential of hydrogen evolution is low, and catalytic is good.The present invention is reduced using the catalyzing cooperation effect between Mo and Ni, Fe
Overpotential of hydrogen evolution, improve electrode catalyst activity；The hole formed using sintering increases material surface roughness, and specific surface area increases
Add, catalytic active center point increases, and improves electrolytic efficiency, and catalytic performance is good.
(3) excellent corrosion resistance, have good stability.The present invention is from the nickel itself with excellent anticorrosive performance as conjunction
Auri body, dielectric corrosion can be resisted；Utilize LaNi5Hydrogen storage function, in the intermittent electrolysis of electrode and long-time power process
In by adsorb hydrogen cathodic discharge react, avoid the dissolution of cathode active ingredient, so as to play a protective role, improve electrode material
The stability in use of material.
(4) excellent in mechanical performance, service life length.The nickel alloy electrolysis that the present invention is obtained using solid-phase sintering technology of preparing
Liberation of hydrogen composite cathode material has excellent in mechanical performance, and high mechanical strength, good toughness, high temperature resistant is wear-resistant, service life length etc.
Advantage, meet practical application in industry requirement.
(5) it is economic and environment-friendly, can industrialized production.Ni, Fe used in the present invention, Mo, C element powder wide material sources, valency
Lattice are cheap；The present invention is using powdered reaction synthesis hair technology of preparing, and utilization rate of raw materials is high, preparing cost, low, technique briefly may be used
Control, and produced without industrial wastewater, be advantageous to environmental protection, be adapted to industrial-scale production.
Brief description of the drawings
Fig. 1 is the Ni-Fe-Mo-C/LaNi prepared in embodiment 15The surface topography map of porous electrode.
Fig. 2 is the Ni-Fe-Mo-C/LaNi prepared in embodiment 15The cathodic polarization curve of porous electrode.
Embodiment
Herein below provides the representative embodiment of the present invention, and these embodiments are only exemplary, and are not used in limit
Invention as described herein scope processed, these embodiments are merely to illustrate embodiments of the invention.
Embodiment 1
By Ni, Fe, Mo, C, LaNi5Five kinds of powder prepare in proportion, and wherein Fe contents are 25wt%, and powder diameter is 3 μ
m；Mo contents are 5wt%, and powder diameter is 3 μm；C content is 5wt%；LaNi5Content is 1wt%, and powder diameter is 80 μm.Will
The powder prepared is placed on V-type and mixes the stearic acid at the uniform velocity being mixed on powder machine and powder gross mass 2% being added after 10h, re-dry 10h,
With 250MPa pressure cold-press moulding, dwell time it is about 2min under cold press；The sample pressed is placed in vacuum drying oven,
Vacuum is 1 × 10-2Keep 10 DEG C/min programming rate to rise to 100 DEG C from room temperature in the case of Pa, be incubated 30min；Again with
10 DEG C/min programming rate is warming up to 250 DEG C, is incubated 30min；Then 350 DEG C are warming up to simultaneously with 10 DEG C/min programming rate
30min is incubated at such a temperature；490 DEG C are warming up to 10 DEG C/min programming rate and be incubated 30min at such a temperature again；So
590 DEG C are warming up to 10 DEG C/min programming rate and be incubated 60min at such a temperature afterwards；Again with 10 DEG C/min programming rate
It is warming up to 800 DEG C and is incubated 40min at such a temperature, then cool to room temperature with the furnace, it is porous nickel alloy electricity to obtain material
Solve liberation of hydrogen composite cathode material.The micromorphology figure of resulting materials is as shown in Figure 1.Material as shown in Figure 1 has abundant
Interconnected pore, and even pore distribution, pore size is at 1 μm~10 μm.
In order to study the catalytic hydrogen evolution performance of porous nickel alloy electrolysis liberation of hydrogen composite cathode material, the sample of formation will be fired
A 1cm is left with epoxy resin fixing seal2Geometrical surface, electro-chemical test is carried out in 6mol/L KOH solution.
Electro-chemical test uses standard three electrode system：Auxiliary electrode is platinized platinum；Reference electrode is Hg/HgO；Working electrode is made for sintering
The Ni-Fe-Mo-C/LaNi obtained5Porous electrode.Tester used in the present invention is CS350 electrochemical workstations, sweep speed
For 1mVs-1, scanning range is 0V~-2V, and test temperature is kept for 30 DEG C using water bath with thermostatic control.First electrode is carried out before testing
Cyclic voltammetry scan -1.0V~0.2V removes the impurity of electrode surface and unstable material so as to activated electrode.Ni-Fe-
Mo-C/LaNi5As shown in Fig. 2 when electrode potential reaches -1.6V, current density is the cathodic polarization curve of porous electrode
0.30A/cm2。
Embodiment 2
By Ni, Fe, Mo, C, LaNi5Five kinds of powder prepare in proportion, and wherein Fe contents are 30wt%, and powder diameter is 3 μ
m；Mo contents are 10wt%, and powder diameter is 3 μm；C content is 10wt%；LaNi5Content is 2wt%, and powder diameter is 80 μm.
The powder prepared is placed on after at the uniform velocity mixing 10h on the mixed powder machine of V-type, adds the stearic acid of powder gross mass 1%, re-dry
8h, with 200MPa pressure cold-press moulding, dwell time it is about 2min under cold press；The sample pressed is placed in vacuum drying oven
In, it is 1 × 10 in vacuum-2Keep 10 DEG C/min programming rate to rise to 120 DEG C from room temperature in the case of Pa, be incubated 30min；
280 DEG C are warming up to 10 DEG C/min programming rate again, is incubated 30min；Then 360 are warming up to 10 DEG C/min programming rate
DEG C and be incubated 40min at such a temperature；500 DEG C are warming up to 10 DEG C/min programming rate and be incubated at such a temperature again
30min；Then 600 DEG C are warming up to 10 DEG C/min programming rate and are incubated 70min at such a temperature；Again with 10 DEG C/min's
Programming rate is warming up to 920 DEG C and is incubated 30min at such a temperature, then cools to room temperature with the furnace, it is as porous to obtain material
Nickel alloy electricity solution liberation of hydrogen composite cathode material.
Repeat the sample preparation in embodiment 1 and electrochemistry experiment step carries out electrochemistry experiment again, obtain similar to Example 1
Pore structure and chemical property.
Embodiment 3
By Ni, Fe, Mo, C, LaNi5Five kinds of powder prepare in proportion, and wherein Fe contents are 25wt%, and powder diameter is 3 μ
m；Mo contents are 1wt%, and powder diameter is 3 μm；C content is 1wt%；LaNi5Content is 0.5wt%, and powder diameter is 30 μm.
The powder prepared is placed on after at the uniform velocity mixing 10h on the mixed powder machine of V-type, adds the stearic acid of powder gross mass 1.5%, re-dry
9h, with 50MPa pressure cold-press moulding, dwell time it is about 3min under cold press；The sample pressed is placed in vacuum drying oven,
It is 1 × 10 in vacuum-2Keep 10 DEG C/min programming rate to rise to 130 DEG C from room temperature in the case of Pa, be incubated 20min；Again
300 DEG C are warming up to 10 DEG C/min programming rate, is incubated 20min；Then 380 DEG C are warming up to 10 DEG C/min programming rate
And 20min is incubated at such a temperature；550 DEG C are warming up to 10 DEG C/min programming rate and be incubated 40min at such a temperature again；
Then 640 DEG C are warming up to 10 DEG C/min programming rate and are incubated 50min at such a temperature；Again with 10 DEG C/min heating speed
Degree is warming up to 1000 DEG C and is incubated 40min at such a temperature, then cools to room temperature with the furnace, it is porous nickel alloy to obtain material
It is electrolysed liberation of hydrogen composite cathode material.
Repeat the sample preparation in embodiment 1 and electrochemistry experiment step carries out electrochemistry experiment again, obtain similar to Example 1
Pore structure and chemical property.
Embodiment 4
By Ni, Fe, Mo, C, LaNi5Five kinds of powder prepare in proportion, and wherein Fe contents are 28wt%, and powder diameter is 3 μ
m；Mo contents are 5wt%, and powder diameter is 3 μm；C content is 2wt%；LaNi5Content is 0.5wt%, and powder diameter is 50 μm.
The powder prepared is placed on after at the uniform velocity mixing 10h on the mixed powder machine of V-type, adds the stearic acid of powder gross mass 3%, re-dry
12h, with 150MPa pressure cold-press moulding, dwell time it is about 3min under cold press；The sample pressed is placed in vacuum drying oven
In, it is 1 × 10 in vacuum-2Keep 10 DEG C/min programming rate to rise to 120 DEG C from room temperature in the case of Pa, be incubated 20min；
280 DEG C are warming up to 10 DEG C/min programming rate again, is incubated 20min；Then 370 are warming up to 10 DEG C/min programming rate
DEG C and be incubated 20min at such a temperature；510 DEG C are warming up to 10 DEG C/min programming rate and be incubated at such a temperature again
30min；Then 630 DEG C are warming up to 10 DEG C/min programming rate and are incubated 70min at such a temperature；Again with 10 DEG C/min's
Programming rate is warming up to 940 DEG C and is incubated 40min at such a temperature, then cools to room temperature with the furnace, it is as porous to obtain material
Nickel alloy electricity solution liberation of hydrogen composite cathode material.
Repeat the sample preparation in embodiment 1 and electrochemistry experiment step carries out electrochemistry experiment again, obtain similar to Example 1
Pore structure and chemical property.
Embodiment 5
By Ni, Fe, Mo, C, LaNi5Five kinds of powder prepare in proportion, and wherein Fe contents are 20wt%, and powder diameter is 5 μ
m；Mo contents are 10wt%, and powder diameter is 5 μm；C content is 5wt%；LaNi5Content is 1wt%, and powder diameter is 50 μm.
The powder prepared is placed on after at the uniform velocity mixing 10h on the mixed powder machine of V-type, adds the stearic acid of powder gross mass 2%, re-dry
9h, with 50MPa pressure cold-press moulding, dwell time it is about 3min under cold press；The sample pressed is placed in vacuum drying oven,
It is 1 × 10 in vacuum-2Keep 10 DEG C/min programming rate to rise to 110 DEG C from room temperature in the case of Pa, be incubated 20min；Again
270 DEG C are warming up to 10 DEG C/min programming rate, is incubated 20min；Then 360 DEG C are warming up to 10 DEG C/min programming rate
And 20min is incubated at such a temperature；520 DEG C are warming up to 10 DEG C/min programming rate and be incubated 30min at such a temperature again；
Then 620 DEG C are warming up to 10 DEG C/min programming rate and are incubated 70min at such a temperature；Again with 10 DEG C/min heating speed
Degree is warming up to 900 DEG C and is incubated 40min at such a temperature, then cools to room temperature with the furnace, it is porous nickel alloy to obtain material
It is electrolysed liberation of hydrogen composite cathode material.
Repeat the sample preparation in embodiment 1 and electrochemistry experiment step carries out electrochemistry experiment again, obtain similar to Example 1
Pore structure and chemical property.
Embodiment 6
By Ni, Fe, Mo, C, LaNi5Five kinds of powder prepare in proportion, and wherein Fe contents are 23wt%, and powder diameter is 5 μ
m；Mo contents are 8wt%, and powder diameter is 5 μm；C content is 2wt%；LaNi5Content is 1wt%, and powder diameter is 10 μm.Will
The powder prepared is placed on after V-type mixes and at the uniform velocity mix 10h on powder machine, adds the stearic acid of powder gross mass 4%, re-dry 10h,
With 100MPa pressure cold-press moulding, dwell time it is about 3min under cold press；The sample pressed is placed in vacuum drying oven,
Vacuum is 1 × 10-2Keep 10 DEG C/min programming rate to rise to 120 DEG C from room temperature in the case of Pa, be incubated 40min；Again with
10 DEG C/min programming rate is warming up to 300 DEG C, is incubated 40min；Then 380 DEG C are warming up to simultaneously with 10 DEG C/min programming rate
40min is incubated at such a temperature；530 DEG C are warming up to 10 DEG C/min programming rate and be incubated 30min at such a temperature again；So
600 DEG C are warming up to 10 DEG C/min programming rate and be incubated 60min at such a temperature afterwards；Again with 10 DEG C/min programming rate
It is warming up to 850 DEG C and is incubated 30min at such a temperature, then cool to room temperature with the furnace, it is porous nickel alloy electricity to obtain material
Solve liberation of hydrogen composite cathode material.
Repeat the sample preparation in embodiment 1 and electrochemistry experiment step carries out electrochemistry experiment again, obtain similar to Example 1
Pore structure and chemical property.
Embodiment 7
By Ni, Fe, Mo, C, LaNi5Five kinds of powder prepare in proportion, and wherein Fe contents are 22wt%, and powder diameter is 5 μ
m；Mo contents are 5wt%, and powder diameter is 5 μm；C content is 3wt%；LaNi5Content is 2wt%, and powder diameter is 50 μm.Will
The powder prepared is placed on after V-type mixes and at the uniform velocity mix 10h on powder machine, adds the stearic acid of powder gross mass 0.5%, re-dry
8h, with 50MPa pressure cold-press moulding, dwell time it is about 3min under cold press；The sample pressed is placed in vacuum drying oven,
It is 1 × 10 in vacuum-2Keep 10 DEG C/min programming rate to rise to 110 DEG C from room temperature in the case of Pa, be incubated 20min；Again
260 DEG C are warming up to 10 DEG C/min programming rate, is incubated 30min；Then 370 DEG C are warming up to 10 DEG C/min programming rate
And 20min is incubated at such a temperature；520 DEG C are warming up to 10 DEG C/min programming rate and be incubated 40min at such a temperature again；
Then 630 DEG C are warming up to 10 DEG C/min programming rate and are incubated 70min at such a temperature；Again with 10 DEG C/min heating speed
Degree is warming up to 960 DEG C and is incubated 30min at such a temperature, then cools to room temperature with the furnace, it is porous nickel alloy to obtain material
It is electrolysed liberation of hydrogen composite cathode material.
Repeat the sample preparation in embodiment 1 and electrochemistry experiment step carries out electrochemistry experiment again, obtain similar to Example 1
Pore structure and chemical property.
The embodiment is to the illustrative present invention, not for the limitation present invention.Any those skilled in the art
The embodiment can be modified under the spirit and scope without prejudice to the present invention, therefore the rights protection model of the present invention
Enclose, should be as listed by the claim of the present invention.
Claims (10)
1. a kind of preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material, its specific preparation method include：
(1) powder is prepared：By Ni, Fe, Mo, C, LaNi5Five kinds of powder prepare by a certain percentage, wherein Fe, Mo, C, LaNi5Account for altogether
22.5~52wt% of total content；
(2) powder mixes：The powder prepared is well mixed, adds stearic acid, dries 5~14h；
(3) pressure forming：Dried powder is subjected to isostatic cool pressing, obtains green compact；
(4) green sintering：Green compact are placed in vacuum drying oven, keep 10~15 DEG C/min programming rate rise to 100 from room temperature~
130 DEG C, it is incubated 20~40min；250~300 DEG C are warming up to 10~15 DEG C/min programming rate again, is incubated 20~40min；
Then 350~380 DEG C are warming up to 3~10 DEG C/min programming rate and are incubated 20~40min at such a temperature；Again with 10~
15 DEG C/min programming rate is warming up to 490~550 DEG C and is incubated 30~50min at such a temperature；Then with 3~10 DEG C/min
Programming rate be warming up to 590~640 DEG C and at such a temperature be incubated 50~80min；Again with 10~15 DEG C/min heating speed
Degree is warming up to 800~1000 DEG C and is incubated 30~50min at such a temperature；Cool to room temperature with the furnace, that is, obtain porous nickel alloy
It is electrolysed liberation of hydrogen composite cathode material.
2. the preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material according to claim 1, it is characterised in that
The powder diameter of Ni powder is 3~5 μm in the step (1), and percentage is 48~77.5wt%.
3. the preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material according to claim 1, it is characterised in that
The powder diameter of Fe powder is 3~5 μm in the step (1), and percentage is 20~30wt%.
4. the preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material according to claim 1, it is characterised in that
The powder diameter of Mo powder is 3~5 μm in the step (1), and percentage is 1~10wt%.
5. the preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material according to claim 1, it is characterised in that
The percentage of C powder is 1~10wt% in the step (1).
6. the preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material according to claim 1, it is characterised in that
LaNi in the step (1)5The powder diameter of alloyed powder is 10~80 μm, LaNi5The percentage of powder is 0.5~2wt%.
7. the preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material according to claim 1, it is characterised in that
Stearic addition accounts for the 0.5~4% of powder total mass fraction described in step (2).
8. the preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material according to claim 1, it is characterised in that
The pressure of powder compacting is 50MPa~250MPa in the step (3), and the dwell time is 2~3min.
9. the preparation method of porous nickel alloy electrolysis liberation of hydrogen composite cathode material according to claim 1, it is characterised in that
Vacuum in the step (4) in vacuum drying oven is 1 × 10-2~1 × 10-3Pa。
10. the system of the porous nickel alloy electrolysis liberation of hydrogen composite cathode material according to any claim in claim 1 to 9
Preparation Method, it is characterised in that C powder used in the step (1) is carbon black, LaNi5Powder is AB5Type hydrogen storage alloy.
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| CN107268019A (en) * | 2017-06-16 | 2017-10-20 | 湘潭大学 | A kind of porous Ni-base alloy is electrolysed the preparation method of cathode material for hydrogen evolution |
| CN108247060A (en) * | 2018-01-14 | 2018-07-06 | 湘潭大学 | A kind of preparation method of nickel-base alloy electrolysis cathode for hydrogen evolution porous material |
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| NL7511044A (en) * | 1975-09-19 | 1977-03-22 | Philips Nv | ELECTRODE FOR PRIMARY OR SECONDARY BATTERY AND PROCEDURE FOR MANUFACTURE OF SUCH ELECTRODE. |
| JPS5949669B2 (en) * | 1976-09-07 | 1984-12-04 | 松下電器産業株式会社 | Hydrogen storage electrode |
| NO325620B1 (en) * | 2003-10-21 | 2008-06-30 | Revolt Technology Ltd | Electrode, Method of Preparation thereof, Metal / Air Fuel Cell and Metal Hydride Battery Cell |
| CN1291510C (en) * | 2004-05-28 | 2006-12-20 | 中国科学院上海微***与信息技术研究所 | Non-cobalt negative material of metal hydrogen storage/nickel battery and preparing method thereof |
| CN101633985A (en) * | 2009-05-21 | 2010-01-27 | 瑞科稀土冶金及功能材料国家工程研究中心有限公司 | Preparation method of RE-Fe-B part hydrogen storage alloy |
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