CN103042217B - A kind of preparation method of water electrolysis hydrogen production electrode material - Google Patents
A kind of preparation method of water electrolysis hydrogen production electrode material Download PDFInfo
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- CN103042217B CN103042217B CN201210508704.0A CN201210508704A CN103042217B CN 103042217 B CN103042217 B CN 103042217B CN 201210508704 A CN201210508704 A CN 201210508704A CN 103042217 B CN103042217 B CN 103042217B
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 55
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 55
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 42
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000007772 electrode material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 43
- 238000009413 insulation Methods 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000010792 warming Methods 0.000 claims abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 11
- 238000009826 distribution Methods 0.000 abstract description 8
- 239000010406 cathode material Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 25
- 239000011148 porous material Substances 0.000 description 12
- 229910003310 Ni-Al Inorganic materials 0.000 description 7
- 239000000446 fuel Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000005329 float glass Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Landscapes
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention discloses a kind of preparation method of water electrolysis hydrogen production electrode material, described method is carried out as follows: (1) cold moudling: Ni powder and Al powder are mixed and made into mixture, then pressed compact are made in mixture cold moudling; Based on described Ni powder and Al powder, described Ni grain weight amount 80 ~ 95%, 5 ~ 20% of described Al grain weight amount; (2) sinter, cool: pressed compact is heated to 350 ~ 500 DEG C under vacuum, insulation 60 ~ 90min, is then warming up to 700 ~ 950 DEG C, and insulation 30 ~ 120min, is cooled to room temperature, obtains described water electrolysis hydrogen production electrode material; Water electrolysis hydrogen production electrode material of the present invention, even aperture distribution, it has high-ratio surface, high activity, service life is longer, and catalytic efficiency is high, and production method is simple, cost is low, for water electrolysis hydrogen production provides a kind of selection of new cathode material, has broad application prospects.
Description
(1) technical field
The present invention relates to a kind of preparation of electrode, particularly a kind of preparation method of water electrolysis hydrogen production electrode material.
(2) background technology
The energy and environment are two necessary conditions realizing sustainable development.Fuel cell, with the advantage of its uniqueness, is considered to most promising car power source, and its extensive use can alleviate the pressure of the energy and environmental protection two aspect.Compared with methyl alcohol, other fossil fuels, the application of hydrogen is very wide, as fields such as electronics industry, metallurgical industry, food processing, float glass, fine chemistry industries.Hydrogen, as the energy, is the fuel of following generating, fuel cell used for electric vehicle.Make fuel with hydrogen, oxygen makes oxidant, by the combustion reaction of fuel, is the hydrogen-oxygen fuel cell of electric energy by converts chemical energy, is rising new electrical source of power.This battery has the advantages such as conversion efficiency is high, capacity is large, specific energy is high, power bracket is wide, need not charge.
The method of current industrial water electrolysis hydrogen production mainly contains: one be by steam by scorching hot coke (being called carbon reduction method), obtain the hydrogen that purity is about 75%; Two be by steam by scorching hot iron, obtain the hydrogen of purity below 97%; Three is extract hydrogen by water-gas, and the hydrogen purity obtained is also lower; 4th kind of method is exactly water electrolysis method, and obtained hydrogen purity can up to more than 99%, and this is the industrial a kind of important method preparing hydrogen.Employing the method hydrogen manufacturing cost is low, hydrogen content is high, can meet the needs of hydrogen fuel cell.But adopt in the method hydrogen production process and various side reaction meeting also can occur to system introducing foreign gas, thus bring certain interference to the purification of hydrogen.The problems such as Raney Ni is a kind of porous cathode material as electrolytic hydrogen production, but it exists aperture too small (being often less than 10nm), and in liberation of hydrogen process, hydrogen gets lodged in hole and can not get rid of in time, active reduction.
Key technology of the present invention is to adopt thinner Ni, Al powder to make the porous material that aperture is normal distribution, and is incorporated into electrolytic hydrogen production field, has opened up the application of porous intermetallic compound.
(3) summary of the invention
The object of the invention is to provide one to be had and enriches specific surface, and the porous cathode material that aperture is relatively large, and namely a kind of have high-ratio surface, the water electrolysis hydrogen production electrode material of high catalytic activity and preparation method.
The technical solution used in the present invention is:
A preparation method for water electrolysis hydrogen production electrode material, described method is carried out as follows: (1) cold moudling: Ni powder and Al powder are mixed and made into mixture, then pressed compact are made in mixture cold moudling; Described Ni powder and the powder diameter of Al powder are 1 ~ 15 μm, based on described Ni powder and Al powder, and described Ni grain weight amount 80 ~ 95%, 5 ~ 20% of described Al grain weight amount; (2) sinter, cool: by pressed compact 1 × 10
-2~ 1 × 10
-3heated under vacuum to 350 ~ 500 DEG C of Pa, insulation 60 ~ 90min, is then warming up to 700 ~ 950 DEG C, and insulation 30 ~ 120min, is cooled to room temperature, obtains described water electrolysis hydrogen production electrode material.
Further, described Ni powder average grain diameter is 1 ~ 8 μm.
Further, described Al powder average grain diameter is 1 ~ 8 μm.
Further, described Ni grain weight amount is 85 ~ 95% of Ni powder and Al powder gross weight.
Further, the described mixture cold moudling of step (1) carries out under the condition in pressurize 10 second under 80 ~ 300Mpa, preferably under 150Mpa pressurize 10 second condition under carry out.
Further, the condition of step (2) described sintering, cooling is: by pressed compact 1 × 10
-3350 ~ 500 DEG C are at the uniform velocity warming up to the speed of 5 ~ 8 DEG C/min under Pa vacuum condition, insulation 60 ~ 90min, and then be at the uniform velocity warming up to 700 ~ 950 DEG C with the speed of 5 ~ 8 DEG C/min, insulation 30 ~ 120min, be cooled to room temperature, obtain described water electrolysis hydrogen production electrode material.
Further, the preparation method of water electrolysis hydrogen production electrode material of the present invention is recommended as: (1) cold moudling: Ni powder and Al powder are mixed and made into mixture, then pressed compact are made in mixture cold moudling; Based on described Ni powder and Al powder, described Ni grain weight amount 85 ~ 95%, 5 ~ 15% of described Al grain weight amount; Described Ni powder average grain diameter is 3 ~ 8 μm, and described Al powder average grain diameter is 3 ~ 8 μm; (2) sinter, cool: by pressed compact 1 × 10
-3with 5 ~ 8 DEG C/min(preferably 5 DEG C/min under Pa vacuum condition) speed be at the uniform velocity warming up to 400 ~ 500 DEG C, the preferred 60min of insulation 60 ~ 80min(), then with 5 ~ 8 DEG C/min(preferably 5 DEG C/min) speed be at the uniform velocity warming up to 750 ~ 950 DEG C, the preferred 60min of insulation 60 ~ 120min(), be cooled to room temperature, obtain described water electrolysis hydrogen production electrode material.
The present invention compared with prior art, has the following advantages:
(1) preparation technology of water electrolysis hydrogen production electrode material of the present invention (i.e. Ni-Al porous material) is simple, and sintering temperature is low, and in preparation process, energy consumption is low.
(2) the Ni-Al porous material obtained by the present invention, make full use of the mesopore in fine powder pressed compact between powder size and the reaction pore-creating in sintering process, obtained pore structure size uniform, present normal distribution, and hole enriches, porosity reaches 35-45%, and porous cathode material specific area is large.
(3) the Ni-Al porous cathode material obtained by, the crystallite dimension in its skeleton structure is tiny, and average grain size is 14 ran, has high catalytic activity.
(4) the Ni-Al porous material obtained by has excellent alkali-resistant property energy, and therefore it can keep good Pore Characteristics and good catalytic stability in electrolytic process.
In a word, water electrolysis hydrogen production electrode material of the present invention, even aperture distribution, it has high-ratio surface, high activity, service life is longer, and catalytic efficiency is high, and production method is simple, cost is low, for water electrolysis hydrogen production provides a kind of selection of new cathode material, has broad application prospects.
(4) accompanying drawing explanation
Fig. 1 is the SEM figure of water electrolysis hydrogen production electrode material prepared by embodiment 1.
Fig. 2 is the graph of pore diameter distribution of water electrolysis hydrogen production electrode material prepared by embodiment 1.
(5) detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment 1 water electrolysis hydrogen production electrode catalyst active testing
Adopt average grain diameter to be the nickel powder of 3 microns and average grain diameter to be the aluminium powder of 3 microns, the proportioning accounting for Ni powder and Al powder gross weight 15wt% by Ni grain weight amount is carried out batch mixing and is made mixture, then strip pressed compact is made in mixture pressurize 10 cold moudling in second under the pressure of 150MPa, pressed compact is wide is 6mm, thickness is 2mm, and length is 6mm.Pressed compact is placed in 1 × 10
-3under Pa vacuum condition, first rise to 500 DEG C with the heating rate of 5 DEG C/min, insulation 1h; Then 900 DEG C are risen to the heating rate of 5 DEG C/min, insulation 1h; Finally cool to room temperature (25 DEG C) with the furnace, obtain described water electrolysis hydrogen production electrode material.Adopt spot welding from extraction electrode line electrode material afterwards.Water electrolysis hydrogen production electrode material of the present invention is porous material, and the PoreMaster 60GT mercury injection apparatus test adopting Kang Ta instrument company of the U.S. to produce show that its most of pore-size distribution is between 1 ~ 2 micron, and porosity is 40%.As shown in Figure 1, pore-size distribution as shown in Figure 2 for the microscopic appearance figure (SEM) of obtained electrode.
Measure catalytic activity of the present invention, concrete technological parameter is as follows:
First N is used before electrolysis determination of activity
2catch up with gas, the decomposition voltage activation 5min of-1.5V is adopted afterwards in the conventional alkaline electrolyte (being generally the KOH aqueous solution) of 6mol/L, leave standstill 15min, afterwards with the speed on-load voltage of 10mV/S, measure effective current density in liberation of hydrogen current density and unit are.The results are shown in Table 1, Ni sheet and nickel foam all purchased from Changsha Liyuan New Material Co., Ltd., geometric area and water electrolysis hydrogen production electrode prepared by porous Ni-Al(and the present invention) identical.The catalytic activity that the exchange current density of Ni-Al porous material of the present invention, take-off potential and the current density value under same potential all show this invention material will be much better than pure nickel and nickel foam.
The electro catalytic activity data of the electrode that table 1 obtains in linear sweep limits
Embodiment 2: water electrolysis hydrogen production electrode catalyst active testing
Adopt average grain diameter to be the nickel powder of 8 microns and average grain diameter to be the aluminium powder of 8 microns, the proportioning accounting for Ni powder and Al powder gross weight 15wt% by Ni grain weight amount is carried out batch mixing and is made mixture, then strip pressed compact is made in mixture pressurize 10 cold moudling in second under the pressure of 150MPa, pressed compact is wide is 6mm, thickness is 2mm, and length is 6mm.Pressed compact is placed in 1 × 10
-3under Pa vacuum condition, first rise to 450 DEG C with the heating rate of 5 DEG C/min, insulation 1h; Then 900 DEG C are risen to the heating rate of 5 DEG C/min, insulation 1h; Finally cool to room temperature with the furnace, obtain described water electrolysis hydrogen production electrode material.Adopt spot welding from extraction electrode line electrode material afterwards.Water electrolysis hydrogen production electrode material of the present invention is porous material, and its most of pore-size distribution is between 3 ~ 5 microns, and porosity is 35%, and the surface roughness of electrode is 530 microns.The catalytic activity method of testing of electrode is as embodiment 1, and its take-off potential is-0.9V vs Hg/HgO, and exchange current density is 1.8mA/cm
2.
Embodiment 3: water electrolysis hydrogen production electrode catalyst stability test
Water electrolysis hydrogen production electrode embodiment 1 prepared carries out catalytic stability test, and assay method is cyclic voltammetry, and scanning potential region is-0.7 ~-1.4V, and sweep speed is 10mV/s, and the scan period is 500 circulations, and other conditional parameter is as follows:
The geometric area 1cm of working electrode of the present invention
2
Result is as shown in table 2, and Ni-Al porous material of the present invention has the catalytic stability of excellent electrolytic hydrogen production as can be seen from the table.
Current density value under the-1.39V current potential that table 2 cyclic voltammetric records
Embodiment 4 water electrolysis hydrogen production electrode alkali-resistant property can be tested
Water electrolysis hydrogen production electrode embodiment 1 prepared carries out alkali-resistant property can be tested, assay method is that the electrode of 0.5142g is immersed in 90 DEG C, in the 6M/L KOH aqueous solution, within every 10 hours, take out, use distilled water ultrasonic cleaning, dry, weigh, be reentered into 90 DEG C more afterwards, in the 6M/L KOH aqueous solution.Obtained electrode was through 2000 hours, and the weight of electrode maintains about 0.5130g, and the porosity of electrode and pore size are substantially constant.
Claims (3)
1. the preparation method of a water electrolysis hydrogen production electrode material, it is characterized in that described method is carried out as follows: (1) cold moudling: Ni powder and Al powder are mixed and made into mixture, then second is made pressed compact in mixture pressurize 10 under 80 ~ 300MPa; Described Ni powder and the powder diameter of Al powder are 1 ~ 8 μm, and based on described Ni powder and Al powder, described Ni grain weight amount is 80 ~ 95%, and described Al grain weight amount is 5 ~ 20%; (2) sinter, cool: by pressed compact 1 × 10
-3350 ~ 500 DEG C are at the uniform velocity warming up to the speed of 5 ~ 8 DEG C/min under the vacuum condition of Pa, insulation 60 ~ 90min, and then be at the uniform velocity warming up to 700 ~ 950 DEG C with the speed of 5 ~ 8 DEG C/min, insulation 30 ~ 120min, be cooled to room temperature, obtain described water electrolysis hydrogen production electrode material.
2. the preparation method of water electrolysis hydrogen production electrode material as claimed in claim 1, is characterized in that described Ni grain weight amount is 85 ~ 95%.
3. the preparation method of water electrolysis hydrogen production electrode material as claimed in claim 1, is characterized in that described method is: (1) cold moudling: Ni powder and Al powder are mixed and made into mixture, then pressed compact are made in mixture cold moudling; Based on described Ni powder and Al powder, described Ni grain weight amount is 85 ~ 95%, and described Al grain weight amount is 5 ~ 15%, and described Ni powder footpath is 3 ~ 8 μm, and described Al powder footpath is 3 ~ 8 μm; (2) sinter, cool: by pressed compact 1 × 10
-3400 ~ 500 DEG C are at the uniform velocity warming up to the speed of 5 ~ 8 DEG C/min under Pa vacuum condition, insulation 60 ~ 80min, is then at the uniform velocity warming up to 750 ~ 950 DEG C with the speed of 5 ~ 8 DEG C/min, insulation 60 ~ 120min, be cooled to room temperature, obtain described water electrolysis hydrogen production electrode material.
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| 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 |
| CN108380882B (en) * | 2018-02-05 | 2020-12-18 | 湘潭大学 | Ni-Cr-Al-Cu porous material and preparation method thereof |
| CN109055973B (en) * | 2018-07-09 | 2020-04-21 | 太原理工大学 | Preparation and use methods of aluminum-doped three-dimensional nano porous metal sulfide hydrogen evolution electrode |
| CN110438525A (en) * | 2019-08-08 | 2019-11-12 | 广东省新材料研究所 | A kind of porous electrode and its application producing gas for electrochemistry |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4116804A (en) * | 1976-11-17 | 1978-09-26 | E. I. Du Pont De Nemours And Company | Catalytically active porous nickel electrodes |
| CN1093825A (en) * | 1993-04-12 | 1994-10-19 | 中国有色金属工业总公司昆明贵金属研究所 | Aluminum-nickel-based conductor and preparation method thereof |
| CN101805910A (en) * | 2009-02-18 | 2010-08-18 | 黄富成 | Hydrogen-oxygen generating electrode plate and method for manufacturing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5579803A (en) * | 1978-12-07 | 1980-06-16 | Showa Denko Kk | Production of cathode for aqueous alkali metal halide solution electrolysis |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4116804A (en) * | 1976-11-17 | 1978-09-26 | E. I. Du Pont De Nemours And Company | Catalytically active porous nickel electrodes |
| CN1093825A (en) * | 1993-04-12 | 1994-10-19 | 中国有色金属工业总公司昆明贵金属研究所 | Aluminum-nickel-based conductor and preparation method thereof |
| CN101805910A (en) * | 2009-02-18 | 2010-08-18 | 黄富成 | Hydrogen-oxygen generating electrode plate and method for manufacturing the same |
Non-Patent Citations (1)
| Title |
|---|
| Ni-Al金属间化合物多孔材料的制备;董虹星;《中南大学博士学位论文》;20111031;正文第20-22、27、29-30、52-55、120-123页 * |
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