CN109647476A - A kind of preparation method of metal and the compound HER catalyst of metal oxide - Google Patents
A kind of preparation method of metal and the compound HER catalyst of metal oxide Download PDFInfo
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- CN109647476A CN109647476A CN201811386984.6A CN201811386984A CN109647476A CN 109647476 A CN109647476 A CN 109647476A CN 201811386984 A CN201811386984 A CN 201811386984A CN 109647476 A CN109647476 A CN 109647476A
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- nicomoo
- reaction kettle
- catalyst
- nickel foam
- metal
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- 239000003054 catalyst Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 8
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 8
- 239000002184 metal Substances 0.000 title claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 6
- 150000001875 compounds Chemical class 0.000 title claims abstract description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000006260 foam Substances 0.000 claims abstract description 11
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 5
- 239000012456 homogeneous solution Substances 0.000 claims abstract description 5
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims abstract description 3
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000010970 precious metal Substances 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910015667 MoO4 Inorganic materials 0.000 description 2
- 229910003266 NiCo Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 229910017299 Mo—O Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- -1 oxide Chemical compound 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910001134 stannide Inorganic materials 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/60—
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- 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
Abstract
The present invention relates to the preparation methods of a kind of metal and the compound HER catalyst of metal oxide, including the following steps: 1) washes and dries nickel foam；2) Co (NO is weighed3)2·6H2O and Na2MoO4·2H2O is dissolved in appropriate amount of deionized water, forms uniform solution；3) above-mentioned homogeneous solution is transferred in inner liner of reaction kettle, then nickel foam is placed in inner liner of reaction kettle vertically, be then heated to keep the temperature 3-10h at 100-200 DEG C for reaction kettle, reaction kettle is then naturally cooled into room temperature；4) nickel foam in 3) is taken out, washes and dries, obtains NF@NiCOMoO presoma；5) by the NF@NiCOMoO presoma 4) obtained in Ar and H2Atmosphere in 300-700 DEG C of calcining 0.5-3h, obtain final NF@NiCOMoO-H2Catalyst.
Description
Technical field
The invention belongs to electro-catalysis water decompositions to produce hydrogen technical field, be related to a kind of metal and metal oxide composite electro catalytic
Produce the preparation method of hydrogen material.
Background technique
With the continuous development of society with fossil fuel largely using cause earth environment seriously polluted and resource it is withered
The problems such as exhausting.In order to solve these problems, we are badly in need of finding a kind of cleaning, the safe and efficient and reproducible energy replaces
For traditional fossil fuel.Hydrogen Energy becomes numerous alternative energies as a kind of green, cleaning and efficient renewable energy
One of.In numerous hydrogen production process, electrolysis water (including cathode produces hydrogen reaction HER and anode produces oxygen and reacts OER) produces hydrogen process not
Pollution can be generated, a kind of method for being acknowledged as effective hydrogen manufacturing.
Precious metals pt is become due to low overpotential and quick kinetics and is measured catalyst H2-producing capacity
Scale.However, low reserves and high cost limit always extensive use of the precious metals pt in practical commercial production.Therefore, it visits
The weight that the non-precious metal catalyst of Suo Gaoxiao, durability and low cost are used to that precious metals pt material is replaced to be electro-catalysis area research
Point and key, this is with important commercial value and meaning.
In recent years, transistion metal compound, including hydroxide, oxide, sulfide, phosphide, boride, nitridation
Object, stannide, antimonide have been achieved for excellent electrolysis water performance.However, under alkaline condition, low electric conductivity and slowly
Kinetics lead to its poor HER performance.To improve HER performance under alkaline condition, researchers do a large amount of work
Make.Such as: doping is to improve electric conductivity and accelerate HER kinetics；Cellular is made with the more active sites of exposure；With
Self-supporting conducting base combines, and avoids the use of the reunion and additive that prepare the material of electrode, the electronics greatly promoted
Transmission；Lacking oxygen is introduced, the band gap of material can not only be adjusted, accelerates electron-transport, and more production hydrogen activity positions can be created
Point.However the catalyst of these methods preparation still has biggish gap with Pt.Recently, gold is prepared by simple hydrogenation treatment
Belong to and presents the catalytic performance close to Pt with metal oxide materials.Metal oxide can weaken the bond energy of O-H, accelerate H2O points
The cracking of son；Metal alloy can accelerate the formation of hydrogen molecule and bubble hydrogen is made quickly to be desorbed, be current due to low chemical valence
Improve the most important method of HER performance.
Summary of the invention
The present invention provides a kind of method for preparing efficient HER catalyst by hydro-thermal and hydrogenation treatment.Operating method is simple
Controllably, low in cost, the material of preparation can directly be applied without any post-processing, simplify process flow.System of the present invention
Standby technique is as follows:
A kind of preparation method of metal and the compound HER catalyst of metal oxide, including the following steps:
1) nickel foam is washed and dried；
2) will be according to 1:(0.2-5) substance amount proportion, weigh Co (NO3)2·6H2O and Na2MoO4·2H2O is dissolved in
In appropriate amount of deionized water, uniform solution is formed；
3) above-mentioned homogeneous solution is transferred in inner liner of reaction kettle, then nickel foam is placed in inner liner of reaction kettle vertically, so
Reaction kettle is heated to afterwards to keep the temperature 3-10h at 100-200 DEG C, reaction kettle is then naturally cooled into room temperature；
4) nickel foam in 3) is taken out, washes and dries, obtains NF@NiCOMoO presoma；
5) by the NF@NiCOMoO presoma 4) obtained in Ar and H2Atmosphere in 300-700 DEG C of calcining 0.5-3h, obtain
Final NF@NiCOMoO-H2Catalyst.
The present invention modifies Ni-Co-Mo-O by the NiCo alloying pellet that hydro-thermal and hydrogenation treatment are prepared for a kind of self-supporting
Nanosheet composite material.Meanwhile hydrogenation treatment is also introduced into a large amount of nano-pore and Lacking oxygen so that preparation material realize it is excellent
Different HER performance.
Detailed description of the invention
Fig. 1 is NF@NiCOMoO-H prepared by the embodiment of the present invention 12Scanning electron microscope image, therefrom can be with
Find out that nanometer sheet there are many small NiCo nano particles；
Fig. 2 is NF@NiCOMoO-H prepared by the embodiment of the present invention 12Transmission electron microscope image；
Fig. 3 is NF@NiCOMoO-H prepared by the embodiment of the present invention 12X-ray diffraction analyze map；
Fig. 4 is NF@NiCOMoO-H prepared by the embodiment of the present invention 12With NF, NF@NiCOMoO-Ar (example 3) and Pt/
The HER performance comparison of C；
Fig. 5 is the HER performance comparison that 1 material prepared of the embodiment of the present invention and example 4 and 5 prepare material, i.e., does not exist together
Manage influence of the temperature to HER performance.
The present invention does not address place and is suitable for the prior art.
Specific embodiment
Technology path of the invention is as follows:
1) by nickel foam (NF, 2 × 3cm2) immerse in the dilute hydrochloric acid solution of 1-5M, ultrasonic 20-60min removes surface oxidation
Then object with deionized water and alcohol washes and is dried in vacuo；
2) by the Co (NO of 1-5mmol3)2·6H2The Na of O and 1-5mmol2MoO4·2H2O is dissolved in 60-90mL deionized water
In, stirring 30min forms uniform solution；
3) above-mentioned homogeneous solution is transferred in 100mL polytetrafluoroethyllining lining, then by NF (2 × 3cm2) be placed on vertically instead
It answers in kettle liner, is then heated to keep the temperature 3-10h at 100-200 DEG C for reaction kettle, reaction kettle is then naturally cooled into room temperature；
4) NF in 3) is taken out, it is dry at 30-60 DEG C in a vacuum drying oven with deionized water and alcohol washes, it obtains
NF@NiCOMoO presoma；
5) by the NF@NiCOMoO presoma 4) obtained in Ar (0-500sccm) and H2300- in (0-50sccm) atmosphere
700 DEG C of calcining 0.5-3h, obtain final NF@NiCOMoO-H2Catalyst.
The specific embodiment of preparation method of the present invention is given below.Preparation that these embodiments are only used for that the present invention will be described in detail
Method is not intended to limit the protection scope of the claim of this application.
Embodiment 1
1) by nickel foam (NF, 2 × 3cm2) enter in the dilute hydrochloric acid solution of 3M, ultrasonic 30min removes surface scale, so
It with deionized water and alcohol washes and is dried in vacuo afterwards；
2) by the Co (NO of 3mmol3)2·6H2The Na of O and 3mmol2MoO4·2H2O is dissolved in 80mL deionized water, stirring
30min forms uniform solution；
3) above-mentioned homogeneous solution is transferred in 100mL polytetrafluoroethyllining lining, then by NF (2 × 3cm2) be placed on vertically instead
It answers in kettle liner, reaction kettle is then heated to 150 DEG C of heat preservation 6h, reaction kettle is then naturally cooled into room temperature；
4) NF in 3) is taken out, it is dry at 50 DEG C in a vacuum drying oven with deionized water and alcohol washes, obtain NF
NiCOMoO presoma；
5) 500 DEG C of calcining 2h, acquisition in Ar:H2 (v/v, 20/180) atmosphere by the NF@NiCOMoO presoma 4) obtained
NF@NiCOMoO-H2Composite catalyst.
Embodiment 2
Unlike the first embodiment: only carrying out preceding 4 steps of example 1, the calcining without step 5.
Embodiment 3
Unlike the first embodiment: 5) by the NF@NiCOMoO presoma 4) obtained in pure Ar (180sccm) atmosphere
500 DEG C of calcining 2h obtain NF@NiCOMoO-Ar composite material.
Embodiment 4
Unlike the first embodiment: 5) by the NF@NiCOMoO presoma 4) obtained in Ar:H2 (v/v, 20/180) atmosphere
In 400 DEG C of calcining 2h.
Embodiment 5
Unlike the first embodiment: 5) by the NF@NiCOMoO presoma 4) obtained in Ar:H2 (v/v, 20/180) atmosphere
In 600 DEG C of calcining 2h.
Claims (1)
1. the preparation method of a kind of metal and the compound HER catalyst of metal oxide, including the following steps:
1) nickel foam is washed and dried；
2) will be according to 1:(0.2-5) substance amount proportion, weigh Co (NO3)2·6H2O and Na2MoO4·2H2O is dissolved in right amount
In deionized water, uniform solution is formed；
3) above-mentioned homogeneous solution is transferred in inner liner of reaction kettle, then nickel foam is placed in inner liner of reaction kettle vertically, then will
Reaction kettle is heated to keep the temperature 3-10h at 100-200 DEG C, and reaction kettle is then naturally cooled to room temperature；
4) nickel foam in 3) is taken out, washes and dries, obtains NF@NiCOMoO presoma；
5) by the NF@NiCOMoO presoma 4) obtained in Ar and H2Atmosphere in 300-700 DEG C of calcining 0.5-3h, obtain final
NF@NiCOMoO-H2Catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811386984.6A CN109647476B (en) | 2018-11-20 | 2018-11-20 | Preparation method of metal and metal oxide composite HER catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811386984.6A CN109647476B (en) | 2018-11-20 | 2018-11-20 | Preparation method of metal and metal oxide composite HER catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109647476A true CN109647476A (en) | 2019-04-19 |
| CN109647476B CN109647476B (en) | 2021-06-08 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811386984.6A Expired - Fee Related CN109647476B (en) | 2018-11-20 | 2018-11-20 | Preparation method of metal and metal oxide composite HER catalyst |
Country Status (1)
| Country | Link |
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| CN (1) | CN109647476B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112108149A (en) * | 2019-06-21 | 2020-12-22 | 南京大学昆山创新研究院 | Preparation method of electrocatalytic material, corresponding material and use method |
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| CN104988536A (en) * | 2015-08-04 | 2015-10-21 | 重庆大学 | Method for preparing high-performance molybdenum-based hydrogen evolution electrode by phosphatizing molybdate precursor |
| CN105386077A (en) * | 2014-08-28 | 2016-03-09 | 丰田自动车工程及制造北美公司 | Water oxidation catalyst including cobalt molybdenum |
| CN105448543A (en) * | 2015-12-29 | 2016-03-30 | 东华大学 | Preparation method for CoMoO4 nanostructure supercapacitor electrode material taking foam nickel as substrate |
| CN107195482A (en) * | 2017-05-04 | 2017-09-22 | 华侨大学 | A kind of nanometer rods array composite and its preparation method and application |
| CN107999075A (en) * | 2017-12-29 | 2018-05-08 | 济南大学 | A kind of aza material preparation method of NiO nanoparticle doped carbon and application |
| CN108314092A (en) * | 2017-12-29 | 2018-07-24 | 安泰科技股份有限公司 | A kind of foamed nickel supported nano bar-shape cobalt molybdate and its preparation method and application |
-
2018
- 2018-11-20 CN CN201811386984.6A patent/CN109647476B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105386077A (en) * | 2014-08-28 | 2016-03-09 | 丰田自动车工程及制造北美公司 | Water oxidation catalyst including cobalt molybdenum |
| CN104988536A (en) * | 2015-08-04 | 2015-10-21 | 重庆大学 | Method for preparing high-performance molybdenum-based hydrogen evolution electrode by phosphatizing molybdate precursor |
| CN105448543A (en) * | 2015-12-29 | 2016-03-30 | 东华大学 | Preparation method for CoMoO4 nanostructure supercapacitor electrode material taking foam nickel as substrate |
| CN107195482A (en) * | 2017-05-04 | 2017-09-22 | 华侨大学 | A kind of nanometer rods array composite and its preparation method and application |
| CN107999075A (en) * | 2017-12-29 | 2018-05-08 | 济南大学 | A kind of aza material preparation method of NiO nanoparticle doped carbon and application |
| CN108314092A (en) * | 2017-12-29 | 2018-07-24 | 安泰科技股份有限公司 | A kind of foamed nickel supported nano bar-shape cobalt molybdate and its preparation method and application |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112108149A (en) * | 2019-06-21 | 2020-12-22 | 南京大学昆山创新研究院 | Preparation method of electrocatalytic material, corresponding material and use method |
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