CN108283926A - A kind of growth in situ ferronickel double-metal hydroxide preparation method with laminated structure in nickel foam - Google Patents
A kind of growth in situ ferronickel double-metal hydroxide preparation method with laminated structure in nickel foam Download PDFInfo
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- CN108283926A CN108283926A CN201810044072.4A CN201810044072A CN108283926A CN 108283926 A CN108283926 A CN 108283926A CN 201810044072 A CN201810044072 A CN 201810044072A CN 108283926 A CN108283926 A CN 108283926A
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- nickel foam
- nickel
- metal hydroxide
- ferronickel
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 41
- 239000006260 foam Substances 0.000 title claims abstract description 38
- 229910000863 Ferronickel Inorganic materials 0.000 title claims abstract description 19
- 229910000000 metal hydroxide Inorganic materials 0.000 title claims abstract description 17
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004202 carbamide Substances 0.000 claims abstract description 8
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 5
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 claims description 5
- 150000002823 nitrates Chemical class 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims 1
- 239000012467 final product Substances 0.000 claims 1
- 239000000047 product Substances 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 15
- 238000006243 chemical reaction Methods 0.000 abstract description 15
- 239000003792 electrolyte Substances 0.000 abstract description 9
- 239000001301 oxygen Substances 0.000 abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 238000005868 electrolysis reaction Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000007769 metal material Substances 0.000 abstract 2
- 229910016874 Fe(NO3) Inorganic materials 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 239000002803 fossil fuel Substances 0.000 abstract 1
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 abstract 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical class [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010953 base metal Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- 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
A kind of preparation method of the invention discloses growth in situ in the nickel foam ferronickel double-metal hydroxide with layer structure, belongs to electrochemical field.The material is made using Nickelous nitrate hexahydrate, Fe(NO3)39H2O, urea, ammonium fluoride and nickel foam for primary raw material, and the elctro-catalyst of electrolysis water oxygen has successfully been prepared.The layer structure of the catalyst provides abundant active site, due to the presence of base foam nickel, enhances electric conductivity, and excellent catalytic activity is shown when it being made to produce VPO catalysts as electro-catalysis.Oxygen evolution reaction (OER) activity of traditional non-noble metallic materials under alkaline electrolyte is also undesirable.Therefore, the OER catalytic performances of non-noble metallic materials under alkaline condition are promoted, are had great importance for solving fossil fuel energy crisis.In the present invention, the earth reserves of nickel and iron are very abundant, and OER catalytic performances are excellent under alkaline condition for the ferronickel double-metal hydroxide of gained layer structure, are very promising catalysis materials.
Description
Technical field
The invention belongs to electro-catalysis fields, and in particular to a kind of growth in situ ferronickel with laminated structure in nickel foam
The preparation method of the oxygen evolution reaction catalysts of double-metal hydroxide.
Background technology
For the energy crisis and environmental crisis of current getting worse, electrolysis aquatic products hydrogen production oxygen be such issues that solve row it
One of effective method, noble metal catalyst seriously hinders the commercialization of electrolysis water due to the problems such as its price is high, and reserves are low
Process.Surface is studied, by controlling the pattern and structure of non-noble metal nano particle, catalytic activity can be effectively improved, have
Replace the potentiality of noble metal catalyst, but also has a certain distance apart from noble metal catalyst.Therefore base metal is improved to urge
The catalytic activity of agent is an important issue.Currently, double-metal hydroxide is caused due to its unique laminated structure
The extensive interest of academia, the position of trivalent metal substitution divalent metal and quantity can all have catalytic activity significant shadow
It rings, therefore, suitable reaction condition and suitable metal proportioning are the key that obtain the material with excellent catalytic activity.Together
When, due to growth mechanism, the double-metal hydroxide of sheet is easy to occur with chondritic, on this basis, is added
Substrate makes the laminated structure of easy balling-up is uniformly vertical to be inserted into substrate, that is, increases active site, and enhance material
Electric conductivity makes its OER catalytic activity be greatly improved.We are timely by controlling the ratio and reaction temperature of nickel and iron
Between, successfully synthesize and be grown in the ferronickel double-metal hydroxide with uniform laminated structure in substrate, by test, tool
There are the OER catalytic performances of current one stream.
Invention content
There is the double-metal hydroxide of laminated structure.
Preparation process of the present invention is simple, does not need expensive device, and products obtained therefrom quality high-performance is good, in future for being electrolysed
There is bright foreground in the large-scale application of aquatic products hydrogen production oxygen.
A kind of growth in situ ferronickel double-metal hydroxide preparation method with laminated structure in nickel foam, made
Journey includes the following steps:
1) six water nickel nitrates of 1.163g are weighed, nine water ferric nitrates of 0.1616g, 1.2g urea, 0.296g ammonium fluorides are dissolved into
In 80mL deionized waters.It is handled 30 minutes under the action of magnetic stirring apparatus, obtains uniform solution;
2) 1cm*5cm nickel foams are cut, acetone is respectively placed in, is washed 30 minutes in ethyl alcohol and distilled water;
3) solution configured in step 1 is transferred in 100ml autoclaves, after the nickel foam washed is vertical
It is inserted into solution, reaction kettle is put into 12 hours of reaction in 120 degree of baking ovens;
4) after reaction kettle is cooled to room temperature, nickel foam is taken out, nickel foam is changed into yellow green by silver color at this time, uses ethyl alcohol
With distilled water supersound washing, drying growth in situ ferronickel double-metal hydroxide with laminated structure in nickel foam;
5) OER catalytic activity of the above-mentioned product under 1M KOH electrolyte is tested with electrochemical workstation.
The raw material that the present invention uses is mainly the nickel source of rich reserves in the earth, source of iron and urea, raw material sources extensively, ring
It protects green, safe.
Growth in situ prepared by the method for the present invention ferronickel double-metal hydroxide with laminated structure in nickel foam, can
As the electrolysis aquatic products VPO catalysts haveing excellent performance, there is higher catalytic activity and good stability.
The ferronickel double-metal hydroxide with laminated structure can in nickel foam for growth in situ prepared by the method for the present invention
A large amount of synthesis, do not need expensive device, can be widely used in electro-catalysis application.
Description of the drawings
Fig. 1 is the ferronickel bimetallic hydrogen-oxygen that the growth in situ that specific embodiment 1 obtains has laminated structure in nickel foam
The SEM of compound schemes, hence it is evident that visible to have apparent laminated structure;
Fig. 2 is the ferronickel bimetallic hydrogen-oxygen that the growth in situ that specific embodiment 1 obtains has laminated structure in nickel foam
OER catalytic activity of the compound under alkaline electrolyte, the half wave potential under 1M KOH electrolyte are 0.76V.
Fig. 3 is the ferronickel bimetallic hydrogen-oxygen that the growth in situ that specific embodiment 1 obtains has laminated structure in nickel foam
Stability of the compound under alkaline electrolyte, after 20 hours of test under 1M KOH electrolyte, current density can also
Maintain initial 92%.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
Attached drawing, the technical solution of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on described the embodiment of the present invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of without creative work, shall fall within the protection scope of the present invention.
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
1) six water nickel nitrates of 1.163g are weighed, nine water ferric nitrates of 0.1616g, 1.2g urea, 0.296g ammonium fluorides are dissolved into
In 80mL deionized waters.It is handled 30 minutes under the action of magnetic stirring apparatus, obtains uniform solution;
2) 1cm*5cm nickel foams are cut, acetone is respectively placed in, is washed 30 minutes in ethyl alcohol and distilled water;
3) solution configured in step 1 is transferred in 100ml autoclaves, after the nickel foam washed is vertical
It is inserted into solution, reaction kettle is put into 12 hours of reaction in 120 degree of baking ovens;
4) after reaction kettle is cooled to room temperature, nickel foam is taken out, nickel foam is changed into yellow green by silver color at this time, uses ethyl alcohol
With distilled water supersound washing, drying growth in situ ferronickel double-metal hydroxide with laminated structure in nickel foam;
5) OER catalytic activity of the above-mentioned product under 1M KOH electrolyte is tested with electrochemical workstation.
Embodiment 2
1) six water nickel nitrates of 1.018g are weighed, nine water ferric nitrates of 0.3232g, 1.2g urea, 0.296g ammonium fluorides are dissolved into
In 80mL deionized waters.It is handled 30 minutes under the action of magnetic stirring apparatus, obtains uniform solution;
2) 1cm*5cm nickel foams are cut, acetone is respectively placed in, is washed 30 minutes in ethyl alcohol and distilled water;
3) solution configured in step 1 is transferred in 100ml autoclaves, after the nickel foam washed is vertical
It is inserted into solution, reaction kettle is put into 12 hours of reaction in 120 degree of baking ovens;
4) after reaction kettle is cooled to room temperature, nickel foam is taken out, nickel foam is changed into yellow green by silver color at this time, uses ethyl alcohol
With distilled water supersound washing, drying growth in situ ferronickel double-metal hydroxide with laminated structure in nickel foam;
5) OER catalytic activity of the above-mentioned product under 1M KOH electrolyte is tested with electrochemical workstation.
Embodiment 3
1) six water nickel nitrates of 1.163g are weighed, nine water ferric nitrates of 0.4848g, 1.2g urea, 0.296g ammonium fluorides are dissolved into
In 80mL deionized waters.It is handled 30 minutes under the action of magnetic stirring apparatus, obtains uniform solution;
2) 1cm*5cm nickel foams are cut, acetone is respectively placed in, is washed 30 minutes in ethyl alcohol and distilled water;
3) solution configured in step 1 is transferred in 100ml autoclaves, after the nickel foam washed is vertical
It is inserted into solution, reaction kettle is put into 12 hours of reaction in 120 degree of baking ovens;
4) after reaction kettle is cooled to room temperature, nickel foam is taken out, nickel foam is changed into yellow green by silver color at this time, uses ethyl alcohol
With distilled water supersound washing, drying growth in situ ferronickel double-metal hydroxide with laminated structure in nickel foam;
5) OER catalytic activity of the above-mentioned product under 1M KOH electrolyte is tested with electrochemical workstation.
It should be understood that although with reference to its illustrative embodiment, particularly shown and description is carried out to the present invention,
It should be understood by those skilled in the art that without departing substantially from the spirit and model by the present invention as defined in the claims
Under conditions of enclosing, the variation of various forms and details can be carried out wherein, can carry out the arbitrary combination of various embodiments.
Claims (4)
1. a kind of growth in situ the ferronickel double-metal hydroxide preparation method with laminated structure, feature in nickel foam exist
In the described method comprises the following steps:
1) a certain amount of six water nickel nitrate, nine water ferric nitrates, urea and ammonium fluoride are added in distilled water solution, are stirred evenly;
2) a certain size nickel foam acetone, ethyl alcohol and distilled water fully wash, and are put into matched solution after dry;
3) the above-mentioned solution containing nickel foam is transferred in autoclave, is put into baking oven and reacts a period of time;
4) after autoclave is cooled to room temperature, nickel foam is taken out, is washed in ultrasonic pond with distilled water, it is to obtain the final product former after dry
Position is grown in the ferronickel double-metal hydroxide with layer structure in nickel foam;
5) chemical property of above-mentioned product is tested with electrochemical workstation.
2. preparation method according to claim 1, which is characterized in that ferronickel molar concentration rate described in step 1) is
0.04mol/L ratios 0.004mol/L, urea concentration 0.2mol/L, a concentration of 0.08mol/L of ammonium fluoride.
3. preparation method according to claim 1, which is characterized in that nickel foam size described in step 2) is 1*5cm.
4. preparation method according to claim 1, which is characterized in that the oven temperature described in step 3) is 120 degree,
Reaction time is 12 hours.
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