CN113649054B - NiFe@NC/Al-SrTiO 3 Composite photocatalyst and application thereof - Google Patents
NiFe@NC/Al-SrTiO 3 Composite photocatalyst and application thereof Download PDFInfo
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- CN113649054B CN113649054B CN202111014961.4A CN202111014961A CN113649054B CN 113649054 B CN113649054 B CN 113649054B CN 202111014961 A CN202111014961 A CN 202111014961A CN 113649054 B CN113649054 B CN 113649054B
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- 229910002367 SrTiO Inorganic materials 0.000 title claims abstract description 121
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 92
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 title claims abstract description 88
- 239000002131 composite material Substances 0.000 title claims abstract description 60
- 239000001257 hydrogen Substances 0.000 claims abstract description 38
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 38
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 230000001699 photocatalysis Effects 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 239000002086 nanomaterial Substances 0.000 claims abstract description 16
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 44
- 238000000137 annealing Methods 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 12
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- 239000000956 alloy Substances 0.000 claims description 8
- 239000002105 nanoparticle Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 2
- 229910052782 aluminium Inorganic materials 0.000 claims 2
- 239000002253 acid Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 20
- 229910000510 noble metal Inorganic materials 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract description 6
- 230000004888 barrier function Effects 0.000 abstract description 5
- 230000005540 biological transmission Effects 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 5
- 230000031700 light absorption Effects 0.000 abstract description 4
- 229910052697 platinum Inorganic materials 0.000 abstract description 4
- 238000006479 redox reaction Methods 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 13
- 235000019441 ethanol Nutrition 0.000 description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 11
- 238000001354 calcination Methods 0.000 description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000003917 TEM image Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000000725 suspension Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000010287 polarization Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 241000282414 Homo sapiens Species 0.000 description 3
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 2
- 238000004577 artificial photosynthesis Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- -1 potassium ferricyanide Chemical compound 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- IHCCLXNEEPMSIO-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 IHCCLXNEEPMSIO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910002555 FeNi Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010893 electron trap Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 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
- 230000001788 irregular Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000009674 qiangzhi Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
Classifications
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- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention provides a NiFe@NC/Al-SrTiO 3 Composite photocatalyst and application thereof. The research of the invention shows that the NiFe@NC nano material can be used as a catalyst promoter of a photocatalyst to promote Al-SrTiO 3 The light absorption performance of the light-emitting diode can accelerate the transmission and separation of photogenerated electrons, improving the utilization efficiency of photo-generated charges and reducing Al-SrTiO 3 The surface oxidation-reduction reaction energy barrier further prepares the composite photocatalyst NiFe@NC/Al-SrTiO 3 The catalyst is used for preparing hydrogen by photocatalytic decomposition of water, and shows high-efficiency photocatalytic decomposition of water to prepare hydrogen. And the NiFe@NC cocatalyst has low cost and simple preparation process, is suitable for large-scale application, and solves the problems of high cost, small reserves of noble metal cocatalysts Pt, rh and the like and inapplicability to large-scale application.
Description
Technical Field
The invention belongs to the technical field of nano photocatalyst materials. More particularly, it relates to a NiFe@NC/Al-SrTiO 3 Composite photocatalyst and application thereof.
Background
Fossil energy (coal, oil, natural gas, etc.) is currently the subject of global energy supply. Consumption of fossil energy is a major factor in environmental pollution and greenhouse effect. On the other hand, the reserves of fossil energy are limited, while the development of human society is infinite, and the huge energy consumption of human beings acceleratesExhaustion of fossil energy. Environmental pollution and energy shortage are major problems facing the human society in the 21 st century, and searching for sustainable clean alternative energy has attracted unprecedented attention. Solar energy is the most promising renewable energy source, because it is inexhaustible, inexhaustible and widely distributed. However, due to the dispersion and intermittence of solar radiation, the energy extracted from the sun must be efficiently converted into chemical energy that can be stored, transported and used as needed (nat. Mater.,2017, 16, 23-34). This requirement has driven the development of sustainable artificial photosynthesis, aimed at simulating natural photosynthesis, utilizing solar energy to drive H 2 O and CO 2 Converted to fuel (chem. Soc. Rev.,2009, 38, 253-278). Of the solar fuels produced by artificial photosynthesis, hydrogen energy (H2) is one of the most attractive because of its high energy density (the calorific value of combustion of hydrogen per kilogram is about 1.4×10 8 J, the combustion heat value of which is 3.9 times of that of alcohol and 3 times of that of gasoline. ) And no pollutant is generated during combustion. And H is 2 Can also be used as raw materials for synthesizing bulk chemicals. Thus, the solar energy is utilized to decompose water to produce H 2 Provides possibility for solving the energy shortage and environmental pollution.
Generally speaking, H of the photocatalyst surface 2 With O 2 Driven by reduction and oxidation promoters, respectively (nat. Rev. Mater.,2017,2, 17050). Wherein noble metal Pt with larger work function can easily form a Schottky barrier with a semiconductor, can be used as an excellent electron trapping trap, and promotes H due to good adsorption of protons 2 (chem. Rev.2020, 120,2, 919-985). However, the reverse reaction of water splitting also tends to occur on Pt nanoparticles, as Pt exhibits lower O 2 Overpotential for the reduction reaction (j.catalyst.2008, 259, 133-137). This problem can be avoided by using Ru (j.Phys.chem.c 2011, 115, 3057-3064) or Rh (angel.chem.int.ed.2006, 45, 7806-7809) instead of Pt to catalyze the water decomposition. In addition, the photocatalytic oxygen evolution half reaction is the determining step of the photocatalytic water decomposition rate, because it involves the reaction of H 2 O forms O 2 The four electron oxidation path of (2) requires an energy of 1.23 eV. Is thatTo achieve a high rate of water oxidation half reaction, noble metal oxides, e.g. RuO 2 (J.am.chem.Soc.2005, 127, 4150-4151) and IrO 2 (J.am.chem.Soc.2009, 131, 926-927) and the like are considered to be the best oxygen evolution promoters.
Although these noble metals and noble metal oxides have high catalytic efficiency as promoters, they have limited reserves and are costly and unfavorable for large-scale applications. Based on the above considerations, there is a need to develop new, low cost promoters for non-noble metal materials for photocatalytic decomposition of aqueous hydrogen.
Disclosure of Invention
Aiming at the problems of high cost, small reserves of noble metal cocatalysts Pt and Rh and the like and inapplicability to large-scale application in the prior art, the invention provides the application of the low-cost non-noble metal NiFe@NC in the cocatalysts serving as the photocatalyst, and the cocatalysts can promote the Al-SrTiO 3 The light absorption performance of the photo-induced charge-trapping device can accelerate the transmission and separation of photo-induced electrons, improve the utilization efficiency of photo-induced charges and reduce Al-SrTiO 3 The surface oxidation-reduction reaction energy barrier is further prepared into a composite photocatalyst NiFe@NC/Al-SrTiO 3 The catalyst is used for preparing hydrogen by photocatalytic decomposition of water, and shows high-efficiency photocatalytic decomposition of water to prepare hydrogen.
The invention aims at providing the application of NiFe@NC nanomaterial as a cocatalyst of a photocatalyst.
Another object of the invention is to provide the use of nife@nc nanomaterial as a cocatalyst in the preparation of a photocatalyst.
Another object of the present invention is to provide a NiFe@NC/Al-SrTiO 3 A composite photocatalyst.
It is a further object of the present invention to provide said NiFe@NC/Al-SrTiO 3 The application of the composite photocatalyst in the photocatalytic decomposition of water to produce hydrogen.
The above object of the present invention is achieved by the following technical solutions:
the research of the invention shows that the NiFe@NC nano material can be used as a cocatalyst to improve the main photocatalyst Al-SrTiO 3 Is a photocatalytic hydrogen evolution rate of (2)Therefore, the application of the NiFe@NC nanomaterial in the cocatalyst serving as a photocatalyst is within the protection scope of the invention.
Preferably, the photocatalyst is Al-SrTiO 3 。
The preparation method of the NiFe@NC nanomaterial refers to the prior art of Sibo Chen, xunfu Zhou, jihai Liao, siyuan Yang, xiaosong Zhou, qiangzhi Gao, shanqing Zhang, yuepping Fang, xinhua Zhong, shengsen Zhang.FeNi intermetallic compound nanoparticles wrapped with N-doped graphitized carbon: a novel cocatalyst for boosting photocatalytic hydrogen evolution [ J ]. Journal of Materials Chemistry A,2020,3481-3490.
As a preferred embodiment, the preparation method of the nife@nc nanomaterial comprises the following steps:
2.0g sodium citrate (C) 6 H 5 Na 3 O 7 ) 2.0g of potassium ferricyanide [ K ] 3 Fe(CN) 6 ]And 2.0g of nickel nitrate [ Ni (NO) 3 ) 2 ·6H 2 O]Dissolving in 200mL deionized water, stirring for 5min, and standing for 24h. Then, centrifugally separating to obtain precipitate, filtering and washing for several times, and stoving in a vacuum box at 60 deg.c to obtain Ni 3 [Fe(CN) 6 ] 2 ·xH 2 O. Grinding Ni 3 [Fe(CN) 6 ] 2 ·xH 2 Transferring the O powder into a muffle furnace, and calcining for 2 hours at 650 ℃ in a nitrogen atmosphere to obtain NiFe@NC.
The invention also provides a NiFe@NC/Al-SrTiO 3 The composite photocatalyst consists of the NiFe@NC nano material and Al-SrTiO 3 Is prepared by the method.
NiFe@NC/Al-SrTiO 3 In the composite photocatalyst, a main photocatalyst Al-SrTiO 3 Light is absorbed to generate photo-generated electrons and holes. Wherein NiFe@NC is used as a cocatalyst to promote Al-SrTiO 3 The light absorption performance of (2) can accelerate the transmission and separation of photogenerated electrons and improve the utilization efficiency of photogenerated charges, and most importantly, niFe@NC can reduce Al-SrTiO 3 Surface oxidation-reduction reaction energy barrier, niFe@NC as productThe hydrogen promoter can accept electrons and promote hydrogen evolution reaction, so that the main photocatalyst Al-SrTiO is effectively improved 3 Compared with Al-SrTiO, the photocatalytic hydrogen evolution rate of (2) 3 Photocatalyst, niFe@NC/Al-SrTiO 3 The composite photocatalyst has higher efficient photocatalytic decomposition pure water hydrogen production activity.
Preferably, the preparation method of the composite photocatalyst comprises the following steps:
mixing the NiFe@NC nanomaterial with Al-SrTiO 3 Mixing, adding ethanol, grinding uniformly, and annealing under inert atmosphere to obtain the NiFe@NC/Al-SrTiO 3 A composite photocatalyst.
In addition, the invention also provides the NiFe@NC/Al-SrTiO 3 A preparation method of a composite photocatalyst,
the NiFe@NC/Al-SrTiO of the invention 3 The preparation method of the composite photocatalyst uniformly loads NiFe@NC serving as a cocatalyst on aluminum-doped strontium titanate (Al-SrTiO) 3 ) Obtaining NiFe@NC/Al-SrTiO on the surface 3 The composite photocatalyst material has the advantages of simple process, strong operability and good repeatability, can realize solar energy conversion by a low-cost route, and has good application prospect.
Preferably, the NiFe@NC and Al-SrTiO 3 The mass ratio of (2-30): 100.
more preferably, the NiFe@NC and Al-SrTiO 3 The mass ratio of (2) is 1:9 to 39.
Preferably, the annealing treatment is carried out at a temperature of 150-300 ℃ for 1-6 hours.
Preferably, the ethanol is added in an amount corresponding to Al-SrTiO 3 The mass ratio of (2-5): 1.
more preferably, the ethanol is added in an amount corresponding to Al-SrTiO 3 The mass ratio of (3.68-4.62): 1.
preferably, the milling is ball milling or milling in an agate mortar.
Preferably, the inert atmosphere comprises a nitrogen atmosphere, an argon atmosphere.
As a preferred embodiment, the al—srtio 3 The preparation method of (2) comprises the following steps:
s1, weighing 6.2g of SrCO 3 Placing the mixture in a muffle furnace, and calcining for 1h at 300 ℃;
s2, calcining SrCO 3 And 3.4g TiO 2 Fully mixing and grinding uniformly, putting into a muffle furnace, calcining at 1000 ℃ for 10 hours to obtain SrTiO 3 A powder sample;
s3, weighing 0.74g SrTiO 3 、0.0082g Al 2 O 3 、10.6600g SrCl 2 ·6H 2 O, placing the mixture in a muffle furnace after mixing and grinding, and calcining for 10 hours at 1150 ℃.
S4, washing and drying the calcined sample to obtain Al-SrTiO 3 。
Finally, the application of the composite photocatalyst in the aspect of photocatalytic decomposition of water to produce hydrogen is also within the protection scope of the invention. The NiFe@NC/Al-SrTiO is adopted 3 The composite photocatalyst is used for carrying out photocatalysis to produce hydrogen, compared with Al-SrTiO 3 The photocatalyst has higher hydrogen production activity.
Compared with the prior art, the invention has the beneficial effects that:
the research of the invention shows that the NiFe@NC nitrogen-doped carbon-coated NiFe alloy nano particles can be used as strontium titanate (Al-SrTiO) 3 ) Hydrogen-producing promoter of (a) to promote Al-SrTiO 3 The light absorption performance of the light-emitting diode can accelerate the transmission and separation of photogenerated electrons, improving the utilization efficiency of photo-generated charges and reducing Al-SrTiO 3 Surface oxidation-reduction reaction energy barrier. Further prepared NiFe@NC/Al-SrTiO 3 Compared with Al-SrTiO, the composite photocatalyst 3 The photocatalyst has higher efficient photocatalytic decomposition pure water hydrogen production activity. And the NiFe@NC cocatalyst has low cost and is suitable for large-scale application.
Drawings
FIG. 1 is an XRD pattern for the NiFe@NC promoter prepared in example 1.
FIG. 2 is a TEM image of NiFe@NC promoter prepared in example 1.
FIG. 3 is an Al-SrTiO prepared in example 2 3 XRD pattern of the photocatalyst.
FIG. 4 is an Al-SrTiO prepared in example 2 3 TEM image of photocatalyst。
FIG. 5 is a NiFe@NC/Al-SrTiO prepared in example 3 3 XRD pattern of the composite photocatalyst.
FIG. 6 is a NiFe@NC/Al-SrTiO prepared in example 3 3 TEM image of composite photocatalyst.
FIG. 7 NiFe@NC/Al-SrTiO prepared in example 3 3 Composite photocatalyst, niFe@NC promoter prepared in example 1, al-SrTiO prepared in example 2 3 The total hydrogen production amount of the photocatalyst and the composite photocatalysts prepared in comparative examples 1 to 4 accumulated with the irradiation time.
FIG. 8 is an Al-SrTiO prepared in example 2 3 Photocatalyst and NiFe@NC/Al-SrTiO prepared in example 3 3 Electrocatalytic hydrogen evolution polarization curve of the composite photocatalyst.
FIG. 9 is an Al-SrTiO prepared in example 2 3 Photocatalyst and NiFe@NC/Al-SrTiO prepared in example 3 3 Photocurrent response curve of the composite photocatalyst.
Detailed Description
The invention is further described in connection with the accompanying drawings and the detailed description, which are not intended to be limiting in any way. Raw materials reagents used in the examples of the present invention are conventionally purchased raw materials reagents unless otherwise specified.
The instrument used for TEM analysis is JSM-2010 type projection electron microscope (TEM) of Japan electronic company to observe microscopic morphology of sample surface, acceleration voltage is 200KV, and the sample is prepared by dispersing absolute ethyl alcohol, then dripping copper mesh, and drying in air.
The apparatus used for XRD analysis was a physical Rigaku Ultima type IV X-ray diffractometer (XRD) characterization of the crystalline phase structure material of the final product prepared. The test conditions are Cu target, K alpha radiation, 40kV,40mA, step width of 0.02 DEG, and scanning range of 10-80 deg. And placing the powder in a groove of a sample table for flattening the powder, and directly detecting.
Example 1 NiFe@NC nanomaterial
1. Preparation
S1, 2.0g of sodium citrate, 2.0g of potassium ferricyanide and 2.0g of nickel nitrate are dissolved in 200mL of deionized water, stirred for 5min and then kept stand for reaction for 24h.
S2, centrifugally separating the reaction product to obtain a precipitate, and then drying the precipitate in a vacuum box at 60 ℃ for 10 hours to obtain Ni 3 [Fe(CN) 6 ]2·xH 2 O powder.
S3, grinding the Ni 3 [Fe(CN) 6 ]2·xH 2 Transferring the O powder into a muffle furnace, and calcining for 2 hours at 650 ℃ in a nitrogen atmosphere to obtain NiFe@NC.
2. Structural characterization
(1) FIG. 1 is an XRD pattern for NiFe@NC of this example, showing three strong diffraction peaks at 43.60 °, 50.79 ℃and 74.68 °, corresponding to Fe, respectively 0.64 Ni 0.36 The (111), (200) and (220) crystal planes of the alloy (PDF#: 47-1405) indicate that the NiFe@NC material contains Fe 0.64 Ni 0.36 And (3) alloy.
(2) FIG. 2 is a TEM image of NiFe@NC of the present embodiment, fe 0.64 Ni 0.36 The alloy nano particles are coated by nitrogen doped carbon with the thickness of about 10-15nm and the grain diameter of 30-80nm, which shows that the NiFe@NC material has a core-shell structure, wherein the core is Fe 0.64 Ni 0.36 The shell layer of the alloy nano-particle is a nitrogen-doped carbon layer.
EXAMPLE 2 photocatalyst aluminum-doped strontium titanate (Al-SrTiO) 3 )
1. Preparation
S1, weighing 6.2g of strontium carbonate (SrCO 3 ) Placing the mixture in a muffle furnace, and calcining the mixture at 300 ℃ for 1h. Calcining SrCO 3 With 3.4g of titanium dioxide (TiO 2 ) Fully mixing and grinding uniformly, putting into a muffle furnace, calcining at 1000 ℃ for 10 hours to obtain SrTiO 3 Powder samples.
S2, weighing 0.74g SrTiO 3 、0.0082g Al 2 O 3 10.6600g SrCl 2 ·6H 2 O, grinding uniformly; the ground mixed powder was placed in a muffle furnace and calcined at 1150 ℃ for 10h.
S3, taking out a calcined sample, washing with water, and drying to obtain Al-SrTiO 3 Powder samples.
2. Structural characterization
(1) FIG. 3 shows the Al-SrTiO of the present embodiment 3 Wherein the diffraction peaks at 2 theta of 32.3 DEG, 40.0 DEG, 46.6 DEG, 57.9 DEG, 67.8 DEG and 77.1 DEG respectively correspond to SrTiO 3 The (110), (111), (200), (211), (220) and (310) crystal planes of (PDF#: 73-0661) indicate that Al-SrTiO is successfully prepared 3 。
(2) FIG. 4 shows the Al-SrTiO of the present embodiment 3 From the TEM image of (C), it can be seen that Al-SrTiO 3 Is irregular nano-particle with the particle size of 300-600nm.
Example 3 NiFe@NC/Al-SrTiO 3 Composite photocatalyst
1. Preparation
0.02g of NiFe@NC prepared in example 1 and 0.18g of Al-SrTiO prepared in example 2 were mixed 3 Adding into an agate mortar, adding 0.8g of ethanol, grinding for 1h, and annealing at 200 ℃ for 2h under the protection of nitrogen after the ethanol volatilizes to obtain NiFe@NC/Al-SrTiO 3 A composite photocatalyst.
2. Characterization of
(1) FIG. 5 is a NiFe@NC/Al-SrTiO prepared in this example 3 XRD pattern of the composite photocatalyst. From XRD patterns, it can be seen that the positions at 43.60 °, 50.79 ° and 74.68 °, respectively correspond to Fe 0.64 Ni 0.36 The (111), (200) and (220) crystal planes of the alloy (PDF#: 47-1405). SrTiO corresponding to diffraction peaks at 32.3 °, 40.0 °, 46.6 °, 57.9 °, 67.8 °, 77.1 °, respectively 3 The (110), (111), (200), (211), (220) and (310) crystal planes of (PDF#: 73-0661). Indicating that NiFe@NC/Al-SrTiO is successfully prepared 3 A composite photocatalyst.
(2) FIG. 6 is a NiFe@NC/Al-SrTiO prepared in this example 3 TEM image of composite photocatalyst, from the image, it can be seen that promoter NiFe@NC is uniformly loaded on photocatalyst Al-SrTiO 3 Is a surface of the substrate.
Example 4 NiFe@NC/Al-SrTiO 3 Composite photocatalyst
1. Preparation
0.01g of NiFe@NC prepared in example 1 and 0.19g of Al-SrTiO prepared in example 2 were mixed 3 Adding into agate mortar, adding 0.7g ethanol, grinding for 1 hr, volatilizing ethanol, annealing at 150deg.C under nitrogen protection for 6 hr to obtainNiFe@NC/Al-SrTiO 3 A composite photocatalyst.
Example 5 NiFe@NC/Al-SrTiO 3 Composite photocatalyst
1. Preparation
0.005g of NiFe@NC prepared in example 1 and 0.195g of Al-SrTiO prepared in example 2 were mixed 3 Adding into agate mortar, adding 0.9g ethanol, grinding for 1h, and annealing at 300 ℃ under nitrogen protection for 1h after ethanol is volatilized to obtain NiFe@NC/Al-SrTiO 3 A composite photocatalyst.
Comparative example 1
This comparative example provides a NiFe@NC/Al-SrTiO 3 A composite photocatalyst was prepared in the same manner as in example 3 except that the mass of NiFe@NC was 0.07g and the mass of Al-SrTiO was 3 The mass of the catalyst is 18g, and the mass of the ethanol added is 80g, namely NiFe@NC and Al-SrTiO 3 The mass ratio of (2) is 0.4:99.6.
comparative example 2
This comparative example provides a NiFe@NC/Al-SrTiO 3 The preparation method of the composite photocatalyst is the same as in example 3, except that the mass of NiFe@NC is 0.27g, namely NiFe@NC and Al-SrTiO 3 The mass ratio of (2) is 60:40.
comparative example 3
This comparative example provides a NiFe@NC/Al-SrTiO 3 The preparation method of the composite photocatalyst is the same as that of example 3, except that the annealing treatment is performed at 100 ℃ for 8 hours.
Comparative example 4
This comparative example provides a NiFe@NC/Al-SrTiO 3 The preparation method of the composite photocatalyst is the same as that of example 3, except that the annealing treatment is performed at 500 ℃ for 1 hour.
Experimental example 1 experiment for producing hydrogen by photocatalytic decomposition of pure water
1. Experimental method
For NiFe@NC/Al-SrTiO prepared in example 3 3 Composite photocatalyst, niFe@NC prepared in example 1, al-SrTiO prepared in example 2 3 The composite photocatalysts prepared in comparative examples 1 to 4 were subjected to a photocatalytic decomposition water production hydrogen test.
Photocatalytic decomposition of waterThe reaction was carried out in a Labsolar 6A photocatalytic reaction system (Beijing Porphy's) which may be in communication with a vacuum pump. 20mg of the photocatalyst was added to a reactor containing 100mL of deionized water, dispersed ultrasonically for 3min, and stirred well. The reactor was connected to the system and sealed, the whole system was evacuated to 2.0kPa with a vacuum pump, the reactor was kept at a constant temperature with 15 ℃ condensed water, and the suspension in the reactor was kept in suspension with magnetic stirring. The reactor is top-illuminated, a 300W xenon lamp is used as a light source, the input voltage is 220V, the current is 15A, and a light filter (A.M 1.5) can be assembled on a lamp cap. After the reaction starts, taking one sample every 30min through an automatic sample injection system, and sending the sample into an online gas chromatograph to detect H generated by the reaction 2 。
2. Experimental results
FIG. 7 is a NiFe@NC/Al-SrTiO prepared in example 3 3 Composite photocatalyst, niFe@NC prepared in example 1, al-SrTiO prepared in example 2 3 The total amount of hydrogen produced by the catalysis of the composite photocatalyst prepared in comparative examples 1-4 accumulated with the time of illumination.
As can be seen from FIG. 7, the total light is irradiated for 4 hours, and Al-SrTiO prepared in example 2 3 Neither the photocatalyst nor the nife@nc cocatalyst prepared in example 1 had hydrogen generating activity. Under the same conditions, niFe@NC/Al-SrTiO prepared in example 3 3 The total hydrogen yield of the composite photocatalyst is 27.12 mu mol, and the result shows that NiFe@NC serving as a cocatalyst can effectively improve the main photocatalyst Al-SrTiO 3 Is a photocatalytic hydrogen evolution rate. Therefore, the invention provides a high-efficiency composite photocatalyst NiFe@NC/Al-SrTiO 3 . Under the same conditions, niFe@NC/Al-SrTiO prepared in comparative example 1, comparative example 2, comparative example 3 and comparative example 4 3 The total hydrogen production of the composite photocatalyst was 7.56, 2.04, 20.43 and 11.42. Mu. Mol, respectively, which are inferior to those of example 3, indicating that NiFe@NC/Al-SrTiO prepared under optimal control conditions 3 The composite photocatalyst has good photocatalytic activity.
Experimental example 2 electrocatalytic hydrogen evolution polarization curve
1. Experimental method
For Ni prepared in example 3Fe@NC/Al-SrTiO 3 Composite photocatalyst and Al-SrTiO prepared in example 2 3 The electrocatalytic hydrogen evolution polarization curves of the photocatalysts are compared.
Preparing a working electrode: mu.L of Nafion (5 wt%) solution was mixed with 5.0mg of NiFe@NC/Al-SrTiO 3 Composite photocatalyst or Al-SrTiO 3 The photocatalyst was added to 1.0mL of ethanol and dispersed by ultrasound to give a suspension. 100. Mu.L of the suspension was applied dropwise to an FTO conductive glass substrate (2X 1 cm) 2 ) And (3) naturally drying, and annealing at 150 ℃ for 60min in an argon atmosphere to obtain the working electrode.
Photoelectrochemical testing was performed on an electrochemical workstation (CHI 650E) equipped with a three-electrode system, with platinum and Ag/AgCl (saturated KCl) electrodes as counter and reference electrodes, respectively. At 0.5M Na 2 SO 4 The solution was used as an electrolyte. At a scanning rate of 5 mV.s -1 The polarization curve of the electrocatalytic Hydrogen Evolution Reaction (HER) was tested.
2. Experimental results
FIG. 8 is a preparation of Al-SrTiO of example 2 3 Photocatalyst and NiFe@NC/Al-SrTiO prepared in example 3 3 Electrocatalytic hydrogen evolution polarization curve of the composite photocatalyst. Compared with pure Al-SrTiO 3 ，NiFe@NC/Al-SrTiO 3 The hydrogen evolution overpotential of (c) becomes smaller, which means that the promoter NiFe@NC can lower the potential barrier of the hydrogen evolution reaction and promote the progress of the hydrogen evolution reaction.
Experimental example 3 photocurrent response curve
1. Experimental method
For NiFe@NC/Al-SrTiO prepared in example 3 3 Composite photocatalyst and Al-SrTiO prepared in example 2 3 The photocurrent response curves of the photocatalysts were compared.
Preparing a working electrode: mu.L of Nafion (5 wt%) solution was mixed with 5.0mg of NiFe@NC/Al-SrTiO 3 Composite photocatalyst or Al-SrTiO 3 The photocatalyst was added to 1.0mL of ethanol and dispersed by ultrasound to give a suspension. 100. Mu.L of the suspension was applied dropwise to an FTO conductive glass substrate (2X 1 cm) 2 ) And (3) naturally drying, and annealing at 150 ℃ for 60min in an argon atmosphere to obtain the working electrode.
Photoelectrochemical testing was performed on an electrochemical workstation (CHI 650E) equipped with a three-electrode system, with platinum and Ag/AgCl (saturated KCl) electrodes as counter and reference electrodes, respectively. At 0.5M Na 2 SO 4 The solution was used as an electrolyte. A300W xenon lamp was used as a light source to record a transient photocurrent curve (i-t) at a voltage of 0.4V vs. Ag/AgCl.
2. Experimental results
FIG. 9 is an Al-SrTiO prepared in example 2 3 Photocatalyst and NiFe@NC/Al-SrTiO prepared in example 3 3 Photocurrent response curve of the composite photocatalyst. Compared with Al-SrTiO 3 ，NiFe@NC/Al-SrTiO 3 The photocurrent density of the catalyst is greatly improved, which indicates that the promoter NiFe@NC can accelerate charge transmission, promote charge separation efficiency and improve the utilization efficiency of photo-generated electrons.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (7)
- The application of NiFe@NC nanomaterial in a cocatalyst serving as a photocatalyst is characterized in that the photocatalyst is Al-SrTiO 3 The Al-SrTiO 3 The nano material is nitrogen-doped carbon-coated NiFe alloy nano particles serving as strontium titanate Al-SrTiO 3 The application of the hydrogen-producing promoter is that NiFe@NC nano material and Al-SrTiO 3 Mixing, adding ethanol, grinding, and annealing under inert atmosphere.
- 2. NiFe@NC/Al-SrTiO 3 The composite photocatalyst is characterized by being prepared from NiFe@NC nano material and aluminum doped titaniumStrontium acid Al-SrTiO 3 The preparation method of the composite photocatalyst comprises the following steps: niFe@NC nanomaterial and Al-SrTiO 3 Mixing, adding ethanol, grinding uniformly, and annealing under inert atmosphere to obtain the NiFe@NC/Al-SrTiO 3 The composite photocatalyst is prepared from NiFe@NC nanomaterial which is nitrogen-doped carbon-coated NiFe alloy nanoparticles serving as strontium titanate Al-SrTiO 3 Hydrogen-producing promoter of (a), said Al-SrTiO 3 Aluminum doped strontium titanate.
- 3. The composite photocatalyst of claim 2, wherein the nife@nc and Al-SrTiO 3 The mass ratio of (2-30): 100.
- 4. the composite photocatalyst according to claim 2, wherein the annealing treatment is performed at a temperature of 150 to 300 ℃ for a time of 1 to 6 hours.
- 5. The composite photocatalyst according to claim 2, wherein the ethanol is added in an amount corresponding to the amount of Al-SrTiO 3 The mass ratio of (2-5): 1.
- 6. the composite photocatalyst of claim 2, wherein the milling is ball milling or milling in an agate mortar.
- 7. The use of the composite photocatalyst according to any one of claims 2 to 6 for photocatalytic decomposition of aqueous hydrogen.
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