CN116395751A - Preparation and piezoelectric catalysis application of samarium-doped bismuth ferrite nano material - Google Patents
Preparation and piezoelectric catalysis application of samarium-doped bismuth ferrite nano material Download PDFInfo
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 71
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 70
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
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- 239000001257 hydrogen Substances 0.000 claims abstract description 40
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 40
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 26
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 20
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- 239000000463 material Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 9
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
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- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 6
- YZDZYSPAJSPJQJ-UHFFFAOYSA-N samarium(3+);trinitrate Chemical compound [Sm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YZDZYSPAJSPJQJ-UHFFFAOYSA-N 0.000 claims description 6
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- 229910017135 Fe—O Inorganic materials 0.000 description 1
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- C01G49/0018—Mixed oxides or hydroxides
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- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/843—Arsenic, antimony or bismuth
- B01J23/8437—Bismuth
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Abstract
The invention belongs to the field of nano-material piezoelectric catalysis, and relates to preparation and piezoelectric catalysis application of samarium doped bismuth ferrite nano-materials. Compared with pure phase bismuth ferrite, the samarium doped bismuth ferrite has obviously improved piezoelectric effect, and the catalyst generates energy band bending under the action of ultrasound to generate positive and negative charges on the surface of the material, thereby being beneficial to efficiently catalyzing and decomposing water to generate hydrogen. Compared with pure-phase bismuth ferrite, the samarium-doped bismuth ferrite piezoelectric catalysis hydrogen production amount is 3.4 times that of the pure-phase bismuth ferrite material, and the hydrogen production efficiency is effectively improved. The invention discloses a method for producing hydrogen by decomposing water, which has simple process flow, strong operability and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of piezoelectric catalysis, and particularly relates to preparation of a samarium doped bismuth ferrite nano material and application of the composite material in piezoelectric catalysis hydrogen production.
Background
Because fossil fuels have limited resources, the shortage of energy has not been able to meet the daily increasing energy demands, and fossil fuels have serious environmental impact in use, hydrogen energy has been recognized as one of the clean energy sources in the future. Through continuous exploration and drilling, a novel method capable of carrying out sewage treatment and clean energy preparation, piezoelectric catalysis, starts to gradually enter the field of view of researchers. Piezoelectric catalysis is an emerging catalytic process that can directly convert discrete mechanical energy into chemical energy, and has attracted considerable research interest to researchers, as compared to those known sewage treatment processes.
The piezoelectric effect refers to that mechanical stress is applied to the piezoelectric material in modes of ultrasonic, stirring, water flow, extrusion and the like, so that potential polarization occurs in the piezoelectric material, and according to different polarization directions, reverse piezoelectric effect or positive piezoelectric effect can be possibly caused to generate, a large number of electrons and holes are generated, and the polarized electrons can serve as a reductive active substance in hydrogen evolution reaction, so that efficient generation of hydrogen is realized.
In recent years, researchers have reported low cost, bandgap-wide semiconductor materials in which bismuth ferrite p-type (BiFeO 3 The semiconductor abbreviated as BFO has the advantages of narrow band gap (2.2 eV), good carrier transmission capability and the like, and is an ideal photocatalytic semiconductor material. However, some of its inherent drawbacks, such as BiFeO 3 Because of its conduction band edge of about 0.33eV, compared to H 2 /H 2 O redox potential correction is impossible to perform photocatalytic hydrogen evolution, but a sufficiently strong piezoelectric field may cause conduction band tilt, thereby correcting its conduction band edge to the redox potential of Hydrogen Evolution Reaction (HER), biFeO 3 The nano particles can realize the piezoelectric catalysis decomposition of the water to produce hydrogen and pure phase BiFeO under the action of mechanical force 3 Due to the energy band structure and piezoelectric performance, the piezoelectric catalysis hydrogen production efficiency is low, and in order to overcome the defect, the samarium doped BiFeO is prepared by adopting a coprecipitation method 3 Nanomaterial to further enhance BiFeO 3 And the piezoelectric catalytic hydrogen production performance is studied.
Disclosure of Invention
The invention aims to solve the problem that due to BiFeO 3 Limited band structure and piezoelectric performance, resulting in piezoelectric catalysisThe hydrogen production efficiency is lower. Currently, the modification of a multi-metal oxide by doping rare earth elements is one of the main methods for improving the material performance. Doping of rare earth elements can lead to the improvement of the piezoelectric performance of the material and the change of the energy band structure, thereby improving BiFeO 3 Is used for the piezoelectric catalysis hydrogen production performance. The invention relates to preparation of samarium-doped bismuth ferrite composite nano material and research on hydrogen production performance of piezoelectric catalysis.
The invention relates to preparation and piezoelectric catalysis application of samarium doped bismuth ferrite nano-materials, which mainly relate to the following steps: the preparation and characterization of samarium doped bismuth ferrite nano material and the research of the piezoelectric catalysis hydrogen production performance of the nano material are specifically carried out by the following steps:
dissolving bismuth nitrate, ferric nitrate and samarium nitrate in a dilute nitric acid solution, and performing ultrasonic treatment to form a uniform transparent colorless solution; then adjusting the pH value of the solution to enable the solution to be alkaline, centrifuging the solution to obtain a precipitate, and drying to obtain a certain amount of solid;
grinding the solid obtained in the first step, and placing the ground powder into a tube furnace to be heated from room temperature to a calcination temperature at a certain heating rate for calcination to obtain calcined solid powder;
step three, washing the solid powder calcined in the step two with acid washing water, centrifuging, alternately carrying out three times, finally washing with ethanol, and vacuum drying to obtain samarium-doped bismuth ferrite nano-particles;
in the first step, the molar ratio of bismuth nitrate to samarium nitrate is 0.8:0.2.
The volume ratio of the dilute nitric acid solution to the water is as follows: 1:30 to 40.
And in the first step, the pH value is alkaline and is 9-10.
The drying conditions in the first step are as follows: the oven temperature is 50-70 ℃, more preferably 60 ℃; the time is 9 to 14 hours, preferably 12 hours.
And in the second step, the heating rate is 4-8 ℃/min, preferably 5 ℃/min.
The calcination temperature in the second step is 300-500 ℃, preferably 500 ℃.
The calcination time in the second step is 30 to 60 minutes, more preferably 60 minutes.
The centrifugation speed in the third step is 9000r/min.
The conditions of vacuum drying described in the third step: the temperature is 50-70 ℃, preferably 60 ℃; the vacuum degree is-25 to-30 kpa, preferably-30 kpa; the time is 9 to 14 hours, preferably 12 hours.
The application of samarium doped bismuth ferrite nano material in piezocatalysis decomposition of water to produce hydrogen is specifically as follows: uniformly dispersing samarium-doped bismuth ferrite material in Na 2 SO 3 Introducing N into the solution 2 Oxygen is removed and the amount of hydrogen produced is measured by gas chromatography under the influence of mechanical force.
The mechanical force in the fourth step is specifically generated by the following method: and carrying out ultrasonic treatment on the solution containing the samarium-doped bismuth ferrite nano material.
Preferably, the ultrasonic frequency is 20-60 kHz, more preferably 40kHz.
The samarium-doped bismuth ferrite nano material is characterized and the piezoelectricity catalytic hydrogen production performance is tested by an X-ray powder diffractometer, a transmission electron microscope, a gas chromatograph and other instruments.
The invention has the advantages and effects that:
the method is simple to operate, the samarium doped bismuth ferrite nano material is synthesized by a coprecipitation method, the energy band can be narrowed by doping the rare earth ions to modify the bismuth ferrite, the conduction band is corrected, the energy band is inclined due to piezoelectric catalysis, and the samarium doped bismuth ferrite conduction band is more corrected than the bismuth ferrite conduction band potential, so that the improvement of the piezoelectric catalysis hydrogen production efficiency of the semiconductor nano material is facilitated. Compared with pure-phase bismuth ferrite, the samarium-doped bismuth ferrite piezoelectric catalysis hydrogen production amount is 3.4 times that of the pure-phase bismuth ferrite material, and the hydrogen production efficiency is effectively improved. The invention has simple process, easily obtained materials and lower cost, and is beneficial to industrial production.
Description of the drawings:
FIG. 1 is an X-ray powder diffraction pattern of samarium doped bismuth ferrite nanomaterial;
FIG. 2 is a transmission electron microscope image of samarium doped bismuth ferrite nanomaterial;
FIG. 3 is a fluorescence spectrum diagram of samarium doped bismuth ferrite nano-material;
FIG. 4 is a bar graph comparing hydrogen yields of bismuth ferrite and samarium doped bismuth ferrite nanomaterials.
Detailed Description
Embodiment 1:
dissolving 0.4268g of bismuth nitrate, 0.4040g of ferric nitrate and 0.097g of samarium nitrate in 33mL of dilute nitric acid solution, and performing ultrasonic treatment to form a uniform transparent colorless solution; then the pH value of the solution is regulated to 9.8, and the solution is centrifugated and put into a drying box to be dried for 12 hours at 60 ℃ to obtain solid powder;
step two, grinding the solid to powder by an agate mortar after the solid is cooled to room temperature, putting the powder into a tube furnace, heating to 300 ℃ at a heating rate of 5 ℃/min, calcining for 40 minutes, heating to 500 ℃ and calcining for 60 minutes to obtain calcined powder;
step three, the calcined powder is alternately centrifugally washed for 3 times by dilute nitric acid and deionized water, washed twice by absolute ethyl alcohol, and dried in vacuum at 60 ℃ to obtain samarium-doped bismuth ferrite nano-materials;
step four, 100mg of the samarium doped bismuth ferrite nano material obtained by the above method is uniformly dispersed into 100ml of Na 2 SO 3 In the solution, nitrogen was introduced into the sealed reactor for 30 minutes to remove oxygen, and then the amount of hydrogen above the reactor was measured under ultrasonic vibration from the 0 th minute, once every 20 minutes for a total of 1 hour.
The following tests are adopted to verify the effects of the invention:
1. preparation and characterization of samarium-doped bismuth ferrite nano material
And carrying out crystal phase structural characterization on the prepared samarium doped bismuth ferrite nano material and the pure-phase bismuth ferrite nano material by X-ray powder diffraction (XRD). The XRD patterns of samarium doped bismuth ferrite nanomaterial and pure phase bismuth ferrite nanomaterial are shown in FIG. 1, corresponding to the standard card for bismuth ferrite (JCPDS, no. 86-1518). As shown, diffraction peaks 2θ=22.4 °, 31.8 °, 32.0 °, 39.5 °, 45.8 °, and 51.3 ° correspond to iron, respectivelyThe (012), (104), (110), (202), (024) and (116) crystal planes of bismuth acid. The XRD diffraction pattern of the bismuth ferrite nano material is consistent with a standard PDF card (JCPDS No. 86-1518), and no other impurity phase appears in the bismuth ferrite, thus proving that the prepared bismuth ferrite has a standard rhombic perovskite structure. The XRD pattern of the samarium-doped bismuth ferrite nano material is basically consistent with that of bismuth ferrite, and diffraction peaks of other impurity phases are not found in the pattern. However, after Sm ion doping, the (104) and (110) crystal planes are bimodal to single peaks, and the diffraction peaks are shifted to the right. This is because of Sm 3+ 
Is smaller than Bi in bismuth ferrite 3+ />
Due to Sm after doping 3+ The radius is small, and the diffraction peak is right shifted after doping according to the Bragg diffraction equation 2dsin theta = nlambda, which shows that the substitution of Sm ions causes the compression of Fe-O bonds and the effective stretching of Bi-O bonds, and the structural distortion is more obvious. The results also show that the samarium doped bismuth ferrite nano material is successfully prepared.
The appearance of the prepared samarium-doped bismuth ferrite nano material is observed through a transmission electron microscope, as shown in fig. 2, the prepared samarium-doped bismuth ferrite nano material has an irregular square-like sheet appearance, and the average particle size is about 40-160 nm. The average particle size is slightly reduced after samarium ions are incorporated as compared with bismuth ferrite.
The separation and transfer conditions of the photo-generated carriers of the bismuth ferrite and samarium doped bismuth ferrite nano-materials are studied through fluorescence spectrum (PL) comparison. As shown in FIG. 3, the PL intensity of the samarium-doped bismuth ferrite nano material is obviously lower than that of bismuth ferrite, and the fluorescence quenching phenomenon shows that the prepared samarium-doped bismuth ferrite nano material effectively improves the separation efficiency of photo-generated electrons and holes.
2. Research on hydrogen production performance
The hydrogen production performance of bismuth ferrite and samarium doped bismuth ferrite nano material under ultrasonic vibration is detected by using a gas chromatograph, and the hydrogen production performance is carried out for 1 small under mechanical vibration (40 kHz)And (5) hydrogen production test. The comparison of hydrogen production of bismuth ferrite and samarium doped bismuth ferrite nanomaterials is shown in FIG. 4, wherein the hydrogen production of the bismuth ferrite nanomaterials is 766.4 mu mol.g only under the excitation of mechanical vibration (40 kHz) for 1h -1 Under the same conditions, the hydrogen yield of the samarium doped bismuth ferrite nano material is about 2592.1 mu mol.g when the mechanical vibration is carried out for 1h -1 The hydrogen production rate of the pure bismuth ferrite nano material is 3.4 times of that of the pure bismuth ferrite nano material, and the hydrogen production efficiency is obviously improved.
In conclusion, the method successfully synthesizes the samarium doped bismuth ferrite nano material by using the coprecipitation method and using bismuth nitrate, ferric nitrate and samarium nitrate as reactants. The piezoelectric catalysis hydrogen production performance of the samarium doped bismuth ferrite nano material is obviously improved. The method for producing hydrogen by using mechanical energy and piezoelectricity to catalyze and decompose water has simple process flow, strong operability and wide application prospect. The source of mechanical energy is wide, the effective utilization and conversion of mechanical energy and the generation of hydrogen energy are significant for the sustainable development of future society.
Claims (9)
1. The preparation method of the samarium-doped bismuth ferrite nano material is characterized by comprising the following steps of:
dissolving bismuth nitrate, ferric nitrate and samarium nitrate in a dilute nitric acid solution, and performing ultrasonic treatment to form a uniform transparent colorless solution; then adjusting the pH value to make the solution alkaline, centrifuging the solution to obtain a precipitate, and drying to obtain a certain amount of solid;
grinding the solid obtained in the first step, and placing the ground powder into a tube furnace for calcination to obtain calcined solid powder;
and thirdly, washing the solid powder calcined in the second step with acid washing water, centrifuging, alternately carrying out three times, finally washing with ethanol, and drying in vacuum to obtain the samarium-doped bismuth ferrite nano-particles.
2. The method according to claim 1, characterized in that:
the molar ratio of bismuth nitrate to samarium nitrate is 0.8:0.2;
the volume ratio of the concentrated nitric acid to the water in the dilute nitric acid solution in the first step is 1: 30-40 configuration;
the pH value in the first step is alkaline 9-10;
the drying conditions in the first step are as follows: the temperature of the oven is 50-70 ℃ and the time is 9-14 h.
3. The method according to claim 1, characterized in that:
step two, the heating rate is 4-8 ℃/min;
the calcination temperature in the second step is 300-500 ℃;
the calcination time in the second step is 30-60 min.
4. The method according to claim 1, characterized in that:
the centrifugal speed in the third step is 9000r/min;
conditions of vacuum drying in step three: the temperature is 50-70 ℃, the vacuum degree is minus 25-minus 30kpa, and the time is 9-12 h.
5. A samarium doped bismuth ferrite nanomaterial prepared by the method of claims 1 to 4.
6. The use of samarium-doped bismuth ferrite nanomaterial according to claim 5 in piezocatalytically decomposing water to produce hydrogen.
7. The application of samarium doped bismuth ferrite nano material in piezocatalysis decomposition of water to produce hydrogen is characterized by comprising the following specific steps: uniformly dispersing samarium-doped bismuth ferrite material in Na 2 SO 3 Introducing N into the solution 2 Oxygen is removed and the amount of hydrogen produced is measured by gas chromatography under the influence of mechanical force.
8. The method according to claim 7, characterized in that the mechanical force is generated in particular by: and carrying out ultrasonic treatment on the solution containing the samarium-doped bismuth ferrite nano material.
9. The method according to claim 7, wherein: the ultrasonic frequency is 20-60 kHz.
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| CN115007164A (en) * | 2022-06-27 | 2022-09-06 | 中山大学 | Preparation of rod-shaped bismuth ferrite piezoelectric catalyst and application of rod-shaped bismuth ferrite piezoelectric catalyst in preparation of hydrogen peroxide and hydrogen by catalytic cracking of water |
| WO2023272413A1 (en) * | 2021-06-27 | 2023-01-05 | 苏州大学 | Application of tin disulfide nanocatalyst in production of hydrogen by piezoelectric catalytic decomposition of water |
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| WO2023272413A1 (en) * | 2021-06-27 | 2023-01-05 | 苏州大学 | Application of tin disulfide nanocatalyst in production of hydrogen by piezoelectric catalytic decomposition of water |
| CN113896245A (en) * | 2021-09-30 | 2022-01-07 | 新沂市锡沂高新材料产业技术研究院有限公司 | Samarium-doped bismuth ferrite nano material and preparation method thereof |
| CN115007164A (en) * | 2022-06-27 | 2022-09-06 | 中山大学 | Preparation of rod-shaped bismuth ferrite piezoelectric catalyst and application of rod-shaped bismuth ferrite piezoelectric catalyst in preparation of hydrogen peroxide and hydrogen by catalytic cracking of water |
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