CN112973705A - Rare earth Er-doped NiO photocatalytic material, preparation method and application - Google Patents

Rare earth Er-doped NiO photocatalytic material, preparation method and application Download PDF

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CN112973705A
CN112973705A CN202110304674.0A CN202110304674A CN112973705A CN 112973705 A CN112973705 A CN 112973705A CN 202110304674 A CN202110304674 A CN 202110304674A CN 112973705 A CN112973705 A CN 112973705A
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rare earth
photocatalytic material
nio
solution
doped nio
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CN112973705B (en
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杨凯
禹振振
余长林
穆萍
夏君
郝金鸽
赵凯燕
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Jiangxi University of Science and Technology
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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
    • 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
    • B01J23/83—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 rare earths or actinides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/40—Carbon monoxide

Abstract

The invention provides a rare earth Er doped NiO photocatalytic material, a preparation method and application thereof, wherein the method comprises the following steps: weighing Ni (NO)3)2·5H2Adding deionized water into the solution to prepare a first solution, adding NaOH into the first solution to precipitate the first solution to obtain a first mixture, stirring the first mixture to obtain a first mixed solution, washing the first mixed solution by using the deionized water and absolute ethyl alcohol, and drying the first mixed solution to obtain a precursor Ni (OH)2(ii) a Respectively weighing KCl, LiCl and Er (NO)3)3·5H2O and a precursor Ni (OH)2And fully grinding to obtain a second mixture, placing the second mixture in an alumina crucible, grinding, mixing, stirring uniformly, calcining, naturally cooling to room temperature, alternately washing with deionized water and ethanol for multiple times, and finally drying to obtain the rare earth Er doped NiO photocatalytic material. The rare earth Er-doped NiO photocatalytic material provided by the invention can improve photocatalytic CO2ReducedEfficiency.

Description

Rare earth Er-doped NiO photocatalytic material, preparation method and application
Technical Field
The invention relates to the technical field of photocatalyst preparation, in particular to a rare earth Er-doped NiO photocatalytic material, a preparation method and application thereof.
Background
In today's global environment, the disposal of greenhouse gases (CO) in the atmosphere is being pursued due to the gradual depletion of fossil fuels and the increase of greenhouse gas emissions2) Are increasing and are becoming more and more urgent, as well as other associated problems of harmful environmental pollution. Generally, by reacting CO2Can be converted into CO and various useful low-carbon fuels, and can reduce CO in the atmosphere2Concentration to achieve a "closed-loop" carbon sequestration protocol.
With high energy demand CO2CO capture vs. geological sequestration2Seems to be a more attractive, feasible and promising approach for humans to address both energy and environmental issues. To date, many processes have been explored for converting carbon dioxide to hydrocarbon fuels, including catalytic, photocatalytic, electrocatalytic, and photoelectrocatalytic processes.
Currently, some potential methods for carbon dioxide abatement, using solar energy and heterogeneous photocatalysts to economically and sustainably photo-convert carbon dioxide and water, so-called artificial photosynthesis, can simulate natural photosynthesis and ideally enable the production of solar fuels and high-value chemicals (e.g., CO, formic acid, methane and methanol). Since 2011, the discussion of CO has2The research on selective photoreduction to solar fuels is increasing. More importantly, many different modification strategies have been developed including band gap engineering, surface vacancy engineering, crystal face engineering, micro/nano engineering, CO-catalyst engineering, and interface engineering (heterojunctions and Z-type systems) to improve semiconductor selectivity to CO2Activity and stability of photoreduction.
Nickel (II) oxide (NiO) is a natural p-type wide bandgap semiconductor (about 3.5eV) composed of a rich array of non-toxic elements on earth. Compared with a film which is easy to prepare into polycrystalline powder or a nano structure, the material is relatively cheap, low in toxicity and high in chemical/thermal stability, and is applied to the fields of photocatalysts, lithium ion batteries, magnetic materials, adsorbents, electrochromic devices, gas sensors and the like. The photocatalytic performance of NiO has been used for degrading organic pollutants such as methylene blue and rhodamine B (RhB), and the research is carried out under ultraviolet irradiation, because the wide forbidden band of NiO hinders the photocatalytic activity under visible light. Furthermore, it is reported that the rapid recombination of electron-hole pairs is another disadvantage that limits the NiO efficiency. In fact, by controlling the synthesis conditions, NiO samples with different numbers of defects (vacancies), colors, surface areas, morphologies, and visible light response can be generated to optimize the performance of NiO.
However, in the prior art, a method capable of effectively modifying NiO is lacked, so that the photocatalytic performance is poor, and the photocatalytic performance requirement in the actual application requirement cannot be well met.
Disclosure of Invention
Based on the above, the invention aims to solve the problems that in the prior art, the photocatalytic performance is poor and the photocatalytic performance requirement in the actual application requirement cannot be well met due to the lack of a method capable of effectively modifying NiO.
The invention provides a preparation method of a rare earth Er doped NiO photocatalytic material, wherein NiO is taken as a matrix, and a rare earth element Er is doped in a crystal lattice of the matrix NiO, and the method comprises the following steps:
step one, preparing precursor Ni (OH) by precipitation method2：
Weighing Ni (NO)3)2·5H2Adding deionized water, preparing at room temperature to obtain a first solution, adding weighed solid NaOH into the first solution, precipitating the first solution to obtain a first mixture, magnetically stirring the first mixture for a first time to obtain a first mixed solution, washing the first mixed solution with deionized water and absolute ethyl alcohol respectively, placing in a drying oven,controlling the drying at the first temperature for a second time to obtain a precursor Ni (OH)2；
Step two, preparing the photocatalytic material by a molten salt calcination method:
respectively weighing KCl, LiCl and Er (NO)3)3·5H2O and the precursor Ni (OH) prepared in the step one2Adding the mixture into a mortar for fully grinding to obtain a second mixture, placing the obtained second mixture into an alumina crucible, grinding, mixing and stirring uniformly, calcining for a third time under the environment of a second temperature, naturally cooling to room temperature, alternately washing for multiple times by deionized water and ethanol, and finally drying for a fourth time under the environment of a third temperature in a drying box to obtain the rare earth Er doped NiO photocatalytic material.
The invention provides a preparation method of a rare earth Er-doped NiO photocatalytic material, which comprises the steps of firstly preparing a precursor Ni (OH) by a precipitation method2Then weighing KCl, LiCl and Er (NO)3)3·5H2O, and the prepared precursor Ni (OH)2And preparing the rare earth Er-doped NiO photocatalytic material by a molten salt calcination method. In the invention, the rare earth Er-doped NiO photocatalytic material NiO-Er with oxygen-rich vacancies is designed and synthesized by a precipitation-molten salt calcination method, and due to the introduced rare earth ions, the light absorption capacity of the material is enhanced, the oxygen vacancy content is increased, so that the photocatalytic performance is obviously improved, and the requirement of the actual photocatalytic performance is met.
The preparation method of the rare earth Er-doped NiO photocatalytic material comprises the step two, wherein the mass ratio of LiCl to KCl is A: B, and Ni (OH)2And Er (NO)3)3·5H2The mass ratio of O is C: D;
wherein, the mass range of A is 2.5-2.7 g, the mass range of B is 3.1-3.3 g, the amount of C is 4-5 mmol, and the amount of D is 0.1-0.5 mmol.
The preparation method of the rare earth Er-doped NiO photocatalytic material comprises the step one, wherein the first solution is Ni (NO)3)2Solution of said Ni (NO)3)2The preparation method of the solution comprises the following steps:
adding a first molar amount of Ni (NO)3)2·5H2O is completely dissolved in a first predetermined volume of deionized water to obtain the Ni (NO)3)2And (c) a solution, wherein the first molar mass is 8-10 mmol, and the first preset volume is 32-40 ml.
The preparation method of the rare earth Er-doped NiO photocatalytic material comprises the step one, wherein the mass of solid NaOH added in the step one is 0.64-0.8 g, and the volumes of deionized water and absolute ethyl alcohol added in the step one are 10-15 mL.
The preparation method of the rare earth Er-doped NiO photocatalytic material comprises the steps that the first time is 0.5-1 h, the first temperature is 60 ℃, the second time is 8h, the second temperature is 400 ℃, the third time is 3h, the third temperature is 60 ℃ and the fourth time is 8 h.
The preparation method of the rare earth Er-doped NiO photocatalytic material comprises the step one, wherein the obtained Ni (NO) is prepared3)2The color of the solution is green; after addition of NaOH, the Ni (NO)3)2The solution turns from green to light green;
the rare earth Er-doped NiO photocatalytic material obtained after calcination and drying is black.
The preparation method of the rare earth Er-doped NiO photocatalytic material comprises the following steps of:
the prepared precursor Ni (OH)2And placing the sealed container in a sealed container, vacuumizing the sealed container, and then placing the sealed container in an electric field with preset electric field intensity and a magnetic field with preset magnetic field intensity for standing for 2 hours.
The preparation method of the rare earth Er-doped NiO photocatalytic material comprises the steps that the preset electric field intensity is 3-25V/m, and the preset magnetic field intensity is 1-20A/m.
The invention also provides a rare earth Er doped NiO photocatalytic material, wherein the photocatalytic material is prepared by the preparation method.
The invention also provides an application of the rare earth Er doped NiO photocatalytic material, and the rare earth Er doped NiO photocatalytic material is prepared by the preparation method, wherein the rare earth Er doped NiO photocatalytic material is used for converting greenhouse gas CO in the air2Converted to CO to block the carbon recycle chain.
Additional features and advantages of the disclosure will be set forth in the description which follows, or in part may be learned by the practice of the above-described techniques of the disclosure, or may be learned by practice of the disclosure.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic diagram of CO yield and selectivity of a NiO-2Er sample under different light source irradiation;
FIG. 2 shows CO and H of different samples under 365nm LED lamp illumination according to the present invention2A yield plot;
FIG. 3 is a XRD pattern corresponding to various samples of the present invention;
FIG. 4 is a graph of the diffuse reflectance of UV light for different catalyst materials in accordance with the present invention;
FIG. 5 is a graph of the corresponding room temperature EPR for each sample of the present invention;
FIG. 6 is a graph of photocurrent response corresponding to each sample in the present invention;
FIG. 7 is an impedance plot of a sample of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In the prior art, a method capable of effectively modifying NiO is lacked, so that the photocatalytic performance is poor, and the photocatalytic performance requirement in the actual application requirement cannot be well met.
Example one
In order to solve the technical problem, the invention provides a preparation method of a rare earth Er-doped NiO photocatalytic material, wherein the specific synthesis method comprises the following steps:
(1) step one, preparing precursor Ni (OH) by precipitation method2：
Firstly weighing 8-10 mmol of Ni (NO)3)2·5H2And adding O into 32-40 mL of deionized water, and preparing at room temperature to obtain a solution. Then weighing 0.64-08 g of NaOH to precipitate the NaOH to obtain a first mixture, magnetically stirring the first mixture for 0.5-1 h, washing the obtained first mixed solution with 10-15 mL of deionized water and absolute ethyl alcohol respectively after stirring is finished, and drying the first mixed solution in a drying box at the temperature of 60 ℃ for 8h to obtain a precursor Ni (OH)2；
(2) Step two, preparing the photocatalytic material by a molten salt calcination method:
weighing KCl, LiCl and Er (NO)3)3·5H2O and the precursor Ni (OH) prepared in the step one2And adding the mixture into a mortar for sufficient grinding to obtain a second mixture. And then placing the obtained second mixture in an alumina crucible, calcining for 3h at the temperature of 400 ℃, naturally cooling to room temperature, washing for multiple times by using deionized water and ethanol alternately, and finally drying for 8h in a drying oven at the temperature of 60 ℃ to finally obtain the rare earth Er doped NiO photocatalytic material.
It is noted that, in the present invention, LiCl and KCl are added in a mass ratio of (2.5-27 g): (3.1-33 g), and Ni (OH) is added2And Er (NO)3)3·5℃2The mass ratio of O is (4 to 5mmol) to (0.1 to 05 mmol).
The method for preparing the rare earth Er-doped NiO photocatalytic material containing oxygen vacancies according to the present invention will be described in more detail with reference to several specific examples.
Example two
The preparation method of the rare earth Er-doped NiO photocatalytic material with oxygen-rich vacancies, which is provided by the second embodiment of the invention, comprises the following specific implementation modes:
(1) step one, preparing precursor Ni (OH) by precipitation method2：
First, 10mmol of Ni (NO) is weighed3)2·5H2O was added to 40mL of deionized water to prepare a solution at room temperature, and then 0.8g of NaOH was weighed out and precipitated to obtain a mixture. Magnetically stirring the mixture for 0.5h, after stirring, respectively washing the obtained mixed solution with 10mL of deionized water and absolute ethyl alcohol, and then drying the mixed solution for 8h at the temperature of 60 ℃ in a drying oven to obtain a precursor Ni (OH)2；
(2) Step two, preparing the photocatalytic material by a molten salt calcination method:
weighing KCl, LiCl and Er (NO)3)3·5H2O and the precursor Ni (OH) prepared in the step one2And adding the mixture into a mortar for sufficient grinding to obtain a mixture. The resulting mixture was then placed in an alumina crucible, controlled at a temperature of 400 deg.CCalcining for 3 hours, naturally cooling to room temperature, washing with deionized water and ethanol for multiple times alternately, and finally drying in a drying oven at 60 ℃ for 8 hours to obtain the rare earth Er doped NiO photocatalytic material, which is recorded as NiO-2 Er.
In this example, LiCl and KCl were added in a mass ratio of 2.7 g: 3.3g, and Ni (OH) was added2And Er (NO)3)3·5H2The mass ratio of O was 5 mmol: 0.1 mmol.
EXAMPLE III
The preparation method of the rare earth Er-doped NiO photocatalytic material with oxygen-rich vacancies, which is provided by the third embodiment of the invention, comprises the following specific implementation modes:
(1) step one, preparing precursor Ni (OH) by precipitation method2：
First, 10mmol of Ni (NO) is weighed3)2·5H2O40 mL of deionized water was added to prepare a solution at room temperature, and 0.8g of NaOH was weighed out and precipitated. Magnetically stirring the mixture for 0.5h, after stirring, respectively washing the obtained mixed solution with 10mL of deionized water and absolute ethyl alcohol, and then drying the mixed solution in a drying oven at the temperature of 60 ℃ for 8h to obtain a precursor Ni (OH)2。
(2) Step two, preparing the photocatalytic material by a molten salt calcination method:
respectively weighing KCl, LiCl and Er (NO)3)3·5H2O and the precursor Ni (OH) prepared in the step one2And adding the mixture into a mortar for fully grinding. And then placing the obtained mixture in an alumina crucible, calcining for 3h at the temperature of 400 ℃, naturally cooling to room temperature, alternately washing for multiple times by using deionized water and ethanol, and finally drying for 8h in a drying box at the temperature of 60 ℃ to obtain the rare earth Er doped NiO photocatalytic material, which is marked as NiO-5 Er.
In this example, LiCl and KCl were added in a mass ratio of 2.7 g: 3.3g, Ni (OH)2And Er (NO)3)3·5H2The mass ratio of O was 5 mmol: 0.25 mmol.
Example four
The fourth embodiment of the invention provides a preparation method of a rare earth Er-doped NiO photocatalytic material with oxygen-rich vacancies, which comprises the following specific implementation modes:
(1) step one, preparing precursor Ni (OH) by precipitation method2：
First, 10mmol of Ni (NO) is weighed3)2·5H2O was added to 40mL of deionized water to prepare a solution at room temperature, and then 0.8g of NaOH was weighed out and precipitated to obtain a mixture. Magnetically stirring the mixture for 0.5h, after stirring, respectively washing the obtained mixed solution with 10mL of deionized water and absolute ethyl alcohol, and then drying for 8h at the temperature of 60 ℃ in a drying oven to obtain a precursor Ni (OH)2；
(2) Step two, preparing the photocatalytic material by a molten salt calcination method:
weighing KC, LiCl and Er (NO)3)3·5H2O and the precursor Ni (OH) prepared in the step one2And adding the mixture into a mortar for fully grinding. And then placing the obtained mixture in an alumina crucible, calcining for 3h at the temperature of 400 ℃, naturally cooling to room temperature, alternately washing for multiple times by using deionized water and ethanol, and finally drying for 8h at the temperature of 60 ℃ in a drying box to obtain the rare earth Er doped NiO photocatalytic material, which is marked as NiO-10 Er.
In this example, LiCl and KCl were added in a mass ratio of 2.7 g: 3.3g, and Ni (OH) was added2And Er (NO)3)3·5H2The mass ratio of O was 5 mmol: 0.5 mmol.
In the invention, in addition, in order to further improve the CO content of the rare earth Er doped NiO photocatalytic material2Reduced photocatalytic performance, as compared to the precursor Ni (OH) prepared in step one2Appropriate treatment is performed. Specifically, after step one, and before step two, precursor Ni (OH) may be added2The following operations are carried out:
the prepared precursor Ni (OH)2Placing the container in a closed container, vacuumizing the closed container, and then positioning the closed container in the closed containerStanding for 2h in an electric field with preset electric field intensity and a magnetic field with preset magnetic field intensity. Wherein the preset electric field strength is 3-25V/m, and the preset magnetic field strength is 1-20A/m.
Here, since Ni itself has ferromagnetism, a precursor Ni (OH) is obtained in the production2Then, the precursor is put into a preset electric field and a preset magnetic field for treatment, and the precursor Ni (OH) can be obtained to a certain extent2The granularity is more uniform, the micro crystal lattice sequence is more ordered, and the introduction of oxygen vacancies into NiO crystal lattices can be further promoted, so that the photocatalytic performance is further improved.
EXAMPLE five
In this example, the rare earth Er-doped NiO photocatalytic material prepared as described above was used to photocatalyze CO2Evaluation of the performance of the reduction:
specifically, the evaluation method comprises the following operation steps:
detection of CO and H by gas chromatography hydrogen ion flame detector (FID) and thermal conductivity cell detector (TCD), respectively2Reducing CO by irradiating with 80W LED lamp light source2The photocatalytic activity of the samples was evaluated. Briefly, a 50mL quartz reactor was charged with 30mg of catalyst, 5mg of 2, 2-bipyridinium ruthenium, and 3mL acetonitrile, 2mL DI water, and 1mL triethanolamine solution (as a hole sacrificial agent) were added. Introducing CO for 30min before the reaction is started2The solution is saturated with gas, and then CO is introduced into the gas control reactor2The pressure is 1atm, 1mL of gas is respectively taken every 2H after the illumination is started, and the gas enters a chromatographic detector (TCD and FID) to detect the CO and H of the reaction2And (4) yield.
Wherein, in the dark reaction, the 2, 2-bipyridyl ruthenium has almost no CO2Reducing power. However, when the NiO catalyst was added, the CO was significantly increased2Reducing power. And moreover, the addition of the rare earth Er-doped NiO material can further promote the photocatalytic performance of the NiO material, and the yield of CO in the same time is obviously higher than that of CO in pure NiO.
Specifically, as can be seen from fig. 1 and 2:
CO generation after illumination of rare earth Er-doped NiO material under illumination of LED lampThe rate is obviously higher than that of pure NiO. However, as the doping amount of Er increases ( numbers 2, 5 and 10 in fig. 2 represent the doping ratio of Er), the reactivity is significantly reduced, which is probably due to the fact that more Er is formed as the content of Er increases2O3This results in a further increase in the oxygen vacancy concentration, thereby increasing the number of recombination of electrons and holes. In general, under the irradiation of different light sources, the rare earth Er doped NiO material shows good selectivity.
Referring to fig. 3, fig. 3 is a XRD chart corresponding to different samples in the present invention. The pure NiO shown in FIG. 3 corresponds to the standard card PDF #47-1049 for NiO, whereas Er appears for the composite sample NiO-Er2O3The peak corresponding to the standard card PDF #26-0604 is more obvious in the peak protrusion with the increase of Er, which indicates that more Er is generated2O3。
Referring to fig. 4, fig. 4 is a graph of the diffuse reflection of ultraviolet light (UV-vis-DRS spectrum) corresponding to different catalyst materials in the present invention, as can be seen from fig. 4: the maximum absorption wavelength of a pure NiO sample is 200-400 nm, when 2% of Er is introduced, the light absorption capacity of the pure NiO sample is obviously improved at 200-600 nm, and when the content of the Er is increased, the light absorption capacity is reduced on the contrary.
Referring to fig. 5, fig. 5 is a graph of room temperature EPR corresponding to each sample of the present invention. As can be seen from fig. 5: at a g value of 2.002 with direct calcination of Ni (OH)2Compared with NiO (NiO-KCl) synthesized in molten salt atmosphere, the obtained NiO has more obvious signal response. And the signal of the NiO-2Er is further enhanced, which shows that the molten salt system can effectively introduce oxygen vacancies into the NiO crystal lattice, and the existence of the Er can further stabilize the oxygen vacancies.
Referring to fig. 6 and 7, fig. 6 is a photo current response diagram corresponding to each sample in the present invention, and fig. 7 is an impedance diagram of the sample in the present invention.
Specifically, the photocurrent density-time curve indicates the generation of photo-generated charges by the semiconductor photocatalyst, while a lower photocurrent density indicates a greater probability of recombination of photo-generated electrons and holes. As shown in fig. 6: the photocurrent response of the sample NiO-2Er is stronger, which indicates that the NiO-2Er can generate more photon-generated carriers and can more effectively separate and transfer photon-generated electrons/holes. Electrochemical ac impedance spectroscopy further investigated the charge transfer efficiency of the prepared samples. The size of the curvature radius of the curve in the electrochemical alternating-current impedance spectrum is directly reflected by the size of the resistance of charge transfer.
Referring to fig. 7, as shown in fig. 7: compared with a pure NiO sample, the curvature radius of a curve in an electrochemical alternating-current impedance spectrum of the NiO-2Er composite material is minimum, which shows that the charge transfer resistance is minimum, and the charge separation efficiency is highest, and is consistent with a photocurrent test result.
Finally, it should be noted that: the above-mentioned embodiments are only specific embodiments of the present invention, which are used for illustrating the technical solutions of the present invention and not for limiting the same, and the protection scope of the present invention is not limited thereto, although the present invention is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: any person skilled in the art can modify or easily conceive the technical solutions described in the foregoing embodiments or equivalent substitutes for some technical features within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the embodiments of the present invention, and they should be construed as being included therein. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (10)

1. A preparation method of a rare earth Er doped NiO photocatalytic material is characterized in that NiO is used as a matrix, and rare earth element Er is doped in crystal lattices of the NiO matrix, and the method comprises the following steps:
step one, preparing precursor Ni (OH) by precipitation method2：
Weighing Ni (NO)3)2·5H2Adding deionized water into O, preparing at room temperature to obtain a first solution, adding weighed solid NaOH into the first solution, precipitating the first solution to obtain a first mixture, magnetically stirring the first mixture for a first time, and stirring to obtain a first mixtureMixing the solution, washing the first mixed solution with deionized water and absolute ethyl alcohol respectively, and then drying the first mixed solution in a drying box for a second time under the environment of first temperature control to obtain a precursor Ni (OH)2；
Step two, preparing the photocatalytic material by a molten salt calcination method:
respectively weighing KCl, LiCl and Er (NO)3)3·5H2O and the precursor Ni (OH) prepared in the step one2Adding the mixture into a mortar for fully grinding to obtain a second mixture, placing the obtained second mixture into an alumina crucible, grinding, mixing and stirring uniformly, calcining for a third time under the environment of a second temperature, naturally cooling to room temperature, alternately washing for multiple times by deionized water and ethanol, and finally drying for a fourth time under the environment of a third temperature in a drying box to obtain the rare earth Er doped NiO photocatalytic material.
2. The method for preparing the rare earth Er-doped NiO photocatalytic material as claimed in claim 1, wherein in the second step, the mass ratio of LiCl to KCl is A: B, Ni (OH)2And Er (NO)3)3·5H2The mass ratio of O is C to D;
wherein, the mass range of A is 2.5-2.7 g, the mass range of B is 3.1-3.3 g, the amount of C is 4-5 mmol, and the amount of D is 0.1-0.5 mmol.
3. The method for preparing a rare earth Er-doped NiO photocatalytic material according to claim 2, wherein in the first step, the first solution is Ni (NO)3)2Solution of said Ni (NO)3)2The preparation method of the solution comprises the following steps:
adding a first molar amount of Ni (NO)3)2·5H2O is completely dissolved in a first predetermined volume of deionized water to obtain the Ni (NO)3)2And (c) a solution, wherein the first molar mass is 8-10 mmol, and the first preset volume is 32-40 ml.
4. The preparation method of the rare earth Er-doped NiO photocatalytic material as claimed in claim 3, wherein in the first step, the mass of solid NaOH added is 0.64-0.8 g, and the volumes of deionized water and absolute ethyl alcohol added are 10-15 mL.
5. The method for preparing the rare earth Er-doped NiO photocatalytic material according to claim 1, wherein the first time is 0.5-1 h, the first temperature is 60 ℃, the second time is 8h, the second temperature is 400 ℃, the third time is 3h, the third temperature is 60 ℃ and the fourth time is 8 h.
6. The method for preparing a rare earth Er-doped NiO photocatalytic material according to claim 3, wherein in the first step, the obtained Ni (NO) is configured3)2The color of the solution is green; after addition of NaOH, the Ni (NO)3)2The solution turns from green to light green;
the rare earth Er-doped NiO photocatalytic material obtained after calcination and drying is black.
7. The method of preparing a rare earth Er doped NiO photocatalytic material according to claim 3, wherein after said first step and before said second step, said method further comprises:
the prepared precursor Ni (OH)2And placing the sealed container in a sealed container, vacuumizing the sealed container, and then placing the sealed container in an electric field with preset electric field intensity and a magnetic field with preset magnetic field intensity for standing for 2 hours.
8. The method for preparing the rare earth Er-doped NiO photocatalytic material according to claim 7, wherein the preset electric field strength is 3-25V/m, and the preset magnetic field strength is 1-20A/m.
9. A rare earth Er doped NiO photocatalytic material, characterized in that it is prepared by the method of any one of the preceding claims 1 to 8.
10. The application of the rare earth Er-doped NiO photocatalytic material prepared by the preparation method of any one of the claims 1 to 8 is characterized in that the rare earth Er-doped NiO photocatalytic material is used for converting greenhouse gas CO in the air2Converted to CO to block the carbon recycle chain.
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