CN112960694A - Preparation method of green bismuth vanadate particles - Google Patents
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- 239000002245 particle Substances 0.000 title claims abstract description 56
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 22
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 22
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000011282 treatment Methods 0.000 claims abstract description 16
- 239000011521 glass Substances 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims abstract description 8
- 239000005401 pressed glass Substances 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 5
- 238000013532 laser treatment Methods 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 230000004298 light response Effects 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 description 7
- 230000031700 light absorption Effects 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 6
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- 239000002994 raw material Substances 0.000 description 5
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- B01J35/33—
-
- B01J35/39—
-
- B01J35/50—
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Abstract
The invention provides a preparation method of green bismuth vanadate particles, which comprises the following steps: s11 taking yellow BiVO4Preheating the particles at a temperature to remove the adhered yellow BiVO4Impurities on the surface of the particles; s12 preheating treated yellow BiVO4Placing the particles on a quartz glass substrate and performing tabletting treatment by covering tabletting glass; s13 laser is adopted to perform laser treatment on yellow BiVO of cover pressed glass with certain surface flatness4Performing irradiation for a predetermined time; s14 pairs of green BiVO obtained after irradiation4After the sample is remixed uniformly, the steps S12 and S13 are repeated a plurality of times until the sample powder is green and uniform. BiVO (bismuth VO) of green bismuth vanadate particles prepared by using method4The visible light response performance is realized, and simultaneously, the doping is not required to be carried out by introducing elements into the bulk phase, so that the integrity of the bulk phase can be ensuredAlso avoids BiVO4The lattice is distorted.
Description
Technical Field
The invention relates to the technical field of material chemistry, in particular to a preparation method of green bismuth vanadate particles.
Background
Bismuth vanadate (BiVO)4) Is aThe bright yellow inorganic chemical pigment which is widely applied does not contain heavy metal elements harmful to human bodies, and is a new-generation environment-friendly low-carbon metal oxide material. BiVO4In addition to their properties as colorants, have a wide variety of applications. The photo-induced electron and the hole with high energy activity can kill bacteria such as escherichia coli, staphylococcus aureus and the like. In addition, BiVO4Also applied to the environmental air purification, and decompose organic compounds and toxic substances in the air, such as benzene, formaldehyde, ammonia, TVOC and the like, and play a role in purifying the air. As an excellent semiconductor material, it can also be used as a catalyst to accelerate the progress of chemical reactions. The method has wide application in the aspects of photocatalytic degradation of organic pollutants, photocatalytic decomposition of water, and the like in a photoreaction system such as a photoelectrocatalysis electrode material. Therefore, the response intensity of the compound is further enhanced in the range of visible light (about 45 percent of the total amount of sunlight), the absorption range of the visible light is widened, and the BiVO is expanded4The key technology of the application condition of the semiconductor material.
BiVO with visible light response commonly used at present4The semiconductor material is still yellow monoclinic BiVO4. To further enhance the visible light response intensity, it is generally doped with an element. In this approach, BiVO is directly regulated by element doping4The energy band structure introduces an impurity energy level into the energy band, thereby reducing the forbidden bandwidth of the energy band structure and inducing the energy band structure to have response absorption to visible light of different wave bands. Such as Wang et al (J.alloy. Comp.522(2012)19) pairs BiVO with La, Sm, Nd, Gd, Eu, Y and other elements4By doping and introducing an intermediate energy level into the energy band, the visible light absorption performance of different wavebands can be adjusted and the light response intensity of the visible light absorption can be obviously enhanced. Yao et al (Dalton trains. (2008)1426) use Mo element for BiVO4Doping is carried out, so that the light response intensity in a visible light region is obviously enhanced. In addition, the doping of non-metal elements such as P element and N element can also enhance the response intensity of visible light. However, the elements introduced by the above method are in BiVO4The distribution of bulk or surface is not controllable,and will cause BiVO4Distortion of lattice structure to BiVO4The defects are increased, and the physical and chemical properties of the composite are seriously influenced.
Another method in the prior art is to subject BiVO to4And (5) carrying out semiconductor compounding. ZHao et al (appl.Catal.B: environ.115-116(2012)90) utilize CuO and BiVO4And (4) carrying out recombination, and obviously enhancing the response intensity of the compound to the visible light with the wavelength of 400-700nm by constructing a heterojunction structure. Grimes et al (Nano Lett.11(2011)1928) utilize WO3For BiVO4The composite modification can enhance the visible light response intensity and improve the photoelectric properties such as photocurrent density and the like. In addition, some metals with plasma resonance effect can also promote BiVO4Such as Xue et al (ACS appl. mater. interfaces 4(2012)418) reinforcing BiVO with nano Au particles4Light absorption properties of (a). When BiVO is reduced4The absorption intensity in the visible light region is significantly enhanced by the size of the particles below their quantum size (ACS catal.4(2014) 3498). The disadvantage is that these methods can ensure BiVO4The integrity of the crystal structure is seriously dependent on the light absorption performance of the compound semiconductor, and the compound semiconductor is in BiVO4The distribution and state of the surface can influence the light absorption performance of the whole system, and the BiVO of the quantum dots4Is extremely unstable to BiVO4The practical use of the composite is disadvantageous.
Therefore, it is highly desirable to ensure BiVO4The integrity of the crystal structure can avoid BiVO4BiVO with lattice distortion4The preparation method of (1).
Disclosure of Invention
The invention provides a green bismuth vanadate BiVO4A preparation method of particles, which aims to solve the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme.
A preparation method of green bismuth vanadate particles comprises the following steps:
s11 taking yellow BiVO4The particles are pre-heated at a certain temperature,for removing BiVO attached to the yellow color4Impurities on the surface of the particles;
s12 preheating treated yellow BiVO4Placing the particles on a quartz glass substrate and performing tabletting treatment by covering tabletting glass;
s13 laser is adopted to perform laser treatment on yellow BiVO of cover pressed glass with certain surface flatness4Performing irradiation for a predetermined time;
s14 pairs of green BiVO obtained after irradiation4After the sample is remixed uniformly, the steps S12 and S13 are repeated a plurality of times until the sample powder is green and uniform.
Preferably, the certain temperature in step S11 is 200-300 ℃.
Preferably, the preheating treatment in step S11 is performed in a muffle furnace or a tube furnace under inert gas protection.
Preferably, the predetermined time is 5-15 s.
Preferably, the irradiation is performed 3 to 4 times in the step of S13 for one replacement of the pressed glass.
Preferably, the light source of the laser in the step S13 is: 300nm to 1700nm, the power of the laser light source is as follows: 1W to 1000W.
Preferably, the pulse width of the laser used in the step S13 is 1ps to 1000ns, and the pulse frequency is 10 to 10000 Hz.
Preferably, the yellow BiVO used in the step S114The particle size of the particles is 5nm-1000 nm.
Preferably, the certain surface flatness is that the surface fluctuation error range is-0.1 mm.
The green bismuth vanadate BiVO of the invention4The technical scheme provided by the preparation method of the particles can be seen that the invention utilizes the rapid laser to irradiate BiVO4Particles, preparation of Green bismuth Vanadate BiVO for enhancing visible light response4The particles adopt a laser irradiation technology, the preparation process is clean and pollution-free, the required reaction time is extremely short and is only 3-10 seconds, and the preparation efficiency is higher; because the required reaction time is short, the generation of surface defects is inhibited to the maximum extent; in promoting BiVO4The visible light response performance is simultaneouslyWithout introducing elements into the bulk phase for doping, the method not only can ensure the complete crystal structure of the bulk phase, but also avoids BiVO4Distortion of the crystal lattice; and BiVO obtained therefrom4The particles have enhanced visible light response and uniform powder color, and also exhibit good electrical transport properties.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 shows the green BiVO obtained by the method of example 24Comparing the light absorption performance of the sample and the raw material;
FIG. 2 shows BiVO obtained by the method of example 24Comparing the electric transport properties of the sample and the raw material;
FIG. 3 is BiVO obtained by the method of example 24A crystalline X-ray powder diffraction contrast plot of the sample and the starting material;
fig. 4 is an experimental optical path diagram of example 2.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. It will be understood that when an element is referred to as being "connected" or "coupled" to another element, it can be directly connected or coupled to the other element or intervening elements may also be present. Further, "connected" or "coupled" as used herein may include wirelessly connected or coupled. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including 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. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
For the convenience of understanding of the embodiments of the present invention, the following description will be further explained by taking several specific embodiments as examples with reference to the drawings, and the embodiments of the present invention are not limited thereto.
Example 1
The embodiment provides a preparation method of green bismuth vanadate particles, which comprises the following steps:
s11 taking yellow BiVO4Preheating the particles at a certain temperature of 200 ℃ to 300 ℃ for removing the particles attached to the yellow BiVO4Impurities on the surface of the particles. The preheating treatment can be carried out in a muffle furnace, and in order to ensure the cleanliness of the sample, the preheating treatment can also be carried out in a tube furnace under the protection of inert gas.
Wherein, the yellow BiVO4The particle size of the particles is 5nm-1000 nm.
S12 preheating treated yellow BiVO4The particles are placed on a quartz glass substrate and fed through a cover pressPerforming tabletting treatment;
s13 laser is adopted to obtain a certain surface flatness (the surface fluctuation error range is-0.1 mm) for the yellow BiVO of the cover tabletting glass4The irradiation is carried out for 5-15 s. The color of the glass is changed from transparent to non-transparent after laser irradiation, which affects the irradiation effect of the laser and needs to be replaced in time, and the replacement of the pressed glass is carried out once every 3-4 times of irradiation. The light source of the laser is: 300nm to 1700nm, the power of the laser light source is as follows: 1W to 1000W. The pulse width of the laser is 1ps-1000ns, and the pulse frequency is 10-10000 Hz.
S14 pairs of green BiVO obtained after irradiation4After the sample is remixed uniformly, the steps S12 and S13 are repeated a plurality of times until the sample powder is green and uniform.
It should be noted that the laser irradiation time needs to be selected according to the difference of the laser wavelength and the selected laser power. BiVO4The number of repeated irradiation also needs to be selected according to the difference of the laser wavelength and the selected laser power. The laser irradiation time and the number of repeated irradiation need to be according to BiVO4The difference in particle size is selected.
Example 2
A preparation method of green bismuth vanadate particles comprises the following steps:
(1) mixing yellow monoclinic BiVO4The particles (particle size 200nm) were pre-heated in a muffle furnace at 200 ℃ to clean the surface.
(2) The pretreated BiVO4And (3) performing tabletting treatment on the quartz glass substrate by covering tabletting glass, and ensuring that the surface fluctuation error range of the tabletted sample is-0.1 mm.
(3) BiVO for covering tabletting glass by laser4Carrying out irradiation treatment for 8s, wherein the parameters of the laser are selected as follows: wavelength 1064 nm; the power is 1W; the pulse frequency was 1000 Hz. The pulse width of the laser was 8 ns.
(4) Subjecting the BiVO subjected to primary irradiation in the step (3)4The particles are mixed uniformly again, the steps (2) and (3) are repeated for 6 times to obtain green uniform BiVO4And (3) granules.
FIG. 1 shows the exampleGreen BiVO obtained by the method of example4The comparison graph of the light absorption performance of the sample and the raw material is the test result of solid ultraviolet-visible light diffuse reflection (Uv-Vis). As can be seen, the green BiVO after irradiation4The sample is more original yellow BiVO4The light absorption intensity of the sample in the visible light region is significantly enhanced.
FIG. 2 shows BiVO obtained by the method of this example4And (3) comparing the electric transport properties of the sample and the raw material, namely testing results of a photo-current spectrum and an alternating current impedance spectrum. As can be seen, the green BiVO after irradiation4The sample is more original yellow BiVO4The sample, photocurrent density increased and the ac impedance value decreased.
FIG. 3 shows BiVO obtained by the method of this example4And (3) a crystal X-ray powder diffraction contrast diagram of the sample and the raw material, namely an XRD test result. As can be seen, the green BiVO after irradiation4Sample and original yellow BiVO4The lattice parameters of the sample are completely consistent, which shows that the crystal form and the crystal structure of the sample are kept unchanged before and after the sample is processed.
Fig. 4 is an experimental optical path diagram of the method of the embodiment, and referring to fig. 4, after laser is emitted by a laser, the laser is subjected to reflection focusing twice, and then irradiation treatment is performed on a pre-treated tabletting sample.
Example 3
The embodiment provides a preparation method of green bismuth vanadate particles, which comprises the following steps:
(1) mixing yellow monoclinic BiVO4The particles (particle size 200nm) were pre-heated in a muffle furnace at 200 ℃ to clean the surface.
(2) The pretreated BiVO4And (3) carrying out tabletting treatment on the quartz glass substrate, and ensuring that the surface fluctuation error range of the tabletted sample is-0.1 mm.
(3) BiVO by laser4Carrying out irradiation treatment for 8s, wherein the parameters of the laser are selected as follows: the wavelength is 532 nm; the power is 1W; the frequency is 1000 Hz. The pulse width of the laser was 8 ns.
(4) Subjecting the BiVO subjected to primary irradiation in the step (3)4The particles are mixed uniformly again, the steps (2) and (3) are repeated for 6 times to obtain green uniform BiVO4And (3) granules.
Example 4
The embodiment provides a preparation method of green bismuth vanadate particles, which comprises the following steps:
(1) to monoclinic BiVO4The particles (particle size 200nm) were pre-heated in a muffle furnace at 200 ℃ to clean the surface.
(2) The pretreated BiVO4And (3) performing tabletting treatment on the quartz glass substrate by covering tabletting glass, and ensuring that the surface fluctuation error range of the tabletted sample is-0.1 mm.
(3) BiVO by laser4Carrying out irradiation treatment for 8s, wherein the parameters of the laser are selected as follows: a wavelength of 355 nm; the power is 1W; the frequency is 1000 Hz. The pulse width of the laser was 8 ns.
(4) Subjecting the BiVO subjected to primary irradiation in the step (3)4The particles are mixed uniformly again, the steps (2) and (3) are repeated for 6 times to obtain green uniform BiVO4And (3) granules.
Example 5
A preparation method of green bismuth vanadate particles comprises the following steps:
(1) to monoclinic BiVO4The particles (particle size 500nm) were pre-heated in a muffle furnace at 200 ℃ to clean the surface.
(2) The pretreated BiVO4And (3) performing tabletting treatment on the quartz glass substrate by covering tabletting glass, and ensuring that the surface fluctuation error range of the tabletted sample is-0.1 mm.
(3) BiVO by laser4Carrying out irradiation treatment for 8s, wherein the parameters of the laser are selected as follows: wavelength 1064 nm; the power is 1W; the frequency is 1000 Hz. The pulse width of the laser was 8 ns.
(4) Subjecting the BiVO subjected to primary irradiation in the step (3)4The particles are mixed evenly again, the steps (2) and (3) are repeated for 8 times to obtain green uniform BiVO4And (3) granules.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A preparation method of green bismuth vanadate particles is characterized by comprising the following steps:
s11 taking yellow BiVO4Preheating the particles at a temperature to remove the adhered yellow BiVO4Impurities on the surface of the particles;
s12 preheating treated yellow BiVO4Placing the particles on a quartz glass substrate and performing tabletting treatment by covering tabletting glass;
s13 laser is adopted to perform laser treatment on yellow BiVO of cover pressed glass with certain surface flatness4Performing irradiation for a predetermined time;
s14 pairs of green BiVO obtained after irradiation4After the sample is remixed uniformly, the steps S12 and S13 are repeated a plurality of times until the sample powder is green and uniform.
2. The method as claimed in claim 1, wherein the temperature in step S11 is 200-300 ℃.
3. The method of claim 1, wherein the preheating step in step S11 is performed in a muffle furnace or a tube furnace under inert gas protection.
4. The method of claim 1, wherein the predetermined time is 5-15 s.
5. The method for preparing green bismuth vanadate particles according to claim 1, wherein the irradiation in the step S13 is performed 3 to 4 times to replace the pressed glass.
6. The method for preparing green bismuth vanadate particles according to claim 1, wherein the laser light source in the step S13 is: 300nm to 1700nm, the power of the laser light source is as follows: 1W to 1000W.
7. The method for preparing green bismuth vanadate particles according to claim 1, wherein the pulse width of the laser used in the step S13 is 1ps to 1000ns, and the pulse frequency is 10 to 10000 Hz.
8. The method for preparing green bismuth vanadate particles according to claim 1, wherein the yellow BiVO adopted in the step S114The particle size of the particles is 5nm-1000 nm.
9. The method for preparing green bismuth vanadate particles according to claim 1, wherein the certain surface flatness is a surface undulation error range of-0.1 mm.
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| JP2008019156A (en) * | 2006-06-16 | 2008-01-31 | Nagaoka Univ Of Technology | BiVO4 COLLOID DISPERSION AND METHOD OF MANUFACTURING THE SAME |
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| CN108070375A (en) * | 2016-11-15 | 2018-05-25 | 上海朗研光电科技有限公司 | The preparation method of upconversion fluorescence nano material |
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2021
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