CN111589447A - Heterojunction nano-particle and preparation method and application thereof - Google Patents
Heterojunction nano-particle and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 14
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
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- B01J23/682—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium, tantalum or polonium
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Abstract
The invention relates to the technical field of photocatalysis, in particular to heterojunction nano-particles and a preparation method and application thereof. The photocatalysis efficiency can be effectively improved through the synergistic effect of the ultrasonic and the plasma resonance; meanwhile, the spectrum absorption range of the heterostructure nanoparticles can be widened, and the sunlight utilization rate is effectively improved. The embodiment of the invention provides a heterojunction nanoparticle which is characterized by comprising a carrier and a noble metal loaded on the surface of the carrier, wherein the carrier is selected from piezoelectric materials with photocatalysis, and the carrier and the noble metal form a heterojunction. The embodiment of the invention is used for degrading organic pollutants and preparing hydrogen energy.
Description
Technical Field
The invention relates to the technical field of photocatalysis, in particular to heterojunction nano-particles and a preparation method and application thereof.
Background
In the photocatalysis, under the condition of certain wavelength illumination, a semiconductor material generates the separation of a photon-generated carrier, then a photon-generated electron and a hole are combined with ions or molecules to generate an active free radical with oxidability or reducibility, and the active free radical can drive the oxidation-reduction reaction. Therefore, the semiconductor material can be used as a photocatalyst to be applied to the technical fields of preparation of hydrogen energy, degradation of organic pollutants and the like.
However, the currently developed photocatalysts all have the disadvantages of low light utilization rate, low charge separation efficiency and the like, and the improvement of the catalytic activity of the photocatalyst is limited.
Disclosure of Invention
The invention mainly aims to provide heterojunction nanoparticles, and a preparation method and application thereof. The photocatalysis efficiency can be effectively improved through the synergistic effect of the ultrasonic and the plasma resonance; meanwhile, the spectrum absorption range of the heterostructure nanoparticles can be widened, and the sunlight utilization rate is effectively improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, embodiments of the present invention provide a heterojunction nanoparticle, including a support selected from piezoelectric materials having a photocatalytic effect, and a noble metal supported on a surface of the support, where the support and the noble metal form a heterojunction.
Optionally, the piezoelectric material is selected from BiFeO3、Ba0.5Na0.5TiO3、KNbO3And AgNbO3Any one of the above; the noble metal is selected from any one of Ag, Au and Pd.
Optionally, in the heterojunction nanoparticle, the mass fraction of the noble metal is w, and the balance is the piezoelectric material; wherein w is more than 0% and less than or equal to 10%.
In another aspect, an embodiment of the present invention provides a method for preparing a heterojunction nanoparticle, including: taking a piezoelectric material with a photocatalytic effect as a carrier, and depositing a noble metal compound on the surface of the carrier by a deposition precipitation method to obtain a precursor material; and calcining the precursor material in an air atmosphere to obtain the heterojunction nano-particles.
Optionally, taking a piezoelectric material with a photocatalytic effect as a carrier, and depositing a noble metal compound on the surface of the carrier by a deposition precipitation method to obtain a precursor material; the method comprises the following steps: dissolving the piezoelectric material with the photocatalysis effect by using deionized water, adjusting the pH value of the aqueous solution to be between 9 and 13 by using ammonia water, adding the aqueous solution of the noble metal compound, and reacting for a preset time under heating to obtain the precursor material.
Optionally, the reaction temperature is between 50 and 110 ℃, and the preset time is 1 to 2 hours.
Optionally, the calcination temperature is 300-500 ℃, and the calcination time is 1-2 h.
Optionally, before the precursor material is obtained by depositing a noble metal compound on the surface of a support, which is a piezoelectric material with a photocatalytic function, by a deposition precipitation method, the preparation method further includes: the piezoelectric material is prepared by hydrothermal synthesis.
On the other hand, the embodiment of the invention provides an application of the heterojunction nano-particles as the photocatalyst in preparation of hydrogen energy.
Optionally, hydrogen is produced by decomposing water by ultrasound and/or illumination.
In another aspect, an embodiment of the present invention provides an application of the heterojunction nanoparticle as described above as a photocatalyst in organic matter degradation.
Optionally, the organic contaminants are degraded by ultrasound and/or light.
Optionally, the power of the ultrasound is 20-100W, and the frequency is 20-100 kHz.
The embodiment of the invention provides a heterojunction nano particle and a preparation method and application thereof. By using a piezoelectric material having a photocatalytic function as a carrier, a noble metal is supported on the carrier, and the carrier and the noble metal form a heterojunction. On one hand, the heterojunction nano-particles have the properties of the piezoelectric material and the noble metal, namely, under the action of ultrasound, the piezoelectric material can convert mechanical vibration into electric energy and generate an electric field in the piezoelectric material, and the electric field effectively promotes the separation of photon-generated carriers and can effectively improve the photocatalytic efficiency of the heterojunction nano-particles; secondly, under the irradiation condition of sunlight, the noble metal can also absorb the near infrared light section in the sunlight, thereby improving the light utilization efficiency of the heterojunction nano-particles. On the other hand, by forming a heterojunction, when incident light is incident on two media having different refractive indices at a critical angle
The resonance of metal free electrons, namely the plasma resonance phenomenon, can be caused when the interface (the carrier and the noble metal in the embodiment of the invention) is formed, and the electrons absorb light energy due to the resonance, so that the reflected light is greatly weakened within a certain angle, the solar energy utilization rate can be effectively improved, and the photocatalytic efficiency can be further improved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be 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 is a schematic flow chart of a method for preparing heterojunction nanoparticles according to an embodiment of the present invention;
FIG. 2 shows AgNbO according to an embodiment of the present invention3Nanoparticles, Au/AgNbO3XRD patterns of heterojunction nanoparticles and Au nanoparticles;
FIG. 3 shows an embodiment of the present invention, which employs Au/AgNbO under illumination, ultrasound, and a combination of illumination and ultrasound3A degradation curve comparison graph of degradation of RhB (rhodamine B (Rhodamine B)) by the heterojunction nano-particles;
FIG. 4 shows AgNbO adopted under illumination, ultrasound, and a combination of illumination and ultrasound according to an embodiment of the present invention3A degradation curve comparison graph of nanoparticles degrading RhB;
FIG. 5 shows an embodiment of the present invention, which employs Au/AgNbO under illumination, ultrasound, and a combination of illumination and ultrasound3A hydrogen production curve comparison diagram of heterojunction nano particles to water decomposition hydrogen production;
FIG. 6 shows AgNbO adopted under illumination, ultrasound, and a combination of illumination and ultrasound according to an embodiment of the present invention3The hydrogen production curve of nano particles to water decomposition hydrogen production is compared with the graph.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "center", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In one aspect, embodiments of the present invention provide a heterojunction nanoparticle, including a support selected from piezoelectric materials having a photocatalytic effect, and a noble metal supported on a surface of the support, wherein the support and the noble metal form a heterojunction.
Wherein, for example, the piezoelectric material can be selected from BiFeO3、Ba0.5Na0.5TiO3、KNbO3And AgNbO3Any one of the above; the noble metal may be any one of Ag, Au and Pt group metals.
For convenience of material selection, the noble metal is selected from any one of Ag, Au and Pd.
The embodiment of the invention provides a heterojunction nano particle, which is characterized in that a piezoelectric material with a photocatalytic effect is used as a carrier, a noble metal is loaded on the carrier, and the carrier and the noble metal form a heterojunction. On one hand, the heterojunction nano-particles have the properties of the piezoelectric material and the noble metal, namely, under the action of ultrasound, the piezoelectric material can convert mechanical vibration into electric energy and generate an electric field in the piezoelectric material, and the electric field effectively promotes the separation of photon-generated carriers and can effectively improve the photocatalytic efficiency of the heterojunction nano-particles; secondly, under the irradiation condition of sunlight, the noble metal can also absorb the near infrared light section in the sunlight, thereby improving the light utilization efficiency of the heterojunction nano-particles. On the other hand, by forming the heterojunction, when incident light is incident on the interface of two media (the carrier and the noble metal in the embodiment of the invention) with different refractive indexes at a critical angle, the resonance of metal free electrons, namely a plasma resonance phenomenon, can be caused, and the electrons absorb light energy due to the resonance, so that the reflected light is greatly weakened within a certain angle, the solar energy utilization rate can be effectively improved, and the photocatalytic efficiency can be further improved.
The loading amount of the noble metal is not particularly limited, and in specific applications, the loading amount of the noble metal can be determined by adjusting the preparation method.
In an optional embodiment of the present invention, in the heterojunction nanoparticle, the mass fraction of the noble metal is w, and the balance is the piezoelectric material; wherein w is more than 0% and less than or equal to 10%.
Optionally, the mass fraction w of the noble metal is between 1% and 10%.
In another aspect, an embodiment of the present invention provides a method for preparing the heterojunction nanoparticles, as described above, with reference to fig. 1, including:
and S1, taking the piezoelectric material with the photocatalysis effect as a carrier, and depositing the noble metal compound on the surface of the carrier by a deposition precipitation method to obtain the precursor material.
Specifically, a piezoelectric material with a photocatalytic function is used as a carrier, and a noble metal compound is deposited on the surface of the carrier by a deposition precipitation method to obtain a precursor material; the method comprises the following steps: dissolving the piezoelectric material with photocatalysis by using deionized water, adjusting the pH value of the aqueous solution to be between 9 and 13 by using ammonia water, adding the aqueous solution of a noble metal compound, and reacting for a preset time under heating to obtain the precursor material.
In the embodiment of the invention, the pH value is adjusted to 9-13, so that the nano noble metal catalyst with uniformly dispersed active components, small granularity and high activity can be obtained, and the overall catalytic activity of the heterojunction nano particles can be improved.
Wherein, optionally, the reaction temperature is between 50 and 110 ℃, and the preset time is 1 to 2 hours.
The noble metal compound may be a water-soluble compound, and thus, the loading rate of the noble metal compound on the piezoelectric material can be increased, and the loading amount of the noble metal on the piezoelectric material can be increased.
Illustratively, when the noble metal is Au, the noble metal compound can be chloroauric acid, which can be decomposed into Au and hydrogen chloride gas by calcination after preparation into a precursor material. When the noble metal is Ag, the noble metal compound may be silver nitrate, which is decomposed into Ag and nitrogen dioxide by calcination.
And S2, calcining the precursor material in an air atmosphere to obtain the heterojunction nano-particle.
Wherein, optionally, the calcining temperature can be 300-500 ℃, and the calcining time can be 1-2 h.
The embodiment of the invention provides a preparation method of heterojunction nano-particles, which is simple and easy to realize industrial production and creates conditions for application of the heterojunction nano-particles.
In another embodiment of the present invention, before the precursor material is obtained by depositing a noble metal compound on the surface of a support by a deposition precipitation method using a piezoelectric material having a photocatalytic effect as the support, the preparation method further includes: the piezoelectric material is prepared by hydrothermal synthesis.
Wherein, the piezoelectric material is AgNbO3For example, the piezoelectric material is prepared by a hydrothermal synthesis method, which comprises:
reacting NH4HF2、Ag2O and Nb2O5According to a molar ratio of 3: 1: 1, adding the mixture into deionized water, and stirring the mixture until the mixture is dissolved to prepare a solution; adding the prepared solution into a reaction kettle, reacting for 32 hours at the temperature of 200 ℃, centrifuging, washing and drying to obtain AgNbO3And (3) nanoparticles.
Wherein the drying temperature can be 70-85 deg.C.
On the other hand, the embodiment of the invention provides an application of the heterojunction nano-particles as the photocatalyst in preparation of hydrogen energy.
Optionally, hydrogen is produced by decomposing water by ultrasound and/or illumination.
In order to improve the efficiency of decomposing water to produce hydrogen, the power of the ultrasonic wave is 20-100W, and the frequency is 20-100 kHz.
In another aspect, an embodiment of the present invention provides an application of the heterojunction nanoparticle as described above as a photocatalyst in organic matter degradation.
Optionally, the organic contaminants are degraded by ultrasound and/or light.
Wherein, in order to improve the degradation rate, the power of the ultrasonic wave is 20-100W, and the frequency is 20-100 kHz.
In order to objectively evaluate the technical effect of the invention, the embodiment of the invention takes the piezoelectric material as AgNbO3The noble metal is Au as an example, and the present invention will be described in detail by the following comparative examples, examples and experimental examples.
Comparative example
Reacting NH4HF2、Ag2O and Nb2O5According to a molar ratio of 3: 1: 1, adding the mixture into 70ml of deionized water, stirring the mixture until the mixture is dissolved, and preparing a solution; adding the prepared solution into a 100ml reaction kettle, reacting for 32 hours at the temperature of 200 ℃, centrifuging, washing and drying at 80 ℃ to obtain AgNbO3And (3) nanoparticles.
Example 1
Step 1, preparing AgNbO3The specific method of the nanoparticles is almost the same as that of the comparative example, and the details thereof are not repeated.
Example 2
Step 1, preparing AgNbO3The specific method of the nanoparticles is almost the same as that of example 1, and the details are not repeated herein.
Example 3
Step 1, preparing AgNbO3The specific method of the nanoparticles is almost the same as that of example 1, and the details are not repeated herein.
Examples of the experiments
1. AgNbO obtained by contrast ratio under the condition that the scanning speed is 10 DEG/min3Nanoparticles, Au/AgNbO obtained in example 13XRD tests were performed on the heterojunction nanoparticles and Au nanoparticles, respectively, and the results are shown in fig. 2.
As can be seen from FIG. 2, except for the original perovskite AgNbO3Besides the peak value, after Au deposition, the Au peak is obviously increased, the matching degree of the two peak values and a standard card is perfect, and other miscellaneous peaks are avoided. X-ray diffraction shows that the synthetic material is pure phase Au/AgNbO3Heterojunction nanoparticles.
2. The Au/AgNbO obtained in example 1 was used under the conditions of light irradiation, ultrasound, and combination of light irradiation and ultrasound, respectively3The heterojunction nano-particles degrade RhB ((rhodamine b)), and blank tests are carried out, and the degradation curve is shown in fig. 3.
In the presence of Au/AgNbO3AgNbO obtained by adopting the comparative example under the same conditions of heterojunction nano-particles, illumination, ultrasound and illumination and ultrasound combined conditions3The nanoparticles were used to degrade RhB and blank experiments were performed, and the degradation curves are shown in fig. 4.
As can be seen from FIG. 3, compared with the simple light irradiation and ultrasound effect, the degradation efficiency can be greatly improved under the condition of combining the light irradiation and the ultrasound, which shows that Au/AgNbO3The heterojunction nano-particles have the synergistic effect of ultrasonic vibration and plasma vibration. As can be seen from FIGS. 3 and 4, Au/AgNbO was used under the same conditions3The degradation efficiency of the compound on RhB is higher than that of AgNbO3The degradation efficiency on RhB is improved, and Au/AgNbO is obtained under the condition of combining illumination and ultrasound3Relative to AgNbO3In other words, the RhB degradation rate is accelerated, and therefore, it can be known that: the Au/AgNbO3The heterojunction nano-particles have the synergistic effect of ultrasonic vibration and plasma vibration under the condition of combining illumination and ultrasound, and the RhB degradation efficiency can be greatly improved.
3. The Au/AgNbO obtained in example 1 was used under the conditions of light irradiation, ultrasound, and combination of light irradiation and ultrasound, respectively3The heterojunction nano-particles decompose water to generate hydrogen, and a blank test is carried out, and the hydrogen generation curve is shown in figure 5.
In the presence of Au/AgNbO3Under the same conditions of the heterojunction nanoparticles, the AgNbO3 nanoparticles obtained in the comparative example are respectively used for decomposing water to produce hydrogen under the conditions of illumination, ultrasound and combination of illumination and ultrasound, and a blank test is carried out, wherein the hydrogen production curve is shown in FIG. 6.
As can be seen from FIG. 5, compared with the simple light irradiation and ultrasonic action, the hydrogen production rate can be greatly increased under the condition of combining the light irradiation and the ultrasonic action, which shows that Au/AgNbO3The heterojunction nano-particles have the synergistic effect of ultrasonic vibration and plasma vibration. As can be seen from FIGS. 5 and 6, Au/AgNbO was used under the same conditions3The hydrogen production speed for decomposing water is larger than that of AgNbO3The hydrogen production speed of water decomposition is accelerated, and the Au/AgNbO is adopted under the condition of combining illumination and ultrasound3Relative to AgNbO3In terms of this, the hydrogen production amount significantly increases, and therefore, it can be known that: the Au/AgNbO3The heterojunction nano-particles have the synergistic effect of ultrasonic vibration and plasma vibration under the condition of combining illumination and ultrasound, and the hydrogen production efficiency can be greatly improved.
As described above, by using a piezoelectric material having a photocatalytic function as a carrier and supporting a noble metal on the carrier, the carrier and the noble metal form a heterojunction. On one hand, the heterojunction nano-particles have the properties of the piezoelectric material and the noble metal, namely, under the action of ultrasound, the piezoelectric material can convert mechanical vibration into electric energy and generate an electric field in the piezoelectric material, and the electric field effectively promotes the separation of photon-generated carriers and can effectively improve the photocatalytic efficiency of the heterojunction nano-particles; secondly, under the irradiation condition of sunlight, the noble metal can also absorb the near infrared light section in the sunlight, thereby improving the light utilization efficiency of the heterojunction nano-particles. On the other hand, by forming the heterojunction, when incident light is incident on the interface of two media (the carrier and the noble metal in the embodiment of the invention) with different refractive indexes at a critical angle, the resonance of metal free electrons, namely a plasma resonance phenomenon, can be caused, and the electrons absorb light energy due to the resonance, so that the reflected light is greatly weakened within a certain angle, the solar energy utilization rate can be effectively improved, and the photocatalytic efficiency can be further improved. Meanwhile, the comparison shows that under the condition of combining illumination and ultrasound, the photocatalysis efficiency can be greatly improved through the synergistic effect of ultrasound and plasma resonance.
The scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of changes or substitutions within the technical scope of the present invention, and the present invention is intended to be covered thereby. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. Heterojunction nanoparticles comprising a support selected from piezoelectric materials having photocatalytic effects, and a noble metal supported on the surface of the support, wherein the support and the noble metal form a heterojunction.
2. The heterojunction nanoparticle of claim 1, wherein the piezoelectric material is selected from BiFeO3、Ba0.5Na0.5TiO3、KNbO3And AgNbO3Any one of the above;
the noble metal is selected from any one of Ag, Au and Pd.
3. Heterojunction nanoparticle according to claim 1 or 2, wherein in the heterojunction nanoparticle the mass fraction of the noble metal is w, the balance being the piezoelectric material; wherein w is more than 0% and less than or equal to 10%.
4. A method of preparing heterojunction nanoparticles as claimed in any of claims 1 to 3, comprising:
taking a piezoelectric material with a photocatalytic effect as a carrier, and depositing a noble metal compound on the surface of the carrier by a deposition precipitation method to obtain a precursor material;
and calcining the precursor material in an air atmosphere to obtain the heterojunction nano-particles.
5. The method for preparing heterojunction nanoparticles according to claim 4, wherein a piezoelectric material with a photocatalytic effect is used as a carrier, and a noble metal compound is deposited on the surface of the carrier by a deposition precipitation method to obtain a precursor material; the method comprises the following steps:
dissolving the piezoelectric material with the photocatalysis effect by using deionized water, adjusting the pH value of the aqueous solution to be between 9 and 13 by using ammonia water, adding the aqueous solution of the noble metal compound, and reacting for a preset time under heating to obtain the precursor material.
6. The method for preparing heterojunction nanoparticles according to claim 5, wherein the reaction temperature is between 50 and 110 ℃ and the predetermined time is 1 to 2 hours.
7. The method for preparing heterojunction nanoparticles as claimed in any of claims 4 to 6, wherein the temperature of the calcination is 300-500 ℃ and the time of the calcination is 1-2 h.
8. The method for preparing heterojunction nanoparticles according to claim 5, wherein before the precursor material is obtained by depositing a noble metal compound on the surface of the support by a deposition precipitation method using a piezoelectric material having a photocatalytic effect as a support, the method further comprises:
the piezoelectric material is prepared by hydrothermal synthesis.
9. Use of the heterojunction nanoparticles of any of claims 1 to 3 as a photocatalyst for the production of hydrogen energy or for the degradation of organic substances.
10. Use according to claim 9, wherein the heterojunction nanoparticles catalytically decompose water by ultrasound and/or light to produce hydrogen;
or, the heterojunction nanoparticles catalytically degrade organic contaminants by ultrasound and/or light;
wherein the power of the ultrasound is 20-100W, and the frequency is 20-100 kHz.
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