CN112960672B - SiC particles with visible light response and preparation method thereof - Google Patents
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- 239000002245 particle Substances 0.000 title claims abstract description 108
- 230000004298 light response Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 230000001678 irradiating effect Effects 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 16
- 238000005530 etching Methods 0.000 claims description 6
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- 230000004044 response Effects 0.000 claims description 4
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- 229910010271 silicon carbide Inorganic materials 0.000 description 113
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 106
- 230000031700 light absorption Effects 0.000 description 11
- 239000004065 semiconductor Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
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- 239000001301 oxygen Substances 0.000 description 1
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- 239000002957 persistent organic pollutant Substances 0.000 description 1
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- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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Abstract
The invention discloses a SiC particle with visible light response and a preparation method thereof, wherein the preparation method comprises the following steps: (1) preheating raw material SiC particles; (2) removing an oxide layer on the surface of the SiC particles after the preheating treatment and other organic impurities attached to the surface of the SiC particles; (3) tabletting the SiC particles obtained in the step (2); (4) irradiating the SiC particles subjected to tabletting treatment in the step (3) by using laser to obtain brown SiC particles; (5) and (3) after uniformly mixing the brown SiC particles obtained in the step (4) again, repeating the steps (3) and (4) until the brown color of the whole powder sample is uniform. The method can not only improve the visible light response performance of SiC, but also ensure the complete crystal structure of the SiC bulk phase, avoid the distortion of SiC crystal lattices and inhibit the generation of defects to the greatest extent; the prepared SiC particles have good absorption to visible light and show good electric transport property under the action of light.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to SiC particles with visible light response and a preparation method thereof.
Background
Silicon carbide (SiC) is one of typical representatives of third-generation semiconductors, has excellent properties such as chemical stability, high thermal conductivity, high electron mobility, high mechanical strength, and the like, and has been increasingly used in high-power electronic devices, light-emitting diodes, radio-frequency devices, and the like in recent years. In addition, because of high hardness, low cost and environmental friendliness, SiC powder is one of the most widely used abrasives in industry. As an excellent semiconductor material, the material can effectively absorb ultraviolet light, and has wide application in photoreaction systems, such as photoelectrocatalysis electrode materials, organic pollutant photocatalytic degradation, hydrogen production by photocatalytic water decomposition and the like. However, the wide forbidden band of SiC makes it unable to absorb visible light efficiently (about 45% of the total amount of sunlight), which greatly limits its application conditions. The development of the SiC semiconductor material with visible light response is a key technical problem for expanding the application condition of the SiC semiconductor material.
The currently common method for preparing SiC semiconductor materials with visible light response is element doping and semiconductor compounding. Elemental doping is considered to be the most direct and effective method for adjusting the light absorption properties of SiC. In the method, the energy band structure of SiC is directly adjusted by element doping, and impurity energy levels are introduced into the energy band, so that the forbidden bandwidth is reduced, and the SiC is induced to have response absorption to visible light of different wave bands. For example, Hou et al (Nanoscale 7(2015)8955) dopes SiC by using B element, introduces an intermediate energy level in the SiC energy band, and widens the photoresponse range to 400-700 nm. Guo et al (Acta phys. -chim. sin.30(2014)135) also utilize B co-doping SiC to significantly enhance its intensity in the light response range of the visible region. In addition, Al element and N element are also used for doping SiC, and the methods can not only adjust the energy band structure of SiC and induce the response to visible light, but also adjust the N-type or p-type conversion of SiC. However, the distribution of elements introduced by the method in the SiC bulk phase or surface is not controllable, and the SiC lattice structure is distorted, so that SiC defects are increased, and the physical and chemical properties of the SiC are seriously affected.
The SiC is compounded by the semiconductors, and the semiconductors selected in the method generally have good visible light absorption performance. Fang et al (J.Mater.chem.A., 3(2015)4652) utilize AgPO 4 The compound has good absorption performance to visible light of 400-700nm by being compounded with SiC. Wang et al (chem. Eng.J.281(2015)102) utilize BiVO 4 The SiC is subjected to composite modification, so that the light absorption performance of the composite in the visible light region of 400-700nm is improved. Peng et al (j.mater.chem.a,2(2014)6296) can also improve the visible light absorption performance of the composite by performing composite modification treatment on SiC with CdS. In addition, some metals with plasmon resonance effect can also improve the visible light absorption performance of SiC, such as Wang et al (appl.surf.sci.456(2018)871) which modifies SiC with nano Au particles. SiC obtained by the metal loading methods has good absorption performance in the visible light wave band of 400-700 nm. However, although this method can ensure the integrity of the SiC crystal structure, it depends heavily on the light absorption properties of the compound semiconductor, and the distribution and state of the compound semiconductor on the SiC surface affect the light absorption properties of the whole system, which is not favorable for the practical application of the SiC compound.
Disclosure of Invention
In order to solve the problems of lattice damage caused by introducing element impurities and generation of a large number of defects on a bulk phase or a surface in the process of preparing a SiC material with visible light response, the invention provides SiC particles with visible light response and a preparation method thereof, wherein the preparation method utilizes a rapid laser irradiation technology to rapidly and cleanly prepare brown SiC particles; the prepared SiC particles have good absorption to visible light and show good electric transport property under the action of light.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: in one aspect, the invention provides a method for preparing SiC particles with visible light response, comprising the steps of:
(1) preheating raw material SiC particles;
(2) removing the oxide layer on the surface of the SiC particles subjected to the preheating treatment in the step (1) and other organic impurities attached to the surface of the SiC particles;
(3) tabletting the SiC particles obtained in the step (2);
(4) irradiating the SiC particles subjected to tabletting treatment in the step (3) by using laser to obtain brown SiC particles;
(5) and (3) after uniformly mixing the brown SiC particles obtained in the step (4) again, repeating the steps (3) and (4) until the brown color of the whole powder sample is uniform.
Further, the crystal form of the raw material SiC particles includes a cubic crystal form and/or a hexagonal crystal form.
Further, the particle size of the raw material SiC particles is 5nm-10000 nm. The particle size of the raw material SiC particles is not within this range and the preparation of SiC particles having visible light response cannot be achieved with the scheme protected by the present application.
Further, the temperature of the preheating treatment in the step (1) is 700-.
Further, the preheating treatment in the step (1) may be performed in a muffle furnace; in order to ensure the cleanliness of the sample, the sample can be treated under the protection of inert gas containing oxygen in a tube furnace.
Further, the step (2) is specifically as follows: and soaking and etching the SiC particles subjected to the preheating treatment by using hydrofluoric acid.
Further, the surface flatness of the sample after the tabletting treatment in step (3) was ± 0.1 mm. If the flatness is not enough to meet the requirement, the scattering of the laser in the step (4) will affect the irradiation effect.
Further, in the step (4), a light-transmitting cover plate is arranged between the SiC sample and the laser irradiation source, so that the powder is prevented from flying around under the irradiation of the high-energy laser.
Further, the wavelength of the laser light source in the step (4) is 300nm-1700 nm; the power of the laser light source is 1W-1000W.
Further, the laser in the step (4) is a pulse laser;
preferably, the width of the laser pulse is 1 picosecond to 1000 nanoseconds, and the frequency of the laser pulse is 10 to 10000 hertz.
Further, the time of the laser irradiation in the step (4) is 5 to 15 seconds.
In another aspect, the invention provides a visible light-responsive SiC particle prepared by any one of the above methods for preparing a visible light-responsive SiC particle.
The invention has the beneficial effects that:
(1) the laser irradiation technology adopted by the invention has the advantages of clean preparation process, no pollution, extremely short reaction time of only 5-15 seconds and higher preparation efficiency.
(2) Due to the short reaction time required, the generation of surface defects is suppressed to the maximum extent.
(3) The element does not need to be introduced into the bulk phase for doping, so that the complete crystal structure of the bulk phase is ensured, and the lattice distortion is avoided.
(4) The prepared SiC particles not only have good visible light response performance (the absorption intensity of visible light is improved by 200 percent), but also show good electric transport property, and the powder has uniform color.
Drawings
FIG. 1 is a comparative optical photograph of a sample of brown uniform SiC powder after laser irradiation in example 1 of the present invention and the starting material.
FIG. 2 is a graph showing the comparison of the light absorption properties of a brown uniform SiC powder sample and a starting material after laser irradiation in example 1 of the present invention, i.e., the solid ultraviolet-visible light diffuse reflection (Uv-Vis) test result; wherein (a) is a result graph of the visible light absorption intensity of the sample, and (b) is a result graph of the sample forbidden band width of the sample after mathematical change fitting.
FIG. 3 is a graph showing the comparison of the electric transport properties of a brown-colored uniform SiC powder sample and a starting material after laser irradiation in example 1 of the present invention, i.e., the results of a photo-current spectroscopy and an AC impedance spectroscopy test; wherein (a) is a graph of photocurrent versus time; (b) is an alternating current impedance diagram.
Detailed Description
In order to more clearly explain the objects, technical solutions and advantages of the present invention, the present invention is further described below with reference to the accompanying drawings and examples. The specific embodiments described herein are merely illustrative and explanatory of the invention and do not delimit the scope of application of the invention.
Example 1
A preparation method of SiC particles with visible light response comprises the following steps:
(1) preheating hexagonal crystal form 6H-SiC particles (the particle size is 5 mu m) in a muffle furnace at 700 ℃ for 2H;
(2) soaking and etching the SiC particles subjected to the preheating treatment in the step (1) by hydrofluoric acid (HF) to clean the surfaces of the SiC particles, and removing an oxide layer on the surfaces of the SiC particles and other organic impurities attached to the surfaces of the SiC particles;
(3) tabletting the SiC particles obtained in the step (2) on a quartz glass substrate, and ensuring the surface flatness of the tabletted sample to be +/-0.1 mm;
(4) irradiating the SiC particles subjected to tabletting treatment in the step (3) for 8 seconds by using laser (tabletting glass is arranged between the SiC particles and a laser irradiation source), so as to obtain brown SiC particles, wherein the parameters of the laser are as follows: wavelength 1064 nm; the power is 1W; the frequency is 1000 Hz; pulse width 8 ns;
(5) and (4) after uniformly mixing the brown SiC particles obtained in the step (4), repeating the steps (3) and (4) for 6 times to obtain brown uniform SiC particles.
The schematic diagram of the comparison of the optical photographs of the brown uniform SiC particles and the starting hexagonal 6H-SiC particles is shown in FIG. 1.
A comparison graph of light absorption performance of the brown uniform SiC particles and the hexagonal crystal form 6H-SiC particles serving as the raw material is shown in figure 2, namely a solid ultraviolet-visible light diffuse reflection (Uv-Vis) test result is shown in figure 2. As can be seen from the figure, the light absorption intensity of the irradiated SiC sample in the visible light region is significantly enhanced compared to the original SiC sample.
The comparison graph of the electric transport properties of the brown uniform SiC particles and the hexagonal crystal form 6H-SiC particles as the raw material is shown in FIG. 3, namely the test results of a photo-current spectrum and an alternating-current impedance spectrum are shown in FIG. 3. As can be seen from the figure, compared with the original SiC sample, the irradiated SiC sample has the advantages of increased photocurrent density and reduced alternating current impedance value, which shows that the irradiated SiC sample shows good electrical transport properties.
Example 2
A preparation method of SiC particles with visible light response comprises the following steps:
(1) preheating hexagonal crystal form 6H-SiC particles (the particle size is 5 mu m) in a muffle furnace at 700 ℃ for 2H;
(2) soaking and etching the SiC particles subjected to the preheating treatment in the step (1) by hydrofluoric acid (HF) to clean the surfaces of the SiC particles, and removing an oxide layer on the surfaces of the SiC particles and other organic impurities attached to the surfaces of the SiC particles;
(3) tabletting the SiC particles obtained in the step (2) on a quartz glass substrate, and ensuring the surface flatness of the tabletted sample to be +/-0.1 mm;
(4) irradiating the SiC particles subjected to tabletting treatment in the step (3) for 8 seconds by using laser (tabletting glass is arranged between the SiC particles and a laser irradiation source), so as to obtain brown SiC particles, wherein the parameters of the laser are as follows: the wavelength is 532 nm; the power is 1W; the frequency is 1000 Hz; pulse width 8 ns;
(5) and (4) after uniformly mixing the brown SiC particles obtained in the step (4), repeating the steps (3) and (4) for 6 times to obtain brown uniform SiC particles.
Example 3
A preparation method of SiC particles with visible light response comprises the following steps:
(1) preheating hexagonal crystal form 6H-SiC particles (the particle size is 5 mu m) in a muffle furnace at 700 ℃ for 2H;
(2) soaking and etching the SiC particles subjected to the preheating treatment in the step (1) by hydrofluoric acid (HF) to clean the surfaces of the SiC particles, and removing an oxide layer on the surfaces of the SiC particles and other organic impurities attached to the surfaces of the SiC particles;
(3) tabletting the SiC particles obtained in the step (2) on a quartz glass substrate, and ensuring the surface flatness of the tabletted sample to be +/-0.1 mm;
(4) irradiating the SiC particles subjected to tabletting treatment in the step (3) for 8 seconds by using laser (tabletting glass is arranged between the SiC particles and a laser irradiation source), so as to obtain brown SiC particles, wherein the parameters of the laser are as follows: wavelength 1064 nm; the power is 3W; the frequency is 1000 Hz; pulse width 8 ns;
(5) and (4) after uniformly mixing the brown SiC particles obtained in the step (4), repeating the steps (3) and (4) for 6 times to obtain brown uniform SiC particles.
Example 4
A preparation method of SiC particles with visible light response comprises the following steps:
(1) preheating cubic crystal 3C-SiC particles (the particle size is 5 mu m) in a muffle furnace at 700 ℃ for 2 h;
(2) soaking and etching the SiC particles subjected to the preheating treatment in the step (1) by hydrofluoric acid (HF) to clean the surfaces of the SiC particles, and removing an oxide layer on the surfaces of the SiC particles and other organic impurities attached to the surfaces of the SiC particles;
(3) tabletting the SiC particles obtained in the step (2) on a quartz glass substrate, and ensuring the surface flatness of the tabletted sample to be +/-0.1 mm;
(4) irradiating the SiC particles subjected to tabletting treatment in the step (3) for 8 seconds by using laser (tabletting glass is arranged between the SiC particles and a laser irradiation source), so as to obtain brown SiC particles, wherein the parameters of the laser are as follows: wavelength 1064 nm; the power is 1W; the frequency is 1000 Hz; pulse width 8 ns;
(5) and (4) after uniformly mixing the brown SiC particles obtained in the step (4), repeating the steps (3) and (4) for 6 times to obtain brown uniform SiC particles.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (5)
1. A preparation method of SiC particles with visible light response is characterized by comprising the following steps:
(1) preheating raw material SiC particles, wherein the crystal form of the raw material SiC particles comprises a cubic crystal form and/or a hexagonal crystal form, the particle size of the raw material SiC particles is 5nm-10000nm, the preheating temperature is 700-1000 ℃, and the preheating time is 2-3 h;
(2) removing the oxide layer on the surface of the SiC particles subjected to the preheating treatment in the step (1) and other organic impurities attached to the surface of the SiC particles;
(3) tabletting the SiC particles obtained in the step (2);
(4) irradiating the SiC particles subjected to tabletting treatment in the step (3) by using laser to obtain brown SiC particles, wherein the wavelength of a laser light source is 300-1700 nm, the power of the laser light source is 1-1000W, and the laser irradiation time is 5-15 seconds;
(5) and (3) after uniformly mixing the brown SiC particles obtained in the step (4) again, repeating the steps (3) and (4) until the brown color of the whole powder sample is uniform.
2. The method for preparing SiC particles having a visible light response according to claim 1, wherein the step (2) is specifically: and soaking and etching the SiC particles subjected to the preheating treatment by using hydrofluoric acid.
3. The method for producing SiC particles having a visible-light response according to claim 1, wherein the surface flatness of the pressed sample in step (3) is ± 0.1 mm.
4. The method for producing SiC particles having a visible-light response according to claim 1, wherein the laser light in step (4) is a pulsed laser light.
5. The method for preparing SiC particles having a visible light response according to claim 4, wherein the width of the laser pulse is 1 picosecond to 1000 nanoseconds and the frequency of the laser pulse is 10 to 10000 Hz.
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