CN113509952A - Ytterbium and erbium co-doped Yb-Er/g-C3N4Photocatalyst and synthesis method and application thereof - Google Patents
Ytterbium and erbium co-doped Yb-Er/g-C3N4Photocatalyst and synthesis method and application thereof Download PDFInfo
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- 229910052691 Erbium Inorganic materials 0.000 title claims abstract description 14
- 229910052769 Ytterbium Inorganic materials 0.000 title claims abstract description 14
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 title claims abstract description 13
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000001308 synthesis method Methods 0.000 title abstract description 3
- 239000011941 photocatalyst Substances 0.000 claims abstract description 43
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000003197 catalytic effect Effects 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims abstract description 7
- 229940075624 ytterbium oxide Drugs 0.000 claims abstract description 7
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 19
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 19
- 229940043267 rhodamine b Drugs 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 13
- 230000015556 catabolic process Effects 0.000 claims description 11
- 238000006731 degradation reaction Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 238000005215 recombination Methods 0.000 abstract description 6
- 230000006798 recombination Effects 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000969 carrier Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 14
- 239000007788 liquid Substances 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical group N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 229910052755 nonmetal Inorganic materials 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000000643 oven drying Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- JIHQDMXYYFUGFV-UHFFFAOYSA-N 1,3,5-triazine Chemical group C1=NC=NC=N1 JIHQDMXYYFUGFV-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- -1 ytterbium-erbium ion Chemical class 0.000 description 1
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Abstract
The invention discloses ytterbium and erbium co-doped Yb-Er/g-C3N4Photocatalyst, and a synthesis method and application thereof. The g-C is prepared by taking melamine as a raw material and adopting a high-temperature calcination method3N4(ii) a Yb-Er/g-C is prepared from ytterbium oxide and erbium oxide by microwave-assisted heating method3N4. Ytterbium and erbium codoped Yb-Er/g-C prepared by the invention3N4Photocatalysis inhibits the recombination of photon-generated carriers, and can effectively improve energy conversion efficiency, thereby improving the catalytic efficiency of visible light and near infrared light. The organic pollutants are degraded by using the Yb-Er/g-C under the irradiation of visible light and near infrared light3N4Has important practical application value in environmental purification and clean energy production.
Description
Technical Field
The invention belongs to the technical field of preparation of photocatalytic materials, and particularly relates to preparation of Yb-Er/g-C by a microwave-assisted heating method3N4A method for preparing photocatalyst and application.
Background
With the development of modern society increasingly restricted by energy and environmental problems, the photocatalytic technology is receiving increasingly wide attention. The photocatalytic material can be hydrolyzed by sunlight to produce hydrogen, and can decompose harmful substances, thereby solving the energy and environmental problems in human development. Organic graphite phase carbon nitride (g-C)3N4) And the photocatalyst consists of C and N elements only, and shows great potential of eliminating pollutants by using the non-metal photocatalyst. g-C3N4The spinel material is a stable spinel material, has proper band gap, unique performance and stable photochemical characteristics, is widely applied to the fields of pigments, fireproof materials, photochemical water splitting hydrogen production, anode materials of lithium ion batteries and the like, and is also a high-efficiency photocatalyst for degrading organic pollutants by visible light.
However, g-C prepared by conventional methods3N4Not only has small specific surface area, but also has low quantum efficiency due to rapid recombination of photo-generated electrons and holesThis limits its further applications. Therefore, it is necessary to research modification of semiconductor photocatalysts, and the purpose and effect of the modification include improvement of excited charge separation, suppression of carrier recombination to improve quantum efficiency.
The doping modification method is a common and effective means for improving the electronic structure and surface properties of semiconductor materials, and is mainly divided into non-metal doping and metal doping. g-C3N4A layered structure with voids that facilitates uniform doping of the dopant. Dopants and g-C3N4The original molecular orbit generates orbital hybridization, and then the energy band structure, the electronic structure and the optical property of the molecular orbit are changed. With metal ion pairs g-C3N4After doping, the g-C is influenced by the coordination bond formed between the doped metal ion and the nitrogen atom3N4The electronic structure reduces the band gap energy, improves the absorption of visible light, and inhibits the recombination of photo-generated electron-hole pairs, thereby improving the photocatalytic efficiency.
Disclosure of Invention
The invention aims to provide a method for synthesizing Yb-Er/g-C by a microwave-assisted heating method3N4A preparation method of the photocatalyst.
The technical scheme adopted by the invention is as follows: ytterbium and erbium co-doped Yb-Er/g-C3N4A photocatalyst, the ytterbium and erbium co-doped Yb-Er/g-C3N4Photocatalyst in molar ratio of Yb3+:Er3+:g-C3N4＝(0.1-0.02):(0.01-0.005):1。
Ytterbium and erbium co-doped Yb-Er/g-C3N4The preparation method of the photocatalyst comprises the following steps:
1) calcining melamine in nitrogen atmosphere to obtain g-C3N4；
2) G to C3N4And contains Yb3+Solution and Er-containing3+The solution is evenly mixed under the ultrasonic condition, heated, centrifuged and dried under the microwave condition to obtain Yb-Er/g-C3N4A photocatalyst.
Preferably, in the preparation method, in the step 1), the temperature rise rate is controlled to be 5 ℃/min, the temperature is raised to 500-550 ℃, and the mixture is roasted at 500-550 ℃ for 4-5 h.
Preferably, the above production method, the Yb-containing3+The preparation method of the solution comprises the following steps: dissolving appropriate amount of ytterbium oxide in concentrated hydrochloric acid, heating and stirring, evaporating to dryness, and adding appropriate amount of deionized water to obtain Yb-containing material3+And (3) solution.
Preferably, the preparation method is that the Er is contained3+The preparation method of the solution comprises the following steps: dissolving appropriate amount of erbium oxide in concentrated hydrochloric acid, heating and stirring, evaporating to dryness, and adding appropriate amount of deionized water to obtain Er-containing solution3+And (3) solution.
Preferably, in the above preparation method, step 2), the heating under microwave conditions is: reacting for 3-5min under 700W.
Preferably, in the above preparation method, step 2), the drying is: drying for 12h at the temperature of 60-80 ℃.
The ytterbium and erbium co-doped Yb-Er/g-C provided by the invention3N4The photocatalyst is applied to the catalytic degradation of organic dye under visible light or near infrared light.
Preferably, the organic dye is rhodamine B.
The invention has the beneficial effects that:
g-C3N4the non-metal N-type semiconductor is a non-metal N-type semiconductor, is widely concerned by people due to good chemical stability, thermal stability and photoelectric characteristics, has a forbidden band width of 2.7eV, can absorb visible light with a wavelength of less than 460nm, but has low quantum efficiency, weak visible light absorption response, high charge recombination, small specific surface area and easy recombination of photo-generated electrons and holes, and thus, has low photocatalytic activity. To increase g-C3N4The invention uses ytterbium oxide and erbium oxide to modify graphite-like phase carbon nitride to prepare a photocatalytic material with near infrared light catalytic effect. Yb-Er/g-C prepared by the invention3N4The low photoluminescence intensity can effectively improve the efficiency of energy conversion. The photo-generated carriers will be transported into the semiconductorThe photocatalyst is compounded on the surface, thereby emitting light and heating, and influencing the photocatalytic efficiency. Treated g-C3N4The infrared photocatalysis can be realized under the irradiation of 980nm infrared light.
Drawings
FIG. 1 shows Yb-Er/g-C prepared in different molar ratios3N4XRD pattern of photocatalyst.
FIG. 2 shows g-C prepared in example 13N4(a) And Yb 2% -Er0.5%/g-C3N4(b) SEM image of (d).
FIG. 3 shows Yb 2% -Er0.5%/g-C prepared in example 13N4A graph of rhodamine B catalytic degradation by the photocatalyst under visible light.
FIG. 4 shows Yb-Er/g-C prepared in different molar ratios3N4A comparison graph of the efficiency of the photocatalyst for catalyzing and degrading rhodamine B under visible light.
FIG. 5 shows Yb 2% -Er0.5%/g-C prepared in example 13N4A graph of rhodamine B catalytic degradation by the photocatalyst under near infrared light.
Detailed Description
Example 1 Yb-Er Co-doped Yb-Er/g-C3N4Photocatalytic (mono) pure g-C3N4Preparation of
Melamine was placed in an alumina crucible, heated to 550 ℃ from room temperature at a heating rate of 5 ℃ per minute in a tube furnace (under a constant flow of nitrogen gas), held at 550 ℃ for 4 hours, and then naturally cooled to room temperature. The nitrogen is turned off and the light yellow solid is taken out and ground into powder to obtain pure g-C3N4A photocatalyst.
(II) Yb 2% -Er0.5%/g-C3N4Preparation of
1) 0.4925g of ytterbium oxide is dissolved in 10mL of concentrated hydrochloric acid, heated, stirred and dissolved, evaporated to dryness, and added with deionized water again to obtain Yb3+Yb concentration of 0.00005mol/mL3+And (3) solution.
2) 0.47815g of erbium oxide is dissolved in 10mL of concentrated hydrochloric acid, heated, stirred and dissolved, evaporated to dryness, and added with deionized water again to obtain Er3+Er with the concentration of 0.00005mol/mL3+And (3) solution.
3) At 0.92g (0.01mol) of pure g-C3N4To the photocatalyst, 4ml of Yb was added3+Solution, 1ml Er3+Mixing the solution under ultrasonic condition, stirring, transferring into crucible, placing into microwave oven, reacting at 700W for 5min, centrifuging, oven drying the precipitate at 80 deg.C for 12 hr to obtain Yb3+:Er3+:g-C3N40.02:0.005:1 Yb-Er/g-C3N4Photocatalysis marked as Yb 2% -Er0.5%/g-C3N4A photocatalyst.
(III) Yb 2% -Er 1%/g-C3N4Preparation of
1) 0.4925g of ytterbium oxide is dissolved in 10mL of concentrated hydrochloric acid, heated, stirred and dissolved, evaporated to dryness, and added with deionized water again to obtain Yb3+Yb concentration of 0.00005mol/mL3+And (3) solution.
2) 0.47815g of erbium oxide is dissolved in 10mL of concentrated hydrochloric acid, heated, stirred and dissolved, evaporated to dryness, and added with deionized water again to obtain Er3+Er with the concentration of 0.00005mol/mL3+And (3) solution.
3) At 0.92g (0.01mol) of pure g-C3N4To the photocatalyst, 4ml of Yb was added3+Solution, 2ml Er3+Mixing the solution under ultrasonic condition, stirring, transferring into crucible, placing into microwave oven, reacting at 700W for 5min, centrifuging, oven drying the precipitate at 80 deg.C for 12 hr to obtain Yb3+:Er3+:g-C3N40.02:0.01:1 Yb-Er/g-C3N4Photocatalysis marked as Yb 2% -Er 1%/g-C3N4A photocatalyst.
(IV) Yb 10% -Er 1%/g-C3N4Preparation of
1) 0.4925g of ytterbium oxide is dissolved in 10mL of concentrated hydrochloric acid, heated, stirred and dissolved, evaporated to dryness, and added with deionized water again to obtain Yb3+Yb concentration of 0.00005mol/mL3+And (3) solution.
2) 0.47815g of erbium oxide was dissolved in 10mL of concentrated hydrochloric acid and heatedStirring to dissolve, evaporating to dryness, and adding deionized water again to obtain Er3+Er with the concentration of 0.00005mol/mL3+And (3) solution.
3) At 0.92g (0.01mol) of pure g-C3N420ml of Yb was added to the photocatalyst3+Solution, 2ml Er3+Mixing the solution under ultrasonic condition, stirring, transferring into crucible, placing into microwave oven, reacting at 700W for 5min, centrifuging, oven drying the precipitate at 80 deg.C for 12 hr to obtain Yb3+:Er3+:g-C3N40.1:0.01:1 Yb-Er/g-C3N4Photocatalysis marked as Yb 10% -Er 1%/g-C3N4A photocatalyst.
(V) detection
FIG. 1 shows Yb-Er/g-C prepared in different molar ratios3N4XRD pattern of photocatalyst. Wherein (a) is unmodified g-C3N4(b) Yb 2% -Er0.5%/g-C3N4(C) Yb 2% -Er 1%/g-C3N4，(d)Yb10％-Er1％/g-C3N4. As can be seen from FIG. 1, the samples all exhibited g-C3N4Two characteristic peaks (13 ° and 27.3 °). One is 2 θ — 13 °, which is mainly due to the characteristic diffraction of the in-plane 3 s-triazine unit structure of the material, with a miller index of (100). The other is 27.3 ° which is mainly due to a diffraction peak formed by the interlayer periodic packing, and the miller index is (002). Prepared Yb3+、Er3+Codoped g-C3N4Catalyst and unmodified g-C3N4The positions of diffraction peaks are consistent, which shows that g-C is doped3N4The crystal structure of (2) is not changed, and is a layered carbon nitride structure with graphite layers stacked one on top of the other. And the XRD spectrum does not find characteristic diffraction peaks of ytterbium, erbium simple substance and oxide thereof, which indicates that ytterbium-erbium ion co-doped graphite-phase carbon nitride Yb-Er/g-C is successfully prepared3N4。
FIG. 2 is g-C of preparation3N4(a) And Yb 2% -Er0.5%/g-C3N4(b) SEM image of (d). As can be seen from FIG. 2, the samples all exhibited irregularitiesA block structure of (1).
Example 2 Yb-Er codoped Yb-Er/g-C3N4Application of photocatalyst in catalytic degradation of organic dye under visible light
The method comprises the following steps: with a xenon lamp (300W, 20A) as a light source, 0.05g of Yb-Er/g-C co-doped with Yb-Er was weighed3N4The photocatalyst is placed in a 100ml beaker, and 50ml of rhodamine B solution to be degraded with the concentration of 10mg/L is added. Considering that a sample has certain adsorbability, the rhodamine B solution mixed with the photocatalytic material is stirred for 30min in a dark place, and 2ml of the rhodamine B solution is sampled before and after the light is shielded, so that an adsorption-desorption balance state is formed between the photocatalyst and the rhodamine B, and errors caused by adsorption are avoided. And finally, aligning the lamp cap of the xenon lamp to the photocatalytic system to be tested. Sampling 2ml at regular intervals after illumination, placing the sampled sample liquid in a centrifuge for 5min at 8000rpm, placing supernatant liquid in a cuvette, testing the concentration of residual rhodamine B in the sample liquid by uv-3600, and evaluating the catalytic performance of the catalyst sample by the absorbance of the sample liquid.
FIG. 3 shows Yb 2% -Er0.5%/g-C prepared in example 13N4A graph of rhodamine B catalytic degradation by the photocatalyst under visible light. As can be seen from fig. 3, under irradiation of visible light, the absorption intensity of the characteristic absorption peak of the RhB solution at 550nm gradually decreases with time, which indicates that the molecular structure of RhB is destroyed, resulting in a decrease in its absorbance. It can be seen that Yb 2% -Er0.5%/g-C3N4The photocatalyst has good visible light catalytic performance.
FIG. 4 shows Yb-Er/g-C prepared in different molar ratios3N4A comparison graph of the efficiency of the photocatalyst for catalyzing and degrading rhodamine B under visible light. Wherein A is unmodified g-C3N4B is Yb 2% -Er0.5%/g-C3N4C is Yb 2% -Er 1%/g-C3N4D is Yb 10% -Er 1%/g-C3N4. As can be seen from FIG. 4, ytterbium and erbium co-doped Yb-Er/g-C of the present invention3N4The degradation efficiency of the photocatalyst is obviously higher than that of unmodified g-C3N4Wherein the sample Yb 2% -Er 1%/g-C3N4Most obviously, the degradation efficiency of rhodamine B is improved from 38.6 percent to 93.4 percent after 52min illumination. Under the same illumination time, Yb 2% -Er0.5%/g-C3N4The degradation efficiency is 88.2 percent, and Yb 10-Er 1%/g-C3N4The content was 92.7%.
Example 3 Yb-Er Co-doped Yb-Er/g-C3N4Application of photocatalyst in catalytic degradation of organic dye under near infrared light
Yb 2% -Er0.5%/g-C prepared as in example 13N4And (5) carrying out a performance test on the photocatalytic material by the photocatalyst.
The method comprises the following steps: using 980nm laser as light source, weigh 0.1g of Yb 2% -Er0.5%/g-C3N4The photocatalyst is placed in a condensation cup, and 30ml of rhodamine B solution to be degraded with the concentration of 10mg/L is added into the condensation cup. Considering that a sample has certain adsorbability, the rhodamine B solution mixed with the photocatalytic material is stirred for 1 hour in a dark place, and 2ml of the rhodamine B solution is sampled before and after the light is shielded, so that an adsorption-desorption balance state is formed between the photocatalyst and the rhodamine B, and errors caused by adsorption are avoided. Finally, the light source is directed at the photocatalytic system to be tested. Sampling 2ml every 2h after illumination, placing the sampled sample liquid in a centrifuge for 5min at 8000rpm, placing supernatant liquid in a cuvette, testing the concentration of residual rhodamine B in the sample liquid by uv-3600, and evaluating the catalytic performance of the catalyst sample by the absorbance of the sample liquid.
FIG. 5 shows Yb 2% -Er0.5%/g-C prepared in example 13N4A graph of rhodamine B catalytic degradation by the photocatalyst under near infrared light. As shown in fig. 5, under 980nm light irradiation, the absorption intensity of the characteristic absorption peak of the RhB solution at 550nm gradually decreases with time, which indicates that the molecular structure of RhB is destroyed, resulting in a decrease in its absorbance. It can be seen that Yb 2% -Er0.5%/g-C3N4The photocatalyst has infrared light photocatalysis performance to a certain extent.
Claims (9)
1. Ytterbium and erbium co-doped Yb-Er/g-C3N4A photocatalyst, characterized in that ytterbium and erbium are co-presentDoping Yb-Er/g-C3N4Photocatalyst in molar ratio of Yb3+:Er3+:g-C3N4＝(0.1-0.02):(0.01-0.005):1。
2. Ytterbium and erbium co-doped Yb-Er/g-C3N4The preparation method of the photocatalyst is characterized by comprising the following steps:
1) calcining melamine in nitrogen atmosphere to obtain g-C3N4；
2) G to C3N4And contains Yb3+Solution and Er-containing3+The solution is evenly mixed under the ultrasonic condition, heated, centrifuged and dried under the microwave condition to obtain Yb-Er/g-C3N4A photocatalyst.
3. The preparation method according to claim 2, wherein in the step 1), the temperature rise rate is controlled to be 5 ℃/min, the temperature is raised to 500-550 ℃, and the roasting is carried out for 4-5h at 500-550 ℃.
4. The method according to claim 2, wherein the Yb is contained3+The preparation method of the solution comprises the following steps: dissolving appropriate amount of ytterbium oxide in concentrated hydrochloric acid, heating and stirring, evaporating to dryness, and adding appropriate amount of deionized water to obtain Yb-containing material3+And (3) solution.
5. The method of claim 2, wherein said Er is present in said solution3+The preparation method of the solution comprises the following steps: dissolving appropriate amount of erbium oxide in concentrated hydrochloric acid, heating and stirring, evaporating to dryness, and adding appropriate amount of deionized water to obtain Er-containing solution3+And (3) solution.
6. The method according to claim 2, wherein in step 2), the microwave heating is: reacting for 3-5min under 700W.
7. The method according to claim 2, wherein in step 2), the drying is: drying for 12h at the temperature of 60-80 ℃.
8. The method of claim 1 wherein Yb and Er are codoped with Yb-Er/g-C3N4The photocatalyst is applied to the catalytic degradation of organic dye under visible light or near infrared light.
9. Use according to claim 8, wherein the organic dye is rhodamine B.
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