CN106540731A - Plasma and the enhanced multiband responsive photocatalyst preparation method of upper conversion - Google Patents
Plasma and the enhanced multiband responsive photocatalyst preparation method of upper conversion Download PDFInfo
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- CN106540731A CN106540731A CN201610862358.4A CN201610862358A CN106540731A CN 106540731 A CN106540731 A CN 106540731A CN 201610862358 A CN201610862358 A CN 201610862358A CN 106540731 A CN106540731 A CN 106540731A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- 235000006040 Prunus persica var persica Nutrition 0.000 claims abstract description 4
- 239000004202 carbamide Substances 0.000 claims abstract description 4
- 238000005119 centrifugation Methods 0.000 claims abstract description 4
- 238000001556 precipitation Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- 238000000197 pyrolysis Methods 0.000 claims abstract description 3
- 240000006413 Prunus persica var. persica Species 0.000 claims abstract 2
- 239000010931 gold Substances 0.000 claims description 43
- 229910052737 gold Inorganic materials 0.000 claims description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004549 pulsed laser deposition Methods 0.000 claims description 3
- 241000446313 Lamella Species 0.000 claims description 2
- 239000004005 microsphere Substances 0.000 claims description 2
- 241000165940 Houjia Species 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000010865 sewage Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000931526 Acer campestre Species 0.000 description 1
- 244000144730 Amygdalus persica Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 240000005809 Prunus persica Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000003947 neutron activation analysis Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/349—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of flames, plasmas or lasers
Abstract
Plasma and the enhanced multiband responsive photocatalyst preparation method of upper conversion, are related to a kind of photocatalyst preparation method, and methods described prepares the pure g C in surface using normal pressure, the method without additional auxiliary and atmosphere regulation and control pyrolysis carbamide3N4Material；Y (NO) is weighed respectively3, Yb (NO)3, Tm (NO)3With Er (NO)3With prepared g C3N4It is dissolved in the deionized water of 60mL, is subsequently adding NaF；After fully dissolving, transfer the solution into 125 mL with teflon-lined reactor, hydrothermal method obtains NYF/g C3N4Composite；The Au NPs dispersion liquids of preparation are added to into NYF/g C3N4In, mix after shaking up, at room temperature quiescent culture；By peach precipitation by centrifugation, and cleaned with ethanol and deionized water successively, drying obtains Au NPs/NYF/g C3N4Photocatalyst.The present invention prepares photocatalyst the Nomenclature Composition and Structure of Complexes clearly, is a kind of valuable catalysis material for processing sewage.
Description
Technical field
The present invention relates to a kind of photocatalyst preparation method, more particularly to a kind of plasma and upper conversion are enhanced more
Wave band responsive photocatalyst preparation method.
Background technology
The TiO of high praise is enjoyed the advantages of cheap, stable chemical nature2Photocatalyst, as itself is larger
Energy gap（～3.0-3.2 eV）, can only absorb the ultraviolet light for only accounting for solar spectrum 5%, and account for respectively 48% and 44% can
See that light cannot be applied near infrared light wave band.
Non-metal kind graphite-structure semiconducting nitride carbon（g-C3N4）Energy gap is less（～2.7 eV）, being capable of response portion
Divide visible ray.Wherein, nitrogen-atoms and carbon atom sp2The Pi-conjugated systems formed by hydridization have special characteristic electron, in addition
Simple preparation technology and stable physics and chemical property so that g-C3N4Become the semiconductor light of researchers' extensive concern
Catalyst.However, g-C3N4All the time it is faced with photocatalysis efficiency low, photo-generate electron-hole is to recombination probability height and responding to visible light
The bottleneck problem such as wave-length coverage is little.How to reduce the recombination probability of photo-generated carrier and strengthen photocatalytic activity, how further
Widen g-C3N4Photocatalysis response range to the bigger visible ray of wavelength and near-infrared region, become already photocatalysis research neck
Domain major issue urgently to be resolved hurrily.
Under visible light illumination, gold nano grain（Au NPs）Generation " thermoelectricity is excited due to surface plasma body resonant vibration
Son "." thermoelectron " can be transferred to g-C by Au NPs surfaces3N4Conduction band so that participate in light-catalyzed reaction, realize g-C3N4It is right
Larger visible light wavelengths ground is utilized.Under ultraviolet light and partially visible light irradiation, Au NPs can be used as the receptor of light induced electron.
g-C3N4Electronics produced by being excited is delivered to Au NPs by conduction band, can effectively suppress the compound of photo-generated carrier, extend
The life-span of electron-hole pair.Therefore, with g-C3N4Compare, Au NPs/ g-C3N4It is visible light-responded that composite can widen which
Scope, improves light-catalyzed reaction efficiency.
In addition, it is in order to more efficiently utilize sunlight, still indispensable for the capture of near infrared light.Group of the lanthanides
Element（Yb3+, Er3+, Tm3+）Doping NaYF4Up-conversion luminescent material（NYF）Multiple energy photons can be absorbed（It is near red
Outward）And launch high-energy photons（It is ultraviolet or visible）.NYF and Au NPs/g-C3N4Combine, under the irradiation of near infrared light, send out
The Uv and visible light of injection is again by g-C3N4Light-catalyzed reaction is absorbed and is participated in Au NPs, it is achieved thereby that near
The indirect utilization of infrared light.But so far, for the Au NPs/NYF/g-C of multiband response3N4Composite photo-catalyst
Prepare and its light-catalysed application of ultraviolet, visible and near-infrared is not seen in report.
The content of the invention
It is an object of the invention to provide a kind of plasma and the enhanced multiband responsive photocatalyst system of upper conversion
Preparation Method, the method is with g-C3N4, golden nanometer particle and rare earth up-conversion it is anti-under hydrothermal conditions according to certain mol proportion
Should, and obtain target photocatalyst.The photocatalyst the Nomenclature Composition and Structure of Complexes of preparation is clear and definite, in ultraviolet, visible and near infrared light
Under, sewage disposal can be carried out.
The purpose of the present invention is achieved through the following technical solutions：
Plasma and the enhanced multiband responsive photocatalyst preparation method of upper conversion, methods described include procedure below：
The pure g-C in surface is prepared using normal pressure, the method without additional auxiliary and atmosphere regulation and control pyrolysis carbamide3N4Material；Respectively
Weigh Y (NO)3, Yb (NO)3, Tm (NO)3With Er (NO)3With prepared g-C3N4It is dissolved in the deionized water of 60mL, then
Add NaF；After fully dissolving, transfer the solution into 125 mL with teflon-lined reactor, hydro-thermal side
Method obtains NYF/g-C3N4Composite；Using KrF pulse lasers（Wavelength is 248 nm, and repetition rate is 20 Hz）For bombarding
Gold target prepares Au NPs；The Au NPs dispersion liquids of preparation are added to into NYF/g-C finally3N4In, after mixing shakes up, at room temperature
Quiescent culture；By peach precipitation by centrifugation, and cleaned with ethanol and deionized water successively, drying obtains Au
NPs/NYF/g-C3N4Photocatalyst.
Described plasma and the enhanced multiband responsive photocatalyst preparation method of upper conversion, the KrF pulses
Optical maser wavelength is 248 nm, and repetition rate is 20 Hz.
Described plasma and the enhanced multiband responsive photocatalyst preparation method of upper conversion, the g-C3N4Material
Material is with the g-C of two-dimensional layered structure3N4Based on support, up-conversion luminescent material NaYF4：Yb3+, Er3+, Tm3+Microsphere and
Au NPs of the surface without part obtained using pulsed laser deposition method in liquid is uniformly adhered to g-C3N4On lamella.
Advantages of the present invention with effect is：
（1）The stable existences in the solution of Au NPs obtained in pulsed laser deposition method are adopted in a liquid, are difficult to reunite.And surface
Exist without organic ligand, be conducive to Au NPs and g-C3N4Between high efficiency charge transfer, namely under ultraviolet light electronics from
g-C3N4Suppress the compound of photo-generated carrier to Au NPs, it is seen that promote " thermoelectron " under light irradiation from Au NPs to g-C3N4
Injection and promote visible light catalytic to react.
（2）g-C3N4, Au NPs's and NYF is combined prepared photocatalyst（Au NPs/NYF/g-C3N4）, with etc.
Ion resonance body and up-conversion luminescence such as strengthen at the characteristic, and while respond ultraviolet, visible and near infrared light, and have more excellent
Photocatalysis performance.
（3）The present invention adopts common industrial chemicals and simple synthesis technique, and process is simple, it is easy to implement, in reaction
Required solvent is deionized water, meets the requirement of " Green Chemistry ".
The present invention a kind of new Technology Ways to be provided in field of semiconductor photocatalyst using full solar spectral, for solution
Certainly increasingly serious problem of environmental pollution is significant.
Description of the drawings
Fig. 1 is Au NPs/NYF/g-C3N4The TEM figures of composite photo-catalyst.
Specific embodiment
Present disclosure is further elucidated with reference to specific embodiment, but which is not intended to limit the protection model of the present invention
Enclose.
Embodiment 1
（1）25 g carbamide are put into into porcelain boat, heat treatment is carried out in tube furnace in the way of temperature programming.With 1oThe speed of C/min
Rate, from 25oC to 300oC, is incubated 1 h, then to 400oC, is incubated 2 h, finally to 500oC, and it is incubated 2 h.The Huang for obtaining
Color product carries out washing 3 ~ 6 times with the nitric acid and deionized water of 0.1 mol/L, to remove the basic group for adsorbing the residual on surface
Group.Product after washing is 90o6 h are dried under C, g-C is finally given3N4。
（2）Weigh 3.6 g Y (NO)3, 1.08 g Yb (NO)3, 0.026 g Tm (NO)3With 0.005 g Er (NO)3With
（1）In prepared 3.6 g g-C3N4It is dissolved in the deionized water of 60 mL, is subsequently adding the NaF of 1.8 g.Treat fully dissolving
Afterwards, transfer the solution into 125 mL with teflon-lined reactor in, in 200oHydro-thermal reaction 8 under the conditions of C
h.Room temperature, products therefrom dehydrated alcohol and deionized water 1 are naturally cooled to afterwards:1 mixed solution is washed 3 ~ 6 times, and
80o10 h are dried under C, NYF/g-C is obtained3N4Composite.
（3）KrF pulse lasers（Wavelength is 248 nm, and repetition rate is 20 Hz）It is straight for bombarding gold target preparation Au NPs
Footpath is 8 mm, and thickness is the bottom that the Au targets of 1.5 mm are placed on 6 mL beakers, and pure water is filled in beaker（pH≈6.5）, the water surface
Distance to Au targets surface is about 10 mm, and the energy density of laser is 30.0 J/cm2.Measured point by Neutron activation analysiss
In dispersion liquid, the concentration of Au NPs is about 50 ppm.Au NPs average diameters are about 16 nm.
（4）Will be a certain amount of（5mL）Freshly prepd Au NPs dispersion liquids are added to the NYF/g-C of 25 mg3N4In, mixing shakes up
Afterwards, 30 min of quiescent culture at room temperature.Peach precipitation is passed through into centrifugation, and it is clear successively with ethanol and deionized water
Wash, finally 60o12 h are dried under C and obtains 1wt %Au NPs16 nm/NYF/g-C3N4Photocatalyst.
Embodiment 2
As described in Example 1, except that by step（3）It is averagely straight that the aqueous solution pH of middle immersion Au targets is adjusted to 8.8, Au NPs
It is for about 9 nm that footpath becomes；Step（4）The volume of the Au NPs dispersion liquids of middle addition is changed into 15 mL, then final catalyst is containing 3wtThe 3 of % Au NPswt %Au NPs9 nm/NYF/g-C3N4。
Embodiment 3
As described in Example 1, except that by step（3）It is average that the aqueous solution pH of middle immersion Au targets is adjusted to 11.31, Au NPs
It is for about 7 nm that diameter becomes；Step（4）The volume of the Au NPs dispersion liquids of middle addition is changed into 25 mL, then final catalyst be containing
Have 5 wtThe 5 of % Au NPswt %Au NPs7 nm/NYF/g-C3N4。
Claims (3)
1. plasma and the enhanced multiband responsive photocatalyst preparation method of upper conversion, it is characterised in that methods described
Including procedure below：
The pure g-C in surface is prepared using normal pressure, the method without additional auxiliary and atmosphere regulation and control pyrolysis carbamide3N4Material；Claim respectively
Take Y (NO)3, Yb (NO)3, Tm (NO)3With Er (NO)3With prepared g-C3N4It is dissolved in the deionized water of 60mL, Ran Houjia
Enter NaF；After fully dissolving, transfer the solution into 125 mL with teflon-lined reactor, hydrothermal method
Obtain NYF/g-C3N4Composite；Using KrF pulse lasers（Wavelength is 248 nm, and repetition rate is 20 Hz）For bombarding gold
Target prepares Au NPs；The Au NPs dispersion liquids of preparation are added to into NYF/g-C finally3N4In, it is after mixing shakes up, quiet at room temperature
Put culture；By peach precipitation by centrifugation, and cleaned with ethanol and deionized water successively, drying obtains Au NPs/
NYF/g-C3N4Photocatalyst.
2. plasma according to claim 1 and the enhanced multiband responsive photocatalyst preparation method of upper conversion,
Characterized in that, the KrF pulse laser wavelengths are 248 nm, repetition rate is 20 Hz.
3. plasma according to claim 1 and the enhanced multiband responsive photocatalyst preparation method of upper conversion,
Characterized in that, the g-C3N4Material is with the g-C of two-dimensional layered structure3N4Based on support, up-conversion luminescent material NaYF4：
Yb3+, Er3+, Tm3+The Au NPs without part are uniform for microsphere and the surface that obtained using pulsed laser deposition method in a liquid
Be attached to g-C3N4On lamella.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108295880A (en) * | 2018-01-23 | 2018-07-20 | 莆田学院 | A kind of magnetic, multi-functional photochemical catalyst nanocomposite and preparation method thereof |
| CN108816266A (en) * | 2018-06-25 | 2018-11-16 | 肇庆市华师大光电产业研究院 | A kind of YF/g-C3N4Composite material and its application in photocatalysis |
| CN111408396A (en) * | 2020-03-13 | 2020-07-14 | 沈阳化工大学 | Au/Cu5FeS4/g-C3N4Preparation method of plasma composite photocatalyst |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111408396A (en) * | 2020-03-13 | 2020-07-14 | 沈阳化工大学 | Au/Cu5FeS4/g-C3N4Preparation method of plasma composite photocatalyst |
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| CN106540731B (en) | 2018-12-18 |
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