CN103920520B - A kind of ultrasonic assistant sedimentation synthesis of nano SnO 2/ g-C 3n 4the preparation method of composite visible light catalyst - Google Patents
A kind of ultrasonic assistant sedimentation synthesis of nano SnO 2/ g-C 3n 4the preparation method of composite visible light catalyst Download PDFInfo
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Abstract
The invention discloses a kind of ultrasonic assistant sedimentation synthesis of nano SnO
2/ g-C
3n
4the preparation method of composite visible light catalyst, belongs to depollution of environment catalysis material preparing technical field.The method process comprises: adopt microwave hydrolysis and micro-wave drying method to prepare nano SnO
2, prepare g-C by the polycondensation reaction of melamine
3n
4, then by both in proportion ground and mixed evenly after be scattered in methanol solvate, then adopt ultrasonic assistant sedimentation by nano SnO
2uniform deposition is at g-C
3n
4surface, obtains nano SnO
2/ g-C
3n
4composite visible light catalyst.Nano SnO prepared by the present invention
2/ g-C
3n
4composite visible light catalyst has excellent visible light catalytic performance and good catalytic stability, and its raw material sources are extensive, and preparation method is simple, and the reaction time is short, and preparation efficiency is high, is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of ultrasonic assistant sedimentation synthesis of nano SnO
2/ g-C
3n
4the preparation method of composite visible light catalyst, belongs to depollution of environment photocatalyst material preparing technical field.
Background technology
Find that from 1972 nano titanium oxide can decomposition water under light illumination, Nano semiconductor photocatalysis technology causes the extensive concern in the world, and is considered to the green environment purification techniques of most development prospect and application prospect.Traditional Nano semiconductor photocatalyst material is as nano-TiO
2be widely studied with ZnO etc., but be subject to the impact of himself energy gap comparatively large (3.2eV), deposited and respond the problems such as weak, quantum efficiency is low under visible light, seriously govern the practical application of photocatalysis technology.Therefore the problem urgently to be resolved hurrily that development of new efficient visible light catalysis material becomes current photocatalysis field is found.
Found by research in recent years, g-C
3n
4there is conjugated pi structure and be material the most stable in all carbonitride allotropes, there is the machinery of very high heat endurance, chemical stability and excellence, electrical and optical properties.Wang Xinchen etc. (NatureMaterials, 2009,8:76-80) determine g-C by experiment
3n
4optical band gap is 2.7eV, under visible light illumination can the hydrogen manufacturing of catalytic decomposition water, is the potential novel visible catalysis material of a class.But regrettably, g-C
3n
4the quantum efficiency generating hydrogen at 420nm place is about 0.1%, therefore g-C
3n
4the limitation that self cannot break through is had in actual application.In order to improve g-C
3n
4visible light catalysis activity and catalytic stability, researcher has carried out a series of g-C
3n
4study on the modification as dye sensitization, transition metal modified, nano semiconductor material and g-C
3n
4the methods such as forming hetero-junctions that combines improves g-C
3n
4photocatalytic activity.MiaoXu (ACSAppliedMaterials & Interfaces, 2013,5:12533-12540) uses Ag
2o and g-C
3n
4hetero-junctions composite semiconductor light-catalyst is prepared with liquid phase synthesizing method under room temperature.Work as g-C
3n
4with Ag
2effectively can suppress light induced electron and hole-recombination probability when O ratio is 1:4, improve photocatalytic, degradation rate is pure g-C
3n
411 times.The people such as Zhu Yongfa (Energy & EnvironmentalScience, 2011,4:2922 – 2929) utilize g-C
3n
4conjugated pi structure, by g-C
3n
4hydridization is carried out, ZnO and g-C after hydridization with ZnO
3n
4between produce cooperative effect, improve separation of charge efficiency and suppress ZnO photoetch, observed photoelectric current under visible light.
Tetragonal SnO
2be the nano semiconductor material of broad-band gap, be widely used in fields such as lithium battery, air-sensitive and opto-electronic conversion.Recent research finds, nano SnO
2be one and compare TiO
2electron acceptor better with ZnO, is more conducive to prepare highly active hetero-junctions catalyst.The people such as MTamezUddin (InorganicChemistry, 2012,51:7764-7773) adopt two-step method to prepare mesoporous nano SnO
2-ZnO heterojunction photochemical catalyst, effectively suppresses SnO
2-ZnO photocatalyst photo-generate electron-hole compound, thus the photocatalytic activity improving heterojunction photocatalyst.The people such as GuangsheLi (ChemicalEngineeringJournal, 2014,246:277 – 286) are with K
2snO
3for raw material hydrolysis 12h in the autoclave of 180 DEG C obtains nano SnO through 80 DEG C of dry 24h again
2, then joined the g-C after ultrasonic disperse 30min
3n
4in ethanolic solution, after mechanical agitation 24h evaporates alcohol solvent, then calcine 1h at 400 DEG C, prepare the good nanometer g-C of photocatalytic activity
3n
4/ SnO
2composite visible light catalytic material.But this preparation method's Problems existing is, need experience reaction or dried journey for several times, and reaction temperature is high, pressure is large, and the reaction time is long, also easily causes the reunion of nano particle, can affect nanometer g-C
3n
4/ SnO
2giving full play to of composite photocatalytic activity.
Summary of the invention
The object of the present invention is to provide a kind of ultrasonic assistant sedimentation synthesis of nano SnO
2/ g-C
3n
4the preparation method of composite visible light catalyst, the nano SnO prepared in this way
2/ g-C
3n
4composite has excellent visible light catalytic performance and good stability, and preparation method is simple, and the reaction time is short, and preparation efficiency is high.
For achieving the above object, the present invention is achieved by following technical proposals: with SnCl
45H
2o is raw material, adopts microwave induced hydrolysis, produces a large amount of SnO fast
2nucleus, and form small grains, suppress crystal grain to be grown up further; Adopt microwave rapid draing simultaneously, remove high-temperature calcination process from, ensure that nano SnO
2the size of particle is homogeneous, does not reunite.Be that presoma adopts condensation methods to prepare g-C with melamine
3n
4, then adopt ultrasonic assistant deposition process by prepared nano SnO
2with g-C
3n
4carry out compound, the high-speed micro-jet utilizing ultrasonic cavitation effect to produce makes nano SnO
2at g-C
3n
4high-speed impact is carried out on surface, by nano SnO
2deposit securely with good dispersity or be embedded in g-C
3n
4surface, obtained nano SnO
2/ g-C
3n
4composite visible light catalyst.Described preparation method mainly comprises the steps:
A. by 1.0g ~ 10.5gSnCl
45H
2o adds in 10mL ~ 20mL methyl alcohol, and ultrasonic disperse 20min, is made into SnCl
4methanol solution, then under agitation to this SnCl
4methanol solution in add weak aqua ammonia and regulate the pH of solution to be 2 ~ 3, slowly add 50mL ~ 100mL distilled water again, continuing to stir 10min ~ 15min makes reactant liquor mix, then put into micro-wave oven and respectively add thermal response 5min ~ 15min under microwave power 300W and 500W, room temperature is cooled to, suction filtration after having reacted.Filter cake carries out dry heat process under microwave, and microwave drying condition is each 2min ~ 6min of 300W and 500W, obtains white powder, be nano SnO after taking out grinding
2.
B. get 3.0g ~ 20.0g melamine and carry out polycondensation reaction in the inherent Muffle furnace of crucible, with the ramp to 300 DEG C of 10 DEG C/min ~ 30 DEG C/min, constant temperature 30min; Again with the ramp to 400 DEG C of 30 DEG C/min ~ 50 DEG C/min, constant temperature 30min; Afterwards with the ramp to 500 DEG C of 30 DEG C/min ~ 50 DEG C/min, constant temperature 30min; Finally with the ramp to 520 of 5 DEG C/min ~ 20 DEG C/min DEG C ~ 600 DEG C, constant temperature 0.5h ~ 2h.React complete to take out after sample cools naturally, grind into powder.Gained powder is placed in Muffle furnace again and carries out secondary polycondensation reaction, with the ramp of 10 DEG C/min ~ 30 DEG C/min to 500 DEG C ~ 580 DEG C constant temperature 0.5h ~ 2h, after system cools naturally, take out sample grinding after having reacted, obtain g-C
3n
4.
C. by the g-C of above-mentioned prepared 0.15g ~ 0.8g
3n
4with 0.1g ~ 0.7g nano SnO
2after ground and mixed 20min ~ 30min, then join in 20mL ~ 40mL methyl alcohol, ultrasonic disperse 10min ~ 20min under air-proof condition, then uncoveredly ultrasonicly powder is become to mixture, continue ultrasonic disperse 5min ~ 10min again, gained powder distilled water and methyl alcohol are respectively washed 3 times, dry 0.5h ~ 1h at 50 DEG C ~ 70 DEG C, after taking out grinding, obtain nano SnO
2/ g-C
3n
4composite visible light catalyst.
Preferably, SnCl in step a
4snCl in methanol solution
4concentration be 0.6mol/L ~ 1.0mol/L.
Preferably, under microwave power 300W and 500W, respectively 8min ~ 12min is heated in step a microwave hydrolysis process.
Preferably, in step a microwave drying process, adopt each 2min ~ 3min of power 300W and 500W, interval 1min.
Preferably, SnO described in step c
2and g-C
3n
4mixing quality is than 1:1 ~ 1:4.
Preferably, nano SnO in step c
2with g-C
3n
4the concentration of mixture in methyl alcohol be 20g/L ~ 30g/L.
The invention has the advantages that:
(1) microwave hydrolysis and micro-wave drying method is adopted to prepare nano SnO
2, obtain the SnO that average grain diameter is 2nm ~ 3nm
2, fast, efficiency is high in reaction, and avoids the problems such as grain growth that conventional high-temperature calcination process causes, reunion and catalytic activity reduction.
(2) nano SnO is prepared
2/ g-C
3n
4adopt ultrasonic assistant method during composite visible light catalyst, both can make nano SnO
2and g-C
3n
4keep good dispersity in a solvent, the high-speed micro-jet that ultrasonic cavitation effect produces simultaneously can make nano SnO again
2at g-C
3n
4high-speed impact is carried out on surface, thus by nano SnO
2deposit securely with good dispersity or be embedded in g-C
3n
4surface.Ultrasonic assistant method makes recombination process complete fast, and reaches the incomparable effect of common mechanical complex method.
(3) nano SnO
2be one and compare TiO
2electron acceptor better with ZnO, with g-C
3n
4there is after compound significant cooperative effect, can accept fast and shift g-C
3n
4by the light induced electron that optical excitation produces, thus effectively suppress the recombination probability of photo-generate electron-hole, make prepared nano SnO
2/ g-C
3n
4composite visible light catalyst shows excellent visible light catalytic performance.
(4) this method raw material sources are extensive, low price, and preparation method is simple, and reaction speed is fast, and the time is short, and preparation efficiency is high, is suitable for large-scale production.
Accompanying drawing explanation
The nano SnO of Fig. 1 prepared by embodiment 1
2/ g-C
3n
4the X ray diffracting spectrum of composite visible light catalyst;
The nano SnO of Fig. 2 prepared by embodiment 1
2/ g-C
3n
4the transmission electron microscope photo of composite visible light catalyst;
The nano SnO of Fig. 3 prepared by embodiment 1
2/ g-C
3n
4composite visible light catalyst (a) and pure g-C
3n
4(b) and nano SnO
2c () be catalytic degradation methyl orange experimental result picture under visible light;
The nano SnO of Fig. 4 prepared by embodiment 1
2/
g-C
3n
4the circulation experiment result figure of composite visible light catalyst visible light photocatalytic degradation methyl orange.
Detailed description of the invention
Embodiment 1
Get 2.10gSnCl
45H
2o is dissolved in 10mL methyl alcohol, and ultrasonic disperse 20min, is made into SnCl
4concentration is the methanol solution of 0.6mol/L, adding weak aqua ammonia under agitation regulates pH to be 2.5, slowly add 50mL distilled water again, continuing to stir 15min makes reactant liquor mix, put into micro-wave oven, under microwave power 300W and 500W, respectively add thermal response 10min, after having reacted, be cooled to room temperature, suction filtration.Filter cake carries out drying process under microwave, and drying condition is each 3min of microwave power 300W and 500W, interval 1min, takes out, and grinding, obtains white powder, be nano SnO
2.Get 15g melamine and put into Muffle furnace in crucible, under semiclosed condition, carry out polycondensation reaction, Muffle furnace heating schedule is set with the ramp to 300 DEG C of 10 DEG C/min, constant temperature 30min; Continue to be warming up to 400 DEG C with the speed of 40 DEG C/min, constant temperature 30min; With the ramp to 500 DEG C of 40 DEG C/min, constant temperature 30min; 5 DEG C/min is warming up to 560 DEG C, constant temperature 2h, takes out, grind into powder after sample cools naturally.Carry out polycondensation reaction by uncovered in crucible for gained powder, with the ramp to 580 DEG C of 15 DEG C/min, constant temperature 1h, takes out and grinds to obtain g-C after system cools naturally
3n
4.By 0.35gg-C
3n
4and 0.15gSnO
2grind 20min in mortar after, join in 20mL methyl alcohol, sealing ultrasonic disperse 20min, uncovered ultrasonic disperse becomes powder to mixture again, after continuing ultrasonic disperse 10min, powder is respectively washed 3 times with distilled water and methyl alcohol respectively, at 50 DEG C, dry 0.5h, obtains nano SnO after grinding
2/ g-C
3n
4composite visible light catalyst.
Nano SnO prepared in the present embodiment
2/ g-C
3n
4the X ray diffracting spectrum of composite visible light catalyst as shown in Figure 1.In Fig. 1,27.4 °, 13.2 ° place's diffraction maximum corresponding g-C respectively
3n
4(002) and (100) crystal face, 33.5 °, 51.4 ° place's diffraction maximums respectively corresponding nano SnO
2(101) and (211) crystal face, with g-C
3n
4and SnO
2standard spectrogram (JCPDS87-1526 with JCPDS070-6153) identical.Nano SnO prepared by showing from Fig. 2
2/ g-C
3n
4the transmission electron micrograph of composite photo-catalyst can be found out, g-C
3n
4for smooth and smooth layer structure, SnO
2evenly be embedded in g-C
3n
4surface, average grain diameter is 2 ~ 3nm, and soilless sticking phenomenon.
Prepared nano SnO
2/ g-C
3n
4the performance test of composite visible light catalyst is as follows: in open reactor, add the nano SnO prepared by 0.1g
2/ g-C
3n
4composite visible light catalyst and 100mL concentration are the methyl orange solution of 10mg/L, be 3 by concentrated sulfuric acid adjust ph, stir after 1h reaches adsorption equilibrium under dark condition, open visible light source (two 36W fluorescent lamps, add a cover optical filter below filtering 400nm light) irradiate, sample from reaction system in a certain time interval, after high speed centrifugation separated light catalyst, get supernatant liquor ultraviolet-visible spectrophotometer and measure full wave absorbance, the change in concentration situation of methyl orange in solution is detected.The nano SnO of Fig. 3 prepared by embodiment 1
2/ g-C
3n
4composite visible light catalyst (a) and pure g-C
3n
4(b) and nano SnO
2c () be catalytic degradation methyl orange experimental result picture under visible light.
As can be seen from Figure 3, when radiation of visible light 100min, the nano SnO prepared by the present embodiment
2/ g-C
3n
4the visible light photocatalytic degradation rate of visible light catalyst to methyl orange reaches 95%, and the pure g-C prepared under the same terms
3n
4be 15% to the visible light photocatalytic degradation rate of methyl orange, pure nano SnO
2to the degradation rate of methyl orange less than 3%, substantially do not have visible light photocatalytic degradation active.Nano SnO prepared by this method is described
2/ g-C
3n
4between two kinds of components in composite visible light catalyst, there is obvious cooperative effect, effectively can suppress the recombination probability of photo-generate electron-hole, the visible light catalysis activity of composite catalyst is significantly improved.
Embodiment 2
Get 4.20gSnCl
45H
2o is dissolved in 10mL methyl alcohol, and ultrasonic disperse 20min, is made into SnCl
4concentration is the methanol solution of 1.2mol/L, adding weak aqua ammonia under agitation regulates pH to be 2.5, slowly add 50mL distilled water again, continuing to stir 15min makes reactant liquor mix, put into micro-wave oven, under microwave power 300W and 500W, respectively add thermal response 10min, after having reacted, be cooled to room temperature, suction filtration.Filter cake carries out drying process under microwave, and drying condition is each 3min of microwave power 300W and 500W, and interval 1min, then takes out and grind, and obtains white powder, is nano SnO
2.Get 10g melamine and put into Muffle furnace in crucible, under semiclosed condition, carry out polycondensation reaction, Muffle furnace heating schedule is set with the ramp to 300 DEG C of 10 DEG C/min, constant temperature 30min; Continue to be warming up to 400 DEG C with the speed of 30 DEG C/min, constant temperature 30min; With the ramp to 500 DEG C of 30 DEG C/min, constant temperature 30min; 5 DEG C/min is warming up to 560 DEG C, constant temperature 1h, takes out, grind into powder after sample cools naturally.Carry out polycondensation reaction by uncovered in crucible for gained powder, with the ramp of 20 DEG C/min to 560 DEG C, constant temperature 1.5h, takes out after system cools naturally, obtains g-C after grinding
3n
4.By 0.40gg-C
3n
4and 0.10gSnO
2grind 20min in mortar after, join in 20mL methyl alcohol, sealing ultrasonic disperse 10min, uncovered ultrasonic disperse becomes powder to mixture again, and after continuing ultrasonic disperse 10min, powder respectively washs 3 times with distilled water and methyl alcohol respectively, at 50 DEG C, dry 0.5h, obtains nano SnO after grinding
2/ g-C
3n
4composite visible light catalyst.Experiment records the above-mentioned nano SnO when radiation of visible light 100min
2/ g-C
3n
4composite photo-catalyst is 76% to the photocatalytic activity of methyl orange solution.
Embodiment 3
Get 6.20gSnCl
45H
2o is dissolved in 30mL methyl alcohol, and ultrasonic disperse 20min, is made into SnCl
4concentration is the methanol solution of 0.6mol/L, adding weak aqua ammonia under agitation regulates pH to be 2.5, slowly add 100mL distilled water again, continuing to stir 15min makes reactant liquor mix, put into micro-wave oven, under microwave power 300W and 500W, respectively add thermal response 10min, after having reacted, be cooled to room temperature, suction filtration.Filter cake carries out drying process under microwave, and drying condition is each 3min of microwave power 300W and 500W, interval 1min, takes out, and grinding, obtains white powder, be nano SnO
2.Get 20g melamine and put into Muffle furnace in crucible, under semiclosed condition, carry out polycondensation reaction, Muffle furnace heating schedule is set with the ramp to 300 DEG C of 10 DEG C/min, constant temperature 30min; Continue to be warming up to 400 DEG C with the speed of 30 DEG C/min, constant temperature 30min; With the ramp to 500 DEG C of 30 DEG C/min, constant temperature 30min; 5 DEG C/min is warming up to 580 DEG C, constant temperature 1h, takes out, grind into powder after sample cools naturally.Carry out polycondensation reaction by uncovered in crucible for gained powder, with the ramp of 20 DEG C/min to 580 DEG C of constant temperature 1h, take out after system cools naturally and grind to obtain g-C
3n
4.By 0.25gg-C
3n
4and 0.25gSnO
2grind 20min in mortar after, join in 20mL methyl alcohol, sealing ultrasonic disperse 20min, uncovered ultrasonic disperse becomes powder to mixture again, and after continuing ultrasonic disperse 5min, powder respectively washs 3 times with distilled water and methyl alcohol respectively, at 50 DEG C, dry 0.5h, obtains nano SnO after grinding
2/ g-C
3n
4composite visible light catalyst.Experiment records the above-mentioned nano SnO when radiation of visible light 100min
2/ g-C
3n
4composite visible light catalyst is 87% to the photocatalytic activity of methyl orange solution.
Embodiment 4
Choose the nano SnO prepared by embodiment 1
2/ g-C
3n
4composite visible light catalyst carries out cycle down solution methyl orange solution experiments under visible light to investigate its photocatalysis stability.In circulation experiment, nano SnO
2/ g-C
3n
4composite visible light catalyst is used to repeat methyl orange solution of degrading, and after illumination 160min, catalyst is through centrifugation, and washing, carry out the test of methyl orange solution degraded next time after drying, result is by shown in accompanying drawing 4.The nano SnO of Fig. 4 prepared by embodiment 1
2/ g-C
3n
4the circulation experiment result figure of composite visible light catalyst visible light photocatalytic degradation methyl orange, as can be seen from the circulation experiment result in Fig. 4, after being cycled to repeat use through 4 times, this photochemical catalyst still keeps efficient photocatalytic activity, shows that this photochemical catalyst has good photocatalysis stability.
Claims (4)
1. a ultrasonic assistant sedimentation synthesis of nano SnO
2/ g-C
3n
4the preparation method of composite visible light catalyst, is characterized in that, with SnCl
45H
2o is raw material, adopts microwave hydrolysis and micro-wave drying method to prepare nano SnO
2, be that presoma adopts condensation methods to prepare g-C with melamine
3n
4, then nano SnO is prepared by liquid phase deposition under ultrasonic assistant
2/ g-C
3n
4composite visible light catalyst, its method comprises the steps:
A. by 1.0g ~ 10.5gSnCl
45H
2o adds in 10mL ~ 20mL methyl alcohol, and ultrasonic disperse 20min, is made into SnCl
4methanol solution, then under agitation to this SnCl
4methanol solution in add weak aqua ammonia and regulate the pH of solution to be 2 ~ 3, slowly add 50 ~ 100mL distilled water again, continuing to stir 10min ~ 15min makes reactant liquor mix, put it into afterwards in micro-wave oven, under microwave power 300W and 500W, respectively heat 5min ~ 15min to be hydrolyzed reaction, room temperature is cooled to after having reacted, suction filtration, filter cake is carried out dry heat process under microwave, microwave drying condition is each 2min ~ 6min of 300W and 500W, obtain white powder after being ground by filter cake, be nano SnO
2;
B. get 3.0g ~ 20.0g melamine and carry out polycondensation reaction in the inherent Muffle furnace of crucible, first with the ramp to 300 DEG C of 10 DEG C/min ~ 30 DEG C/min, constant temperature 30min; Again with the ramp to 400 DEG C of 30 DEG C/min ~ 50 DEG C/min, constant temperature 30min; Afterwards with the ramp to 500 DEG C of 30 DEG C/min ~ 50 DEG C/min, constant temperature 30min; Finally with the ramp to 520 of 5 DEG C/min ~ 20 DEG C/min DEG C ~ 600 DEG C, constant temperature 0.5h ~ 2h; React complete to take out after sample cools naturally, and grind into powder, gained powder is placed in Muffle furnace again and carries out secondary polycondensation reaction, with the ramp of 10 DEG C/min ~ 30 DEG C/min to 500 DEG C ~ 580 DEG C constant temperature 0.5h ~ 2h, after system cools naturally, take out sample grinding after having reacted, obtain g-C
3n
4;
C. by the 0.1g ~ 0.7g nano SnO prepared by step a and b
2with the g-C of 0.15g ~ 0.8g
3n
4after ground and mixed 20min ~ 30min, join in 20mL ~ 40mL methyl alcohol again, ultrasonic disperse 10min ~ 20min under air-proof condition, then uncoveredly ultrasonicly powder is become to mixture, continue ultrasonic disperse 5min ~ 10min again, gained powder distilled water and methyl alcohol are respectively washed 3 times, dry 0.5h ~ 1h at 50 DEG C ~ 70 DEG C, then can nano SnO be obtained after grinding
2/ g-C
3n
4composite visible light catalyst.
2. ultrasonic assistant sedimentation synthesis of nano SnO as claimed in claim 1
2/ g-C
3n
4the preparation method of composite visible light catalyst, is characterized in that, SnCl in described step a
4methanol solution in SnCl
4concentration be 0.6mol/L ~ 1.0mol/L.
3. ultrasonic assistant sedimentation synthesis of nano SnO as claimed in claim 1
2/ g-C
3n
4the preparation method of composite visible light catalyst, is characterized in that, respectively heats 8min ~ 12min in described step a microwave hydrolysis course of reaction under microwave power 300W and 500W condition.
4. ultrasonic assistant sedimentation synthesis of nano SnO as claimed in claim 1
2/ g-C
3n
4the preparation method of composite visible light catalyst, is characterized in that, nano SnO described in step c
2with g-C
3n
4mass ratio be 1:1 ~ 1:4, nano SnO
2with g-C
3n
4the concentration of mixture in methyl alcohol be 20g/L ~ 30g/L.
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| CN111569932B (en) * | 2020-06-17 | 2023-04-11 | 吉林大学 | Composite material and preparation method, photocatalyst and application thereof |
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