CN107866235A - A kind of method for preparing heterojunction photocatalyst - Google Patents
A kind of method for preparing heterojunction photocatalyst Download PDFInfo
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- CN107866235A CN107866235A CN201711013003.9A CN201711013003A CN107866235A CN 107866235 A CN107866235 A CN 107866235A CN 201711013003 A CN201711013003 A CN 201711013003A CN 107866235 A CN107866235 A CN 107866235A
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- deionized water
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000011943 nanocatalyst Substances 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000004140 cleaning Methods 0.000 claims description 16
- CBOIHMRHGLHBPB-UHFFFAOYSA-N hydroxymethyl Chemical compound O[CH2] CBOIHMRHGLHBPB-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 7
- 239000002105 nanoparticle Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 230000002045 lasting effect Effects 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052753 mercury Inorganic materials 0.000 abstract description 11
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 7
- 239000003546 flue gas Substances 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 29
- 239000003054 catalyst Substances 0.000 description 9
- 229910002651 NO3 Inorganic materials 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- URVGHPZOLQFKJZ-UHFFFAOYSA-N [Bi]=O.[I] Chemical compound [Bi]=O.[I] URVGHPZOLQFKJZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- -1 cadmium sulfide modified iodine oxygen bismuth Chemical class 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 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
- B01J27/06—Halogens; Compounds thereof
-
- 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
- B01J37/08—Heat treatment
-
- 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
- B01J37/341—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 electric or magnetic fields, wave energy or particle radiation
- B01J37/343—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 electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
Abstract
The invention provides a kind of method for preparing heterojunction photocatalyst, CdS, BiOI nanocatalyst are first prepared respectively, and CdS uniform loads are then formed by CdS/BiOI heterojunction photocatalysts to BiOI surfaces, then by calcination process by ultrasonic disperse.Hetero-junctions can efficiently separate photo-generate electron-hole pair, overcome the shortcomings that BiOI quantum efficiencies are low, so that prepared CdS/BiOI heterojunction photocatalysis materials have good catalytic performance under visible light conditions, being capable of effectively photochemical catalytic oxidation power-plant flue gas Elemental Mercury, the lower demercuration efficiency of LED irradiation reaches more than 80%, solves the problems, such as mercury emissions.In addition, preparation technology is simple, manufacturing cost is low.
Description
Technical field
The invention belongs to chemical field, is related to a kind of organic catalyst, and specifically one kind prepares high-performance optical catalysis
The method for aoxidizing nano-tube/CdS/BiOI heterojunction photocatalysts of power-plant flue gas mercury.
Background technology
Mercury as a kind of extremely toxic substance, have high volatile, easily in vivo with the property such as permanent enrichment in food chain,
Environmental and human health impacts are caused greatly to endanger, extensive attention has been caused to its emission control.Coal combustion is main people
For mercury emissions source, China accounts for 40% or so of anthropogenic discharge because of the mercury that fire coal is discharged every year, and it is left to account for 35% for wherein power plant
It is right.It is the demercuration technology in current more forward position using photocatalysis oxidation technique.In recent years, BiOI as a kind of visible light-inducing,
Narrow gap semiconductor and be widely studied.But BiOI quantum efficiency lower limits its further commercial Application.Therefore,
Need badly and develop the photochemical catalyst with high-quantum efficiency.
The content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of side for preparing heterojunction photocatalyst
Method, the described this method for preparing heterojunction photocatalyst will solve heterojunction photocatalyst catalytic efficiency of the prior art
It is low, preparation technology is complicated, prepare the high technical problem of cost.
The invention provides a kind of method for preparing heterojunction photocatalyst, comprise the following steps:
1) it is 1 in molar ratio:5 ratio weighs Cd (CH3COO)2·2H2O and CH4N2S, by Cd (CH3COO)2·2H2O and
CH4N2S is dissolved in deionized water, and lasting stirring obtains settled solution, solution is poured into hydrothermal reaction kettle, at 130 DEG C -160 DEG C
At a temperature of be incubated 18h-30h, use deionized water eccentric cleaning after then naturally cooling to room temperature, be transferred to afterwards in baking oven do
It is dry, obtain CdS nano particles;
2) Bi (NO are weighed3)3·5H2O is dissolved in (CH2OH)2Form solution A, described Bi (NO3)3·5H2O and (CH2OH)2
Material ratio be 1~2g:20~50ml;Weigh KI and be dissolved in (CH2OH)2Form solution B, described KI and (CH2OH)2Material
Than for 0.50g:20~50ml;By 1:1 volume ratio, solution A is added in B solution, uniform solution C is obtained, solution C is poured into
In hydrothermal reaction kettle, 18h-30h is incubated at a temperature of 130 DEG C -160 DEG C, naturally cool to after room temperature respectively with deionized water,
Ethanol eccentric cleaning, it is transferred in baking oven and dries afterwards, obtain BiOI nanocatalysts;
3) obtained BiOI nanocatalysts and CdS are dissolved into deionized water, described BiOI nanocatalysts and
CdS mass ratio is 1:0.2~0.4, ultrasonic disperse 20min-120min form CdS/BiOI suspensions, and eccentric cleaning is dried,
60min-180min is finally calcined at a temperature of 200 DEG C -350 DEG C CdS/BiOI heterojunction photocatalysts are made.
The invention provides a kind of synthesis side for the cadmium sulfide modified iodine oxygen bismuth photochemical catalyst that technique is simple, cost is more low
Method, it is using ultrasonic wave added calcination method synthesis CdS/BiOI heterojunction photocatalysts.First, CdS, BiOI is individually prepared to receive
Rice catalyst.Obtained BiOI nanocatalysts and a certain amount of CdS are dissolved into deionized water, will by ultrasonic disperse
CdS uniform loads by target solution eccentric cleaning for several times, finally obtain to BiOI surfaces by high-temperature calcination, natural cooling
CdS/BiOI heterojunction photocatalysts.
Hetero-junctions can efficiently separate photo-generate electron-hole pair, overcome the shortcomings that BiOI quantum efficiencies are low so that made
Standby CdS/BiOI heterojunction photocatalysis materials have good catalytic performance under visible light conditions, being capable of effectively photocatalytic-oxidation
Change power-plant flue gas Elemental Mercury, the lower demercuration efficiency of LED irradiation reaches more than 80%, solves the problems, such as mercury emissions.In addition, preparation technology
Simply, manufacturing cost is low.
Cadmium sulfide modified iodine oxygen bismuth (CdS/BiOI) photochemical catalyst obtained by the present invention can be used as power-plant flue gas photocatalysis
Oxidation catalyst.It can be seen that the simulated flue gas (nitrogen, air) for carrying element mercury passes through light-catalyzed reaction in experimentation
The content of element mercury significantly reduces after device.
The present invention compares with prior art, and its technological progress is significant.Technique of the invention is simple, cost is low.Utilize
Photochemical catalyst made from this method, micro cadmium sulfide are supported on iodine oxygen bismuth surface, hence it is evident that improve the quantum efficiency of iodine oxygen bismuth, energy
The preferable photochemical catalytic oxidation gas mercury under visible light conditions.
Brief description of the drawings
Fig. 1:The SEM figures of the sample of case study on implementation 1.
Fig. 2:The PL figures of the sample of case study on implementation 2.
Fig. 3:The sample of case study on implementation 3 demercuration efficiency figure under simulated flue gas carrier gas.
Embodiment
With reference to embodiment to the detailed description of the invention, so that those skilled in the art more fully understand the present invention, but
The invention is not limited in following case study on implementation.
Cadmium acetate used in the present invention, two water (>=98.5%), thiocarbamide (>=99.0%), bismuth nitrate, five water (>=99.0%),
KI (>=99.0%), ethylene glycol (>=99.0%).Above medicine is bought in Chemical Reagent Co., Ltd., Sinopharm Group, examination
Medicine is tested not to be further processed.
SEM used in the present invention (ESEM) uses Philips XL30 type electron microscopes.
PL spectrum used in the present invention use the SHIMADZU RF5301 type fluorescence Spectra testers that Japan produces, and excite
Wavelength is 320nm.
Online mercury tester used in the present invention is the portable Zeemen effect mercury analyzer RA-915M of LUMEX, zero-signal standard
Deviation<0.2ng/m3。
Embodiment 1
1) 0.85g Cd (CH are weighed3COO)2·2H2O and 1.21g CH4N2S, it is dissolved in 40ml deionized waters, persistently stirs
Mix to obtain settled solution, target solution is poured into 150 DEG C of holding 20h in 50ml hydrothermal reaction kettles, used after naturally cooling to room temperature
Deionized water eccentric cleaning for several times, is transferred in baking oven and dried, obtain CdS nano particles afterwards.
2) by 1.46g Bi (NO3)3·5H2O is dissolved in 20ml (CH2OH)2Form solution A.0.50g KI is dissolved in 20ml
(CH2OH)2Form solution B.By 1:1 volume ratio, solution A is slowly dropped into B solution, obtains uniform solution C.By solution C
160 DEG C of holding 18h in 50ml hydrothermal reaction kettles are poured into, are naturally cooled to after room temperature respectively with deionized water, ethanol eccentric cleaning
For several times, it is transferred in baking oven and dries afterwards, obtains BiOI nanocatalysts.
3) 1g BiOI and 0.2g CdS are dissolved into deionized water, and it is suspended that ultrasonic disperse 30min obtains CdS/BiOI
Liquid, eccentric cleaning are dried, and finally 350 DEG C of holding 60min in Muffle furnace, are made CdS/BiOI heterojunction photocatalysts.
Embodiment 2
1) 3.19mmol Cd (CH are weighed3COO)2·2H2O and 15.95mmol CH4N2S, it is dissolved in 40ml deionized waters
In, lasting stirring obtains settled solution, and target solution is poured into 130 DEG C of holding 30h in 50ml hydrothermal reaction kettles, naturally cooled to
After room temperature with deionized water eccentric cleaning for several times, it is transferred in baking oven and dries afterwards, obtains CdS nano particles.
2) by 1.46g Bi (NO3)3·5H2O is dissolved in 20ml (CH2OH)2Form solution A.0.50g KI is dissolved in 20ml
(CH2OH)2Form solution B.By 1:1 volume ratio, solution A is slowly dropped into B solution, obtains uniform solution C.By solution C
150 DEG C of holding 20h in 50ml hydrothermal reaction kettles are poured into, are naturally cooled to after room temperature respectively with deionized water, ethanol eccentric cleaning
For several times, it is transferred in baking oven and dries afterwards, obtains BiOI nanocatalysts.
3) 1g BiOI and 0.4g CdS are dissolved into deionized water, and it is suspended that ultrasonic disperse 60min obtains CdS/BiOI
Liquid, eccentric cleaning are dried, and finally 300 DEG C of holding 90min in Muffle furnace, are made CdS/BiOI heterojunction photocatalysts.
Embodiment 3
1) 3.19mmol Cd (CH are weighed3COO)2·2H2O and 1.21g CH4N2S, it is dissolved in 40ml deionized waters, holds
Continuous stirring obtains settled solution, and target solution is poured into 160 DEG C of holding 18h in 50ml hydrothermal reaction kettles, naturally cools to room temperature
Afterwards with deionized water eccentric cleaning for several times, it is transferred in baking oven and dries afterwards, obtains CdS nano particles.
2) by 1.46g Bi (NO3)3·5H2O is dissolved in 20ml (CH2OH)2Form solution A.0.50g KI is dissolved in 20ml
(CH2OH)2Form solution B.By 1:1 volume ratio, solution A is slowly dropped into B solution, obtains uniform solution C.By solution C
140 DEG C of holding 24h in 50ml hydrothermal reaction kettles are poured into, are naturally cooled to after room temperature respectively with deionized water, ethanol eccentric cleaning
For several times, it is transferred in baking oven and dries afterwards, obtains BiOI nanocatalysts.
3) 1g BiOI and 0.2g CdS are dissolved into deionized water, and it is suspended that ultrasonic disperse 30min obtains CdS/BiOI
Liquid, eccentric cleaning are dried, and finally 250 DEG C of holding 120min in Muffle furnace, are made CdS/BiOI heterojunction photocatalysts.
Fig. 1 is that the SEM of the sample of case study on implementation 1 schemes, and as can be seen from the figure catalyst distribution is uniform, does not occur agglomeration.
Fig. 2 is that the PL of case study on implementation sample 2 schemes, it can be seen that the CdS/BiOI heterojunction photocatalysts of the present invention are compared to pure
Phase BiOI, photo-generate electron-hole recombination rate substantially reduce, and quantum efficiency gets a promotion.Fig. 3 is the sample of case study on implementation 3 in simulation cigarette
Demercuration efficiency figure under airborne gas, as we know from the figure catalyst of the invention under the conditions of simulated flue gas carrier gas demercuration efficiency compared with BiOI
(16% or so) comparing has larger lifting (80% or so).
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow conversion that bright specification is made, or other related technical areas are directly or indirectly used in,
Similarly it is included within the scope of the present invention.
Claims (1)
- A kind of 1. method for preparing heterojunction photocatalyst, it is characterised in that comprise the following steps:1)It is 1 in molar ratio:5 ratio weighs Cd (CH3COO)2·2H2O and CH4N2S, by Cd (CH3COO)2·2H2O and CH4N2S is dissolved in deionized water, and lasting stirring obtains settled solution, solution is poured into hydrothermal reaction kettle, at 130 DEG C -160 DEG C At a temperature of be incubated 18h-30h, use deionized water eccentric cleaning after then naturally cooling to room temperature, be transferred to afterwards in baking oven do It is dry, obtain CdS nano particles;2)Weigh Bi (NO3)3•5H2O is dissolved in (CH2OH)2Form solution A, described Bi (NO3)3•5H2O and (CH2OH)2Thing Expect that ratio is 1 ~ 2 g:20~50 ml;Weigh KI and be dissolved in (CH2OH)2Form solution B, described KI and (CH2OH)2Material ratio For 0.50g:20 ~50ml;By 1:1 volume ratio, solution A is added in B solution, uniform solution C is obtained, solution C is poured into water In thermal response kettle, 18h-30h is incubated at a temperature of 130 DEG C -160 DEG C, is naturally cooled to after room temperature respectively with deionized water, second Alcohol eccentric cleaning, it is transferred in baking oven and dries afterwards, obtain BiOI nanocatalysts;3)Obtained BiOI nanocatalysts and CdS are dissolved into deionized water, described BiOI nanocatalysts and CdS's Mass ratio is 1:0.2 ~ 0.4, ultrasonic disperse 20min-120min form CdS/BiOI suspensions, and eccentric cleaning is dried, finally existed 60min-180min is calcined at a temperature of 200 DEG C -350 DEG C CdS/BiOI heterojunction photocatalysts are made.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109289873A (en) * | 2018-10-29 | 2019-02-01 | 江苏大学 | A kind of heterojunction material and preparation method and purposes |
CN113398954A (en) * | 2021-05-08 | 2021-09-17 | 华南理工大学 | BiOI/CdS composite photocatalyst and preparation method and application thereof |
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CN103623803A (en) * | 2012-08-30 | 2014-03-12 | 上海纳晶科技有限公司 | Visible light photocatalyst and preparation method therefor |
CN105879888A (en) * | 2016-01-22 | 2016-08-24 | 江苏大学 | Method for preparing CdS/BiOI heterojunction complex photocatalyst |
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2017
- 2017-10-26 CN CN201711013003.9A patent/CN107866235B/en active Active
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CN103623803A (en) * | 2012-08-30 | 2014-03-12 | 上海纳晶科技有限公司 | Visible light photocatalyst and preparation method therefor |
CN105879888A (en) * | 2016-01-22 | 2016-08-24 | 江苏大学 | Method for preparing CdS/BiOI heterojunction complex photocatalyst |
Non-Patent Citations (1)
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109289873A (en) * | 2018-10-29 | 2019-02-01 | 江苏大学 | A kind of heterojunction material and preparation method and purposes |
CN109289873B (en) * | 2018-10-29 | 2021-09-10 | 江苏大学 | Heterojunction material, preparation method and application |
CN113398954A (en) * | 2021-05-08 | 2021-09-17 | 华南理工大学 | BiOI/CdS composite photocatalyst and preparation method and application thereof |
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