CN105879883B - A kind of Visible Light Induced Photocatalytic methylene blue photochemical catalyst α-EuZrS3 - Google Patents
A kind of Visible Light Induced Photocatalytic methylene blue photochemical catalyst α-EuZrS3 Download PDFInfo
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- CN105879883B CN105879883B CN201610210174.XA CN201610210174A CN105879883B CN 105879883 B CN105879883 B CN 105879883B CN 201610210174 A CN201610210174 A CN 201610210174A CN 105879883 B CN105879883 B CN 105879883B
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 39
- 229960000907 methylthioninium chloride Drugs 0.000 title claims abstract description 26
- 239000003054 catalyst Substances 0.000 title claims abstract description 15
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 title claims 12
- 239000013078 crystal Substances 0.000 claims abstract description 32
- 230000000694 effects Effects 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 6
- 230000015556 catabolic process Effects 0.000 claims abstract 7
- 238000006731 degradation reaction Methods 0.000 claims abstract 7
- 238000007146 photocatalysis Methods 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052798 chalcogen Inorganic materials 0.000 claims description 13
- 150000001787 chalcogens Chemical class 0.000 claims description 13
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
- 239000010453 quartz Substances 0.000 claims description 12
- 239000000376 reactant Substances 0.000 claims description 12
- 239000003708 ampul Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229940079593 drug Drugs 0.000 claims description 3
- 239000003814 drug Substances 0.000 claims description 3
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000021050 feed intake Nutrition 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000005286 illumination Methods 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 238000003795 desorption Methods 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- XQAXGZLFSSPBMK-UHFFFAOYSA-M [7-(dimethylamino)phenothiazin-3-ylidene]-dimethylazanium;chloride;trihydrate Chemical compound O.O.O.[Cl-].C1=CC(=[N+](C)C)C=C2SC3=CC(N(C)C)=CC=C3N=C21 XQAXGZLFSSPBMK-UHFFFAOYSA-M 0.000 abstract description 14
- 239000000126 substance Substances 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 238000010189 synthetic method Methods 0.000 abstract description 5
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 239000010815 organic waste Substances 0.000 abstract description 3
- 238000004065 wastewater treatment Methods 0.000 abstract description 3
- 150000001786 chalcogen compounds Chemical class 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 9
- 238000011160 research Methods 0.000 description 7
- 239000011941 photocatalyst Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 150000004770 chalcogenides Chemical class 0.000 description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- -1 Methylene Chemical group 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The present invention relates to a kind of novel visible degradation of methylene blue photochemical catalyst α EuZrS3And its synthetic method, the crystal-chemical formula are EuZrS3, the crystal is α phases, and apparent is black powder, is club shaped structure under microscope.The photochemical catalyst α EuZrS of the present invention3, can have preferable photocatalytic activity under sunlight or visible light conditions, in λ>Photocatalytic activity is more preferable under the visible light of 420nm, can be applied to Organic Waste Water Treatment.Synthetic method of the present invention and experimental procedure are simple, directly can largely synthesize pure phase.α‑EuZrS3There is the photocatalytic effect of excellent decomposition methylene blue in visible region, with it has been reported that multi-element metal chalcogen compound crystal Ba2AsGaSe5,Dy4S4Te3Deng compared to excellent visible light catalysis activity.
Description
Technical field
The present invention relates to a kind of photochemical catalyst and preparation method thereof with Visible Light Induced Photocatalytic methylene blue photocatalytic activity,
More particularly to a kind of novel chalcogen visible-light photocatalyst α-EuZrS3And its synthetic method, belong to catalysis material technology neck
Domain.
Background technology
Solar energy is widely noticed as a kind of energy of clean and effective, for solar energy utilization now there are many realize
Approach, and photocatalysis technology is exactly a kind of efficient and promising method, it is in photocatalysis Decomposition organic pollution and photocatalysis
It is dual in terms of economic development and environment protection that the research of splitting water hydrogen making etc. can alleviate world energy sources structure
Pressure.
The opportunity that photocatalysis research is risen is derived from 1972, and Japanese Scientists Honda and Fujishima are in n-type semiconductor
TiO2The photoelectrocatalysis decomposition of water is found that on electrode, the prelude of photocatalysis technology research has been opened in this discovery.From this,
Multiphase photocatalysis research enters new developing stage, chemist and material supply section scholars and is carried out to the photocatalysis performance of different materials
Extensively, in-depth study.Current usable photochemical catalyst is very limited, is only limitted to TiO2, nano-ZnO, Fe2O3、WO3、
The a few materials such as CdS, ZnS.The work of present researchers is concentrated mainly on two aspects, or to traditional photochemical catalyst
It is modified doping, or the photochemical catalyst of design synthesizing new.Wherein CdS, BIIIn2S4(BII=Zn, Cd) and AI 2-BII-
QIV-S4(AIFor Cu or Ag；BIIFor divalent transition metal element；QIVFor Ge or Sn) etc. chalcogenide materials photocatalysis research
Very much, but seldom the chalcogen photochemical catalyst of new construction type is developed in concern.Currently, only only a few multi-element metal chalcogenide
Object crystal has photocatalytic activity, such as Dy4S4Te3And Ba2AsGaSe5, but both crystal only reported them ultraviolet
Photocatalytic activity under the conditions of light, and our crystal has preferable visible light photocatalysis active.
Currently, the scholar of research photochemical catalyst is essentially all to be carried out on the basis of existing photocatalyst material both at home and abroad
Various forms of modifications, and rarely have the photocatalyst material of exploitation brand new.Developing completely new catalysis material not only can be with
Expand the research system of photochemical catalyst, moreover it is possible to be better understood between the catalytic performance of photochemical catalyst and their crystal structure
Relationship more examples are provided.Therefore, a kind of novel chalcogen catalysis material of the synthesis of simple and quick low cost has important
Meaning.
Invention content
An object of the present invention is to provide a kind of novel inorganic with Visible Light Induced Photocatalytic methylene blue photocatalytic activity
Chalcogen crystal, the crystal-chemical formula are EuZrS3, the crystal is α phases, and apparent is black powder, is rodlike knot under microscope
Structure, the crystal have preferable photocatalytic activity in visible light region.
The present invention also provides novel chalcogen visible-light photocatalyst α-EuZrS3Synthetic method, it is characterised in that：Synthesis
Steps are as follows：
(1) reactant Eu2O3,ZrO2, S and B are according to molar ratio 1:2:6:5 feed intake, and add KI as fluxing agent,
All substances are ground to fine powder in the agate mortar, are pressed into sheet；
(2) above-mentioned sheet drug is packed into quartz ampoule, access vacuum system is melted quartz ampoule with oxyhydrogen flame after vacuumizing and sealed
Mouthful；
(3) quartz ampoule of tablet is transferred to Muffle furnace Program temperature control above-mentioned envelope；
(4) quartz ampoule is opened in draught cupboard and take out reactant, wash filtering 3-5 times repeatedly with deionized water, it is naturally dry
It is dry, obtain black rhabdolith α-EuZrS3。
Reactant Eu described in step (1)2O3,ZrO2, the mass ratio of the gross mass and KI of S and B is 5:4.
The effective vacuum system of quartz described in step (2) is vacuumized up to 1 × 10–4Support.
Temperature programmed control described in step (3) is as follows：5 hours are heated to 300 DEG C from room temperature, keep the temperature 5 hours, then use
It is heated to 650 DEG C within 5 hours, then keeps the temperature 5 hours, be then heated to 950 DEG C with 5 hours again, 10 days are kept the temperature, finally with 5 days
Time cools to 300 DEG C, EP (end of program), cooled to room temperature.
The present invention also provides novel chalcogen visible-light photocatalyst α-EuZrS3Test method：
Rod-like samples α-EuZrS3Photocatalytic activity by decomposing methylene under simulated solar irradiation or visible light conditions
Base indigo plant is assessed；
Before illumination, reactant first continuously stirs 30 minutes in the dark with catalyst, is taken off so that it establishes absorption-
Attached balance is not observed methylene blue count after the stirring in 30 minutes carried out under dark condition and significantly reduces, explanation
α-EuZrS3There is no suction-operated to methylene blue, under the irradiation of visible light or simulated solar irradiation, α-EuZrS3Crystal is effective
Ground reduces the concentration of methylene blue, in λ>Photocatalytic activity is more preferable under the visible light of 420nm.
The present invention provides novel chalcogen visible-light photocatalyst α-EuZrS3In the application of photocatalysis field, the crystal is can
Light-exposed region has preferable photocatalytic activity, can be applied to Organic Waste Water Treatment.
Advantageous effect of the present invention is：
(1) photochemical catalyst α-EuZrS of the invention3, can have preferable light under sunlight or visible light conditions
Catalytic activity, in λ>Photocatalytic activity is more preferable under the visible light of 420nm, can be applied to Organic Waste Water Treatment.
(2) synthetic method and experimental procedure are simple, directly can largely synthesize pure phase.
(3)α-EuZrS3There is the photocatalytic effect of excellent decomposition methylene blue in visible region, with it has been reported that
Multi-element metal chalcogen compound crystal Ba2AsGaSe5,Dy4S4Te3Deng compared to excellent visible light catalysis activity.
Description of the drawings
Fig. 1 is α-EuZrS3The electron scanning micrograph of crystal.
Fig. 2 is a-EuZrS3The X-ray powder diffraction figure of crystal, draw above spectrum is experimental data, and collection of illustrative plates below is
Analogue data.
Fig. 3 is with the α-EuZrS prepared3Crystal photocatalytic degradation methylene under the irradiation of visible light and simulated solar irradiation
Blue effect contrast figure.
Specific implementation mode
The present invention is further explained in the light of specific embodiments.
(1)α-EuZrS3The preparation of crystal.
α-EuZrS3Monocrystalline is that KI is used to pass through solid state reaction kinetics as fluxing agent.All reactants are using general logical
Standard is not purified further.Reactant Eu2O3(99.99%), ZrO2(99.99), S (99.999%) and B
(99%) according to molar ratio 1:2:6:5 feed intake.Eu is weighed respectively with electronic balance2O3(208.3mg),ZrO2(145.9mg),S
(113.9mg) and B (32.0mg) adds 400mg KI (99%, dry in advance) and is used as fluxing agent, by all substances in agate
It is ground to fine powder in mortar, sheet is pressed into tablet press machine.Drug is fitted into the quartz ampoule of an end closure (outer diameter 13mm, thickness
Spend 1mm), access vacuum system is evacuated down to up to 1 × 10–4Support melts quartzy channel closure with oxyhydrogen flame at that time.Tablet will be sealed
Quartz ampoule is transferred to Muffle furnace Program temperature control, is heated to 300 DEG C from room temperature with 5 hours, 5 hours is kept the temperature, then with 5 hours
650 DEG C are heated to, then keeps the temperature 5 hours, is then heated to 950 DEG C with 5 hours again, keeps the temperature 10 days, was finally cooled down with 5 day time
Cool to 300 DEG C, EP (end of program), cooled to room temperature.Quartz ampoule is opened in draught cupboard and takes out reactant, uses deionized water
Washing filtering 3-5 times repeatedly, spontaneously dries, obtains black rhabdolith α-EuZrS3。
α-the EuZrS of preparation are observed by scanning electron microscope (SEM)3Form is as shown in the figure (Fig. 1).It can be seen that owning
α-EuZrS3What monocrystal was all bar-like, diameter is about in 150-200nm, but its length difference is larger, from hundreds of nanometers to
Grade has.Suitable single crystal body progress X-ray single crystal diffraction is chosen under an optical microscope and parses data finally confirms crystalline substance
Body chemical formula is EuZrS3, α phases, rhombic system, Pnma space groups, cell parameter be a=8.465 (3), b=3.808 (1),
The standard spectrogram comparison of the X-ray powder diffraction figure (PXRD) of gained sample and single crystal data simulation is found into the sample
Product diffraction maximum is narrow and strong, without apparent miscellaneous peak, shows that sample is pure phase (Fig. 2).
(2) to the α-EuZrS of preparation3Crystal carries out photocatalytic activity test.
Sample α-the EuZrS of preparation3Photocatalytic activity pass through in simulated solar irradiation and visible light (λ>Under the conditions of 420nm)
Methylene blue is decomposed to be assessed.Before illumination, reactant first continuously stirs 30 minutes in the dark, it is made to establish absorption-
Desorption equilibrium.Methylene blue count is not observed after stirring significantly to change, illustrates α-EuZrS3Methylene blue is not inhaled
Attached effect.Using the decrement of methylene blue as the longitudinal axis, it is seen that light or simulated solar irradiation light application time are done horizontal axis mapping and shown
α-EuZrS3Crystal possesses photocatalytic activity (Fig. 3).Under the irradiation of visible light or simulated solar irradiation, α-EuZrS3Crystal can
To be effectively reduced the concentration of methylene blue, and its photocatalytic activity is more preferable under visible light.In simulated solar irradiation and visible light
After the lower stirring of irradiation 100 minutes, the concentration of methylene blue reduces 75.9% and 69.8% respectively.
The above is only presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, any ripe
Professional and technical personnel is known, without departing from the scope of the present invention, according to the technical essence of the invention, to above real
Apply any simple modification, equivalent replacement and improvement etc. made by example, still fall within technical solution of the present invention protection domain it
It is interior.
Claims (6)
1. a kind of inorganic chalcogen crystal with visible light photocatalysis active degradation of methylene blue, it is characterised in that：The crystallization
Formula is EuZrS3, the crystal is α phases, and apparent is black powder, is club shaped structure under microscope, the crystal is in visible light
Region has preferable photocatalytic activity；Its synthesis step is as follows：
(1) reactant Eu2O3,ZrO2, S and B are according to molar ratio 1:2:6:5 feed intake, and add KI as fluxing agent, by property
Matter is ground to fine powder in the agate mortar, is pressed into sheet；
(2) above-mentioned sheet drug is packed into quartz ampoule, accesses after vacuum system vacuumizes and melts quartzy channel closure with oxyhydrogen flame；
(3) quartz ampoule of tablet is transferred to Muffle furnace Program temperature control above-mentioned envelope；
(4) quartz ampoule is opened in draught cupboard and take out reactant, wash filtering 3-5 times repeatedly with deionized water, spontaneously dry, obtain
To black rhabdolith α-EuZrS3。
2. the inorganic chalcogen crystal with visible light photocatalysis active degradation of methylene blue as described in claim 1, feature
It is：Reactant Eu described in step (1)2O3,ZrO2, the mass ratio of the gross mass and KI of S and B is 5:4.
3. the inorganic chalcogen crystal with visible light photocatalysis active degradation of methylene blue as described in claim 1, feature
It is：The effective vacuum system of quartz described in step (2) is vacuumized up to 1 × 10–4Support.
4. the inorganic chalcogen crystal with visible light photocatalysis active degradation of methylene blue as described in claim 1, feature
It is：Temperature programmed control described in step (3) is as follows：5 hours are heated to 300 DEG C from room temperature, keep the temperature 5 hours, then small with 5
When be heated to 650 DEG C, then keep the temperature 5 hours, be then heated to 950 DEG C with 5 hours again, keep the temperature 10 days, it is finally cold with 5 day time
But 300 DEG C are cooled to, EP (end of program), cooled to room temperature.
5. the crystal test side of the inorganic chalcogen described in claim 1 with visible light photocatalysis active degradation of methylene blue
Method, it is characterised in that：
Rod-like samples α-EuZrS3Photocatalytic activity by under simulated solar irradiation or visible light conditions decompose methylene blue into
Row assessment；
Before illumination, reactant methylene blue and catalyst α-EuZrS3It first continuously stirs in the dark 30 minutes, so that it is built
Vertical absorption-desorption equilibrium, it is significant to be not observed methylene blue count after the stirring in 30 minutes carried out under dark condition
It reduces, illustrates α-EuZrS3There is no suction-operated to methylene blue, under the irradiation of visible light or simulated solar irradiation, α-
EuZrS3Crystal is effectively reduced the concentration of methylene blue, in λ>Photocatalytic activity is more preferable under the visible light of 420nm.
6. the inorganic chalcogen crystal described in claim 1 with visible light photocatalysis active degradation of methylene blue is led in photocatalysis
The application in domain, it is characterised in that：The crystal has preferable photocatalytic activity in visible light region, can be applied to organic pollution
It administers.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1952222A (en) * | 2005-10-20 | 2007-04-25 | 中国科学院福建物质结构研究所 | Method for growth of sulfide crystal containing alkali metal, gallium or indium |
| CN103055899A (en) * | 2012-12-10 | 2013-04-24 | 上海师范大学 | Mesoporous nano spheroidal ZnxCd1-xS particle and preparation method and application thereof |
| CN104846428A (en) * | 2015-04-13 | 2015-08-19 | 山东大学 | Method used for growth of transition metal chalcogenide crystals via metal fluxing agent method |
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| US7393516B2 (en) * | 2003-01-31 | 2008-07-01 | Seo Dong-Kyun | Preparation of metal chalcogenides from reactions of metal compounds and chalcogen |
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| CN1952222A (en) * | 2005-10-20 | 2007-04-25 | 中国科学院福建物质结构研究所 | Method for growth of sulfide crystal containing alkali metal, gallium or indium |
| CN103055899A (en) * | 2012-12-10 | 2013-04-24 | 上海师范大学 | Mesoporous nano spheroidal ZnxCd1-xS particle and preparation method and application thereof |
| CN104846428A (en) * | 2015-04-13 | 2015-08-19 | 山东大学 | Method used for growth of transition metal chalcogenide crystals via metal fluxing agent method |
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