CN104923261A - Method for prolonging service life of CdS nano photocatalyst - Google Patents
Method for prolonging service life of CdS nano photocatalyst Download PDFInfo
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- CN104923261A CN104923261A CN201510246053.6A CN201510246053A CN104923261A CN 104923261 A CN104923261 A CN 104923261A CN 201510246053 A CN201510246053 A CN 201510246053A CN 104923261 A CN104923261 A CN 104923261A
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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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
Abstract
The invention provides a method for prolonging the service life of a CdS nano photocatalyst. The method is characterized by depositing a layer of 1-10 A as protective layer (TiO2, ZnO, Al2O3, AZO, and the like) on the surface of a CdS nano particle synthesized hydrothermally by virtue of an atomic layer deposition technique. On the premise of guaranteeing relatively a high catalytic efficiency, light corrosion occurrence is effectively reduced, and therefore the service life CdS nano photocatalyst is prolonged from 1 hour to over 18 hour. The preparation method effectively reduces the harm to the light CdS nano particle and prolongs the catalyst life of the CdS nano particle.
Description
Technical field
The present invention relates to a kind of method extending the CdS nano-photocatalyst life-span.
Background technology
Nano semiconductor photochemical catalyst is a kind of semiconductor catalyst of nanoscale, usually be prepared from by various physics or chemical method by the oxide of some narrow band gaps or sulfide, its advantage is not need extra energy, only need to absorb sunshine and just can realize photocatalysis, decomposition water produces the organic matter in hydrogen and Decomposition Wastewater, the environmental problem that the current mankind of effective solution face and energy problem.
Current research the most widely Nano semiconductor catalyst is the TiO of yardstick at about 25nm
2(P25), but due to TiO
2band gap width be 3.2eV, this just means that it can only absorb the ultraviolet band accounting for solar spectrum 5%, so just greatly reduces its catalytic efficiency.People by doping various metal and nonmetalloid to TiO
2band gap regulate, its band gap is narrowed, improves its absorption efficiency to visible ray.But mix impurity, while reduction band gap, have also been introduced more complex centre, add the recombination probability of photo-generated carrier, be unfavorable for the raising of photocatalysis efficiency.
Meanwhile, in order to more sunshine can be absorbed, improve photocatalysis efficiency, compare TiO
2narrower some semiconductors of band gap receive to be paid close attention to widely and payes attention to.Such as WO
3, Fe
2o
3deng.But photocatalysis performance, is not only decided by the band gap width of semiconductor, also relevant with the relative position of hydrogen-oxygen energy level in the solution with semiconductor energy gap.WO
3, Fe
2o
3deng material because conduction band positions is higher than product Hydrogen Energy level, so can not produce hydrogen under illumination condition, can only form hetero-junctions with other semi-conducting material could meet the condition producing hydrogen, which increases the difficulty of materials synthesis and the complexity of technique.
CdS (cadmium sulfide) is as a kind of oxidation-reduction type semiconductor, and compared with other oxidation-reduction type semiconductor, have more suitable valence band conduction band positions, relative to titanium dioxide, its reduction potential is enough negative, and reducing power is stronger.Cadmium sulfide is the catalysis of a kind of II-VI group semiconductor, and band gap is 2.4eV, is a kind of narrow gap semiconductor, and compared with this semiconductor that can only be excited in UV light region of titanium dioxide, cadmium sulfide can be absorbed in solar spectrum the visible ray accounting for the overwhelming majority.And cadmium sulfide is direct band-gap semicondictor, can directly transition between energy level, further increase the absorptivity of visible ray.But cadmium sulfide also exists some inherent defects, such as, Zhang, J, Davis, A.P. etc. find that CdS easily photoetch occurs in photocatalytic process, significantly reduce its photocatalysis life-span.(M.J.Mater.Chem，2011，21，14655.；Water.Res.，1991，25，1273。)
The invention provides a kind of method extending the CdS nano-photocatalyst life-span, the method adopts technique for atomic layer deposition to deposited one deck respectively on the CdS nano grain surface of Hydrothermal Synthesis
protective layer.Under the prerequisite ensureing greater catalytic efficiency, the effective generation reducing photoetch, extended to more than 18 hours by the photocatalysis life-span of CdS nano particle from 1 hour.This preparation method effectively decreases the destruction of photoetch to CdS nano particle, extends the catalytic life of CdS nano particle.
Summary of the invention
The invention provides a kind of method extending the CdS nano-photo catalytic life-span, the method with the CdS nano particle of Hydrothermal Synthesis for matrix.Technique for atomic layer deposition is adopted to deposited one deck at CdS nano grain surface
protective layer (TiO
2, ZnO, Al
2o
3, AZO etc.).Under the prerequisite ensureing greater catalytic efficiency, the photocatalysis life-span of CdS nano particle was extended to more than 18 hours by 1 hour.It is characterized in that Hydrothermal Synthesis combines with technique for atomic layer deposition by preparation process.Described synthetic method concrete steps are as follows:
1) by cadmium acetate, thiocarbamide, neopelex and ammoniacal liquor make solution 1 in molar ratio at 5: 15: 1: 40.A certain amount of CdS and deionized water are made precursor solution 2.By both with 1: 4 ratio fully mix;
2) mixed solution of step 1 is added in hydrothermal reaction kettle, in baking oven, be heated to 120 DEG C, keep 2 hours, then naturally cool;
3) reacted suspension step 2 obtained carries out centrifugal, the solid matter deionized water obtained after centrifugal is carried out ultrasonic cleaning, repeatedly several times;
4) solid matter that step 3 obtains is put into drying box, bone dry, obtain Nano cadmium sulphide powder;
5) cadmium sulfide powder step 4 obtained is sent in ald vacuum chamber, carries out the protective layer needed for ald;
6) sample step 5 obtained, gets 40mg, and pouring 100mL concentration into is in the methylene blue solution of 10mg/L, Keep agitation, after adsorption equilibrium in half an hour, carries out photocatalysis experiment under being placed on analog solar light.
The invention provides a kind of method extending the CdS photocatalysis life-span, it is characterized in that Hydrothermal Synthesis combines with technique for atomic layer deposition by preparation process.Wherein, first step Hydrothermal Synthesis, simple to operate, with the method can prepare effluent mutually evenly, purity is high, crystal formation good, single dispersing, shape and size are controlled nanoparticle; Second step ald protective layer, the ingenious advantage utilizing technique for atomic layer deposition can carry out Atomic layer deposition, at CdS surface deposition layer protective layer (TiO
2, ZnO, Al
2o
3aZO etc.); electronics is utilized then to wear principle; make photo-generated carrier can arrive surface and solution haptoreaction by protective layer; reach catalysis object; prevent again because the hydroxyl of the strong oxidizing property of light-catalyzed reaction generation directly contacts with CdS surface in solution, generation photoetch, significantly extends the life-span of catalyst simultaneously.As shown in Figure 1; what the feature of this method was to utilize CdS photoetch is from its catalytic activity point; and first the high activity of its active site can be beneficial in the process utilizing ald; first the protective layer deposited is grown up on active site, and this growth pattern can make only growing
when protective layer; just can protect the active site on CdS surface completely; photoetch is stoped to occur; ultra-thin protective layer makes photo-generated carrier be easy to occur then to wear simultaneously; arrive protective layer and liquid comes into contact and then catalysis occurs and occur; this guarantees the high catalytic activity of catalyst, the photocatalysis life-span of CdS nano particle can be extended to more than 18 hours by 1 hour by the method, saw Fig. 2.
Accompanying drawing explanation
Fig. 1 is that this method is at CdS outside deposition TiO
2schematic diagram.
Fig. 2 is coated
tiO
2the curve of the CdS photocatalytic degradation methylene blue of front and back.
Detailed description of the invention
Below will the present invention is further illustrated by specific embodiment.
Embodiment 1
1) by the cadmium acetate of 0.025mol, the thiocarbamide of 0.075mol, and the neopelex of 0.005mol and 0.2mol ammoniacal liquor make the 10ml aqueous solution.0.002mol CdS and 40ml deionized water are made presoma.Both are poured in 50mL polytetrafluoroethylene (PTFE) cover and fully mix; Mixed solution and polytetrafluoroethylene (PTFE) cover are put into 50ml stainless steel hydrothermal reaction kettle, then hydrothermal reaction kettle is put into baking oven, be heated to 120 DEG C, keep 2 hours, then naturally cool; The suspension that obtains after reaction is carried out centrifugal, the solid matter deionized water obtained after centrifugal is carried out ultrasonic cleaning, 5 times repeatedly; By cleaning the solid matter that obtains at 70 DEG C of temperature dry 12 hours, obtain Nano cadmium sulphide powder; The cadmium sulfide powder obtained by Hydrothermal Synthesis is sent in ald vacuum chamber, carries out the ald of required protective layer.When vacuum arrives requirement of experiment, pass into presoma: four diaminourea first titanium and water, the presoma burst length is 50ms, in preparation process, with high-purity argon gas (99.999%) for carrier gas, carrier gas flux: 20sccm, reaction temperature 150 DEG C, reaction time 25s, presoma scavenging period is 25s, goes out in CdS superficial growth
tiO
2.Get the sample that 40mg is obtained, pouring 100mL concentration into is in the methylene blue solution of 10mg/L, Keep agitation, after adsorption equilibrium in half an hour, carries out photocatalysis experiment under being placed on analog solar light.The absorption intensity using visible ultraviolet-uisible spectrophotometer to test methylene blue changes over time, measures the palliating degradation degree of methylene blue with this.
Embodiment 2
1) by the cadmium acetate of 0.025mol, the thiocarbamide of 0.075mol, and the neopelex of 0.005mol and 0.2mol ammoniacal liquor make the 10ml aqueous solution.0.002mol CdS and 40ml deionized water are made presoma.Both are poured in 50ml polytetrafluoroethylene (PTFE) cover and fully mix; Mixed solution and polytetrafluoroethylene (PTFE) cover are put into 50ml stainless steel hydrothermal reaction kettle, then hydrothermal reaction kettle is put into baking oven, be heated to 120 DEG C, keep 2 hours, then naturally cool; The suspension that obtains after reaction is carried out centrifugal, the solid matter deionized water obtained after centrifugal is carried out ultrasonic cleaning, 5 times repeatedly; By cleaning the solid matter that obtains at 70 DEG C of temperature dry 12 hours, obtain Nano cadmium sulphide powder; The cadmium sulfide powder obtained by Hydrothermal Synthesis is sent in ald vacuum chamber, carries out the ald of required protective layer.When vacuum arrives requirement of experiment, pass into presoma: diethyl zinc and water, the presoma burst length is 20ms, in preparation process, with high-purity argon gas (99.999%) for carrier gas, carrier gas flux: 20sccm, reaction temperature is 150 DEG C, reaction time 25s, presoma scavenging period is 20s, goes out in CdS superficial growth
znO.Get the sample that 40mg is obtained, pouring 100mL concentration into is in the methylene blue solution of 10mg/L, Keep agitation, after adsorption equilibrium in half an hour, carries out photocatalysis experiment under being placed on analog solar light.Use visible ultraviolet-uisible spectrophotometer to test the change of the absorption intensity of methylene blue, measure the palliating degradation degree of methylene blue with this.
Embodiment 3
1) by the cadmium acetate of 0.025mol, the thiocarbamide of 0.075mol, and the neopelex of 0.005mol and 0.2mol ammoniacal liquor make the 10ml aqueous solution.0.002mol CdS and 40ml deionized water are made presoma.Both are poured in 50ml polytetrafluoroethylene (PTFE) cover and fully mix; Mixed solution and polytetrafluoroethylene (PTFE) cover are put into 50ml stainless steel hydrothermal reaction kettle, then hydrothermal reaction kettle is put into baking oven, be heated to 120 DEG C, keep 2 hours, then naturally cool; The suspension that obtains after reaction is carried out centrifugal, the solid matter deionized water obtained after centrifugal is carried out ultrasonic cleaning, 5 times repeatedly; By cleaning the solid matter that obtains at 70 DEG C of temperature dry 12 hours, obtain Nano cadmium sulphide powder; The cadmium sulfide powder obtained by Hydrothermal Synthesis is sent in ald vacuum chamber, carries out the ald of required protective layer.When vacuum arrives requirement of experiment, pass into presoma: trimethyl aluminium and water, the presoma burst length is 20ms, in preparation process, with high-purity argon gas (99.999%) for carrier gas, carrier gas flux: 20sccm, reaction temperature 150 DEG C, reaction time 25s, presoma scavenging period is 20s, goes out in CdS superficial growth
al
2o
3.Get the sample that 40mg is obtained, pouring 100mL concentration into is in the methylene blue solution of 10mg/L, Keep agitation, after adsorption equilibrium in half an hour, carries out photocatalysis experiment under being placed on analog solar light.Use visible ultraviolet-uisible spectrophotometer to test the change of the absorption intensity of methylene blue, measure the palliating degradation degree of methylene blue with this.
Embodiment 4
1) by the cadmium acetate of 0.025mol, the thiocarbamide of 0.075mol, and the neopelex of 0.005mol and 0.2mol ammoniacal liquor make the 10ml aqueous solution.0.002mol CdS and 40ml deionized water are made presoma.Both are poured in 50ml polytetrafluoroethylene (PTFE) cover and fully mix; Mixed solution and polytetrafluoroethylene (PTFE) cover are put into 50ml stainless steel hydrothermal reaction kettle, then hydrothermal reaction kettle is put into baking oven, be heated to 120 DEG C, keep 2 hours, then naturally cool; The suspension that obtains after reaction is carried out centrifugal, the solid matter deionized water obtained after centrifugal is carried out ultrasonic cleaning, 5 times repeatedly; By cleaning the solid matter that obtains at 70 DEG C of temperature dry 12 hours, obtain Nano cadmium sulphide powder; The cadmium sulfide powder obtained by Hydrothermal Synthesis is sent in ald vacuum chamber, carries out the ald of required protective layer.When vacuum arrives requirement of experiment, pass into presoma: diethyl zinc and water, the presoma burst length is 20ms, in preparation process, with high-purity argon gas (99.999%) for carrier gas, carrier gas flux: 20sccm, reaction temperature is 150 DEG C, reaction time 25s, presoma scavenging period is 20s.And then with trimethyl aluminium and water as presoma, the presoma burst length is 20ms, with high-purity argon gas (99.999%) for carrier gas, carrier gas flux: 20sccm, reaction temperature is 150 DEG C, reaction time 25s, presoma scavenging period is 20s, goes out in CdS superficial growth
aZO.Get the sample that 40mg is obtained, pouring 100mL concentration into is in the methylene blue solution of 10mg/L, Keep agitation, after adsorption equilibrium in half an hour, carries out photocatalysis experiment under being placed on analog solar light.Use visible ultraviolet-uisible spectrophotometer to test the change of the absorption intensity of methylene blue, measure the palliating degradation degree of methylene blue with this.
Claims (6)
1. one kind extends the method in CdS nano-photocatalyst life-span; it is characterized in that the surface of the nano-tube/CdS particle at Hydrothermal Synthesis; ultra-thin protective layer (the TiO of one deck is deposited by technique for atomic layer deposition (Atomic Layer Deposition, ALD)
2, ZnO, Al
2o
3, AZO etc.), prepare a kind of CdS nano-photocatalyst at Surface coating matcoveredn, the CdS particle size size after coated protective layer is between 10-50nm, and protective layer thickness exists
between, this novel photocatalysis material under the maintenance greater catalytic efficiency prerequisite, the significant prolongation catalytic life of CdS nano-photocatalyst.
2. the method extending the CdS nano-photocatalyst life-span as claimed in claim 1, it is characterized in that hydrothermal synthesis method and technique for atomic layer deposition to combine, concrete steps are as follows:
1) by cadmium acetate, thiocarbamide, neopelex and ammoniacal liquor make solution 1 in molar ratio at 5: 15: 1: 40.A certain amount of CdS and deionized water are made precursor solution 2.By both with 1: 4 ratio fully mix;
2) by step 1) mixed solution add in hydrothermal reaction kettle, in baking oven, be heated to 120 DEG C, keep more than 1 hour, then naturally cool;
3) by step 2) in the reacted suspension that obtains carry out centrifugal, the solid matter deionized water obtained after centrifugal is carried out ultrasonic cleaning and centrifugal, repeatedly several times;
4) by step 3) solid matter that obtains puts into drying box, bone dry, obtains Nano cadmium sulphide powder;
5) by step 4) the cadmium sulfide powder that obtains sends in ald vacuum chamber, carries out the protective layer needed for ald;
6) by step 5) sample that obtains, get 40mg, pouring 100mL concentration into is in the methylene blue solution of 10mg/L, Keep agitation, after adsorption equilibrium in half an hour, carries out photocatalysis experiment under being placed on simulated solar irradiation.
3. the method extending the CdS nano-photocatalyst life-span as claimed in claim 1, is characterized in that the TiO using Atomic layer deposition method (ALD) to deposit
2time, using organic titanium and water as presoma, the presoma burst length is greater than 5ms, in preparation process, with high pure nitrogen or argon gas for carrier, carrier gas flux is kept to be greater than 10sccm, reaction temperature is greater than 50 DEG C, and be less than 400 DEG C, the reaction time is greater than 1s, presoma scavenging period is greater than 3s, goes out in CdS superficial growth
tiO
2.Repeat that this preparation process 1-10 is secondary to be grown
tiO
2protective layer.
4. the method extending the CdS nano-photocatalyst life-span as claimed in claim 1, when it is characterized in that the ZnO using Atomic layer deposition method deposition, using organic zinc and water as presoma, the presoma burst length is greater than 5ms, in preparation process, with high pure nitrogen or argon gas for carrier, keep carrier gas flux to be greater than 10sccm, reaction temperature is greater than 50 DEG C, be less than 400 DEG C, reaction time is greater than 1s, and presoma scavenging period is greater than 3s, goes out in CdS superficial growth
znO.Repeat that this preparation process 1-10 is secondary to be grown
znO protective layer.
5. the method extending the CdS nano-photocatalyst life-span as claimed in claim 1, is characterized in that the Al using Atomic layer deposition method deposition
2o
3time, using organo-aluminium and water as presoma, the presoma burst length is greater than 5ms, in preparation process, with high pure nitrogen or argon gas for carrier, carrier gas flux is kept to be greater than 10sccm, reaction temperature is greater than 50 DEG C, and be less than 400 DEG C, the reaction time is greater than 1s, presoma scavenging period is greater than 3s, goes out in CdS superficial growth
al
2o
3.Repeat that this preparation process 1-10 is secondary to be grown
al
2o
3protective layer.
6. the method extending the CdS nano-photocatalyst life-span as claimed in claim 1, when it is characterized in that the AZO using Atomic layer deposition method deposition, using organic zinc and water as presoma, the presoma burst length is greater than 5ms, in preparation process, with high pure nitrogen or argon gas for carrier, keep carrier gas flux to be greater than 10sccm, reaction temperature is greater than 50 DEG C, is less than 400 DEG C, reaction time is greater than 1s, and presoma scavenging period is greater than 3s; And then with the metal precursor of aluminium and water as presoma, the presoma burst length is greater than 5ms, in preparation process, with high pure nitrogen or argon gas for carrier, keep carrier gas flux to be greater than 10sccm, reaction temperature is greater than 50 DEG C, be less than 400 DEG C, reaction time is greater than 1s, and presoma scavenging period is greater than 3s, goes out in CdS superficial growth
aZO.Repeat that this preparation process 1-5 is secondary to be grown
aZO protective layer.
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| CN105498802A (en) * | 2015-12-04 | 2016-04-20 | 福州大学 | ZnO-Au-CdS ternary composite photocatalyst |
| CN108421423A (en) * | 2018-04-04 | 2018-08-21 | 东莞市石鼓污水处理有限公司 | A kind of preparation method of photocatalysis sewage processing composite membrane |
| CN109876828A (en) * | 2019-01-29 | 2019-06-14 | 浙江大学 | A kind of TNT/CdS/TiO2/ Pt nuclear shell structure nano pipe and preparation method thereof |
| KR20200086182A (en) * | 2019-01-08 | 2020-07-16 | 재단법인 하이브리드 인터페이스기반 미래소재 연구단 | Manufacturing method of Thin Film Passivation Layer by Atomic Layer Deposition for Improving the Durability of Metal Catalyst |
| CN112777565A (en) * | 2019-11-05 | 2021-05-11 | 中国科学院大连化学物理研究所 | Semiconductor photocatalytic water splitting method capable of inhibiting reverse reaction |
| CN113856760A (en) * | 2021-09-23 | 2021-12-31 | 杭州师范大学 | MOF-NO2TiO under confinement2Nano composite photocatalyst and preparation method thereof |
| CN114042476A (en) * | 2021-11-15 | 2022-02-15 | 杭州师范大学 | MOF-TiO2Preparation method of graphene quantum dot nano composite photocatalyst |
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|---|---|---|---|---|
| CN105498802A (en) * | 2015-12-04 | 2016-04-20 | 福州大学 | ZnO-Au-CdS ternary composite photocatalyst |
| CN105498802B (en) * | 2015-12-04 | 2017-12-08 | 福州大学 | A kind of zinc oxide gold cadmium sulfide ternary composite type photochemical catalyst |
| CN108421423A (en) * | 2018-04-04 | 2018-08-21 | 东莞市石鼓污水处理有限公司 | A kind of preparation method of photocatalysis sewage processing composite membrane |
| KR20200086182A (en) * | 2019-01-08 | 2020-07-16 | 재단법인 하이브리드 인터페이스기반 미래소재 연구단 | Manufacturing method of Thin Film Passivation Layer by Atomic Layer Deposition for Improving the Durability of Metal Catalyst |
| KR102216361B1 (en) * | 2019-01-08 | 2021-02-16 | 재단법인 하이브리드 인터페이스기반 미래소재 연구단 | Manufacturing method of Thin Film Passivation Layer by Atomic Layer Deposition for Improving the Durability of Metal Catalyst |
| CN109876828A (en) * | 2019-01-29 | 2019-06-14 | 浙江大学 | A kind of TNT/CdS/TiO2/ Pt nuclear shell structure nano pipe and preparation method thereof |
| CN109876828B (en) * | 2019-01-29 | 2020-06-23 | 浙江大学 | TNT/CdS/TiO2Pt core-shell structure nanotube and preparation method thereof |
| CN112777565A (en) * | 2019-11-05 | 2021-05-11 | 中国科学院大连化学物理研究所 | Semiconductor photocatalytic water splitting method capable of inhibiting reverse reaction |
| CN112777565B (en) * | 2019-11-05 | 2022-11-22 | 中国科学院大连化学物理研究所 | Semiconductor photocatalytic water splitting method capable of inhibiting reverse reaction |
| CN113856760A (en) * | 2021-09-23 | 2021-12-31 | 杭州师范大学 | MOF-NO2TiO under confinement2Nano composite photocatalyst and preparation method thereof |
| CN114042476A (en) * | 2021-11-15 | 2022-02-15 | 杭州师范大学 | MOF-TiO2Preparation method of graphene quantum dot nano composite photocatalyst |
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Application publication date: 20150923 |