CN104056644B - A kind of ZnO/ZnSe nano material, preparation method and application thereof - Google Patents
A kind of ZnO/ZnSe nano material, preparation method and application thereof Download PDFInfo
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- CN104056644B CN104056644B CN201410348485.3A CN201410348485A CN104056644B CN 104056644 B CN104056644 B CN 104056644B CN 201410348485 A CN201410348485 A CN 201410348485A CN 104056644 B CN104056644 B CN 104056644B
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- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 239000011701 zinc Substances 0.000 claims abstract description 19
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 27
- 239000008367 deionised water Substances 0.000 claims description 23
- 229910021641 deionized water Inorganic materials 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 15
- 229940043267 rhodamine b Drugs 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 230000001699 photocatalysis Effects 0.000 claims description 9
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 239000000975 dye Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 239000012456 homogeneous solution Substances 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical class [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 239000002135 nanosheet Substances 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000000758 substrate Substances 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 230000001351 cycling effect Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000003491 array Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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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 invention provides a kind of ZnO/ZnSe nano material, preparation method and application thereof.The present invention compared with prior art, has synthesized the heterogeneous array structure of ZnO/ZnSe nm wall by simple cryochemistry liquid phase conversion in zinc metal sheet substrate.ZnO/ZnSe nm wall provided by the invention heterogeneous array structure visible light catalyst has that catalytic activity is high, good cycling stability and technique is simple, cost is low advantage.
Description
Technical field
The invention belongs to nano-heterogeneous structure material preparation method and Environmental Chemistry cross-application field, be specifically related to a kind of photocatalysis ZnO/ZnSe nano-heterogeneous structure material preparations and applicatio field.
Background technology
Along with industrial expansion, dyestuff (from fabric, paper and other industry) residual in sewage becomes a source of environmental problem.Semiconductor is used to become the promising method of one of wastewater pollutants process as photochemical catalyst light auxiliary catalysis degradable organic pollutant.ZnO as a kind of important wide with gap and direct with gap semiconductor (the with gap of block ZnO is 3.37eV), electron mobility (205 ~ 300cm
2vs
-1) exceed TiO
2(0.1 – 4cm
2vs
-1), have catalytic efficiency high, the low and Environmental Sustainability of cost, is widely regarded as the very promising photochemical catalyst of one.But zno-based originally can only utilize ultraviolet light (only accounting for 3 ~ 5% of the solar spectrum reaching the earth), and can not utilize visible ray (accounting for 44 ~ 47% of solar spectrum).In addition, the right quick compound of the photo-generate electron-hole in ZnO photocatalytic process improves a major obstacle of its photocatalysis efficiency.Therefore, the key improving ZnO photocatalytic activity uses another material to modify ZnO surface to improve sunshine utilization ratio and to promote the separation that light produces electric charge.Being coupled that light absorption is extended to visible-range and reduces charge recombination tendency by narrow with gap semiconductor on the surface at ZnO is the very promising method of one.
ZnSe belongs to environmentally friendly narrow gap semiconductor, form ZnO/ZnSe nano-heterogeneous structure with ZnO and there is visible light catalysis activity, but the report of correlative study is at present less, still not about the synthesis of the heterogeneous array structure of ZnO/ZnSe nm wall and the report for visible light catalytic, therefore the heterogeneous array structure of ZnO/ZnSe nm wall is synthesized, for visible light photocatalytic degradation organic dyestuff, tool has very important significance.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of ZnO/ZnSe nano material and preparation method thereof, utilize cryochemistry liquid phase transformation approach, technique is simple, cost is low.
A further object of the invention, provides ZnO/ZnSe nano material to apply as the visible light photocatalytic degradation of organic dyestuff.
A kind of ZnO/ZnSe nano material provided by the invention, for the ZnO nano sheet of diameter 500nm adhering to the ZnSe nanometer sheet that size is 50nm.
The preparation method of a kind of ZnO/ZnSe nano material provided by the invention, comprises the following steps:
(1) 1,6-hexamethylene diamine is added in deionized water, stir, obtain solution A; Nine hydrated sodium sulfides are dissolved in solution A, obtain solution B, solution B being poured into polytetrafluoroethylene (PTFE) is in the stainless steel autoclave of liner, clean zinc metal sheet is placed on obliquely in this solution, add thermal response, after reaction terminates, naturally cool to room temperature, gray product on zinc metal sheet respectively cleans 3 times with deionized water and absolute ethyl alcohol respectively, then 50 DEG C of vacuum drying 6h;
(2) selenium powder is joined in the mixed solution of ammoniacal liquor and deionized water, continuous stirring forms homogeneous solution, add sodium borohydride, after continuing to stir 30min, the zinc metal sheet being coated with product of inserting step (1) gained, adds thermal response, after end, the zinc metal sheet deionized water and absolute ethyl alcohol that are coated with product are respectively cleaned 3 times, 50 DEG C of vacuum drying 6h, obtain the heterogeneous array structure of ZnO/ZnSe nm wall.
In step (1), the volume ratio of deionized water and 1,6-hexamethylene diamine is 19-7:1;
The concentration obtaining vulcanized sodium in solution B described in step (1) is 0.025-0.035mol/L;
Thermal response is added, temperature 120-150 DEG C, reaction time 8-10h described in step (1);
In step (2), the volume ratio of ammoniacal liquor used and deionized water is 0.6-1:1;
In step (2), the concentration of selenium powder in the mixed solution of ammoniacal liquor and deionized water is 0.003-0.005mol/L;
In step (2), the mol ratio 2-2.1:1 of sodium borohydride and selenium powder;
In step (2), described adds thermal response, temperature 60-90 DEG C, reaction time 5-8h;
The present invention also provides a kind of ZnO/ZnSe nano material as the photocatalytic applications of visible light photocatalytic degradation organic dyestuff rhodamine B (RhB).
The heterogeneous array structure sample of ZnO/ZnSe nm wall the present invention prepared is cut into 1 × 1.5cm size, and putting into 5mL concentration is 1.0 × 10
-5also stir 1h in the dark in the RhB solution of mol/L, make catalyst surface reach the attached balance of absorption-desorption.Afterwards, 300W xenon lamp is used to carry out radiation of visible light.Use ultraviolet-visible spectrophotometer (ShimadzuUV-2550) to measure the absorption spectrum of solution every 20min, determined the concentration of RhB by the characteristic absorption peak at 554nm place.
The present invention compared with prior art, by simple cryochemistry liquid phase transformation approach, forms novel ZnSe nano-sheet shell structurre, obtains the heterogeneous array structure of ZnO/ZnSe nm wall on the surface of ZnO nano chip arrays structure.Visible light catalyst for organic dyestuff rhodamine B photocatalytic degradation provided by the invention has that catalytic activity is high, good cycling stability and technique is simple, cost is low advantage.
Accompanying drawing explanation
Fig. 1 is X-ray powder diffraction (XRD) figure of ZnO/ZnSe nano material prepared by embodiment 1;
Fig. 2 is SEM (SEM) figure of ZnO/ZnSe nano material prepared by embodiment 1;
Fig. 3 is transmission electron microscope (TEM) figure of single ZnO/ZnSe nm wall in the ZnO/ZnSe nano material of embodiment 1 preparation;
Fig. 4 is high resolution transmission electron microscopy (HRTEM) figure of shell ZnSe nanometer sheet in the ZnO/ZnSe nano material of embodiment 1 preparation;
Fig. 5 is the ultra-violet absorption spectrum of embodiment 2ZnO/ZnSe nano material visible light photocatalytic degradation RhB;
Fig. 6 is the concentration changes with time curve of embodiment 2ZnO/ZnSe nano material and ZnO nano chip arrays visible light photocatalytic degradation RhB.
Detailed description of the invention
Embodiment 1
A preparation method for ZnO/ZnSe nano material, comprises the following steps:
(1) 1, the 6-hexamethylene diamine of 2mL is added drop-wise in the deionized water of 38mL, stirs, obtain solution A; 0.297g nine hydrated sodium sulfide is dissolved in solution A, obtains solution B.Solution B being poured into polytetrafluoroethylene (PTFE) is in the stainless steel autoclave of liner.Then, clean zinc metal sheet (99.9%1 × 3cm) is placed in this solution obliquely.10h is reacted at autoclave being sealed in 150 DEG C.After reaction terminates, naturally cool to room temperature.Gray product on zinc metal sheet respectively rinses 3 times with deionized water and absolute ethyl alcohol respectively, then 50 DEG C of vacuum drying 6h.
(2) 0.01g selenium powder joins in the mixed solution of 20mL ammoniacal liquor and 20mL deionized water, constantly stirs and forms homogeneous solution, then add 0.01g sodium borohydride in 100mL glass reaction bottle.After stirring 30min, the zinc metal sheet being coated with product of inserting step (1) gained.Reaction bulb is added thermal response 5h at 90 DEG C.After reaction terminates, the zinc metal sheet deionized water and absolute ethyl alcohol being coated with product is respectively rinsed 3 times, 50 DEG C of vacuum drying 6h.
The structure of product and morphology characterization:
With RigakuTTRIIIX-ray powder diffractometer (Cu target), Discriminating materials is carried out to embodiment 1 products therefrom, as shown in Figure 1.Except the diffraction maximum of zinc metal sheet substrate and ZnO, the diffraction maximum corresponding to 2 θ angle 27.5o and 54.2o can belong to (111), (311) crystal face (JCPDSNo:80-0021) of Emission in Cubic ZnSe respectively.XRD analysis result shows, sample prepared by zinc metal sheet substrate is made up of ZnO and ZnSe two-phase.
Carried out morphology analysis by SEM to product, result as shown in Figure 2.Show that sample is nm wall array structure.
Carried out morphology analysis with transmission electron microscope to the product got off ultrasonic from substrate, result as shown in Figure 3.Show that sample is the structure of nanometer sheet being adhered to less nanometer sheet.
Analyze the shell of product further with high resolution transmission electron microscopy, result as shown in Figure 4.The interplanar distance of 0.32nm can index be (111) crystal face of Emission in Cubic ZnSe.
Embodiment 2
A kind of visible light photocatalytic degradation organic dyestuff application of ZnO/ZnSe nano material.
Heterogeneous for the ZnO/ZnSe nm wall of above-mentioned preparation array structure product is cut into 1 × 1.5cm size, and putting into 5mL concentration is 1.0 × 10
-5also stir 1h in the dark in the RhB solution of mol/L, make catalyst surface reach the attached balance of absorption-desorption.Afterwards, 300W xenon lamp is used to carry out radiation of visible light.Use ultraviolet-visible spectrophotometer (ShimadzuUV-2550) to measure the absorption spectrum of solution every 20min, determined the concentration of RhB by the characteristic absorption peak at 554nm place.As shown in Figure 5, curve is as shown in Figure 6 over time for degradation process concentration for the UV absorption spectrogram of degradation results.After radiation of visible light 120min, degradation rate reaches 93%.Obviously, cooperative effect between nm wall heterojunction structure component significantly enhances photocatalytic activity, the distribution density that the heterogeneous array structure of nm wall is high in addition can farthest embody the photocatalytic activity relevant to its structure with spacing wide between adjacent nanostructures, the destruction of the micro-structural effectively avoiding powder catalyst often to face and reunion, this applies the guarantee provided advantageously for photocatalytic degradation.
Embodiment 3
A kind of ZnO/ZnSe nano material is as the cycle performance of visible light catalyst rhodamine B degradation.
Taken out by array structure catalyst tweezers after photocatalytic degradation, rinse several times with deionized water and absolute ethyl alcohol, be reentered in fresh RhB solution and carry out photocatalytic degradation experiment, result is as shown in table 1.Result of study shows that this photochemical catalyst degradation rate after 10 times that circulates still reaches 91.2%, and show that this photochemical catalyst has good photocatalysis cyclical stability to RhB, this is very attractive for practical application.
Table 1 is the circulation result of embodiment 3ZnO/ZnSe nm wall heterogeneous array structure visible light photocatalytic degradation RhB.
Table 1
Embodiment 4
A preparation method for ZnO/ZnSe nano material, comprises the following steps:
(1) 1, the 6-hexamethylene diamine of 5mL is added drop-wise in the deionized water of 35mL, stirs, obtain solution A; 0.336g nine hydrated sodium sulfide is dissolved in solution A, obtains solution B.Solution B being poured into polytetrafluoroethylene (PTFE) is in the stainless steel autoclave of liner.Then, clean zinc metal sheet (99.9%1 × 3cm) is placed in this solution obliquely.9h is reacted at autoclave being sealed in 120 DEG C.After reaction terminates, naturally cool to room temperature.Gray product on zinc metal sheet respectively rinses 3 times with deionized water and absolute ethyl alcohol respectively, then 50 DEG C of vacuum drying 6h.
(2) 0.015g selenium powder joins in the mixed solution of 20mL ammoniacal liquor and 20mL deionized water, constantly stirs and forms homogeneous solution, then add 0.015g sodium borohydride in 100mL glass reaction bottle.After stirring 30min, the zinc metal sheet being coated with product of inserting step (1) gained.Reaction bulb is added thermal response 8h at 70 DEG C.After reaction terminates, the zinc metal sheet deionized water and absolute ethyl alcohol being coated with product is respectively rinsed 3 times, 50 DEG C of vacuum drying 6h.
Claims (4)
1. a ZnO/ZnSe nano material, is characterized in that, described ZnO/ZnSe nano material be diameter 500nm ZnO nano sheet on adhere to the ZnSe nanometer sheet that size is 50nm;
The preparation method of described ZnO/ZnSe nano material comprises the following steps:
(1) 1,6-hexamethylene diamine is added in deionized water, stir, obtain solution A; Nine hydrated sodium sulfides are dissolved in solution A, obtain solution B, solution B being poured into polytetrafluoroethylene (PTFE) is in the stainless steel autoclave of liner, clean zinc metal sheet is placed on obliquely in this solution, add thermal response, after reaction terminates, naturally cool to room temperature, gray product on zinc metal sheet respectively cleans 3 times with deionized water and absolute ethyl alcohol respectively, then 50 DEG C of vacuum drying 6h;
(2) selenium powder is joined in the mixed solution of ammoniacal liquor and deionized water, continuous stirring forms homogeneous solution, add sodium borohydride, after continuing to stir 30min, the zinc metal sheet being coated with product of inserting step (1) gained, adds thermal response, after end, the zinc metal sheet deionized water and absolute ethyl alcohol that are coated with product are respectively cleaned 3 times, 50 DEG C of vacuum drying 6h, obtain the heterogeneous array structure of ZnO/ZnSe nm wall;
The concentration obtaining vulcanized sodium in solution B described in step (1) is 0.025-0.035mol/L;
Thermal response is added, temperature 120-150 DEG C, reaction time 8-10h described in step (1);
In step (2), the concentration of selenium powder in the mixed solution of ammoniacal liquor and deionized water is 0.003-0.005mol/L; The mol ratio 2-2.1:1 of sodium borohydride and selenium powder; Described adds thermal response, temperature 60-90 DEG C, reaction time 5-8h.
2. ZnO/ZnSe nano material according to claim 1, is characterized in that, in step (1), the volume ratio of deionized water and 1,6-hexamethylene diamine is 19-7:1.
3. ZnO/ZnSe nano material according to claim 1, is characterized in that, in step (2), the volume ratio of ammoniacal liquor used and deionized water is 0.6-1:1.
4. a ZnO/ZnSe nano material according to claim 1 is as the photocatalytic applications of visible light photocatalytic degradation organic dyestuff rhodamine B (RhB).
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| CN104384527B (en) * | 2014-12-10 | 2016-06-01 | 黑龙江大学 | The preparation method of the two-dimentional transition metal/metal oxides mixed phase nanometer sheet of a kind of self-supporting |
| CN107138170A (en) * | 2017-05-03 | 2017-09-08 | 吉林师范大学 | A kind of preparation method of ZnO/ZnSe hetero-junctions nanobelt photocatalyst film |
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