CN104592269B - Double triazole cadmium iodide complex of oxygen ether with potential fluorescent material and preparation method thereof - Google Patents
Double triazole cadmium iodide complex of oxygen ether with potential fluorescent material and preparation method thereof Download PDFInfo
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- CN104592269B CN104592269B CN201510088032.6A CN201510088032A CN104592269B CN 104592269 B CN104592269 B CN 104592269B CN 201510088032 A CN201510088032 A CN 201510088032A CN 104592269 B CN104592269 B CN 104592269B
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- triazole
- cadmium iodide
- oxygen ether
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- fluorescent material
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- OKIIEJOIXGHUKX-UHFFFAOYSA-L Cadmium iodide Inorganic materials [Cd+2].[I-].[I-] OKIIEJOIXGHUKX-UHFFFAOYSA-L 0.000 title claims abstract description 25
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 239000001301 oxygen Substances 0.000 title claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 16
- 229940075417 cadmium iodide Drugs 0.000 title claims abstract description 15
- -1 triazole cadmium iodide Chemical class 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title abstract description 8
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical group ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 22
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 230000005260 alpha ray Effects 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 230000005855 radiation Effects 0.000 claims description 3
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical compound C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 6
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 abstract description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract 2
- 239000000975 dye Substances 0.000 description 14
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 14
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- 229910000027 potassium carbonate Inorganic materials 0.000 description 7
- YAWIAFUBXXPJMQ-UHFFFAOYSA-N 1-bromo-4-(4-bromophenoxy)benzene Chemical compound C1=CC(Br)=CC=C1OC1=CC=C(Br)C=C1 YAWIAFUBXXPJMQ-UHFFFAOYSA-N 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 229960004643 cupric oxide Drugs 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000000113 differential scanning calorimetry Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002447 crystallographic data Methods 0.000 description 2
- 150000002460 imidazoles Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000002798 polar solvent Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- JTYRXXKXOULVAP-UHFFFAOYSA-N 1,2-dibromo-3-phenoxybenzene Chemical compound BrC1=CC=CC(OC=2C=CC=CC=2)=C1Br JTYRXXKXOULVAP-UHFFFAOYSA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- MOFINMJRLYEONQ-UHFFFAOYSA-N [N].C=1C=CNC=1 Chemical class [N].C=1C=CNC=1 MOFINMJRLYEONQ-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000005564 crystal structure determination Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000001795 light effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003217 pyrazoles Chemical class 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/08—Cadmium compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/18—Metal complexes
- C09K2211/188—Metal complexes of other metals not provided for in one of the previous groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Plural Heterocyclic Compounds (AREA)
Abstract
The invention discloses double triazole cadmium iodide complex of oxygen ether with potential fluorescent material and preparation method thereof, wherein double triazole cadmium iodide the complex { [Cd (L) of oxygen ether2I2]·CHCl3(1) structural motif as shown in Figure 1.Also disclose { [Cd (L) simultaneously2I2]·CHCl3The preparation method of (1) (L=1 (4 (4 (1H 1,2,4 triazole 1 base) phenoxy group) phenyl) 1H 1,2,4 triazole).It is to use " solvent-thermal method ", i.e. CdI2·2H2O and L at DMF and water 90oIt is slowly dropped to room temperature after reacting three days under C and obtains being suitable for the yellow rhabdolith of X ray single crystal diffraction.The present invention further discloses double triazole cadmium iodide the complex { [Cd (L) of oxygen ether2I2]·CHCl3(1) (L=1 (4 (4 (1H 1,2,4 triazole 1 base) phenoxy group) phenyl) 1H 1,2,4 triazole) as the application in terms of potential fluorescent material.
Description
The present invention obtains state natural sciences fund general project (21471113), young top-notch personnel's support plan, sky
Education Commission of Jinshi City general project (20140506), Tianjin Normal University's Middl-age and youth faculty Academic innovations advance planning item
(52XC1401), meter is cultivated by Tianjin State Scientific and Technological Commission general project (11JCYBJC03600) and Tianjin innovation team of institution of higher education
Draw the subsidy of (TD12-5038).
Technical field
The invention belongs to organic and Inorganic synthese technical field, relate to double triazole cadmium iodide the complex { [Cd (L) of oxygen ether2I2]·CHCl3(1) (L=1-(4-(4-(1H-1,2,4-triazole-1-base) phenoxy group) phenyl)-1H-1,2,4-three nitrogen
Azoles) preparation method and as the application of potential fluorescent material.
Background technology
1,2,4-triazole and derivative thereof have the coordination feature of pyrazoles and imidazoles concurrently, are that the bridging that coordination ability is stronger is joined
Body, has synthesized and has characterized substantial amounts of monokaryon, multinuclear and multidimensional compound the most.These parts can be former with the nitrogen on 1,2
Son forms N1, N2-bridging pattern with metallic ion coordination, can be by 2,4 for 4 unsubstituted 1,2,4-triazole derivatives
On nitrogen-atoms formed N2, N4-bridging pattern, this N2, N4-bridging pattern is with the N1 of imidazoles in metalloenzyme, N3-bridging pattern
Similar.Specific use for triazole class compounds is also manifested by the design of molecular device, and synthesis has different dimension
Metal complex has been the vital step of device.
The present invention is i.e. to use " solvent-thermal method ", i.e. CdI2·2H2O, L, DMF and water are 90oAfter reacting three days under C slowly
It is down to room temperature and obtains being suitable for yellow the rhabdolith { [Cd (L) of X-ray single crystal diffraction2I2]·CHCl3} (1) (L = 1-(4-
(4-(1H-1,2,4-triazole-1-base) phenoxy group) phenyl)-1H-1,2,4-triazole).This complex is alternatively arranged as potential
Fluorescent material aspect is applied.
Summary of the invention
Offer double triazole cadmium iodide the complex { [Cd (L) of a kind of oxygen ether is provided2I2]·
CHCl3(1) (L=1-(4-(4-(1H-1,2,4-triazole-1-base) phenoxy group) phenyl)-1H-1,2,4-triazole) list
Brilliant and preparation method thereof.
Following technical scheme is current inventor provides for this:
Double triazole cadmium iodide the complex { [Cd (L) of oxygen ether2I2]·CHCl3} (1) (L = 1-(4-(4-(1H-1,2,4-
Triazole-1-base) phenoxy group) phenyl)-1H-1,2,4-triazole) structural motif as shown in Figure 1.
The present invention further discloses double triazole cadmium iodide the complex { [Cd (L) of oxygen ether2I2]·CHCl3} (1) (L =
1-(4-(4-(1H-1,2,4-triazole-1-bases) phenoxy group) phenyl)-1H-1,2,4-triazoles) monocrystalline, it is characterised in that should
Mono-crystalline structures uses APEX II CCD single crystal diffractometer, uses through graphite monochromatised Mok alpha ray (λ=0.71073
)) it is incident radiation, collect point diffraction with ω-2 θ scan mode, obtain cell parameter through least square refinement, from difference
Fourier electron-density map utilizes SHELXL-97 direct method to solve single crystal data:
The crystallographic data of table 1. complex 1
Double triazole cadmium iodide the complex { [Cd (L) of oxygen ether of the present invention2I2]·CHCl3} (1) (L = 1-(4-(4-
(1H-1,2,4-triazole-1-bases) phenoxy group) phenyl)-1H-1,2,4-triazoles) preparation method of monocrystalline, its feature is being adopted
With " solvent-thermal method ", i.e. CdI2·2H2O, L, DMF and water are 90oIt is down to room temperature to prepare this complex after reacting three days under C
L。
One preferred example of the present invention:
The preparation of 1-(4-(4-(1H-1,2,4-triazole-1-base) phenoxy group) phenyl)-1H-1,2,4-triazole (L)
" one kettle way " is used, by 4,4 '-dibromodiphenyl ether, 1H-1,2,4-triazoles, potassium carbonate and cupric oxide at polar solvent
Prepare in a heated condition；The wherein bromo-4-of 1-(4-bromobenzene epoxide) benzene: 1H-1,2,4-triazole: potassium carbonate: cupric oxide mole
Ratio is 2:10:30:1；
4,4 '-dibromodiphenyl ether 1H-1,2,4-triazole
The present invention preferably 4,4 '-dibromodiphenyl ether: 1H-1,2,4-triazole: potassium carbonate: the mol ratio of cupric oxide is 2:10:
30:1；Reaction temperature 80-200 DEG C, 12-120 hour reaction time.In polar solvent, use " one kettle way ", by 4,4 '-two
This organic compound prepared in a heated condition by dibromodiphenyl ether, 1H-1,2,4-triazole, potassium carbonate and cupric oxide；
Presently preferred embodiment
1-(4-(4-(1H-1,2,4-triazole-1-base) phenoxy group) phenyl)-1H-1,2,4-triazole (L) (0.1
mmol)、CdI2·2H2O (0.2 mmo), water (10 mL) and DMF (6 mL) are put in 23 mL water heating kettles.90oC heating three
It is slowly dropped to room temperature after it, after driving still, obtains being suitable for the yellow rhabdolith of X-ray single crystal diffraction.Productivity: 40%.Elementary analysis
(C20H22CdN6O7) theoretical value (%): C, 42.08；H, 3.88；N, 14.72.Measured value: C, 42.11；H, 3.91；N, 14.74.
The present invention further discloses double triazole cadmium iodide complex [Cd (the L) (H of oxygen ether2O)2(CH3COO)2] (1) (L
=1-(4-(4-(1H-1,2,4-triazole-1-base) phenoxy group) phenyl)-1H-1,2,4-triazole) can be as potential fluorescence
Material aspect is applied.
Double triazole cadmium iodide the complex { [Cd (L) of a kind of oxygen ether disclosed by the invention2I2]·CHCl3} (1) (L = 1-
(4-(4-(1H-1,2,4-triazole-1-base) phenoxy group) phenyl)-1H-1,2,4-triazole) monocrystalline have the advantage that and spy
Point is:
(1) operation is simple and easy to do.
(2) reaction yield is high, and the purity of products obtained therefrom is high.
(3) { [Cd (L) prepared by the present invention2I2]·CHCl3(1) (L=1-(4-(4-(1H-1,2,4-tri-nitrogen
Azoles-1-base) phenoxy group) phenyl)-1H-1,2,4-triazoles) production cost is low, and method is easy, is suitable for large-scale production.
Accompanying drawing explanation
The crystal structure primitive figure of Fig. 1: complex 1；
The one-dimensional catenary structure figure of Fig. 2: complex 1.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further, and embodiment is only explanatory, is in no way intended to it
Limit the scope of the present invention by any way.Raw materials used 4,4 '-dibromodiphenyl ether, 1H-1,2,4-triazole, potassium carbonate and oxygen
Change copper etc. to be commercially available.All of raw material is all to buy from chemical reagents corporation both domestic and external, not through continuing purification
But directly use.
Embodiment 1
4,4 '-dibromodiphenyl ether: 1H-1,2,4-triazole: potassium carbonate: the mol ratio of cupric oxide is 2:10:30:1
It is separately added into CuO (0.5 in equipped with 50 mL three neck round bottom flasks of magneton, reflux condenser and thermometer
Mmol), potassium carbonate (15 mmol), 1H-1,2,4-triazole (5 mmol), 4,4 '-dibromodiphenyl ether (1 mmol) and 20
mL DMF.Start stirring 100oC, reacts 24 hours.After reaction terminates, reactant liquor being down to room temperature, filter, filtrate adds
100 mL water, separate out a large amount of precipitation, suction filtration, collect filter cake, 1-(4-(4-(1H-1,2,4-triazole-1-bases) phenoxy group) benzene
Base)-1H-1,2,4-triazole (L).Yield 60%.
Embodiment 2
1-(4-(4-(1H-1,2,4-triazole-1-base) phenoxy group) phenyl)-1H-1,2,4-triazole (L) (0.1
mmol)、CdI2·2H2O (0.2 mmo), 10 mL water and 6 mL DMF are put in 23 mL water heating kettles.90oAfter C heats three days
It is slowly dropped to room temperature, after driving still, obtains being suitable for the yellow rhabdolith of X-ray single crystal diffraction.Productivity: 40%.Elementary analysis
(C20H22CdN6O7) theoretical value (%): C, 42.08；H, 3.88；N, 14.72.Measured value: C, 42.11；H, 3.91；N, 14.74.
Embodiment 3
Crystal structure determination use APEX II CCD single crystal diffractometer, use through graphite monochromatised Mok alpha ray λ=
0.71073) it is incident radiation, collects point diffraction with ω-2 θ scan mode, obtain structure cell ginseng through least square refinement
Number, utilizes software to solve crystal structure from difference Fourier electron-density map, and through Lorentz lorentz and polarity effect correction.All of
H atom is synthesized by difference Fourier and determines through preferable position calculation.Detailed axonometry data are shown in Table 1.Structural motif is shown in
Fig. 1, one-dimensional catenary structure is shown in Fig. 2.
The crystallographic data of table 1. complex 1
Embodiment 4
The concrete instance that dyestuff or luminous agent use
Method: differentiated pulse volt-ampere (DPV) the curve negotiating Princeton Applied Research Laboratory of dye solution is developed
PARSTAT 2273 electrochemical workstation is measured.The DPV test of solution uses three-electrode system, and glass-carbon electrode is working electrode,
Auxiliary electrode is platinum plate electrode, homemade Ag/AgNO3Electrode is reference electrode；Electrolyte is the acetonitrile of 0.1mol L-1TBAP
Solution.With the Oxidation of Ferrocene reversible point of reduction to as internal standard, obtain the corrected value between test system and standard hydrogen electrode system.
Monochromatic incident light photoelectric transformation efficiency (IPCE) describes DSCs photoelectric transformation efficiency under monochromatic light effect, is to turn
Move on to the electron number of external circuit and the ratio of incident light subnumber.During measurement, 500 W xenon lamps are used to pass through as light source, incident light
The multifunctional assembled grating spectrograph of WDS-5 type obtains the monochromatic light under different wave length λ；Monochromatic light exposure is in the light sun of battery
Pole, is read current value I by Keithley2400 digital sourcemeter.Monochromatic good fortune illumination is micro-by USB4000 plug-and-play
Type light spectral instrument is measured.
Step: in order to have any actual knowledge of dyestuff at TiO2Adsorbance on film, by dye sensitization TiO2Nanometer crystal film (geometric surface
Long-pending about 1 cm2) it is immersed in 10 mL 0.01 mol L-1NaOH methanol solution in overnight, treat that dyestuff desorbs completely
The absorbance of rear mensuration solution.Wash one's face and rinse one's mouth according to absorbance and molar absorptivity and can calculate dyestuff on unit are nanometer crystal film
Adsorbance.The adsorbance of this complex is 4.8 × 10-4 mol/cm2。
Result: compared with the methanol solution of dyestuff, dyestuff is at TiO2Absorption spectrum on film the most substantially broadens and red shift.This
Show that dye molecule is at TiO2Define the first and J-aggregation of tail.Say from the operation principle of DSCs, the light that dye aggregation causes
Spectrum width and red shift are highly beneficial for the widening of photoelectric respone scope of dyestuff.But meanwhile, dye aggregation is known from experience
It is substantially reduced its electron injection efficiency, thus causes the degraded performance of DSCs.So, in dye solution, generally add eutectoid content
Agent suppresses the gathering of dyestuff.This complex is in methanol solution and at TiO2The fluorometric investigation of the purple solution on membrane electrode is adopted
With 2.5 × 10-5The methanol solution of mol/L, maximum emission wavelength is positioned at 580 nm.
After the preferred embodiment described in detail, it is familiar with this skilled worker and is clearly understood that, without departing from above-mentioned
Can carry out various change and amendment under claim and spirit, all technical spirit according to the present invention are to above example institute
Any simple modification, equivalent variations and the modification made, belongs to the scope of technical solution of the present invention.And the present invention is not illustrated
The restriction of example embodiment in book.
Claims (2)
1. the monocrystalline of the double triazole cadmium iodide complex of oxygen ether, it is characterised in that this mono-crystalline structures uses APEX II CCD mono-
Brilliant diffractometer, uses through graphite monochromatised Mok alpha ray, and λ=0.71073 is incident radiation, with ω-2 θ scan mode
Collect point diffraction, obtain cell parameter through least square refinement, utilize software to solve from difference Fourier electron-density map
Single crystal data:
The structure of the double triazole cadmium iodide complex monocrystal of described oxygen ether: [Cd (L)2I2]·CHCl3；L = 1-(4-(4-(1H-1,
2,4-triazole-1-base) phenoxy group) phenyl)-1H-1,2,4-triazole.
2. the monocrystalline of the double triazole cadmium iodide complex of oxygen ether described in claim 1 is as the application in terms of potential fluorescent material.
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| CN105524003A (en) * | 2016-01-05 | 2016-04-27 | 天津师范大学 | 4-(4-(4-(4H-1,2,4-triazol-4-yl) phenoxy) phenyl)-4H-1,2,4-triazol-single crystal and application thereof |
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| CN103086988B (en) * | 2013-02-21 | 2014-10-29 | 天津师范大学 | Phenyl bistriazole compound, and preparation method and application thereof |
| CN103772305A (en) * | 2014-01-14 | 2014-05-07 | 天津师范大学 | Oxyether triazole compound, and preparation method and application thereof |
| CN104193691B (en) * | 2014-09-11 | 2016-02-10 | 南京农业大学 | The synthetic method of a kind of three-(4-triazol radical phenyl) amine and cadmium complex thereof |
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