CN109879880A - A kind of near-infrared solid luminescent semiconductor material and its preparation method and application - Google Patents
A kind of near-infrared solid luminescent semiconductor material and its preparation method and application Download PDFInfo
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Abstract
The present invention provides a kind of near-infrared solid luminescent semiconductor material, and molecular formula is [(Me)2‑DABCO]2M5Pb2I13(M Cu, Ag one such or two kinds), belongs to monoclinic system, C2/c space group, cell parameter α=γ=90 °, β=105.3290 (10)~105.3370 (10) °,Preparation process of the present invention is simple, cheap, at low temperature fluorescence intensity and temperature line relationship, high sensitivity, and there is fluorescence temperature to sense effect, can be used as the intracorporal near-infrared fluorescent temperature sensing material of biology.
Description
Technical field
The invention belongs to technical field of material, and in particular to a kind of near-infrared solid luminescent semiconductor material and its system
Preparation Method and application.
Background technique
Luminescent material is in life lighting, display, optical communication, photoswitch, imaging, sensing, biomarker and medical diagnosis etc.
Field has important research and application value.Luminescent material can be divided into fluorescent material and phosphorescence according to the length of luminescent lifetime
Material can be divided into up-conversion and lower transition material according to the difference that energy is converted again.More luminescent material is applied at present
The materials such as oxide, the complex of rare earth metal are mainly based upon, luminous efficiency is high, stability is high, but structure type compares
Single, performance regulation is difficult to realize.Compared to phosphor, luminous organic material is with driving voltage is low, brightness is high, hair
The advantages that light efficiency is high and easily realizes large area of color display, but light quantum, which produces that low, service life is short and stability is poor etc., to be lacked
Fall into the commercial applications process for but again limiting luminous organic material.Therefore people imagine by inorganic component and organic component into
The mode of row hydridization organically combines the inorganic functional advantage with organic two kinds of different components, to break through it is single inorganic or
The defect of person's luminous organic material aspect of performance.In this context, hybrid inorganic-organic luminescent material causes scientist and work
The research interest and extensive concern of industry.
Hybrid inorganic-organic metal halide has structure type abundant and semiconducting behavior, in field of photovoltaic materials
With important application value.The especially ABX of perovskite structure type3Type halide, due to its special total vertex connection
Mode can be using Effective Regulation perovskite structure as three-dimensional framework, two by adjusting the charge and steric configuration of organic amine cation
Tie up layer and one-dimensional chain.The steric configuration of organic amine cation has the symmetry of octahedral structure unit in inorganic framework simultaneously
Very important regulating and controlling effect further adjusts the band structure and photoelectric properties of organic-inorganic hybrid material.Organic and inorganic is miscellaneous
The photoelectric properties for changing metal halide depend mainly on the structure of inorganic framework and the deformation extent of component units, and deformation extent is got over
Height, polarizability is bigger, and photoelectric activity is higher.Therefore regulate and control the fundamental means of hybrid inorganic-organic metal halide photoelectric properties
It is to adjust the deformation extent of inorganic structure unit.Previous research is often through introducing different organic formwork agent, using having
The structure of the steric configuration regulation inorganic framework of machine template and the deformation behaviour of structural motif, and for mixing metal halide
Research is always blank.d10Transient metal complex has excellent luminescent properties, occupies in solid luminescent Material Field important
Application value.
Summary of the invention
Relatively simple, the property for rare earth luminescent material in the prior art and organic inorganic hybridization metal halide structure type
The disadvantages of capable of being difficult to, the present invention provide a kind of near-infrared solid luminescent semiconductor material and its preparation method and application.
The technical solution adopted by the present invention are as follows:
Near-infrared solid luminescent semiconductor material of the present invention, molecular formula are [(Me)2-DABCO]2M5Pb2I13, belong to
In monoclinic system, C2/c space group, cell parameter
α=γ=90 °, β=105.3290 (10)~105.3370 (10) °, Wherein: M is
Cu, Ag are one such or two kinds, (Me)2- DABCO is N, N- dimethyl-triethylene diamine.
[(Me)2-DABCO]2M5Pb2I13Have following structure feature: MI4Structure is connected by sharing I atom between tetrahedron
At M5I11Cluster, M5I11Pass through PbI between cluster5Structural unit connects to form [M5Pb2I13]4-One-dimensional chain, organic cation [(Me)2-
DABCO]2+It is filled between no chain, and connects to form Magnetic Properties of Three-Dimensional Supramolecular Complex structure by hydrogen bond.
The preparation method of near-infrared solid luminescent semiconductor material of the present invention, specifically comprises the following steps:
It i) is that 1~1.5:2~3:1~1.5 ratio weighs DABCO, MI, PbI according to molar ratio2As reaction raw materials,
It is added to 4~5mLN, the in the mixed solvent of dinethylformamide, 0.5~1mL hydroiodic acid and 1~2mL methanol will mix molten
Liquid is packed into polytetrafluoroethylliner liner, then is sealed in reaction kettle, wherein M Cu, Ag are one such or two kinds；
Ii) reaction kettle is put into drying box, 140~160 DEG C isothermal reaction 6~8 days, after reaction in air
Naturally cool to room temperature；
Iii it) opens reaction kettle and the yellow block being obtained by filtration is washed with distilled water 2-3 by mixture vacuumizing filtration
Secondary, 80 degree of 8~10 hours of drying, can be obtained [(Me) in vacuum drying oven2-DABCO]2M5Pb2I13Yellow crystals, yield
Between 37~41%.
Near-infrared solid luminescent semiconductor material obtained by the present invention can absorb all ultraviolet light with it is a part of visible
Light has stronger optical absorption between 200-550nm, and band gap is located at 2.3~2.5eV, belongs to a kind of semiconductor material, can be with
By ultraviolet light or purple light excited transmitting fluorescence.
Near-infrared solid luminescent semiconductor material obtained by the present invention has good thermal stability, can be from subzero
200 DEG C are stabilized to 280 DEG C or more, can satisfy the use needs in low temperature to mesophilic range.
The luminous intensity of near-infrared solid luminescent semiconductor material provided by the invention can occur with ambient temperature variation
It is apparent to change.From 300K to 80K in temperature range, the intensity of emission peak is continuously reduced, wherein [(Me)2-DABCO]2Cu5Pb2I13Luminous intensity changed linearly within the scope of 80-180K with temperature, and [(Me)2-DABCO]2Ag5Pb2I13Hair
Luminous intensity changes within the scope of 80-140K with temperature linearity；Fluorescence intensity varies with temperature sensitiveer, and changing value can achieve
70~80%, in 180K, sensitivity is 3.1~3.2, suitable with the sensitivity of rare earth compounding.Therefore provided by the present invention
Near-infrared solid luminescent semiconductor material can be used as a kind of near-infrared fluorescent temperature sensing material, connect applied to organism etc. is non-
Temperature detection in touch working environment.
The present invention introduces d on the basis of single metal halide10Transition metal Cu, Ag pass through mixed metal ion
Method develops a kind of mixed metal halide of the organic-inorganic with near-infrared luminous performance, has in low-temperature region excellent
Fluorescence temperature senses effect, this is that first hybrid inorganic-organic metal halide solid-state with near-infrared luminous performance is sent out
Luminescent material.
The present invention passes through hybrid transition metal Ag and Cu, as the ratio of Ag:Cu is different, obtained near-infrared solid-state hair
406~422nm of photosemiconductor material it is purple light excited under, at room temperature can be close within the scope of 753~801nm with launch wavelength
Infrared light, maximum emission peak is 801nm at room temperature 300K, and minimum emission peak is 753nm, and Stock displacement reaches 347-
379nm, half-peak breadth can reach 215-247nm, emission peak can continuously change within the scope of 753~801nm, be a kind of adjustable
Humorous near-infrared solid luminescent material.
Compared with prior art, the present invention having the advantages that.
Mixed metal halide near-infrared solid luminescent material preparation process provided by the present invention is simple, cheap,
There is fluorescence temperature to sense effect, can be used as in organism for fluorescence intensity and temperature line relationship under low temperature, high sensitivity
Near-infrared fluorescent temperature sensing material.
Detailed description of the invention
Fig. 1 is mixed metal halide [(Me)2-DABCO]2M5Pb2I13Crystal structure figure；
Fig. 2 is to mix metal halide [(Me) in embodiment 12-DABCO]2Cu5Pb2I13Excitation spectrum and emission spectra；
Fig. 3 is to mix metal halide [(Me) in embodiment 22-DABCO]2Ag5Pb2I13Excitation spectrum and emission spectra；
Fig. 4 is to mix metal halide [(Me) in embodiment 12-DABCO]2Cu5Pb2I13Emission spectra at different temperatures；
Fig. 5 is to mix metal halide [(Me) in embodiment 22-DABCO]2Ag5Pb2I13Emission spectra at different temperatures；
Fig. 6 is to mix metal halide [(Me) in embodiment 12-DABCO]2Cu5Pb2I13Fluorescence intensity vary with temperature song
Line；
Fig. 7 is to mix metal halide [(Me) in embodiment 22-DABCO]2Ag5Pb2I13Fluorescence intensity vary with temperature song
Line；
Fig. 8 is to mix metal halide [(Me) in embodiment 12-DABCO]2Cu5Pb2I13Fluorescence intensity vary with temperature spirit
Sensitivity；
Fig. 9 is that embodiment 2 mixes metal halide [(Me)2-DABCO]2Cu5Pb2I13Fluorescence intensity vary with temperature it is sensitive
Degree；
Figure 10 is the transmitting that metal halide [(Me) 2-DABCO] 2M5Pb2I13 (M=Ag and Cu) is mixed in embodiment 3 and 4
Spectrum.
Specific embodiment
Below with reference to embodiment and Figure of description, the present invention will be further described.
Embodiment 1
DABCO (0.05g), CuI, PbI are weighed according to the ratio that molar ratio is 1:2:12As reaction raw materials, it is added to
Mixed solution is packed into polytetrafluoroethylene (PTFE) by 4mLN, the in the mixed solvent of dinethylformamide, 0.5mL hydroiodic acid and 1mL methanol
Liner, then be sealed in reaction kettle, it is reacted 6 days for 140 DEG C in drying box, cooled to room temperature, filter mixed liquor will filter
To pale yellow color lump be washed with distilled water 2-3 times, 80 degree of 8 hours of drying in vacuum drying oven, can be obtained near-infrared solid-state hair
Luminescent material finished product, i.e., mixed metal halide [(Me)2-DABCO]2Cu5Pb2I13Pale yellow crystals, yield 37%.
Embodiment 2
DABCO (0.05g), AgI, PbI are weighed according to the ratio that molar ratio is 1:2.5:12As reaction raw materials, it is added to
Mixed solution is packed into polytetrafluoroethyl-ne by 5mLN, the in the mixed solvent of dinethylformamide, 0.8mL hydroiodic acid and 1.5mL methanol
Alkene liner, then be sealed in reaction kettle, it is reacted 7 days for 160 DEG C in drying box, cooled to room temperature, filter mixed liquor will filter
Obtained pale yellow color lump is washed with distilled water 2-3 times, and 80 degree of 10 hours of drying, can be obtained [(Me) in vacuum drying oven2-
DABCO]2Cu5Pb2I13Pale yellow crystals, yield 40%.
Embodiment 3
DABCO (0.05g), CuI, AgI, PbI are weighed according to the ratio that molar ratio is 1:1:1:12As reaction raw materials, add
Enter to 5mLN, the in the mixed solvent of dinethylformamide, 0.8mL hydroiodic acid and 1.5mL methanol, mixed solution is packed into poly- four
Vinyl fluoride liner, then be sealed in reaction kettle, it is reacted 7 days for 160 DEG C in drying box, cooled to room temperature, filter mixed liquor, it will
The pale yellow color lump being obtained by filtration is washed with distilled water 2-3 times, and 80 degree of 10 hours of drying, can be obtained in vacuum drying oven
[(Me)2-DABCO]2Cu2.5Ag2.5Pb2I13Pale yellow crystals, yield 40%.
Embodiment 4
DABCO (0.050g), CuI, AgI, PbI are weighed according to the ratio that molar ratio is 1:0.4:1.6:12It is former as reaction
Material, is added to 4mLN, and mixed solution is packed into poly- by the in the mixed solvent of dinethylformamide, 1mL hydroiodic acid and 2mL methanol
Tetrafluoroethene liner, then be sealed in reaction kettle, it is reacted 8 days for 180 DEG C in drying box, cooled to room temperature, filter mixed liquor,
The pale yellow color lump being obtained by filtration is washed with distilled water 2-3 times, 80 degree of 10 hours of drying, can be obtained in vacuum drying oven
[(Me)2-DABCO]2CuAg4Pb2I13Pale yellow crystals, yield 41%.
Fig. 1 is mixed metal halide [(Me)2-DABCO]2M5Pb2I13Crystal structure figure, wherein [M5Pb2I13]4-Be by
[MI4] and [PbI6] share the one-dimensional catenary structure that I atom is formed by connecting, [(Me)2-DABCO]2+For free cation, filling
In [M5Pb2I13]4-Between.
Fig. 2 is to mix metal halide [(Me) in embodiment 12-DABCO]2Cu5Pb2I13Excitation spectrum and emission spectra, wherein
Maximum excitation peak position belongs to feux rouges in 753nm in 406nm, maximum emission peak position.
Fig. 3 is to mix metal halide [(Me) in embodiment 22-DABCO]2Ag5Pb2I13Excitation spectrum and emission spectra；Wherein
Maximum excitation peak position belongs near infrared light in 801nm in 422nm, maximum emission peak position.
Fig. 4 is to mix metal halide [(Me) in embodiment 12-DABCO]2Cu5Pb2I13Emission spectra at different temperatures,
As temperature reduces, emission peak intensity is gradually increased, and mainly due to reducing with temperature, heat radiation weakens, optical transition ratio
Increase, transmitting enhancing；
Fig. 5 is to mix metal halide [(Me) in embodiment 22-DABCO]2Ag5Pb2I13Emission spectra at different temperatures,
As temperature reduces, emission peak intensity is gradually increased, and mainly due to reducing with temperature, heat radiation weakens, optical transition ratio
Increase, transmitting enhancing；
Fig. 6 is to mix metal halide [(Me) in embodiment 12-DABCO]2Cu5Pb2I13Fluorescence intensity vary with temperature song
Line, with the linear variation of temperature within the scope of 80-180K, 180K or more emission peak intensity reduces very fast emission peak intensity；
Fig. 7 is to mix metal halide [(Me) in embodiment 22-DABCO]2Ag5Pb2I13Fluorescence intensity vary with temperature song
Line, for emission peak intensity with the linear variation of temperature within the scope of 80-140K, 140K or more emission peak intensity is weak rapidly；
Fig. 8 is to mix metal halide [(Me) in embodiment 12-DABCO]2Cu5Pb2I13Fluorescence intensity vary with temperature spirit
Sensitivity, sensitivity are increased with temperature and are increased, and reach maximum value, temperature sense sensitivity with higher at room temperature；
Fig. 9 is that embodiment 2 mixes metal halide [(Me)2-DABCO]2Cu5Pb2I13Fluorescence intensity vary with temperature it is sensitive
Degree.
Figure 10 is to mix metal halide [(Me) in embodiment 3 and 42-DABCO]2M5Pb2I13Several difference Ag；When Cu ratio
Emission spectra, as Ag:Cu ratio is different, the emission peak positions of halide can between 753-801nm consecutive variations, belong to
A kind of infraluminescence semiconductor of Wavelength tunable section.
Claims (9)
1. a kind of near-infrared solid luminescent semiconductor material, it is characterised in that: molecular formula is [(Me)2-DABCO]2M5Pb2I13, belong to
In monoclinic system, C2/c space group, cell parameter α
=γ=90 °, β=105.3290 (10)~105.3370 (10) °, Wherein: M is
Cu, Ag are one such or two kinds, (Me)2- DABCO is N, N- dimethyl-triethylene diamine.
2. near-infrared solid luminescent semiconductor material according to claim 1, it is characterised in that: [(Me)2-DABCO]2M5Pb2I13Have following structure feature: MI4M is connected and composed by sharing I atom between tetrahedron5I11Cluster, M5I11Lead between cluster
Cross PbI5Structural unit connects to form [M5Pb2I13]4-One-dimensional chain, organic cation [(Me)2-DABCO]2+Be filled in no chain it
Between, and connect to form Magnetic Properties of Three-Dimensional Supramolecular Complex structure by hydrogen bond.
3. near-infrared solid luminescent semiconductor material according to claim 1, it is characterised in that: [(Me)2-DABCO]2M5Pb2I13Wavelength be 406~422nm it is purple light excited under, near infrared light of the launch wavelength within the scope of 753~801nm.
4. the preparation method of near-infrared solid luminescent semiconductor material a method according to any one of claims 1-3, it is characterised in that: adopt
It is synthesized with solvent thermal reaction, with DABCO, MI, PbI2As reaction raw materials, be added to n,N-Dimethylformamide, hydroiodic acid and
The in the mixed solvent of methanol obtains mixed liquor, mixed liquor is packed into polytetrafluoroethylliner liner, then be sealed in reaction kettle, by reaction kettle
It is placed in temperature reaction in drying box, cooled to room temperature after reaction, filter mixed liquor steams the pale yellow color lump being obtained by filtration
Distilled water washing, vacuum drying can be obtained [(Me)2-DABCO]2M5Pb2I13Pale yellow crystals.
5. the preparation method of near-infrared solid luminescent semiconductor material according to claim 4, it is characterised in that: DABCO,
MI、PbI2The molar ratio of dosage is 1~1.5:2~3:1~1.5.
6. the preparation method of near-infrared solid luminescent semiconductor material according to claim 4, it is characterised in that: N, N- bis-
The dosage of methylformamide, hydroiodic acid and methanol is respectively 4~5mL, 0.5~1mL, 1~2mL.
7. the preparation method of near-infrared solid luminescent semiconductor material according to claim 4, it is characterised in that: drying box
Interior reaction temperature is 140-160 DEG C, and the reaction time is 6-8 days；Vacuum drying temperature is 80 DEG C, drying time 8-10h.
8. the application of near-infrared solid luminescent semiconductor material a method according to any one of claims 1-3, it is characterised in that: [(Me)2-
DABCO]2M5Pb2I13As near-infrared fluorescent temperature sensing material, applied to the temperature detection in non-contact operation environment.
9. the application of near-infrared solid luminescent semiconductor material according to claim 8, it is characterised in that: when M is Cu,
[(Me)2-DABCO]2Cu5Pb2I13Luminous intensity changed linearly within the scope of 80-180K with temperature；When M is Ag [(Me)2-
DABCO]2Ag5Pb2I13Luminous intensity changed linearly within the scope of 80-140K with temperature.
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2019
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| CN105839187A (en) * | 2016-05-06 | 2016-08-10 | 华侨大学 | Organic-inorganic hybridization semiconductor crystal material and synthesis method and application thereof |
| CN106433617A (en) * | 2016-09-20 | 2017-02-22 | 江苏科技大学 | Fluorescent chemical compound for adjusting white-light LED and preparing method and application thereof |
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Application publication date: 20190614 |