CN102408117B - Cu3(CN)3NH3 crystal-based strong fluorescent material and preparation method thereof - Google Patents
Cu3(CN)3NH3 crystal-based strong fluorescent material and preparation method thereof Download PDFInfo
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- CN102408117B CN102408117B CN201010289662.7A CN201010289662A CN102408117B CN 102408117 B CN102408117 B CN 102408117B CN 201010289662 A CN201010289662 A CN 201010289662A CN 102408117 B CN102408117 B CN 102408117B
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Abstract
The invention discloses a Cu3(CN)3NH3 crystal-based novel strong fluorescent material and a preparation method thereof, and relates to preparation of a high-efficiency luminous crystal material. The component of the Cu3(CN)3NH3 crystal material prepared by the method is [Cu3(CN)3NH3]n. The stable Cu3(CN)3NH3 crystal material with high luminous efficiency is prepared by a mild hydrothermal method on 2,5-bis(4-cyanophenyl)-1,3,4-oxadiazole serving as a template. X-ray single crystal diffraction, X-ray powder diffraction, an infrared absorption spectrum, a thermogravimetric curve, an excitation spectrum, an emission spectrum, an absorption spectrum and the like show the single crystal characteristic, heat stability and high-efficiency luminous characteristic of the luminous crystal material; and the obtained crystal material can emit bright yellow light when irradiated by a fluorescent lamp.
Description
Technical field
The present invention relates to High Efficiency Luminescence crystalline material and preparation method thereof, especially [Cu
3(CN)
3nH
3] crystallo-luminescence material and preparation method thereof.
Background technology
High efficient luminous material, because its higher energy conversion efficiency effectively can avoid the higher-energy loss that exists in inefficient luminescent material, and then effectively improves energy utilization efficiency, therefore receives and pay close attention to more and more widely.Optical crystal material, because its crystallization property is better, can avoid the stronger non-radiative relaxation effect existed in non-crystalline material, thus they substantially increases luminous efficiency.In addition because they have compared with light stable physics and photochemical character, features such as stablizing can be kept in wide temperature range, as practical luminescent material, therefore can just become a study hotspot of high efficient luminous material.But because most crystallo-luminescence material is all prepared by high temperature crystal pulling method or molten-salt growth method, so its preparation condition requires harsher, and cost is higher, also causes certain pollution to environment.Therefore, the preparation method that utilization is comparatively easy and relative gentle experiment condition prepare the extensive concern that stable and efficient crystallo-luminescence material receives everybody.But mostly belonging to Inorganic-organic Hybrid Material by crystalline material prepared by gentle water/solvent-thermal method, such material easily changes under illumination or heating condition, does not have actual application value.Therefore the inorganic crystal material of inorganic stabilizers is the major objective that everybody pursues.There is the Cu of thermostability and light stability
3(CN)
3nH
3crystal is exactly a kind of high efficient luminous material prepared under low-temperature hydrothermal condition.
Summary of the invention
The present invention proposes a kind of preparation method of hyperfluorescenceZeng Yongminggaoyingguang crystalline material
The component of the hyperfluorescenceZeng Yongminggaoyingguang crystalline material adopting the present invention to prepare is: Cu
3(CN)
3nH
3.
The present invention adopts following preparation technology:
HyperfluorescenceZeng Yongminggaoyingguang crystalline material Cu
3(CN)
3nH
3preparation.Under room temperature, by CuCN, 2,5-bis-(4-cyanophenyl)-1,3,4-oxadiazoles, join in autoclave in ammoniacal liquor and deionized water, and at room temperature stir the solution obtaining mixing, and heat-treat the solution obtained.After thermal treatment terminates, with lower rate of temperature fall cool to room temperature.After cooling, removed by solution, the precipitation obtained washes with water repeatedly, obtains yellow bulk crystals [Cu
3(CN)
3nH
3]
n.
X-ray single crystal diffraction shows the Cu prepared
3(CN)
3nH
3crystal is single crystal structure.Prove that all crystals obtained is two-dimensional layered structure by X-ray powder diffraction.The cyanogen foundation group utilizing infrared absorption spectrum to demonstrate to exist in structure.Prove that this material can keep stable in the scope of temperature 0 to 200 degrees Celsius by thermogravimetric analysis, there is the value applied in wide temperature range.Utilizing under fluorescent lamp, stronger yellow emission can be realized.This material excitation band is wider, and what obtain is bright gold-tinted, adds that its preparation cost is cheap, therefore has actual application value.
Efficient material C u prepared by the present invention
3(CN)
3nH
3it is simple that crystalline material has technique, and cost is low, reproducible, and luminous efficiency is high, can carry out the advantage such as producing in enormous quantities.The present invention with prepare both at home and abroad luminescent crystal material compared with, have thermostability high, light stability is great, and luminous efficiency is high, is a kind of excellent High Efficiency Luminescence crystalline material.
Accompanying drawing explanation
The accompanying drawing 1: [Cu obtained by X-ray single crystal diffraction
3(CN)
3nH
3]
ncrystalline structure.
Accompanying drawing 2:[Cu
3(CN)
3nH
3]
nthe infrared absorption spectrum of crystal.
Accompanying drawing 3:[Cu
3(CN)
3nH
3]
nthe X-ray powder diffraction spectrum of crystal and the spectrogram that obtained by single crystal structure matching.
Accompanying drawing 4:[Cu
3(CN)
3nH
3]
nthe diffuse-reflectance absorption spectrum of crystal.
Accompanying drawing 5:[Cu
3(CN)
3nH
3]
nthe excitation spectrum of crystalline rare earth, emission spectrum; Illustration is the luminous photo of sample under the portable ultra violet lamp of 4-W.
Accompanying drawing 6:[Cu
3(CN)
3nH
3]
nthe thermogravimetric curve of crystal.
Embodiment
Example 1:(1) take 200.0mg CuCN, 40.0mg 2,5-bis-(4-cyanophenyl)-1,3,4-oxadiazole, joins in the autoclave of 20ml in 1ml25% ammoniacal liquor and 14ml deionized water, and at room temperature stir 5h obtain mixing all and solution.This mixing solutions is heated 72h at 180 DEG C, then with 3 DEG C of h
-1rate of temperature fall under cool to room temperature.The precipitation obtained washes with water repeatedly, obtains yellow bulk crystals.Calculating its productive rate according to the CuCN used is 52.5%.With the portable fluorescence of 4W irradiate can see bright Yellow luminous.
(2) take 300.0mg CuCN, 20.0mg 2,5-bis-(4-cyanophenyl)-1,3,4-oxadiazoles, join in the autoclave of 20ml in 10ml 25% ammoniacal liquor and 24ml deionized water, and at room temperature stir 15h obtain mixing all and solution.This mixing solutions is heated 120h at 80 DEG C, then with 2 DEG C of h
-1rate of temperature fall under cool to room temperature.The precipitation obtained washes with water repeatedly, obtains yellow bulk crystals.Calculating its productive rate according to the CuCN used is 25.5%.With the portable fluorescence of 4W irradiate can see bright Yellow luminous.
(3) take 100.0mg CuCN, 50.0mg 2,5-bis-(4-cyanophenyl)-1,3,4-oxadiazoles, join in the autoclave of 20ml in 6ml 25% ammoniacal liquor and 18ml deionized water, and at room temperature stir 5h obtain mixing all and solution.This mixing solutions is heated 27h at 210 DEG C, then with 40 DEG C of h
-1rate of temperature fall under cool to room temperature.The precipitation obtained washes with water repeatedly, obtains yellow bulk crystals.Calculating its productive rate according to the CuCN used is 59%.With the portable fluorescence of 4W irradiate can see bright Yellow luminous.
(4) take 50.0mg CuCN, 150.0mg 2,5-bis-(4-cyanophenyl)-1,3,4-oxadiazoles, join in the autoclave of 40ml in 8ml 25% ammoniacal liquor and 6ml deionized water, and at room temperature stir 7h obtain mixing all and solution.This mixing solutions is heated 26h at 100 DEG C, then with 6 DEG C of h
-1rate of temperature fall under cool to room temperature.The precipitation obtained washes with water repeatedly, obtains yellow bulk crystals.Calculating its productive rate according to the CuCN used is 35%.With the portable fluorescence of 4W irradiate can see bright Yellow luminous.
Claims (1)
1. prepare based on Cu for one kind
3(CN)
3nH
3the method of the hyperfluorescenceZeng Yongminggaoyingguang material of crystal, it is characterized in that: under room temperature, by 200.0mg CuCN, 40mg 2,5-bis-(4-cyanophenyl)-1,3,4-oxadiazole, 1mL 25% ammoniacal liquor and 14mL deionized water join in autoclave, and at room temperature stir the solution obtaining mixing, at 180 DEG C, 72h is heated to the solution obtained, after thermal treatment terminates, with 3 DEG C of h
-1rate of temperature fall cool to room temperature; After cooling, removed by solution, the precipitation obtained washes with water repeatedly, obtains yellow bulk crystals Cu
3(CN)
3nH
3.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010289662.7A CN102408117B (en) | 2010-09-21 | 2010-09-21 | Cu3(CN)3NH3 crystal-based strong fluorescent material and preparation method thereof |
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|---|---|---|---|
| CN201010289662.7A CN102408117B (en) | 2010-09-21 | 2010-09-21 | Cu3(CN)3NH3 crystal-based strong fluorescent material and preparation method thereof |
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|---|---|
| CN102408117A CN102408117A (en) | 2012-04-11 |
| CN102408117B true CN102408117B (en) | 2015-03-04 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1454961A (en) * | 2003-05-15 | 2003-11-12 | 中国科学院长春应用化学研究所 | Transmission type polymer electroluminescent material and preparing method thereof |
| CN1861607A (en) * | 2006-05-10 | 2006-11-15 | 浙江工业大学 | Fluorane kind derivant, its preparation and application |
| CN101698672A (en) * | 2009-11-06 | 2010-04-28 | 南京大学 | Tricarbonal rhenium (I) complexes containing carrier-transporting groups (oxadiazole or carbazole), preparation method and application thereof |
-
2010
- 2010-09-21 CN CN201010289662.7A patent/CN102408117B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1454961A (en) * | 2003-05-15 | 2003-11-12 | 中国科学院长春应用化学研究所 | Transmission type polymer electroluminescent material and preparing method thereof |
| CN1861607A (en) * | 2006-05-10 | 2006-11-15 | 浙江工业大学 | Fluorane kind derivant, its preparation and application |
| CN101698672A (en) * | 2009-11-06 | 2010-04-28 | 南京大学 | Tricarbonal rhenium (I) complexes containing carrier-transporting groups (oxadiazole or carbazole), preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| Synthesis, Crystal Structure and Luminescent Property of a New Copper(I) Iodide Complex Based on 3,5-Dimethyl-4-amino-triazole;Zhao Zhen-Guo et.al.;《结构化学》;20100215;第29卷(第2期);245-249 * |
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|---|---|
| CN102408117A (en) | 2012-04-11 |
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