CN102408117A - Cu3(CN)3NH3 crystal-based novel strong fluorescent material and preparation method thereof - Google Patents
Cu3(CN)3NH3 crystal-based novel strong fluorescent material and preparation method thereof Download PDFInfo
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- CN102408117A CN102408117A CN2010102896627A CN201010289662A CN102408117A CN 102408117 A CN102408117 A CN 102408117A CN 2010102896627 A CN2010102896627 A CN 2010102896627A CN 201010289662 A CN201010289662 A CN 201010289662A CN 102408117 A CN102408117 A CN 102408117A
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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 efficient luminescent crystal material and preparation method thereof, especially [Cu
3(CN)
3NH
3] the crystallo-luminescence material and preparation method thereof.
Background technology
High efficient luminous material because its higher energy conversion efficiency can effectively be avoided the higher-energy loss that in inefficient luminescent material, exists, and then improves energy utilization efficiency effectively, has therefore received concern more and more widely.Optical crystal material because its crystallization property is better, can avoid the stronger radiationless relaxation effect that in non-crystalline material, exists, thereby they has improved luminous efficiency greatly.Because they have than light stable physics and photochemical character, can in awide temperature range, keep characteristics such as stable in addition, can be used as practical luminescent material, study focus for one that is therefore just becoming high efficient luminous material.Yet because most crystallo-luminescence materials all prepare through high temperature crystal pulling method or molten-salt growth method, so its preparation condition requires relatively harshness, and cost is higher, also environment is caused certain pollution.Therefore, utilize simple and convenient preparation method comparatively and gentle relatively experiment condition prepare stable and efficiently the crystallo-luminescence material received everybody extensive concern.Yet the crystalline material through gentle water/solvent-thermal method preparation belongs to the inorganic-organic hybrid material mostly, and such material changes under illumination or heating condition easily, does not have actual application value.Therefore inorganic stable inorganic crystal material is the major objective that everybody pursues.Cu with thermostability and light stability
3(CN)
3NH
3Crystal is exactly a kind of high efficient luminous material that under the low-temperature hydrothermal condition, prepares.
Summary of the invention
The present invention proposes a kind of preparation method of novel hyperfluorescence crystalline material
Adopt the component of the hyperfluorescence crystalline material of the present invention's preparation to be: Cu
3(CN)
3NH
3
The present invention adopts and is prepared as follows technology:
Hyperfluorescence crystalline material Cu
3(CN)
3NH
3Preparation.Under the room temperature, with CuCN, 2,5-two (4-benzene nitrile)-1,3, the 4-oxadiazole joins in the autoclave in ammoniacal liquor and the deionized water, and at room temperature stirs the solution that obtains mixing, and the solution that obtains is heat-treated.After thermal treatment finishes, with lower rate of temperature fall cool to room temperature.After the cooling, solution is removed, the deposition that obtains with water washing repeatedly after, obtain xanchromatic bulk crystals [Cu
3(CN)
3NH
3]
n
The X ray single crystal diffraction shows the Cu for preparing
3(CN)
3NH
3Crystal is a single crystal structure.The all crystals that obtains through the X-ray powder diffraction proof is two-dimensional layered structure.The cyanogen foundation group that utilizes FTIR to prove to exist in the structure.Can in the scope of 0 to 200 degree centigrade of temperature, keep stable through this material of thermogravimetric analysis proof, have the value of in wide temperature range, using.Utilizing under the fluorescent lamp, can realize stronger yellow emission.This material excitation band broad, the gold-tinted for becoming clear that obtains adds that its preparation cost is cheap, therefore has actual application value.
The u of material C efficiently of the present invention's preparation
3(CN)
3NH
3It is simple that crystalline material has technology, and cost is low, good reproducibility, and luminous efficiency is high, advantage such as can produce in enormous quantities.The present invention and domestic and international preparation the luminescent crystal material compare, have the thermostability height, light stability is great, luminous efficiency is high, is a kind of good new and effective luminescent crystal material.
Description of drawings
The accompanying drawing 1: [Cu that obtains through X-ray single crystal diffraction
3(CN)
3NH
3]
nCrystalline structure.
Accompanying drawing 2: [Cu
3(CN)
3NH
3]
nThe crystalline FTIR.
Accompanying drawing 3: [Cu
3(CN)
3NH
3]
nCrystalline X-ray powder diffraction spectrum and the spectrogram that obtains through the single crystal structure match.
Accompanying drawing 4: [Cu
3(CN)
3NH
3]
nCrystalline diffuse-reflectance absorption spectrum.
Accompanying drawing 5: [Cu
3(CN)
3NH
3]
nThe PLE 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 crystalline thermogravimetric curve.
Embodiment
Instance 1: (1) takes by weighing 200.0mg CuCN, and 40.0mg 2,5-two (4-benzene nitrile)-1,3, the 4-oxadiazole joins in the autoclave of 20ml in 1ml25% ammoniacal liquor and the 14ml deionized water, and stir at room temperature that 5h obtains mixing all and solution.This mixing solutions is heated 72h down at 180 ℃, then with 3 ℃ of h
-1Rate of temperature fall under cool to room temperature.The deposition that obtains with water washing repeatedly after, obtain the xanchromatic bulk crystals.Calculating its productive rate according to the CuCN that uses is 52.5%.Can see bright Yellow luminous with the portable fluorescence irradiation of 4W.
(2) take by weighing 300.0mg CuCN, 20.0mg 2,5-two (4-benzene nitrile)-1,3, the 4-oxadiazole joins in the autoclave of 20ml in 10ml 25% ammoniacal liquor and the 24ml deionized water, and stir at room temperature that 15h obtains mixing all and solution.This mixing solutions is heated 120h down at 80 ℃, then with 2 ℃ of h
-1Rate of temperature fall under cool to room temperature.The deposition that obtains with water washing repeatedly after, obtain the xanchromatic bulk crystals.Calculating its productive rate according to the CuCN that uses is 25.5%.Can see bright Yellow luminous with the portable fluorescence irradiation of 4W.
(3) take by weighing 100.0mg CuCN, 50.0mg 2,5-two (4-benzene nitrile)-1,3, the 4-oxadiazole joins in the autoclave of 20ml in 6ml 25% ammoniacal liquor and the 18ml deionized water, and stir at room temperature that 5h obtains mixing all and solution.This mixing solutions is heated 27h down at 210 ℃, then with 40 ℃ of h
-1Rate of temperature fall under cool to room temperature.The deposition that obtains with water washing repeatedly after, obtain the xanchromatic bulk crystals.Calculating its productive rate according to the CuCN that uses is 59%.Can see bright Yellow luminous with the portable fluorescence irradiation of 4W.
(4) take by weighing 50.0mg CuCN, 150.0mg 2,5-two (4-benzene nitrile)-1,3, the 4-oxadiazole joins in the autoclave of 40ml in 8ml 25% ammoniacal liquor and the 6ml deionized water, and stir at room temperature that 7h obtains mixing all and solution.This mixing solutions is heated 26h down at 100 ℃, then with 6 ℃ of h
-1Rate of temperature fall under cool to room temperature.The deposition that obtains with water washing repeatedly after, obtain the xanchromatic bulk crystals.Calculating its productive rate according to the CuCN that uses is 35%.Can see bright Yellow luminous with the portable fluorescence irradiation of 4W.
Claims (3)
1. one kind prepares based on Cu
3(CN)
3NH
3The method of the novel hyperfluorescence material of crystalline is characterized in that: under the room temperature, and with CuCN, 2; 5-two (4-benzene nitrile)-1,3, the 4-oxadiazole; Join in the autoclave in ammoniacal liquor and the deionized water, and at room temperature stir the solution that obtains mixing, and the solution that obtains is heat-treated.After thermal treatment finishes, with lower rate of temperature fall cool to room temperature; After the cooling, solution is removed, the deposition that obtains with water washing repeatedly after, obtain xanchromatic bulk crystals Cu
3(CN)
3NH
3
2. as claimed in claim 1 a kind of based on Cu
3(CN)
3NH
3The novel hyperfluorescence preparation methods of crystalline, it is characterized in that: described mixing solutions is heat-treated, 50-230 ℃ of insulation down.
3. as claimed in claim a kind based on Cu
3(CN)
3NH
3The novel hyperfluorescence material of crystalline is at solid-state laser, the high-efficiency fluorescence powder, and biological labled material, fields such as flat-panel monitor and photosensitive detecting element have using value.
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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 true CN102408117A (en) | 2012-04-11 |
| CN102408117B 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 |
|---|
| ZHAO ZHEN-GUO ET.AL.: "Synthesis, Crystal Structure and Luminescent Property of a New Copper(I) Iodide Complex Based on 3,5-Dimethyl-4-amino-triazole", 《结构化学》 * |
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|---|---|
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