CN102533247B - A kind of containing dysprosium fluorescent crystal and preparation method thereof - Google Patents

A kind of containing dysprosium fluorescent crystal and preparation method thereof Download PDF

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Publication number
CN102533247B
CN102533247B CN201010602188.9A CN201010602188A CN102533247B CN 102533247 B CN102533247 B CN 102533247B CN 201010602188 A CN201010602188 A CN 201010602188A CN 102533247 B CN102533247 B CN 102533247B
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carboxylic acid
fluorescent crystal
pyrazine carboxylic
dysprosium
crystal
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CN201010602188.9A
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CN102533247A (en
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陈文勇
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Abstract

A kind of dysprosium fluorescent crystal that contains relates to a kind of compound [Dy (L) 3(H 2o) 2] n6nH 2o (wherein L is 2-pyrazine carboxylic acid).This compound adopts solvent thermal reaction legal system standby, with Dy (Ac) 34H 2o and 2-pyrazine carboxylic acid, also prepares single crystal by reacting by heating synthesis after adding distil water simultaneously.This compound can be applied to manufacturing fluorescent material.

Description

A kind of containing dysprosium fluorescent crystal and preparation method thereof
Art
Patent of the present invention relates to a kind of containing dysprosium fluorescent crystal [Dy (2-pyrazine carboxylic acid) 3(H 2o) 2] n6nH 2o.
Background technology
The development degree of material, information and energy three industries has been acknowledged as the important symbol of a national overall national strength power, and wherein material is again the basic substance of information and energy industry.The generation of each important novel material is all the milestone of human social development process.This century, one of most important research field was exactly the research and development of novel material.Rare-earth luminescent material, as a kind of important material, plays a part abnormal important in contemporary luminescent material and biological fluorescent labeling field.
In general, strong fluorescence can be sent time f-f charge transtion occurs rare earth.But the uptake factor of rare earth ion is usually lower, thus rare earth ion is caused to be difficult to luminescence or luminescence is more weak.In order to improve the uptake factor of rare earth ion, we adopt the organic ligand with conjugated structure as aromatic ring carboxylic acid etc. and rare-earth ion coordination, will pass to rare earth ion after light energy absorption, make rare earth ion can be luminous.2-pyrazine carboxylic acid is a kind of aromatic ring carboxylic acid with conjugated structure, and it can with the effective coordination of rare earth ion and by the transmission ofenergy of absorption to rare earth ion.Therefore we adopt the method that 2-pyrazine carboxylic acid and rare earth dysprosium ion react, and have synthesized one containing dysprosium fluorescent crystal.
Summary of the invention
The object of patent of the present invention will synthesize one containing dysprosium fluorescent crystal.For this reason, need to select suitable raw material to carry out building-up reactions.
We adopt solvent thermal reaction method for this reason, with Dy (Ac) 34H 2o and 2-pyrazine carboxylic acid, synthesizes novel containing dysprosium fluorescent crystal [Dy (2-pyrazine carboxylic acid) by reacting by heating after adding distil water 3(H 2o) 2] n6nH 2o.
Novel containing dysprosium fluorescent crystal [Dy (2-pyrazine carboxylic acid) 3(H 2o) 2] n6nH 2o tool has the following advantages: reaction process does not introduce impurity, prepares simple; Reaction conditions is gentle, equipment that need not be complicated; Can directly obtain body monocrystalline, need not further growth monocrystalline.
Embodiment
Embodiment 1, about containing dysprosium fluorescent crystal [Dy (2-pyrazine carboxylic acid) 3(H 2o) 2] n6nH 2the synthesis of O and single crystal growing.
Containing dysprosium fluorescent crystal [Dy (2-pyrazine carboxylic acid) 3(H 2o) 2] n6nH 2the synthesis of O and bulk growth adopt solvent thermal reaction method to complete simultaneously.
Chemical reagent used, manufacturer and charging capacity are:
First accurately claim to obtain the reactant of respective quality by the mol ratio of each reactant, put into the solvent thermal jar that volume is 23mL, add 10mL distilled water, sealing.The solvent thermal jar closed is put into muffle furnace, uses temperature controller control temperature, be warming up to 180 DEG C by room temperature in 5 hours, 180 DEG C of constant temperature 7 days, then be down to 30 DEG C in 6 hours, then turn off power supply.From muffle furnace, take out solvent thermal jar, open, colourless bulk crystals (productive rate > 60%) can be obtained.
Measure through x-ray crystal structure, compound [Dy (2-pyrazine carboxylic acid) 3(H 2o) 2] n6nH 2the spacer of O is Pbca (No.61), and its cell parameter is z=8, unit-cell volume fluorescence spectrum test shows, compound [Dy (2-pyrazine carboxylic acid) 3(H 2o) 2] n6nH 2o sends very strong fluorescence.

Claims (1)

1. containing a dysprosium fluorescent crystal, it is characterized in that: molecular formula is [Dy (2-pyrazine carboxylic acid) 3(H 2o) 2] n6nH 2o, spacer is Pbca (No.61), and its cell parameter is z=8, unit-cell volume
CN201010602188.9A 2010-12-12 2010-12-12 A kind of containing dysprosium fluorescent crystal and preparation method thereof Expired - Fee Related CN102533247B (en)

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CN102533247B true CN102533247B (en) 2015-09-30

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108219791A (en) * 2018-01-26 2018-06-29 温州大学 A kind of fluorescent crystal material and its preparation process flow based on rare earth oxide
CN108504350A (en) * 2018-04-27 2018-09-07 上海应用技术大学 A kind of pyrazine fluorescent crystal material and preparation method thereof

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* Cited by examiner, † Cited by third party
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WO2003003009A1 (en) * 2001-06-29 2003-01-09 7Tm Pharma A/S Use of metal-ion chelates in validating biological molecules as drug targets in test animal models
CN100415715C (en) * 2003-02-11 2008-09-03 杜锡光 Super-phthalocyanine compound with six isoindole structure subunits in laver oxazine cycle and its synthesis and use
DE10310887A1 (en) * 2003-03-11 2004-09-30 Covion Organic Semiconductors Gmbh Matallkomplexe
CA2645456A1 (en) * 2006-03-10 2007-09-20 Mallinckrodt Inc. Photoactive compounds and compositions and uses thereof
JP4951759B2 (en) * 2007-01-01 2012-06-13 国立大学法人九州工業大学 Redox-responsive luminescent probe and detection method using the same

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CI01 Publication of corrected invention patent application

Correction item: Inventor

Correct: Chen Wentong

False: Chen Wenyong

Number: 39

Volume: 31

CI03 Correction of invention patent

Correction item: Inventor

Correct: Chen Wentong

False: Chen Wenyong

Number: 39

Page: The title page

Volume: 31

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Granted publication date: 20150930

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CF01 Termination of patent right due to non-payment of annual fee