CN102071460B - Method for preparing europium-doped lanthanum phosphate porous nanorods on basis of herring sperm DNA template - Google Patents
Method for preparing europium-doped lanthanum phosphate porous nanorods on basis of herring sperm DNA template Download PDFInfo
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- CN102071460B CN102071460B CN2010105502383A CN201010550238A CN102071460B CN 102071460 B CN102071460 B CN 102071460B CN 2010105502383 A CN2010105502383 A CN 2010105502383A CN 201010550238 A CN201010550238 A CN 201010550238A CN 102071460 B CN102071460 B CN 102071460B
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- sperm dna
- herring sperm
- lapo
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Abstract
The invention discloses a method for preparing europium-doped lanthanum phosphate porous nanorods on basis of a herring sperm DNA template and belongs to the technical field of nano material preparation. The method comprises three steps: (1) preparing mixed solution, namely dissolving Eu2O3 in nitric acid, evaporating the solution to obtain Eu(NO3)3 crystals, adding deionized water, adding La(NO3)3.6H2O to obtain mixed solution of La(NO3)3.6H2O and Eu(NO3)3, and dripping aqueous solution of herring sperm DNA into the mixed solution of La(NO3)3.6H2O and Eu(NO3)3 to obtain the mixed solution, wherein the mole percentage of europium nitrate in the mixed solution of La(NO3)3.6H2O and Eu(NO3)3 is 5 percent; (2) preparing a LaPO4:5-percent Eu<3+> precipitate, namely dripping aqueous solution of (NH4)3PO4 into the mixed solution to obtain the LaPO4:5-percent Eu<3+> precipitate; and (3) preparing LaPO4:5-percent Eu<3+> porous nanorods, namely transferring the LaPO4:5-percent Eu<3+> precipitate to a hydro-thermal reaction kettle, reacting at 160 DEG C for 12 hours, performing centrifugal separation on the precipitate, washing the precipitate by using absolute ethanol, and drying the precipitate at 60 DEG C and under vacuum for 12 hours to obtain crystalline LaPO4:5-percent Eu<3+> porous nanorods, wherein the diameter of the nanorods is 20 to 50 nanometers, and the length of the nanorods is 100 to 200 nanometers. The method is simple, easy to implement, economic and environmentally-friendly and has a bright application prospect.
Description
Technical field
The present invention relates to the nano material preparation research field, relate to a kind of method that europium lanthanum orthophosphate porous nano rod is mixed in preparation based on the herring sperm dna template specifically.
Background technology
RE phosphate has good thermostability and environmental stability, extensively is used as luminescent material matrix, and wherein studying more is LaPO
4Europium ion-doped lanthanum phosphate nano luminous material is a kind of important red fluorescence material, has broad application prospects, and has caused people's great attention.People have adopted coprecipitation method, reverse microemulsion process, sol-gel method, hydro-thermal and several different methods such as solvent-thermal method, electrostatic spinning technique to prepare the LaPO of multiple pattern
4: Eu
3+Nano material is like nanoparticle, nanometer rod, nano wire, nano thin-film and nanofiber etc.For example, prepared LaPO for employing oxalate coprecipitation methods such as snow crystal
4: Eu
3+Nanocrystalline (Shenyang University of Technology's journal, 2009,31 (6), 649-653); Li Peng etc. have adopted prepared by reverse microemulsion method LaPO
4Nanoparticle (South-Center University For Nationalities's journal: natural science edition, 2002,21 (3), 19-21); Employing sol-gel methodes such as Gao Rui have prepared LaPO
4: Eu
3+Nanometer rod (the China YouSe Acta Metallurgica Sinica: English edition, 2010,20 (3), 432-436); Employing polyvalent alcohol methods such as Wang Zhenling have prepared LaPO
4Nanoparticle (Chinese rare-earth journal, 2006,24 (3), 269-273); DongXiangting etc. have adopted hydrothermal method controlledly synthesis LnPO
4(Ln=La, Gd, Y) nanocrystalline (Journal of Materials Science:Mater.Electron., 2010,21,38-44); Employing gel network methods such as Qi Yan have prepared LaPO
4Nanoparticle (luminous journal, 2006,27 (3), 397-401); In the upright new LaPO that adopted Hydrothermal Preparation of waiting
4: Eu
3+Nanoparticle and nano wire (Chinese rare-earth journal: English edition, 2004,22 (1), 57-62); Employing sol-gel methodes such as M.Yu have prepared LaPO
4: Eu
3+Nano thin-film (Journalof Materials Chemistry, 2003,13,1413-1419); Employing wet chemistry methods such as Heike Meyssamy have prepared LaPO
4: Eu
3+Nanoparticle and nanofiber (Advannced Materials, 1999,11 (10), 840-844); Employing solvent-thermal methods such as Tian Li have synthesized LaPO
4Nanometer rod (Chinese invention patent, application number: 200810029502.1); Step Wen Bo etc. utilizes oleic acid and oleyl amine to prepare monodispersed rare earth doping phosphoric acid lanthanum fluorescence quantum point (Chinese invention patent, application number: 200810200176.6) as complexed surfactant auxiliary heat cracked method; Employing polyvalent alcohols such as Wang Hongzhi are that solvent, application coprecipitation method have prepared rare-earth doped lanthanum phosphate nano luminous particles (Chinese invention patent, application number: 200710044033.6); Xiao Xiuzhen etc. adopt zero(ppm) water and N, and dinethylformamide is a mixed solvent, and the deposition that precipitin reaction obtains is carried out hydro-thermal again, has prepared lanthanum orthophosphate nano luminous body (Chinese invention patent, the application number: 200810035855.2) of europium or terbium ion doping.
With DNA is the focus that template synthesizing inorganic nano material has become research.For example, employing DNA such as Liu Xianhua are that template has been assembled zinc oxide nano-chain (Chinese invention patent, application number: 200910229007.X); Employing DNA such as Xu Hui are that template has prepared metal nano conductor (Chinese invention patent, application number: 200810031316.1); Employing DNA such as Li Na are that template has prepared chain shaped barium fluoride nanospheres (Chinese invention patent, application number: 200810079482.9).Do not see that at present Application of DNA is that template prepares LaPO
4: Eu
3+The relevant report of porous nano rod.
It is template that the present invention adopts herring sperm dna, with Lanthanum trinitrate (La (NO
3)
36H
2O), europium sesquioxide (Eu
2O
3) and ammonium phosphate ((NH
4)
3PO
4) be raw material, with the deionized water solvent, use hydrothermal method, under the experiment condition of the best, prepared LaPO
4: Eu
3+The porous nano rod, in the present invention, the molecular fraction of adulterated europium ion is 5%, is labeled as LaPO
4: 5%Eu
3+, i.e. that the present invention is prepared is LaPO
4: 5%Eu
3+The porous nano rod.
Summary of the invention
Preparation LaPO in background technology
4: Eu
3+Nanoparticle, nanometer rod, nano wire, nano thin-film and nanofiber etc. have adopted coprecipitation method, reverse microemulsion process, sol-gel method, hydro-thermal and solvent-thermal method, electrostatic spinning technique etc.; With DNA is the inorganic nano material that template has been synthesized patterns such as nano chain, nm-class conducting wire and nanometer ball.The pattern of employed template, preparation product is all different with method of the present invention in the background technology.It is template that the present invention adopts herring sperm dna, uses hydrothermal method, has prepared LaPO
4: 5%Eu
3+The porous nano rod.
The present invention is achieved in that herring sperm dna is dissolved in the deionized water, prepares the certain density herring sperm dna aqueous solution.Use nitric acid dissolve Eu
2O
3The back evaporation obtains Eu (NO
3)
3Crystal adds deionized water, obtains Eu (NO
3)
3Solution adds La (NO again
3)
36H
2O obtains [La (NO
3)
3+ Eu (NO
3)
3] mixing solutions, the herring sperm dna aqueous solution is joined [La (NO
3)
3+ Eu (NO
3)
3] in the mixing solutions, add (NH again
4)
3PO
4The aqueous solution precipitates, and the mixture that obtains is transferred to carried out hydrothermal treatment consists in the hydrothermal reaction kettle, afterwards deposition is carried out spinning, absolute ethanol washing and vacuum drying treatment after, obtain LaPO
4: 5%Eu
3+The porous nano rod.The steps include:
(1) preparation mixing solutions
Herring sperm dna is dissolved in the deionized water, prepares the certain density herring sperm dna aqueous solution, take by weighing a certain amount of Eu
2O
3, obtain Eu (NO with evaporation behind the nitric acid dissolve
3)
3Crystal adds deionized water, obtains Eu (NO
3)
3Solution adds La (NO again
3)
36H
2O obtains [La (NO
3)
3+ Eu (NO
3)
3] mixing solutions, the herring sperm dna aqueous solution is joined [La (NO
3)
3+ Eu (NO
3)
3] in the mixing solutions, promptly form [La (NO
3)
3+ Eu (NO
3)
3+ herring sperm dna] mixing solutions.Described [La (NO
3)
3+ Eu (NO
3)
3+ herring sperm dna] La (NO in the mixing solutions
3)
3With Eu (NO
3)
3Mol ratio be 95: 5.
(2) preparation LaPO
4: 5%Eu
3+Deposition
To described [La (NO
3)
3+ Eu (NO
3)
3+ herring sperm dna] mixed solution and dripping (NH
4)
3PO
4The aqueous solution obtains LaPO
4: 5%Eu
3+Deposition.
(3) preparation LaPO
4: 5%Eu
3+The porous nano rod
With described LaPO
4: 5%Eu
3+Deposition is transferred in the hydrothermal reaction kettle, in 160 ℃ of reaction 12h, the deposition after the hydro-thermal is carried out spinning, after absolute ethyl alcohol is given a baby a bath on the third day after its birth time, in 60 ℃ of vacuum-drying 12h, obtains LaPO
4: 5%Eu
3+The porous nano rod, diameter 20～50nm, length 100～200nm.
At the LaPO described in the said process
4: 5%Eu
3+The porous nano rod has good crystalline form, diameter 20～50nm, and length 100～200nm has realized goal of the invention.
Description of drawings
Fig. 1 is LaPO
4: 5%Eu
3+The transmission electricity border photo of porous nano rod, this figure double as Figure of abstract;
Fig. 2 is LaPO
4: 5%Eu
3+The X-ray diffraction spectrogram of porous nano rod;
Fig. 3 is LaPO
4: 5%Eu
3+The exciting light spectrogram of porous nano rod;
Fig. 4 is LaPO
4: 5%Eu
3+The emmission spectrum figure of porous nano rod.
Embodiment
The Lanthanum trinitrate that the present invention selected for use (La (NO
3)
36H
2O), nitric acid (HNO
3), ammonium phosphate ((NH
4)
3PO
4), herring sperm dna and absolute ethyl alcohol be commercially available analytical pure product, europium sesquioxide (Eu
2O
3) purity be 99.99%; Used glassware and equipment are instrument and equipments commonly used in the laboratory.
Embodiment: get the 0.0623g herring sperm dna, it in the 20mL deionized water, stirring at low speed half a hour, is mixed with the dna solution that concentration is 3.12mg/mL.According to La
3+/ Eu
3+Mol ratio be 95: 5, take by weighing 0.0350g europium sesquioxide (Eu
2O
3) in beaker, the volume ratio that adds nitric acid and deionized water is that 1: 1 salpeter solution dissolves it fully, slowly unnecessary nitric acid is removed in evaporation, and is to be cooled to room temperature, adds the 60mL deionized water, obtains Eu (NO
3)
3Solution.Take by weighing the La (NO of 1.732g
3)
36H
2O joins Eu (NO
3)
3In the solution, stirring is dissolved it fully.The dna solution for preparing is added drop-wise to the La (NO for preparing
3)
3With Eu (NO
3)
3Mixing solutions in, stir 24h under the room temperature, the lanthanum ion of positively charged and the electronegative phosphate radical on europium ion and the DNA and the N atom on the base are fully adsorbed.Take by weighing (the NH of 0.5315g
4)
3PO
4, and add the 20mL deionized water dissolving, and slowly be added drop-wise in the above-mentioned mixing solutions, continue to stir 1h again.This mixture is transferred in the stainless steel hydrothermal reaction kettle of 3 50mL band teflon lined, in 160 ℃ of reaction 12h, naturally cooled to room temperature, spinning behind absolute ethanol washing three times, in 60 ℃ of vacuum-drying 12h, obtains LaPO
4: 5%Eu
3+The porous nano rod.Described LaPO
4: 5%Eu
3+Be the porous nano rod, diameter 20～50nm, length 100～200nm sees shown in Figure 1.Described LaPO
4: 5%Eu
3+The porous nano rod has good crystal formation, the spacing d value of its diffraction peak and relative intensity and LaPO
4The listed d value of PDF standard card (35-0731) consistent with relative intensity, belong to oblique system, spacer is P21/n, sees shown in Figure 2.When the monitoring wavelength is 589nm, described LaPO
4: 5%Eu
3+The excitation spectrum main peak of porous nano rod is positioned at the strong bands of a spectrum at 254nm place, belongs to O
2--Eu
3+Between the charge migration band, see shown in Figure 3.Under the ultraviolet excitation of 254nm, LaPO
4: 5%Eu
3+The porous nano rod is launched the bright red that main peak is positioned at 589nm, and it is corresponding to Eu
3+Ionic
5D
0→
7F
1Transition belongs to Eu
3+Ionic forces magnetic dipole transition, sees shown in Figure 4.
Certainly; The present invention also can have other various embodiments; Under the situation that does not deviate from spirit of the present invention and essence thereof; Those of ordinary skill in the art work as can make various corresponding changes and distortion according to the present invention, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (4)
1. the method that europium lanthanum orthophosphate porous nano rod is mixed in preparation based on the herring sperm dna template is characterized in that, adopts hydrothermal method, uses herring sperm dna to be template, and the employing deionized water is a solvent, and the preparation product is LaPO
4: 5%Eu
3+The porous nano rod the steps include:
(1) preparation mixing solutions
Solvent adopts deionized water, and the preparation herring sperm dna aqueous solution takes by weighing a certain amount of Eu
2O
3, obtain Eu (NO with evaporation behind the nitric acid dissolve
3)
3Crystal adds deionized water, obtains Eu (NO
3)
3Solution adds La (NO again
3)
36H
2O obtains [La (NO
3)
3+ Eu (NO
3)
3] mixing solutions, the herring sperm dna aqueous solution is joined [La (NO
3)
3+ Eu (NO
3)
3] in the mixing solutions, promptly form [La (NO
3)
3+ Eu (NO
3)
3+ herring sperm dna] mixing solutions;
(2) preparation LaPO
4: 5%Eu
3+Deposition
To described [La (NO
3)
3+ Eu (NO
3)
3+ herring sperm dna] mixed solution and dripping (NH
4)
3PO
4The aqueous solution obtains LaPO
4: 5%Eu
3+Deposition;
(3) preparation LaPO
4: 5%Eu
3+The porous nano rod
With described LaPO
4: 5%Eu
3+Deposition is transferred in the hydrothermal reaction kettle, in 160 ℃ of reaction 12h, the deposition after the hydro-thermal is carried out spinning, after absolute ethyl alcohol is given a baby a bath on the third day after its birth time, in 60 ℃ of vacuum-drying 12h, obtains LaPO
4: 5%Eu
3+The porous nano rod, diameter 20～50nm, length 100～200nm.
2. a kind of method that europium lanthanum orthophosphate porous nano rod is mixed in preparation based on the herring sperm dna template according to claim 1 is characterized in that that use in lanthanum source and europium source is Lanthanum trinitrate La (NO
3)
36H
2O and europium sesquioxide Eu
2O
3
3. a kind of method that europium lanthanum orthophosphate porous nano rod is mixed in preparation based on the herring sperm dna template according to claim 1 is characterized in that described [La (NO
3)
3+ Eu (NO
3)
3+ herring sperm dna] La (NO in the mixing solutions
3)
3With Eu (NO
3)
3Mol ratio be 95: 5.
4. a kind of method that europium lanthanum orthophosphate porous nano rod is mixed in preparation based on the herring sperm dna template according to claim 1 is characterized in that said ammonium phosphate (NH
4)
3PO
4Be precipitation agent.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101260302A (en) * | 2008-04-10 | 2008-09-10 | 同济大学 | Method for preparing europium or terbium ion doping lanthanum orthophosphate nano luminous body |
| CN101281158A (en) * | 2008-05-20 | 2008-10-08 | 北京化工大学 | DNA sensitivity electrode modified by hydrotalcite nanometer slice and preparation thereof |
| CN101323442A (en) * | 2008-07-16 | 2008-12-17 | 中山大学 | Solvent-thermal synthesis of lanthanum phosphate nanorod |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101260302A (en) * | 2008-04-10 | 2008-09-10 | 同济大学 | Method for preparing europium or terbium ion doping lanthanum orthophosphate nano luminous body |
| CN101281158A (en) * | 2008-05-20 | 2008-10-08 | 北京化工大学 | DNA sensitivity electrode modified by hydrotalcite nanometer slice and preparation thereof |
| CN101323442A (en) * | 2008-07-16 | 2008-12-17 | 中山大学 | Solvent-thermal synthesis of lanthanum phosphate nanorod |
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