CN103979515A - YPO4 nano particle synthesized by assist of surfactant cetyltrimethyl ammonium bromide (CTAB) and preparation method of YPO4 nano particle - Google Patents

YPO4 nano particle synthesized by assist of surfactant cetyltrimethyl ammonium bromide (CTAB) and preparation method of YPO4 nano particle Download PDF

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CN103979515A
CN103979515A CN201410206587.1A CN201410206587A CN103979515A CN 103979515 A CN103979515 A CN 103979515A CN 201410206587 A CN201410206587 A CN 201410206587A CN 103979515 A CN103979515 A CN 103979515A
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ctab
nano particle
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ypo
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CN103979515B (en
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刘运
李朋
郭雅欣
史晓磊
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a YPO4 nano particle synthesized by assist of a surfactant cetyltrimethyl ammonium bromide (CTAB) and a preparation method of the YPO4 nano particle. A hydrothermal method is adopted, and Eu-doped YPO4 cross nanorod bundle is synthesized by reaction of the prepared YNO3 and EuNO3 and NH4H2PO4 solutions under the structure-directing effect of the surfactant CTAB. The method comprises the following steps: firstly, mixing and stirring the YNO3 solution with the EuNO3 solution, and then dropwise adding the prepared CTAB solution and additionally mixing; dropwise adding the NH4H2PO4 solution after stirring, and then adjusting the pH value of the mixed solution by using a dilute nitric acid; transferring the mixed solution to a reaction kettle with a polytetrafluoroethylene lining after stirring the mixed solution, carrying out sealed heating reaction, and then naturally cooling to room temperature; centrifuging, washing and drying to obtain the product. The product is prepared by the hydrothermal method, and is simple in process, and the prepared sample is the cross nanorod bundle, and is high in crystallinity and large in size.

Description

A kind of by the auxiliary synthetic YPO of Surfactant CTAB 4nano particle and preparation method thereof
Technical field
The present invention relates to a kind of intersection nanometer rod pencil YPO 4preparation method, be specifically related to a kind of by the auxiliary synthetic YPO of Surfactant CTAB 4nano particle and preparation method thereof.
Background technology
Rare earth luminescent material occupies very consequence in whole solid luminescence field, because special electron structure makes rare earth element have the incomparable character of general element.In recent years, because have the advantages such as receptivity is strong, luminosity is high, synthesis temperature is moderate, RE phosphate was widely used at illumination, quantum optics, colour television set and thermoluminescence detection field, had caused researcher interest widely.Therefore, the method for finding the RE phosphate of manufacture craft simple and product multifunction and special appearance is in industrial production or scientific research, all to have important value, also aspect synthetic other nano material, has directive significance.
YPO 4in RE phosphate, occupy critical role, be widely used in the doped substrate of rare earth ion.Rare earth ion doped YPO 4by several different methods, obtain, comprising coprecipitation method, sol-gel method, solid reaction process etc.We know, the performance of rare earth phosphate nano material depends on its pattern to a great extent, size, structure and composition thereof.In above-mentioned synthetic method, hydrothermal method technique is simple, and reaction conditions is gentle, can control well the pattern of product, size, structure, and meanwhile tensio-active agent, controlling crystal morphology, is also being played the part of important role in structure.Hejuan Song etc. have synthesized Eu doping YPO with EDTA assisting alcohol-hydrothermal method 4nanometer bundle (Materials Science and Engineering:B, 2013,178 (16): 1012); Hua Lai etc. have synthesized the Eu doping YPO of different size with different tensio-active agent (EDTA, citric acid, oxalate) 4nanometer rod (Ceramics International, 2014,40 (1), 1885).Up to now, also not with the auxiliary synthetic intersection nanometer rod pencil Eu doping YPO of Surfactant CTAB 4the relevant report of nano particle.
Summary of the invention
The object of the invention is to overcome the shortcoming existing in above-mentioned prior art, provide a kind of by the auxiliary synthetic YPO of Surfactant CTAB 4nano particle and preparation method thereof, has simple to operately, and degree of crystallinity is high, be uniformly dispersed, and the advantage that size is large.
For achieving the above object, the present invention is by the following technical solutions: comprising:
A kind of by the auxiliary synthetic YPO of Surfactant CTAB 4the preparation method of nano particle, comprises the following steps:
(1) prepare Y (NO 3) 3, Eu (NO 3) 3solution, CTAB solution and NH 4h 2pO 4solution, standby;
(2) get step 1) standby Y (NO 3) 3solution and Eu (NO 3) 3solution mixes, Y (NO after mixing 3) 3and Eu (NO 3) 3mol ratio be (9:1)-(4:1), in backward mixed solution, drip CTAB solution, after stirring, reaction generates Y xeu 1-xnO 3, rear dropping NH 4h 2pO 4solution, until Y xeu 1-xnO 3, CTAB, NH 4h 2pO 4three's mol ratio is 1:1:1, after obtain mixing solutions;
(3) regulating step 2) the mixing solutions pH value that obtains is to 1-3;
(4) by step 3) mixing solutions transfer in reactor after stirring and seal, at 120 ℃-200 ℃, be incubated 12-36h, generate precipitation to reaction, after by reactor cool to room temperature;
(5) by step 4) the throw out centrifugation that obtains, throw out is washed dry afterwards, finally obtain by the auxiliary synthetic YPO of Surfactant CTAB 4nano particle.
In step (1): described Y (NO 3) 3the preparation method of solution: by Y 2o 3be dissolved in concentrated nitric acid, add the unnecessary concentrated nitric acid of heat abstraction, then to add deionized water to be made into concentration be 0.4molL -1y (NO 3) 3solution;
Described Eu (NO 3) 3the preparation method of solution: by Eu 2o 3be dissolved in concentrated nitric acid, add the unnecessary concentrated nitric acid of heat abstraction, then to add deionized water to be made into concentration be 0.2molL -1eu (NO 3) 3solution;
The preparation method of described CTAB solution: CTAB is joined in deionized water and heated and stirred is dissolved it, formation concentration is 0.1molL -1cTAB solution;
Described NH 4h 2pO 4the preparation method of solution: by NH 4h 2pO 4being dissolved in wiring solution-forming concentration in deionized water is 0.2molL -1.
In step (2): described in be uniformly mixed liquid time be 20-30min.
In step (3), regulating the reagent of mixing solutions pH value is rare nitric acid.
In the churning time described in step (4), be 40-60min.
At the reactor described in step (4), be stainless steel cauldron, liner is tetrafluoroethylene, and reactor volume compactedness is 60%-80%.
Described throw out washing drying process is: by centrifugation postprecipitation thing, water and washing with alcohol, after put into the dry 8-12h of 70 ℃ of-80 ℃ of loft drier.
A kind of by the auxiliary synthetic YPO of Surfactant CTAB 4the YPO that the preparation method of nano particle makes 4nano particle: nano particle is cluster shape, and the long 8-12 μ m of average rod, diameter 1.5-2.5 μ m.
The present invention has following beneficial effect: the prior art of comparing, the present invention adopts hydrothermal method, under the structure-directing effect of Surfactant CTAB, utilizes YNO 3and EuNO 3with NH 4h 2pO 4the synthetic Eu doping of solution reaction YPO 4intersection nano rod bundle, first by YNO 3solution and EuNO 3solution mix and blend, then drips the CTAB solution additional stirring that prepare, after stirring, drips NH 4h 2pO 4solution, then regulates the pH value of mixing solutions; After being uniformly mixed solution, this mixing solutions is transferred in reactor, sealing, at 120 ℃-200 ℃, reaction produces precipitation, naturally cools to room temperature; Through centrifugal, washing, is dried and finally obtains product again.The present invention adopts hydrothermal method synthetic, simple to operate, can be by regulating differential responses condition to control pattern and the size of product; By XRD figure and SEM figure, can find out the nanometer rod pencil Eu doping YPO making by present method 4nano particle, degree of crystallinity is high, is uniformly dispersed, and size is larger.The present invention adopts hydrothermal method synthetic, simple to operate, can, by regulating differential responses condition to control pattern and the size of product, be applicable to batch production.And the crossed rodlike Eu of preparation doping YPO 4nano particle is to exploitation YPO 4base fluorescent material is significant.
Accompanying drawing explanation
Fig. 1 is Eu doping YPO prepared by the present invention 4the XRD figure spectrum of intersection nano rod bundle powder;
Fig. 2 is Eu doping YPO prepared by the present invention 4the SEM photo of intersection nano rod bundle powder under 2000 times;
Fig. 3 is Eu doping YPO prepared by the present invention 4the SEM photo of intersection nano rod bundle powder under 6000 times.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
A kind of by the auxiliary synthetic YPO of Surfactant CTAB 4the preparation method of nano particle, comprises the following steps:
(1) preparing concentration is 0.4molL -1y (NO 3) 3, concentration is 0.2molL- 1eu (NO 3) 3solution, concentration are 0.1molL -1cTAB solution and concentration be 0.2molL -1nH 4h 2pO 4solution, standby, Y (NO 3) 3the preparation method of solution: by Y 2o 3be dissolved in concentrated nitric acid, add the unnecessary concentrated nitric acid of heat abstraction, then add deionized water to be made into Y (NO 3) 3solution; By Eu 2o 3be dissolved in concentrated nitric acid, add the unnecessary concentrated nitric acid of heat abstraction, then add deionized water to be made into Eu (NO 3) 3solution; CTAB is joined in deionized water and heated and stirred is dissolved it, form CTAB solution; By NH 4h 2pO 4be dissolved in wiring solution-forming in deionized water;
(2) get step 1) standby Y (NO 3) 3solution and Eu (NO 3) 3solution mixes, Y (NO after mixing 3) 3and Eu (NO 3) 3mol ratio be (9:1-4:1), to mixed solution and dripping CTAB solution, stir 20-30min after reaction generate Y xeu 1-xnO3, drips NH in rear solution 4h 2pO 4solution, until Y xeu 1-xnO3, CTAB, NH 4h 2pO 4three's mol ratio is 1:1:1, after obtain mixing solutions;
(3) use rare nitric acid regulating step 2) the mixing solutions pH value that obtains is to 1-3;
(4) by step 3) mixing solutions stir after 40-60min, transfer in band teflon-lined stainless steel cauldron and seal, and reactor volume compactedness is 60%-80%, at 120 ℃-200 ℃, react 12-36 hour, to precipitation while not increasing, after naturally cool to room temperature;
(5) by step 4) the throw out centrifugation that obtains, after by centrifugation postprecipitation thing, water and washing with alcohol three times, after put into the dry 8-12h of 70 ℃ of-80 ℃ of loft drier, finally obtain by the auxiliary synthetic intersection nanometer rod pencil Eu doping YPO of Surfactant CTAB 4nano particle.
A kind of by the auxiliary synthetic intersection nanometer rod pencil Eu doping YPO of Surfactant CTAB 4the intersection nanometer rod pencil Eu doping YPO that the preparation method of nano particle makes 4nano particle: nano particle is intersection cluster shape, and the long 8-12 μ m of average rod, diameter 1.5-2.5 μ m.
Below in conjunction with embodiment, further illustrate.
Embodiment 1:
(1) get the 0.4molL of 4.35ml -1y (NO 3) 3solution, then adds Eu (NO 3) 3solution fully mixes, Y after mixing 3+: Eu 3+=9:1;
(2) weighing 2mmolCTAB puts in 15ml deionized water, heated and stirred makes its dissolving, after its cool to room temperature, it is slowly joined in the mixing solutions of step (1) gained, and the additional 20min that stirs, to guarantee that CTAB is completely by positively charged ion parcel evenly;
(3) weigh 2mmolNH 4h 2pO 4be dissolved in 15ml deionized water, be added dropwise in the mixing solutions of step (2) gained, stir 20min, guarantee that it mixes;
(4) under agitation condition, with rare nitric acid, regulate the pH=1 of mixing solutions;
(5) above-mentioned mixing solutions is stirred to 40min, transfer in band teflon-lined stainless steel cauldron, sealing is reacted after 12h at 180 ℃, naturally cools to room temperature;
(6) by the throw out centrifugation obtaining, when centrifugal, rotating speed is 10000r/min, and centrifugation time is 5min, and water and ethanol repeated washing throw out, centrifugation, puts into the dry 12h of 70 ℃ of loft drier, obtains the auxiliary synthetic nanometer rod pencil Eu doping YPO by CTAB 4nano particle.
Embodiment 2:
(1) get the 0.4molL of 4.35ml -1y (NO 3) 3solution, then adds Eu (NO 3) 3solution fully mixes rear Y 3+: Eu 3+=6:1;
(2) weighing 2mmolCTAB puts in 15ml deionized water, heated and stirred makes its dissolving, after its cool to room temperature, it is slowly joined in the mixing solutions of step (1) gained, and the additional 25min that stirs, to guarantee that CTAB is completely by positively charged ion parcel evenly;
(3) weigh the NH of 2mmol 4h 2pO 4be dissolved in 15ml deionized water, be added dropwise in the mixing solutions of step (2) gained, stir 20min, guarantee that it mixes;
(4) under agitation condition, with rare nitric acid, regulate the pH=2 of final gained mixing solutions;
(5) above-mentioned mixing solutions is stirred to 50min, transfer in band teflon-lined stainless steel cauldron, sealing is reacted after 36h at 120 ℃, naturally cools to room temperature;
(6) by the throw out centrifugation obtaining (rotating speed is 10000r/min), centrifugation time is 5min, and water and ethanol repeated washing throw out, centrifugation, put into the dry 10h of 75 ℃ of loft drier, obtain the auxiliary synthetic nanometer rod pencil Eu doping YPO by CTAB 4nano particle.
Embodiment 3:
(1) get the 0.4molL of 4.35ml -1y (NO 3) 3solution, then adds Eu (NO 3) 3solution fully mixes rear Y 3+: Eu 3+=4:1;
(2) weighing 2mmolCTAB puts in 15ml deionized water, heated and stirred makes its dissolving, after its cool to room temperature, it is slowly joined in the mixing solutions of step (1) gained, and the additional 30min that stirs, to guarantee that CTAB is completely by positively charged ion parcel evenly;
(3) weigh the NH of 2mmol 4h 2pO 4be dissolved in 15ml deionized water, be added dropwise in the mixing solutions of step (2) gained, stir 20min, guarantee that it mixes;
(4) under agitation condition, with rare nitric acid, regulate the pH=1 of final gained mixing solutions;
(5) above-mentioned mixing solutions is stirred to 60min, transfer in band teflon-lined stainless steel cauldron, sealing is reacted after 12h at 200 ℃, naturally cools to room temperature;
(6) by the throw out centrifugation obtaining (rotating speed is 10000r/min), centrifugation time is 5min, and water and ethanol repeated washing throw out, centrifugation, put into the dry 8h of 80 ℃ of loft drier, obtain the auxiliary synthetic nanometer rod pencil Eu doping YPO by CTAB 4nano particle.
Fig. 1 be utilize that prepared by method described in the embodiment of the present invention 1 by the auxiliary synthetic Eu doping YPO of Surfactant CTAB 4intersection nano rod bundle sample X ray diffracting spectrum, all diffraction peaks position in figure can be all YPO with six sides mutually 4(JCPDS Card42-0082) is corresponding for standard diffracting spectrum, shows that prepared sample is YPO 4.
Fig. 2 and Fig. 3 be utilize that prepared by method described in the embodiment of the present invention 1 by the auxiliary synthetic Eu doping YPO of Surfactant CTAB 4the field emission scanning electron microscope photo intersecting under nano rod bundle sample different multiples.From this two width figure, can find out the Eu doping YPO that CTAB is auxiliary synthetic 4become intersection cluster shape, the long 8-12 μ m of rod, diameter 1.5-2.5 μ m, the long 10 μ m of average rod, diameter 2 μ m, smooth surface, degree of crystallinity is high.
The present invention adopts Hydrothermal Synthesis system, and by the amount of adjusting reaction time, CTAB, the stoichiometric ratio of phosphate radical and rare earth ion etc. are to YPO 4: structure, the pattern of Eu intersection nano rod bundle are controlled, significant to exploitation novel fluorescent material.
Of the present invention by Surfactant CTAB auxiliary water thermal synthesis YPO 4the method of nano particle is applicable to synthetic other rare earth phosphate nano materials too.
The foregoing is only one embodiment of the present invention, is not unique embodiment, this area scientific research, and technician, by reading the present invention, not deviating from any equivalent transformation of doing under this technological process, is claim of the present invention and contains.

Claims (8)

1. by Surfactant CTAB, assist synthetic YPO for one kind 4the preparation method of nano particle, is characterized in that: comprise the following steps:
(1) prepare Y (NO 3) 3, Eu (NO 3) 3solution, CTAB solution and NH 4h 2pO 4solution, standby;
(2) get step 1) standby Y (NO 3) 3solution and Eu (NO 3) 3solution mixes, Y (NO after mixing 3) 3and Eu (NO 3) 3mol ratio be (9:1)-(4:1), in backward mixed solution, drip CTAB solution, after stirring, reaction generates Y xeu 1-xnO 3, rear dropping NH 4h 2pO 4solution, until Y xeu 1-xnO 3, CTAB, NH 4h 2pO 4three's mol ratio is 1:1:1, after obtain mixing solutions;
(3) regulating step 2) the mixing solutions pH value that obtains is to 1-3;
(4) by step 3) mixing solutions transfer in reactor after stirring and seal, at 120 ℃-200 ℃, be incubated 12-36h, generate precipitation to reaction, after by reactor cool to room temperature;
(5) by step 4) the throw out centrifugation that obtains, throw out is washed dry afterwards, finally obtain by the auxiliary synthetic YPO of Surfactant CTAB 4nano particle.
2. according to claim 1 a kind of by the auxiliary synthetic YPO of Surfactant CTAB 4the preparation method of nano particle, is characterized in that, in step (1):
Described Y (NO 3) 3the preparation method of solution: by Y 2o 3be dissolved in concentrated nitric acid, add the unnecessary concentrated nitric acid of heat abstraction, then to add deionized water to be made into concentration be 0.4molL -1y (NO 3) 3solution;
Described Eu (NO 3) 3the preparation method of solution: by Eu 2o 3be dissolved in concentrated nitric acid, add the unnecessary concentrated nitric acid of heat abstraction, then to add deionized water to be made into concentration be 0.2molL -1eu (NO 3) 3solution;
The preparation method of described CTAB solution: CTAB is joined in deionized water and heated and stirred is dissolved it, formation concentration is 0.1molL -1cTAB solution;
Described NH 4h 2pO 4the preparation method of solution: by NH 4h 2pO 4being dissolved in wiring solution-forming concentration in deionized water is 0.2molL -1.
3. according to claim 1 a kind of by the auxiliary synthetic YPO of Surfactant CTAB 4the preparation method of nano particle, is characterized in that, in step (2): described in be uniformly mixed liquid time be 20-30min.
4. according to claim 1 a kind of by the auxiliary synthetic YPO of Surfactant CTAB 4the preparation method of nano particle, is characterized in that, in step (3), regulating the reagent of mixing solutions pH value is rare nitric acid.
5. according to claim 1 a kind of by the auxiliary synthetic YPO of Surfactant CTAB 4the preparation method of nano particle, is characterized in that, in the churning time described in step (4), is 40-60min.
6. according to claim 1 a kind of by the auxiliary synthetic YPO of Surfactant CTAB 4the preparation method of nano particle, is characterized in that, at the reactor described in step (4), is stainless steel cauldron, and liner is tetrafluoroethylene, and reactor volume compactedness is 60%-80%.
7. according to claim 1 a kind of by the auxiliary synthetic YPO of Surfactant CTAB 4the preparation method of nano particle, is characterized in that, described throw out washing drying process is: by centrifugation postprecipitation thing, water and washing with alcohol, after put into the dry 8-12h of 70 ℃ of-80 ℃ of loft drier.
8. a kind of by the auxiliary synthetic YPO of Surfactant CTAB according to described in any one in claim 1-7 4the YPO that the preparation method of nano particle makes 4nano particle, is characterized in that: nano particle is cluster shape, and the long 8-12 μ m of rod, diameter 1.5-2.5 μ m.
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CN104830339A (en) * 2015-05-27 2015-08-12 陕西科技大学 Method for converting rare-earth-doped YPO4 (yttrium phosphate) crystal from hexagonal phase to tetragonal phase and improving luminescence property of rare-earth-doped YPO4 crystal
CN108384544A (en) * 2018-01-05 2018-08-10 东北大学 A kind of tetragonal YPO4:Ln3+Spherical fluorescent grain and preparation method

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CN104830339A (en) * 2015-05-27 2015-08-12 陕西科技大学 Method for converting rare-earth-doped YPO4 (yttrium phosphate) crystal from hexagonal phase to tetragonal phase and improving luminescence property of rare-earth-doped YPO4 crystal
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