CN105481011A - Method for hydrothermally preparing neodymium vanadate nanorod array - Google Patents

Method for hydrothermally preparing neodymium vanadate nanorod array Download PDF

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CN105481011A
CN105481011A CN201510955778.2A CN201510955778A CN105481011A CN 105481011 A CN105481011 A CN 105481011A CN 201510955778 A CN201510955778 A CN 201510955778A CN 105481011 A CN105481011 A CN 105481011A
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hydro
neodymium
vanadic acid
stick array
nanometer stick
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田俐
赵瑞妮
王金晶
王会锋
李斐
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Hunan University of Science and Technology
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Hunan University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a method for hydrothermally preparing a neodymium vanadate nanorod array. The method mainly comprises the steps that a neodymium nitrate aqueous solution of 0.5 mol/L and a Na2EDTA aqueous solution are mixed to be uniform under magnetic stirring, and then a sodium vanadate aqueous solution of 0.5 mol/L is added; the pH of the initial solution is adjusted to 10, after stirring is conducted for a period of time, the initial solution is moved into a hydrothermal reaction kettle, a hydrothermal reaction is conducted for 6-36 h on the condition that the temperature ranges from 180 DEG C to 220 DEG C, centrifugal separation is conducted, precipitate is washed with absolute ethyl alcohol and water and then dried, and the neodymium vanadate nanorod array is obtained. According to the method, the neodymium vanadate nanorod array is synthesized through a hydrothermal method, and the method has the advantages of being simple in technology, convenient to operate, mild in reaction condition, low in cost, environmentally friendly and the like. The obtained product is high in purity, good in crystalline form and strong in regulation capacity; self-assembly of nanocrystals is achieved in the growth and preparation processes, the industrial production conditions and the environment-friendly requirement are met, and scale production is facilitated.

Description

A kind of hydro-thermal prepares the method for vanadic acid neodymium nanometer stick array
Technical field
The invention belongs to rare earth luminescent material preparing technical field, be specifically related to a kind of method that hydro-thermal prepares vanadic acid neodymium nanometer stick array.
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, about the research of rare earth nano functional materials finds, the microstructure of functional materials such as grain size, dimension, crystal morphology, crystallinity, particle dispersion etc. have a significant impact optical, electrical, the catalytic performance of device and the machining property of material.In addition, the ordered structure being various yardstick by brilliant for mono-dispersed nano self-assembly can produce more excellent overall coordination character, this constructs the basis with complex function superstructure body, for constructing novel nano device based on nano material, expansion Monodisperse nanocrystals has great importance in the application of the more areas such as catalysis, solar cell, nanometer biotechnology.
Vanadic acid neodymium is a kind of important rare earth compound, usually belongs to cubic Zircon cut structure, has good optical property and photocatalysis performance.It all has potential using value in optical, electrical, the field such as magnetic and catalysis.Vanadic acid neodymium nanometer stick array is hopeful to show more excellent, novel performance.At present, NdVO is prepared 4method to mainly contain ultrasonic method, template, hydrothermal method, microwave method, sol-gel method, composite fused salt method etc. multiple, the structure directing agent that CTAB and P123 two kinds is different as used by ultrasonic method or microwave method synthesis NdVO 4nano particle, with (NH 4) 0.5v 2o 5nano wire does template hydrothermal method two step and has synthesized NdVO 4nanometer rod, by composite fused salt method NdCl 36H 2o and V 2o 5for Material synthesis NdVO 4nano wire etc.But these methods mainly prepare monodispersed NdVO 4, and preparation method is more complicated, condition is harsh, and environment is unfriendly, and cost is higher.
Summary of the invention
The object of the invention is to overcome the shortcoming existed in above-mentioned prior art, there is provided that a kind of preparation method is simple, mild condition, with low cost, environmental friendliness, particle purity are high, good crystalline and have the hydro-thermal of stronger ability of regulation and control to prepare the method for vanadic acid neodymium nanometer stick array
Hydro-thermal of the present invention prepares the method for vanadic acid neodymium nanometer stick array, comprises the steps:
(1) by 0.5mol/L aqueous neodymium nitrate and Na 2the EDTA aqueous solution mixes under magnetic stirring, obtains mixed liquor A, wherein neodymium nitrate and Na 2the molar ratio range of EDTA is 1:1 ~ 1:1.25;
(2) by ammonium meta-vanadate and sodium hydroxide, be dissolved in distilled water, be stirred to and dissolve completely, the sodium vanadate solution of obtained 0.5mol/L, obtains mixed liquid B;
(3) join in mixed liquor A by mixed liquid B, wherein the mol ratio of Nd, V and NaOH is 1:1:2, and the pH of regulator solution is 10, after magnetic agitation 10min, is transferred in tetrafluoroethylene reactor, and hydrothermal temperature is react 6 ~ 48h at 180 ~ 220 DEG C;
(4), after hydro-thermal reaction terminates, after question response still naturally cools to room temperature, centrifugation, with distilled water and dehydrated alcohol washing precipitation several times respectively, after oven dry, obtains vanadic acid neodymium nanometer stick array.
Concrete, in step (3), the Nd (NO in final mixed solution 3) 3, Na 3vO 4and Na 2the mol ratio of EDTA three is 1:1:1.1 ~ 1:1:1.25.
Concrete, in step (3), the pH adopting the NaOH regulator solution of 4M is 10.
Concrete, the temperature of step (3) described hydro-thermal reaction is 180 ~ 200 DEG C.
Concrete, step (3) described hydro-thermal reaction is carried out in teflon-lined autoclave, and reactor volume compactedness is 60%.
Concrete, described in step (4), washing precipitation number of times is 2 times, and drying temperature is 60 ~ 70 DEG C, and dry environment is loft drier, and time of drying is about 12h.
Compared with prior art, the present invention has following beneficial effect: preparation method of the present invention selects hydrothermal method to prepare, by the Nd (NO in adjusting reaction time, initial action solution 3) 3, Na 2eDTA and NaVO 4mol ratio, synthesized vanadic acid neodymium nanometer stick array.Present invention process route is simple, with low cost, is easy to control; Obtained vanadic acid neodymium nanometer stick array, purity is high, pattern is single, self-assembly good, nanometer rod size uniform in gained array, length reaches hundreds of nanometer, and diameter is about tens nanometer, arrangement is closely neat, individual nanorod length and array area size control by reaction conditions, and to achieve nanocrystal simultaneously self-assembly in the process of growth and preparation be array, significant to exploitation novel fluorescent material.
Accompanying drawing explanation
The XRD figure of the vanadic acid neodymium nanometer stick array of Fig. 1 prepared by the embodiment of the present invention 1 to embodiment 5, the vanadic acid neodymium of preparation is Tetragonal.
Fig. 2 to Fig. 5 is respectively the stereoscan photograph (adopting the JSM-6380LV type scanning electronic microscope of NEC Zhu Shi commercial firm, acceleration voltage 20kV) of the embodiment of the present invention 1, embodiment 2, embodiment 4, vanadic acid neodymium nanometer stick array prepared by embodiment 5.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1:
(1) by 1mmolNa 2eDTA is dissolved in 5ml distilled water, after stirring, adds the neodymium nitrate solution of 2ml0.5mol/L, is stirred to and evenly obtains mixed liquor A;
(2) by 1mmolNH 4vO 3be dissolved in the distilled water of 5mL with 2mmolNaOH, be stirred to and dissolve completely, obtain mixed liquid B;
(3) mixed liquid B is joined in mixed liquor A, by the NaOH solution adjust ph to 10 of 4mol/L, after magnetic agitation 10min, be transferred to in teflon-lined autoclave, hydro-thermal reaction 6h at 180 DEG C;
(4) after hydro-thermal reaction terminates, after question response still naturally cools to room temperature, centrifugation, distinguishes washing precipitation 2 times with distilled water and dehydrated alcohol, after 60 DEG C of oven dry 12h, obtains vanadic acid neodymium nanometer stick array; As shown in curve in Fig. 11, all diffraction peaks of product can with the NdVO of bottom 4base peak (JCPDSNo.15-0769) corresponding.Figure 2 shows that the stereoscan photograph of prepared vanadic acid neodymium nanometer stick array.
Embodiment 2:
(1) by 1.15mmolNa 2eDTA is dissolved in 5ml distilled water, after stirring, adds the neodymium nitrate solution of 2ml0.5mol/L, is stirred to and evenly obtains mixed liquor A;
(2) by 1mmolNH 4vO 3be dissolved in the distilled water of 5mL with 2mmolNaOH, be stirred to and dissolve completely, obtain mixed liquid B;
(3) mixed liquid B is joined in mixed liquor A, by the NaOH solution adjust ph to 10 of 4mol/L, after magnetic agitation 10min, be transferred to in teflon-lined autoclave, hydro-thermal reaction 24h at 180 DEG C;
(4) after hydro-thermal reaction terminates, after question response still naturally cools to room temperature, centrifugation, distinguishes washing precipitation 2 times with distilled water and dehydrated alcohol, after 70 DEG C of oven dry 12h, obtains vanadic acid neodymium nanometer stick array; As shown in curve in Fig. 12, all diffraction peaks of product can with the NdVO of bottom 4base peak (JCPDSNo.15-0769) corresponding.Figure 3 shows that the stereoscan photograph of prepared vanadic acid neodymium nanometer stick array.
Embodiment 3:
(1) by 1.25mmolNa 2eDTA is dissolved in 5ml distilled water, after stirring, adds the neodymium nitrate solution of 2ml0.5mol/L, is stirred to and evenly obtains mixed liquor A;
(2) by 1mmolNH 4vO 3be dissolved in the distilled water of 5mL with 2mmolNaOH, be stirred to and dissolve completely, obtain mixed liquid B;
(3) mixed liquid B is joined in mixed liquor A, by the NaOH solution adjust ph to 10 of 4mol/L, after magnetic agitation 10min, be transferred to in teflon-lined autoclave, hydro-thermal reaction 24h at 180 DEG C;
(4) after hydro-thermal reaction terminates, after question response still naturally cools to room temperature, centrifugation, distinguishes washing precipitation 2 times with distilled water and dehydrated alcohol, after 60 DEG C of oven dry 12h, obtains vanadic acid neodymium nanometer stick array; As shown in curve in Fig. 13, all diffraction peaks of product can with the NdVO of bottom 4base peak (JCPDSNo.15-0769) corresponding.
Embodiment 4:
(1) by 1.15mmolNa 2eDTA is dissolved in 5ml distilled water, after stirring, adds the neodymium nitrate solution of 2ml0.5mol/L, is stirred to and evenly obtains mixed liquor A;
(2) by 1mmolNH 4vO 3be dissolved in the distilled water of 5mL with 2mmolNaOH, be stirred to and dissolve completely, obtain mixed liquid B;
(3) mixed liquid B is joined in mixed liquor A, by the NaOH solution adjust ph to 10 of 4mol/L, after magnetic agitation 10min, be transferred to in teflon-lined autoclave, hydro-thermal reaction 36h at 220 DEG C;
(4) after hydro-thermal reaction terminates, after question response still naturally cools to room temperature, centrifugation, distinguishes washing precipitation 2 times with distilled water and dehydrated alcohol, after 70 DEG C of oven dry 12h, obtains vanadic acid neodymium nanometer stick array; As shown in curve in Fig. 14, all diffraction peaks of product can with the NdVO of bottom 4base peak (JCPDSNo.15-0769) corresponding.Figure 4 shows that the stereoscan photograph of prepared vanadic acid neodymium nanometer stick array.
Embodiment 5:
(1) by 1.15mmolNa 2eDTA is dissolved in 5ml distilled water, after stirring, adds the neodymium nitrate solution of 2ml0.5mol/L, is stirred to and evenly obtains mixed liquor A;
(2) by 1mmolNH 4vO 3be dissolved in the distilled water of 5mL with 2mmolNaOH, be stirred to and dissolve completely, obtain mixed liquid B;
(3) mixed liquid B is joined in mixed liquor A, by the NaOH solution adjust ph to 10 of 4mol/L, after magnetic agitation 10min, be transferred to in teflon-lined autoclave, hydro-thermal reaction 48h at 180 DEG C;
(4) after hydro-thermal reaction terminates, after question response still naturally cools to room temperature, centrifugation, distinguishes washing precipitation 2 times with distilled water and dehydrated alcohol, after 60 DEG C of oven dry 12h, obtains vanadic acid neodymium nanometer stick array; As shown in curve in Fig. 15, all diffraction peaks of product can with the NdVO of bottom 4base peak (JCPDSNo.15-0769) corresponding.Figure 5 shows that the stereoscan photograph of prepared vanadic acid neodymium nanometer stick array.
From above-described embodiment, the present invention adopts hydrothermal method, by the Na in adjusting reaction time, initial action solution 2the amount of EDTA, has synthesized vanadic acid neodymium nanometer stick array.Compared with existing synthetic method, present invention process route is simple, with low cost, is easy to control, obtained vanadic acid neodymium nanometer stick array, purity is high, pattern is single, self-assembly is good, nanometer rod size uniform in gained array, length can reach hundreds of nanometer, diameter is about tens nanometer, arrangement is closely neat, the assembling area of individual nanorod length and array regulates and controls by controlling reaction conditions, the superlattice assembly inorganic Monodisperse nanocrystals being built into rule is the basis constructing the novel micro nanometer rice device with complex function superstructure body further, and this can expand Monodisperse nanocrystals in catalysis, solar cell, the application of the more areas such as nanometer biotechnology.

Claims (6)

1. hydro-thermal prepares a method for vanadic acid neodymium nanometer stick array, it is characterized in that comprising the steps:
(1) by 0.5mol/L aqueous neodymium nitrate and Na 2the EDTA aqueous solution mixes under magnetic stirring, obtains mixed liquor A, wherein neodymium nitrate and Na 2the molar ratio range of EDTA is 1:1 ~ 1:1.25;
(2) by ammonium meta-vanadate and sodium hydroxide, be dissolved in distilled water, be stirred to and dissolve completely, the sodium vanadate solution of obtained 0.5mol/L, obtains mixed liquid B;
(3) join in mixed liquor A by mixed liquid B, wherein the mol ratio of Nd, V and NaOH is 1:1:2, and the pH of regulator solution is 10, after magnetic agitation 10min, is transferred in tetrafluoroethylene reactor, and hydrothermal temperature is react 6 ~ 48h at 180 ~ 220 DEG C;
(4), after hydro-thermal reaction terminates, after question response still naturally cools to room temperature, centrifugation, with distilled water and dehydrated alcohol washing precipitation several times respectively, after oven dry, obtains vanadic acid neodymium nanometer stick array.
2. hydro-thermal prepares the method for vanadic acid neodymium nanometer stick array according to claim 1, it is characterized in that: in step (3), the Nd (NO in described final mixed solution 3) 3, Na 3vO 4and Na 2the mol ratio of EDTA three is 1:1:1.1 ~ 1:1:1.25.
3. hydro-thermal prepares the method for vanadic acid neodymium nanometer stick array according to claim 1, it is characterized in that: in step (3), and the pH adopting the NaOH regulator solution of 4M is 10.
4. hydro-thermal prepares the method for vanadic acid neodymium nanometer stick array according to claim 1, it is characterized in that: the temperature of step (3) described hydro-thermal reaction is 180 ~ 200 DEG C.
5. hydro-thermal prepares the method for vanadic acid neodymium nanometer stick array according to claim 1, it is characterized in that: step (3) described hydro-thermal reaction is carried out in teflon-lined autoclave, and reactor volume compactedness is 60%.
6. hydro-thermal prepares the method for vanadic acid neodymium nanometer stick array according to claim 1, it is characterized in that: described in step (4), washing precipitation number of times is 2 times, and drying temperature is 60 ~ 70 DEG C, and dry environment is loft drier, and time of drying is about 12h.
CN201510955778.2A 2015-12-17 2015-12-17 Method for hydrothermally preparing neodymium vanadate nanorod array Pending CN105481011A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106082336A (en) * 2016-07-26 2016-11-09 安徽建筑大学 The preparation method of rare earth Yttrium Orthovanadate

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CN101786662A (en) * 2010-03-22 2010-07-28 北京化工大学 Cerium vanadate nano-rod assembly and preparation method thereof
CN102140691A (en) * 2011-02-12 2011-08-03 河北联合大学 Method for synthesizing vanadium acid zinc micro/nanowire material by adopting hydrothermal method
CN102320658A (en) * 2011-07-22 2012-01-18 河北联合大学 Method for synthesizing alkaline earth metal vanadate micro/nano materials by adopting hydrothermal/solvothermal method

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN101786662A (en) * 2010-03-22 2010-07-28 北京化工大学 Cerium vanadate nano-rod assembly and preparation method thereof
CN102140691A (en) * 2011-02-12 2011-08-03 河北联合大学 Method for synthesizing vanadium acid zinc micro/nanowire material by adopting hydrothermal method
CN102320658A (en) * 2011-07-22 2012-01-18 河北联合大学 Method for synthesizing alkaline earth metal vanadate micro/nano materials by adopting hydrothermal/solvothermal method

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106082336A (en) * 2016-07-26 2016-11-09 安徽建筑大学 The preparation method of rare earth Yttrium Orthovanadate

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