CN105384192A - Method for preparing one-dimensional nanorod self-assembled flower type three-dimensional Nb2O5 - Google Patents

Method for preparing one-dimensional nanorod self-assembled flower type three-dimensional Nb2O5 Download PDF

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CN105384192A
CN105384192A CN201510809085.2A CN201510809085A CN105384192A CN 105384192 A CN105384192 A CN 105384192A CN 201510809085 A CN201510809085 A CN 201510809085A CN 105384192 A CN105384192 A CN 105384192A
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deionized water
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CN105384192B (en
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翟静
吴艳波
赵晓敏
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Yanshan University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G33/00—Compounds of niobium
    • 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
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/45—Aggregated particles or particles with an intergrown morphology

Abstract

The invention discloses a method for preparing one-dimensional nanorod self-assembled flower type three-dimensional Nb2O5. The method mainly comprises the following steps: by taking NbCl5, HO2CCO2H.2H2O and NH4F as raw materials, controlling the NH4F concentration and dripping speed, adding the mixed solution into a stainless steel high pressure reactor with a polytetrafluoroethylene liner under the condition that any surfactant and template agent are not added, reacting at the temperature of 160-220 DEG C for 16-20 hours, cooling to room temperature, taking the material out of the reactor, performing suction filtration on the solution, washing for several times so as to remove impurities by using deionized water, drying at the temperature of 60 DEG C for 2 hours, thereby obtaining a white powdery substance; performing high-temperature calcination on the white powdery substance at the temperature of 450-600 DEG C in a muffle furnace for 2 hours, thereby obtaining the flower type three-dimensional Nb2O5. The method disclosed by the invention is simple in operating process, low in time consumption, readily available in raw materials, non-toxic and harmless in solvent and environmentally friendly.

Description

A kind of monodimension nano stick is self-assembled into the three-dimensional Nb of flower pattern 2o 5preparation method
Technical field the invention belongs to field of material technology, particularly a kind of preparation method of nano material.
Background technology Nb 2o 5as a kind of important oxide material, because having outstanding physics and chemistry character, in fields such as photoelectrocatalysis, solar cell, biosensor, lithium ion battery and hybrid super capacitors, there is potential application, especially the application in hybrid super capacitor, cause the extensive concern of investigator in recent years, become the focus of research both at home and abroad, but Nb 2o 5lower specific conductivity itself and best crystalline structure shortcoming very rambunctious thereof constrain its application in hybrid super capacitor.Research shows that the pattern of control electrode material on slight level and microtexture can improve its specific conductivity, and has been reported the super capacitor anode material Co of one dimension, two dimension and three-dimensional (being assembled by the one dimension Nano structure) nanostructure obtained by controlling pattern 3o 4there is good chemical property, but also do not have preparation to be self-assembled into the three-dimensional Nb of flower pattern by monodimension nano stick at present 2o 5the relevant report of nano material.
Summary of the invention the object of the present invention is to provide the three-dimensional Nb that a kind of method is simple, raw material is easy to get, nontoxic monodimension nano stick is self-assembled into flower pattern 2o 5preparation method.
The present invention is mainly with NbCl 5, HO 2cCO 2h2H 2o, NH 4f is raw material, and the method adopting hydro-thermal reaction method to combine with high-temperature calcination prepares the three-dimensional Nb that monodimension nano stick is self-assembled into flower pattern 2o 5nano material.
Preparation method of the present invention is as follows:
(1) 0.273gNbCl is added by every 10mL deionized water 5ratio, vigorous magnetic stir under by NbCl 5be dissolved in deionized water, produce white flock precipitate, form white opacity liquid.
(2) by NbCl 5: HO 2cCO 2h2H 2o mol ratio is the ratio of 1:5, by the HO of 1M 2cCO 2h2H 2o dropwise adds in the white opacity liquid of step (1) gained until solution is transparent.
(3) 0.1389 ~ 0.2894gNH is added by every 10mL deionized water 4the ratio of F, by NH 4f is dissolved in deionized water, then the ratio of 3:2 by volume, by NH 4in the clear solution of F solution instillation step (2) gained, dropwise rear continuation and stir 2h.
(4) solution of step (3) is put into teflon-lined stainless steel autoclave, at 160 ~ 220 DEG C, react 16 ~ 20h.
(5) take out reactor after being cooled to room temperature, by solution suction filtration, with deionized water wash for several times to remove impurity, then at 60 DEG C of temperature dry 2h, obtain white powder material.
(6) white powder material step (5) obtained in 450 ~ 600 DEG C of high-temperature calcination 2h, obtains the three-dimensional Nb being self-assembled into flower pattern by monodimension nano stick in retort furnace 2o 5.
The present invention compared with prior art tool has the following advantages:
1, the three-dimensional Nb2O5 nano material being self-assembled into flower pattern by monodimension nano stick has been synthesized first.
2, without the need to adding any tensio-active agent and template.
3, this method operating process is simple, and consuming time few, raw material is easy to get, and nontoxic solvent is harmless, environmental friendliness.
Accompanying drawing explanation
Fig. 1 is that the monodimension nano stick that the embodiment of the present invention 1 obtains is self-assembled into the three-dimensional Nb of flower pattern 2o 5the XRD figure of nano material.
Fig. 2 is that the monodimension nano stick that the embodiment of the present invention 1 obtains is self-assembled into the three-dimensional Nb of flower pattern 2o 5the SEM figure of nano material.
Embodiment
Embodiment 1
By 0.546gNbCl under vigorous magnetic stirs 5be dissolved in 20mL deionized water, produce white flock precipitate, form white opacity liquid.Then by the HO of about 10mL1M 2cCO 2h2H 2o dropwise adds in this white opacity liquid until solution is transparent.The 0.3704gNH will taken again 4f is dissolved in the deionized water of 20mL, then by this NH 4f solution instills in the clear solution of above-mentioned gained, dropwises rear continuation and stirs 2h.This reaction solution is proceeded to 80mL with in teflon-lined stainless steel autoclave, 180 DEG C of reaction 18h, take out reactor after being cooled to room temperature, by product suction filtration, with deionized water wash for several times to remove impurity, then at 60 DEG C of temperature dry 2h, obtain white powder material.By this white powder material in retort furnace in 500 DEG C of high-temperature calcination 2h, obtain the three-dimensional Nb that monodimension nano stick is self-assembled into flower pattern 2o 5(as shown in Figure 2).Its crystalline structure is orthorhombic phase structure (as shown in Figure 1).
Embodiment 2
By 0.546gNbCl under vigorous magnetic stirs 5be dissolved in 20mL deionized water, produce white flock precipitate, form white opacity liquid.Then by the HO of about about 10mL 1M 2cCO 2h2H 2o dropwise adds until solution is transparent in this white opacity liquid, then the 0.2788gNH that will take 4f is dissolved in the deionized water of 20mL, then by this NH 4f solution instills in the clear solution of above-mentioned gained, dropwises rear continuation and stirs 2h.This reaction solution is proceeded to 80mL with in teflon-lined stainless steel autoclave, 160 DEG C of reaction 20h, take out reactor after being cooled to room temperature, by product suction filtration, with deionized water wash for several times to remove impurity, then at 60 DEG C of temperature dry 2h, obtain white powder material.By this white powder material in retort furnace in 550 DEG C of high-temperature calcination 2h, obtain the three-dimensional Nb that monodimension nano stick is self-assembled into flower pattern 2o 5nano material.Its crystalline structure is orthorhombic phase structure.
Embodiment 3
By 0.546gNbCl under vigorous magnetic stirs 5be dissolved in 20mL deionized water, produce white flock precipitate, form white opacity liquid.Then by the HO of about about 10mL 1M 2cCO 2h2H 2o dropwise adds in this white opacity liquid until solution is transparent.The 0.463gNH will taken again 4f is dissolved in the deionized water of 20mL, then by this NH 4f solution instills in the clear solution of above-mentioned gained, dropwises rear continuation and stirs 2h.This reaction solution is proceeded to 80mL with in teflon-lined stainless steel autoclave, 200 DEG C of reaction 16h, take out reactor after being cooled to room temperature, by product suction filtration, with deionized water wash for several times to remove impurity, then at 60 DEG C of temperature dry 2h, obtain white powder material.By this white powder material in retort furnace in 450 DEG C of high-temperature calcination 2h, obtain the Nb that monodimension nano stick is self-assembled into flower pattern 2o 5nano material.Its crystalline structure is orthorhombic phase structure.
Embodiment 4
By 0.546gNbCl under vigorous magnetic stirs 5be dissolved in 20mL deionized water, produce white flock precipitate, form white opacity liquid.Then by the HO of about about 10mL 1M 2cCO 2h2H 2o dropwise adds in this white opacity liquid until solution is transparent.The 0.5556gNH will taken again 4f is dissolved in the deionized water of 20mL, then by this NH 4f solution instills in the clear solution of above-mentioned gained, dropwises rear continuation and stirs 2h.This reaction solution is proceeded to 80mL with in teflon-lined stainless steel autoclave, 220 DEG C of reaction 16h, take out reactor after being cooled to room temperature, by product suction filtration, with deionized water wash for several times to remove impurity, then at 60 DEG C of temperature dry 2h, obtain white powder material.By this white powder material in retort furnace in 600 DEG C of high-temperature calcination 2h, obtain the Nb that monodimension nano stick is self-assembled into flower pattern 2o 5nano material.Its crystalline structure is orthorhombic phase structure.

Claims (1)

1. a monodimension nano stick is self-assembled into the three-dimensional Nb of flower pattern 2o 5preparation method, it is characterized in that: it comprises the steps:
(1) 0.273gNbCl is added by every 10mL deionized water 5ratio, vigorous magnetic stir under by NbCl 5be dissolved in deionized water, produce white flock precipitate, form white opacity liquid;
(2) by NbCl 5: HO 2cCO 2h2H 2the mol ratio of O is the ratio of 1:5, by 1MHO 2cCO 2h2H 2o dropwise adds in the white opacity liquid of step (1) gained until solution is transparent;
(3) 0.1389 ~ 0.2894gNH is added by every 10mL deionized water 4the ratio of F, by NH 4f is dissolved in deionized water, then the ratio of 3:2 by volume, by NH 4in the clear solution of F solution instillation step (2) gained, dropwise rear continuation and stir 2h;
(4) solution of step (3) is put into teflon-lined stainless steel autoclave, at 160 ~ 220 DEG C, react 16 ~ 20h;
(5) take out reactor after being cooled to room temperature, by solution suction filtration, with deionized water wash for several times to remove impurity, then at 60 DEG C of temperature dry 2h, obtain white powder material;
(6) white powder material step (5) obtained in 450 ~ 600 DEG C of high-temperature calcination 2h, obtains the three-dimensional Nb being self-assembled into flower pattern by monodimension nano stick in retort furnace 2o 5.
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Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN106115781A (en) * 2016-06-23 2016-11-16 南阳师范学院 A kind of Hemicentrotus seu Strongylocentrotus shape Nb2o5electrode material and preparation method thereof
CN106206077A (en) * 2016-06-30 2016-12-07 江苏大学 A kind of preparation method and its usage of nanometer niobium pentaoxide/FTO aqueous super capacitor electrode material
CN106532028A (en) * 2016-12-07 2017-03-22 南阳师范学院 Urchin-shaped niobium pentoxide used for negative electrode material of lithium ion battery, and preparation method for urchin-shaped niobium pentoxide
CN106517326A (en) * 2016-12-07 2017-03-22 南阳师范学院 Flower-like niobium pentoxide material and preparation method thereof
CN106542578A (en) * 2016-12-07 2017-03-29 南阳师范学院 A kind of Hemicentrotus seu Strongylocentrotuss shape niobium pentaoxide electrode material and preparation method thereof
CN106745255A (en) * 2016-12-07 2017-05-31 南阳师范学院 Sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchy and preparation method thereof
CN106809879A (en) * 2017-02-27 2017-06-09 湖南工业大学 A kind of niobium pentoxide nano stick material with regular hollow quadratic box-like and its preparation method and application
CN107359328A (en) * 2017-06-30 2017-11-17 陕西科技大学 A kind of preparation method of lithium ion battery botryoidalis niobium oxide/carbon composite electrode material

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106115781A (en) * 2016-06-23 2016-11-16 南阳师范学院 A kind of Hemicentrotus seu Strongylocentrotus shape Nb2o5electrode material and preparation method thereof
CN106206077A (en) * 2016-06-30 2016-12-07 江苏大学 A kind of preparation method and its usage of nanometer niobium pentaoxide/FTO aqueous super capacitor electrode material
CN106532028A (en) * 2016-12-07 2017-03-22 南阳师范学院 Urchin-shaped niobium pentoxide used for negative electrode material of lithium ion battery, and preparation method for urchin-shaped niobium pentoxide
CN106517326A (en) * 2016-12-07 2017-03-22 南阳师范学院 Flower-like niobium pentoxide material and preparation method thereof
CN106542578A (en) * 2016-12-07 2017-03-29 南阳师范学院 A kind of Hemicentrotus seu Strongylocentrotuss shape niobium pentaoxide electrode material and preparation method thereof
CN106745255A (en) * 2016-12-07 2017-05-31 南阳师范学院 Sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchy and preparation method thereof
CN106532028B (en) * 2016-12-07 2019-12-13 南阳师范学院 sea urchin-shaped niobium pentoxide for lithium ion battery cathode material and preparation method thereof
CN106809879A (en) * 2017-02-27 2017-06-09 湖南工业大学 A kind of niobium pentoxide nano stick material with regular hollow quadratic box-like and its preparation method and application
CN107359328A (en) * 2017-06-30 2017-11-17 陕西科技大学 A kind of preparation method of lithium ion battery botryoidalis niobium oxide/carbon composite electrode material
CN107359328B (en) * 2017-06-30 2019-12-20 陕西科技大学 Preparation method of grape-shaped niobium oxide/carbon composite electrode material for lithium ion battery

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