CN104528827A - Hydrothermal preparation method for nanometer NbO2F powder - Google Patents

Hydrothermal preparation method for nanometer NbO2F powder Download PDF

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Publication number
CN104528827A
CN104528827A CN201410856776.3A CN201410856776A CN104528827A CN 104528827 A CN104528827 A CN 104528827A CN 201410856776 A CN201410856776 A CN 201410856776A CN 104528827 A CN104528827 A CN 104528827A
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powder
nanometer
reactor
nbo2f
nbo
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CN104528827B (en
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唐培松
陈海锋
曹枫
潘国祥
张玉建
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Zhejiang Haite Alloy Co ltd
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Huzhou 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
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
    • 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
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/90—Other properties not specified above

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Abstract

The invention relates to a hydrothermal preparation method for nanometer NbO2F powder and relates to a preparation method for a niobium oxyfluoride nanometer material. According to the hydrothermal preparation method, the hydrothermal technology is used for preparing the nanometer NbO2F powder with the main raw materials of Nb2O5 powder, hydrofluoric acid with the concentration, by mass, of 20% and polyving akohol, wherein the mean grain size of the grains of the nanometer NbO2F powder ranges from 50 nm to 80 nm, the band gap of the nanometer NbO2F powder is 3.35 eV, and the nanometer NbO2F powder has the good photocatalytic activity. The hydrothermal preparation method comprises the two steps of preparing a reaction precursor and preparing nanometer powder under the hydrothermal condition. By means of the hydrothermal preparation method for the nanometer NbO2F powder, the technological cost is low, energy is saved, environmental friendliness is achieved, and industrial production is easy.

Description

Nanometer NbO 2the hydrothermal preparing process of F powder
Technical field
The present invention relates to the preparation of oxyfluoride nano material, particularly relate to a kind of nanometer NbO 2f raw powder's production technology.
Background technology
NbO 2f (a fluorodioxy niobium) is the one of oxyfluoride series, as document Journal of Power Sources, 2006,162:1312-1321, Journal of Solid State Chemistry, 2002,166:73-80 and Journal of PhysicalChemistry B, it is the same that 2005,109:13420-13423 etc. report, NbO 2f is a kind of semiconductor material, is with a wide range of applications in the field such as battery material and photochemical catalysis.
At present, NbO is prepared 2the method of F is more single, usually with metal niobium (Nb) powder and hydrofluoric acid (HF) for main raw material, adopt dissolving-method of evaporation to prepare.As niobium powder is dissolved in the hydrofluoric acid of 48% by document (Journal of Solid State Chemistry, 2002,166:73-80) report, evaporating solns, to dry, then dryly at 200 DEG C obtains product in 24 hours.Current preparation NbO 2there is length consuming time, easily contaminate environment in the dissolving-method of evaporation of F, cost is high and cannot obtain the deficiencies such as nanoscale product, and commercial application prospect causes anxiety.
Hydrothermal method typically refers in closed reactor (as reactor), adopt water as reaction system, by heating reaction system, create the reaction environment of a relatively-high temperature, high pressure, make usual indissoluble or insoluble substance dissolves and reaction or recrystallization, thus a kind of method of sintetics.Nanometer product prepared by hydrothermal method has that powder is thin, purity is high, good dispersity, narrowly distributing, crystal formation are good usually, and technique is simple, is easy to the advantage such as industrialization and efficient energy-saving.Hydrothermal method has a wide range of applications in nano material synthesis field.At present, hydrothermal method is adopted to prepare nanometer NbO 2f powder have not been reported.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of directly synthesis of nano NbO is provided 2the hydrothermal preparing process of F powder.
The object of the invention is to be achieved through the following technical solutions, concrete steps are:
(1) preparation of precursors
At ambient temperature, X mole of Nb is taken 2o 5powder, proceeds to powder and has in teflon-lined reactor; In stink cupboard, in reactor, add Y mole of HF, and then add polyvinyl alcohol (PVA-124) the solution Z milliliter that concentration is 2.0g/L, stir with glass stick, obtain precursors.
(2) preparation of nano-powder under hydrothermal condition
Reactor sealing is placed on isothermal reaction in the baking oven of 180 DEG C ~ 190 DEG C, after 12 ~ 24 hours, allows reactor naturally cool to room temperature in an oven; Product in reactor is poured in plastic beaker, filters and washing, finally product is dried in 60 DEG C to 80 DEG C baking ovens and obtain nanometer NbO 2f powder product.
X is limited to 0.005 mole to 0.015 molar range by the present invention, Y is limited to 0.125 mole to 0.75 molar range, controls to make Y: X to equal 25: 1 to 50: 1 scope; Z is limited to 3 milliliters to 9 milliliters scopes, controls to make Z: X to equal 600: 1.The HF used in reaction is the solution of HF, to be namely mass percentage concentration be 20% hydrofluoric acid solution; The molar weight of Y is calculated by the mass percentage of HF in hydrofluoric acid solution, employs the hydrofluoric acid solution 12.5 grams that mass percentage concentration is 20% as referred to when Y is 0.125 mole.
Compared with prior art, positively effect of the present invention is:
(1) the present invention adopts relatively cheap Nb 2o 5powder instead of expensive metal Nb powder, and (document commonly uses the HF solution of 48% or the HF solution of 48% and HNO to use the HF solution of relatively cheap 20% 3the solution that solution is made into), save cost.
(2) reaction process is carried out in closed reactor, does not have the direct discharge of HF (HF belongs to toxic substance) in experimentation, makes technique safety and environmental protection more.
(3) in reaction system, add polyvinyl alcohol (PVA-124) solution, the dissemination of polyvinyl alcohol is nanometer NbO 2the formation of F creates condition.
(4) nanometer NbO has been prepared 2f is NbO 2f lays a good foundation in the application of wider scope.
In a word, compared with prior art, the positively effect that the present invention adopts hydrothermal method to prepare is: achieve that cost is low, energy-conserving and environment-protective, be easy to suitability for industrialized production nanoscale product NbO 2the object of F powder.
Accompanying drawing explanation
Fig. 1: embodiment 1 gained NbO 2the X ray diffracting spectrum of F product;
Fig. 2: embodiment 1 gained NbO 2f product retouch electromicroscopic photograph;
Fig. 3: embodiment 1 gained NbO 2the UV-Vis DRS absorption spectrum of F product;
Fig. 4: embodiment 1 gained NbO 2f product and the percent of decolourization curve over time for the commodity titanium dioxide P25 photo-catalytic degradation of methyl-orange of reference.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail.This specific embodiment is only explanation of the invention; it is not limitation of the present invention; those skilled in the art can make to the present embodiment the amendment not having creative contribution as required, as long as but be all subject to the protection of patent law in right of the present invention.
Embodiment 1
At ambient temperature, 0.005 mole of Nb is taken 2o 5powder, powder is proceeded to volume be 100ml have in teflon-lined reactor; In stink cupboard, 0.25 mole of HF (namely 25 gram mass percentage concentrations are the hydrofluoric acid solution of 20%) is added in reactor, and then add polyvinyl alcohol (PVA-124) the solution 3ml that concentration is 2.0g/L, after stirring with glass stick, reactor is sealed.Baking oven isothermal reaction reactor being placed in 180 DEG C, after 24 hours, allows reactor naturally cool to room temperature in an oven, pours in plastic beaker by the product in reactor, filters and washs 3 times, is finally put into by product in 80 DEG C of baking ovens to dry to obtain Nb 2o 5powder product.To the product obtained carry out respectively X-ray diffraction analysis (XRD), scanning electron microscope (SEM) and UV-Vis DRS absorption spectrum (DRS) test, result as shown in Figure 1, Figure 2 and Figure 3.
Fig. 1 adopts XD-6 type X-ray diffraction analysis instrument, the XRD figure of powder method analytical test product.As can be seen from Figure 1, the XRD figure spectrum of products obtained therefrom and the NbO of standard 2f (JCPDS:47-1231) coincide, and illustrates that the product of synthesis is NbO 2f.
Fig. 2 is the SEM photo adopting Hitachi S-4800 type field emission scanning electron microscope test products.As can be seen from Figure 2, NbO 2f product exists for master with the particle of median size 50 ~ 80nm.
Fig. 3 is the Hitachi UV4100 type ultraviolet-visible spectrometer adopting band integrating sphere, with the BaSO of standard 4make reference, by NbO 2f pressed powder, then carries out test and obtains UV-Vis DRS spectrum, and be converted to diffuse-reflectance absorption spectrum by Kubelka-Munk equation.As can be seen from Figure 3, NbO 2the ABSORPTION EDGE wavelength X of F is 370nm.Formula E (eV)=1240/ λ is utilized to calculate NbO 2the band gap width of F is 3.35eV.
In order to characterize NbO 2the photocatalytic activity of F nano-powder, photochemical catalysis experiment is carried out in homemade photocatalytic reaction device: light source is 150W high voltage mercury lamp; By 20mg nanometer NbO 2f powder joins in simulated sewage tropeolin-D (MO) solution of 10ml 20mg/L, carries out photocatalytic degradation experiment after lucifuge adsorption equilibrium 10min; Take out centrifugation after degraded required time and remove powder, calculate its percent of decolourization with the typical curve of MO solution maximum absorption band 464nm place absorbancy, compare photochemical catalysis experiment with the commodity titanium dioxide P25 that academia is conventional, experimental result as shown in Figure 4.As can be seen from Figure 4, NbO 2f increases sharply to before MO solution degradation percent of decolourization 30min, degradable close to 100% when having reached 95.3%, 60min during 50min, NbO 2f product expression has gone out excellent photocatalytic activity.Although and reference P25 is increasing the degradation and decolorization rate of MO solution, just reach 69% during 60min, this is showing NbO 2the photocatalytic activity of F product is better than P25.
Embodiment 2
At ambient temperature, 0.015 mole of Nb is taken 2o 5powder, powder is proceeded to volume be 100ml have in teflon-lined reactor; In stink cupboard, the HF (namely 37.5 gram mass percentage concentrations are the hydrofluoric acid solution of 20%) of 0.375 mole is added in reactor, and then add polyvinyl alcohol (PVA-124) the solution 9ml that concentration is 2.0g/L, after stirring with glass stick, reactor is sealed.Baking oven isothermal reaction reactor being placed in 190 DEG C, after 18 hours, allows reactor naturally cool to room temperature in an oven, pours in plastic beaker by the product in reactor, filters and washs 3 times, is finally put into by product in 60 DEG C of baking ovens to dry to obtain nanometer NbO 2f powder product.According to the photochemical catalysis experimental technique that embodiment 1 is identical, during the MO solution 50min of photocatalytic degradation 20mg/L, reach 100% degradable when MO percent of decolourization reaches 95.6%, 60min, NbO 2f product expression has gone out excellent photocatalytic activity.
Embodiment 3
At ambient temperature, 0.10 mole of Nb is taken 2o 5powder, powder is proceeded to volume be 100ml have in teflon-lined reactor; In stink cupboard, add in reactor 4.0 moles (namely 40 gram mass percentage concentrations are the hydrofluoric acid solution of 20%), and then add polyvinyl alcohol (PVA-124) the solution 6ml that concentration is 2.0g/L, after stirring with glass stick, reactor is sealed.Baking oven isothermal reaction reactor being placed in 190 DEG C, after 12 hours, allows reactor naturally cool to room temperature in an oven, pours in plastic beaker by the product in reactor, filters and washs 3 times, is finally put into by product in 70 DEG C of baking ovens to dry to obtain nanometer NbO 2f powder product.According to the photochemical catalysis experimental technique that embodiment 1 is identical, during the MO solution 50min of photocatalytic degradation 20mg/L, reach 100% degradable when MO percent of decolourization reaches 95.1%, 60min, NbO 2f product expression has gone out excellent photocatalytic activity.

Claims (2)

1. nanometer NbO 2the hydrothermal preparing process of F powder, is characterized in that comprising the following steps: (1) at ambient temperature, takes X mole of Nb 2o 5powder, proceeds to powder and has in teflon-lined reactor; In stink cupboard, in reactor, add Y mole of HF, and then add polyvinyl alcohol (PVA-124) the solution Z milliliter that concentration is 2.0g/L, stir with glass stick, obtain precursors; (2) reactor sealing to be placed in the baking oven of 180 DEG C ~ 190 DEG C isothermal reaction after 12 ~ 24 hours, reactor is allowed to naturally cool to room temperature in an oven, product in reactor is poured in plastic beaker, filter and washing, finally product is dried in 60 DEG C to 80 DEG C baking ovens and obtain nanometer NbO 2f powder product.
2. the nanometer NbO in claim 1 2the hydrothermal preparing process of F powder, it is characterized in that X being limited to 0.005 mole to 0.015 molar range, Y is limited to 0.125 mole to 0.75 molar range, controls to make Y: X to equal 25: 1 to 50: 1 scope; Z is limited to 3 milliliters to 9 milliliters scopes, controls to make Z: X to equal 600: 1.
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN107117655A (en) * 2017-06-27 2017-09-01 中国矿业大学 A kind of two-phase coexistent Nb3O7The preparation method of F nano-particles
CN107473267A (en) * 2017-09-13 2017-12-15 中国矿业大学 Economical, safe and environment-friendly Nb3O7Preparation method of F nano material
CN110294495A (en) * 2019-05-28 2019-10-01 山东理工大学 A method of preparing TaO2F nanometer rods
CN110357158A (en) * 2019-05-28 2019-10-22 山东理工大学 A kind of three-dimensional sea urchin shape nanostructure TaO2The preparation method of F material
CN111137921A (en) * 2020-01-04 2020-05-12 山东理工大学 Preparation method of tantalum oxyfluoride nanosheet

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C. BOHNKE ET AL.: "Electrochemical intercalation of lithium into the perovskite-type NbO2F: influence of the NBO2F particle size", 《J SOLID STATE ELECTROCHEM》 *
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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN107117655A (en) * 2017-06-27 2017-09-01 中国矿业大学 A kind of two-phase coexistent Nb3O7The preparation method of F nano-particles
CN107473267A (en) * 2017-09-13 2017-12-15 中国矿业大学 Economical, safe and environment-friendly Nb3O7Preparation method of F nano material
CN110294495A (en) * 2019-05-28 2019-10-01 山东理工大学 A method of preparing TaO2F nanometer rods
CN110357158A (en) * 2019-05-28 2019-10-22 山东理工大学 A kind of three-dimensional sea urchin shape nanostructure TaO2The preparation method of F material
CN110294495B (en) * 2019-05-28 2021-12-14 山东理工大学 Preparation of TaO2Method for F nano rod
CN110357158B (en) * 2019-05-28 2021-12-14 山东理工大学 Three-dimensional sea urchin-shaped nano-structure TaO2Preparation method of F material
CN111137921A (en) * 2020-01-04 2020-05-12 山东理工大学 Preparation method of tantalum oxyfluoride nanosheet
CN111137921B (en) * 2020-01-04 2022-05-20 山东理工大学 Preparation method of tantalum oxyfluoride nanosheet

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